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TMECC

The document outlines the development of a manual for test methods related to composting and compost, prepared by the U.S. Department of Agriculture and the U.S. Composting Council. It details the phases of the Minnesota Compost Utilization Project, which aimed to standardize testing protocols for compost analysis, and emphasizes the importance of safety, ongoing revisions, and collaborative evaluation. The manual serves as a comprehensive guide for scientifically sound testing methods applicable to composting feedstocks and finished compost.

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0% found this document useful (1 vote)
998 views457 pages

TMECC

The document outlines the development of a manual for test methods related to composting and compost, prepared by the U.S. Department of Agriculture and the U.S. Composting Council. It details the phases of the Minnesota Compost Utilization Project, which aimed to standardize testing protocols for compost analysis, and emphasizes the importance of safety, ongoing revisions, and collaborative evaluation. The manual serves as a comprehensive guide for scientifically sound testing methods applicable to composting feedstocks and finished compost.

Uploaded by

ibtalbertogp
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd

JOINT PROJECT OF THE UNITED STATES DEPARTMENT OF AGRICULTURE AND THE UNITED STATES COMPOSTING COUNCIL

Preface

Prepared for:
THE US COMPOSTING COUNCIL RESEARCH AND EDUCATION FOUNDATION, AND
THE UNITED STATES DEPARTMENT OF AGRICULTURE

Editor in Chief:
Wayne H. Thompson

Co-Editors:
Philip B. Leege
Patricia D. Millner
Maurice E. Watson

Test Methods for the Examination of Composting and Compost August 12, 2001
iii
DISCLAIMERS
(1) The methodologies described in TMECC do not purport to address all safety concerns associated with their
use. It is the responsibility of the user of these methods to establish appropriate safety and health practices,
and to determine the applicability of regulatory limitations prior to their use.
(2) All methods and sampling protocols provided in TMECC are subject to revision and update to correct any
errors or omissions, and to accommodate new widely accepted advances in techniques and methods. Please
report omissions and errors to the U.S. Composting Council Research and Education Foundation. An on-line
submission form and instructions are provided on the TMECC web site, http://www.tmecc.org/addenda.
(3) Process alternatives, trade names, or commercial products as mentioned in TMECC are only examples and
are not endorsed or recommended by the U.S. Department of Agriculture or the U.S. Composting Council
Research and Education Foundation. Alternatives may exist or may be developed.

The U.S. Department of Agriculture (USDA) prohibits discrimination in all its programs and activities on
the basis of race, color, national origin, sex, religion, age, disability, political beliefs, sexual orientation,
and marital or family status. (Not all prohibited bases apply to all programs.) Persons with disabilities who
require alternative means for communication of program information (Braille, large print, audiotape, etc.)
should contact USDA's TARGET Center at (202) 720-2600 (voice and TDD).
To file a complaint of discrimination, write USDA, Director, Office of Civil Rights, Room 326-W, Whitten
Building, 1400 Independence Avenue, SW, Washington, DC 20250-9410 or call (202) 720-5964 (voice or
TDD). USDA is an equal opportunity provider and employer.
Preface

MANUAL DEVELOPMENT

This manual of test methods has benefited from the Phase II—Temporal Variability. Sampling continued
expertise and input of numerous individuals. In on a monthly basis for one year at the previously
addition, several groups cooperated and many mentioned sites. Five additional facilities were added
contributors provided valuable suggestions for for the duration of the first year’s monthly sampling
improvement. Throughout its development, the focus phase.
always remained on producing a technically sound Phase III—Temporal Variability. Sampling frequency
manual of test methods and protocols. The was decreased to a quarterly basis for seven facilities
development stages of the TMECC project are during the second year of sampling. One facility was
described below. lost to fire.
Stage 1. Project Concept Development Test Parameters from MN-CUP
The US Composting Council's Standards and Practices During the MN-CUP project, approximately 40
Committee and Markets Development Committee parameters were considered. The methods were
developed a list of key process variables to measure modified and adapted from existing ASTM, ASA-
and manage, and attributes to report for the following: SSSA, SW-846 and AOAC methods developed for
composting feedstock; the composting process; other materials. Test parameters considered:
finished compost, product safety and regulatory
compliance, and marketing claims. I. Chemical Analyses—using US EPA 3051
digest modified for compost’s high organic matter and
Stage 2. Minnesota Compost Utilization Project ICP-AES determinations for metals and salts; cold
(MN-CUP) vapor for Hg; wet combustion determination for N
(total Kjeldahl nitrogen, micro-digest technique);
The Standards and Practices Committee worked
cooperatively with the Minnesota Office of colorimetric NO3 and NH4; and cation exchange
capacity (modified ammonium displacement technique
Environmental Assistance, the University of
Minnesota’s Department of Soil, Water, and Climate on milled material).
Research Analytical Laboratory, and Malcolm Pirnie II. Physical Analyses—for total solids and
for two years to survey eight municipal solid waste moisture (wet basis); ash (volatile solids); man-made
composting facilities in Minnesota. This was an inerts (plastics, metal, glass); bulk density; water-
observational study designed to document feedstock, holding capacity; and air-capacity.
in-process and finished compost sampling and III. Biological Analyses—for stability (oxygen
preservation protocols, laboratory preparation steps and uptake); growth and germination (a direct seeding
analytical methodologies. The documented sampling technique); and organic carbon using dry combustion.
and analytical methods are presented along with others
in this manual in the form and style of ASTM methods. IV. Pathogens Analysis—included fecal coliforms
(determined at private laboratories outside of the
The MN-CUP study was divided into three phases: University of MN system).
Phase I—Sample Variability. For the first two months, V. Organics Analyses—included volatile fatty
three separate compost samples were collected at each acids and polychlorinated biphenyls (PCB’s
of three locations to document variability within one determined at private laboratories outside of the
batch at one site. One of the three samples from each University of MN system).
location was subdivided into ten subsamples during
Stage 3. Draft of Sampling and Analysis Protocols
laboratory sample preparation to evaluate within-
sample variability. A scientifically based catalog and laboratory manual of
NOTE—A Reference Sample (in-house) of municipal solid methods was drafted for use with feedstock and
waste compost was created with excess material from one of compost analysis to initiate the standardization process
the original three locations. This material was first air-dried at for regulatory and market requirements, and
36°C, sieved through a 4-mm sieve and milled with a Stein mill
(carbide-tipped blade). The milled material was oven-dried at
management of the composting process.
70°C to minimize enzymatic degradation, mixed in a tumble This work included formatting, enhancement and
blender for 2 d, split with a sample splitter and stored in 2 L critical review of methods devised and modified at the
polyethylene bottles at room temperature (~28°C).
University of Minnesota’s Department of Soil, Water
and Climate Research Analytical Laboratory, St. Paul,

Test Methods for the Examination of Composting and Compost August 12, 2001
v
Preface

by Robert Munter's group and private laboratories for Product—Revision of the First Draft of Test Methods
the MN-CUP project. Other methods developed during for the Examination of Composting and Compost.
parallel compost projects were added to complement
the MN-CUP work, funded by the Composting Council Stage 5. Collaborative Evaluation, On-Going
Research and Education Foundation and The Procter & Goal—Develop consensus for test definitions:
Gamble Company are included in the manual.
5.1 provide replicated samples of composts from
Goal—To provide a science-based manual of rigorous varying feedstock types and combinations; include a
test methods specifically appropriate to feedstocks and minimum of three laboratories per test to establish
finished compost, as distinct from soil, manure, and method precision with resulting data to be used in
fertilizers, and applicable to regulatory and market precision tables to identify and document sources of
requirements, and to augment these methods with a bias,
suite of quick tests for managing the composting
5.2 synthesize user feedback to identify and
process.
document consensus among participating laboratories
Stage 4. Introduction and Peer Review—December for acceptance of at least one test method for each test
1997 parameter where appropriate,
Goal—Introduce TMECC to the composting 5.3 remove antiquated methods, and
community and familiarize users with its intended 5.4 solicit for and add missing test methods.
purpose and content; solicit feedback to refine and Products—Reference Editions of Test Methods for the
expand manual content. A review draft of TMECC Examination of Composting and Compost.
was provided to approximately 160 laboratories,
compost production facilities, and academic Stage 6. USDA Greenhouse and Field Testing
institutions. Collaborating groups and individuals were
Goal—Identify and document correlation among
requested to perform the following:
different test method values and calibrate tests to
4.1 analyses of composts by methods provided in obtain interpretive information about using the
TMECC, compost.
4.2 document commentary and critiques of Product—Test interpretation guidelines for compost
existing methods, and application management.
4.3 solicit for and add missing test methods.

August 12, 2001 Test Methods for the Examination of Composting and Compost
vi
Acknowledgments

ACKNOWLEDGMENTS

EDITOR-IN-CHIEF

Thompson, Wayne H. Edaphos International


Houston, TX

CO-EDITORS
Name Affiliation
Leege, Philip B. The Philip B. Leege Company, Ltd.
Cincinnati, OH

Millner, Patricia D. Soil Microbial Systems Laboratory


USDA-ARS-BARC
Beltsville, MD

Watson, Maurice E. Ohio Agri-Research and Development Center, and


Ohio Compost and Manure Management Program
Ohio State University
Wooster, OH

REVIEW COORDINATORS
Coordinators Affiliation Peer Review Subject Area
Watson, Maurice E. Ohio Agri-Research and Development Center, and 1 – Field Sample Collection
Ohio Compost and Manure Management Program
Ohio State University
Wooster, OH
Shields, Frank Soil Control Lab 2 – Laboratory Sample Preparation
A Division of Control Laboratories, Inc.
Watsonville, CA
Fitzpatrick, George E. Fort Lauderdale Research and Education Center 3 – Physical Parameters
University of Florida
Gainesville, FL
Miller, Robert O. Department of Soil and Crop Sciences 4 – Analytical, Inorganic Chemistry
Colorado State University
Fort Collins, CO
Das, Keshav C. Department of Biological and Agricultural Engineering 5 – Physical Chemistry
University of Georgia
Athens, GA
Thompson, Wayne H. Edaphos International 6 – Stability, Maturity and Biological Activity
Houston, TX
Cole, Michael A. Department of Natural Resources and Environmental Sciences 7 – Organic Chemistry
University of Illinois
Urbana-Champaign, IL
Switzenbaum, Michael S. Department of Civil and Environmental Engineering 8 – Physical Organic Chemistry
University of Massachusetts
Amherst, MA
Michel, Frederick C. Jr. Ohio Agri-Research and Development Center 9 – Microbiology and Pathogens Testing
Department of Food, Agricultural and Biological Engineering
Ohio State University
Wooster, OH

Test Methods for the Examination of Composting and Compost August 12, 2001
vii
Acknowledgments

PEER REVIEW PARTICIPATION


Reviewer Affiliation Test Methods (listed by peer review subject area)
Adler, Paul USDA-ARS – Kearneysville, WV 3 – 03.01, 03.02, 03.04, 03.07, 03.09, 03.10
5 – 04.10, 04.11
Aiello, Kevin Middlesex County Utilities Authority – Sayreville, NJ 5 – 04.09, 04.10, 04.11
Anderson, Kim A. Analytical Sciences Laboratory 2 – 02.02, 03.06-A, 03.08-A
Department of Food Sciences and Toxicology
Holm Research Center, University of Idaho – Moscow, ID
Asdal, Smund The Norwegian Crop Research Institute 6 – 05.05
Apelsvoll Research Centre, Division Landvik
Apelsvoll – NORWAY
Barkman, Joel E. P.E. Wilbark Consultants, Inc. – Fort St. John, BC 3 – 03.01
CANADA
Beffa, Trello Laboratoire de Microbiologie 9 – 07.01, 07.02, 07.03
Universite Neuchatel – Neuchatel, SWITZERLAND
Beharee, Vihita University of Natal – Natal, SOUTH AFRICA 5 – 04.09, 04.10, 04.11
Bess, Vicki BBC Laboratories, Inc. – Tempe, AZ 5 – 04.09, 04.10, 04.11
6 – 05.05, 05.08
Bidlingmaier, Werner Professur Abfallwirtschaft, Fakultat Bauingenieurwesen 2 – 02.02, 03.06-A, 03.08-A
Bauhaus-Universität, Weimar – GERMANY 5 – 04.09, 04.10, 04.11
Bloom, Paul R. Department of Soil, Water, and Climate 4 – 04.01, 04.07
University of Minnesota – St. Paul, MN 6 – 05.05, 05.07, 05.08
Bouwkamp, John Department of Horticulture 6 – 05.02
University of Maryland – College Park, MD
Breitenbeck, Gary Department of Agronomy 1 – 02.01
Louisiana State University – Baton Rouge, LA 2 – 02.02, 03.06-A, 03.08-A
Briceno, Jorge A. Centro de Investigaciones Agronomicas 3 – 03.01, 03.02, 03.09
Universidad de Costa Rica – COSTA RICA
Brinton, William F., Jr. Woods End Research Laboratory – Mount Vernon, ME 2 – 02.01-A, 02.01-B
3 – 03.01, 05.01
6 – 05.02-G, 05.03, 05.06, 05.07-B, 05.08, 05.09
8 – 05.04-B
Buchanan, Marcus Buchanan Associates – Scotts Valley, CA 6 – 05.02-G
Butler, Tracy Soil Microbial Systems Laboratory 6 – 05.05-A
USDA-ARS-BARC – Beltsville, MD
Chaney, Rufus L. Environmental Chemistry Laboratory 4 – 04.12-E
USDA-ASR-BARC – Beltsville, MD 6 – 05.02-E
Chu, Paul A&L Eastern Lab – Richmond, VA 4 – 04.01, 04.02, 04.03, 04.04, 04.05, 04.06, 04.07, 04.08,
04.12, 04.13
Cole, Michael Natural Resources and Environmental Sciences 2 – 02.02, 03.06-A, 03.08-A
University of Illinois – Urbana-Champaign, IL
Cook, Bruce Department of Soil, Water, and Climate 6 – 05.08-B
University of Minnesota – St. Paul, MN
Crenshaw, Teresa A. Delaware Department of Agriculture – Dover, DE 1 – 02.01
Croteau, Gerald A. E&A Environmental Consultants, Inc. – Bothel, WA 6 – 05.03, 05.06-A
Dancer, William E. Research Analytical Laboratory 4 – 04.06-Hg, 04.12-A, 04.13, 04.14
Department of Soil, Water, and Climate
University of Minnesota – St. Paul, MN
Dellavalle, Nat Dellavalle Laboratory - Frezno, CA 4 – 04.02
Eliason, Roger Research Analytical Laboratory 3 – 03.01, 05.01
Department of Soil, Water, and Climate 4 – 04.12-A, 04.13, 04.14
University of Minnesota – St. Paul, MN

August 12, 2001 Test Methods for the Examination of Composting and Compost
viii
Acknowledgments

PEER REVIEW PARTICIPATION, continued


Reviewer Affiliation Test Methods (listed by peer review subject area)
Elwell, David Ohio Agri-Research and Development Center 6 – 05.08-A
Department of Agricultural Engineering
Ohio State University – Wooster, OH
Epstein, Eliot E&A Environmental Consulting – Stoughton, MA 6 – 05.02
Ernst, Joann Environmental Education and Testing Services Inc. 5 – 04.10, 04.11
Bellingham, WA 7 – 06.03, 06.04-A
9 – 07.02-A
Evanylo, Greg Virginia Polytech and State University – Blacksburg, VA 5 – 04.09, 04.10, 04.11
Farrell, Brenda F. The Keck Center for Computational Biology 3 – 03.04
Department of Biochemistry and Cell Biology 8 – 05.04, 05.10-A
Rice University – Houston, TX
Flock, Mark A. Brookside Laboratory, Inc. – New Knoxville, OH 2 – 02.02, 03.06-A, 03.08-A
4 – 04.01, 04.02, 04.03, 04.04, 04.05, 04.06, 04.07, 04.08,
04.12, 04.13
Gouin, Frank R. Department of Horticulture (Professor Emeritus) 3 – 03.01, 03.02, 03.04, 03.07, 03.09, 03.10, 05.01
University of Maryland – Baltimore, MD 6 – 05.05-B, 05.02-B
Grebus, Marcella E. Department of Plant Pathology 6 – 05.05-A, 05.08-A
University of California – Riverside, CA
Guttererres, Fancisco California Integrated Waste Management Board 1 – 02.01
Sacramento, CA 2 – 02.02, 03.06-A, 03.08-A
3 – 03.01, 03.02
Halbach, Tom Department of Soil, Water, and Climate 3 – 03.01-C, 03.09, 03.10-C, 03.10-E
University of Minnesota – St. Paul, MN 6 – 05.05-C, 05.07-A
Hampton, Monica- Southwest Florida Research and Education Center 5 – 04.10, 04.11
Ozores University of Florida – Immokalee, FL
Hanninen, Kari Department of Biology and Environmental Sciences 1 – 02.01
University of Jyuaskyla – Jyuaskyla, FINLAND
Hanson, Dean Central Analytical Laboratory 2 – 02.02, 03.06-A, 03.08-A
Oregon State University – Corvallis, OR
Harrison, Robert B. College of Forest Resources 2 – 02.02-D
University of Washington – Seattle, WA
Hernandez, T. Centro de Edafología y Biología Aplicada del Segura 6 – 05.04
(CEBAS), dependiente del Consejo Superior de
Investigaciones Científicas (C.S.I.C) – Murcia, SPAIN
Hoitink, Henricus A. Ohio Agri-Research and Development Center 6 – 05.08-A
Department of Plant Pathology
Ohio State University – Wooster, OH
Ingram, David Soil Microbial Systems Laboratory 9 – 07.00, 07.01, 07.02, 07.03
USDA-ARS-BARC – Beltsville, MD
King, Mark Maine Department of Environmental Protection 2 – 02.02, 03.06-A, 03.08-A
Augusta, ME
Kotuby-Amacher, Janice Utah State University – Logan, UT 4 – 04.01, 04.02, 04.03, 04.04, 04.05, 04.06, 04.07, 04.08,
04.12, 04.13
Li, Yuncong Department Soil and Water Science 2 – 02.02, 03.06-A, 03.08-A
Tropical Research and Education Center 4 – 04.09, 04.10, 04.11
University of Florida – Gainesville, FL
Loane, John California Integrated Waste Management Board 2 – 02.02, 03.06-A, 03.08-A
Sacramento, CA
Logan, Tina Thornton Laboratory – Tampa, FL 2 – 02.02, 03.06-A, 03.08-A
Low, Clifford B. Perry Labs – Watsonville, CA 2 – 02.02, 03.06-A, 03.08-A
MacLeod, John A. Agriculture and Agricultural Food 2 – 02.02, 03.06-A, 03.08-A
Canada Research Center – Charlottetown, PEI CANADA
Mamo, Martha Department of Agronomy 4 – 04.01, 04.02
University of Nebraska – Lincoln, NE 6 – 05.07

Test Methods for the Examination of Composting and Compost August 12, 2001
ix
Acknowledgments

PEER REVIEW PARTICIPATION, continued


Reviewer Affiliation Test Methods (listed by peer review subject area)
McGinley, Charles M. St. Croix Sensory, Inc. – St. Croix, WI 6 – 05.06
Meckes, Mark Biohazard Assessment Research Branch 9 – 07.00
National Exposure Research Laboratory
U.S. Environmental Protection Agency – Cincinnati, OH
Michel, Frederick C. Jr. Ohio Agri-Research and Development Center 6 – 05.08-A
Department of Food, Agricultural and Biological 8 – 05.04, 05.10-A
Engineering
Ohio State University – Wooster, OH
Miller, Melinda Whatcom County Health and Human Services, 3 – 03.01-A, 03.01-B
Environmental Health – Bellingham, WA
Miller, Robert O. Department of Soil and Crop Sciences 1 – 02.01
Colorado State University – Fort Collins, CO 5 – 04.10, 04.11
Munter, Robert C. Research Analytical Laboratory (Retired) 3 – 03.02, 03.09, 03.10-D
Department of Soil, Water, and Climate 4 – 04.01, 04.02, 04.03, 04.04, 04.05, 04.06, 04.07, 04.12,
University of Minnesota – St. Paul, MN 04.13
5 – 04.09, 04.10, 04.11
6 – 05.05-A, 05.08-A
Normandin, Vicki IAS Labs – Phoenix, AZ 4 – 04.01, 04.02, 04.03, 04.04, 04.05, 04.06, 04.07, 04.08,
04.12, 04.13
Overcash, Michael R. Department of Chemical Engineering 7 – 06.01, 06.02, 06.03, 06.04, 06.05, 06.06, 06.07
North Carolina State University – Raleigh, NC
Parker, Lois A&L Great Lakes Laboratories, Inc. – Fort Wayne, IN 2 – 02.02-B, 02.02-C
4 – 04.02-D, 04.12
5 – 04.10, 04.11
6 – 05.05-A, 05.07-A, 05.08-B
Pettygrove, Stuart University of California – Davis, CA 5 – 04.10, 04.11
Reddy, C.A. Department of Microbiology 9 – 07.00, 07.01, 07.02, 07.03
Michigan State University – East Lansing, MI
Schaefer, Frank Biohazard Assessment Research Branch 9 – 07.04
National Exposure Research Laboratory
U.S. Environmental Protection Agency – Cincinnati, OH
Schnug, Ewald Institute of Plant Nutrition and Soil Science 4 – 04.01, 04.02, 04.03, 04.04, 04.05, 04.06, 04.07, 04.12,
Federal Agricultural Research Center 04.13
Braunschweig – GERMANY 5 – 04.10, 04.11
6 – 05.07
Shields, Frank Soil Control Lab, A Division of Control Laboratories Inc. 4 – 04.01-A, 04.02, 04.03, 04.04, 04.05, 04.08
Watsonville, CA 5 – 04.10, 04.11
6 – 05.02-F, 05.02-G, 05.05, 05.07, 05.09
Shiralipour, Aziz Center for Biomass Programs 6 – 05.05-B, 05.09
Institute of Food and Agricultural Sciences 8 – 05.10
University of Florida – Gainesville, FL
Switzenbaum, Michael S. Department of Civil and Environmental Engineering 6 – 05.02-G, 05.08
University of Massachusetts – Amherst, MA 8 – 05.04, 05.10
Szmidt, Robin The Scottish Agricultural College 5 – 04.10, 04.11
Aberdeen, Scotland – UNITED KINGDOM
Torleiv Næss Ugland The Norwegian Crop Research Institute 6 – 05.05
Apelsvoll Research Centre, Division Landvik
Apelsvoll – NORWAY
van de Kamp, Maartin University of Massachusetts – Amherst, MA 2 – 02.02, 03.06-A, 03.08-A, 03.12
West, James Soil and Plant Laboratory – Santa Clara, CA 2 – 02.02, 03.06-A, 03.08-A
Wolf, Ann M. Ag Analytical Services Laboratory 5 – 04.10, 04.11
Pennsylvania State University – University Park, PA

August 12, 2001 Test Methods for the Examination of Composting and Compost
x
Table of Contents

TABLE OF CONTENTS

01.00 INTRODUCTION

01.01 TMECC CONTENT ............................................................................................................................................... 01.00-1


01.01-A PURPOSE......................................................................................................................................................................01.00-1
01.01-B FOREWORD .................................................................................................................................................................01.00-1
01.01-C REFERENCED METHODS ..........................................................................................................................................01.00-1

01.02 THE COMPOSTING PROCESS ............................................................................................................................ 01.00-2


01.02-A KEY PROCESS VARIABLES ......................................................................................................................................01.00-2

01.03 COMPOSTING TECHNOLOGY GROUPS .......................................................................................................... 01.00-7


01.03-A OPERATION CHARACTERISTICS ............................................................................................................................01.00-7

02.00 SAMPLE COLLECTION AND LABORATORY PREPARATION

02.01 FIELD SAMPLING OF COMPOST MATERIALS............................................................................................... 02.01-1


02.01-A COMPOST SAMPLING PRINCIPLES AND PRACTICES .........................................................................................02.01-7
02.01-B SELECTION OF SAMPLING LOCATIONS FOR WINDROWS AND PILES ...........................................................02.01-14
02.01-C FIELD SAMPLING PLAN FOR COMPOSTED MATERIAL .....................................................................................02.01-16
02.01-D BATCH FEEDSTOCK MATERIAL SAMPLING STRATEGIES ...............................................................................02.01-21
02.01-E DATA QUALITY MANAGEMENT AND SAMPLE CHAIN OF CUSTODY............................................................02.01-22
02.01 SUMMARY...................................................................................................................................................................02.01-24

02.02 LABORATORY SAMPLE PREPARATION......................................................................................................... 02.02-1


02.02-A SAMPLE MIXING AND SPLITTING..........................................................................................................................02.02-6
02.02-B SAMPLE SIEVING FOR AGGREGATE SIZE CLASSIFICATION ...........................................................................02.02-7
02.02-C MAN-MADE INERT REMOVAL AND CLASSIFICATION ......................................................................................02.02-9
02.02-D MILLING AND GRINDING SAMPLES, HARRISON METHOD ..............................................................................02.02-11
02.02-E MILLING AND GRINDING SAMPLES, MUNTER METHOD..................................................................................02.02-12
02.02-F MODIFICATIONS FOR FEEDSTOCK SAMPLE PREPARATION............................................................................02.02-13
02.02 SUMMARY...................................................................................................................................................................02.02-14

03.00 PHYSICAL EXAMINATION

03.01 AIR CAPACITY..................................................................................................................................................... 03.01-1


03.01-A QUICK-TEST FOR BULK DENSITY, POROSITY/PORE SPACE, FREE AIRSPACE AND WATER-
HOLDING CAPACITY OF UNSIEVED COMPOST...................................................................................................03.01-4
03.01-B QUICK-TEST FOR BULK DENSITY, POROSITY/PORE SPACE, FREE AIRSPACE AND WATER-
HOLDING CAPACITY OF SIEVED COMPOST ........................................................................................................03.01-4
03.01-C FIELD DENSITY, FREE AIRSPACE AND WATER-HOLDING CAPACITY...........................................................03.01-7
03.01 METHODS SUMMARY...............................................................................................................................................03.01-9

03.02 ASH......................................................................................................................................................................... 03.02-1


03.02-A UNMILLED MATERIAL IGNITED AT 550°C WITHOUT INERTS REMOVAL.....................................................03.02-4
03.02-B MILLED MATERIAL IGNITED AT 550°C WITH INERTS REMOVAL...................................................................03.02-5
03.02-C UNMILLED MATERIAL IGNITED AT 550°C WITH INERTS REMOVAL .............................................................03.02-6
03.02 METHODS SUMMARY...............................................................................................................................................03.02-8

Test Methods for the Examination of Composting and Compost August 12, 2001
xi
Table of Contents

03.03 BULK DENSITY.................................................................................................................................................... 03.03-1


03.03 METHODS SUMMARY...............................................................................................................................................03.03-3

03.04 WETTABILITY...................................................................................................................................................... 03.04-1


03.04-A WICKING RATE OF COMPOST .................................................................................................................................03.04-8
03.04-B WATER-DROP PENETRATION RATE ......................................................................................................................03.04-11
03.04 METHODS SUMMARY...............................................................................................................................................03.04-13

03.05 FILM PLASTICS .................................................................................................................................................... 03.05-1


03.05-A FILM PLASTIC SURFACE AREA DETERMINATIONS USING DIGITAL PROCESSING ....................................03.05-3
03.05 METHODS SUMMARY...............................................................................................................................................03.05-5

03.06 GLASS SHARDS, METAL FRAGMENTS AND HARD PLASTICS .................................................................. 03.06-1
03.06-A WET SIEVING TECHNIQUE.......................................................................................................................................03.06-3
03.06 METHODS SUMMARY...............................................................................................................................................03.06-4

03.07 PROCESS TO REDUCE SHARPS ........................................................................................................................ 03.07-1

03.08 MAN MADE INERTS............................................................................................................................................ 03.08-1


03.08-A CLASSIFICATION OF INERTS...................................................................................................................................03.08-3

03.09 TOTAL SOLIDS AND MOISTURE ...................................................................................................................... 03.09-1


03.09-A TOTAL SOLIDS AND MOISTURE AT 70±5°C..........................................................................................................03.09-3
03.09 METHODS SUMMARY...............................................................................................................................................03.09-4

03.10 WATER HOLDING CAPACITY........................................................................................................................... 03.10-1


03.10-A QUICK-TEST FOR BULK DENSITY, POROSITY/PORE SPACE, FREE AIRSPACE AND WATER
HOLDING CAPACITY OF UNSIEVED COMPOST...................................................................................................03.01-4
03.10-B QUICK-TEST FOR BULK DENSITY, POROSITY/PORE SPACE, FREE AIRSPACE AND WATER
HOLDING CAPACITY OF SIEVED COMPOST .......................................................................................................03.01-4
03.10-C FIELD DENSITY, FREE AIR SPACE AND WATER-HOLDING CAPACITY..........................................................03.01-5
03.10-D BULK DENSITY AND WATER-HOLDING CAPACITY, OF WATER-SATURATED COMPOST,
MODIFIED ASTM D 2980-71 ......................................................................................................................................03.10-6
03.10-E QUICK-TEST TO APPROXIMATE WATER-HOLDING CAPACITY OF COMPOST.............................................03.10-9
03.10 METHODS SUMMARY...............................................................................................................................................03.10-10

04.00 CHEMICAL PROPERTIES

04.01 ORGANIC CARBON ............................................................................................................................................. 04.01-1


04.01-A COMBUSTION WITH CO2 DETECTION....................................................................................................................04.01-3
04.01 METHODS SUMMARY...............................................................................................................................................04.01-4

04.02 NITROGEN ............................................................................................................................................................ 04.02-1


04.02-A TOTAL KJELDAHL NITROGEN, SEMI-MICRO KJELDAHL TECHNIQUE ..........................................................04.02-6
04.02-B NITRATE NITROGEN DETERMINATION................................................................................................................04.02-9
04.02-C AMMONIUM NITROGEN DETERMINATION..........................................................................................................04.02-11
04.02-D TOTAL NITROGEN BY COMBUSTION....................................................................................................................04.02-13
04.02 METHODS SUMMARY ...............................................................................................................................................04.02-14

04.03 PHOSPHORUS....................................................................................................................................................... 04.03-1


04.03-A TOTAL PHOSPHORUS................................................................................................................................................04.03-2
04.03-B WATER-SOLUBLE PHOSPHORUS............................................................................................................................04.03-3

04.04 POTASSIUM .......................................................................................................................................................... 04.04-1


04.04-A TOTAL POTASSIUM ...................................................................................................................................................04.04-2
04.04-B WATER-SOLUBLE POTASSIUM ...............................................................................................................................04.04-3

August 12, 2001 Test Methods for the Examination of Composting and Compost
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Table of Contents

04.05 SECONDARY AND MICRO-NUTRIENT CONTENT ........................................................................................ 04.05-1


04.05-MG MAGNESIUM ...............................................................................................................................................................04.05-4
04.05-CA CALCIUM .....................................................................................................................................................................04.05-5
04.05-S SULFUR ........................................................................................................................................................................04.05-6
04.05-NA SODIUM........................................................................................................................................................................04.05-7
04.05-B BORON .........................................................................................................................................................................04.05-8
04.05-CL CHLORIDE ...................................................................................................................................................................04.05-9
04.05-CO COBALT .......................................................................................................................................................................04.05-10
04.05-CU COPPER ........................................................................................................................................................................04.05-11
04.05-FE IRON..............................................................................................................................................................................04.05-12
04.05-MN MANGANESE...............................................................................................................................................................04.05-13
04.05-MO MOLYBDENUM...........................................................................................................................................................04.05-14
04.05-ZN ZINC ..............................................................................................................................................................................04.05-15
04.05 METHODS SUMMARY...............................................................................................................................................04.05-16

04.06 HEAVY METALS AND HAZARDOUS ELEMENTS ......................................................................................... 04.06-1


04.06-AS ARSENIC ......................................................................................................................................................................04.06-5
04.06-BE BERYLLIUM ................................................................................................................................................................04.06-6
04.06-CD CADMIUM....................................................................................................................................................................04.06-7
04.06-CU COPPER ........................................................................................................................................................................04.06-8
04.06-CR CHROMIUM .................................................................................................................................................................04.06-9
04.06-PB LEAD.............................................................................................................................................................................04.06-10
04.06-HG MERCURY....................................................................................................................................................................04.06-11
04.06-MO MOLYBDENUM...........................................................................................................................................................04.06-15
04.06-NI NICKEL.........................................................................................................................................................................04.06-16
04.06-SE SELENIUM ...................................................................................................................................................................04.06-17
04.06-SR STRONTIUM ................................................................................................................................................................04.06-18
04.06-V VANADIUM .................................................................................................................................................................04.06-19
04.06-ZN ZINC ..............................................................................................................................................................................04.06-20
04.06 METHODS SUMMARY...............................................................................................................................................04.06-21

04.07 OTHER ELEMENTS.............................................................................................................................................. 04.07-1


04.07-AL ALUMINUM .................................................................................................................................................................04.07-2
04.07-SB ANTIMONY..................................................................................................................................................................04.07-3
04.07-BA BARIUM .......................................................................................................................................................................04.07-4
04.07-CN CYANIDES ...................................................................................................................................................................04.07-5
04.07-AG SILVER .........................................................................................................................................................................04.07-6
04.07-TL THALLIUM...................................................................................................................................................................04.07-7
04.07 METHODS SUMMARY...............................................................................................................................................04.07-8

04.08 INORGANIC CARBON......................................................................................................................................... 04.08-1


04.08-A CALCIUM CARBONATE EQUIVALENCY ...............................................................................................................04.08-2
04.08 METHODS SUMMARY...............................................................................................................................................04.08-3

04.09 CATION EXCHANGE CAPACITY FOR COMPOST.......................................................................................... 04.09-1


04.09-A CEC BY AMMONIUM DISPLACEMENT AFTER WASHING .................................................................................04.09-3
04.09-B CEC BY DIRECT DISPLACEMENT ...........................................................................................................................04.09-5
04.09 METHODS SUMMARY...............................................................................................................................................04.09-7

04.10 ELECTRICAL CONDUCTIVITY FOR COMPOST ............................................................................................. 04.10-1


04.10-A 1:5 SLURRY METHOD, MASS BASIS .......................................................................................................................04.10-3
04.10 METHODS SUMMARY...............................................................................................................................................04.10-5
04.10 APPENDIX TO 04.10—TEMPERATURE CORRECTION .........................................................................................04.10-6

04.11 ELECTROMETRIC pH DETERMINATIONS FOR COMPOST.......................................................................... 04.11-1


04.11-A 1:5 SLURRY pH............................................................................................................................................................04.11-3
04.11 METHODS SUMMARY...............................................................................................................................................04.11-5

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Table of Contents

04.12 DIGESTION TECHNIQUES.................................................................................................................................. 04.12-1


04.12-A MICROWAVE ASSISTED NITRIC ACID DIGESTION OF COMPOST ...................................................................04.12-6
04.12-B NITRIC ACID DIGESTION OF COMPOST AND SOILS...........................................................................................04.12-10
04.12-C DRY ASH SAMPLE DIGESTION FOR PLANT NUTRIENTS...................................................................................04.12-11
04.12-D WATER-SOLUBLE ELEMENTS.................................................................................................................................04.12-13
04.12-E AQUA REGIA PROCEDURE.......................................................................................................................................04.12-14
04.12 METHODS SUMMARY...............................................................................................................................................04.12-15

04.13 ATOMIC ABSORPTION SPECTROMETRY....................................................................................................... 04.13-1


04.13-A COLD VAPOR AAS TECHNIQUE FOR MERCURY IN COMPOST ........................................................................04.13-7
04.13-B ATOMIC ABSORPTION SPECTROPHOTOMETRY METHODS, US EPA METHOD 7000A ................................04.13-10
04.13 METHODS SUMMARY...............................................................................................................................................04.13-13

04.14 INDUCTIVELY COUPLED PLASMA ANALYSIS (ICP) ................................................................................... 04.14-1


04.14-A INDUCTIVELY COUPLED PLASMA-ATOMIC EMISSION SPECTROSCOPY, US EPA METHOD 6010A.........04.14-11
04.14 METHODS SUMMARY...............................................................................................................................................04.14-13
04.14 APPENDIX TO 04.14—ICP ANALYSIS .....................................................................................................................04.14-14

04.15 SOLUBLE SALTS.................................................................................................................................................. 04.15-1

05.00 ORGANIC AND BIOLOGICAL PROPERTIES

05.01 BIODEGRADABLE VOLATILE SOLIDS............................................................................................................ 05.01-1

05.02 INDICATOR RATIOS ........................................................................................................................................... 05.02-1


05.02-A CARBON TO NITROGEN RATIO...............................................................................................................................05.02-6
05.02-B CARBON TO PHOSPHORUS RATIO .........................................................................................................................05.02-7
05.02-C AMMONIUM TO NITRATE RATIO ...........................................................................................................................05.02-8
05.02-D CARBON TO SULFUR RATIO....................................................................................................................................05.02-9
05.02-E CADMIUM TO ZINC RATIO ......................................................................................................................................05.02-10
05.02-F AGRICULTURAL INDEX ...........................................................................................................................................05.02-12
05.02-G CCQC MATURITY INDEX..........................................................................................................................................05.02-13
05.02 METHODS SUMMARY...............................................................................................................................................05.02-15

05.03 COLOR ................................................................................................................................................................... 05.03-1


05.03-A FIELD ASSESSMENT OF COMPOST COLOR AND ODOR.....................................................................................05.03-3
05.03 METHODS SUMMARY...............................................................................................................................................05.03-5

05.04 ENZYME ACTIVITY AND ANALYSIS .............................................................................................................. 05.04-1


05.04-A PHOSPHATASES .........................................................................................................................................................05.04-6
05.04-B DEHYDROGENASES ..................................................................................................................................................05.04-10
05.04-C PROTEASES .................................................................................................................................................................05.04-12
05.04-D CELLULASES...............................................................................................................................................................05.04-14
05.04-E PEROXIDASES.............................................................................................................................................................05.04-16
05.04 SUMMARY OF METHODS .........................................................................................................................................05.04-18

05.05 BIOLOGICAL ASSAYS ........................................................................................................................................ 05.05-1


05.05-A SEEDLING EMERGENCE AND RELATIVE GROWTH ...........................................................................................05.05-4
05.05-B IN-VITRO GERMINATION AND ROOT ELONGATION..........................................................................................05.05-6
05.05-C EARTHWORM BIOASSAY: THE MINNESOTA “Z”-TEST......................................................................................05.05-8
05.05 METHODS SUMMARY...............................................................................................................................................05.05-10

August 12, 2001 Test Methods for the Examination of Composting and Compost
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Table of Contents

05.06 ODOR ..................................................................................................................................................................... 05.06-1


05.06-A FIELD ASSESSMENT OF COMPOST ODOR ............................................................................................................05.06-7
05.06-B FIELD SAMPLING OF BIOFILTER ODOR EMISSIONS ..........................................................................................06.06-8
05.06 METHODS SUMMARY...............................................................................................................................................05.06-9
05.06 APPENDIX I TO 05.06—EXAMPLE OF PERFORMANCE STANDARDS FOR ODOROUS EMISSIONS
FROM A PERMANENT CONSTRUCTED FACILITY...............................................................................................05.06-10
05.06 APPENDIX II TO 05.06—ODOR NOTIFICATION FORM ........................................................................................05.06-11
05.06 APPENDIX III TO 05.06—RESIDENT ODOR COMPLAINT FORM........................................................................05.06-12

05.07 ORGANIC MATTER ............................................................................................................................................. 05.07-1


05.07-A LOSS ON IGNITION ORGANIC MATTER METHOD...............................................................................................05.07-10
05.07-B HUMIC SUBSTANCES: FULVIC ACID AND HUMIC ACID EXTRACTION AND
CHARACTERIZATION................................................................................................................................................05.07-11
05.09-C CALCULATION FOR ORGANIC MATTER DECOMPOSITION..............................................................................05.09-13
05.07 METHODS SUMMARY...............................................................................................................................................05.07-15

05.08 RESPIROMETRY .................................................................................................................................................. 05.08-1


05.08-A SOUR: SPECIFIC OXYGEN UPTAKE RATE............................................................................................................05.08-7
05.08-B CARBON DIOXIDE EVOLUTION RATE...................................................................................................................05.08-11
05.08-C IN-SITU OXYGEN REFRESH RATE ..........................................................................................................................05.08-13
05.08-D DEWAR SELF-HEATING TEST..................................................................................................................................05.08-14
05.08-E SOLVITA MATURITY INDEX....................................................................................................................................05.08-17
05.08-F BIOLOGICALLY AVAILABLE CARBON .................................................................................................................05.08-19
05.08 METHODS SUMMARY...............................................................................................................................................05.08-21

05.09 VIABLE WEED SEED IN COMPOST.................................................................................................................. 05.09-1


05.09-A SHIELDS RINSE METHOD.........................................................................................................................................05.09-4
05.09-B PEAT MOSS DILUTION METHOD ............................................................................................................................05.09-5
05.09 METHODS SUMMARY...............................................................................................................................................05.09-7

05.10 VOLATILE FATTY ACIDS .................................................................................................................................. 05.10-1


05.10-A VOLATILE FATTY ACIDS IN COMPOST EXTRACT BY GAS CHROMATOGRAPHY......................................05.10-3
05.10 METHODS SUMMARY...............................................................................................................................................05.10-8

06.00 SYNTHETIC ORGANIC COMPOUNDS

06.00 ANALYSIS OF SYNTHETIC ORGANIC CHEMICALS IN COMPOST ............................................................ 06.00-1

06.01 CHLORINATED HERBICIDES ............................................................................................................................ 06.00-4

06.02 DIOXIN/FURANS.................................................................................................................................................. 06.00-5

06.03 ORGANOCHLORINE PESTICIDES..................................................................................................................... 06.00-6

06.04 ORGANOPHOSPHORUS PESTICIDES............................................................................................................... 06.00-8

06.05 POLYCHLORINATED BIPHENYLS ................................................................................................................... 06.00-9

06.06 SEMIVOLATILE ORGANIC COMPOUNDS....................................................................................................... 06.00-11

06.07 VOLATILE ORGANIC COMPOUNDS ................................................................................................................ 06.00-12

Test Methods for the Examination of Composting and Compost August 12, 2001
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Table of Contents

07.00 PATHOGENS

07.00 INTRODUCTION TO PATHOGEN TESTING..................................................................................................... 07.00-1

07.01 COLIFORM BACTERIA ....................................................................................................................................... 07.01-1


07.01-A TOTAL COLIFORMS...................................................................................................................................................07.01-4
07.01-B FECAL COLIFORMS ...................................................................................................................................................07.01-6
07.01-C ESCHERICHIA COLI ....................................................................................................................................................07.01-8
07.01 METHODS SUMMARY...............................................................................................................................................07.01-10

07.02 SALMONELLA........................................................................................................................................................ 07.02-1


07.02-A 1-2 DETECTION TEST AND SALMONELLA QUANTIFICATION PROCEDURE ...................................................07.02-3
07.02-B ENRICHMENT AND QUANTIFICATION OF SALMONELLA IN COMPOST .......................................................07.02-6
07.02-C CONFIRMATION PROTOCOLS .................................................................................................................................07.02-8
07.02 METHODS SUMMARY...............................................................................................................................................07.02-10

07.03 ENTEROCOCCI ..................................................................................................................................................... 07.03-1


07.03-A ENTEROCOCCUS.........................................................................................................................................................07.03-3
07.03 METHODS SUMMARY...............................................................................................................................................07.03-5

07.04 PARASITIC HELMINTHS .................................................................................................................................... 07.04-1


07.04-A VIABILITY OF ASCARIS OVA IN COMPOST ...........................................................................................................07.04-3
07.04 METHODS SUMMARY...............................................................................................................................................07.04-6
07.04 APPENDIX TO 07.04—INITIAL PERFORMANCE AND RECOVERY (IPR) AND ONGOING
PERFORMANCE AND RECOVERY (OPR) FOR VIABLE ASCARIS OVA..............................................................07.04-7

07.05 RECOVERY AND ASSAY OF TOTAL CULTURABLE VIRUSES ................................................................... 07.05-1


07.05 US EPA 625R92013, FROM EPA600/4-84/013(R7), SEPTEMBER 1989 REVISION (SECTION 3)........................07.05-1

August 12, 2001 Test Methods for the Examination of Composting and Compost
xvi
Abbreviations

ABBREVIATIONS
Oac -acetate µm micrometer(s)
ACS America Chemical Society meq milli equilivent(s)
ASTM American Society for Testing Materials mL milliliter(s)
ASA American Society of Agronomy mm millimeter(s)
Å Ångström units (10-8 cm, or 0.1 nm) mMhos milliMhos, equal to mS
AshW ash weight determined at 550°C ms millisecond(s)
AOAC Association of Official Analytical Chemists min minute(s), time
Atm Atmosphere(s), 1 atm = 101,325 Pa M mega
AA atomic absorption MSW mixed municipal solid waste
cm centimeter(s) MMW mixed municipal waste
cmol centi mol(s), cmol kg-1 ! meq 100 g-1 M molar
CCFREF Composting Council Research and Education MW molecular weight
Foundation MSW municipal solid waste
C coulomb ng nanogram(s)
d day(s), time nm nanometer(s)
" delta, change, or difference USCC US Composting Council, The
°C degrees Celsius NIH National Institute of Health, US
°F degrees Fahrenheit N normal concentration
°C = 5 ÷ 9 × (°F – 32) No. number, #
dw dry weight basis, equal to TS basis OM organic matter
÷ divided by, division symbol Ω ohm, unit of resistance (1 Mhos-1)
dS deci-Seiman, equal to dMhos oz ounce(s) US fluid (0.02957 L)
EC Enzyme Commission o.d. outer diameter (dimension)
= equal to dw oven-dry weight basis determined at 70±5°C
≡ equivalent to ODW oven-dry weight basis determined at 70±5°C
EtOH ethanol Pa pascal(s)
Fig figure, illustration, chart, drawing, diagram ppb parts per billion (1 x 109), e.g., µg kg-1
ft foot (feet) (30.480061 cm) ppm parts per million (1 x 106), e.g., mg kg-1
e.g. for example % percent (parts per 100); percentage
gal gallon(s), US liquid (3.7853 L) pt pint(s), US liquid (0.4732 L)
GC gas chromatography TD pipette volume to deliver
g gram(s) lb pound(s) (453.6 g)
g gravitational force, cm sec·sec-1, ft sec·sec-1 psi pounds per square inch (0.06805 atm)
> greater than, more than, exceeds PRS process to reduce sharps
h hour(s), time qt quart(s), US liquid (0.9463 L)
in. inch(es) (2.54 cm) s second(s), time
ICP- inductively coupled plasma - atomic emission S Seiman, equal to Mhos
AES/M spectroscopy/mass spectroscopy rpm revolutions per minute
i.d. inner diameter (dimension) SSSA Soil Science Society of America
ISO International Organization for Standardization STP standard temperature (25°C) and pressure
kg kilogram(s) (101,325 Pa)
< less than, under, below t time
L liter(s), liquid × times, multiplication symbol
mhos unit of conductance (Sieman’s unit, Ω-1) USDA United States Department of Agriculture
MS mass spectrometry US EPA United States Environmental Protection Agency
MΩ megohm(s) W watts
m meter(s) yd yard(s) (0.9144 m)
µg microgram(s) SM Standard Methods for the Examination of Water
µL microliter(s) and Wastewaters

Test Methods for the Examination of Composting and Compost August 12, 2001
xvii
Manual Format

MANUAL FORMAT
The first number indicates the chapter, the second
1. Test Method Categories
number indicates the test parameter, and the letter
1.1 The test methods presented in TMECC are corresponds with the test method, while the last
separated into seven [7] chapters categorized by sample number indicates the figure or table within a method.
collection and preservation (02.00), physical attribute EXAMPLE—Fig 04.02-A1 Conceptual example of a standard
tests (03.00), chemical analysis (04.00), and organic addition plot.
and biological determinations (05.00), with references EXAMPLE—Table 04.04-A1 General interpretation guidelines
to pertinent synthetic organic chemicals determination for greenhouse growth media analyzed by the Saturated Media
methods (06.00) and pathogen testing procedures Extract method (dS m-1).
(07.00). Each test method is designed for analyzing
3. Test Method Page Format
compost materials at one or more of the six [6]
composting process steps described in chapter 01.00, 3.1 A test method applications guide is provided
and to document compost safety standards or market as the header for each test method to indicate which
attributes. methods are appropriate for each of the six composting
process steps. Test methods are represented by alpha-
2. Test Method Coding System numeric code by column under each process step.
2.1 Alpha-Numeric Test Method Codes—Each 3.2 Each test parameter is presented in three parts:
test method code contains two integers and one
3.2.1 parameter introduction and background;
hyphenated letter. The first integer identifies the
chapter and the second integer represents the test 3.2.2 procedural outlines where more than one
parameter, while the hyphenated letter represents one procedure may be presented for a parameter; and
of various possible test methods that may be used for 3.2.3 method summaries.
the measurement, or determination of a test parameter.
3.3 An abbreviated test method application guide
EXAMPLE 1—the code “05.08-D” represents test method “D” of for each test method is provided on the first page of
test parameter eight [8] in chapter five [05].
each method.
2.2 Referenced Methods—Test methods of
interest may not be included in TMECC because: 4. Method Guide Format
2.2.1 the method is proprietary; 4.1 The application guide headings provide the
2.2.2 methods are well documented in other following test method information (Fig 00.01-1).
manuals; or 4.1.1 Test Parameter—product attribute, such as
2.2.3 the method has not yet been adequately pH, total solids, etc.
optimized for use with composting materials. 4.1.2 Test Method—analytical procedure or quick
2.3 Page Numbering—Page numbers are located test for measuring the parameter.
on the outside lower corner of each page. The page 4.1.3 Reporting Units—reporting units and
number is preceded by the hyphenated chapter number moisture basis, such as mg kg-1 dw, g g-1 % wet basis, g
and section number. cm-3 dw, etc. Refer to the list of abbreviations
EXAMPLE—“02.01-8” represents page eight of section one [1] presented in this preface for a description of each
in chapter two [2]. abbreviation used in this manual.
2.4 Figures and Tables—The alpha-numeric code 4.1.4 Test Method Applications—Test method
for test methods is expanded to include an additional codes are inserted where analysis is appropriate for the
number following the hyphenated letter. Both figures indicated process management steps, or safety and
and tables are numbered from one for each test method. market attributes (detailed in chapter one).

Test Method: Parameter (see 4.1.1). Test method (see 4.1.2) Units: (see 4.1.3)
Test Method Applications
Process Management Product Attributes
Step 1: Step 2: Step 3: Step 4: Step 5: Step 6: Step 7: Safety Market
Feedstock Feedstock Composting Odor Treatment Compost Curing Compost Compost Standards Attributes
Recovery Preparation Screening and Storing and
Refining Packaging
(see 4.1.4)
Fig 00.01-1 Test method applications guide.

August 12, 2001 Test Methods for the Examination of Composting and Compost
xviii
Manual Format

SAMPLE FATE CHART

Place sample in refrigerated


storage at 4°C for no more
Sample Collection than two weeks.
(Section 02.01) Sample scheduled for
No
amount: 12 L (~3 gal) immediate preparation If long-term storage is
required, store sample at
- 4°C (if method permits).

Yes

Sample Preparation
(Section 02.02) Store approximately 1/3 of sample as
1. backup material.
Blend and Split Sample
Sieve and prepare material for analysis. Follow sample preparation
2. as prescribed in protocol. Refer to sample handling for each method.

03.00 Physical Analysis 04.00 Chemical Analysis 05.00 Organic and 06.00 Organic
Biological Properties Contaminants
1. Most analyses are performed 1. Most analyses are and
on samples at as-received performed on air-dried, 1. Most analyses are 07.00 Pathogens
moisture. milled, inert-free materials. performed on samples at as- Testing
2. Preparation often includes a 2. Analyses that require as- received moisture.
sieving step. received moist samples 2. Preparation often includes a 1. Analyses are performed on
3. Recommended storage include pH, NO3, NH4 and sieving step. samples at as-received
temperature is 4°C for short- soluble salts. moisture.
3. Recommended storage
term and -4°C for long-term. 3. Short-term storage for air- 2. Recommended short-term
temperature is 4°C, no more
dried material is in sealed storage temperature is 4°C.
than one [1] week. Frozen
containers at ambient storage is not recommended 3. Aseptic techniques are
temperature. for most biological samples. employed to minimize
cross-contamination.

Air-Dried Moist Sample


Material Material

NOTE—A very small finely milled sample aliquot is used (0.5 g to 4 g). NOTE—Sample aliquot size varies with test method. Sample preparation
Refer to specific test for details. often includes sieving for size classification.
Refer to specific test for details.
a. Amount to prepare: 250 cm3.
b. Store air-dried material at room temperature in a sealed container. a. Store as-received materials in sealed containers at 4°C for no more than
Oven-dry the material for long-term storage to minimize enzymatic two [2] weeks and in a frozen state at -4°C for long-term storage.
degradation at room temperature. b. Organic Contaminant Testing: Use inert storage containers that will
c. Special care is required to maintain sample homogeneity to maximize not contaminate the sample. Refer to Table 02.01-6.
precision. c. Pathogen Testing: prepare sample for analysis immediately upon
d. Total Nitrogen Testing: A significant amount of nitrogen may volatilize receipt. Use aseptic procedures to avoid cross-contamination.
from samples high in ammonia. Cross-contamination is possible.

Fig 00.01-2 Fate chart of sample flow from collection through laboratory preparation and analysis.

Test Methods for the Examination of Composting and Compost August 12, 2001
xix
Manual Format

August 12, 2001 Test Methods for the Examination of Composting and Compost
xx
Test Methods for the Examination of Composting and Compost

Purpose
Test Methods for the Examination of Composting and Compost (TMECC) provides detailed
protocols for the composting industry to verify the physical, chemical, and biological condition
of composting feedstocks, material in process and compost products at the point of sale.
Material testing is needed to verify compost product safety and market claims. TMECC provides
protocols to sample, monitor, and analyze materials at all stages of the composting process, (e.g.,
prior to, during and after composting), to help maintain process control, verify product attributes,
assure worker safety, and to avoid degradation of the environment in and around the composting
facility.
Standardized methods to characterize compost are needed by compost producers, state regulatory
and permitting agencies, compost product marketing specialists, state and commercial testing
laboratories, and agriculturalists, horticulturalists, landscapers, and other consumer sectors. Use
of standard methods and protocols for sampling, laboratory analysis, reporting, and interpretation
of test results will promote production and marketing of quality composts that meet a core set of
analytical standards.
TMECC is approved for publication through the USGPO as part of USDA’s Conservation
Resources Technical Bulletin Series.

Overview of TMECC Development

Summary
TMECC was jointly published by the US Department of Agriculture (USDA) and the
Composting Council Research and Education Foundation (CCREF). The TMECC Project was
initiated by The Procter and Gamble Company in mid 1995 under the direction of Phil B. Leege,
and adopted by the Composting Council Research and Education Foundation in late 1995 under
the leadership of Dr. Charles Cannon, former Executive Vice President of the Composting
Council. Refer to Fig 1 through Fig 3 for diagrams that illustrate key participants and their
responsibilities during the TMECC development and peer-review process.
TMECC evolution and the TMECC Project is categorized by six developmental stages: i) draft
of methods; ii) compilation of methods; iii) content peer-review; iv) round-robin testing; v)
addition of interpretation and end-use guidelines; and vi) maintenance and addenda distribution.
The initial draft of methods was completed in December 1995 and the enhanced compilation of
methods was completed in December 1997. TMECC content peer-review was initiated in March

1
The 2002 Compost Analysis Proficiency (CAP) Testing Program is managed by Robert O. Miller. CAP was
established, in part, as a vehicle to measure performance, and to examine the credibility of TMECC. Visit
http://tmecc.org/cap/ for detailed information.
1998 and formally completed in August 2001. Proficiency testing is underway and was
implemented as follows: a preliminary round-robin using triplicate samples from 15 composting
facilities and three laboratories was carried out in 2000 through collaboration with the USCC’s
Seal of Testing Assurance2 (STA) program and USDA-ARS-BARC-SASL (Fig 4); in 2001 and
2002, round robin-testing was expanded to include 23 laboratories through collaboration between
Compost Analysis Proficiency (CAP), STA and the TMECC Project (Fig 5).
Stage six of TMECC development will incorporate the proficiency testing program as part of a
new and expanded peer-review process; data generated through proficiency testing will serve as
a feedback mechanism used to update and maintain TMECC. CCREF is seeking formal
relationships with professional organizations to fulfill the need for critical technical oversight of
the peer-review process. Refer to Fig 6 and Fig 7 for diagrams that illustrate proposed feedback
and TMECC maintenance mechanisms.

Stages I and II ! Compilation


The first stage of the TMECC Project which spanned approximately three years was principally
funded by The Procter and Gamble Company and the MN Office of Environmental Assistance.
This effort included bench-level evaluation of existing test methods at the U of MN Research
Analytical Laboratory. Tests were performed on samples of source separated and mixed
municipal solid waste composts. This effort involved modification of existing test methods
developed for other materials, (e.g., soils, water, biosolids, etc.). A preliminary draft of TMECC
was compiled using test methods employed at the U of MN and later expanded to include other
generally accepted methods plus a small number of new techniques for analyzing compost
parameters which had no generally accepted or readily available method. The product of the first
stage of the TMECC Project was a 1,000-page peer-review draft entitled “The First Edition of
TMECC”.

P&G-Sponsored Draft, 1993-1995 P&G-Sponsored Enhancement, 1995-1998

TMECC TMECC
Preliminary Draft, 1995 First Edition, 1998

Philip B. Leege Wayne H. Thompson Philip B. Leege Wayne H. Thompson


Managing Co-Editor Co-Editor Managing Co-Editor Co-Editor

Fig 1. Stages I and II of the TMECC Project. The preliminary draft was compiled and later
expanded to include additional methods. The final product of this effort was the peer-review
draft, “First Edition of TMECC”.

Stage III ! Peer-Review of the First Edition


The third stage of the TMECC Project was a coordinated peer-review of TMECC, the 1,000-
page volume developed during stages one and two of the project (Fig 2). The peer-review
process spanned a period of four years and was principally funded by the USDA.

2
The 2002 Seal of Testing Assurance (STA) is the USCC composting product data disclosure and end-use guideline
program for compost producers and distributors. The program targets compost producers and is intended to promote
the use of established compost sample collection and testing procedures, and to indicate appropriate end-use
guidelines for their tested compost products. Visit http://tmecc.org/sta/ for detailed information.
TMECC sections were grouped into nine academic categories. A group leader was recruited to
manage each review category. Each group leader recruited his/her team of peer-reviewers. The
first edition of TMECC was then distributed to more than 175 reviewers selected for category-
specific feedback. Individual reviewer input was compiled by each group leader and
incorporated into TMECC by the Editor-in-Chief. The revised sections were then approved by
the co-editors and re-submitted to the group leaders for their acceptance of the final draft of their
assigned sections.
The peer-review process evolved into a rigorous re-write of TMECC. The latest USGPO
working draft incorporates comprehensive critiques from over 175 compost analytical experts
from around the world. This completely revised work was submitted to the USDA in December
2000 as a project deliverable; USDA extended the review process before granting its approval
and acceptance of TMECC as a compost sampling and laboratory manual.

USDA-Sponsored Peer Review of TMECC, March 1998 - August 2001

TMECC
USDA Working Draft, 2001 Philip B. Leege
Managing Co-Editor

Maurice E. Watson
Co-Editor

Wayne H. Thompson
Editor-in-Chief Patricia D. Millner
Co-Editor and Coordinator for
USDA Technical Review

Maurice Watson Frank Shields George E. Fitzpatrick


Group 1 Leader Group 2 Leader Group 3 Leader
Sample Collection Sample Preparation Physical Attributes

Robert O. Miller Keshav C. Das Wayne H. Thompson


Group 4 Leader Group 5 Leader Group 6 Leader
Analytical Chemistry Physical Chemistry Biological Activity

Michael A. Cole Mike S. Switzenbaum Frederick C. Michel, Jr.


Group 7 Leader Group 8 Leader Group 9 Leader
Synthetic Organics Physical Organic Chemistry Pathogens Testing

Fig 2. Stage III of the TMECC Project. The peer-review process was initiated in March
1998. USDA Technical Review was initiated in December 2000 and completed in August
2001.
Dr. Patricia Millner supervised the USDA internal review and worked directly with Editor-in-
Chief of TMECC to implement all modifications required by USDA. Dr. Millner presented a
prospectus to publish TMECC as a USDA Conservation Resources Technical Bulletin to the
USGPO in October 2000; the prospectus to publish was approved in March 2001. The prospect
of releasing TMECC as a USGPO document prompted USDA to intensify the review process
which extended the Stage III completion date by an additional nine months. The USDA internal
technical review was formally completed in August 2001 and the working draft was submitted to
the USGPO editorial staff in August 2001. Refer to Fig 3, and Appendix I for the list of methods
provided in TMECC.
USDA-Sponsored distribution of TMECC as a USGPO working draft, August 2001

TMECC Philip B. Leege


USDA-Sponsored Wayne H. Thompson Co-Editor
USGPO Publication, 2001 Editor-in-Chief
Maurice E. Watson
Co-Editor

Patricia D. Millner
USGPO Editorial Review Patricia D. Millner
USDA-ARS, BARC-SASL
Co-Editor

Fig 3. USGPO Review Process – The last step in Stage III of the TMECC Project.

Stage IV ! Laboratory Proficiency Testing


Laboratory proficiency testing is a QA/QC tool used by laboratory personnel to verify their
analytical performance relative to other laboratories that use common methods and analytical
protocols for specified parameters. The Compost Analysis Proficiency Testing program (CAP)
was initiated through collaboration with managers of the North American Proficiency Testing
Program (NAPT) to provide the compost laboratory analysis industry with an inter-laboratory
QA/QC program, to develop reference materials, and to provide comparative data needed to
measure performance and precision of TMECC analytical methods.
Laboratory proficiency testing is the fourth stage of the TMECC Project and is considered on-
going. The USDA-Sponsored Seal of Testing Assurance Pilot (STA-2000) was implemented to
serve as a preliminary round-robin designed to reveal operational oversights in common test
methods. This was implemented prior to the formation of CAP and prior to the submission
TMECC as a project deliverable to USDA. Refer to Fig 4 for the list of participants.
Preliminary examination of the USDA-sponsored round robin results provided crucial
information which allowed the TMECC editors to clarify important steps in various laboratory
protocols with a resulting improvement in across-lab precision.

STA Pre-Release of TMECC, February 2000

TMECC
STA Pre-Release, 2000
Philip B. Leege
Co-Editor

Maurice E. Watson
Co-Editor
Wayne H. Thompson
Editor-in-Chief
Patricia D. Millner
Co-Editor

Lois Parker Frank Shields


Patricia D. Millner
A&L Great Lakes Lab, Inc. Soil Control Lab
USDA-BARC-SASL
Fort Wayne, IN Watsonville, CA

Fig 4. Stage IV of the TMECC Project. Preliminary round-robin testing was carried out by
three laboratories on triplicate compost samples from fifteen facilities.
Round-robin testing of TMECC was expanded in 2001 and 2002 to include participating CAP
laboratories (Fig 5). Preliminary results from the first 2001 sample exchange of the 2001 CAP
program were not conclusive; results from later exchanges are needed to construct a more
meaningful data set; and additional steps were implemented to incorporate more descriptive and
detailed performance data reporting and comments from participating laboratory personnel.
Participation in CAP is expected to increase after TMECC is released as a USGPO document.
CAP Pre-Release of TMECC, March 2001

TMECC
CAP Pre-Release, 2001
Philip B. Leege
Co-Editor

Maurice E. Watson
Co-Editor
Wayne H. Thompson
Editor-in-Chief
Patricia D. Millner
Co-Editor

Robert O. Miller
CAP Program Manager

A&L Anal Labs AEA Labs BBC Lab, Inc.


Memphis, TN Chicago, IL Tempe, AZ
Tier II
Labs
A&L Grt Lakes Lab IAS Labs Soil Control Lab
Fort Wayne, IN Phoenix, AZ Watsonville, CA

A&L W. Agri Labs MDS Pharma Svs. Servi-Tech Labs


Modesto, CA Lincoln, NE Dodge City, KS

Ag Anal. Svs. Lab Metro Denver Lab Soil & Feed Lab
University Park, PA Denver, CO Charlottetown, PIE
Tier I
Labs
Brookside Lab, Inc. MN Valley Testing Univ. of Delaware
New Knoxville, OH Labs - New Ulm, MN Newark, DE

Dellavalle Lab, Inc. Plant, Soil & Env. Sci. USAG Anal Svs, Inc.
Fresno, CA Orono, ME Pasco, WA

USU Analytical Labs


Logan, UT

Fig 5. Stage IV of the TMECC Project. Round-robin testing through the CAP testing
program.

Stage V ! Interpretation and End-Use Guidelines


The fifth stage of the TMECC Project is considered on-going. Interpretation guidelines were
incorporated during Group 6 peer-review for two biological activity sections, the respirometry
(05.08) and indicator ratios (05.02) sections. Much more effort must be expended and
information compiled before this aspect of TMECC can be considered comprehensive.

Incorporate Interpretation Guidelines into TMECC, on-going

SPAC Co-Editors
TMECC
Addenda to the USGPO
Release, 2002
USDA Co-Editors

Editor-in-Chief
SSSA Co-Editors

TMECC USDA-Sponspored 1. Compile End-Use


Website Compost Research performance data

Fig 6. Stage V of the TMECC Project. Incorporation of interpretation guidelines.


Stage VI ! Maintenance and Updates, PROPOSED for 2002 and Later
The sixth stage of the TMECC Project will begin after TMECC is formally released through the
USGPO as a USDA document. The Standards and Practices Committee of the US Composting
Council is in the process of forming oversight subcommittees. Subcommittees will consist of
compost analytical specialists who will provide technical oversight for the maintenance and
enhancement of TMECC. The effort to form category-specific review subcommittees requires
solicitation of technical assistance, paid and/or voluntary, from current participants of the
TMECC review process and other qualified individuals associated with participating
organizations, (e.g., Soil Science Society of America [SSSA], Soil and Plant Analysis Council
[SPAC], etc.). The primary source of performance data and technical feedback will be collected
through the CAP programs; secondary sources may include direct comment via feedback
mechanisms available on-line at the TMECC web site, (e.g., discussion list, on-line manuscript
submissions, etc.). Pending the availability of project funds, analysis of CAP results will be
expanded to include site visits and a review process assembled to evaluate laboratory
interpretation of TMECC methods. Finally, mechanisms to create TMECC addenda will be
established to provide addenda to the compost analytical community (Fig 6 and Fig 7).

Udate and Maintain the USGPO Release of TMECC, 2002

IPSC Co-Editors
TMECC
Addenda to the USGPO
Release, 2002
USDA Co-Editors

CCREF/USCC
Editor-in-Chief
SSSA Co-Editors

1. Compile and examine


CAP data,
TMECC CAP Progam
2. Visit labs to document
Website Participants
protocol interpretation and
implementation, and

Other TMECC 3. Submit corrections and


Users omissions

Fig 7. Stage VI of the TMECC Project (PROPOSED). Maintenance and updates of TMECC
through feedback and review mechanisms.
Appendix I: TMECC Contents
CHAPTER " INTRODUCTION 03.04 WETTABILITY
03.04-AWICKING RATE OF COMPOST
01.01 TMECC CONTENT
03.04-B WATER-DROP PENETRATION RATE
01.01-APURPOSE
03.04 METHODS SUMMARY
01.01-B FOREWORD
01.01-C REFERENCED METHODS 03.05 FILM PLASTICS
03.05-AFILM PLASTIC SURFACE AREA
01.02 THE COMPOSTING PROCESS DETERMINATIONS USING DIGITAL
01.02-AKEY PROCESS VARIABLES PROCESSING
01.03 COMPOSTING TECHNOLOGY GROUPS 03.05 METHODS SUMMARY
01.03-AOPERATION CHARACTERISTICS 03.06 GLASS SHARDS, METAL FRAGMENTS AND
CHAPTER 2 SAMPLE COLLECTION AND HARD PLASTICS
LABORATORY PREPARATION 03.06-AWET SIEVING TECHNIQUE
02.01 FIELD SAMPLING OF COMPOST 03.06 METHODS SUMMARY
MATERIALS 03.07 PROCESS TO REDUCE SHARPS
02.01-ACOMPOST SAMPLING PRINCIPLES AND 03.08 MAN MADE INERTS
PRACTICES 03.08-ACLASSIFICATION OF INERTS
02.01-B SELECTION OF SAMPLING LOCATIONS FOR 03.09 TOTAL SOLIDS AND MOISTURE
WINDROWS AND PILES
03.09-ATOTAL SOLIDS AND MOISTURE AT 70±5°C
02.01-C FIELD SAMPLING PLAN FOR COMPOSTED
03.09 METHODS SUMMARY
MATERIAL
02.01-DBATCH FEEDSTOCK MATERIAL SAMPLING 03.10 WATER HOLDING CAPACITY
STRATEGIES 03.10-AQUICK-TEST FOR BULK DENSITY,
02.01-E DATA QUALITY MANAGEMENT AND SAMPLE POROSITY/PORE SPACE, FREE AIRSPACE AND
CHAIN OF CUSTODY WATER HOLDING CAPACITY OF UNSIEVED
COMPOST
02.01 SUMMARY
03.10-B QUICK-TEST FOR BULK DENSITY,
02.02 LABORATORY SAMPLE PREPARATION POROSITY/PORE SPACE, FREE AIRSPACE AND
02.02-ASAMPLE MIXING AND SPLITTING WATER HOLDING CAPACITY OF SIEVED
02.02-B SAMPLE SIEVING FOR AGGREGATE SIZE COMPOST
CLASSIFICATION 03.10-C FIELD DENSITY, FREE AIR SPACE AND
02.02-C MAN-MADE INERT REMOVAL AND WATER-HOLDING CAPACITY
CLASSIFICATION 03.10-DBULK DENSITY AND WATER-HOLDING
02.02-DMILLING AND GRINDING SAMPLES, CAPACITY, OF WATER-SATURATED
HARRISON METHOD COMPOST, MODIFIED ASTM D 2980-71
02.02-E MILLING AND GRINDING SAMPLES, MUNTER 03.10-E QUICK-TEST TO APPROXIMATE WATER-
METHOD HOLDING CAPACITY OF COMPOST
02.02-F MODIFICATIONS FOR FEEDSTOCK SAMPLE 03.10 METHODS SUMMARY
PREPARATION
02.02 SUMMARY
CHAPTER 4 CHEMICAL PROPERTIES
04.01 ORGANIC CARBON
CHAPTER 3 PHYSICAL EXAMINATION 04.01-ACOMBUSTION WITH CO2 DETECTION
03.01 AIR CAPACITY 04.01 METHODS SUMMARY
03.01-AQUICK-TEST FOR BULK DENSITY, 04.02 NITROGEN
POROSITY/PORE SPACE, FREE AIRSPACE AND
04.02-ATOTAL KJELDAHL NITROGEN, SEMI-MICRO
WATER-HOLDING CAPACITY OF UNSIEVED
KJELDAHL TECHNIQUE
COMPOST
04.02-B NITRATE NITROGEN DETERMINATION
03.01-B QUICK-TEST FOR BULK DENSITY,
POROSITY/PORE SPACE, FREE AIRSPACE AND 04.02-C AMMONIUM NITROGEN DETERMINATION
WATER-HOLDING CAPACITY OF SIEVED 04.02-DTOTAL NITROGEN BY COMBUSTION
COMPOST 04.02 METHODS SUMMARY
03.01-C FIELD DENSITY, FREE AIRSPACE AND 04.03 PHOSPHORUS
WATER-HOLDING CAPACITY
04.03-ATOTAL PHOSPHORUS
03.01 METHODS SUMMARY
04.03-B WATER-SOLUBLE PHOSPHORUS
03.02 ASH 04.04 POTASSIUM
03.02-AUNMILLED MATERIAL IGNITED AT 550°C
04.04-ATOTAL POTASSIUM
WITHOUT INERTS REMOVAL
04.04-B WATER-SOLUBLE POTASSIUM
03.02-B MILLED MATERIAL IGNITED AT 550°C WITH
INERTS REMOVAL 04.05 SECONDARY AND MICRO-NUTRIENT
03.02-C UNMILLED MATERIAL IGNITED AT 550°C CONTENT
WITH INERTS REMOVAL 04.05-MG MAGNESIUM
03.02 METHODS SUMMARY 04.05-CA CALCIUM
03.03 BULK DENSITY 04.05-S SULFUR
03.03 METHODS SUMMARY 04.05-NA SODIUM
04.05-B BORON 04.13 ATOMIC ABSORPTION SPECTROMETRY
04.05-CL CHLORIDE 04.13-ACOLD VAPOR AAS TECHNIQUE FOR
04.05-CO COBALT MERCURY IN COMPOST
04.05-CU COPPER 04.13-B ATOMIC ABSORPTION
SPECTROPHOTOMETRY METHODS, US EPA
04.05-FE IRON
METHOD 7000A
04.05-MN MANGANESE
04.13 METHODS SUMMARY
04.05-MO MOLYBDENUM
04.05-ZN ZINC
04.14 INDUCTIVELY COUPLED PLASMA
ANALYSIS (ICP)
04.05 METHODS SUMMARY
04.14-AINDUCTIVELY COUPLED PLASMA-ATOMIC
04.06 HEAVY METALS AND HAZARDOUS EMISSION SPECTROSCOPY, US EPA METHOD
ELEMENTS 6010A
04.06-AS ARSENIC 04.14 METHODS SUMMARY
04.06-BE BERYLLIUM 04.15 SOLUBLE SALTS
04.06-CD CADMIUM
04.06-CU COPPER CHAPTER 5 ORGANIC AND BIOLOGICAL
04.06-CR CHROMIUM PROPERTIES
04.06-PB LEAD 05.01 BIODEGRADABLE VOLATILE SOLIDS
04.06-HG MERCURY 05.02 INDICATOR RATIOS
04.06-MO MOLYBDENUM 05.02-ACARBON TO NITROGEN RATIO
04.06-NI NICKEL 05.02-B CARBON TO PHOSPHORUS RATIO
04.06-SE SELENIUM 05.02-C AMMONIUM TO NITRATE RATIO
04.06-SR STRONTIUM 05.02-DCARBON TO SULFUR RATIO
04.06-VVANADIUM 05.02-E CADMIUM TO ZINC RATIO
04.06-ZN ZINC 05.02-F AGRICULTURAL INDEX
04.06 METHODS SUMMARY 05.02-G CCQC MATURITY INDEX
05.02 METHODS SUMMARY
04.07 OTHER ELEMENTS
04.07-AL ALUMINUM 05.03 COLOR
04.07-SB ANTIMONY 05.03-AFIELD ASSESSMENT OF COMPOST COLOR
AND ODOR
04.07-BA BARIUM
05.03 METHODS SUMMARY
04.07-CN CYANIDES
04.07-AG SILVER 05.04 ENZYME ACTIVITY AND ANALYSIS
04.07-TL THALLIUM 05.04-APHOSPHATASES
04.07 METHODS SUMMARY 05.04-B DEHYDROGENASES
05.04-C PROTEASES
04.08 INORGANIC CARBON
05.04-DCELLULASES
04.08-ACALCIUM CARBONATE EQUIVALENCY
05.04-E PEROXIDASES
04.08 METHODS SUMMARY
05.04 SUMMARY OF METHODS
04.09 CATION EXCHANGE CAPACITY FOR
COMPOST 05.05 BIOLOGICAL ASSAYS
04.09-ACEC BY AMMONIUM DISPLACEMENT AFTER 05.05-ASEEDLING EMERGENCE AND RELATIVE
WASHING GROWTH
04.09-B CEC BY DIRECT DISPLACEMENT 05.05-B IN-VITRO GERMINATION AND ROOT
ELONGATION
04.09 METHODS SUMMARY
05.05-C EARTHWORM BIOASSAY: THE MINNESOTA
04.10 ELECTRICAL CONDUCTIVITY FOR “Z”-TEST
COMPOST 05.05 METHODS SUMMARY
04.10-A1:5 SLURRY METHOD, MASS BASIS
05.06 ODOR
04.10 METHODS SUMMARY
05.06-AFIELD ASSESSMENT OF COMPOST ODOR
04.10 APPENDIX TO 04.10—TEMPERATURE
05.06-B FIELD SAMPLING OF BIOFILTER ODOR
CORRECTION
EMISSIONS
04.11 ELECTROMETRIC PH DETERMINATIONS 05.06 METHODS SUMMARY
FOR COMPOST 05.06 APPENDIX I TO 05.06—EXAMPLE OF
04.11-A1:5 SLURRY PH PERFORMANCE STANDARDS FOR ODOROUS
04.11 METHODS SUMMARY EMISSIONS FROM A PERMANENT
04.12 DIGESTION TECHNIQUES CONSTRUCTED FACILITY
04.12-AMICROWAVE ASSISTED NITRIC ACID 05.06 APPENDIX II TO 05.06—ODOR NOTIFICATION
DIGESTION OF COMPOST FORM
04.12-B NITRIC ACID DIGESTION OF COMPOST AND 05.06 APPENDIX III TO 05.06—RESIDENT ODOR
SOILS COMPLAINT FORM
04.12-C DRY ASH SAMPLE DIGESTION FOR PLANT 05.07 ORGANIC MATTER
NUTRIENTS 05.07-ALOSS ON IGNITION ORGANIC MATTER
04.12-D WATER-SOLUBLE ELEMENTS METHOD
04.12-E AQUA REGIA PROCEDURE
04.12 METHODS SUMMARY
05.07-B HUMIC SUBSTANCES: FULVIC ACID AND
HUMIC ACID EXTRACTION AND CHAPTER 7 PATHOGENS
CHARACTERIZATION 07.00 INTRODUCTION TO PATHOGEN TESTING
05.09-C CALCULATION FOR ORGANIC MATTER 07.01 COLIFORM BACTERIA
DECOMPOSITION 07.01-ATOTAL COLIFORMS
05.07 METHODS SUMMARY 07.01-B FECAL COLIFORMS
05.08 RESPIROMETRY 07.01-C ESCHERICHIA COLI
05.08-ASOUR: SPECIFIC OXYGEN UPTAKE RATE 07.01 METHODS SUMMARY
05.08-B CARBON DIOXIDE EVOLUTION RATE 07.02 SALMONELLA
05.08-C IN-SITU OXYGEN REFRESH RATE 07.02-A1-2 DETECTION TEST AND SALMONELLA
05.08-DDEWAR SELF-HEATING TEST QUANTIFICATION PROCEDURE
05.08-E SOLVITA MATURITY INDEX 07.02-B ENRICHMENT AND QUANTIFICATION OF
05.08-F BIOLOGICALLY AVAILABLE CARBON SALMONELLA IN COMPOST
05.08 METHODS SUMMARY 07.02-C CONFIRMATION PROTOCOLS
05.09 VIABLE WEED SEED IN COMPOST 07.02 METHODS SUMMARY
05.09-ASHIELDS RINSE METHOD 07.03 ENTEROCOCCI
05.09-B PEAT MOSS DILUTION METHOD 07.03-AENTEROCOCCUS
05.09 METHODS SUMMARY 07.03 METHODS SUMMARY
05.10 VOLATILE FATTY ACIDS 07.04 PARASITIC HELMINTHS
05.10-AVOLATILE FATTY ACIDS IN COMPOST 07.04-AVIABILITY OF ASCARIS OVA IN COMPOST
EXTRACT BY GAS CHROMATOGRAPHY 07.04 METHODS SUMMARY
05.10 METHODS SUMMARY 07.04 APPENDIX TO 07.04—INITIAL PERFORMANCE
AND RECOVERY (IPR) AND ONGOING
CHAPTER 6 SYNTHETIC ORGANIC COMPOUNDS PERFORMANCE AND RECOVERY (OPR) FOR
06.00 ANALYSIS OF SYNTHETIC ORGANIC VIABLE ASCARIS OVA
CHEMICALS IN COMPOST 07.05 RECOVERY AND ASSAY OF TOTAL
06.01 CHLORINATED HERBICIDES CULTURABLE VIRUSES
06.02 DIOXIN/FURANS 07.05 US EPA 625R92013, FROM EPA600/4-84/013(R7),
SEPTEMBER 1989 REVISION (SECTION 3)
06.03 ORGANOCHLORINE PESTICIDES
06.04 ORGANOPHOSPHORUS PESTICIDES
06.05 POLYCHLORINATED BIPHENYLS
06.06 SEMIVOLATILE ORGANIC COMPOUNDS
06.07 VOLATILE ORGANIC COMPOUNDS
Introduction
01.01 Manual Content

01.01 TMECC MANUAL CONTENT

01.01-A PURPOSE
1. Compost Quality Verification product safety and market claims. TMECC provides
protocols to sample, monitor, and analyze materials at
1.1 Test Methods for the Examination of Composting all stages of the composting process, i.e., prior to,
and Compost—TMECC provides detailed protocols for during and after composting to help maintain process
the composting industry to verify the physical, control, verify product attributes, assure worker safety,
chemical, and biological condition of composting and to avoid degradation of the environment in and
feedstocks, material in process and compost products at around the composting facility.
the point of sale. Material testing is needed to verify

01.01-B FOREWORD
2. Manual Development attributes that are important for managing specific
applications. Other test parameters and their methods
2.1 Test Methods for the Examination of Composting are of academic interest for research applications.
and Compost—TMECC is a laboratory manual
modeled after American Society for Testing and 2.2.1 Detailed instruction is presented for sample
Materials (ASTM). TMECC provides benchmark collection, preparation, analysis and reporting to
methods for compost analysis to enable comparison of address all phases of composting, feedstock evaluation,
analytical results. Each parameter is presented in its the composting process, and final compost product
own section and generally includes more than one characterization.
protocol or test method. The manual contains more 2.2.2 Sections are grouped into chapters that cover
parameters than might be of concern or interest for a sampling and sample preparation (02); physical
particular situation. properties (03); inorganic chemical properties (04);
2.2 The Standards and Practices, and Market organic and biological properties (05); organic
Development Committees of the US Composting contaminants (06); and pathogens (07).
Council developed a list of pertinent compost product 2.2.3 Each section includes a brief description of the
attributes. Some compost parameters are regulated for parameter’s function in the composting process, for
the protection of public health, safety, and the safety of the product, or in product performance.
environment, while others are product performance

01.01-C REFERENCED METHODS


3. List of Sources Methods of Soil Analysis, Parts I, II and III. Soil Science
Society of America. 1996
3.1 Testing procedures included in TMECC were
North Central Regional (NCR) Publication No. 221
adapted for compost analysis and are based upon, or (Revised). Recommended Chemical Soil Test
developed from the following reference sources: Procedures for the North Central Region Bulletin No.
Analytic procedures used in US EPA Report SW-846, Test 499 (Revised) October 1988 “Recommended Test
Methods for Evaluating Solid Waste, 3rd Edition, Procedures for Greenhouse Growth Media”.
November 1990, as revised. Standard Methods for the Examination of Water and
Association of Official Analytical Chemists (AOAC) Wastewater, 18th Edition, 1992.
Official Methods of Analysis, 1990, 15th edition. The American Society for Testing and Materials (ASTM)
Standard Test Methods, 1988.

Test Methods for the Examination of Composting and Compost August 12, 2001
01.00-1
Introduction
The Composting Process 01.02

01.02 THE COMPOSTING PROCESS

01.02-A KEY PROCESS VARIABLES


1. Management of Key Process Variables 1.2.2 Feedstock Nutrient Balance is the carbon to
nitrogen ratio [C:N] and initial carbon to phosphorus
1.1 Process control parameters include initial carbon
ratio [C:P] needed for vigorous microbial activity and
to nitrogen and carbon to phosphorus ratios, pile
complete degradation/stabilization.
structure and porosity, pile oxygen percent, pile
moisture percent, and pile temperature. Process 1.2.3 Pile Oxygen Percent indicates the exchange of
management includes aggregate size distribution carbon dioxide and other gasses generated through
(particle size), additives and amendments, biological microbial metabolic activity. An adequate supply of
activation and microbial diversity, turning and mixing, oxygen promotes aerobic activity that minimizes odor
aeration, pH and pathogen and weed seed reduction. generation associated with anaerobic conditions.
Odor production must be minimized and in many cases 1.2.4 Pile Moisture Percent is measured to ensure
treated before discharge. Odor management is that sufficient moisture is available within and around
discussed in two parts, odor control and odor treatment. each particle such that pores are not completely filled
The management of process control operating with water (leading to anaerobic conditions) but
parameters is presented in the Compost Facility sufficient to create a moisture film around each particle
Operating Guide, US Composting Council, 1994 and in that supports microbial growth and enzymatic activity.
Municipal-Scale Composting: A decision Makers Pile moisture above 35% will aid in dust control.
Guide to Technology Selection - Composting for
Municipalities; Planning and Design Considerations, 1.2.5 Pile Temperature is a measure of heat
Natural Resource, Agriculture, and Engineering generation by catabolic activity of thermophilic
Service, Cornell University, 1998 (Bulletin NRAES- bacteria. A sustained pile temperature above 55°C kills
94). pathogens and most weed seeds. Eventually, after
significant degradation of the readily available organic
1.2 Key Process Variables define conditions in the matter, pile temperatures decrease and a period (curing
pile for composting. The Key Process Variables must stage) ensues during which mesophilic microbes
be managed during the composting process to ensure (actinomycetes, bacteria, and fungi) begin the slower
consistent marketable product in the shortest time see rate decomposition of the less readily available energy
Table 01.02-A1 Management of Key Process sources (hemicellulose, cellulose, lignocellulose and
Variables. lignin) .
1.2.1 Pile Porosity is a measure of the space between 1.2.6 Retention Time under various temperature
adjacent particles needed for circulation of air and a regimes ensures full stabilization of feedstocks, and full
film of moisture that surrounds particles. degradation of organic phytotoxins that form during the
early stages of composting and during the initial stages
of curing.
Table 01.02-A1 Management of Key Process Variables.
FEED-
STOCK PROCESSING STEPS
KEY PROCESS Feedstock Step 1: Step 2: Step 3: Step 4: Step 5: Step 6: Step 7:
Collected Feedstock Feedstock Composting Odor Compost Compost Compost
VARIABLES and Recovery Preparation Treatment Curing Screening Storing and
Delivered and Refining Packaging

Pile Porosity        
Feedstock Nutrient Balance   
Pile Oxygen Percent     
Pile Moisture Percent      
Pile Temperature  
Retention Time     

August 12, 2001 Test Methods for the Examination of Composting and Compost
01.00-2
Introduction
01.02 The Composting Process

2. Product Attribute Check-List 2.2 An appropriate sampling and testing plan must be
designed specifically for each process step and each
2.1 A check list of product attributes, feedstock
finished product. Refer to TMECC 02.01 Sample
choices, and process steps where compost producers
Collection and Preparation for guidance.
can intervene to manage and control product attributes
is presented in Table 01.02-A2 Management of Product
Attribute Development.
Table 01.02-A2 Management of Product Attribute Development.

MANAGEMENT OF PRODUCT ATTRIBUTE DEVELOPMENT


Feed-Stock Processing Steps
PRODUCT Feedstock Step 1: Step 2: Step 3: Step 4: Step 5: Step 6: Step 7:
ATTRIBUTES Collected Feedstock Feedstock Composting Odor Compost Compost Compost
and Recovery Preparation Treatment Curing Screening Storing and
Delivered and Refining Packaging
SAFETY REQUIREMENTS
Regulated elements      
Pathogens    
MARKET ATTRIBUTES
Man-made inerts   
Growth screening       
Biological stability       
Organic matter content      
pH       
Soluble salt content  
Water-holding capacity       
Bulk density      
Sieve size and Porosity     
Moisture content     
Plant nutrient content       

3. Process Steps and Test Method Selection may match customer and user needs without adding
unwanted and unnecessary value that will not be
3.1 The composting process can be generally compensated with product sales revenue.
characterized by Fig 01.02-A1 Composting Process
Model.
Material Collected & Recyclable
1. Feedstock Recovery
Delivered to Facility Materials
Materials Collected & 1. Feedstock Recovery
Delivered to Facility
2. Feedstock Preparation 4. Odor Treatment
2. Feedstock Preparation
3. Thermophilic Raw Compost
Composting Organic Products
3. Thermophilic
4. Odor Treatment
Composting
5. Compost Curing Cured Compost
5. Compost Curing
6. Compost Screening Screened Compost
6. Compost Screening and Refining Refined Compost
and Refining
7. Compost Storage Other
7. Compost Storing and Packaging Finished Products
and Refining
Finished Product
Fig 01.02-A2. Composting Products Model
Fig 01.02-A1 Composting Process Model.
3.3 Sampling and testing of feedstock and material
3.2 Processing steps 1, 3, 5, 6, and 7 increase the undergoing biological degradation is required to
value of finished product, and require some investment provide the necessary data for process control.
in equipment, time and labor. Parts of these steps may 3.4 Test methods were developed to manage the
include specific criteria to comply with operating broad range of data needed by processors and
permit requirements, (e.g., pathogen treatment during marketers. Each test method is introduced with a
step 3 composting, and perhaps during step 5 compost header; refer to Table 01.02-A3 Test Method Header.
curing). The optional portions that can increase market The header shows the Test Method name and Units of
value should be undertaken only if the value added can measurement and a checklist of Test Method
be covered by sales returns. The Composting Products Applications either to the management of process unit
Model (Fig 01.02-A2) shows sources for products that operations steps one through seven, and verification of

Test Methods for the Examination of Composting and Compost August 12, 2001
01.00-3
General Introduction
The Composting Process 01.02

Product Attributes for compliance with safety standards and market specifications.
Table 01.02-A3 Test Method Header.
Test Method: Parameter. Test Name Units:
Test Method Applications
Process Management Product Attributes
Step 1: Step 2: Step 3: Step 4: Step 5: Step 6: Step 7: Safety Market
Feedstock Feedstock Composting Odor Treatment Compost Compost Compost Standards Attributes
Recovery Preparation Curing Screening and Storing and
Refining Packaging

4. Process Management Discussion matching segregation at the side of the collection


truck(s); (2) delivery to a central processing facility; (3)
4.1 Step 1: Feedstock Recovery—Recovery of recovery of marketable material for recycling, e.g., old
feedstock is the separation of compostable material newsprint and corrugated cardboard, ferrous,
from non-compostable material, hazardous waste, and aluminum, glass, etc.; (4) perhaps recovery of refuse-
other contaminants that can impact compliance with derived fuel; (5) separation of oversize material; (6)
compost quality requirements. Recovery can occur at removal of non-compostable materials, e.g., stones and
various stages of the process, such as sorting by the cigarette filter tips; (7) removal of other materials
generator, collection at curbside, and delivery to a potentially detrimental to compost quality; and (8)
central processing facility where final separation takes recovery of compostable material. (Removal of some
place. For example: non-compostable material can take place after
4.1.1 Recovery of compostable feedstock from composting is complete, if the material being removed
leaves, brush and yard trimmings source-separated by does not cause chemical contamination that prevents
the generator commonly includes the following: (1) compliance with either regulatory or market quality
accumulation in a separate container by the generator; standards.)
(2) curbside and other collection and delivery to a 4.1.4 Separation at a central facility is generally by a
central processing facility; (3) opening and removing combination of manual and mechanical methods, and is
plastic bags, if present; and (4) removing non- shown on the schematic diagram as separation of
compostable and contaminant material that can recyclables, refuse-derived fuel, and rejects disposal.
accompany leaves, brush and yard trimmings (e.g.,
lumber scraps, toys, garden hoses, used vehicle oil and 4.1.5 After recovery, the feedstock is ready to be
air filters, aerosol cans, bricks, concrete and rocks, and prepared for composting. For two compostable
plastic bags). feedstock sources, namely source-separated municipal
solid waste and mixed municipal solid waste, the
4.1.2 Recovery of compostable feedstock from recovered feedstock is sometimes called mixed organic
municipal solid waste is more complex. Two options material.
exist. Option one relies on generators to presort the
compostable and compost compatible material (based 4.2 Step 2: Feedstock Preparation—The feedstock
on a list of acceptable materials provided to them) into preparation step may include physical processing and
a container that is placed at curbside for collection. the addition of compost compatible materials which
Collection can be either separate from other recyclable imparoves composting efficiency. Feedstock
and waste material, or commingled with other waste preparation may include the following:
and secondary resource material. Option two consists 4.2.1 Addition of carbon, nitrogen and phosphorus
of curbside collection of the generator’s accumulation sources by mixing two or more feedstocks to establish a
of material mixed to some degree (as specified) with desired ratio of carbon to nitrogen, and perhaps carbon
other household non-hazardous waste. Collection can to phosphorus, to control odor generation, and to
be either separate from other recyclable material, or achieve market requirements for product stability.
commingled. After delivery to a central processing 4.2.2 Adjusting initial porosity to satisfy
facility, material received from both options are requirements for free airspace (to aid oxygen and gas
handled and processed in essentially the same manner, exchange) and water-holding capacity (moisture).
because both include not less than 3 to 11% “mistakes” Reducing the particle size through shredding or
that must be identified and removed from composting tumbling increases surface area, helps creates uniform
feedstock material. “Mistakes” can include recyclable particle size, improves aeration (if particles aren't too
material and material that can potentially cause small), and reduces volume. An alternative is particle
compost quality problems. size selection through screening. Adding a bulking
4.1.3 Recovery includes: (1) collection and perhaps agent, such as wood chips, to increase porosity and aid
segregation of presorted material at curbside by a

August 12, 2001 Test Methods for the Examination of Composting and Compost
01.00-4
General Introduction
01.02 The Composting Process

air flow through the composting mass is normally 4.5 Step 5: Compost Curing—Customers that require
necessary. a mature product may specify a greater degree of
4.2.3 Adding water to the feedstock to adjust the product biological stability. Compost curing is the last
moisture level to a desirable range. stage of composting that occurs after much of the
readily metabolized material has been decomposed.
4.2.4 Adding a small volume of compost that is in its
Compost curing provides for additional stabilization,
peak heat thermophilic phase can ‘jump start’ the
and allows further decomposition of cellulose and
process by providing a cross-section of biological
lignin. Cured compost is a highly stabilized product
species for rapid colonization and biological activity.
that results from exposing compost to a prolonged
4.2.5 Mixing to homogenize the feedstock, starter period of humification and mineralization, ranging
compost, and other additives, to distribute water from six to eight months.
uniformly, and to break down oversized particles of
4.6 Step 6: Compost Screening and Refining—
feedstock.
Screening is necessary to remove contaminants such as
4.3 Step 3: Composting—Composting is a natural oversized material, stones, metal fragments, glass, film
biological degradation process that is controlled and plastic, hard plastic, and sharps. Residue from
accelerated at a composting facility. Composting is the screening and refining can be recycled, or it might be
transformation of biologically decomposable material disposed of at an incinerator or landfill. Screening also
through a controlled process of biooxidation that results enables size classification to suit customer needs.
in the release of carbon dioxide, water, and minerals, Some customers may require that essentially all man-
and in the production of stabilized organic matter made inert material is removed from compost to
(compost or humus) that is biologically active. enhance its aesthetic acceptability. Further refining can
Because the biological process of composting follows a remove small stones, glass, metal fragments, hard
similar course regardless of the organic materials that plastic, film plastic, and sharps. This step typically
are present in the feedstock, the schematic diagram follows the compost curing step so as to retain bulking
(Fig. 01.02-A1) shows composting as a step common to material in the compost as long as possible as an aid to
each feedstock and one that may include the following: aeration
4.3.1 Aeration to maintain optimum conditions for 4.7 Compliance with Compost Safety Standards—
aerobic microbial activity, to supply oxygen, to buffer Standards to protect public health, safety, and the
pH and immobilize ammonium, to remove heat, to environment typically focus on the content of trace
remove carbon dioxide, to remove moisture, to strip metals and pathogens in compost. However, soluble
volatile compounds, and to avoid anaerobic conditions salts, pH, man-made inerts, film plastic and organics
and odor generation. may also be the focus of compliance standards in some
4.3.2 Temperature control to reduce pathogens to cases. Verification is by standard methods for
background levels and destroy weed seeds, and to sampling, preparation and analysis. If a compost
maximize the rate of decomposition both during the product meets the minimum standards for safety, the
high temperature thermophilic phase and afterward product is a “General Use Compost” and may be
during the mesophilic phase. distributed for use as a soil amendment. Although a
product may meet minimum requirements for public
4.3.3 Addition of make-up water to maintain health, safety, and the environment, it may not,
moisture content for aerobic conditions, and to however, suit a particular customer's aesthetic
maximize organic decomposition. requirements for example, or a customer's requirements
4.3.4 Mechanical agitation or turning to thoroughly for stability or for nutrient value. Product marketing
mix make-up water uniformly throughout the issues will dictate the extent of curing, refining, and
decomposing mass, to break up air channels and amending necessary to meet customers' needs. If the
clumps, to prevent fly reproduction, and to produce a product does not meet the suggested minimum
uniform product. standards, the product may be reprocessed to meet the
4.4 Step 4: Odor Treatment—Process air is captured standards, or may be marketed as a “Designated Use
and routed through a biofilter or other positive Compost”, with specific restrictions on its use
treatment method. In a biofilter, operating conditions appropriate to its characteristics. For example:
must favor porosity, ample oxygen and moisture to 4.7.1 A compost which does not meet the minimum
ensure conditions highly favorable to active microbial standards for compost stability could be (1) composted
populations that are not associated with odor-causing for another week or more until it is sufficiently stable to
compounds such as hydrogen sulfide, volatile fatty meet the stability standard, or (2) used in an application
acids and ammonia. where its relatively low stability would not be harmful.

Test Methods for the Examination of Composting and Compost August 12, 2001
01.00-5
General Introduction
The Composting Process 01.02

4.7.2 A compost which contains more film plastic Compost. These three grades of compost are
than the standard could be (1) refined to remove the manufactured for reliable and sustainable end markets.
film plastic, or (2) marketed for restricted use where the Each of the three grades of compost may be amended
film plastic content would be acceptable. with supplemental material (amendments) added during
composting or to compost, to provide attributes
4.8 The Composting Schematic Diagram (The
required by customers for certain compost products,
Process Model, Fig 01.02-A3) was developed as an aid
such as product bulk, product nutrient value, product
to a broad understanding of process steps in the
pH, and soils blend. Marketing consultants have
manufacture of compost suitable for general
defined a dozen or more major market segments.
distribution or for designated uses.
Marketers supply compost to many segments and more
4.8.1 As noted previously, a product that complies are being developed.
with regulatory standards for safety is suitable for
4.8.3.1 Raw Compost is generally suitable for use
distribution and use as a soil amendment. It is
as landfill cover material and as surface mine
classified “General Use Compost”.
reclamation material. It may be suitable for other
4.8.2 “Designated Use Compost”, on the other hand, additional uses.
is the classification that does not comply with safety
4.8.3.2 Refined Compost is generally suitable for
standards and its distribution and use is subject to
field nursery use, sod production, silviculture,
regulatory control. The authors elected not to show
agriculture, commercial landscaping, and specialty
market segments for this class of compost on the model
applications such as erosion control and for biofilters.
schematic, because use is restricted by local or state
It may be suitable for other additional uses.
regulation. Uses are potentially numerous. It might be
used, for example, as landfill daily cover, or refined for 4.8.3.3 Cured Compost may generally be used for
land reclamation, and/or cured for other designated, high-end landscaping, delivered topsoil, bagged/retail
restricted markets. markets, container nurseries, and specialty applications,
(e.g., wetlands redevelopment, etc.).
4.8.3 General Use Compost classification is shown
as the source of supply for three grades of compost,
namely Raw Compost, Refined Compost, and Cured

August 12, 2001 Test Methods for the Examination of Composting and Compost
01.00-6
Introduction
01.03 Composting Technology Groups

01.03 COMPOSTING TECHNOLOGY GROUPS

01.03-A OPERATION CHARACTERISTICS


1. Technologies 2.1.1 Food Processing Residuals—compostable
material remaining after fruit, vegetables, grains, nuts,
1.1 Technologies used for composting cover a broad
and meat are processed for consumption.
spectrum of options. The composting industry
recognizes five groups of composting technologies, as 2.1.2 Manure and Agricultural By-Products—
shown in the Table 01.03-A1. generated at racetracks, feedlot and other animal
feeding operations, farms, nurseries, and greenhouses.
Table 01.03-A1 Composting Technology Groups. Compost produced from residuals generated from
Management Strategies farms, nurseries, and greenhouses can be readily
Step 3: Composting GROUP 1 GROUP 2 GROUP 3 GROUP 4 GROUP 5
recycled into those operations. However, huge
Weather Protection Open Open Covered Covered Covered
Pile Configuration Piles Windrows Piles and Windrows Tunnel and
quantities of manure generated at racetracks, feedlots,
Tunnels Trenches Vessel and swine and poultry confinement facilities can pose a
Beds and Systems
Bays significant challenge to facility operators.
Process Passive Active Active Active Active 2.1.3 Forestry and Forest Product Residuals—
Management of
Key Process Variables includes bark and sawdust, and fiber fines residue and
biosolids generated by the papermaking process. Bark
Pile Undisturbed Turned Static Turned Turned and sawdust can be used in the composting industry as
Structure
a carbon source with other feedstock material or as a
Feedstock nutrient Unmanaged Initial C:N Initial C:N Initial C:N Initial C:N
balance ratio set ratio set ratio set ratio set bulking material to increase porosity of the feedstock
Pile Oxygen and pH Unmanaged Convective Forced Mechanical Forced mix.
Aeration Aeration Aeration Aeration
Pile Moisture Unmanaged Mix in Mix in Mix in Mix in 2.1.4 Biosolids, or Sewage Sludge—the solid
Make-up Make-up Make-up Make-up material generated by the biological treatment of
Pile Temperature Unmanaged Turning Blower Blower Blower sewage at a wastewater treatment plant. In addition to
Control Control Control Control
Retention Time 12-14 2-12 2-6 2-5 2-4 being composted, sewage sludge can be recycled for
months months months months months beneficial use by direct application onto land as a
fertilizer.
1.1.1 The five [5] technology categories are based on 2.1.5 Leaves, Brush and Yard Trimmings (Yard
the predominant composting unit operation Waste)—typically consists of leaves, brush, grass
characteristics, a technology classification system clippings, plant trimmings, and plant remains.
devised and peer-reviewed for the Composting Facility Historically this material has been collected with
Operating Guide, US Composting Council, 1994 municipal solid waste and incinerated or landfilled.
(http://compostingcouncil.org). Many communities have restricted incineration and
1.2 The composting industry categorization of landfilling of these materials. Instead, they are
technologies is generic. Specific technology suppliers separately collected and recycled for beneficial use by
offer variations within a technology group. A single directing it to a mulching or composting facility.
technology should offer a combination of alternatives 2.1.6 Source Separated Organic Waste (SSOW)—
that will address the seven steps of the composting consists of the compostable and composting compatible
process. fraction of municipal solid waste, accumulated and
1.3 Sampling and testing plans must be designed to presorted by the generator, and collected separately
suit the specific approach used in each composting from household hazardous material and sometimes non-
project. compostable material. The compostable and
1.4 Sampling and testing marketable product provides composting compatible fraction can be directed to a
the data needed to demonstrate compliance with central composting facility. For example, a
environmental standards and to provide users with compostable organics collection program that relies on
information needed to plan for proper application of source separation by the generator could include leaves,
compost products. brush and yard trimmings, food scraps, wet and soiled
paper, diapers and sanitary products, pet waste, and dry
2. Composting Feedstocks paper packaging that is not recycled because of weak or
2.1 Six types of source materials commonly nonexistent markets. Source-separated organic waste
composted: includes residential, institutional and commercial

Test Methods for the Examination of Composting and Compost August 12, 2001
01.00-7
Introduction
Composting Technology Groups 01.03

sources, and can include the domestic portion of the Equipment and labor for sorting is often required and
industrial solid waste stream. returns should offset costs.
2.1.7 Mixed Municipal Solid Waste (MSW)— 3.1.2 Step 2—Feedstock Preparation involves
includes various discards from residential, commercial, establishing the initial porosity and degradability, i.e.,
and institutional sources that are commonly taken to C:N and C:P ratios, moisture content, etc.
incinerators or landfills. The largest components of 3.1.3 Step 3—Thermophilic Composting reduces
mixed municipal solid waste are typically paper and pathogens, which is a fundamental requirement for
paper products, leaves, brush and yard trimmings, feedstock processing and destroys most weed seeds. At
wood, food scraps, glass, plastics, and metals. The this point, markets may be able to accept the material
composition of mixed MSW varies depending on the even though it is neither biologically stable nor free of
characteristics of the waste generators in the service organic phytotoxins that inhibit seed germination and
area, but usually from about 50% to 65% is plant growth. (e.g., land applied for sufficient time to
compostable when recovered by separation at a central reach a level of stability and maturity before planting
facility. Mixed municipal solid waste will contain that benefits crop growth and soil conservation).
relatively fewer recyclables and a relatively higher
fraction of compostable material when an aggressive 3.1.4 Step 5—Compost Curing increases biological
source-separated recycling collection program operates stability, may further reduce pathogens, and with
in conjunction with mixed municipal solid waste aeration eliminates organic phytotoxins. The degree of
collection. curing should match the intended use of the product.
A bagged product will require a high degree of curing
2.2 Market attributes of finished compost product are because of its potential use as potting soil and garden
influenced both by the feedstock used and by bed amendment. Product that will be sold in bulk for
composting process control. direct application for agricultural, landscape, roadside,
2.3 Sampling and testing plans must be designed to or reclamation settings may not require as much curing
suit the specific feedstocks used in each composting as compost used a potting soil.
project. 3.1.5 Step 6—Compost Screening and Refining
3. Compost Product Overview removes oversized material and other unwanted
material, and can provide the particle size and texture
3.1 A variety of value-added products are developed
of product for particular end use requirements.
by processors (Fig 01.02-A2 Composting Products
Screening and refining equipment is an investment that
Model).
should increase product revenues.
3.1.1 Step 1—Feedstock Recovery involves an
3.1.6 Step 7—Compost Storing and Packaging deals
inspection of materials received at the tip floor or
with seasonal demand patterns that don't match
receiving area to removed unwanted items from the
feedstock availability patterns and may generally be
feedstock. This step may also be used to gather items
inevitable. No degradation of product should be
that have commercial value in the traditional recycle
allowed, and if storage is inevitable it can be exploited
markets, such as ferrous, plastics, and clean paper.
to add still more value for the highest markets of all
that include bagged and amended products.

August 12, 2001 Test Methods for the Examination of Composting and Compost
01.00-8
Sample Collection and Laboratory Preparation
02.01 Field Sampling of Compost Materials

Test Method: Field Sampling of Compost Materials. Five Protocols Units: NA


Test Method Applications
Process Management Product Attributes
Step 1: Step 2: Step 3: Step 4: Step 5: Step 6: Step 7: Safety Market
Feedstock Feedstock Composting Odor Treatment Compost Curing Compost Compost Standards Attributes
Recovery Preparation Screening and Storing and
Refining Packaging
02.01-A 02.01-A 02.01-A 02.01-A 02.01-A 02.01-A 02.01-A 02.01-A 02.01-A
02.01-B 02.01-B 02.01-B 02.01-B 02.01-B 02.01-B 02.01-B 02.01-B 02.01-B
02.01-C 02.01-C
02.01-D 02.01-D 02.01-D 02.01-D 02.01-D 02.01-D 02.01-D
02.01-E 02.01-E 02.01-E 02.01-E 02.01-E 02.01-E

02.01 FIELD SAMPLING OF COMPOST MATERIALS


DISCLAIMERS 1.2 Values stated in SI units are to be regarded as the
(1) The methodologies described in TMECC do not purport to address all standard. Values given in parentheses are provided for
safety concerns associated with their use. It is the responsibility of the information only.
user of these methods to establish appropriate safety and health
practices, and to determine the applicability of regulatory limitations 2. Referenced Documents
prior to their use.
(2) All methods and sampling protocols provided in TMECC are subject to ASTM D 5231-92, Determination of the Composition of
revision and update to correct any errors or omissions, and to Unprocessed Municipal Waste. In Annual Book of
accommodate new widely accepted advances in techniques and ASTM Standards, Vol. 04.08
methods. Please report omissions and errors to the U.S. Composting
Council Research and Education Foundation. An on-line submission ASTM D 4547-91, Sampling Waste and Soils for Volatile
form and instructions are provided on the TMECC web site, Organics. In Annual Book of ASTM Standards, Vol.
http://www.tmecc.org/addenda.
04.08
(3) Process alternatives, trade names, or commercial products as mentioned
in TMECC are only examples and are not endorsed or recommended by A Plain English Guide to the EPA Part 503 Biosolids
the U.S. Department of Agriculture or the U.S. Composting Council Rule. US EPA Office of Wastewater Management.
Research and Education Foundation. Alternatives may exist or may be
developed.
EPA/832/R-93/003, September 1994.
Test Methods for Evaluating Solid Waste,
1. Source Physical/Chemical Methods. US EPA SW-846. 3rd
1.1 This section covers sampling procedures for Edition, September, 1986.
compost and composting feedstock. Statistical Quality Control Handbook. Western Electric
1.1.1 Method 02.01-A Compost Sampling Principles Company, Inc. 2nd Edition. 1958.
and Practices adapted from sampling procedure 3. Terminology
documents provided by Dr. William F. Brinton, Woods 3.1 aliquot, n—a sub-sample of a material prepared
End Research Laboratory, 1996. for, and subjected to laboratory analysis. A sub-sample
1.1.2 Method 02.01-B Selection of Sampling size smaller than 1 g may be used to represent more
Locations for Windrows and Piles. than 1000 kg of compost.
1.1.3 Method 02.01-C Sampling Plan for 3.2 attribute verification, n—a laboratory protocol
Composted Material—adapted from the US EPA’s that includes standard reference materials, checks and
Test Methods for Evaluating Solid Waste, blanks to validate analytical determinations.
Physical/Chemical Methods, SW-846, Third Edition, 3.3 confidence interval, n—a statistical range with a
September, 1986. Consideration and importance was specified probability that a given parameter lies within
placed on sampling composted solid waste rather than that range. The magnitude of the range increases as the
sampling sediments, sludges, or soils for waste specified probability is increased.
analysis. Most information remained unchanged. The
majority of the information on sampling was taken from 3.4 process monitoring, n—samples collected at
Chapter Nine, Volume II of the U.S. EPA Solid Waste predetermined intervals within the composting process
- 846 Manual. to track the targeted changes in biological, chemical
and physical characteristics; key process variables in
1.1.4 Method 02.01-D Composting Feedstock compost piles that should be monitored include
Material Sampling Strategies. porosity, oxygen percent, moisture percent,
1.1.5 Method 02.01-E Data Quality Management temperature, retention time or age.
and Sample Chain of Custody. 3.5 process variability, n—deviations from optimal
management procedures of compost production that

Test Methods for the Examination of Composting and Compost August 27, 2001
02.01-1
Sample Collection and Laboratory Preparation
Field Sampling of Compost Materials 02.01

may induce deviations in the desired result and sub- composting process begins with the material placed in piles,
optimal finished compost. windrows or reaction vessels for composting.

3.6 product variability, n—heterogeneity of the 4.2.2 Prepared Feedstock Sampling—Samples


chemical, biological and physical characteristics of a should be taken after feedstock preparation before
compost product attributable to both the composting composting. Facility operators can provide the best
process and the heterogeneity of input feedstocks. information for the locations to obtain feedstock
samples.
3.7 representative sample, n—a sample that
accurately reflects the average chemical, biological and 4.2.3 Composting and Compost Curing Process
physical characteristics of interest from the source of Control Sampling Locations—The sampling location
feedstock, bulk material or compost batch in question. for process monitoring during composting, step 3, and
compost curing, step 6, is indicated in Fig 02.01-B1
3.8 sample collection frequency, n—retrieval of Hypothetical Sample Collection Pattern from a
representative samples at intervals that accurately Compost Pile.
represent the status within the process step of interest
for the bulk of compost in question or batch of concern. 4.2.4 Finished Compost Sampling Locations—
Finished compost is expected to match the needs of the
3.9 statistical validity, n—determinations made from customers, and may be obtained from step 3,
a sample that accurately represent the average Composting; step 5, Compost Curing; step 6, Compost
characteristics of the compost of interest. Screening and Refining; and step 7, Compost Storing
4. Sampling Collection and the Composting and Packaging as indicated in Chapter 01.00 Fig 01.02-
Process A2 Composting Products Model. Finished compost
samples are taken from the actual product that is
4.1 A generalized model developed to represent the released for distribution to an end-user.
aerobic composting process is presented in Fig 02.01-1
Composting Unit Operations Model. 5. Summary of Methods
4.1.1 Market attribute analytical values for a finished 5.1 Method 02.01-A Compost Sampling Principles
compost vary according to the type or blend of and Practices—Review of sampling design schemes
composting feedstocks and composting process. adapted from sampling procedure documents provided
Value-added compost products are illustrated in by Dr. William F. Brinton, Woods End Research
Chapter 01.00 Fig 01.02-A2 Composting Products Laboratory, Inc.
Model. Sampling and testing plans must be designed to 5.2 Method 02.01-B Selection of Sampling Locations
suit the feedstock used in composting, the specific for Windrows and Piles—Descriptions of sample
approach to feedstock preparation and composting collection as sets of compost sub-samples collected and
process management in each composting project, and combined to represent the average chemical, physical
specifically for each finished product. and biological characteristics of the compost material
4.2 Selection of Sampling Method: for a batch windrow or pile of cured or curing compost.
4.2.1 Feedstock Sampling Location—The sampling 5.3 Method 02.01-C Sampling Plan for Composted
location for composting feedstock is after feedstock Material—Review of US EPA SW-846 sampling plan
recovery (step 1) has been completed. Feedstock guidelines and statistical procedures for estimating
sampling is performed after routine removal of required minimum number of samples.
recyclable and/or problem materials. Samples should 5.4 Method 02.01-D Composting Feedstock Material
be taken before feedstock preparation (step 2), i.e., Sampling Strategies—A representative sample of
before shredding or size reduction, and before feedstock is collected to identify its chemical and
supplemental nutrients, bulking agents or water have physical characteristics.
been added. The facility operators can provide the best
information for the locations to obtain feedstock 5.5 Method 02.01-E Data Quality Management and
samples. Sample Chain of Custody—Consideration for third-
party sample collection and preparation. Also, an
NOTE 1—Once the feedstock preparation, (step 2 of the
composting process model), is completed, the actual
example form and description of the parameters needed
for a chain of custody report.

August 27, 2001 Test Methods for the Examination of Composting and Compost
02.01-2
Sample Collection and Laboratory Preparation
02.01 Field Sampling of Compost Materials

Recyclable Materials
Materials Collected and 1. Feedstock Recovery
Delivered to the Facility Dangerous
Materials

Chemical
Contaminants
Particle Sizing
Additives
Water
Bulking
2. Feedstock
Air Preparation
Recycled
Compost Water
Mixing
DO NOT Turn and Mix

Air
Water 3. Composting 4. Odor Treatment
Turning and
Mixing

Air
Exhaust
Water 5. Compost Curing
Turning and
Mixing

6. Compost Screening Residue


Air
and Refining

Amendments
7. Compost Storing
Finished Products
Second Level Detail Model Turning and and Packaging
Mixing

Fig 02.01-1 Composting Unit Operations Model.

6. Significance and Use 6.4 Method 02.01-D Composting Feedstock Material


Sampling Strategies—A general guide for feedstock
6.1 Method 02.01-A Compost Sampling Principles
sample collection. Specific methods should be
and Practices—Source of general guidelines and
modified for differing feedstock materials.
considerations needed to develop an appropriate
compost sampling plan. 6.5 Method 02.01-E Data Quality Management and
Sample Chain of Custody—A method of tracking a
6.2 Method 02.01-B Compost Material Sampling
collected sample from date, time and location of
Strategies—A general guide for compost sample
sampling through completion of laboratory analysis.
collection and preservation from compost curing piles.
6.3 Method 02.01-C Sampling Plan for Composted 7. Interference and Limitations
Material (from SW-846 Chapter Nine, part 1)—The 7.1 Analytical error associated with sampling and
initial, and perhaps most critical element in a program handling is compounded when multiple properties with
designed to evaluate the physical, chemical and conflicting sampling needs are measured from the same
biological properties of a compost is the plan for sample. For example, it is a good idea to subdivide and
sampling the material in question. It is understandable remix samples repeatedly if mineral and metal tests are
that analytical studies, with their sophisticated being performed. This improves homogeneity and
instrumentation and high cost, are often perceived as reduces sample variance. Unfortunately, this same
the dominant element in a characterization program. method induces excessive volatilization of some of the
Yet, despite that sophistication and high cost, analytical compounds, and causes microbial cross-contamination.
data generated by a scientifically defective sampling Therefore, the sampling plan must specify a separate
plan have limited utility. sampling and handling scheme for each test parameter
that requires special sampling.

Test Methods for the Examination of Composting and Compost August 27, 2001
02.01-3
Sample Collection and Laboratory Preparation
Field Sampling of Compost Materials 02.01

7.2 Method 02.01-B Compost Material Sampling 8.2 For most feedstock or compost samples, use
Strategies—As compost heterogeneity increases, the containers made of stainless steel, plastic, glass or
number of sub-samples should be increased. If Teflon. These materials will not change compost
insufficient numbers of samples are collected, chemical quality. Laboratories provide advice on
analytical results will not represent the compost in appropriate sample containers, preservatives and
question. shipping instructions when requested.
7.2.1 Moisture loss or gain during sample handling 8.3 A representative compost sample must be
and splitting may become significant. It is therefore collected from appropriate sampling locations and
necessary to mix and split a sample under sheltered consist of no less than 15 point-samples. Sampling
conditions, such as inside a building where wind, locations along the perimeter of the compost pile where
temperature and sunlight or precipitation will not compost point-samples will be extracted and vertical
distort the compost moisture. distances from the ground or composting pad surface
7.3 Method 02.01-C Sampling Plan for Composted shall be determined at random, and shall be
Material—Knowledge of or access to statistical representative of the compost on the site.
procedures is required. 8.3.1 Determine the number and types of sampling
7.4 Method 02.01-D Composting Feedstock Material and shipping containers to be used. The composite
Sampling Strategies—Sample heterogeneity of sample is placed in a sanitized container and
feedstock may be much higher than that of the finished thoroughly mixed. Follow proper quality
composted product. It is crucial that all sampling plan assurance/quality control procedures for sample
collection procedures are followed to maximize the preservation, storage, transportation and transfer.
reliability and accuracy of the feedstock sample Sample the cured compost and aliquot 12 L (3 gal)
analytical results. sub-samples from the composite sample and place in a
sanitized plastic container and seal.
7.4.1 Moisture loss or gain during sample handling
and splitting may become significant. It is therefore 8.3.2 Utilize the Student's “t”-test with a confidence
necessary to mix and split a sample under sheltered interval of 80% to statistically analyze the test data.
conditions, such as inside a building where wind, Refer to TMECC 02.01-A, paragraph 9.10 Sampling
temperature and sunlight or precipitation will not Intervals for guidance in determining sample collection
distort the feedstock moisture. frequency.
8.4 Test Methods versus Sampling Methods—The
8. Sample Handling
laboratory test method and analytical parameter of
8.1 Collect samples from areas of the compost pile interest dictate the method of sample collection, type of
that are representative of the general appearance, and container for shipping and storage of samples and
avoid collecting atypically moist samples (> 60% sample handling procedures required. Table 02.01-1
moisture, wet basis). If balls form during the process provides a partial list of analytical traits that are
of blending and mixing of point-samples, the compost affected by sample collection and handling. In general,
sample is too wet. Excessively moist compost will volatile compounds and elements, physical bulk factors
cause unreliable physical and biological evaluation. and microbiological samples require special
considerations when developing the sampling plan.
Table 02.01-1 Partial list of test parameters that require special sampling and handling considerations.
Alteration of Sampling for
Test Parameter Principle Constraint Associated Error Corrective Action
Total-N Volatilization loss of NH3 Underestimation of total N Place in container quickly
during sample handling and volatile N with minimal stirring
Volatile fatty acids (VFA) Volatilization loss of VFA Underestimation of VFA Place in container quickly
during sample handling content with minimal stirring
Microbiology (pathogens) Contamination from tools, Over or under estimation of Use only clean, sterile
buckets, air pathogens containers and implements
Bulk Density Excess sample moisture Overestimation of Take large, oversized samples
volume/weight

8.4.1 In each case the determination for a trait of sampling, but accuracy of the expected determination
interest can be changed adversely by improper sample may be biased and incorrect.
collection and handling, and consequently lead to 8.5 Containers, Post-Sample Handling—For each
erroneous conclusions. Analytical precision or relative type of parameter measured after sampling specific
variability may not be affected by inappropriate containers and holding times should be observed prior

August 27, 2001 Test Methods for the Examination of Composting and Compost
02.01-4
Sample Collection and Laboratory Preparation
02.01 Field Sampling of Compost Materials

to and during transport to a laboratory (see Tables store samples at 4°C when delays in lab preparation are
02.01-2 through 02.01-6). Use multiple containers to anticipated.
preserve sample integrity as necessary. 8.5.4 Collection and storage of samples for organic
8.5.1 Despite the wide variation in sample holding compound analysis - polychlorinated biphenyls (PCBs),
times and condition requirements, all compost samples polynuclear aromatic hydrocarbons (PAHs) or volatile
targeted for general testing should be chilled fatty acids (VFAs) - require glass containers with
immediately upon collection and preparation. Refer to Teflon lids, or exclusively Teflon containers. Sample
Tables 02.01-2 through 02.01-6 to find the most containers should be filled to overflowing with material
appropriate storage temperature for each test parameter to minimize airspace in the container and reduce
of interest. volatilization of organic compounds during storage.
8.5.2 When plastic containers are acceptable, use 8.5.5 Include proper Chain-of-Custody information:
double Ziploc®-type 4-8 L (1-2 gal) bags marked on the date, time, name of the sampling entity and name
exterior with a marking pen with insoluble ink, and individual responsible for sample. Refer to Method
placed with several cool-packs in a large polystyrene 02.01-E Data Quality Management and Sample Chain
cooler or similar insulated container. of Custody for an example form and description of
8.5.3 Ship the samples to the laboratory for delivery parameters needed to complete a chain of custody
within 24 h or less. Request that the laboratory staff report.
Table 02.01-2 Physical Parameters: Sampling containers and conditions for compost and source ingredient testing.
Maximum Holding Time
Test Parameter of Interest Container Conditions
Allowed in Lab
Bulk Density, Hydraulic Conductivity,
P, G 4°C 7d
Porosity, Water Holding Capacity
Temperature NA NA Immediate, no delay
Total Solids P, G 4°C 24 h
NOTE 2—P=Plastic; G=Glass

Table 02.01-3 Organic and Biological Properties: Sampling containers and conditions for compost and source ingredient testing.
Maximum Holding Time
Test Parameter of Interest Container Conditions
Allowed in Lab
Respirometry P, G 4°C 24 h
Organic Carbon P, G 4°C 14 d
Volatile Fatty Acids G (2 L CWM) 4°C 14 d
Volatile Solids P, G 4°C 14 d
NOTE 3—P=Plastic; G=Glass

Table 02.01-4 Chemical Parameters: Sampling containers and conditions for compost and source ingredient testing.
Maximum Holding Time
Test Parameter of Interest Container Conditions
Allowed in Lab
Acidity/Alkalinity (pH),
Electrical Conductivity,
Kjeldahl Nitrogen, Nitrate Nitrogen
(NO3-N), Nitrite Nitrogen (NO2-N), P, G 4°C 48 h
Ammonia Nitrogen and Ammonium
Nitrogen (NH3-N, NH4-N),
Sulfide
All other Metals P, G 4°C 6 months
Chloride, Sulfate P, G 4°C 28 d
Chromium VI P, G 4°C 24 h
Mercury P, G 4°C 28 d
NOTE 4—P=Plastic; G=Glass

Test Methods for the Examination of Composting and Compost August 27, 2001
02.01-5
Sample Collection and Laboratory Preparation
Field Sampling of Compost Materials 02.01

Table 02.01-5 Pathogens: Sampling containers and conditions for compost and source ingredient testing.
Maximum Holding Time
Test Parameter of Interest Container Conditions
Allowed in Lab
Enteric Virus G -70°C >8h
Enteric Virus SP, G 4°C 8h
Coliforms and other bacteria SP, G 4°C 48 h
Helminth Ova SP, G 4°C 1 month
NOTE 5—SP=Sterilized Polypropylene; G= Sterilized Glass

Table 02.01-6 Synthetic Organic Compounds: Sampling containers and conditions for compost and source ingredient testing.
Maximum Holding Time
Test Parameter of Interest Container Conditions Allowed in Lab
Chlorinated Herbicides, and G, Teflon lined cap
4°C 7 d until extraction
Chlorinated Hydrocarbons, PCB (2-1/2 L.A.J.)
16 oz B.R.
Chlorinated Pesticides 4°C 7 d until extraction
(2-1/2 L.A.J.)
Dioxins & Furans,
Nitroaromatics and Isophorone, and G, Teflon lined cap 4°C
7 d until extraction
Polycyclic Aromatic Hydrocarbons, (2-1/2 L.A.J.) store in dark
PAH
Phthalate esters G, Teflon lined cap 4°C 7 d until extraction
G, Teflon lined septum
Purgeable aromatic hydrocarbons 4°C 14 d prior lab testing
(40-mL Glass V)
G, Teflon-lined Septum
Semi-Volatile Organics 4°C 7d
(2.5-L Jug)
G, Teflon-lined Septum
TCLP Sample 4°C 7 d until extraction
(2.5-L Jug)
G, Teflon lined septum
Volatile Organic Compounds (VOC) 4°C 14 d preserved in HCl†
(40-mL Glass V)
NOTE 6—P=Plastic; G=Glass, HDPE=High Density Polyethylene
†—Evaluation data is being sought to confirm this requirement for curing and finished composts.

August 27, 2001 Test Methods for the Examination of Composting and Compost
02.01-6
Sample Collection and Laboratory Preparation
02.01 Field Sampling of Compost Materials

Test Method: Compost Sampling Principles and Practices Units: NA


Test Method Applications
Process Management Product Attributes
Step 1: Step 2: Step 3: Step 4: Step 5: Step 6: Step 7: Safety Market
Feedstock Feedstock Composting Odor Treatment Compost Curing Compost Compost Standards Attributes
Recovery Preparation Screening and Storing and
Refining Packaging
02.01-A 02.01-A 02.01-A 02.01-A 02.01-A 02.01-A 02.01-A 02.01-A 02.01-A

02.01-A COMPOST SAMPLING PRINCIPLES AND PRACTICES


COMMENT—This section was adapted from sampling consideration and a sample collection process must be
procedure documents provided by Dr. William F. Brinton, designed to support to this requirement.
Woods End Research Laboratory, 1996.

9. Justification for Compost Sampling Regulatory


Identify
Yes regulatory
9.1 Sampling of compost and compost products is an sampling? rules
essential aspect of process monitoring, quality control,
marketing and labeling, and regulatory compliance. No
Like other functions of site management, sample
collection involves carefully planned and often labor Process
intensive activities. Four common reasons for compost Management
Quality Define use
Yes
sampling are described: Control for data
Market label
9.1.1 Ingredient Analysis—basic data on source requirement
ingredients are needed for the design of a composting
process or identification of an optimal composting No
feedstock recipe.
Source
ingredients
9.1.2 Process Design and Monitoring—composting (feedstock evaluation)

process evaluation requires information on material


Process Define use
characteristics and process benchmarks. Specific design?
Yes
for data
Bench scale

sample collection protocol is designed for each


parameter of interest. Process
management
9.1.3 Marketing and Labeling—specification sheets
or product labels for compost are needed to compare
product with others in the marketplace.
Identify qualified Acquire appropriate Train staff to collect Collect
9.1.4 Regulatory Compliance—compost process and laboratory and
communicate
sampling tools and and preserve representative
sample(s), prepare
shipping representative
product requires periodic testing for compliance with sample analytical
requirements.
materials. samples for shipment and
send to Laboratory
specified traits including certain metals, pathogens,
stability and maturity. Fig 02.01-A1 Compost sampling decision tree, overview of
sampling objectives.
9.2 Use of Sampling Data—Sampling decisions
require an understanding of the need for data 9.3 Types of Sampling—Two types of sample
collection, specifically how to sample and when to collection are used: point-sampling and composite-
collect samples. The sampling decision tree presented sampling:
in Fig 02.01-A1 illustrates a decision process to assist 9.3.1 point sampling—site-specific sample collection
in the development of proper sample collection from within the general mass is used to identify and
methods, to identify sampling interval and sample size, quantify points of extreme variability, hot spots or
and the end use of sample data. When regulations do problem zones. Point-sampling alone should not be
not apply, as is the case for recipe formulation, process used unless special conditions exist.
monitoring for quality assurance (QA) and internal
quality control (QC), it is important to clearly 9.3.2 composite-sampling—a single sample for
understand the intended use of the data and to laboratory analysis composed of multiple, well-blended
determine the appropriate sampling procedures. For point- or sub-samples uniformly distributed throughout
example, if C:N ratio interpretation is considered very the entire volume that, after mixing, accurately
important, then very low variations in sample carbon represents an average or median value of the property
and nitrogen determinations become a major or trait of interest for a batch or general mass. Properly
implemented composite sampling is preferable for most
sampling plans because it provides a reliable estimate

Test Methods for the Examination of Composting and Compost August 27, 2001
02.01-7
Sample Collection and Laboratory Preparation
Field Sampling of Compost Materials 02.01

of the average or median property or trait of a batch or 9.5 Importance of Representative Sampling—A
segment of a continuous stream, rather than a specific representative sample defines a material’s average
spot trait. characteristic, typical for the entire material being
9.3.2.1 stratified sampling—a modified composite sampled. Under virtually all composting conditions,
sampling scheme is used to document gradients and the mass of compost material is large and
define heterogeneity as a function of position within the heterogeneous. A representative sample of compost is
bulk or general mass of sampled material, where the not easily obtained; and sampling must be repeated
general mass is subdivided into separate zones and a over time to compensate for naturally high variations.
series of point-samples are collected and composited Under proper management and as compost-curing
within each zone. Stratified sampling should be used advances, variability within a curing pile or windrow
when heterogeneity of compost is unknown and when will decrease.
regulatory constraints require knowledge of the relative
spatial and temporal variability. This is most often Field Sampling Methods Samples for Lab Lab Results
based upon the standard deviation and mean; refer to
Method 02.01-B for equations applied in calculations 1 1

for approximating the required number of sub-samples A 1 1


a1
Xa1
Stratified
to accurately estimate the average value for the Sampling 2
2
Xa2
a2
parameter or trait of interest. 2
3
2

9.3.2.2 interval sampling—sampling from moving 3 a3


Xa3
3

conveyor belts.
9.4 Sampling Plan—The constraints of the material
and the composting technology must be considered B Xb1
Composite
when an optimal sampling plan is designed. Sampling 1
b1
Combinations of composite and point sampling are 2
illustrated within the four sampling schemes presented 3
in Fig 02.01-A2. The sampling scheme selected must
address limitations of the selected test parameter and
should not distort the analytical result.
C
9.4.1 Stratified sampling (Scenario A, Fig 02.01-A2) Entire Area, Xc1
is used to determine variability, profile gradients and or Batch
Sampling c1
spatial uniformity characteristics. In most cases,
composite sampling (Scenario B, Fig 02.01-A2) is
satisfactory when the amount of variability within the
mass is known to be insignificant. It involves
combining several representative sub-samples into one D
composite sample that is then thoroughly mixed, then Single Grab
Sampling Xd1
split for shipment to the laboratory. Area or batch
1 d1
sampling (Scenario C, Fig 02.01-A2) and single grab-
or point-sampling (Scenario D, Fig 02.01-A2) are for X

special cases where one sample is collected at one Fig 02.01-A2 The sampling schematic.
location. Area or batch sampling is typified by a whole
mass collected as one sample unit. This method is most 9.6 Variables that Compromise Quality of
appropriate when moving the mass from a vessel to a Sampling—Sample collection technique and variability
curing pile. A single point-sample does not provide a of compost and cured compost affect the relative
representative sample for the bulk mass. Batch accuracy of sampling and the reliability of laboratory
sampling and point sampling should be employed to analytical determinations. Failure to adjust sampling
characterize an obvious or potential anomaly at one protocols according to the nature and source of
specific point, time or location within a process. A variations may invalidate test results and lead to
good example of a single point sample to detect inappropriate management or marketing decisions.
anomalies is shown as X in Fig. 02.01-A2 D, a location 9.6.1 Bias Introduced by the Sampler—Inaccurate
referred to as the “toe” of a static aerated pile, and one sample collection is often due to systematic or
which is vulnerable to suboptimal temperatures needed intentionally selective sampling introduced by the
to achieve pathogen reduction. For this reason, it is sampler. Significant error will result from attempts by
sometimes specifically included to verify pathogen the sample collector to counteract perceived variability.
content of compost that has finished the thermophilic Examples include avoiding the collection of sub-
phase.

August 27, 2001 Test Methods for the Examination of Composting and Compost
02.01-8
Sample Collection and Laboratory Preparation
02.01 Field Sampling of Compost Materials

samples from wet pockets or systematically excluding The error introduced to C:N values for samples of this
large particles from the composite sample. Deliberate range is significant.
bias results from an attempt by the sampler to 9.6.2.6 Layering, compaction and gradients of
prepare samples that appear superior in a perceived composts arise as a result of inadequate initial mixing,
physical trait that does not actually represent the infrequent or excessive turning/mixing during feedstock
bulk or batch of interest. preparation, or during the composting process because
9.6.2 Sample Heterogeneity—The following are key of equipment/ventilation actions such as inappropriate
sources of non-uniformity that can give rise to selection and use of bulking materials. Any one or
significant sampling errors. more of these can easily confound sampling attempts.
9.6.2.1 Sub-sample size affects sampling accuracy. 9.7 Sampling Practice—Sampling begins with the
In general, a representative composite sample contains decision to evaluate materials and proceeds to
large (> 1000 cm3) and plentiful sub-samples (>15 determining how and in what time frame the sample is
samples). needed. Practical steps include identifying the
9.6.2.2 Complete and thorough mixing throughout important parameters to be analyzed and working
the composting process improves the quality and ease backwards through the decision tree to identify how to
of sampling. Poor initial mixing effects variability of obtain a suitable sample for the specific technology and
the parameters throughout the composting process. parameter of interest. Following this process, a
Repeated use of turning machinery during composting sampling protocol and sample log is constructed.
improves homogeneity. However, within days or even Technological constraints sometimes present significant
hours after turning, mixing or re-piling, the composting challenges for sampling, however, in most cases,
mass may develop gradients of stability, moisture, reliable samples can be obtained once a thorough
bacteria and ammonia. When pre-mixing, blending or analysis of the process plan is conducted.
turning are not employed, as in static pile composting 9.8 Composting Technology Systems and Sample
or compost curing, the sampling plan should include Collection—The physical/mechanical nature of the
more sub-samples per composite sample to compensate feedstock preparation and composting operation may
for inherently high variability within the mass. impose constraints on sampling. Each composting
9.6.2.3 Soil and stones are frequently picked up technology imposes specific limitations on sampling.
during routine compost production operations. These Representative samples may not be obtainable with
pose problems for good sampling. In some cases, the some technologies. Therefore, a facility's sampling
sampler may bias the sample by deliberately excluding plan must take into account the realistic strategy for
gravel and stones present in a compost (soil can not be obtaining representative samples. In general, highly
easily seen). On the other hand, a laboratory that engineered compost processes impose more constraints
receives a sample containing stones or small gravel on sampling than a simple composting process. For
may not sub-sample, pre-screen, and grind, resulting in example, outdoor windrows are more easily sampled
variable results. Staff responsible for sampling must than large rotating drums.
correctly diagnose the situation and advise the 9.8.1 Ten basic types of composting systems are
analytical laboratory about it. In some cases, presented in Fig 02.01-A3 and their associated
laboratories must issue disclaimers about their own sampling constraints are outlined in Table 02.01-A1.
sub-sampling technique. Each system introduces particular traits or constraints
9.6.2.4 Foreign and non-compostable matter almost that impact how (and why) samples are collected. New
invariability poses problems to the sampler, and also forms of compost technology under development may
the laboratory. This is most likely the case with expand the list, but the generic form of the prescribed
municipal solid waste (MSW) and certain industrial by- models cover most existing composting technologies.
products where large and variable amounts of such 9.8.2 Sampling Plan Basics—The two process-
substances are present. The best approach is to take focused modes of compost sampling are: i) In-Process
large sub-samples and blend frequently before sampling for monitoring during a specific composting
removing the final sub-sample for examination or technology process; and ii) End-Process sampling.
testing. There is presently no generally accepted or There may be multiple steps or multiple processes
standard practice for gauging the minimum sample size involved in an overall system. Sample collection for
required in such situations. testing commonly occurs at the end of a specific step of
9.6.2.5 Varying particle size is one of the most the composting process, mostly for convenience and to
common sources of sample variability. For example, a be certain that the sample is representative of the batch.
composting feedstock mix may have exactly 27% wood Sample collection during a process imposes significant
chips, but inability to sub-sample adequately could constraints because of the inherent variability of in-
result in finding anywhere from 11 to 38% wood chips. process materials. Sampling at these points must be

Test Methods for the Examination of Composting and Compost August 27, 2001
02.01-9
Sample Collection and Laboratory Preparation
Field Sampling of Compost Materials 02.01

carefully designed to sample across any existing 9.8.3.4 Type D. Agitated-Bed systems generally
gradient of non-uniformity. move compost along the length of the system at a fixed
9.8.3 Discussion in the following section identifies rate per day. Should sampling be necessary during the
technologies and primary constraints or requirements process, care must be taken to understand the
for representative sampling. variability imposed by nature of daily additions to the
system. In some cases, the actual technology physically
9.8.3.1 Type A. Home Bins come in many shapes
restricts access for various reasons including worker
and sizes, from fixed solid containers, loose wooden
safety. In such situations, samples can be collected at
structures to rotating solid-tanks. The appropriate
the discharge end where material comes off the bin.
framework for sampling is to select the material
Several sub-samples should be taken each day, cooled
representing the finished product. Some systems
immediately; and several days’ accumulated samples
provide doors at the bottom of a bin from which
(except for bacteriological and others parameters
samples may be easily removed; other bins require
limited by a 48 h holding time) can be composited to
disassembling or removal from the pile and hand-
form a bulk sample.
mixing of the mass. Precaution must be taken to assure
a homogenous mixture under any circumstance. 9.8.3.5 Type E. Enclosed Vessel reactors are either
NOTE 7—The inclusion of home composting bins in TMECC is
circular or oblong containers, bins or towers (these
not a suggestion or endorsement for regulatory control, but for systems may or may not contain internal moving parts)
information and perspective only. While home composting bins and cannot be easily accessed for sampling. Sample
are not a mainstay of commercial composting and not currently collection is best performed at the vessel’s discharge
or likely to be regulated by state or local jurisdictions when the
end product is used by the home generator and producer, the
end. In-process sampling for quality control and
principles described in TMECC for assessing overall quality of process monitoring is not always practical with these
compost are suitable for use on such products. systems.
9.8.3.2 Type B. Turned Windrows are either batch 9.8.3.6 Type F. Rotating Vessels are horizontal
or continuous piles. In the former common case, the tanks, usually positioned on a gradient. They are used
entire windrow is made from similar ingredients at for continuous and sometimes for batch composting.
about the same time (e.g., within 3 d). In the latter Most systems do not have ports to access the material
case, materials are added lengthwise over time. In both during processing, making in-process sampling
cases, non-uniformity is observed down the length of impractical. As with the enclosed vessel design,
the pile and is greatest with continuous modes of sampling is usually performed at the discharge end of
composting. Sampling of windrows requires the vessel. Rotating vessels are often used during
compositing over a discrete length, either the entire “Feedstock Preparation” for many technology types,
pile, or a sub-section identified to have similar age or and sampling is performed on the download conveyor.
other characteristics. Windrow turning machines are 9.8.3.7 Type G. Cure Piles are frequently very large
useful for preparing uniform mixtures suitable for and may contain material composited from several
composite sampling; however, a single pass with a piles. Because of their heterogeneity and size, and the
turning machine will not result in an evenly mixed pile, typical lack of turning and mixing, they usually display
3-4 passes commonly are required. If turning is extreme gradients of moisture, maturity and bulk
performed frequently, the need for multiple turns prior density. Under these circumstances, one effective way
to sampling diminishes. to adequately sample is to use a large tractor loader to
9.8.3.3 Type C. Static Piles are recognized for their break into the pile, moving and mixing the materials in
non-uniformity. These piles exhibit gradients of the process. The sampling plan must incorporate a
temperature, aeration and exposure to elements that stratified sampling scheme and point sampling to
reduce homogeneity over time. To obtain a distinguish gradients and map spatial non-uniformity.
representative sample from a static pile, extreme 9.8.3.8 Type H. Bagged Product results from a
disruption and mixing is required. Breaking down the mixing and screening process that is assumed to
pile with a bucket loader and re-mixing after removal produce uniform material prior to bagging. Additional
of the outer cover may be necessary. If mixing is not mixing of the bulk mass after bagging and prior to
complete, sub-samples should be taken from each sampling is precluded. Therefore, a statistically
region during pile breakdown, or from the bucket as representative sample must consist of many sub-
material is removed. However, if the purpose of samples collected from different bags. Additionally,
sampling is to characterize non-uniformity, then effort the physical constraint of extracting small sample cores
must be made to get to the region of concern where a from separate bags that are palletized compounds the
representative sample can be collected. This could be problems of collecting proper samples.
performed using a core sampler, or by breaking open
the pile with heavy equipment. 9.8.3.9 Type I. Source Ingredients are notorious for
non-uniformity. Large sub-samples that accurately

August 27, 2001 Test Methods for the Examination of Composting and Compost
02.01-10
Sample Collection and Laboratory Preparation
02.01 Field Sampling of Compost Materials

represent the distribution of ingredients must be well more obvious. In general, these units contain highly
mixed, and if possible (when appropriate), shredded to uniform materials and are sometimes so small that the
reduce the sample size while retaining sample integrity. entire unit becomes the sample from which sub-samples
Large mechanical equipment may improve the sample are drawn for separate analyses. Because non-
collection and preparation process. uniformity increases with miniaturization, lab systems
9.8.3.10 Type J. Lab Systems are a special case of are usually designed with small openings into discrete
composting and are usually handled as a discrete sections of tanks to facilitate extraction of small sub-
sampling problem on an individual institutional basis. samples. This allows the operator to monitor the
However, with the increasing popularity of bench scale formation of gradients and non-uniformity in miniature
testing, particularly for bioremediation composting, the lab systems.
value of describing sample units and types becomes
Table 02.01-A1 Sampling operations, constraints and required tools for ten types of composting technologies.
Type Sampling Action Constraints Preferred Tools
A. Home Bins Must open bin, remove cover and sides, Not homogenous, may be hard or Pail and spading fork
and mix by hand impossible to open
B. Turned Windrows Sample after turning with machine from Pile varies along length, turning machine 5-gal pail, spading shovel,
surface of pile if well mixed may not homogenize in one pass corer
C. Static Piles Remove chip cover, and dig into depth, Extreme non-uniformity, layering and 5-gal pail, spading shovel,
may require bucket loader and multiple clumping, inadvertent mixing with cover corer or auger, bucket loader
depth sampling or surface residues; may be sealed inside
tube
D. Agitated-Bed Sample after turning or agitation event, Difficult access except at discharge, piles 5-gal pail, spading shovel,
or sample discharge vary along length with age of source
E. Enclosed Vessel Sample from side doors or top port after Very difficult or impossible access; 5-gal pail, spading shovel,
agitation potential layering corer, auger
F. Rotating Vessels Sample from discharge/output end or Difficult or impossible to sample except 5-gal pail, shovel or scoop
take-away conveyor at discharge; output varies with time
G. Compost Curing Remove chip cover, and dig into depth, Very large piles, non-uniformity, 5-gal pail, spading shovel,
Piles may require bucket loader and multiple difficult access, compaction and corer, auger, bucket loader
depth sampling layering; surface cover mixing
H. Bagged Product Sample multiple bags, cores drawn Bag damage, difficult access 5-gal pail, trowel or soil-corer
I. Source Composite from each pile separately, Non-uniformity may be great, poorly Large pail, shovel; bucket
Ingredients remove surface mixed, difficult access loader
J. Lab Systems Open system and remove with core Small scale, difficult access 5-gal pail, Spatula, trowel,
sampler soil-corer

9.9 Sampling Interval—There are no process-specific 9.9.2 Weight Reduction Factor, R:


formulas that dictate sampling intervals for source R= C÷F Equation 9.9.2
ingredients and compost, except when biosolids are where:
composted (Table 02.01-A2). Sampling intervals of R= weight reduction factor of incoming feedstock, %,
composting materials for reporting purposes may be C= mass of finished compost per week, t dw, and
fixed by certain regulations. It is advisable to consult
F= mass of incoming feedstock per week, t dw
local or state sampling guidelines. As a general rule,
NOTE 1A—If the actual weight reduction factor is unknown,
incoming feedstocks should be sampled every two use 0.70 until the actual value can be determined. Refer to
weeks, or every 3,000 to 5,000 tons of finished product. Method 03.09 Total Solids and Moisture for a description of
9.9.1 Formula to estimate sampling interval, d: how to determine dry weight of compost and feedstocks.

S= T÷F×R Equation 9.9.1 Table 02.01-A2 Sampling intervals for composted biosolids.
where: Amount produced
S= sampling interval in days, d (metric tons of biosolids Monitoring Frequency for
T= sampling threshold in tons (e.g., 4,000 t), t, compost per 365-day period) Pathogens and Trace Elements
F= tons of incoming feedstock per day, t d-1, and < 290 Once per year (1 yr-1)
R= weight reduction factor of incoming feedstock, %. ! 290 to < 1,500 One per quarter (4 times yr-1)
! 1,500 to < 15,000 Once per 60 days (6 times yr-1)
! 15,000 Once per month (12 times yr-1)
Adapted from US EPA 40CFR503

Test Methods for the Examination of Composting and Compost August 27, 2001
02.01-11
Sample Collection and Laboratory Preparation
Field Sampling of Compost Materials 02.01

9.9.3 Sampling raw source ingredients—Example 1.


Samples shall be taken from incoming material that has
been shredded, tumbled or otherwise reduced in
particle size. From the material exiting the
shredder/mixer, one point-sample shall be obtained
every 2 h, over an operational period of 6-8 h, for a A. Home Bin B. Turned Windrow
total of 4 samples. Sample size should be C. Static Pile
approximately 1000 cm3 (~ 1 qt) per sample. The four
samples shall then be thoroughly mixed together
(composite), and a portion of the mixture (composite
sub-sample) taken for analysis. If point-sampling
directly from the shredder or mixing mill is not
possible, the incoming material shall be sampled no D. Agitated Bin
E. Enclosed Vessel
more than 24 h after passing through the shredding
equipment.
9.9.4 Example 2—Sampling compost materials. For
each sampling event, a single composite sample shall F. Rotating Vessel
be made up of multiple sub-samples for each pile or
batch, unless otherwise directed. G. Curing Pile

H. Bagged Product
9.9.5 Example 3—Sample locations. Construct and
label a diagram of sample locations for your
composting system. The example provided in TMECC
02.01-B indicates a minimum of fifteen sub-samples
per pile. This procedure establishes a composite or I. Fresh Debris

general characterization of the attributes in a compost J. Other

pile.
Fig 02.01-A3 Composting technologies.
9.9.5.1 Refer to section 02.01-B for a strategy to
sample generic windrows of compost. 9.9.6 Example 4—Sample Variance Exercise. The
9.9.5.2 Samples collected during the composting coefficient of variation (CV) expresses the relative
process are not composited in the same manner as variability for a parameter of interest across multiple
finished samples because point-specific problems must samples. The CV is expressed as a percentage and
be identified and monitored. Factors such as anaerobic calculated by dividing the sample standard deviation by
materials and volatile fatty acids (VFA) may need to be the sample mean and multiplied by 100.
determined from point-samples extracted from multiple 9.9.6.1 The ability to distinguish differences
locations in the same pile. between arithmetically similar sample values decreases
as the CV increases. It is difficult to draw specific
conclusions about analytical results when variability is
high. Under circumstances where variability is
consistently high either the sampling plan must be
redesigned to account for the excessively high
variability, or the parameter should be discarded as a
standard measure.
9.9.6.2 Consider a hypothetical case where two
standard parameters are used to evaluate compost
stability, C:N and VFA. Assume that the upper limit of
acceptable variability for the parameters are set at 15%
for C:N, and 45% for VFA. Low CV thresholds are
generally assigned to system and process critical
measures, and high CV thresholds are assigned to less
critical standard measures.
NOTE 2A—This is a hypothetical case. It may be very difficult
to establish meaningful CV limits without a large amount of
data from many composts across time for a given test
parameter. In addition, depending on the test, an individual test
parameter may show a very large CV for repeated analysis of
one sample.

August 27, 2001 Test Methods for the Examination of Composting and Compost
02.01-12
Sample Collection and Laboratory Preparation
02.01 Field Sampling of Compost Materials

9.9.6.3 In the example given in Table 02.01-A2, the 9.10.4 Trier,


CV for VFA testing is greater than the CV for C:N 9.10.5 Pipe—PVC or plastic,
analysis, but the latter is unacceptable, given the use of
the data, whereas the former is acceptable. In this 9.10.6 Tarpaulin—plastic,
hypothetical case, large variations across VFA samples 9.10.7 Pail—16- to 20-L (4- to 5-gal), square pails.
are less significant than smaller variations associated Use standard 5-gal plastic pails only when square pails
with C:N. This is because variations in VFA's are are not available (e.g., square pails are available through
transient and either readily corrected or do not diminish Cleveland Bottle & Supply Co.; 850 East 77th Street; Cleveland, OH
compost quality relative to its intended use, whereas 44103; telephone: 216 881 3330; FAX: 216 881 7325; URL:
highly variable C:N ratios indicate potentially serious http://www.clevelandbottle.com/squrpail.html). Pails must be
problems with the composting process and product cleaned well with soapy water, rinsed, and dried
quality. between samples.
9.10.8 Trowel—Standard garden, high-density
Table 02.01-A3 Compost sample data analyzed for variability
polypropylene (HDPP) for sub-sample mixing and bag-
Sample C:N Ratio VFA mg kg-1 filling; trowels must be cleaned well with soapy water,
1 35 12,000 rinsed, and dried between samples.
2 19 18,000
9.10.9 Sample Containers—Use a container that is
3 39 19,000
appropriate for the laboratory analysis to be performed
4 22 25,000
on the collected compost sample. Refer to Tables
5 42 9,000
02.01-2 through 02.01-6, and Figure 02.01-B3.
Average: 31.4 16,600
Standard Deviation: 10.3 6,268 9.10.10 Labels and Logbook
%CV: 33 38 9.10.10.1 Labels—Name of technician, operator,
Acceptable CV: 15% 45% inspector, facility name, pile identification, date, time,
Suitability of Data: REJECT ACCEPT sample number and location in pile using length, width
and height coordinates from an identified end and depth
9.10 Sampler Devices—There is no single from surface measured perpendicular to surface,
standardized compost sampling device. Tools and purpose of sample/test, method of sample preservation.
devices for soil and forage sampling are relatively 9.10.10.2 Logbook—Name of technician, operator,
simple and efficient and are useful for compost or inspector; and facility name. Pile data including:
sampling, but they have severe limitations. pile identification; feedstock-mix; type of pile; date
9.10.1 Slotted Tube Sampler—Single or double, started; weather conditions at time of sampling (for
slotted tube and rod, all slotted ends and a minimum 5- exposed piles only); pile orientation relative to natural
cm (2-in.) diameter. The Pennsylvania State Forage drainage. Sample data including: date and time of
Sampler, or equivalent, is a satisfactory core sampler sample collection; location where samples were
for composts that do not contain significant foreign collected in pile using length, width and height
objects. coordinates from an identified end and depth from
surface measured horizontally; description of the
9.10.2 Shovel—Standard long, handled, pointed tip;
sampling point; purpose of sample/test, method of
typical horticultural narrow shovel, cleaned well with
sample preservation, point or composite sample;
soapy water, rinsed, and dried between samples.
number and volume of the samples taken; date and time
9.10.3 Thief Sampler, samples were shipped.

Test Methods for the Examination of Composting and Compost August 27, 2001
02.01-13
Sample Collection and Laboratory Preparation
Field Sampling of Compost Materials 02.01

Test Method: Selection of Sampling Locations for Windrows and Piles Units: NA
Test Method Applications
Process Management Product Attributes
Step 1: Step 2: Step 3: Step 4: Step 5: Step 6: Step 7: Safety Market
Feedstock Feedstock Composting Odor Treatment Compost Curing Compost Compost Standards Attributes
Recovery Preparation Screening and Storing and
Refining Packaging
02.01-B 02.01-B 02.01-B 02.01-B 02.01-B 02.01-B 02.01-B

02.01-B SELECTION OF SAMPLING LOCATIONS FOR WINDROWS AND PILES

1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20

Fig 02.01-B1 Hypothetical sample collection pattern from a compost windrow.

NOTE 1B—In this example, a scale from 1-20 is superimposed 11.2 Plastic Gloves.
on the long dimension of a compost windrow. Five distances
(3, 6, 10, 13 and 18 m) are randomly selected to each side of 11.3 Tarp—clean plastic, canvas, or other type of
the windrow, (e.g., numbers randomly pulled from a hat), to mixing surface if feedstock is liquid sludge.
assign sample collection locations. Point-samples are collected
from within three zones at each cutout. 11.4 Cold Packs—chemical ice packs, or 4-L plastic
NOTE 2B—The illustrated cut-outs are depicted on one side of bags (e.g., heavy duty Ziploc® freezer bags) filled with
the windrow; in a real operation, the cut-outs must be randomly approximately 0.5 L of water and frozen flat. One ice
assigned to each side of the windrow. Cone-shaped piles have pack per 4-L sample container of compost to be
a circular base. Measure around the base of a cone-shaped pile shipped, (e.g., three ice packs are recommended for
and randomly assign cutout positions along the pile’s meridian,
or circumference.
three compost 4-L samples).
11.5 Aluminum Foil—lining for plastic shipping pail,
10. Apparatus for Method B
and
10.1 Sampling Container—five 16- to 20-L (4- to 5-
11.6 Packing Material—newspaper or other
gal), plastic (HDPP), glass.
appropriate bulking material to be used as packing or
10.1.1 Organic Contaminant Tests—For samples to fill to minimize sample movement within the shipping
be analyzed for the presence of organic contaminants, container (square pail) during shipping.
please refer to Table 02.01-6 Organic Contaminant
11.7 Adhesive Tape—duct tape, 5-cm (2-in.) width.
Tests: Sampling containers and conditions for compost
and source ingredient testing. Modify sample 12. Procedures for Method B
packaging steps presented in this section accordingly. 12.1 Cut into Finished Compost—Using tractor skid-
10.2 Sampling Device—silage auger, tilling spade, or loader, bobcat or shovel, or sample boring device, cut
other appropriate sampling device. into the finished compost pile or windrow at five or
10.3 Tractor Loader—with loader, (e.g., Bobcat, more randomly selected positions. Collect samples
etc.). from the full profile and breadth of the compost
windrow or pile. Refer to Fig 02.01-B1.
10.4 Trowel—high-density polypropylene (HDPP),
for stirring and mixing composite sample. 12.2 Collect Point-Samples—Samples of equal
volume are extracted from the compost pile at three
10.5 Pail—16- to 20-L (4- to 5-gal), square pails, Use depths or zones measured from the pile's uppermost
standard 5-gal plastic pails for shipping only when surface. Collect no less than five point-samples from
square pails are not available (e.g., square pails are available each of the three depths or zones illustrated in Fig
through Cleveland Bottle & Supply Co.; 850 East 77th Street;
Cleveland, OH 44103; telephone: 216 881 3330; Fax: 216 881 7325;
02.01-B2. The five point samples for each zone must
URL: http://www.clevelandbottle.com/squrpail.html). be collected in a manner to accurately represent the
horizontal cross-section of the windrow or pile. Use a
11. Reagents and Materials for Method B sanitized sampling tool (a gloved hand, clean shovel or
11.1 Plastic Bags—three 4-L (1 gal) durable bags auger) when collecting samples and when transferring
with seal, (e.g., Ziploc® Freezer bags). samples to the 5-gal sample collection pail.

August 27, 2001 Test Methods for the Examination of Composting and Compost
02.01-14
Sample Collection and Laboratory Preparation
02.01 Field Sampling of Compost Materials

monitoring for the presence of gradients along the


longer dimension of a windrow. Pack and prepare five
1
separate samples (i.e., five separate composite samples,
one from each cutout) for shipment as described in step
2 12.5.
3 12.4.2 Stratified Samples within Cutouts—Use this
sampling strategy to evaluate for the presence of spatial
Fig 02.01-B2 Five horizontally dispersed point-samples are
variations or gradients that occur with changes in pile
collected from each of three depths or zones within each cutout. depth or distance from the windrow core to its surface.
NOTE 3B—(1) upper 1/3 of compost profile height; (2) middle 12.5 Prepare for Shipment and Storage:
1
/3 of compost profile height; and (3) lower 1/3 of compost 12.5.1 Transfer the blended compost to three 4-L (1-
profile height, where compost pile does not exceed the
recommended overall height of 3 m. Create more than three
gal) sample bags, (e.g., plastic Ziploc® freezer bags).
sampling depths or zones within each cutout when the curing 12.5.2 Line the shipment pail with aluminum foil or
pile exceeds a height of 3 m, relative variability is high or the other reflective material to minimize sample heat-gain.
property of interest is found at very low concentrations, near the
laboratory detection limit. Place the sample bags containing the compost sample
into the plastic pail and interleave with ice packs for
12.3 Composite Point-Samples—Place all 15 point shipping (refer to Fig 02.01-B3).
samples from one cutout together into one sanitized
plastic pail. Completely mix the point samples by 12.5.3 Cover the pail with its lid. Seal and secure the
stirring thoroughly with a sanitized wooden stick or lid with a packing tape. Send the sample pail by one-
lath, and by covering and shaking the pail to further day express delivery service to your selected laboratory
mix the samples. for analysis. Include a chain of custody information
sheet with environmental regulatory samples (Refer to
12.3.1 Repeat the blending process at least four times Method 02.01-E).
until all point samples are thoroughly blended to form
NOTE 3B—Maintain cool samples at 4°C (39.2°F) to diminish
one composite sample that accurately represents the microbial and chemical activity prior to and during sample
compost for the cutout. shipment.
12.3.2 Proceed to the next compost sample cutout
and repeat this process to collect one thoroughly Foil lined plastic pail lid
blended composite sample from each of the five
cutouts.
12.3.3 Composite Sample—Transfer the five
composite samples from the sample collection pails
onto a mixing tarp or other appropriately sanitized Sample
Three 4-L sample containers
surface or container, such as into a large pail where all
samples can be mixed, blended and then covered to Ice Pack
minimize moisture loss. Thoroughly blend the five Two 4-L ice packs
composite samples to form one large sample that Sample
represents the average condition of the entire batch or
windrow in question. Ice Pack
12.3.3.1 Quarter the composite sample and
thoroughly mix and quarter again. Continue to Sample
subdivide and split the sample into quarters and mix as
described until sample size reaches approximately 12 L
(3 gal).
12.4 Stratified Sampling—This sample collection
strategy is used to evaluate for the presence of spatial Foil lined shipping pail
variations or gradients in compost characteristics across
and through a windrow or pile.
12.4.1 Stratified Samples across Cutouts—Use this
sampling strategy to test for differences in compost
characteristics between sample cutouts and along the
longer dimension of a windrow. Do not composite Fig 02.01-B3 Preparation for shipment.
materials from the five separate cutouts when

Test Methods for the Examination of Composting and Compost August 27, 2001
02.01-15
Sample Collection and Laboratory Preparation
Field Sampling of Compost Materials 02.01

Test Method: Field Sampling Plan for Composted Material Units: NA


Test Method Applications
Process Management Product Attributes
Step 1: Step 2: Step 3: Step 4: Step 5: Step 6: Step 7: Safety Market
Feedstock Feedstock Composting Odor Treatment Compost Curing Compost Compost Standards Attributes
Recovery Preparation Screening and Storing and
Refining Packaging
02.01-C 02.01-C 02.01-C 02.01-C 02.01-C 02.01-C 02.01-C 02.01-C 02.01-C

02.01-C FIELD SAMPLING PLAN FOR COMPOSTED MATERIAL


13. US EPA SW-846 Guideline Review and Sampling Plan Considerations. The sampling plan is
Considerations usually a written document that describes the
objectives, and details the individual tasks and how
13.1 With its hazardous waste management system, they will be performed. The more detailed the
the US EPA requires that certain solid wastes be sampling plan, the less opportunity for oversight or
analyzed for physical and chemical properties. In its misunderstanding during sampling, analysis, and data
hazardous waste management system, it is mostly management.
chemical properties that are of concern, and in the case
of a number of chemical components, the US EPA has 13.3.1 The SW-846 document suggests that a
promulgated levels (regulatory thresholds) that cannot sampling plan be designed with input from the various
be equaled or exceeded. sectors involved in the project, including the following
personnel:
13.1.1 Regulations pertaining to the management of
hazardous waste contain three references regarding the 13.3.1.1 regulatory sampling—in many cases may
sampling of solid wastes for analytical purposes: require state permits and consultations with state
officials.
13.1.1.1 Collect representative samples of waste, so
that they exhibit average properties of the bulk compost 13.3.1.2 end-user—to use the data to attain program
or feedstock. objectives.
13.1.1.2 Collect enough samples (but no less than 13.3.1.3 field team member—an experienced
four samples) over a period of time sufficient to member of the field team who actually collects
represent the variability of the compost or feedstock. samples.
13.2 Sampling Plan Implementation—The US EPA 13.3.1.4 analytical chemist—to review analytical
manual contains a section on implementation of the requirements for sampling, preservation, and holding
sampling plan (SW-846 Chapter Nine, part 2). Within times that will be included in the sampling plan.
that section there is discussion concerning the sampling 13.3.1.5 process engineer or equivalent—it explain
program's objectives for evaluating a compost. (Refer details and constraints of the production process being
to Fig 03.01 Sample fate). sampled.
13.2.1 The example suggests the following questions 13.3.1.6 statistician—to review the sampling
be answered: approach and verify that the resulting data will be
13.2.1.1 Is the sampling being performed to comply suitable for any required statistical calculations for
with environmental regulation? decisions.
13.2.1.2 Samples are to be analyzed for which 13.3.2 quality assurance representative—to review
parameters? the applicability of standard operating procedures and
determine the number of blanks, duplicates, spike
13.2.1.3 Why not others? samples, and other steps required to document the
13.2.1.4 Should samples be analyzed for fewer accuracy and precision of the resulting data.
parameters? 13.3.3 If no one is familiar with the site to be
13.2.1.5 What is the end-use of the generated data? sampled, then a pre-sampling site visit should be
13.2.1.6 What are the required degrees of accuracy arranged to acquire site-specific information. Some
and precision? modifications of the sampling plan may be necessary.
It is necessary to have at least one experienced sampler
13.2.2 These questions may or may not be as as a member of a sampling team.
important for sampling composted solid waste.
14. Statistical Validity of Sampling Plan
13.3 Sampling Plan Considerations—The
implementation section contains a category entitled 14.1 Objectives—The primary objective of a
sampling plan for a compost is to collect an appropriate

August 27, 2001 Test Methods for the Examination of Composting and Compost
02.01-16
Sample Collection and Laboratory Preparation
02.01 Field Sampling of Compost Materials

number of representative samples and subsamples for microbiological analysis. Chemical quality changes
accurate and precise measurement of the chemical, that may take place due to microbiological activity
physical and biological properties of the compost. If between sample collection and laboratory analysis
the chemical measurements are sufficiently accurate should be avoided.
and precise, they will be considered reliable estimates 14.3.4 Chain of custody forms and procedures should
of the chemical properties of the compost. be used with all environmental samples.
14.1.1 Generally, high degrees of accuracy and 14.4 Other Sampling Considerations—Compost
precision are required if one or more chemical samples are taken at each facility for a variety of
components of compost are present at a concentration purposes. Varying levels of expertise and quality
that is close to the applicable regulatory threshold. assurance are required depending on the sampling
Alternatively, relatively low accuracy and low precision purpose or objective. A unique sampling protocol
can be tolerated if the components of concern occur at should be developed for each specific objective. This
levels far below or far above their applicable information should be detailed in a facility operation
thresholds. Low sampling precision is often associated and maintenance (O&M) manual and be accessible to
with considerable savings in analytical costs, as well as all facility staff.
expenses associated with sampling; and is clearly
recognizable even in the simplest of statistical tests. 14.4.1 Key process variables including porosity,
However, low sampling accuracy may not entail cost nutrient balance, oxygen, moisture, temperature and
savings and is always obscured in statistical tests (i.e., it time are monitored and controlled on a continual or
cannot be evaluated). Although it is often desirable to daily basis. Measurements of weight and volume of
design sampling plans for compost to achieve only the waste arriving and compost leaving the facility are
minimally required precision (at least two samples are necessary for planning material movements, personnel
required for any estimate of precision), it is prudent to and transportation requirements, and maintaining
design the plans to attain the greatest possible accuracy. facility aesthetics. Although this is the most frequent
type of sampling conducted, the sampling quality
14.2 Composite Sampling—For composite sampling, assurance requirements are the least significant for
a number of random subsamples are initially collected these activities. Generally, process control and
and combined into a single sample, which is analyzed material handling data do not need to be precise to be
for the chemical constituents of concern. The major useful, (e.g., appropriate application of quick-tests).
disadvantage of composite sampling, as compared with Regulatory compliance and product attribute data must
non-composite sampling, is loss of information about be highly precise and accurate, (e.g., statistically valid
the spatial variability of chemical constituents because sampling program to accurately estimate the average
only a single estimate of the parameter is generated. value of interest).
The benefit is that a credible, general representation of
the entire compost pile is generated from a large 14.5 Sampling Frequency—Operating permits for
number of subsamples which are composited. compost sites require that concentrations of certain
constituents of environmental concern be evaluated,
14.3 Sampling Quality Assurance/Quality Control (e.g., As, Ba, Cd, Cu, Cr, Hg, Mn, Mo, Ni, Pb, Se, Zn,
(QA/QC): pathogens such as Salmonella and fecal coliform, and
14.3.1 Make sure all sampling equipment and organic compounds such as PCB's, PCP's, dioxins,
containers are clean. If equipment is used to collect furans, organochlorine and organophosphorus
multiple samples, provisions for cleaning and pesticides). Regulatory agencies establish compliance
decontamination are required between samples. using individual sample results. It is, therefore, very
14.3.2 Properly label all samples and keep accurate important that sample collection and preparation
records. Record as much information on sample labels techniques provide representative samples.
as possible prior to arriving at the site. Sample labels NOTE 1C—As much as 20,000 m3 of compost may be
and field notes should include material type, location, represented by one subsample as small as 1 g. Because of this,
it is vital that the sample be representative of the total material.
date, approximate age of compost, sampler's name, Quality control and quality assurance for quarterly testing
special sampling procedures used, analytical must be greater than that employed for routine daily
procedures to be performed, preservatives added (if monitoring.
any), and any special observations or incidents during 14.6 Statistical Techniques—Statistical techniques for
the sampling event. obtaining accurate and precise samples are relatively
14.3.3 Point-samples must be stored in a refrigerator simple and easy to implement. Accurate
(4oC) before analysis when delays in shipment to representations of an entire compost pile or batch may
laboratory are anticipated. This preservation is be achieved through random sampling. In random
especially important for feed stock samples, compost to sampling, every unit in the population has a
be evaluated for stabilization or maturity, or theoretically equal chance of being sampled and

Test Methods for the Examination of Composting and Compost August 27, 2001
02.01-17
Sample Collection and Laboratory Preparation
Field Sampling of Compost Materials 02.01

measured. Consequently, statistics generated by the in an underestimate of the appropriate number of


sample (e.g. sample mean and to a lesser degree, samples to collect.
standard deviation) are unbiased estimators of true 14.8 Simple Random Sampling—For convenience, the
population parameters. That is, the sample is statistical calculations for simple random sampling
representative of the population. A common method of (wherein within-batch heterogeneity that may be
selecting a random sample is to divide the population encountered by a compost producer is low) are
by an imaginary grid, assign a series of consecutive provided (adapted from SW-846 Chapter Nine, part 2,
numbers to the units of the grid, and select the number pages 13-14).
to be sampled using a random-numbers table.
NOTE 2C—Haphazardly selected samples are not random and
14.8.1 Obtain preliminary estimate of x for each
therefore not a suitable substitute for a randomly selected chemical component of compost that is of concern.
sample. That is because there is no assurance that a person The above-identified statistic is calculated by Equation
performing undisciplined sampling will not consciously or 14.8.1.
subconsciously favor the selection of certain units of the
n
population.
14.6.1 Sampling precision is achieved by collecting
 xi
i =1
the appropriate number of samples that are uniformly
distributed across the entire volume of compost. x = n Equation 14.8.1
Precision is improved by increasing the number of where:
samples, while maintaining a sampling pattern to x= simple random sample mean,
guarantee a spatially uniform distribution. n= total number of sample measurements,
14.6.2 If a batch of compost is randomly x= variable in question (e.g., mercury),
heterogeneous with regard to its chemical i= individual samples ranging from 1 to n, and
characteristics and if that random chemical n
heterogeneity remains constant from batch to batch,  xi
accuracy and appropriate precision can usually be i =1 = sum of all x's (analytical results for individual
achieved by simple or systematic random sampling. samples), from i = 1 through i = n.
More complex stratified random sampling is 14.8.2 Obtain preliminary estimate of variance, s2,
appropriate if a batch of compost is known to be non- for each chemical component of concern. The above-
randomly heterogeneous in terms of its chemical identified statistic is calculated by Equation 14.8.2.
properties and non-random chemical heterogeneity is 2
known to exist from batch to batch. In such cases, the
population is stratified to isolate the known sources of
n
 x 2i −  xi
i =1
( )n
n

i =1
non-random chemical heterogeneity. The units in each 2
s = n −1 Equation 14.8.2
stratum are numerically identified, and a simple random where:
sample is taken from each stratum. This type of s2 = variance of simple random sample,
sampling would be advantageous only if the n= total number of sample measurements,
stratification efficiently divides the waste into strata
x= variable in question (e.g., mercury), and
that exhibit maximum between-strata variability and
i= individual samples ranging from 1 to n.
minimum within-strata variability. In composted solid
waste that is frequently turned and mixed, little if any 14.8.3 Estimate the appropriate number of samples
stratification is likely to occur. If little or no (n1) to be collected from the compost through use of
information is available concerning the distribution of Equation 14.8.3 and Table 02.01-C1. Derive
chemical components, simple or systematic random individual values of n1 for each chemical component of
sampling are the most appropriate sampling strategies. concern (x). The appropriate number of samples to be
14.7 Number of Samples—The appropriate number of taken from the compost is the greatest of the individual
samples to collect is the least number required to n1 values.
generate a sufficiently precise estimate of the true mean t 2.20 s 2
concentration of a chemical component of a compost. 2
From the compost producer’s perspective, this means n= ∆ Equation 14.8.3
that the minimum number of samples needed to where:
demonstrate that the upper limit of the confidence
interval for the true mean is less than the applicable n= number of samples,
regulatory threshold value. It is always prudent to 2
t = tabulated “t” value for two-tailed
.20
collect a greater number of samples than indicated by confidence interval and a probability of 0.20,
preliminary estimates of the mean and variance since
poor preliminary estimates of those statistics can result s2 = sample variance, and

August 27, 2001 Test Methods for the Examination of Composting and Compost
02.01-18
Sample Collection and Laboratory Preparation
02.01 Field Sampling of Compost Materials

∆2 = the square of the regulatory threshold completed. Otherwise, continue the study. In the case
minus sample average, defined by US EPA, (e.g., 100 of a set of analytical data that does not exhibit obvious
mg kg-1 for barium in elutriate of EP toxicity). abnormality and for which x is greater than s2,
perform the following calculations with non-
Table 02.01-C1 Tabulated values of Student’s “t” for evaluating transformed data. Otherwise, consider transforming the
compost.
data by the square root transformation (if x is about
Degrees of Tabulated “t” Degrees of Tabulated “t”
freedom value freedom value equal to s2) or the arcsine transformation (if x is less
(n-1) (n-1) than s2) and performing all subsequent calculations with
1 3.078 16 1.337 transformed data.
2 1.886 17 1.333 14.8.6 Determine the confidence interval (CI) for
3 1.638 18 1.330 each chemical component of concern by Equation
4 1.533 19 1.328 14.8.6. If the upper limit of the CI is less than the
5 1.476 20 1.325 applicable regulatory threshold (applied in Equation
6 1.440 21 1.323
14.8.3), the chemical component is not considered to be
7 1.415 22 1.321
present in the compost at a hazardous concentration,
8 1.397 23 1.319
and the study is completed. Otherwise, the opposite
9 1.393 24 1.318
conclusion is tentatively reached.
10 1.372 25 1.316
11 1.363 26 1.315 CI = x ± t 0.20 s x Equation 14.8.6
12 1.356 27 1.314 where:
13 1.350 28 1.313 t 0.20 = referred to in Table 02.01-C1 Tabulated values of
14 1.345 29 1.311 Student’s “t” for evaluating compost for
15 1.341 30 1.310 appropriate degrees of freedom.
40 1.303
14.8.7 If a tentative conclusion of hazard is reached,
60 1.296
re-estimate the total number of samples (n2) to be
120 1.289
collected from the compost by use of Equation 14.8.3.
When deriving n2, employ the newly calculated (not
14.8.3.1 Randomly collect at least n1 (or n2 - n1, n3
preliminary) values of x and s2. If additional n2 - n1
- n2, etc., as will be indicated in step 8) samples from
samples of compost cannot reasonably be collected, the
the compost. Maximize the physical size (volume) of study is completed, and a definitive conclusion of
all samples that are collected from the strata. hazard is reached. Otherwise, collect an extra n2 - n1
NOTE 3C—Collection of a few extra samples will provide
protection against poor preliminary estimates of x and s2. samples of compost.
14.8.3.2 Analyze the n1 (or n2 - n1, n3 - n2, etc.) 14.8.8 Repeat the basic operations described in Steps
samples for each chemical component of concern. 14.8.3 through 14.8.7 until the compost is judged to be
Superficially (graphically) examine each set of non-hazardous or, if the opposite conclusion continues
analytical data from each stratum for obvious to be reached, until increased sampling effort is
departures from normality. impractical.
14.8.4 Calculate the standard deviation (s) for each 14.9 Stratified Random Sampling—For convenience,
set of analytical data by Equations 14.8.1, 14.8.2, the statistical calculation steps for stratified random
14.8.4 and 14.8.5. sampling that must be performed in situations that may
be encountered by a compost producer where within-
s= s2 Equation 14.8.4 batch heterogeneity is high are provided below (from
2 SW-846 Chapter Nine, part 2, pages 18-19).
14.8.5 Calculate x , s , and standard error (sx) for
each set of analytical data by, Equations 14.8.1, 14.8.2, 14.9.1 Obtain preliminary estimate of x for each
and 14.8.5. chemical component of concern. The identified
s statistic is calculated by Equation 14.9.1.

sx = n Equation 14.8.5
14.8.5.1 If x for a chemical component is equal to
or greater than the applicable regulatory threshold
(from Equation 14.8.3) and is believed to be an
accurate estimator of µ (population mean), the
component is considered to be present in the compost
at a hazardous concentration, and the study is

Test Methods for the Examination of Composting and Compost August 27, 2001
02.01-19
Sample Collection and Laboratory Preparation
Field Sampling of Compost Materials 02.01

r
W k xk 14.9.6 Calculate x , s2, the standard deviation (s),
x = k =1 Equation 14.9.1 and sx for each set of analytical data by, respectively,
where: Equations 14.9.1, 14.9.2, 14.8.4 and 14.8.5.
x = stratified random sample mean, 14.9.7 If x for a chemical component is equal to or
xk = stratum mean, and greater than the applicable regulatory threshold (from
Wk = fraction of population represented by stratum k Equation 14.8.3) and is believed to be an accurate
(number of strata [k] range from 1 to r). estimator of µ (population mean), the component is
14.9.2 Obtain preliminary estimate of s2 for each considered to be present in the compost at a hazardous
chemical component of compost that is of concern. concentration, and the study is completed. Otherwise,
The identified statistic is calculated by Equation 14.9.2. continue the study. In the case of a set of analytical
r data that does not exhibit obvious abnormality and for
 W k s2k which x is greater than s2, perform the following
s2 = k =1 Equation 14.9.2 calculations with non-transformed data. Otherwise,
where: consider transforming the data by the square root
s2 = stratified random sample variance, transformation (if x is about equal to s2) or the arcsine
s2k = stratum variance, and transformation (if x is less than s2) and performing all
Wk = fraction of population represented by stratum k
subsequent calculations with transformed data.
(number of strata [k] range from 1 to r). 14.9.8 Determine the confidence interval (CI) for
14.9.3 Estimate the appropriate number of samples each chemical component of concern by Equation
(n1) to be collected from the compost through use of 14.8.6. If the upper limit of the CI is less than the
Equation 14.8.3 and Table 02.01-A1 Tabulated values applicable regulatory threshold (applied in Equation
of Student’s “t” for evaluating compost. Derive 14.8.3), the chemical component is not considered to be
individual values of n1 for each chemical component of present in the compost at a hazardous concentration,
concern. The appropriate number of samples to be and the study is completed. Otherwise, the opposite
taken from the compost is the greatest of the individual conclusion is tentatively reached.
n1 values. 14.9.9 If a tentative conclusion of hazard is reached,
14.9.4 Randomly collect at least n1 (or n2 - n1, n3 - re-estimate the total number of samples (n2) to be
n2, etc., as will be indicated in step 8) samples from the collected from the compost by use of Equation 14.8.3.
When deriving n2, employ the newly calculated (not
compost. If sk for each stratum (see Equation 14.9.2) is
believed to be an accurate estimate, optimally allocate preliminary) values of x and s2. If additional n2 - n1
samples among strata (i.e., locate samples among strata samples of compost cannot reasonably be collected, the
so that the number of samples collected from each study is completed, and a definitive conclusion of
stratum is directly proportional to the sk for that hazard is reached. Otherwise, collect an extra n2 - n1
stratum). Otherwise, proportionally allocate samples samples of compost.
among strata according to size of the strata. Maximize 14.9.10 Repeat the basic operations described in
the physical size (volume) of all samples that are Steps 14.9.3 through 14.9.9 of Fig 02.01-1 Composting
collected from the strata. Unit Operations, until the compost is judged to be non-
14.9.5 Analyze the n1 (or n2 - n1, n3 - n2, etc.) hazardous or if the opposite conclusion continues to be
samples for each chemical component of concern. reached until increased sampling effort is impractical.
Superficially (graphically) examine each set of
analytical data from each stratum for obvious
departures from normality.

August 27, 2001 Test Methods for the Examination of Composting and Compost
02.01-20
Sample Collection and Laboratory Preparation
02.01 Field Sampling of Compost Materials

Test Method: Composting Feedstock Material Sampling Strategies Units: NA


Test Method Applications
Process Management Product Attributes
Step 1: Step 2: Step 3: Step 4: Step 5: Step 6: Step 7: Safety Market
Feedstock Feedstock Composting Odor Treatment Compost Curing Compost Compost Standards Attributes
Recovery Preparation Screening and Storing and
Refining Packaging

02.01-D 02.01-D

02.01-D BATCH FEEDSTOCK MATERIAL SAMPLING STRATEGIES


15. Apparatus for Method D 17.1.2 Transfer the contents of the subsample
container onto (into) mixing surface (container) and
15.1 Sampling Container—20-L (5-gal), stainless
proceed to the next randomly selected sample point.
steel, plastic, glass or Teflon.
17.1.3 Repeat steps 17.1.1 and 17.1.2 until the
15.2 Sampling Device—wooden spatula or tiling
predetermined number of subsamples is obtained.
spade, etc.
17.2 Sample Mixing—Place subsamples on clean tarp
15.3 Trowel—high-density polypropylene (HDPP).
or other similar mixing platform, mix sub-samples
15.4 Plastic Storage Pail—20-L (5-gal), square pails, thoroughly using a wooden spatula or comparable
Use standard 5-gallon plastic pails only when square sampling tool.
pails are not available (e.g., Cleveland Bottle & Supply
17.3 Sample Splitting—Subdivide sample into
Co.; 850 East 77th Street; Cleveland, OH 44103;
quarters, thoroughly mixed composite sample into
telephone: 216 881 3330; Fax: 216 881 7325; URL:
fourths. Repeat steps 17.2 and 17.3 until sample size is
www.clevelandbottle.com/squrpail.html.
appropriate for intended analysis.
16. Reagents and Materials for Method D 17.4 Sample Storage and Shipping—Place composite
16.1 Plastic Gloves. sample aliquot in clean container, preferably a Teflon
16.2 Tarp—clean plastic, canvas, or other type of pail or similar inert material.
mixing surface if feedstock is liquid sludge. CAUTION—Do not use galvanized sheet metal collection or
®
mixing tools. The galvanized coating will contaminate the
16.3 Plastic Bags—three 4-L (1 gal) Ziploc freezer sample with zinc.
bags. 17.4.1 Transfer blended feedstock or compost to fill
16.4 Cold Packs—chemical ice packs, three 4-L (1-gal) plastic Ziploc® freezer bags.
16.5 Aluminum Foil—lining for plastic shipping pail, 17.4.2 Line the shipment pail with aluminum foil to
and minimize heat exchange. Place the plastic Ziploc®
16.6 Adhesive Tape—duct tape, 5-cm (2-in.) width. freezer bags containing the feedstock samples in the
plastic pail and interleave with cold packs for shipping
17. Procedure for Method D (refer to Fig 02.01-B3).
17.1 Sample Collection—Identify and collect an 17.4.3 Seal the square pail with its lid. Seal and
appropriate number of subsamples needed to ensure a secure lid with duct tape. Send the square plastic pail
reliable analytical result as described in Methods containing samples by two-day express service to the
02.01-A, B or C. selected laboratory for analysis. Include completed
17.1.1 Place each subsample into a sampling chain of custody forms when necessary.
(subsample) container. NOTE 1D—If any delay is anticipated, cool sample to 4°C
(39.2°F) to diminish microbial and chemical activity prior to
sample shipment.

Test Methods for the Examination of Composting and Compost August 27, 2001
02.01-21
Sample Collection and Laboratory Preparation
Field Sampling of Compost Materials 02.01

Test Method: Data Quality Management and Sample Chain of Custody Units: NA
Test Method Applications
Process Management Product Attributes
Step 1: Step 2: Step 3: Step 4: Step 5: Step 6: Step 7: Safety Market
Feedstock Feedstock Composting Odor Treatment Compost Curing Compost Compost Standards Attributes
Recovery Preparation Screening and Storing and
Refining Packaging

02.01-E 02.01-E 02.01-E 02.01-E 02.01-E 02.01-E

02.01-E DATA QUALITY MANAGEMENT AND SAMPLE CHAIN OF CUSTODY


18. Aspects of Sampling Quality Assurance for 18.4 Tracking Quality—A sample must be properly
Reported Data collected and prepared for shipment, and then properly
manipulated by laboratory personnel who follow
18.1 Three critical steps in the sampling process
specific preparation protocols designed for each
precede laboratory analysis and often dictate data
analytical methodology. Previous sections emphasized
quality.
the importance of properly designed and implemented
18.1.1 sample planning and collection; sampling plans. This section introduces a protocol
18.1.2 sample handling and preservation; and designed to modify data interpretation to interpret
sample variability.
18.1.3 laboratory sample preparation.
18.4.1 Consider the following hypothetical sampling
18.2 Each step in the sampling process must be plan that incorporates an additional step to verify
properly executed in a timely manner by well informed, accuracy of reported results using cross-validation
trained individuals to ensure that the collected sample techniques. One type of a statistically valid sample
accurately represents a compost batch, windrow or pile. management plan requires that samples are properly
18.3 Quality Sample Management—Regulatory and collected at a very high frequency while the actual
certification systems may dictate that samples are number of samples submitted for analysis remains
properly collected, preserved and prepared for analysis. small.
Consider the following hypothetical example of sample 18.4.1.1 Establish Baseline—A significant number
management where a certified third party is introduced of samples that represent the composting process of a
to manage the sampling plan. facility are collected over time and sent to a laboratory
18.3.1 The third party assumes all quality assurance for analysis. Results from these samples serve to
and quality control responsibilities associated with: establish a baseline of information that accurately
18.3.1.1 sample planning and collection; represents the compost produced by the facility and a
given feedstock blend.
18.3.1.2 sample handling and preservation; and
18.4.1.2 Track Deviations from Baseline—After the
18.3.1.3 laboratory sample preparation. baseline is established, samples are collected at
18.3.2 Responsibility for rigorous sample collection specified intervals, over time or per unit of compost
is transferred from facility management to the third produced (refer to TMECC 02.01-A Equation 9.9.1
party. Responsibilities associated with sample storage, Formula to estimate sampling interval), and held in
preparation and laboratory analysis are also transferred cold storage. After a specified interval, (e.g., quarterly
from the analytical laboratory to the third party. or monthly) a small but statically representative number
18.3.3 One of the principal benefits of the third party of prepared samples are randomly selected from the
sampling system is to diminish deviations in sampling stored samples and sent to a laboratory for analysis.
plan interpretation and implementation across separate Because multiple samples would be randomly selected
facilities and laboratories. Third party control can from a larger population of samples, a more reliable
decrease variability by maintaining consistent field statistical inference can be generated than by simply
sampling protocols across all participating facilities. directly submitting monthly or quarterly samples for
Field sample collections would be implemented as analysis.
described in TMECC 02.01 Field Sampling of Compost 18.4.2 Sampling programs of this nature may require
Materials. Consistent sample preparation protocols that field samples, or samples prepared for laboratory
would also be followed for laboratory analysis as analysis, are submitted to a secure or bonded cold-
described in TMECC 02.02 Laboratory Sample storage facility where frequently collected samples are
Preparation for Analysis. inventoried and properly stored. Samples must be
retained in storage for a predetermined time period to

August 27, 2001 Test Methods for the Examination of Composting and Compost
02.01-22
Sample Collection and Laboratory Preparation
02.01 Field Sampling of Compost Materials

safeguard against cases where a need for re-testing may and monitoring protocol. Successful implementation
arise. will increase when data quality relates to an increased
18.4.3 Sampling Costs—Sampling program financial incentive, either artificially through incentives
maintenance costs should be considered when offered by the governing regulatory agency or through
designing an effective monitoring system. It is difficult quality assurance certification programs designed to
to weigh the relative importance of data quality when indirectly increase market share.
there is no clear relationship between financial outcome

Test Methods for the Examination of Composting and Compost August 27, 2001
02.01-23
Sample Collection and Laboratory Preparation
Field Sampling of Compost Materials 02.01

02.01 SUMMARY
19. Report involved in the chain of possession. Refer to Fig
02.01-E1 Chain of Custody form for an example.
19.1 Chain of custody forms and procedures should
be used with all environmental or regulatory samples. 20. Keywords
A chain of custody form is used to track sample 20.1 accuracy; aliquot; attribute verification; bias;
handling from time of collection through laboratory chain of custody; closed vessel system; composite;
analysis, and data reporting. Suggested information for compost; coefficient of variation; %CV, confidence
the chain-of-custody record includes, at a minimum: interval; feedstock; grab-sample; point-sample; point-
Collector’s name; Signature of collector; Date and time sampling; open vessel system; precision; process
of collection; Place and address of collection; monitoring; process variability; product variability;
Requested preprocessing (subsampling, compositing, quality control; quality assurance; representative
sieving); Requested analyses; Sample code number for sample; sample collection frequency; sampling;
each sample (if used); Signature of the persons sampling plan; statistical validity; stratified sampling;
windrow.

August 27, 2001 Test Methods for the Examination of Composting and Compost
02.01-24
CHAIN OF CUSTODY FORM 02.01 Field Sampling of Compost Materials
STA Laboratory: Tel:
LABORATORY USE ONLY Storage Locations
Address: FAX: Freezer _____ Cold Room _____ Storage Shelf _____
Email: _____ _____ _____ _____ _____ _____ _____ _____ _____
City, State Zip code: Sample Condition:
Client/Reporting Company:
Tel: Sample Type:  COMPOSITE  POINT  STRATIFIED
Contact Name: FAX: P.O. Number:
Billing Address: Email: Client STA ID:
USCC Member:  YES  NO ID: ____________________________________
City, State Zip code: SELECTION OF ANALYSIS. Refer to http://tmecc.org/sta for details.
STA Suite; All 503 Rule Tests; Other – Specify additional tests in fields A through D (below).
Send Results to:
NOTE ! Your selection of STA Suite (below) authorizes laboratory personnel to disclose all analytical
City, State Zip code: results AND submit the STA Compost Technical Data Sheet directly to STA program management.
Name or Source of sample(s): A B C D
Name of Sample Collector:
Client Sample Identification Collection Sample Sample Shipping Selected Analysis Lab/Job
(and special instructions) Date/Time Matrix Container Temp. STA 503 A B C D Number
1 Date: Compost  Plastic Bag  Ambient  1
Time: Feedstock  Pail  Wet Ice       
Initials: ________  ________  Dry Ice 
2 Date: Compost  Plastic Bag  Ambient  2
Time: Feedstock  Pail  Wet Ice       
Initials: ________  ________  Dry Ice 
3 Date: Compost  Plastic Bag  Ambient  3
Time: Feedstock  Pail  Wet Ice       
Initials: ________  ________  Dry Ice 
4 Date: Compost  Plastic Bag  Ambient  4
Time: Feedstock  Pail  Wet Ice       
Initials: ________  ________  Dry Ice 
5 Date: Compost  Plastic Bag  Ambient  5
Time: Feedstock  Pail  Wet Ice       
Initials: ________  ________  Dry Ice 
Releasing Date Time Receiving Date Time
Signature 1 Signature 1
Releasing Date Time Receiving Date Time
Signature 2 Signature 2
Releasing Date Time Receiving Date Time
Signature 3 Signature 3
Releasing Date Time Receiving Date Time
Signature 4 Signature 4
Fig 02.01-E1 Chain of Custody. Compost sample chain of custody log Revised August 27, 2001
Sample Collection and Laboratory Preparation
02.02 Laboratory Sample Preparation for Analysis

Test Method: Laboratory Sample Preparation. Six Protocols Units: NA


Test Method Applications
Process Management Product Attributes
Step 1: Step 2: Step 3: Step 4: Step 5: Step 6: Step 7: Safety Market
Feedstock Feedstock Composting Odor Treatment Compost Curing Compost Compost Standards Attributes
Recovery Preparation Screening and Storing and
Refining Packaging
02.02-A 02.02-A 02.02-A 02.02-A
02.02-B 02.02-B 02.02-B 02.02-B 02.02-B
02.02-C 02.02-C 02.02-C 02.02-C 02.02-C
02.02-D 02.02-D 02.02-D 02.02-D
02.02-E 02.02-E 02.02-E 02.02-E
02.02-F 02.02-F

02.02 LABORATORY SAMPLE PREPARATION


DISCLAIMERS 1.4 This document is a working draft and is not
(1) The methodologies described in TMECC do not purport to address all approved for publication. All methods and sampling
safety concerns associated with their use. It is the responsibility of the protocols provided in TMECC are subject to revision
user of these methods to establish appropriate safety and health
practices, and to determine the applicability of regulatory limitations
and update to accommodate new widely accepted
prior to their use. advances in techniques and methods.
(2) All methods and sampling protocols provided in TMECC are subject to
revision and update to correct any errors or omissions, and to 1.5 The process alternatives, trade names, or
accommodate new widely accepted advances in techniques and commercial products are only examples and are not
methods. Please report omissions and errors to the U.S. Composting endorsed or recommended by the U.S. Composting
Council Research and Education Foundation. An on-line submission
form and instructions are provided on the TMECC web site, Council Research and Education Foundation.
http://www.tmecc.org. Alternatives may exist or may be developed.
(3) Process alternatives, trade names, or commercial products as mentioned
in TMECC are only examples and are not endorsed or recommended by 1.6 Omissions and errors should be reported to the
the U.S. Department of Agriculture or the U.S. Composting Council U.S. Composting Council Research and Education
Research and Education Foundation. Alternatives may exist or may be
developed. Foundation. An on-line submission form and
instructions are provided on the TMECC web site,
1. Scope http://www.tmecc.org.
1.1 This section covers laboratory sample handling
and preparation for physical, chemical and biological 2. Referenced Documents
laboratory analysis. 2.1 TMECC:
1.1.1 Method 02.02-A Sample Mixing and Splitting. Method 03.05-A Film Plastic Surface Area
Determinations Using Digital Processing.
1.1.2 Method 02.02-B Sample Sieving for Aggregate
Method 03.06-A Glass Shards, Metal Fragments and Hard
Size Classification.
Plastics Wet Sieving Technique.
1.1.3 Method 02.02-C Man Made Inert Removal 2.2 Other References:
and Classification.
ASTM D 2977-71, Standard Test Method for Particle Size
1.1.4 Method 02.02-D Milling and Grinding Range of Peat Materials for Horticultural Purposes. In
Samples, Harrison. Annual Book of ASTM Standards, Vol. 04.08.
1.1.5 Method 02.02-E Milling and Grinding ASTM D 5231-92, Determination of the Composition of
Samples, Munter. Unprocessed Municipal Waste. In Annual Book of
ASTM Standards, Vol. 04.08
1.1.6 Method 02.02-F Modifications for Feedstock
Cohen, I.R. 1973. Laboratory Procedure for the
Sample Preparation. Preparation of Solid Waste Related Materials for
1.2 Values stated in SI units are to be regarded as the Analysis. pp 1-5. In Methods of Solid Waste Testing.
standard. Values given in parentheses are provided for Bender, D.F., M.L. Peterson, and H. Stierli, ed. EPA-
information only. 6700-73-01. US EPA Cincinnati, OH.
Eik, K., and R.H. Gelderman. 1988. Recommended
1.3 The methodologies described in this section do
Chemical Soil Test Procedures for the North Central
not purport to address all safety concerns, if any, Region. Bul. No. 499 (Revised) Oct. North Dakota
associated with their use. It is the responsibility of the Agricultural Experiment Station, NDSU, Fargo, ND.
user of these methods to establish appropriate safety 58105.
and health practices and to determine the applicability Harrison, R.B., D. Buxton, C.L. Henry, J. Canary, S.
of regulatory limitations prior to their use. Brallier J. Krejsl, X. Dongsen and S. Smith. 1991.

Test Methods for the Examination of Composting and Compost April 7, 2002
02.02-1
Sample Collection and Laboratory Preparation
Laboratory Sample Preparation for Analysis 02.02

Contribution of source material to trace metal fractions backup, and the remaining portions are placed in cold
in RECOMP compost: Report after initial sampling. storage (4°C) or further processed for laboratory
Report to RECOMP of Washington, Inc. analysis.
Method 922.02, Plants. 1990. In J. Am. Soc. Official
Analytical Chem. 4.2 Method 02.02-B Sample Sieving for Aggregate
Size Classification—A 4-L aliquot of as-received
Minnesota Pollution Control Agency (MPCA) Solid Waste
Management Rules 7035.2835.
material is passed through a series of nested sieves.
The moisture and total solids content are determined
Piper, C.S. 1942. Soil and Plant Analyses; A Laboratory
for each size fraction and the sieve size distribution of
Manual of Methods for Examination of Soils and the
Determination of the Inorganic Constituents of Plants.
the bulk sample is calculated.
Univ. of Adelaide. Adelaide. 4.3 Method 02.02-C Man Made Inert Removal and
Soil Survey Laboratory Methods Manual. 1992. Soil Classification—Perform this test on size classed
Survey Investigations Report No. 42, Version 2.0, samples (aliquot size up to 250 cm3). Inerts are hand
August, p.1., National Soil Survey Center, Soil sorted and classified for each size fraction. After the
Conservation Service, USDA. Lincoln, Nebraska. inerts > 4 mm, and sharps > 2 mm are removed from
Smith, J.H., D.L. Carver, M.J. Brown and C.L. Douglas. this fraction, the total fraction < 9.5 mm is milled for
1968. Differences in chemical composition of plant the metal and LOI OM analysis, and other tests that call
sample fractions resulting from grinding and screening. for where air-dried, milled samples.
Agron. J. 60:149-151.
4.3.1 Inert removal prior to milling and acid
Statistical Quality Control Handbook. Western Electric
Company, Inc. 2nd Edition. 1958.
digestion decreases the incidence of inflated metal
analysis. The air-dried working sample aliquot with
Test Methods for Evaluating Solid Waste,
inerts removed is milled to a powder and stored in a
Physical/Chemical Methods, SW-846, US EPA, Third
Edition, September, 1986.
sealed plastic bottle to minimize accumulation of
hygroscopic moisture. Tests performed on milled air-
3. Terminology dried (36°C) samples are heavy metals, plant nutrients
3.1 aliquot, n—a subsample of a material prepared (except N), and organic carbon (OC).
for, and subjected to laboratory analysis. A subsample 4.4 Method 02.02-D Milling and Grinding Samples,
size smaller than 1 g may be used to represent more Harrison—A large sample (250 cm3) of relatively
than 1000 kg of compost. coarse, oven-dried material is milled with a Wiley Mill
3.2 air-dry weight, n—Weight of sample material air- into a fine dust and thoroughly blended. Small aliquots
dried in a forced air oven at 36°C for 48-72 h. (< 5 g) of the milled material are selected to represent
the bulk sample for elemental analysis.
3.3 as-received weight, n—Mass of a sample with a
moisture content of that at time of receipt by a 4.5 Method 02.02-E Milling and Grinding Samples,
laboratory. Munter—Preferred method to minimize sample
heterogeneity. A large sample (250 cm3) of relatively
3.4 fresh weight, n—Weight of undried sample
coarse, air-dried material (< 9.5 mm) with inerts
material, stored and maintained at the same moisture
removed is milled with a Stein Mill equipped with a
content as at time of receipt.
carbide blade into a fine dust and thoroughly blended.
3.5 oven dry weight (ODW), n—Weight of sample Small aliquots (< 5 g) of the milled material are
material dried in a forced air oven at 70±5°C for 18-24 selected to represent the bulk sample for elemental
h, or until sample weight change diminishes to nil. analysis.
3.6 working sample, n—Sieved (square mesh) fresh 4.6 Method 02.02-F Modifications for Feedstock
material. Less than 9.5 mm fraction. Sample Preparation—A large sample (1000 cm3) of
relatively coarse material is milled into a fine dust and
4. Summary of Test Methods
thoroughly blended. Small aliquots (< 5 g) of the
4.1 Method 02.02-A Sample Mixing and Splitting— milled material are selected to represent the bulk
The bulk sample is thoroughly blended. The blended sample for elemental analysis.
sample is split into separate components using a CAUTION—To avoid metal contamination, heavy metals
stainless steel sample splitter. One portion (4L, 1 gal) analyses should be performed only on materials that are milled
of the sample is placed in frozen storage (-4°C) as with carbide-tipped blades.

April 7, 2002 Test Methods for the Examination of Composting and Compost
02.02-2
Sample Collection and Laboratory Preparation
02.02 Laboratory Sample Preparation for Analysis

~½ OF SAMPLE

Mix and Split


Sample Sample Store as Back-up
Received Refer to Method 02.02- ~½ OF SAMPLE frozen (-4°C) or refrigerated (4°C)
(4 L to 12 L) A Sample Mixing and Refer to Tables 02.01-2 thru
Splitting 02.01-6 for holding times and limitations

Sieve Sample
Refer to Method 02.02-B
Sample Sieving for
Aggregate Size
Classification
Physical Tests
Physical Tests Refer to Chapter 3
Refer to Chapter 3

Perform tests on air-dried


Are tests sample. Dry approx. 250 cm3
Perform tests on
to be performed aliquot at 36°C under ~95% RH until
moist sample NO YES
on Air-Dry changes in mass due to moisture loss
(mix/split as necessary) diminish to nil. Replicate as
Samples?
required.

MOISTENED SAMPLE Inert Content and


AS-RECEIVED Removal
Prep samples upon receipt.
Moisten/Dry Split Sample MOISTURE Refer to Method 02.02-C
Prep sample upon receipt. Man Made Inert Removal
to achieve ~ 85% WHC
and Classification

Emergence and Growth


Blend moistened sample with equal Total Solids Mill inert-free test
determine on ~10 g sample. Refer to
volume of rinsed, moist vermiculite.
parallel aliquot; used to Method 02.02-E
Report results for sample and control.
Refer to Method 05.05-A correct results from as-
received to oven dry
weight basis. Refer to
Method 03.09-A Total Solids
CO2 Respirometry (70±5°C) determine on ~10 g
Incubate moistened sample
parallel aliquot; used to
under ~95% RH.
correct results from air-
Refer to Method 05.08-B
dry to oven dry weight
Nitrate-N & Ammonium-N basis. Refer to Method
Refer to Methods 04.02-B and 03.09-A (70±5°C)
04.02-C. Report as mg NO3-N
Total Solids and NH4-N per kg dw basis.
determine on ~10 g
parallel aliquot to correct Elemental Analysis
respirometry result from (e.g., C, N, P, K, Ca,
moistened to oven dry Pathogens Mg, Na, Cl, etc.)
weight basis. Refer to Refer to Sections
Method 03.09-A 07.01 and/or 07.02 Caution: For odorous materials,
(70±5°C)
TN should be determined on as-
received moist material

Optional: LOI Organic


Correct to, and report Matter and Total Nitrogen
on both dry weight and Cation Exchange Capacity
Performed on as-received moist
OM bases Refer to Section 04.09
unmilled rather than air-dry milled
material. Correct to and report as
%, dw basis.

Correct to, and report LOI Organic Matter


on dry weight basis Refer to Method 05.07-A
EC1:5 and pH1:5
Account for sample moisture
content and create a 1:5
solids:liquids slurry.
Report Refer to Methods 04.10-A and Correct to, and report
04.11-A on dry weight basis

Fig 02.02-1 Flow of sample fate through laboratory sample preparation. Only common routine testing is included in this illustration. Please
note that a majority of physical tests (TMECC Chapter 03) are performed on as-received moist material. Notable exceptions include one of the
water-holding capacity tests and both wettability tests which call for dried materials. Additional tests performed on as-received moist material
not listed in the diagram include all other respirometry methods, bioassays, VFA’s, other pathogens and synthetic organic compounds. Refer to
specific TMECC sections and methods for detailed descriptions of, or deviations in, sample preparation protocols.

Test Methods for the Examination of Composting and Compost April 7, 2002
02.02-3
Sample Collection and Laboratory Preparation
Laboratory Sample Preparation for Analysis 02.02

5. Significance and Use 5.6 Method 02.02-F Modifications for Feedstock


Sample Preparation—Refer to specific test methods
5.1 Method 02.02-A Sample Mixing and Splitting—
for applications.
Sample heterogeneity is a serious limiting factor for
biological, chemical and physical analysis. Poor 6. Interference and Limitations
analytical precision is often related to inadequate 6.1 Standardized sample preparation will minimize
sample handling, preparation and blending. For error in analytical results.
example, compost subsamples may arrive at the
laboratory in three separate bags instead of as three 6.2 Samples must be thoroughly mixed and blended
bags of a composite sample. A composite sample is before extracting an aliquot for analysis. Recall, as
blended and subdivided in the field at the time of much as 20,000 m3 of compost is represented by one
sampling. sample aliquot as small as 0.5 g. It is vital that the
received sample be thoroughly blended. Quality
5.2 Method 02.02-B Sample Sieving for Aggregate control and quality assurance must be employed for all
Size Classification—Sample heterogeneity can be compost materials.
attributed to variations in physical, biological and
chemical characteristics across and within sub-samples. 6.2.1 Excessive sample handling can increase
Sample variability is often stratified across aggregate evaporative and volatile loss of some compounds of
sizes. Segregation of a sample according to aggregate interest. Loss is diminished when samples are handled
size fractions facilitates differentiation of these factors and prepared in a cold-room at approximately 4°C.
across material size fractions and their corresponding 6.2.2 Micro-nutrients and heavy metals analysis—
degrees of degradation and other forms of Sample containers must be pre-washed with detergents,
heterogeneity. (e.g., 10% RBS, P-free and B-free), acids, and Type II
5.2.1 Tests performed on moist samples include water. Plastic and glass containers are suitable. Refer
sieve size classification, total N, NH4+, NO3, pH, to Chapter 3 in Annual Book of ASTM Standards for
electrical conductivity, respirometry, pathogen testing, detailed information.
germination and growth, bulk density, water holding 6.3 Method 02.02-B Sample Sieving for Aggregate
capacity (WHC), porosity/pore space, volatile fatty Size Classification—Most sample analyses are
acids (VFA) and LOI organic matter. performed on material sieve fractions smaller than 9.5
5.2.2 Tests performed on samples air-dried at 36°C mm. Larger fractions are generally evaluated for their
include inert count, and after milling include heavy inert content and relative contribution to the volume
metals, plant nutrients (including total N for mature and mass of the bulk sample, and as bulking materials
material low in ammonia), and organic carbon (OC). used to manage pile porosity. Material smaller than 2
mm is soil by definition, and is considered too small to
5.2.3 Tests performed on samples oven dried at evaluate for inert content using standard dry sieving
70±5°C include total solids and moisture, and volatile methods.
solids.
6.4 Method 02.02-C Man Made Inert Removal and
5.3 Method 02.02-C Man Made Inert Removal and Classification—The < 9.5 mm material is dried at a
Classification—Inert materials include metals, hard and lower temperature (36°C) to minimize loss of volatile
film plastics, glass shards, sharps (sewing needles, compounds and elements such as mercury.
straight pins and hypodermic needles), and large stones
and wood fragments. Inert removal prior to acid 6.4.1 This method for removal of inerts is performed
digestion decreases the incidence of inflated metal on air-dried (36°C) sample material. Inert materials
analysis. can easily be over-looked, especially when many
samples are processed too rapidly. The process is time
5.4 Method 02.02-D Milling and Grinding Samples, consuming and should not be rushed.
Harrison—A milled sample can be well mixed to
create a relatively homogeneous material. From this 6.5 Method 02.02-D Milling and Grinding Samples,
milled material, small aliquots of 1 to 2 g can be Harrison—This method was devised for compost
analyzed for metals and other constituents with high samples that do not contain foreign materials such as
precision relative to the entire milled sample. glass, metal or plastics. This method is not
recommended for MSW or yard waste composts that
5.5 Method 02.02-E Milling and Grinding Samples, may contain man-made inerts.
Munter—Sample homogeneity is increased by
thoroughly blending and milling a sample. The 6.6 Method 02.02-E Milling and Grinding Samples,
technique improves precision of elemental and Munter—Grinding pure quartz sand erodes the metal
chemical analyses by homogenizing a sample aliquot blade by a minor amount relative to the amount of
(250-cm3) that represents the bulk sample. metals found in compost. The < 2-mm sieve fraction of
compost may contain abrasive sand, glass and metal

April 7, 2002 Test Methods for the Examination of Composting and Compost
02.02-4
Sample Collection and Laboratory Preparation
02.02 Laboratory Sample Preparation for Analysis

that will erode the carbide blade, but not to the degree pathogen assays to be conducted (Refer to Table 07.00-
found after milling pure quartz sand. 2).
6.7 Method 02.02-F Modifications for Feedstock 7.3 Preservation and Storage of Samples:
Sample Preparation—Refer to specific methods for 7.3.1 Short-Term Storage < 24 h—Moist material
details.
should be placed in cold storage (4°C) until sample
7. Sample Handling preparation is initiated to minimize microbial and
7.1 Finished Compost—Approximately 12 L (3 gal) chemical activity that could alter the material's
of compost material are needed to complete a full suite characteristics. Air-dried milled material and oven-
of analytical procedures including physical, biological dried material should be stored in sealed containers
and chemical tests. The entire composite sample should such as plastic or glass bottles at room temperature.
be blended and split upon receipt. If any delay is 7.3.2 Long-Term Storage > 24 h—Moist material
anticipated, the material should be placed in cold should be placed in frozen storage (-4°C) until sample
storage (4°C) until sample preparation can continue. preparation is initiated to stop microbial and chemical
The sample must be retained for no more than 14 d in activity. Air-dried, milled material and oven-dried
cold storage. Material must be blended in a closed material should be placed in cold storage (4°C) in
container to minimize evaporative water loss. sealed containers such as plastic or glass bottles after
7.2 Samples for Pathogen Analysis—Sterile whirl no more than 14 d to minimize microbial and chemical
packs are often used for samples to be analyzed for activity. Air-dried milled material and oven dried
pathogen content. A separate whirl pack should be material should be stored frozen (-4°C) in sealed
used for each analytic sample, i.e., prepare one aliquot containers such as plastic or glass bottles for periods in
for each sample. Samples should be analyzed excess of 14 d.
immediately or stored appropriately for the type of

Test Methods for the Examination of Composting and Compost April 7, 2002
02.02-5
Sample Collection and Laboratory Preparation
Laboratory Sample Preparation for Analysis 02.02

Test Method: Laboratory Sample Preparation. Sample Mixing and Splitting Units: NA
Test Method Applications
Process Management Product Attributes
Step 1: Step 2: Step 3: Step 4: Step 5: Step 6: Step 7: Safety Market
Feedstock Feedstock Composting Odor Treatment Compost Curing Compost Compost Standards Attributes
Recovery Preparation Screening and Storing and
Refining Packaging
02.02-A 02.02-A 02.02-A 02.02-A

02.02-A SAMPLE MIXING AND SPLITTING


CAUTION—Always clean and disinfect equipment before min to assure complete blending. This allows mixing
processing a second sample. without artificial drying.
NOTE 1A—This method is based upon procedures developed 10.2 Sample Splitting—Split the sample by passing it
for municipal solid waste (MSW) compost materials at the
University of Minnesota Research Analytical Lab , Department through a stainless steel splitter/divider; use stainless
of Soil, Water and Climate, St. Paul. steel or plastic collection pans.
8. Apparatus for Method A 10.3 Sample Storage—Store approximately one-third
to one-half as reserve in a freezer (-4°C). The
8.1 Twin Shell Dry Blender—tumbling mixer
remaining sample portion (4 L to 8 L) is sieved as
modified to hold a closed 20 L (5-gal) plastic pail,
outlined under Sample Sieving for the Particle Size and
(e.g., LB-2191 - The Patterson-Kelly Co. Inc. East
other tests.
Stroudsburg, PA).
8.2 Sample-Splitter, and Divider—stainless steel with 10.4 Whirl Pack Storage—Store at 4°C up to a
2 in. wide chutes, stainless steel collection pans, (e.g., maximum of 30 h.
Soil Test Model Cl-286, Lake Bluff, IL. 60014). CAUTION !—Excessively Moist Samples need to be partially
air-dried prior to mixing, to minimize the formation of balls and
9. Reagents and Materials for Method A clumps. Spread excessively moist material on a large plastic
bag, place in open air, intermittently mixing with gloved hand
9.1 Water—deionized (DI), 17 M!·cm or purer. until the proper moisture level is reached (approximately 40-
9.2 Storage Bags—4-L (1-gal) plastic Ziploc®. 50% moisture). Check the sample every 6-12 h; do not over-
dry.
9.3 Whirl Packs—200-mL (e.g., Nasco whirl-pak®). CAUTION !—Do not use galvanized sheet metal sieves,
collection pans or mixing pails. The galvanized coating will
10. Procedure for Method A contaminate the sample with zinc.
10.1 Sample Mixing—Tumble as-received (fresh)
sample with mixer in sealed 20-L plastic pail for <30

April 7, 2002 Test Methods for the Examination of Composting and Compost
02.02-6
Sample Collection and Laboratory Preparation
02.02 Laboratory Sample Preparation for Analysis

Test Method: Laboratory Sample Preparation. Sample Sieving for Aggregate Size Units: NA
Classification
Test Method Applications
Process Management Product Attributes
Step 1: Step 2: Step 3: Step 4: Step 5: Step 6: Step 7: Safety Market
Feedstock Feedstock Composting Odor Treatment Compost Curing Compost Compost Standards Attributes
Recovery Preparation Screening and Storing and
Refining Packaging
02.02-B 02.02-B 02.02-B 02.02-B 02.02-B

02.02-B SAMPLE SIEVING FOR AGGREGATE SIZE CLASSIFICATION


COMMENT—After splitting the mixed sample, the larger 13.2.3 Repeat these steps until the entire sample is
subsample is immediately weighed and passed through nested sieved and sorted according to size fraction.
sieves (e.g., 50-mm, 25-mm, 16-mm, 9.5-mm, 6.4-mm, and 4-
mm) for the aggregate size classification. 13.3 Sample Splitting—Material that passes through
CAUTION !—Excessively moist compost, >85% WHC, (Refer the 9.5-mm sieve is subdivided into three separate
to Method 03.10), will clump and compact during the sieving aliquots.
process.
13.3.1 A small aliquot (30-50 cm3) is oven dried at
11. Apparatus for Method B 70±5°C for 24 to 36 h in 100-mL beaker to determine
11.1 Sieves—20-cm (8-in.) diameter, stainless steel wet basis sample moisture.
frame and cloth: 50-mm (2-in.), 25-mm (1-in.), 16-mm 13.3.2 A larger aliquot of each fraction (250-300
("-in.), 9.5-mm (#-in.), 6.4-mm (¼-in., optional), and cm3) is air-dried at 36°C for approximately 48-72 h.
4-mm ($ in., #5), (e.g., Gilson Company Inc.,
Worthington, OH 43085-0677, or equivalent). 13.3.3 The remainder is placed in cold storage (4°C)
for tests performed on moist sample material.
11.2 Mechanical Shaker—for nested sieves, (e.g.,
Tyler Model RX-86, or equivalent). 13.4 Determine Moisture Content—Each of the
remaining size fractions is placed in tared drying
11.3 Beakers—100-mL, 250-mL.
containers, weighed and oven dried at 70±5°C for 24-
11.4 Drying Oven—forced air. 72 h (until sample weight change diminishes to nil) to
12. Reagents and Materials for Method B determine moisture content.
CAUTION—Do not flash dry in a microwave. Flash drying
12.1 Drying Containers—capable of retaining mass at elevates temperature above 36°C and can create small spheres
temperatures above 75°C, (e.g., paper bags, brown, #4). of charred material around metal filings.
13. Procedure for Method B 13.5 Reporting Basis—The results for all tests are
13.1 Weigh Sample Aliquot—Weigh and record the reported on a weight basis adjusted to a 70±5ûC dry
fresh weight of at least 2 L (½ gal), but no more than 6 weight (both moist and air-dried aliquots).
L (1½ gal) of the received compost, assuming total COMMENT—Tests are performed on both moist samples and
air-dried samples. It is important to follow the instructions
sample size of 4 L (1 gal). given for each specific test. Samples targeted for metals
NOTE 2B—An equal volume shall be placed in long term frozen analysis are to be air-dried under forced air at 36ûC for
storage (-4°C) - Refer to Method 02.02-A Sample Mixing and approximately 48-72 h.
Splitting.
14. Calculations for Method B
13.1.1 If delays are anticipated, the working sample
scheduled for further analysis should be placed in cold 14.1 Moisture Content (wet basis; %)—correct all
storage (4ûC) from which sub samples are removed as weights to 70±5°C dw basis.
required for different tests. 14.1.1 Air-Dried Samples (36°C):
13.2 Nested Sieving: M = [1 - (A ÷ F) × (O ÷ A)] × 100 Equation 14.1.1
13.2.1 Nest the sieves and transfer approximately 14.1.2 Oven-Dried samples (70±5°C):
250 cm3 aliquot of bulk material onto the top sieve (50 M= (1 - O ÷ F) × 100 Equation 14.1.2
mm); cover and secure the nested sieves onto the where:
mechanical shaker set for 5 min. A= air dry weight at 36°C,
13.2.2 Place the respective size fractions into O= oven dry weight at 70±5°C, and
corresponding labeled and tared drying containers (e.g., F= weight of material at as-received moisture.
#4 paper bags or other suitable containers).

Test Methods for the Examination of Composting and Compost April 7, 2002
02.02-7
Sample Collection and Laboratory Preparation
Laboratory Sample Preparation for Analysis 02.02

14.2 Determine Sieve Size Distribution: Oi = oven dry weight of individual sieve size fractions
(dried at 70±5°C), g,
14.2.1 For each sieve fraction, calculate:
i = sieve size fractions of interest, (e.g., < 4-mm, 4-mm
Ri = Oi ÷ OB × 100 Equation 14.2.1 to 6.4-mm, 6.4-mm to 9.5-mm, 9.5-mm to 16-mm,
where: 16-mm to 25-mm, 25-mm to 50-mm, and >50-mm),
Ri = relative contribution of sieve size fraction “i” to and
bulk weight of sample, %, OB = oven dry weight of bulk sample (dried at 70±5°C),
before sieving, g.

April 7, 2002 Test Methods for the Examination of Composting and Compost
02.02-8
Sample Collection and Laboratory Preparation
02.02 Laboratory Sample Preparation for Analysis

Test Method: Laboratory Sample Preparation. Man Made Inert Removal and Units: NA
Classification
Test Method Applications
Process Management Product Attributes
Step 1: Step 2: Step 3: Step 4: Step 5: Step 6: Step 7: Safety Market
Feedstock Feedstock Composting Odor Treatment Compost Curing Compost Compost Standards Attributes
Recovery Preparation Screening and Storing and
Refining Packaging
02.02-C 02.02-C 02.02-C 02.02-C 02.02-C

02.02-C MAN-MADE INERT REMOVAL AND CLASSIFICATION


NOTE 1C—This method is based upon procedures developed passes the 4-mm sieve to a separate container. Obtain
for MSW compost materials at the University of Minnesota and record the mass of the < 4-mm fraction and set
Research Analytical Lab., Department of Soil, Water and aside for further processing (step 17.4).
Climate, St. Paul, MN 55108.
COMMENT—This test was designed to be performed in 17.2.2 Transfer the remaining fraction (> 4-mm) to a
conjunction with Method 02.02-B Sample Sieving for clean lab tray or other flat, smooth surface.
Aggregate Size Classification.
17.3 Inerts between 4-mm and 9.5-mm—Remove,
15. Apparatus for Method C separate, and classify all pieces of plastic, metal, glass
15.1 Tweezer. and stones. Obtain and record the mass of inert class.
NOTE 2C—Stone removal will minimize damage to the Stein
15.2 Analytical Balance—1 mg to 1 kg. Mill carbide blade. Although the mass of stones is recorded,
15.3 Oven—forced air drying set at 70±5ûC. they are not considered in the “man-made inerts” class.

15.4 Weighing Trays—four (one for each inert class 17.4 Sieve the < 4-mm fraction (from step 17.2.1)
and stones). through a 2-mm sieve and analytically transfer
materials that pass through the 2-mm sieve to a
15.5 Sieves—2-mm, 4-mm, and 9.5-mm. separate, clean and sterile sample container.
15.6 Lab Tray—45 x 65 cm (18 x 26 in.) pressed 17.4.1 Transfer the remaining material (2-mm to 4-
fiberglass, or other smooth surfaced material. mm fraction) to a clean lab tray or other flat, smooth
15.7 Mechanical Shaker—for nested sieves, (e.g., surface and remove all sharps and stones. Weigh and
Tyler Model RX-86). record the mass of the removed sharps and stones.
16. Reagents and Materials for Method C 17.4.2 Recombine Inert-free Size Fractions—
Analytically recombine the stone-free 2-mm to 4-mm
16.1 Sample Containers—capable of retaining mass at
sieve fraction with the < 2 mm fraction. Analytically
temperatures near 75ûC, (e.g., 0.5-L rigid plastic
recombine this with the 4-mm to 9.5-mm fraction.
storage containers).
Transfer the recombined inert-free material to a clean
17. Procedure for Method C storage container and seal for other tests, (e.g., metals,
17.1 Sieve an adequate volume of as-received moist etc.).
bulk sample using the 9.5-mm sieve to generate a 250 17.5 Sieve fractions > 9.5-mm—These fractions
cm3 sample aliquot of < 9.5-mm material. include 9.5-mm to 16-mm, 16-mm to 25-mm, 25-mm to
17.1.1 Transfer approximately 250 cm3 of the 50-mm, and > 50-mm. Steps outlined below may be
material which passes the 9.5-mm sieve to a separate repeated for each size fraction.
clean container (minimum sample size of 250 cm3). 17.5.1 Place up to 250 cm3 of material into a tared
Obtain and record the gross fresh weight, (±0.001 g). container. Obtain and record the gross as-received
17.1.2 Set aside materials that do not pass through weight, (±0.01 g).
the 9.5-mm sieve for later processing (step 17.5). 17.5.2 Dry the sample in a forced air oven at 70±5°C
17.1.3 Air-dry the < 9.5-mm material in a vented for 8 h to 24 h, until weight change due to moisture loss
oven set at 36ûC. Continue to dry the sample until diminishes to nil. Obtain and record the gross oven-dry
weight loss diminishes to nil, (e.g., for approximately weight, (±0.01 g).
36 h to 48 h). Obtain and record the gross air-dry 17.5.3 Place the entire oven-dried aliquot onto a
weight of the 250-cm3 test aliquot. clean tray.
17.2 Separate sample by size fraction: 17.5.3.1 Remove separately with a tweezers, all
3
17.2.1 Sieve the 250-cm test aliquot of the air-dried plastic, metal, glass, sharps, (e.g., sewing needles,
material using a 4-mm sieve. Transfer material that straight pins and hypodermic needles, etc.), and

Test Methods for the Examination of Composting and Compost April 7, 2002
02.02-9
Sample Collection and Laboratory Preparation
Laboratory Sample Preparation for Analysis 02.02

recalcitrant wood chips, (e.g., bulking agents and other 18.3 Total Inerts from Bulk Sample—Multiply total
organic materials not readily degraded during the inerts from step 18.2 by the ratio for each
composting process). Stone removal is not necessary corresponding size fraction of interest, “i”, (from
unless the sample is to be milled. Method 02.02-B, Equation 14.2.1). Sum all fractions
17.5.3.2 Obtain and record the mass of each inert of interest.
class. IT = % [TIi × Ri] × 100 Equation 18.3
17.5.4 Optional—Repeat steps under 17.5 for each where:
sieve fraction. Air-dry and perform and inert counts for IT = total inerts in bulk sample, dry weight basis,
sieve fraction 9.5-mm to 16-mm, 16-mm to 25-mm, 25- 70±5°C, %,
mm to 50-mm, and > 50-mm. TI = percentage of total inerts by sieve size fraction “i”,
(decimal fraction from Equation 18.2), unitless,
18. Calculations for Method C i = sieve size fractions of interest, and
18.1 Ratio of Inert Plastics, Metal and Glass to R = ratio of each sieve size fraction “i”, relative to bulk
Sample by Size Fraction: sample determined in the sieve test. Refer to
Method 02.02-B, Equation 14.2.1.
Pi = IPi ÷ Si Equation 18.1.1
18.4 Total Recalcitrant Wood Chips—Multiply ratio
Mi = IMi ÷ Si Equation 18.1.2
of wood chips (W) from step 18.1 by corresponding
Gi = IGi ÷ Si Equation 18.1.3 size fraction ratio (from Method 02.02-B), sum all
Wi = Wi ÷ Si Equation 18.1.4 fractions values.
where: WT = % (Wi x Ri) × 100 Equation 18.4
i= sieve size fractions of interest, where:
IP = inert plastics weight, g, WT = total recalcitrant wood chips relative to bulk
IM = inert metals weight, g, sample, dry weight basis, %,
IG = inert glass weight, g, W = ratio of wood chips by sieve size fraction “i”,
W= wood chips, not to be considered as man-made (from Equation 18.1.4), unitless,
inerts, g, and i = sieve size fractions of interest, and
S = mass of sample for size fraction “i”, oven- or air- R = ratio of each sieve size fraction “i”, relative to bulk
dried basis, (e.g., 70°C or 36°C), g. sample determined in the sieve test, unitless. Refer
to Method 02.02-B, Equation 14.2.1.
18.1.1 Repeat calculations from step 18.1 for each
sieve size fraction of interest, “i”.
18.2 Total Inerts by Size Fraction:
TIi = [Pi + Mi + Gi] × 100 Equation 18.2
where:
TI = total inerts by size fraction of interest, “i”, %,
i= sieve size fraction of interest,
Pi = ratio of plastics in test aliquot, unitless,
Mi = ratio of metals in test aliquot, unitless,
Gi = ratio of glass in test aliquot, unitless.
18.2.1 Repeat the calculation for each sieve size
fraction of interest using Equation 18.2, “i”.

April 7, 2002 Test Methods for the Examination of Composting and Compost
02.02-10
Sample Collection and Laboratory Preparation
02.02 Laboratory Sample Preparation for Analysis

Test Method: Laboratory Sample Preparation. Milling and Grinding Samples, Units: NA
Harrison Method
Test Method Applications
Process Management Product Attributes
Step 1: Step 2: Step 3: Step 4: Step 5: Step 6: Step 7: Safety Market
Feedstock Feedstock Composting Odor Treatment Compost Curing Compost Compost Standards Attributes
Recovery Preparation Screening and Storing and
Refining Packaging
02.02-D 02.02-D 02.02-D 02.02-D

02.02-D MILLING AND GRINDING SAMPLES, HARRISON METHOD


COMMENT—This method is based upon procedures developed 21.1.2 Some compost constituents of interest can be
for yard waste compost THAT DO NOT CONTAIN INERT volatilized and lost by oven drying. Drying at 70±5°C
CONTAMINANTS - by Robert Harrison; College of Forest
Resources, University of Washington, Seattle, WA 98195. is designed to reduce volatilization. When
volatilization is considered to be a problem in sample
CAUTION—This method is not recommended for use on highly
heterogeneous samples nor on samples that require heavy metal analysis (volatile organic compounds, Hg, etc.), the
determinations. Refer to 02.02-E for a preferred sample milling samples should be ground and analyzed at as-received
technique, i.e., a protocol similar to that commonly employed moisture or air-dried at 36°C, as soon as possible after
on plant tissue samples. sampling. Strive to minimize lag times between
19. Apparatus for Method D sampling, preparation and analysis. Moisture content is
measured on a parallel sample to determine moisture
19.1 Mill—standard Wiley-type, large capacity, size
content and oven dry mass of the sample analyzed.
#4.
21.2 Wiley Mill Screen—A 30-mesh or smaller screen
19.2 Mortar and Pestle.
(<0.5-mm) is placed in the Wiley mill. The screen
20. Reagents and Materials for Method D should be clean and dry.
20.1 Water—type II deionized, minimum resistivity 21.3 The compost is fed into the Wiley mill chamber
of 17 M!·cm, minimum standard. slowly, removing large rock or metal pieces.
20.2 Alconox—mixed with tap water according to CAUTION—Care should be taken to avoid contamination of
samples with dust during this process (Piper, 1942).
manufacturer’s recommendations.
20.3 Methanol. 21.4 Rocks and Stones—If any rock particles are
found, these are first ground to a powder with a mortar
20.4 Hexane. and pestle (if possible), and then introduced into the
20.5 10% HNO3 Solution. Wiley mill chamber.
COMMENT—This will dull the blades, but is necessary to
21. Procedures for Method D produce a representative sample. Individual hard rock pieces
NOTE 2D—Generally, a minimum of 1 kg of compost is taken can be set aside analyzed individually if desirable.
initially as a primary sample.
21.5 Man-Made Inerts—Any large hard metal
21.1 Sample Drying—For analysis of non-volatile fragments, (e.g., steel, etc.) cannot presently be
compost components, compost is first dried at 70±5°C analyzed. However, these are generally not found in
for 24 h in a drying oven. The sample is removed, compost. If metal fragments are found, they can be set
allowed to cool for 1 h, weighed, and the weight aside and analyzed individually. Aluminum and steel
recorded. The sample is then returned to the drying cans and battery cases can generally be ground.
oven for an additional 24 h, removed, cooled and However, it is advisable to snip them into smaller
weighed again. If the sample weight changes less than pieces if they are larger than 0.5 inch in size.
0.1% over the 24 h period, the sample is considered to
21.6 Repeat Milling Steps 3×—The entire compost
be oven-dried at 70±5°C. Oven drying is not
sample is collected and thoroughly mixed by running it
absolutely necessary, but makes the sample much easier
through the Wiley mill a second and a third time.
to grind and equipment easier to clean.
21.7 Clean Wiley Mill—All surfaces contacting
21.1.1 This procedure is designed to remove
compost are cleaned by scrubbing with Alconox and
primarily water adsorbed in compost pores. Some
tap water, rinsed with tap water, rinsed with methanol,
compost samples may contain substances that continue
rinsed with hexane, rinsed with 10% HNO3 solution,
to volatilize over a period of time and continue to lose
rinsed with reagent grade water, and air dried.
weight. In such cases, the samples should be dried for
at least 24 h (2 cycles), and then the weight basis 21.8 Repeat the above grinding procedure for
reported, (e.g., as oven-dried at 75°C for 48 h). additional samples.

Test Methods for the Examination of Composting and Compost April 7, 2002
02.02-11
Sample Collection and Laboratory Preparation
Laboratory Sample Preparation for Analysis 02.02

Test Method: Laboratory Sample Preparation. Milling and Grinding Samples, Units: NA
Munter Method
Test Method Applications
Process Management Product Attributes
Step 1: Step 2: Step 3: Step 4: Step 5: Step 6: Step 7: Safety Market
Feedstock Feedstock Composting Odor Treatment Compost Curing Compost Compost Standards Attributes
Recovery Preparation Screening and Storing and
Refining Packaging
02.02-E 02.02-E 02.02-E 02.02-E

02.02-E MILLING AND GRINDING SAMPLES, MUNTER METHOD


NOTE 1E—This method emulates the protocol commonly 24.1 Milling Cup Preparation:
employed on plant tissue samples and is based on sample
preparation procedures developed by Robert Munter for mixed 24.1.1 Fill the aluminum mill cup to about one fourth
municipal solid waste (MSW) compost; University of to one third capacity.
Minnesota Research Analytical Laboratory, Department of Soil,
Water and Climate, St. Paul. 24.1.2 Lock in cup so it fits tightly in the position to
engage the safety switch.
22. Apparatus for Method E
24.1.3 Milling Time—1 min of milling time is
22.1 Plant Tissue Mill—equipped with tool steel adequate for achieving finely ground samples.
blade with 1 in carbide cutting edge and aluminum mill Additional milling contributes to erosion of metal from
cup (e.g., Stein Mill, model M-2, 15,000 rpm, ½ HP. the steel/carbide blade.
Fred Stein Laboratories, Inc., 121 N. 4th St.,
Atchinson, KS 66002). 24.2 Mill Sample—Turn the switch to ON.
22.2 Bottle—plastic, 250- or 300-mL, wide mouth. 24.3 Milled Sample Storage—Transfer the sample to
a wide mouth plastic bottle for storage and chemical
23. Reagents and Materials for Method E analysis: organic carbon, total nutrients (not including
23.1 None Required. N), and heavy metals.
24. Procedure for Method E 24.4 Clean Mill—It is imperative to remove all
sample residues from the mill and sample cup before
ATTENTION—A 250-mL aliquot of an air-dried working
sample is used for milling. The sample should be free from processing the next sample.
inerts and stones > 2 mm. Stones are removed from the sample Note 2E—Determinations for TN (optional), NO3, NH4, pH,
to protect the carbide blades of the mill, and for consistency of electrical conductivity, other water-soluble elements, biological
results. assays, respirometry, and pathogens screening are performed on
as-received moist compost test aliquots; milling may not be
practical with most as-received moist compost samples.

April 7, 2002 Test Methods for the Examination of Composting and Compost
02.02-12
Sample Collection and Laboratory Preparation
02.02 Laboratory Sample Preparation for Analysis

Test Method: Laboratory Sample Preparation. Feedstock Laboratory Sample Units: NA


Preparation Modifications
Test Method Applications
Process Management Product Attributes
Step 1: Step 2: Step 3: Step 4: Step 5: Step 6: Step 7: Safety Market
Feedstock Feedstock Composting Odor Treatment Compost Curing Compost Compost Standards Attributes
Recovery Preparation Screening and Storing and
Refining Packaging
02.02-F 02.02-F

02.02-F MODIFICATIONS FOR FEEDSTOCK SAMPLE PREPARATION


25. Significance of Method F 26.2.1 Working Sample—After completing all steps
and recording all measurements.
25.1 Feedstock sample fragment sizes and sample
heterogeneity are generally much larger than those of 26.2.1.1 Merge all size classes of feedstock
refined compost materials. For these reasons, materials.
laboratory preparation methods must be slightly 26.2.1.2 Thoroughly blend sample as outlined in
modified to compensate for these differences. 02.02-B.
25.2 As with a compost sample, feedstock sample 26.2.1.3 Subdivide sample by quartering until
heterogeneity is significantly decreased by thorough approximately 1 L of material is isolated.
milling or grinding of a large sample. This technique
improves the precision of elemental and chemical 26.2.1.4 Follow storage procedure as outlined.
analyses by homogenizing the sample aliquot selected 26.3 Method 02.02-C Man Made Inert Removal and
to represent the original feedstock blend. Mill and Classification:
homogenize at least 1000 cm3 of the feedstock sample. 26.3.1 Increase feedstock aliquot size for inert
25.3 Volatile loss of nutrients and other compounds removal to approximately 1,000 cm3 and follow the
may become significant with excessive handling during procedure as outlined.
sample homogenization. When volatile losses are an 26.3.2 Modify the procedures as necessary to
issue, sample preparation shall be performed in a cold compensate for the increased sample size. Document
room with a temperature of no more than 4°C to and report all extraordinary procedural modifications.
minimize volatile losses.
26.4 Methods 02.02-D and 02.02-E Milling and
26. Sample Handling and Procedural Grinding Sample:
Modifications for Feedstocks
26.4.1 Increase feedstock aliquot size for milling to
26.1 Method 02.02-A Sample Mixing and Splitting— at least 1,000 cm3 (1 L) and follow the procedure as
No Modification. Follow procedures as outlined. outlined.
26.2 Method 02.02-B Sample Sieving for Aggregate 26.4.2 Modify the procedures as necessary to
Size Classification—Modifications Required. Follow compensate for the increased sample size. Document
procedures as outlined. and report all extraordinary procedural modifications.

Test Methods for the Examination of Composting and Compost April 7, 2002
02.02-13
Sample Collection and Laboratory Preparation
Laboratory Sample Preparation for Analysis 02.02

02.02 SUMMARY
27. Report 27.6 Method 02.02-F Modifications for Feedstock
Sample Preparation—Report material type(s), method
27.1 Method 02.02-A Sample Mixing and Splitting—
selected for milling, sieve size distribution, inert
Report the mass of material received and its moisture
content of sample by fraction. Refer to specific method
content, wet basis.
for details.
27.2 Method 02.02-B Sample Sieving for Aggregate
Size Classification—Report the percentage of each 28. Precision and Bias
sieve fraction considered, % g g-1, and the moisture 28.1 Inert Plastics, Metal, Glass and Total Inerts:
content of each fraction. 28.1.1 Method 02.02-C Man Made Inert Removal
27.3 Method 02.02-C Man Made Inert Removal and and Classification—Precision of this test was
Classification—Report inerts relative to the bulk determined by the Research Analytical Laboratory,
sample, oven dried weight basis (70±5°C), % g g-1. Department of Soil, Water, and Climate; University of
27.3.1 Report percentages of inerts by inert type Minnesota for the MN-OEA CUP Project, 1993-1994.
relative to the bulk oven-dried sample. St. Paul, MN. Bias of this test has not been
determined. Data are being sought for use in
27.3.1.1 Combined film plastics and hard plastics developing a bias statement.
are reported as plastics without differentiating plastic
type. Film plastics are reported as unit area of film 28.1.1.1 Precision was determined using 10
plastics per unit volume of compost, cm2 m-3. Refer to subsamples taken from a field composite sample for
Method 03.05-A Film Plastic Surface Area each of three mixed municipal solid waste composting
Determinations Using Digital Processing. (MSW) facilities for two sampling periods in 1993.
27.3.1.2 Percent recalcitrant wood chip is reported Table 02.02-C1 Precision estimates for man-made inerts, (%CV for
as a percentage on an oven dried weight basis, % g g-1. plastics, metal, glass), in <6.3 mm air-dried mixed municipal solid
waste compost, 1993.
27.3.2 Report sum total inerts as a percentage of the Site Plastics Metal Glass Number of
bulk oven-dried sample. Samples
27.4 Method 02.02-D Milling and Grinding Samples, A 25 186 47 10
Harrison—Report method selected for milling, drying B 30 0 33 10
temperature and time (°C·h), sieve size fractions C 29 160 166 10
included in the milled sample, and the inert content of A 25 142 94 10
the milled sample. B 35 285 190 10
C 28 155 316 10
27.5 Method 02.02-E Milling and Grinding Samples,
Munter—Report method selected for milling, drying 29. Keywords
temperature and time (°C·h), sieve size fractions 29.1 milling; grinding; sieving; inerts; plastics; metal;
included in the milled sample, and the inert content of glass; stones; rocks; sieve size; particle size; moisture;
milled sample. oven-dried; air-dried; as-received; sample splitting;
sharps

April 7, 2002 Test Methods for the Examination of Composting and Compost
02.02-14
Physical Examination
03.01 Air Capacity

Test Method: Air Capacity. Three Methods. Units: % v v-1


Test Method Applications
Process Management Product Attributes
Step 1: Step 2: Step 3: Step 4: Step 5: Step 6: Step 7: Safety Market
Feedstock Feedstock Composting Odor Treatment Compost Curing Compost Compost Standards Attributes
Recovery Preparation Screening and Storing and
Refining Packaging
03.01-A 03.01-A 03.01-A 03.01-A
03.01-B 03.01-B 03.01-B
03.01-C 03.01-C 03.01-C 03.01-C 03.01-C

03.01 AIR CAPACITY


DISCLAIMERS ASTM D 2980-71, Standard Test Method for Volume
(1) The methodologies described in TMECC do not purport to address all
Weights, Water Holding Capacity, and Air Capacity of
safety concerns associated with their use. It is the responsibility of the Water-Saturated Peat Materials. In Annual Book of
user of these methods to establish appropriate safety and health ASTM Standards, Vol. 04.08. (Re-approved 1990).
practices, and to determine the applicability of regulatory limitations
prior to their use. Haug, Roger T., The Practical Handbook of Compost
(2) All methods and sampling protocols provided in TMECC are subject to Engineering, Lewis Publishers, 1993.
revision and update to correct any errors or omissions, and to Water holding Capacity, Volume Mass and Air Capacity of
accommodate new widely accepted advances in techniques and
methods. Please report omissions and errors to the U.S. Composting Water-Saturated Peat. ASTM D 2989-71. p 77. In Peat
Council Research and Education Foundation. An on-line submission Testing Manual. National Research Council of Canada,
form and instructions are provided on the TMECC web site, Technical Memorandum No. 125. 1979.
http://www.tmecc.org.
(3) Process alternatives, trade names, or commercial products as mentioned Laboratory Procedure for the Preparation of Solid Waste
in TMECC are only examples and are not endorsed or recommended by and Related Materials for Analysis. p 3. In Methods of
the U.S. Department of Agriculture or the U.S. Composting Council Solid Waste Testing. 1973. US EPA. Office of
Research and Education Foundation. Alternatives may exist or may be
developed.
Research and Monitoring. US EPA-6700-73-01, Part I.

1. Scope 3. Terminology
1.1 This section covers the measurement of moisture 3.1 air capacity, n—Proportion of the bulk volume of
content, volume weights (bulk density), porosity, water- compost, finished planting media, or soil that is filled
holding capacity, and air capacity (free air space) of with air at any given time or under a given condition.
compost materials. Compost, finished planting media, or soil with high air
capacity has the capacity to hold more water. Air
1.1.1 Method 03.01-A Quick-Test for Bulk Density, capacity is important in field application because it is
Porosity/Pore Space, Free Airspace and Water related to soil reconsolidation rates. Air capacity is
Holding Capacity of Compost (Unsieved) indicates the ability of a compost to resist water logging
1.1.2 Method 03.01-B Quick-Test for Bulk Density, and low oxygen levels.
Porosity/Pore Space, Free Airspace and Water 3.2 bulk density, n—Weight per unit volume of
Holding Capacity of Compost (Sieved) compost, calculated and reported on an oven dry
1.1.3 Method 03.01-C Field Density, Free Air Space weight basis, 70±5°C, w v-3.
and Water-Holding Capacity 3.3 free air space, n—Air-filled pore volume of an as-
1.2 Values stated in SI units are to be regarded as the received compost material, % v v-1.
standard. Values given in parentheses are provided for 3.4 porosity, n—Sum of water-filled pore volume plus
information only. air-filled pore volume, cm3.
2. Referenced Documents 3.5 pore space, n—Sum of water-filled pore volume
2.1 TMECC: plus air-filled pore volume relative to the overall
volume of the compost, % v v3.
Method 02.01-B Selection of Sampling Locations for
Windrows and Piles 3.6 water holding capacity, n—Percentage of water
Method 02.01-D Batch Feedstock Material Sampling filled pore volume relative to the total volume of water
Strategies saturated compost, % w w-1.
Method 03.09-A Total Solids and Moisture at 70±5°C 3.7 equivalency, n—at STP, 1 g of deionized water !
2.2 Other Sources: 1 cm3 of deionized water ! 1 mL of deionized water !
1 mL of air space ! 1 cm3 of air space.

Test Methods for the Examination of Composting and Compost August 12, 2001
03.01-1
Physical Examination
Air Capacity 03.01

4. Summary of Test Methods in accumulation of carbon dioxide and consequent


4.1 Method 03.01-A Quick-Test for Bulk Density, formation of anaerobic conditions; the latter lead to
Porosity/Pore Space, Free Airspace and Water odors from volatile organic acids, sulfides, and amines.
Holding Capacity of Compost (Unsieved)—A compost formation. Free airspace during odor treatment, if a
sample taken from the pile, as is, of known volume and biofilter is used, should be about 80-90%.
mass is transferred to a graduated beaker and bulk 5.2 Method 03.01-A Quick-Test for Bulk Density,
density is determined. The compost is saturated with Porosity/Pore Space, Free Airspace and Water
water and excess water is drained. Changes in compost Holding Capacity of Compost (Unsieved)—Quick-Test
volume and mass, and the ratio of water retained to determine volume weights (bulk density),
relative to the amount of drained water provide a means porosity/pore space, water-holding capacity, and air
for estimating compost bulk density, porosity/pore capacity (free air space) performed on unsieved, as-
water volumes and free airspace, and water holding received compost.
capacity. 5.2.1 This method provides a quick estimate for
4.2 Method 03.01-B Quick-Test for Bulk Density, compost bulk density, porosity/pore space percent, free
Porosity/Pore Space, Free Airspace and Water airspace percent, and water holding capacity.
Holding Capacity of Compost (Sieved)—A compost Approximately 5 h are required to complete a run,
sample taken from the pile, as is, of known volume, is whereas 24 h are required to perform the method
sieved and systematically transferred to a graduated described under Method 03.10-D Bulk Density, Water-
beaker and bulk density is determined. The compost is Holding Capacity, and Air Capacity of Compost
saturated with water and excess water is drained. Material, Modified ASTM D 2980-71.
Changes in compost volume and mass, and the ratio of 5.3 Method 03.01-B Quick-Test for Bulk Density,
water retained relative to the amount of drained water Porosity/Pore Space, Free Airspace and Water
provide a means for estimating compost bulk density, Holding Capacity of Compost (Sieved)—Quick-Test to
porosity/pore water volumes and free airspace, and determine volume weights (bulk density), pore space,
water holding capacity. water holding capacity, and air capacity (free air space)
4.3 Method 03.01-C Field Density, Free Air Space performed on sieved, as-received compost material.
and Water-Holding Capacity—Compost samples are 5.3.1 This method is identical to Method 03.01-A
systematically transferred to a bucket and weighed to with exception of an additional step in sample
approximate compost density. The bucket containing preparation which requires sample sieving (9.5-mm
the compost is filled with water and weighed; where the sieve).
volume equivalent of the added water is used to
approximate compost pore space. Then, the water is 5.4 Method 03.01-C Field Density, Free Air Space
drained and the remaining water-saturated compost is and Water-Holding Capacity—Field test using a
weighed to approximate the water-holding capacity of typical bucket provides an inexpensive, quick
the compost. approximation of density and porosity for feedstock
blends and in-process composting material for process
5. Significance and Use management. This field procedure is useful for
5.1 When large air spaces are present, high water evaluating the need for bulking agent.
penetration and aeration can occur. If average air space 6. Interference and Limitations
dimension diminishes and total air space remains
unchanged, retention of water increases and the 6.1 In-process compost sample moisture should range
potential for water penetration or flow decreases. from 45-60% (wet basis). Finished product compost
Water retention is greatest in humified materials that sample moisture should range from 40-50% (wet basis).
have small air spaces and low bulk density, whereas Excessively moist samples will compact during
water penetration and aeration is greater in poorly preparation, and inflate bulk density estimates and
humified compost with correspondingly larger air deflate percent free air space estimates. Excessively
spaces. Percent air space in compostable mixtures dry samples are often difficult to saturate with water
needs to be great enough to allow for maintenance of (sometimes hydrophobic) and may result in over-
aerobic condition. estimates of percent free air space.
CAUTION !—Excessively moist or dry initial in-process compost
5.1.1 Free airspace for composting should be greater samples may yield invalid results.
than 60% initially, and at least 35% during curing.
Free airspace less than 60% initially and 35% during 6.2 Three of the 03.01 Methods (A, B, C) do not use
curing inhibits air flow through the pile and will result vacuum to assist water extraction from water filled
pores (c.f. Method 03.10-D). Therefore, incomplete

August 12, 2001 Test Methods for the Examination of Composting and Compost
03.01-2
Physical Examination
03.01 Air Capacity

removal of free water (water-filled air space) from air 7.2 Method 03.01-B Quick-Test for Bulk Density,
pore space will deflate air capacity estimates and inflate Porosity/Pore Space, Free Airspace and Water
water-holding capacity estimates. Holding Capacity of Compost (Sieved)—Material used
6.3 6.3 Method 03.01-C Field Density, Free Air in this test should represent in-process compost product
Space and Water-Holding Capacity—This method uses at 45% - 60% moisture (wet weight basis). The sample
large aliquots and should be used as a rough guide to aliquot should be sieved through a 9.5-mm sieve, as-
generate approximations of sample bulk density, free received.
airspace, and water-holding capacity. 7.3 Method 03.01-C Field Density, Free Air Space
and Water-Holding Capacity—Material used in this
7. Sample Handling
test should represent in-process compost or feedstock
7.1 Method 03.01-A Quick-Test for Bulk Density, blends, moistened to attain 45-60% moisture content
Porosity/Pore Space, Free Airspace and Water (wet weight basis). The sample aliquots should not be
Holding Capacity of Compost (Unsieved)—Material sieved, but represent the particle and fragment size
used in this test should represent in-process compost distribution of the in-process materials in question.
product at 45-60% moisture (wet weight basis). The
sample aliquot should be unsieved, as-received.

Test Methods for the Examination of Composting and Compost August 12, 2001
03.01-3
Physical Examination
Air Capacity 03.01

Test Method: Air Capacity. Quick-Test for Bulk Density, Porosity/Pore Space, Units: % v v-1
Free Airspace and Water Holding Capacity of Compost
Test Method Applications
Process Management Product Attributes
Step 1: Step 2: Step 3: Step 4: Step 5: Step 6: Step 7: Safety Market
Feedstock Feedstock Composting Odor Treatment Compost Curing Compost Compost Standards Attributes
Recovery Preparation Screening and Storing and
Refining Packaging
03.01-A 03.01-A 03.01-A 03.01-A
03.01-B 03.01-B 03.01-B

03.01-A AND 03.01-B QUICK-TEST FOR BULK DENSITY, POROSITY/PORE SPACE,


FREE AIRSPACE AND WATER-HOLDING CAPACITY OF COMPOST
LOOK—Interference and Limitations, and Sampling Handling 9.2 Adhesive Tape—2.5 cm (1 in.) width masking, or
issues are presented as part of the introduction to this section.
equivalent.
CONTRIBUTED BY—This method is based upon procedures
developed for composting process monitoring and finished 10. Procedure for Methods A and B
compost by P.B. Leege and Melinda Miller.
10.1 Sample Oven Dry Weight Determination:
8. Apparatus for Methods A and B 10.1.1 Weigh and record tare weight of dry, open
8.1 Graduated Cylinder—two 1000-mL, for water 150-mL beaker using analytical balance, ±0.1 g.
addition. 10.1.2 Transfer a 50 cm3 aliquot of a parallel sample
8.2 Graduated Beaker with Handle—two 2000-mL. to a tared 150-mL open beaker.
8.2.1 Low-form polypropylene, straight-wall (not 10.1.3 Weigh and record the 50 cm3 aliquot gross as-
tapered). received weight (as received moisture) using analytical
8.2.2 Low-form polypropylene, straight-wall (not balance, ±0.1 g.
tapered), modified in the lab with four 0.3 mm (" in.) 10.1.4 Subtract open tare weight of dry open 150-mL
diameter holes drilled uniformly spaced through the beaker from 50 cm3 aliquot as-received gross weight,
bottom of the beaker at the low concave spots to ±0.01 g, (designate as A50).
promote uniform drainage from the beaker’s contents. 10.1.5 Oven dry the 50 cm3 aliquot in a forced air
8.3 Analytical Balance—top loading, high capacity, oven set at 70±5°C for 18-24 h. Weigh and record the
accurate to ±0.1 g with 0.1-1 kg range. oven-dry weight of 50 cm3 aliquot.
8.4 Drying Oven—forced air. 10.1.6 Subtract the tare weight of the dry, open 150-
8.5 Beaker—150-mL, Pyrex. mL beaker from the gross oven dry weight of the 50
cm3 aliquot to determine sample net oven dry weight,
8.6 Desiccator with Desiccant. ±0.01 g, (designate as O50).
8.7 Rubber Mat—closed-cell polyethylene foam mat, 10.2 Modified Graduated Beaker Preparation:
(4) 0.6-mm (¼-in.) layers stacked.
10.2.1 Drill four 3-mm ("-in.) uniformly spaced
8.8 Funnel—approximately 2.5-cm (~1-in.) diameter holes in the bottom of one 2000-mL beaker.
delivery stem, 15 cm (6 in.) mouth.
10.2.2 Temporarily cover and seal the drain holes of
8.9 Pan—25-cm (10 in.), stainless steel or brass the modified 2000-mL graduated beaker from the
(sieve catch beaker or equivalent). bottom side with 2.5 cm (1 in.) wide masking tape .
8.10 Sieve—stainless steel, 4 or 5 cm mesh (1.5 or 2 Press tape down securely to prevent leakage.
in.), or equivalent metal platform. 10.3 Weigh and record the tare weight of the taped,
8.11 Timer—with alarm. dry, empty modified 2000-mL graduated beaker, ±0.01
8.12 Watch glass—5-cm (2-in.) diameter, or parafilm g.
to cover beaker and graduate cylinder. 10.4 Fill Graduated Beaker with Compost:
9. Reagents and Materials for Methods A and B 10.4.1 Transfer a 600 cm3 aliquot of as-received
compost into the modified 2000-mL graduated beaker
9.1 Water—type II deionized, 17 M#·cm minimum
through the funnel.
resistivity.
NOTE 1A—To ensure uniform packing of compost throughout
the modified graduated beaker, allow beaker containing

August 12, 2001 Test Methods for the Examination of Composting and Compost
03.01-4
Physical Examination
03.01 Air Capacity

compost to fall freely onto a rubber mat once from height of 15 10.7.4 After 30 min cover drain holes with masking
cm (6 in.). Carefully maintain the beaker in an upright position
tape. Slowly and carefully saturate compost sample by
at all times.
pouring water from catch beaker back onto compost
10.4.2 Repeat the filling with 600 cm3 and free filled modified 2000-mL graduated beaker.
falling operation, two more times (three times total).
NOTE 2A—Do not add excess water, avoid water pooling at
After the third free-fall drop, fill the graduated beaker sample surface.
to volume with sample material, 1800 mL. Do not
10.7.5 Repeat this operation at least three times using
repeat free-fall drop after topping off. Topping off
the captured drainage water to ensure that compost
should be limited to 2-3 cm.
sample air spaces fill with water during wetting
10.5 As-Received Sample Weight Determination: process.
10.5.1 Weigh and record gross weight of taped, 10.7.6 Add small volumes of as-received deionized
modified 2000-mL graduated beaker containing 1800 water from 1000 mL cylinder (see step 10.6.6) as
cm3 of as-received compost, ±0.01 g. necessary if recycled drainage water from catch beaker
10.5.2 Subtract initial tare weight of taped, modified fails to re-saturate sample.
2000-mL graduated beaker from weight of taped, 10.7.7 Set aside the covered catch beaker without
modified 2000-mL graduated beaker containing 1800 drying for later use.
cm3 as-received compost, (designated as A1800). NOTE 3A— Previously unfilled pores will fill with water. The
10.6 Saturate Sample with Water: total volume of water needed to saturate sample represents
sample pore space. After saturation is reached, no pockets of
10.6.1 Saturate compost sample slowly and carefully trapped air should be visible.
by pouring deionized water onto compost in the NOTE 4A—Carefully monitor volume of water needed to re-fill
graduated beaker with 1000-mL graduated cylinder. modified graduated beaker. During refilling, systematic water
loss will occur. The amount of water lost may be minimized by
10.6.2 Continue pouring until the top face of using very clean equipment.
compost in the 2000-mL graduated beaker glistens with
NOTE 5A—Sample compaction may occur with mature
free water; be careful not to add excess water. composts. If recycled drainage water is not reabsorbed after
10.6.3 Cover the modified 2000-mL graduated allowing a saturated sample to rest, subtract excess volume of
water from initial water volume needed to saturate compost.
beaker using a watch glass or parafilm and allow wetted Avoid pooling water at sample surface. When excess water is
compost sample to rest for approximately 5 min. retained to avoid over saturation of sample, subtract volume of
excess deionized water (from Step 10.7) from initial volume of
10.6.4 Repeat water addition with 5-min rest periods
water (from Step 10.6). Sample expansion may occur with
until water is no longer absorbed and the compost immature, unstable composts. If recycled drainage water is
surface glistens with a film of free water. Do not add completely reabsorbed after allowing saturated sample to rest,
excess water; avoid pooling at sample surface. add additional water to saturate compost sample. Add water to
initial water volume to saturate compost sample. When water is
10.6.5 Read and record volume of water required to needed to saturate sample, sum volume of added (from Step
saturate compost sample from 1000-mL graduated 10.7) and initial volume of water (from Step 10.6).
cylinder, ±5 mL. 10.8 Water-Saturated Weight and Volume before
10.6.6 Set aside 1000-mL cylinder with any Draining:
remaining water for later use. 10.8.1 Weigh and record gross weight of taped,
10.7 Pore Space Estimate: modified graduated beaker containing water and water-
saturated compost, ±0.01 g.
10.7.1 Place modified graduated beaker containing
water saturated compost upright onto a 3.8 or 5 cm (11/2 10.8.2 Subtract initial tare weight of taped, graduated
or 2 in.) grate atop the unmodified 2000-mL graduated beaker from weight of taped, modified graduated
beaker with handle, or equivalent setup to catch beaker containing water and water-saturated compost,
drainage from bottom of the modified 2000-mL (W1800 WS, no drain), g.
graduated beaker. 10.8.3 Read and record the volume of water-
10.7.2 Holding the modified 2000-mL graduated saturated compost in beaker, (designate as V1800WS, no
beaker over the water catch stand, remove masking tape drain), mL.
from bottom of the beaker to allow water to drain from NOTE 6A—Verify total volume of water added (from Step 10.7)
the saturated compost beaker into catch beaker. by comparing the difference between initial sample weight
(from Step 10.5) and sample weight at saturation (from Step
10.7.3 Capture drained water in catch beaker for 10.8).
reuse.

Test Methods for the Examination of Composting and Compost August 12, 2001
03.01-5
Physical Examination
Air Capacity 03.01

10.9 Drain Cylinder: 11.5 Pore Space Percent (PS, %):


10.9.1 Drain off water into catch beaker for the last PS = PSV ÷ 1800 × 100 Equation 11.5
time through drainage holes and allow sample to rest 11.6 Free Airspace Volume, Mass Equivalent Method
and continue to drain for 4 h. (FASVme):
10.9.1.1 Cover the modified 2000-mL graduated FASVme = W1800 WS, nd - W1800 WS, after drain Equation 11.6
beaker to minimize evaporative water loss during the 4 11.7 Free Airspace Percent (FAS, %):
h final drain period. FAS = FASVme ÷ V1800 × 100 Equation 11.7
10.9.1.2 Capture drainage water in the catch beaker. 11.8 Water Holding Capacity (WHC):
10.9.2 Read and record net volume of drainage water 11.8.1 Percent water holding capacity, volume basis:
released from compost during the 4-h draining period, WHCV = PS - FAS Equation 11.8.1
±0.01 g, combined with water already in catch beaker.
11.8.2 Percent water holding capacity, mass basis:
10.10 Determine Water-Saturated Weight After 4-h WHCM = [W1800 WS, ad – O1800] ÷ O1800 × 100
Draining: Equation 11.8.2
10.10.1 Weigh and record the mass of taped, where:
modified graduated beaker and water-saturated A50 = as-received sample weight of 50 mL aliquot (as
compost, ±0.01 g. received), g, (step 10.1.4),
10.10.2 Subtract initial tare weight of graduated O50 = oven dry weight of 50 mL aliquot, g, (step 10.1.5),
beaker from the weight of beaker containing water- A1800 = initial weight of 1800 cm3 (mL) sample (as
saturated compost, g. (designate as W1800 WS, after drain) received), g, (step 10.5.2),
O1800 = calculated oven dry weight of 1800 cm3 (mL)
NOTE 7A—Compare and verify free airspace volume
determination by dividing volume of drainage water (from Step
sample, g, (step 11.1),
10.9) by total volume of water added to saturate compost W1800 WS, nd = weight of water-saturated compost before final
sample (from Steps 10.7 and 10.8). 4 h draining, g, (step 10.8.2),
10.11 Water-Saturated Volume—Read and record W1800 WS, ad = weight of water-saturated compost after final 4
volume of wetted compost in modified graduated h draining, g, (step 10.10.2),
beaker, ±5 mL. V1800 = initial volume of compost in cylinder (1800 cm3),
mL ! cm3,
10.12 Perform Calculations. V1800 WS, nd = volume of water-saturated compost before final
11. Calculation for Methods A and B 4 h draining, g, (step 10.8.3),
PSV = pore space volume, mL,
11.1 Sample Oven Dry Weight (O1800):
FASVme = free airspace volume using mass equivalents,
O1800 = A1800 × (O50 ÷ A50) Equation 11.1 1 mL ! 1 g,
11.2 Moisture Content (M1800): FASVvm = free airspace volume using volume measures,
M1800 = A1800 × [1 - (O50 ÷ A50)], or Equation 11.2.1 1 mL ! 1 cm3,
M1800 = A1800 - O1800 Equation 11.2.2 BD = bulk density, g cm-3,
PS = pore space, % v v-1,
11.3 Bulk Density (BD):
FAS = free airspace, % v v-1,
BD = O1800 ÷ V1800 Equation 11.3
WHCV = water holding capacity, % v v-1, and
11.4 Pore Space Volume (PSV) WHCM = water holding capacity, % w w-1.
PSV = W1800 WS, nd - O1800 + (1800 - V1800 WS, no drain)
Equation 11.4
3
NOTE 8A—Assume that 1 g of deionized water ! 1 cm of
deionized water ! 1 mL of deionized water ! 1 mL of air space.

August 12, 2001 Test Methods for the Examination of Composting and Compost
03.01-6
Physical Examination
03.01 Air Capacity

Test Method: Air Capacity. Field Density, Free Airspace and Water-Holding Units: See Calculations
Capacity
Test Method Applications
Process Management Product Attributes
Step 1: Step 2: Step 3: Step 4: Step 5: Step 6: Step 7: Safety Market
Feedstock Feedstock Composting Odor Treatment Compost Curing Compost Compost Standards Attributes
Recovery Preparation Screening and Storing and
Refining Packaging
03.01-C 03.01-C 03.01-C 03.01-C 03.01-C 03.01-C 03.01-C

03.01-C FIELD DENSITY, FREE AIRSPACE AND WATER-HOLDING CAPACITY


LOOK—Interference and Limitations, and Sampling Handling NOTE 1C—It may be acceptable to dry the parallel sample
issues are presented as part of the introduction to this section. aliquot at 105°C to decrease the required drying time. Absolute
accuracy of total solids content is not always critical for process
12. Apparatus for Method C management.
12.1 pail—20-L (5-gal), plastic with lip and vertical 14.2 Preparation of Equipment:
walls, fitted with hoop-type handle.
14.2.1 Subdivide the pail into three equal volumes.
12.2 scale—20 kg, accurate to ±50 g. Measure from the inside bottom to the top rim of the
12.3 rule—tape measure or ruler. pail; make a series of four or five marks spaced around
the inside circumference of the pail with the marking
12.4 adhesive tape—1.3 cm (½ in.) width, brightly pen to highlight each of two equally-spaced divisions;
colored such as blue masking tape. refer to the illustration in Fig 03.01-C.
12.5 marking pen—dark colored. 14.2.2 Place a band of brightly colored tape over
12.6 surface—firm, flat, such as cement or pavement. each of the two highlighted divisions on the inside
12.7 cheese cloth—60 x 60 cm (24 x 24 in.) square, circumference of the pail.
or other equivalent material to serve as a strainer or
sieve.
12.8 strap—90-cm (~3-ft) segment of wire, rope or 1/
3

cord to secure strainer or sieve over mouth of pail.


12.9 grate—to facilitate unobstructed drainage of
1/
pail. 3

12.10 graduated cylinder—1000-mL, plastic or glass.


1/
13. Reagents and Materials for Method C 3

13.1 water—20 L (5 gal), tap water


14. Procedure for Method C Fig 03.01-C Sample pail with three equal subdivisions.
14.1 Collect a composite sample of compost as
14.2.3 Obtain the tare weight of the pail. Measure
described in TMECC 02.01-B Selection of Sampling
and record the dry mass of the empty pail.
Locations for Windrows and Piles, or blended
feedstocks as described in TMECC 02.01-D Batch 14.2.4 Determine volume capacity of the pail (m3).
Feedstock Material Sampling Strategies. Fill the pail to the brim with water. Measure and
record the weight of the water-filled pail.
14.1.1 When performing this test on a feedstock
Alternatively, fill the pail using the 1000 graduated
blend, be sure to thoroughly mix the feedstocks before
cylinder and record the volume of water used.
collecting a composite sample.
ASSUMPTION—1000 L of H2O ! 1000 kg of H2O ! 1.000 m3 of
14.1.2 Determine total solids content on a parallel H2O; 1 Lb of H2O ! 5.94×10-4 yd3 ! 4.54×10-4 m3
sample aliquot of the test material as described in
TMECC 03.09 Total Solids and Moisture at 70±5°C.

Test Methods for the Examination of Composting and Compost August 12, 2001
03.01-7
Physical Examination
Air Capacity 03.01

14.3 Bulk Density: 15. Calculations for Method C


14.3.1 Transfer a first aliquot of material from the 15.1 Bulk Density Estimate at Field Moisture:
composite sample to fill the lowest third of the pail to A = [(B - C) ÷ (D - C)] Equation 15.1
the lower band of tape. where:
14.3.2 Systematically compact the sample aliquot. A = bulk density estimate, kg m-3 dw (Lb yd-3) basis,
Drop the sample pail onto a firm flat surface ten times B = mass of the compost-filled pail (step 14.3.6), kg
from a height of 15 cm (6 in.). Using the pail handle, (Lb),
carefully guide each 15-cm pail-drop to ensure that the C = mass of the empty pail (step 14.2.3), kg (Lb), and
pail remains upright and does not tilt or tip upon D = volume of the water-filled pail (step 14.2.4), m3
impact. (yd3).
CONVERSION FACTORS:
14.3.3 Transfer a second aliquot of material from the DImperial 5-gal = 0.022730 m3, and
composite sample to fill the second third of the pail to DUS 5-gal = 0.024755 yd3.
the upper band of tape; repeat the compaction ASSUMPTION—1000 L of H2O ! 1000 kg of H2O ! 1.000 m3 of
procedure (step 14.3.2). H2O; 1 Lb of H2O ! 5.94×10-4 yd3 ! 4.54×10-4 m3
14.3.4 Transfer a third aliquot of material from the 15.2 Free Air Space Estimate by Weight at Field
composite sample to fill the pail to the brim; repeat the Moisture:
compaction procedure (step 14.3.2). A = [(B - C) ÷ (B - D)] × 100 Equation 15.2
14.3.5 Transfer a forth and final aliquot of material where:
from the composite sample to fill the pail to the brim; A = pore space, w w-1, %,
the pail should be completely filled with sample B = mass of the water/compost-filled pail (step 14.4.3),
material; DO NOT COMPACT THE FORTH ALIQUOT. kg (Lb)
14.3.6 Measure and record the mass of the filled pail. C = mass of compost-filled pail (step 14.3.6), kg (Lb),
and
14.4 Free Air Space: D = mass of the empty pail (step 14.2.3), kg (Lb)
14.4.1 Mass based Method—Fill the pail containing 15.3 Free Air Space Estimate by Volume:
the density sample (from step 14.3) with tap water. A = (B ÷ C) × 100 Equation 15.3
14.4.2 Alternate Volume based Method—Transfer where:
tap water into the compost-filled pail using the 1000 A = free air space, v v-1, %,
mL graduated cylinder. Record the volume water B = volume of water added to compost-filled pail (from
required to fill the pail to the brim. step 14.4.1 or 14.4.2), mL, and
14.4.3 Measure and record the mass of the C = volume of water-filled pail (step 14.2.3), mL
compost/water filled pail. CONVERSION FACTORS:
CImperial 5-gal = 22.73046 L, or 22730 mL, and
14.5 Water-Holding Capacity: CUS 5-gal = 18.92706 L, or 18927 mL.
14.5.1 Allow the sample to rest for three h, to allow 15.4 Water-Holding Capacity Estimate by Weight:
the tap water to absorb into the moist, compacted A = [(B - C) - (D - C) × E] ÷ [(D - C) × E]
sample material. Equation 15.4
14.5.2 Cover the mouth of the pail with cheese cloth where:
or other material to function as a filter and securely A = water-holding capacity, kg kg-1 (Lb Lb-1), %,
fasten the filter over the lip of the pail mouth. B = mass of the water-saturated compost-filled pail
(step 14.5.4), kg (Lb),
14.5.3 Invert the water-filled pail onto the elevated C = mass of empty pail (step 14.2.3), kg (Lb),
grate to drain free water from the saturated material.
D = mass of the compost-filled pail (step 14.3.6), kg
Allow to drain for 24 hr. (Lb), and
14.5.4 Remove the filter cloth; measure and record E = total solids ratio (step 14.1.2), unitless.
the combined mass of the pail and water-saturated
compost.

August 12, 2001 Test Methods for the Examination of Composting and Compost
03.01-8
Physical Examination
03.01 Air Capacity

03.01 METHODS SUMMARY


16. Report percentage, %, w w-1, wet weight basis as determined
by forced-air oven-drying at 70±5°C.
16.1 Free Air Space—Express free air space as a
percentage, volume of free air space per unit volume of 17. Precision and Bias
compost (%, v v, ±0.1 %). 17.1.1 Air Capacity, Bulk Density, Water-Holding
16.2 Bulk Density—Express bulk density as mass per Capacity: The precision and bias of the tests (Methods
unit volume of compost on an as-received moisture 03.01 A, B, C) have not been determined. Data are
basis to the nearest ±0.1 w v-3 (kg m3, or Lb yd3). being sought for use in developing a precision and bias
statements.
16.3 Water-Holding Capacity—Express water-
holding capacity as a percentage of the volume (mass 18. Keywords
equivalent) of water retained per unit mass of compost 18.1 air capacity; air space; bulk density; free
(dw basis) to the nearest ±0.1 %, w w-1. airspace; porosity; pore space; water-holding capacity;
16.4 Moisture Content or Total Solids—Report as- field density; field porosity; field test; bucket test
received moisture or total solids content as a

Test Methods for the Examination of Composting and Compost August 12, 2001
03.01-18-9
Physical Examination
Air Capacity 03.01

August 12, 2001 Test Methods for the Examination of Composting and Compost
03.01-10
Physical Examination
03.02 Ash

Test Method: Ash. Three Methods. Units: % g g-1 dw


Test Method Applications
Process Management Product Attributes
Step 1: Step 2: Step 3: Step 4: Step 5: Step 6: Step 7: Safety Market
Feedstock Feedstock Composting Odor Treatment Compost Curing Compost Compost Standards Attributes
Recovery Preparation Screening and Storing and
Refining Packaging
03.02-A 03.02-A 03.02-A 03.02-A
03.02-B 03.02-B
03.02-C

03.02 ASH
DISCLAIMERS
Monitoring and Support Laboratory, Cincinnati, OH
45268.
(1) The methodologies described in TMECC do not purport to address all
safety concerns associated with their use. It is the responsibility of the SM 2540-E, Fixed and Volatile Solids Ignited at 500°C.
user of these methods to establish appropriate safety and health In Standard Methods for the Examination of Water and
practices, and to determine the applicability of regulatory limitations
prior to their use.
Wastewater. Part 2000, Physical and Aggregate
(2) All methods and sampling protocols provided in TMECC are subject to
Properties. 18th edition. 1992.
revision and update to correct any errors or omissions, and to US EPA Method 600/4-79-020, adapted by physical
accommodate new widely accepted advances in techniques and
removal of volatile solids that are not readily
methods. Please report omissions and errors to the U.S. Composting
Council Research and Education Foundation. An on-line submission biodegradable.
form and instructions are provided on the TMECC web site,
http://www.tmecc.org. 3. Terminology
(3) Process alternatives, trade names, or commercial products as mentioned 3.1 ash, n—The inorganic matter, or mineral residue
in TMECC are only examples and are not endorsed or recommended by
the U.S. Department of Agriculture or the U.S. Composting Council of total solids that remains when a compost or
Research and Education Foundation. Alternatives may exist or may be feedstock is combusted at 550°C in the presence of
developed.
excess air; equivalent to fixed solids, % g g-1.
1. Scope 3.2 biodegradable volatile solids, n—The organic
1.1 This section covers the measurement of ash matter fraction; the biodegradable portion of total
content and volatile solids content for compost solids that volatilizes to carbon dioxide and other
materials and feedstocks. gasses when a compost or feedstock is combusted at
1.1.1 Method 03.02-A Unmilled Material Ignited at 550°C in the presence of excess air, % g g-1.
550°C without Inerts Removal. 3.3 fixed solids, n—The inorganic matter, or mineral
1.1.2 Method 03.02-B Milled Material Ignited at residue of total solids that remains when a compost or
550°C with Inerts Removal. feedstock is combusted at 550°C in the presence of
excess air; equivalent to ash, % g g-1.
1.1.3 Method 03.02-C Unmilled Material Ignited at
550°C with Inerts Removal. 3.4 moisture content, n—The liquid fraction
(percentage) of a compost or feedstock that evaporates
1.2 Values stated in SI units are to be regarded as the at 70±5°C, % g g-1.
standard. Values given in parentheses are provided for
information only. 3.5 total solids, n—The solid fraction (percentage) of
a compost or feedstock that does not evaporate at
2. Referenced Documents 70±5°C, which consists of fixed solids, biodegradable
2.1 TMECC: volatile solids, and volatile solids that are not readily
Method 03.09-A Total Solids and Moisture. biodegradable, % g g-1.
Method 05.01 Biodegradable Volatile Solids. 3.6 volatile solids, n—The sum of biodegradable
Method 05.07-A Loss-on-Ignition Organic Matter. materials, non-biodegradable materials, and
biodegradable materials that do not degrade during the
2.2 Other References:
retention time allowed for composting, that volatilize to
Cohen, I.R. 1973. Laboratory Procedure for the carbon dioxide and other gasses when a compost or
Preparation of Solid Waste Related Materials for feedstock is combusted at 550°C in the presence of
Analysis. In Methods of Solid Waste Testing, EPA- excess air, % g g-1.
6700-73-01. US EPA, Cincinnati, OH.
Methods for the Evaluation of Water and Wastewater,
EPA 0600/4-79-020, US EPA, Environmental

Test Methods for the Examination of Composting and Compost August 12, 2001
03.02-1
Physical Examination
Ash 03.02

4. Summary of Test Methods 5.2.1 Organic Matter (OM), which is occasionally


4.1 Method 03.02-A Unmilled Material Ignited at referred to as Biodegradable Volatile Solids (BVS);
550°C without Inerts Removal—Quick-Test to 5.2.2 Ash or fixed solids (Ash, inorganic matter, or
determine moisture and total solids content at 70±5°C, minerals); and
and total ash and volatile solids content by combustion 5.2.3 Volatile Solids that are not readily
at 550°C in the presence of excess air and reported on biodegradable (VS).
an oven dried basis of an unsieved, as-received finished
or in-process compost or feedstock sample. 6. Interference and Limitations
4.1.1 This test is recommended for samples where no 6.1 Biodegradable volatile solids (organic matter) is
consideration need be given to inert materials and determined on a compost sample that is sieved and
biodegradable materials that do not degrade during the whose inert contaminants are removed, i.e., during inert
retention time allowed for composting. classification. Samples must be thoroughly blended
and properly split (subdivided) prior to drying, milling
4.2 Method 03.02-B Milled Material Ignited at
and inert removal. Unmilled coarse samples are almost
550°C with Inerts Removal—Analytical test to
always more variable than finely milled samples. A
determine biodegradable volatile solids contents
small aliquot of milled material will more closely
(organic matter) by combustion at 550°C in the
resemble the bulk milled sample than will a small
presence of excess air and reported on an oven-dried
aliquot of unmilled coarse material.
basis from an air-dried (36°C), sieved and milled
compost sample from which non-biodegradable or 6.1.1 The presence of materials that are not readily
biodegradable materials that do not readily humify have biodegradable such as wood chips and man-made inerts
been removed. such as plastics cause over estimation of the sample
biodegradable volatile solids.
4.2.1 This test method provides an estimate of
biodegradable volatile solids. Compensation for inert 6.1.2 The presence of man-made inerts such as metal
materials and biodegradable materials that do not and glass cause over estimation of the sample ash
degrade during the retention time for composting prior content.
to combustion is accomplished by their removal 6.2 Volatile residues may accumulate on glass
through sample preparation prior to performing this surfaces when ashing temperatures are too low
test. (<500°C) and/or the duration of the ashing process is
4.3 Method 03.02-C Unmilled Material Ignited at too short. If volatile residues accumulate on the ashing
550°C with Inerts Removal—A test to determine vessel, the volatile solids determination will be low.
moisture and total solids content at 70±5°C, 6.3 A sample is oven dried at 70±5°C rather than
biodegradable volatile solids content (organic matter) 105°C, to minimize volatile loss of carbon compounds
by combustion at 550°C in the presence of excess air during determinations of total solids. The significance
and reported on an oven-dried basis of a sieved, as- of this error increases with increasingly mature
received finished or in-process compost, or feedstock materials where the relative volatile solids measure
sample. diminishes to less than ten percent the total solids.
4.3.1 The test employs a calculated weighting 6.4 Negative errors in volatile solids can be produced
method to compensate for inert materials and for through the loss of volatile matter from samples that
biodegradable materials that do not degrade during the require prolonged drying at relatively high
retention time allowed for composing. temperatures. This error may become significant with
5. Significance and Use feedstock where total solids is very high relative to
volatile solids. If this condition exists, consider
5.1 Carbon dioxide and other gasses are evolved measuring for quantities of suspect volatile components
when the biodegradable volatile solids portion (organic by another test, such as the total organic carbon test
matter) of material is combusted at 550°C. The ash (Method 04.01).
residue is mineral fraction of compost that remains in
the fixed solids, or inorganic content of total solids. 7. Sample Handling
5.2 Biodegradable volatile solids (organic matter) and 7.1 Method 03.02-A Unmilled Material Ignited at
ash content in feedstock and compost are two of three 550°C without Inerts Removal—Perform this test on a
material categories in total solids, or dry matter. Total feedstocks, in-process and finished composts. The
solids, or dry matter include: material may contain unclassified inert material. This

August 12, 2001 Test Methods for the Examination of Composting and Compost
03.02-2
Physical Examination
03.02 Ash

test should be implemented as the standard for the and materials >2 mm not readily biodegradable
Volatile Solids Reduction test (Test Method 05.10-A). removed from the sieved material, and milled to a fine
7.1.1 Compost Samples—This test is best performed powder texture.
in conjunction with the total solids and moisture test. 7.2.1 Material for this test should conform to the
Use the same sample for volatile solids determination marketing specifications established for compost
(50 cm3 aliquot of prepared material). product distribution.
7.1.2 Feedstocks Samples—Increase sample size to 7.3 Method 03.02-C Unmilled Material Ignited at
400 cm3 for feedstock sample analysis. This test is best 550°C with Inerts Removal—Perform this test on 50
performed in conjunction with the total solids moisture cm3 aliquot of material screened through a 9.5 mm
test. Use the same sample for volatile solids sieve, oven-dried at 70±5°C, with man-made inerts and
determination (400 cm3 aliquot of prepared material). materials not readily biodegradable removed from the
7.2 Method 03.02-B Milled Material Ignited at sieved material.
550°C with Inerts Removal—Perform this test with a 7.3.1 Material for this test should conform to the
250 cm3 aliquot of material screened through a 9.5-mm marketing specifications established for compost
sieve, air-dried at 36°C, with man-made inerts >2 mm product distribution.

Test Methods for the Examination of Composting and Compost August 12, 2001
03.02-3
Physical Examination
Ash 03.02

Test Method: Ash. Unmilled Material Ignited at 550°C without Inerts Removal Units: % g g-1 dw
Test Method Applications
Process Management Product Attributes
Step 1: Step 2: Step 3: Step 4: Step 5: Step 6: Step 7: Safety Market
Feedstock Feedstock Composting Odor Treatment Compost Curing Compost Compost Standards Attributes
Recovery Preparation Screening and Storing and
Refining Packaging

03.02-A 03.02-A 03.02-A 03.02-A

03.02-A UNMILLED MATERIAL IGNITED AT 550°C WITHOUT INERTS REMOVAL


LOOK—Interference and Limitations, and Sampling Handling 10.3 Ash Weight:
issues are presented as part of the introduction to this section.
10.3.1 Place the watch glass, concave side facing up,
8. Apparatus for Method A on top of the beaker and transfer it to the forced-air
8.1 Balance—analytical, with accuracy of ±0.001 g. muffle furnace; slowly ramp furnace temperature to
550°C, ash at 550°C for 2 h, and then slowly ramp
8.2 Furnace—forced air muffle, set at 550°C.
furnace temperature to approximately 200°C.
8.3 Evaporation Dish—Pyrex beaker, use 150-mL
10.3.2 Transfer beakers containing ashed samples to
beaker with compost samples, and 500-mL beakers
a desiccator and cool to approximately 27°C.
with feedstocks.
10.3.3 Weigh and record gross weight of beaker and
8.4 Watch Glass—2.5 cm (2 in.) diameter for
sample (AshW).
compost, or 5 cm (4 in.) diameter for feedstock.
10.4 Calculations—determine ash content (fixed
8.5 Desiccator Cabinet—vacuum with desiccant tray
solids) and volatile solids content.
containing a color indicator of moisture concentration
or an instrument indicator. 11. Calculations for Method A
9. Reagents and Materials for Method A 11.1 Calculate Total Solids and Moisture content as
percentages as-received wet weight basis:
9.1 None required.
TS = (dw ÷ ARW) × 100 Equation 11.1.1
10. Procedure for Method A M= [1 – (dw ÷ ARW)] × 100 Equation 11.1.2
10.1 Preparation of Evaporating Dish: where:
10.1.1 Heat a clean beaker or crucible to 105°C for TS =total solids, % g g-1,
0.5 h to 1.0 h to drive off all hygroscopic moisture. M= percent moisture, % g g-1,
dw =sample net oven-dried weight determined at
10.1.2 Place heated beaker in desiccator cabinet to 70±5°C, ±0.001 g, and
keep it dry, and allow to cool to approximately 27°C.
ARW = sample net weight at as-received moisture, ±0.001
10.1.3 Record tare weight immediately prior to use. g.
10.2 Determine Initial Sample Weight: 11.2 Calculate organic matter (OM) and ash (Ash)
content as percentages of total solids on an oven dry
10.2.1 Place sample beaker in forced-air oven set at
weight basis:
70±5°C for approximately 18 h – 24 h, until weight
change and moisture loss diminishes to nil. Ash = (AshW ÷ dw) × 100 Equation 11.2.1
3 VS = [1 – (AshW ÷ dw)] × 100 Equation 11.2.2
10.2.2 Transfer 50 cm of oven-dried compost to the
where:
150-mL beaker. For feedstocks, transfer approximately
Ash = percentage of solids at 550°C, % g g-1,
400 cm3 of oven-dried material to a 500-mL beaker.
VS = percentage of solids volatilized at 550°C, % g g-1,
10.2.2.1 Disregard the mass of inerts when using dw = net oven-dry weight at 70±5°C, ±0.001 g, and
this method. AshW = net ash weight at 550°C, ±0.001 g.
10.2.3 Weigh and record gross weight of beaker and
COMMENT—As compost becomes increasingly humified
sample, subtract beaker weight from gross weight to (biological degradation), the relative content of biodegradable
determine net weight of the oven-dried sample (dw). volatile solids approaches zero.

August 12, 2001 Test Methods for the Examination of Composting and Compost
03.02-4
Physical Examination
03.02 Ash

Test Method: Ash. Milled Material Ignited at 550°C with Inerts Removal Units: % g g-1 dw
Test Method Applications
Process Management Product Attributes
Step 1: Step 2: Step 3: Step 4: Step 5: Step 6: Step 7: Safety Market
Feedstock Feedstock Composting Odor Treatment Compost Curing Compost Compost Standards Attributes
Recovery Preparation Screening and Storing and
Refining Packaging
03.02-B 03.02-B

03.02-B MILLED MATERIAL IGNITED AT 550°C WITH INERTS REMOVAL


LOOK—Interference and Limitations, and Sampling Handling 14.4 Determine Oven Dry Weight (dw):
issues are presented as part of the introduction to this section.
14.4.1 Place sample crucible in forced-air oven set at
12. Apparatus for Method B 70±5°C for approximately 18 h – 24 h, until weight
12.1 Analytical Balance, with of ±0.001 g accuracy. change and moisture loss diminishes to nil.
12.2 Crucibles—high-form ceramic with cover, 20- 14.4.2 Place sample crucible in desiccator and cool
mL. to approximately 27°C.
12.3 Desiccator Cabinet—vacuum with desiccant tray 14.4.3 Weigh and record gross weight of crucible
containing color indicator of moisture concentration or and sample.
an instrument indicator. 14.4.4 Subtract crucible weight from gross to
12.4 Forced-Air Drying Oven, for operation at determine net oven-dried weight (dw) of sample.
70±5°C. 14.5 Determine Ash Weight:
12.5 Muffle Furnace—forced-air for operation at 14.5.1 Place the capped crucible to the forced air
550°C. muffle furnace; slowly ramp furnace temperature to
13. Reagents and Materials for Method B 550°C, ash at 550°C for 2 h, and then slowly ramp
furnace temperature to approximately 200°C.
13.1 None required.
14.5.2 Place the crucible and ashed sample in a
14. Procedure for Method B desiccator and cool to approximately 27°C.
14.1 Preparation of Evaporating Crucible: 14.5.3 Weigh and record gross weight of crucible
14.1.1 Heat a crucible to 105°C for 0.5-1.0 h to drive and sample.
off all hygroscopic moisture. 14.5.4 Subtract crucible weight from gross to
14.1.2 Place heated crucible in desiccator cabinet to determine net ash weight.
keep it dry, and allow to cool to approximately 27°C. 14.6 Perform Calculations.
14.1.3 Record tare weight immediately prior to use, 15. Calculations for Method B
±0.001 g.
15.1 Calculate organic matter (OM) and ash (Ash)
14.2 Sample Aliquot—Transfer 10 cm3 aliquot of content as percentages of total solids on an oven dry
prepared, (air-dried), material to a dry, tared crucible. weight basis:
14.3 Initial Weight—Weigh and record gross weight Ash = (AshW ÷ dw) × 100 Equation 15.1.1
of crucible and sample, subtract crucible weight from OM = [1 – (AshW ÷ dw)] × 100 Equation 15.1.2
gross to determine net air-dried weight (inert-free where:
sample would be air-dried at 36°C). Ash = percentage of fixed solids remaining after
combustion at 550°C, % g g-1,
BVS = the organic matter fraction of solids, percentage of
readily biodegradable solids volatilized at 550°C,
% g g-1,
dw = oven-dry weight of the test sample aliquot, g
OM = BVS = LOI organic matter, and
AshW = net ash weight at 550°C, g.

Test Methods for the Examination of Composting and Compost August 12, 2001
03.02-5
Physical Examination
Ash 03.02

Test Method: Ash. Unmilled Material Ignited at 550°C with Inerts Removal Units: % g g-1 dw
Test Method Applications
Process Management Product Attributes
Step 1: Step 2: Step 3: Step 4: Step 5: Step 6: Step 7: Safety Market
Feedstock Feedstock Composting Odor Treatment Compost Curing Compost Compost Standards Attributes
Recovery Preparation Screening and Storing and
Refining Packaging
03.02-C

03.02-C UNMILLED MATERIAL IGNITED AT 550°C WITH INERTS REMOVAL


LOOK—Interference and Limitations, and Sampling Handling material, such as metal fragments, glass shards, sharps,
issues are presented as part of the introduction to this section. leather, textiles, hard and film plastics, and all material
16. Apparatus for Method C that will not biologically degrade, or oversized
biodegradable material such as wood chips and twigs
16.1 Evaporating Dish—Pyrex beaker of 150-mL that will not degrade during the retention time of the
capacity. composting process.
16.2 Watch Glass—Pyrex, 5 cm (2 in.) diameter. 18.2.4.1 Using a soft spatula, scrape the remaining
16.3 Forced-Air Drying Oven, for operation at material across the sieve, and collect the sieve accepts
70±5°C. (4 mm and under).
16.4 Muffle Furnace, for operation at 550°C. 18.2.4.2 Oven dry the hand-sorted trash at 70±5°C
16.5 Desiccator Cabinet—With a desiccant for 18 h - 24 h until sample weight change due to
containing a color indicator of moisture concentration moisture loss diminishes to nil. Weigh and record the
or an instrument indicator. mass of inert material removed (TR) from the air-dry
>4-mm sample.
16.6 Sieve—#5 mesh (4 mm).
18.2.5 Recombine the sieve accepts (under 4 mm)
16.7 Analytical Balance—capable of weighing to 100 and oversized (over 4 mm) biodegradable material.
g, with ±0.1 mg accuracy. Weigh and record weight of recombined compost
17. Reagents and Materials for Method C sample.
17.1 None required. 18.2.6 Place the beaker with recombined compost in
a forced-air drying oven set at 70±5°C and dry for 18-
18. Procedure for Method C 24 h until sample weight change due to moisture loss
18.1 Preparation of Evaporating Dish: diminishes to nil.
18.1.1 Heat a clean beaker to 105°C for 0.5 h - 1.0 h 18.2.7 Remove the beaker and cool in a desiccator
to drive off all hygroscopic moisture. for a minimum of 1 h. Determine oven-dried weight of
18.1.2 Place heated beaker in desiccator cabinet to beaker contents, (dw).
keep it dry, and allow to cool to approximately 27°C. 18.3 Sample Analysis:
18.1.3 Record tare weight of dry beaker immediately 18.3.1 Transfer the recombined oven-dried sample
prior to use. with inert material removed into a tared 150-mL tared
18.2 Preparation of Sample: Pyrex beaker.

18.2.1 Transfer 50 cm3 of as received sample 18.3.1.1 Weigh and record gross weight of sample
material as received to a tared Pyrex beaker. Obtain and beaker. Determine compost sample net weight.
and record total as-received weight of sample in 18.3.2 Place the watch glass, concave side facing up,
beaker, ±0.001 g. on top of the beaker and transfer it to the forced-air
18.2.2 Place beaker with sample into forced-air muffle furnace; slowly ramp furnace temperature to
drying oven set at 36°C and dry for 24 h - 48 h. 550°C, ash at 550°C for 2 h, and then slowly ramp
furnace temperature to approximately 200°C.
18.2.3 Remove beaker and cool in desiccator for
minimum of 1 h. Record dry weight of beaker 18.3.2.1 Transfer beakers containing ashed samples
contents. to a desiccator and cool to approximately 27°C.

18.2.4 Empty the air-dried sample onto a #5 sieve (4- 18.3.2.2 Weigh and record gross weight of the
mm) and remove stones and manufactured inert ashed sample plus beaker. Determine sample net
weight, (AshW).

August 12, 2001 Test Methods for the Examination of Composting and Compost
03.02-6
Physical Examination
03.02 Ash

18.3.3 Sieve the beaker contents through a #20 mesh 19. Calculation for Method C
(4-mm sieve) with a wire brush; weigh the over #20 19.1 Calculate ash content as a percentage of total
mesh material and record net weight of any small trash solids, i.e., dry matter on an oven dry weight basis:
fragments that escaped removal in step 18.2.4. This
Ash = [AshW – TA] ÷ [dw + TR] × 100 Equation 19.1
trash consists of stones and other inerts not volatilized
where:
at 550ºC, (TA).
Ash = fixed solids of biodegradable fraction remaining
after combustion at 550°C, % g g-1,
AshW = net ash weight including fine trash (TA), combusted
at 550°C, g,
dw = net oven-dried weight of recombined sample at
70±5°C, g,
TA = net weight of trash remaining after ashing, over #20
mesh materials, g, and
TR = net oven-dried weight of trash removed prior to
ashing, hand-sorted and removed, g.
19.2 Calculate the organic matter (OM, biodegradable
volatile solids) as a percentage of total solids, i.e., dry
matter on an oven dry weight basis:
OM = [100 – Ash] Equation 19.2
where:
OM = organic matter fraction, biodegradable volatile
solids evolved at 550°C, % g g-1, and
Ash = fixed solids remaining after combustion at 550°C,
from Equation 19.1, % g g-1.

Test Methods for the Examination of Composting and Compost August 12, 2001
03.02-7
Physical Examination
Ash 03.02

03.02 METHODS SUMMARY


20. Report Project, 1993-1994. St. Paul, MN. Bias of this test has
not been determined. Data are being sought for use in
20.1 Report the Following Information: developing a bias statement.
20.1.1 Express results for Organic Matter (OM, %) 21.1.3.1 Precision was determined using 10
and Biodegradable Volatile Solids (BVS, %) as a subsamples taken from one field composite sample for
percentage for the ratio, mass of volatilized compost each of three locations and two months (1993).
per mass of oven-dried compost, % g g-1.
Table 03.02-C1 Percent Ash, %. Variability is expressed as percent
20.1.2 Express results for percent ash (Ash, %) as a relative standard deviation, % CV.
percentage for the ratio, unit mass of ash per unit mass
Number of
of compost on an oven-dried basis, % g g-1. Median Std Dev % CV Samples
20.1.3 Report test method number. 54.0 3.36 6.3 10
20.2 Minimum Detection Limit—Record unit mass to 82.5 1.35 1.6 10
an accuracy of ±0.005 g. 59.4 4.10 6.9 10
38.6 1.45 3.7 10
21. Precision and Bias 53.4 0.77 1.5 10
21.1 Percent Ash and Biodegradable Volatile Solids: 40.6 4.64 11.9 10

21.1.1 Test Method 03.02-A Unmilled Material Table 03.02-C2 Biodegradable Volatile Solids, %. Variability is
Ignited at 550°C without Inerts Removal: expressed as percent relative standard deviation, CV.

21.1.1.1 Feedstocks, In-Process Materials, Finished Number of


Median Std Dev % CV Samples
Compost —The precision and bias of these tests have
not been determined. Data are being sought for use in 46.0 3.36 7.2 10
developing a precision and bias statement. 17.5 1.35 7.7 10
40.6 4.10 10.1 10
21.1.2 Method 03.02-B Milled Material Ignited at 61.4 1.45 2.4 10
550°C with Inerts Removal—The precision and bias of 46.6 0.77 1.6 10
this test have not been determined. Data are being 59.4 4.64 7.6 10
sought for use in developing a precision and bias NOTE 1C—Coefficient of Variation, %CV = Standard
statement. Deviation ÷ Mean × 100.
21.1.3 Method 03.02-C Unmilled Material Ignited 22. Keywords
at 550°C with Inerts Removal—The precision of this
test were determined by the Research Analytical 22.1 ash; biodegradable volatile solids; fixed solids;
Laboratory, Department of Soil, Water, and Climate; moisture content; total solids; volatile solids
University of Minnesota for the MN-OEA CUP

August 12, 2001 Test Methods for the Examination of Composting and Compost
03.02-8
Physical Examination
03.03 Bulk Density

Test Method: Bulk Density. Units: kg m-3 dw (Lb yd-3)


Refer to Method 03.01 Air Capacity for method protocols
Test Method Applications
Process Management Product Attributes
Step 1: Step 2: Step 3: Step 4: Step 5: Step 6: Step 7: Safety Market
Feedstock Feedstock Composting Odor Treatment Compost Curing Compost Compost Standards Attributes
Recovery Preparation Screening and Storing and
Refining Packaging
03.01-A 03.01-A 03.01-A 03.01-A
03.01-B 03.01-B 03.01-B
03.01-C

03.03 BULK DENSITY

REFER TO METHOD 03.01 AIR CAPACITY FOR METHOD PROTOCOLS


DISCLAIMERS 3. Terminology
(1) The methodologies described in TMECC do not purport to address all
safety concerns associated with their use. It is the responsibility of the
3.1 bulk density, n—Weight per unit volume of
user of these methods to establish appropriate safety and health compost, calculated and reported on an oven dry
practices, and to determine the applicability of regulatory limitations weight basis, 70±5°C, kg m-3.
prior to their use.
(2) All methods and sampling protocols provided in TMECC are subject to 3.2 equivalency, n—At STP, 1 g of deionized water !
revision and update to correct any errors or omissions, and to
accommodate new widely accepted advances in techniques and
1 cm3 of deionized water ! 1 mL of deionized water !
methods. Please report omissions and errors to the U.S. Composting 1 mL of air space ! 1 cm3 of air space.
Council Research and Education Foundation. An on-line submission
form and instructions are provided on the TMECC web site, 4. Summary of Test Methods
http://www.tmecc.org.
(3) Process alternatives, trade names, or commercial products as mentioned 4.1 Method 03.03-A (See Method 03.01-A Bulk
in TMECC are only examples and are not endorsed or recommended by Density, Porosity/Pore Space, Free Airspace and
the U.S. Department of Agriculture or the U.S. Composting Council
Research and Education Foundation. Alternatives may exist or may be
Water Holding Capacity of Unsieved Compost)—A
developed. compost sample taken from the pile, as is, of known
1. Scope volume and mass is systematically transferred to a
graduated beaker and bulk density is determined.
1.1 This section covers the measurement of bulk
density for composted materials. 4.2 Method 03.03-B (See Method 03.01-B Bulk
Density, Porosity/Pore Space, Free Airspace and
1.1.1 Refer to TMECC 03.01-A or 03.01-B, or Water Holding Capacity of Sieved Compost)—A
TMECC 03.01-C for protocols. compost sample taken from the pile, as is, of known
1.2 Values stated in SI units are to be regarded as the volume, is sieved and systematically transferred to a
standard. Values given in parentheses are provided for graduated beaker and bulk density is determined.
information only. 4.3 Method 03.03-C (See Method 03.01-C Field
2. Referenced Documents Density, Free Air Space and Water-Holding
Capacity)—A composite compost sample collected
ASTM D 2980-71, Standard Test Method for Volume
Weights, Water Holding Capacity, and Air Capacity of
from a pile or windrow is systematically transferred to a
Water-Saturated Peat Materials. In Annual Book of bucket in the field and weighed to estimate bulk
ASTM Standards, Vol. Vol. 04.08. (Re-approved density.
1990). 4.4 Method 03.10-D (See Bulk Density and Water-
Haug, Roger T., The Practical Handbook of Compost Holding Capacity, of Water-Saturated Compost,
Engineering, Lewis Publishers, 1993. Modified ASTM D 2980-71)—A composite compost
Water holding Capacity, Volume Mass and Air Capacity of sample is systematically transferred to a burette and
Water-Saturated Peat. ASTM D 2989-71. p 77. In Peat weighed to estimate bulk density, dw basis.
Testing Manual. National Research Council of Canada,
Technical Memorandum No. 125. 1979. 4.4.1 Volume weights, porosity/pore space, water
holding capacity, bulk density, compost volumes and
Laboratory Procedure for the Preparation of Solid Waste
and Related Materials for Analysis. p 3. In Methods of air volume are determined on both weight and volume
Solid Waste Testing. 1973. US EPA. Office of basis from these data.
Research and Monitoring. US EPA-6700-73-01, Part I.

Test Methods for the Examination of Composting and Compost August 12, 2001
03.03-1
Physical Examination
Bulk Density 03.03

4.4.2 The bulk density test result is reported as kg m- 5.1.2 Bulk density is used for conversion from
3
with the weight expressed on a 70±5°C dry weight application rate in mass per unit area to thickness of
basis, where volume is measured after the sample is application layer (e.g., tons per acre to inches).
systematically packed as indicated. A dry weight 5.2 As compost matures, its organic carbon content
adjustment ratio is determined on a separate parallel decreases due to chemical and biological conversions
aliquot of compost material. of organic carbon to carbon dioxide. As this occurs,
5. Significance and Use structural support provided by various carbon
compounds degrades and collapses, causing the
5.1 Bulk density is weight per unit volume of
remaining inorganic materials (salts and metals) to
compost.
compact. At the molecular level, this compaction of
5.1.1 Bulk density based on as-received moisture per structure is referred to as molecular close-packing.
unit volume at as-received moisture can be used to This process concentrates materials, both
estimate transportation requirements. biodegradable and non-biodegradable. The result is a
higher unit of mass per unit volume in aged, composted
material than that of the original feedstock blends.

August 12, 2001 Test Methods for the Examination of Composting and Compost
03.03-2
Physical Examination
03.03 Bulk Density

03.03 METHODS SUMMARY


6. Report St. Paul, MN. Bias of this test has not been
determined. Data are being sought for use in
6.1 Report the Following Information—Express developing a bias statement.
results for bulk density as the ratio of mass per unit
volume of compost on an oven-dried basis (70±5°C) to 7.1.2.1 Precision was determined using 10
the nearest ±1.0 kg m-3 (Lb yd-3) dw basis. subsamples taken from a field composite sample for
each of three sites for two sampling periods, (1993).
6.1.1 Report moisture content of compost sample
aliquot used to determine bulk density. Describe Table 03.03-1 Bulk Density, kg m-3. Precision estimates for < 6.4
sample condition. mm as-received MSW compost material (1993).
Number of
7. Precision and Bias Median Std Dev % CV Samples
7.1 Bulk Density: 400 5.0 1.3 10
7.1.1 The precision and bias of the tests for Methods 390 5.0 1.3 10
380 6.7 19.5 6
03.03-A, B, and C have not been determined. Data are
410 6.0 1.6 10
being sought for use in developing a precision and bias
350 9.0 2.7 10
statement.
340 1.5 4.4 10
7.1.2 Method 03.10-D Bulk Density, and Water- NOTE 1—Coefficient of Variation, %CV = Standard Deviation
Holding Capacity of Compost Material, Modified ÷ Mean × 100.
ASTM D 2980-71—The precision of this test were
determined by the Research Analytical Laboratory, 8. Keywords
Department of Soil, Water, and Climate; University of 8.1 bulk density; maturity; weight; volume
Minnesota for the MN-OEA CUP Project, 1993-1994.

Test Methods for the Examination of Composting and Compost August 12, 2001
03.03-3
Physical Examination
Bulk Density 03.03

August 12, 2001 Test Methods for the Examination of Composting and Compost
03.03-4
Physical Examination
03.04 Wettability

Test Method: Wettability. Two Methods. Units: see methods


Test Method Applications
Process Management Product Attributes
Step 1: Step 2: Step 3: Step 4: Step 5: Step 6: Step 7: Safety Market
Feedstock Feedstock Composting Odor Treatment Compost Curing Compost Compost Standards Attributes
Recovery Preparation Screening and Storing and
Refining Packaging
03.04-A 03.04-A 03.04-A 03.04-A 03.04-A
03.04-B 03.04-B 03.04-B 03.04-B 03.04-B

03.04 WETTABILITY
DISCLAIMERS Emerson W. W. and R. D. Bond. 1962. The rate of water
(1) The methodologies described in TMECC do not purport to address all
entry into dry sand and calculation of the advancing
safety concerns associated with their use. It is the responsibility of the contact angle. Aust. J. Soil Res. 1: 9-16.
user of these methods to establish appropriate safety and health
Hammond L. C. and T. L. Yuan. 1968. Methods of
practices, and to determine the applicability of regulatory limitations
prior to their use. measuring water repellency of soils. In Water-repellent
(2) All methods and sampling protocols provided in TMECC are subject to soils, Proc. Symposium on Water University of
revision and update to correct any errors or omissions, and to California, Riverside May, 1968 ed. L. F. Debano and
accommodate new widely accepted advances in techniques and J. Letey.
methods. Please report omissions and errors to the U.S. Composting
Council Research and Education Foundation. An on-line submission Kayser W.V. 1976. J. Colloid and Interface Science
form and instructions are provided on the TMECC web site, 56:622.
http://www.tmecc.org.
(3) Process alternatives, trade names, or commercial products as mentioned King, P.M. 1981. Comparison of methods for measuring
in TMECC are only examples and are not endorsed or recommended by severity of water repellence of sandy soils and
the U.S. Department of Agriculture or the U.S. Composting Council assessment of some factors that affects its measurement.
Research and Education Foundation. Alternatives may exist or may be
developed.
Aust. J. Soil Res. 19:275-85.
Kreft D.R. 1987. Soil Physical Properties as Influenced
1. Scope by the addition of municipal compost. University of
1.1 This section covers proposed tests covers to Minnesota, Minnesota Masters thesis. pp. 57, 84-88,
measure wettability characteristics of compost. 105-106.
Letey L. J. Osborn and R.E. Pelishek. 1962.
1.1.1 Method 03.04-A—Wicking Rate of Compost.
Measurement of liquid-solid contact angles in soil and
1.1.2 Method 03.04-B—Water-Drop Penetration sand. Soil Sci. 93: 149-153.
Rate. Link K. C. and E-U. Schlunder. 1996. A new method for
1.2 Values stated in SI units are to be regarded as the the characterization of the wettability of powders.
standard. Values given in parentheses are provided for Chem. Eng. Technol. 19:432-437.
information only. Watson and Letey. 1970. Indices for characterizing soil-
water repellence based upon contact angle surface
2. Referenced Documents tension relationships. Proc. Soil Sci. Soc. Am. 34:841-
2.1 TMECC: 844.

Method 02.02-B Sample Sieving for Aggregate Size. 3. Terminology


Method 02.02-C Man-made inert Removal. 3.1 absorb, v—To take (something) in through pores
Method 02.02-D Milling and Grinding Samples, Harrison. or interstices.
Method 02.02-E Milling and Grinding Samples, Munter. 3.2 absorption, n—A process in which one material
Method 03.09-A Total Solids and Moisture. (the absorbant) takes in or absorbs another (the
2.2 Scientific Literature: absorbate); as the absorption of moisture by compost.
Adamson, A.W. Physical Chemistry of Surfaces. 4th ed. 3.3 adsorption, n—The accumulation of gases,
1982. John Wiley and Sons, New York. liquids, or solutes on the surface of a solid or liquid.
Berglund, K. and L. Persson. 1996. Water repellence of 3.4 critical micelle concentration (CMC)—The
cultivated organic soils. Acta Agric. Scand., Sect B, 46: concentration of a surfactant above which it
145-152. predominantly forms aggregates including micelles in
Dekker L.W. and C. J. Ritsema. 1994. How water moves solution. Addition of more surfactant results in the
in a water repellent sandy soil. 1. Potential and actual formation of more aggregates while leaving the
water repellency. Water Resour.Res. 30:2507-2517. monomer concentration more or less unchanged.

Test Methods for the Examination of Composting and Compost August 12, 2001
03.04-1
Physical Examination
Wettability 03.04

3.5 fines, n—Particles with a diameter < 2 mm. 4. Summary of Test Methods
3.6 hydrophilic, adj—Having an affinity for water; 4.1 Method 03.04-A Wicking Rate of Compost—The
readily absorbing or dissolving in water. A hydrophilic wettability threshold is determined by establishing
surface is a surface that is readily wet by water e.g., whether a sample of compost can re-wet to more than
clean glass. 35 percent moisture by capillarity. A series of prepared
3.7 hydrophobic, adj—The propensity of a solid to compost samples with varying moisture contents are
repel water. Repelling, tending not to combine with, or exposed to water. The rate and amount of water
incapable of dissolving in water. A hydrophobic absorption by each sample is measured. The
surface is a surface that is not readily wet by water e.g., wettability threshold is reached when the time required
Teflon. to rewet the compost sample exceeds a predetermined
maximum allowable time period.
3.8 micelle, n—A spherical assembly that forms
spontaneously in aqueous solution. The hydrophilic 4.1.1 As-received compost is passed through a 4-mm
heads of the surfactants are exposed to the water with sieve, subdivided into 50 cm3 samples and placed in a
the hydrophobic tails forming the solid core. forced air oven preheated to 36°C. Individual samples
are sequentially removed during drying, weighed and
3.9 surface tension, n—A property of liquids arising the percent moisture content calculated. The same
from unbalanced molecular cohesive forces at or near sample is then transferred to a filtered beaker. The
the surface. In an effort to minimize its surface tension filtered beaker is sealed onto the top of a second glass
or energy the surface area of the liquid at the liquid-air flask using ground glass joints. Water, from a modified
interface tends to contract. The surface tension of a burette fitted with a stop-cock, flows into the flask
liquid is commonly reported as mN m-1 and the surface through an inlet tube at the bottom of the lower flask.
tension of water is 73 mN m-1. Flexible tubing connects the delivery end (bottom) of
3.10 surfactant, n—A surface active agent that the burette with the lower flask’s inlet tube. The
reduces the surface tension of fluids that coat a receiving end (top) of the burette is sealed with a
material. The molecules contain a section that is rubber stopper fitted with a narrow glass capillary tube
hydrophobic (a hydrocarbon tail) and a section that is (tube open to air). The capillary tube is positioned to
hydrophilic ± the headgroup). Examples include: ensure a constant head of pressure.
3.10.1 Brij 58, n—A non-ionic surfactant, chemical 4.1.2 The amount of water absorbed by the compost
name: polyoxyethylene (20) cetyl alcohol p-t-octyl is determined by monitoring the rate and amount of
phenol. The molecular weight is 1120 and the critical water that exits the burette and passes to the sample
micelle concentration is 0.008 g 100 mL-1 or 71.4 µM. (Fig 03.04-A1). At the end of a run, the filtering device
containing the sample is re-weighed and placed in an
3.10.2 Nonidet P-40, n—A non-ionic surfactant.
oven to determine moisture content of moistened
Chemical name: polyoxyethylene (9) p-t-octyl phenol.
compost sample. The run is repeated for each 50 cm3
The molecular weight is 603 and the critical micelle
compost sample, each with different moisture content
concentration is 0.017 g 100 mL-1 or 282 µM.
(i.e., 0, 5, 10, 15, 20, 25 and 30%).
3.10.3 Tween 20, n—A non-ionic surfactant,
4.1.3 Wettability Threshold—The lowest percent
chemical name: polyoxyethylene (20) sorbitol
moisture (wet weight basis) that compost may attain
monostearate. The molecular weight is 1230 and the
without limiting its ability to re-absorb moisture is
critical micelle concentration is 0.006 g 100 mL-1 or
determined If the kinetics of wetting is too slow,
9.92 µM.
additional runs are conducted with non-ionic
3.11 wettability, n—the propensity of a surface to surfactants dissolved in water at or below the critical
adsorb moisture. The state or condition of being micelle concentration.
wettable, or the relative affinity of liquid for the surface
4.2 Method 03.04-B Water-Drop Penetration Rate—
of a solid, such as the affinity of water for paper or
As-received compost is passed through a 4-mm sieve,
leather. Wettability increases directly with increasing
subdivided into 20 cm3 samples and placed in a forced
affinity, as measured by the contact angle formed
air oven preheated to 36°C. Individual samples are
between the liquid and the solid. This increases from
removed from the oven at periodic intervals during
non-wettability at an angle greater than 90 degrees to
drying, weighed and the initial percent moisture content
complete wettability when the contact angle is 0
of the sample is calculated. Approximately six cm3 of
degrees.
compost is placed into three petri dishes and the sample
surface is flattened.

August 12, 2001 Test Methods for the Examination of Composting and Compost
03.04-2
Physical Examination
03.04 Wettability

4.2.1 Three drops (100 µL) of water are carefully bulk or bagged material. The bulk mass for shipping
placed onto each flattened compost sample. The time may be reduced more than 50% by air-drying finished
(up to 1 h) required for the nine drops to penetrate the material prior to shipment; this reduces the cost of
compost is visually monitored and recorded. Runs are shipping. The end-use and method used to dry the
repeated with compost samples at varying moisture compost prior to shipping dictate the re-moistening
contents, (e.g., 0, 5, 10, 15, 20, 25 and 30%). requirements of compost. For applications on farms,
4.2.2 The average time required for droplets to rewetting is usually unnecessary, because mixing with
penetrate compost is reported for each compost moist soil upon application provides adequate moisture.
moisture content. It would also be unnecessary to rewet compost used to
manufacture blends of potting mixtures that will also
5. Significance and Use contain ionic fines (e.g. clays).
5.1 Three practical applications for determining the 6. Literature Review
compost wettability threshold and re-wetting index are
presented: in-process and moisture management during 6.1 Wetting of Solids, Review of Basic Principles:
compost curing; in-plant dust control; and efforts to 6.1.1 Introduction—The ability of water to wet
decrease shipping costs without diminishing compost depends upon the surface characteristics of the
quality. Each case illustrates how changes in the material. If the surface contains a significant fraction
wettability properties of a compost occur during drying of hydrophilic groups (-SO4Na, -COOK, -COOH, -OH,
and how they impact management decisions and costs. R3-NH, -Si(OH-) surrounded by layers of water
In practice, wettability measurements as described in molecules, the surface is readily wet by water. In
this section are rarely used by compost operators during contrast, if the surface contains a significant fraction of
composting or when planning compost uses. The hydrophobic groups (e.g. hydrocarbons, carbon
methods most likely to be used for technical accuracy fluoride, -CH-, -CH2- CH3 CF), the surface is not
are provided. However, rapid, onsite assessments by readily wet by water. Feedstocks used to produce the
compost site operators will often be the first choice finished compost significantly influence the surface
approach because of cost and time limitations. characteristics of compost. For example, as the plastics
5.1.1 Maintaining optimum moisture content during content of feedstock increases, the ability of the
the curing phase of compost—Biological degradation resulting compost to absorb and retain moisture
consumes moisture during curing. The rate of decreases, because water will not wet most stable
degradation diminishes to nil when the compost plastics (e.g., carbon fluoride containing plastics,
moisture content falls below a minimum biological Teflon). In comparison, animal manure composts are
activity moisture threshold of approximately 40%. generally hydrophilic and more readily wet by water.
Curing composts are regularly monitored for moisture 6.1.2 Surface characteristics of feedstocks and
content and require frequent additions of water and compost sometimes change upon drying. As an
further blending to maintain moisture conditions above example, if compost dries during the curing process or
the minimum threshold. In some cases, curing compost during storage, some of the dried fines will readily
is mistakenly left to dry below its wettability threshold accept moisture, while others will require wetting
and as a result, cannot be rapidly re-moistened. agents or surfactants before they may rapidly remoisten
Approved surfactants are sometimes used to accelerate to a desired level. If significant changes occur in the
the re-moistening process of dry compost; ionic surface chemistry of compost (i.e., change from
particles (e.g. clays) that readily rewet are sometimes hydrophilic to more hydrophobic groups), it will be less
blended into a dried compost to hasten re-wetting. able to re-absorb moisture. Changes in surface
5.1.2 Dust Control—When compost moisture falls chemistry vary with drying temperature, drying rate,
below the dust threshold (~35%), fines and other small and relative moisture content of dry fines. Use of
particles become airborne with minimal agitation. This surfactants can be avoided if significant chemical
dust is a nuisance and a potential worker health hazard. changes do not occur and the moisture content of
Often, water is used to control dust, however, rapid compost is maintained above a minimum wettability
drying often induces radical changes in the surface threshold level.
structure of compost fines that can significantly alter 6.1.3 Definition—The technical definition for
the absorptive characteristic of compost, making it wetting of a solid is that the contact angle is zero or so
difficult to rewet air-dried fines and small particles. close to zero that the liquid spreads over the solid
5.1.3 Reduce Shipping Costs—Compost products are easily. Non-wetting implies that the angle is greater
shipped from composting facility to market, as either than 90° and liquid tends to ball up and run off the
surface. The definition of contact angle and

Test Methods for the Examination of Composting and Compost August 12, 2001
03.04-3
Physical Examination
Wettability 03.04

illustrations of non-wetting to wetting solids are shown in Figure 03.04-1.

γ lv
γlv

γ sv γ lv γ sv γ sv
θ θ θ
γsl γ sl

Fig 03.04-1 Definition of a contact angle on a non-porous surface.

6.1.3.1 Consider what happens when a spherical 6.1.5 Surface tension of most liquids decreases
droplet of water is placed on a non-porous solid in linearly with increasing temperature— The surface
contact with water vapor. The droplet will either tension of water decreases 0.138 mN m-1 per °C
spread (wet) or ball-up (not wet) on the solid surface. (Kayser, et al., 1976) the surface tension of ethanol
At equilibrium, there is no more change in the area of decreases 0.086 mN m-1 per °C (Adamson, 1982).
the solid covered and the surface tensions or energies Common aqueous electrolytes like NaCl increase the
of the various interfaces are balanced. This is surface tension of water. The surface tension of 1 M
expressed by Young's equation: NaCl solution is about 74 mN m-1 (Adamson 1982),
γsv-γsl = [γlvcosθ] Equation 6.1.3.1 while nonpolar solvents like ethanol decrease the
where: surface tension of water.
γsv = surface tension at the solid-vapor interface, 6.2 Wetting a Porous Medium
γsl = surface tension at the solid-liquid interface, 6.2.1 Compost is a porous material and wetting
γlv = surface tension at the liquid-vapor interface, and involves not only the spreading on the surface, but the
θ = contact angle penetration of liquid into the pores by capillarity (Fig
6.1.3.2 If the droplet completely wets the surface, 03.04-2).
(i.e., the contact angle is zero), then Young's equation 6.2.2 In this case the wetting process is related to
is not valid and the spreading coefficient (Sslv) is used capillary rise where the driving force for wetting is the
to describe the imbalance of the energies: pressure difference across the curved surface of a
Sslv = [γsv-(γsl + γlv)] Equation 6.1.3.2 meniscus (∆P) and for a spherical meniscus of radius, r,
6.1.3.3 To encourage spreading (Sslv is positive) γsl this can be described with Laplace's equation:
and γlv should be as small as possible. In practice this is ∆P = [2γlv cosθ ÷ r] Equation 6.2.2
accomplished by adding to the liquid phase a surfactant 6.2.3 For a finite contact angle 0° < θ < 180° the
that adsorbs at both the solid-liquid and liquid-vapor pressure gradient can be written as:
interfaces, and lowers the interfacial tensions. ∆P = [2 (γsv-γsl ) ÷ r] Equation 6.2.3
6.1.4 Surface Tension—Water has a surface tension 6.2.4 To improve penetration it is necessary to make
of 72.8 mN m-1 and does not readily wet surfaces of γsl as small as possible, except for a perfectly wetting
low surface energy; examples of such surfaces are liquid, (θ = 0) where it is necessary to make γlv large
graphite, paraffin and many plastics. It does wet polar because equation 6.2.1 becomes:
surfaces; contact angles of 0° are measured on clean
∆P = [2γlv ÷ r] Equation 6.2.4
glass, clean quartz, uncontaminated gold (Adamson,
1982) and freshly cleaved mica. In contrast, ethanol is 6.3 The net goal to improve penetration for a
a liquid with a low surface tension (22 mN m-1) and perfectly wetting liquid is to add a wetting agent or
forms droplets with very small contact angles (< 10°) surfactant that reduces γsl without at the same time
on most surfaces. There are a few plastics that it does reducing γlv. It is unlikely that water will act as a
not wet. Teflon or polytetrafluroethylene (PTFE) is perfectly wetting liquid for compost and the objective
one of the materials that ethanol does not readily wet, it in practice is usually to add a surfactant that makes γsl
forms droplets with a contact angle of about 40° (Hu as small as possible.
and Adamson, 1977). As a general rule, a liquid only
wet solids that are of higher surface energy than its
surface tension.

August 12, 2001 Test Methods for the Examination of Composting and Compost
03.04-4
Physical Examination
03.04 Wettability

6.4.1.1 This is a quick test that could be adapted for


water droplet use with compost. It is not quantitative and not suitable
for determining the wettability threshold, but it would
pore at least indicate if compost were readily rewettable. It
porous surface
could also be used to test surfactants added to improve
the kinetics of wetting.
6.4.2 The Molarity of Ethanol Test—This method
was also suggested by Watson and Letey (1970) and is
Fig 03.04-2 Water droplet on a porous surface. Water both spreads another common method adapted and used by several
across surface and is absorbed through pores. groups to assess the repellency of soil (King, 1981;
Berglund and Persson, 1996). There are several forms
6.3.1 Surfactants—Non-ionic (e.g., Tween 20) as
of this method. Drops (50 µL) of aqueous ethanol
opposed to ionic surfactants are more suitable to use for
solutions of concentrations from 0 to 7 M at 0.2 M
compost, because ionic surfactants tend to be more
intervals are placed on soil samples and their entry time
reactive and have the potential to affect biological
is recorded. The degree of repellence is represented by
activity. For example, they are better denaturing agents
the molarity of ethanol that penetrated the surface in 10
(denature proteins and membranes) and can reduce
seconds.
microbial activity. The amount of surfactant to add is
usually small and always at or below the critical micelle 6.4.2.1 Ethanol is a solvent with a low surface
concentration, adding it at higher concentrations will tension that readily wets most surfaces. The higher the
not lower the surface tension of water and will only concentration of ethanol in aqueous solution the lower
increase the chance of toxicity. the surface tension of the liquid and the more likely it
will wet low energy (and generally hydrophobic) solids.
6.3.2 Heterogeneous media—Finished compost is a
Therefore the more hydrophobic the surface groups of
heterogeneous media with varying surface structure and
compost the higher the concentration of ethanol
porosity. Even within a sample there is variability with
required for wetting and the more water repellent the
respect to porosity and surface structure. Relationships
compost. Unlike soil, some compost may contain inert
presented above are useful for understanding the
plastic components that are not readily wettable, even
principles behind the wettability of compost or the
by low surface tension liquids like ethanol. The
water repellency characteristics of compost, but cannot
presence of plastics could bias results, so methods that
be rigorously applied to heterogeneous material.
require the use of ethanol may not be appropriate for
6.4 Summary of Potentially Adaptable Methods—The compost.
current methods used to measure the water repellency
6.4.3 Determining the liquid-soil contact angle in
of soils and other porous media like pharmaceutical
soil and sand by capillary rise—This method was
powders and fabrics are reviewed.
outlined by Emerson and Bond (1962) and Letey et al.
6.4.1 Water-Drop Penetration Rate—This is a (1961) and was used by King (1981) and others
method proposed by Watson and Letey (1970) to (Hammond and Yuan, 1968). It uses the Young-
measure the repellency of water on soil. A water Laplace equation to determine the contact angle. From
droplet ~ 50 µL is placed on the surface of a soil core Equation 3.3.1 the pressure difference across the
or soil sample and the time taken for the drop to meniscus must be balanced by the hydrostatic pressure
completely penetrate the soil is measured. The average drop in the column of liquid. ∆P = h∆ρg where: h:
penetration time of ten drops is reported for each maximum height of capillary rise, g: acceleration due to
sample. There are several variations of this test. gravity; ∆ρ difference between density of water and air.
Measurement of penetration times for entry times of up Historically the capillary rise method was used to
to 1 h (Berglund, et al., 1996). Measure penetration determine the surface tension of liquids and is very
times for entry times of up to 4 min (King 1981) and accurate provided the liquid wets the glass capillary
classification of the soils depending upon the time the and the exact solutions of the Young-Laplace equation
water takes to enter the soil (Dekker and Ritsema, are used.
1994). Ten classes were distinguished: (i) wettable
(<5 s); (ii) slightly water repellent (5 to 60 s); (iii) 6.4.3.1 If it can be assumed that the porous media is
strongly water repellent (60 to 600 s); (iv) severely equivalent to a bundle of capillaries of average radius r,
water repellent (600 s to 1 hr) and extremely water and the moisture content below the maximum height of
repellent with six classes based on the time needed for capillary rise is constant, equation 6.4.3.1 can be used
infiltration (v) 1-2 h (vi) 2-3 h (vii) 3-4 h (viii) 4 to 5 h to determine an apparent contact angle in porous
(ix) 5 to 6 and (x) > 6 h. media. Because there are two unknowns θ and r, the

Test Methods for the Examination of Composting and Compost August 12, 2001
03.04-5
Physical Examination
Wettability 03.04

approach is to compare the capillary rise of two water (h) or ethanol (ho) is determined and the contact
identically packed columns; immerse one column in a angle at the soil-water interface is calculated with
low surface tension liquid (e.g. ethanol) and assume the equation 6.3.3.2.
liquid completely wets the surface (cos(θ) =1) and 6.4.4.3 There are two reasons that make this method
immerse the other in water and determine the angle at unsuitable for assessing the wettability threshold. The
the soil-water interface from: capillary rise would be difficult to measure in wet (up
cosθ = [∆P ÷ ∆Po] × [γlve ÷ γ lvw] Equation 6.4.3.1 to 30% moisture) compost and the capillary rise of
cosθ = [hg∆ρ ÷ hog∆ρo] × [γlve ÷ γ lvw] Equation 6.4.3.2 water in compost has to be compared with that
where: measured in ethanol. In the method proposed water is
∆P = pressure drop across the air-water meniscus, absorbed through compost by capillary forces, but the
γlvw = surface tension at the water-air interface, height of the capillary rise is not measured only the rate
that compost absorbs water.
∆ρ = difference in density between water and air,
h= maximum height of capillary rise of water, 6.4.5 Dynamic Contact Angle Measurement—The
θ= contact angle at the soil-water interface, most commonly used method for measuring the contact
∆Po = pressure drop across the ethanol-air meniscus, angle of powders is to measure the height of a large
drop on a pre-saturated porous substrate. The substrate
γlve = surface tension at the ethanol-air interface;
is compressed into a tablet and a drop applied to the
∆ρo = difference in density between ethanol and air, and
tablet is not drawn into the material because the pores
ho = maximum height of capillary rise of ethanol. are already saturated. In practice this measurement is
6.4.3.2 This approach was first implemented by difficult, the surface has to be flat and it is not easy to
Letey et al., (1962) with sand columns. They presented prevent a water film forming on the surface of the
evidence that ethanol penetrated sand with the same tablet. Another method for determining the wettability
rate, independent of the treatment whereas the rate of of a porous material is to monitor the change in the
penetration of water depended on treatment. They then contact angle with time (Link and Schlunder, 1996).
concluded that ethanol wets sand (contact angle = 0°) This is similar to the water drop penetration time, but
and used it to determine a contact angle at the sand- more systematic because the shape of the contact angle
water interface. As mentioned, this is probably a is measured at time intervals. A tablet is formed by
reasonable assumption, ethanol is a liquid with a low compressing the powder particles to < 100 µm radius
surface tension (22 mN m-1) and forms droplets with and kept isothermal by placing the tablet on a heating
very small contact angles (< 10°) on many surfaces. plate. A droplet (3 µL) is discharged from a syringe
6.4.4 Capillary Rise—There are two forms of this with the aid of a micrometer screw. The wetting
test determining the equilibrium and dynamic capillary process is observed and recorded by a video camera.
rise: The contact angle of the drop decreases from 180° to
some static value after time t. If the contact angle
6.4.4.1 Equilibrium capillary rise—Glass tubes
dropped from 180° (spherical drop) to zero very
were made hydrophobic by treating them with paraffin
quickly, the substrate would be wet. The rate at which
dissolved in xylene, they were then filled with sand and
the droplet disappears indicates the kinetics of wetting.
immersed in alcohol or water. The capillary rise was
Penetration increases with increased porosity and
monitored periodically and measured after 24 h (Letey
temperature.
et al. 1962). This time was assumed to be sufficient for
equilibration. 6.4.5.1 This method could be adapted for use with
compost, the rate at which the droplet disappears and
6.4.4.2 Dynamic capillary rise—Emerson and Bond
the final size of the contact angle would indicate the
(1962) developed this technique for soils. This method
propensity for compost to wet. Unfortunately, this
requires only about 15 minutes. A positive head is used
method requires fairly expensive equipment, specialty
to push the liquids through a small diameter glass or
software, and a highly trained technician. In addition
plastic tube filled with soil or sand. The tube was
to the standard laboratory equipment, a camera,
immersed in a large water or ethanol reservoir of
commercial grade VCR, computer interface, computer
known height and the average position of the wetting
and image software are required. The technician would
front was measured every 15 sec for about 15 to 30
need to be able to identify interface boundaries which
min. The rate of change of the wetting front dx/dt was
would be very difficult with rough porous surfaces.
plotted against the inverse of the wetting front. The
line is extrapolated to zero to determine the height of 6.4.6 Infiltration Methods—These methods involve
wetting front when dx/dt =0. After subtracting the packing a column with soil or sand and determining the
positive head the maximum capillary rise obtained in rate at which the water flows through the medium.

August 12, 2001 Test Methods for the Examination of Composting and Compost
03.04-6
Physical Examination
03.04 Wettability

Columns are positioned horizontally, vertically upward, tests performed on composts with a moisture content
or vertically downward (Letey, et al., 1962; King, above 0 % (wet weight basis).
1981; and Berglund and Persson, 1996).
7. Interference and Limitations
6.4.7 Comparison of Test Methods—King (1981)
7.1 Interference and limitations of this test are not
compared tests used to assess the water repellence of
determined. Data are being sought for use in
soils. He examined over 100 sandy soils and compared
developing an interference and limitations statement.
the molarity of the ethanol test, dynamic contact angle
measurement, water drop penetration time and an 8. Sample Handling
infiltration method that used gravity to assist flow. He 8.1 Perform this test on feedstocks or finished
found strong correlation among tests. The soils were composts. The material may contain levels of
categorized according to results of the test. However, unclassified inert material that meets end-use standards.
reproducible tests were only observed with air and
oven-dried samples. Increasing the moisture content of 8.1.1 Procedures are performed on a sieved sample
the soils affected the reproducibility of the tests, in all aliquot of compost maturity classes of interest,
cases it was recommended that tests be performed with including feedstock if appropriate.
air- or oven-dried soil (King, 1981). His observations 8.1.2 This test may be performed in conjunction with
implied that repeatability might become limiting for sample sieving as outlined under Method 02.02-B and
Method 02.02-C.

Test Methods for the Examination of Composting and Compost August 12, 2001
03.04-7
Physical Examination
Wettability 03.04

Test Method: Wettability. Wicking Rate of Compost Units: % at tcritical


Test Method Applications
Process Management Product Attributes
Step 1: Step 2: Step 3: Step 4: Step 5: Step 6: Step 7: Safety Market
Feedstock Feedstock Composting Odor Treatment Compost Curing Compost Compost Standards Attributes
Recovery Preparation Screening and Storing and
Refining Packaging
03.04-A 03.04-A 03.04-A 03.04-A 03.04-A

03.04-A WICKING RATE OF COMPOST


LOOK—Interference and Limitations, and Sampling Handling 10.6 Other Surfactants—Use other suitable non-ionic
issues are presented as part of the introduction to this section.
surfactant made up at its critical micelle concentration.
CONTRIBUTED BY—Dr. Brenda F. Farrell, Edaphos International
11. Apparatus Preparation for Method A
9. Apparatus for Method A
11.1 Acid wash all glass components (filter device,
9.1 Drying Oven—forced air, vented, temperature set flask and burette) with 10% nitric (NO3) acid and rinse
at 36°C and 70±5°C. thoroughly with distilled water.
9.2 Bag—20 brown paper, #6, or equivalent container 11.2 Soak all components in ethanol for 1 h and
suitable for air-drying samples. rinsed with water (17 M!·cm resistivity).
9.3 Sieve—4-mm mesh, plastic or stainless steel. 11.3 Allow all glass components to dry.
9.4 Analytical Balance—accurate to ±0.001 g. 11.4 Assemble apparatus as illustrated in Fig 03.04-
9.5 Wicking Apparatus—filtering device (modified A1.
beaker with a sintered glass bottom), flask, burette, 11.4.1 Fill the flask and burette with water to a level
capillary tube, rubber stopper and tubing. Refer to Fig in line with the lower side of the sintered glass.
03.04-A1.
11.4.2 Close the stopcock and fill the burette to the
9.6 Syringe with tuberculin needle—10 of 10-mL top with water.
syringe fitted with a 5-cm tuberculin needle.
11.4.3 Cap the burette with a soft rubber stopper
9.7 Volumetric flasks—three, 500-mL. coated with glycerol that is fitted with the capillary
10. Reagents and Materials for Method A tube.
10.1 Water—deionized 17 M!·cm water; surface 11.4.4 Position the capillary tube to ensure that its
tension of the water used in the experiments should be lower end is directly in line with the lowest measured
measured and reported with the results. increment on the burette and directly in line with the
lower side of the sintered glass.
10.2 Brij 58—71.4 µM aqueous solution. Add 250
mL of water to a 500-mL volumetric flask. Add 0.04 g 11.4.5 When the stopper is secure, remove excess
of Brij 58. Fill to a final volume of 500 mL with water. water with the syringe fitted with a tuberculin needle.
(optional) Insert the needle through the rubber stopper and use the
syringe to extract excess water from the burette.
10.3 Nonidet P-40—282 µM aqueous solution. Add Sufficient water is removed to bring the water meniscus
250 mL of water to a 500-mL volumetric flask. Add into alignment with the upper-most volume mark of the
0.085 g of Nonidet P-40. Fill to a final volume of 500 burette, and simultaneously, air reaches the very bottom
mL with water. (optional). end of the capillary tube. Remove the needle and the
10.4 Nitric acid, 10%—Add 750 mL of water into a perforation in the rubber formed by the needle will
1-L volumetric flask; add 100 mL of concentrated nitric close and seal itself providing the rubber stopper is
acid. Fill to a final volume of 1 L with water. malleable and properly lubricated.
CAUTION—The nitric acid solution is highly corrosive and must 12. Sample Preparation for Method A
be made up in fume hood.
12.1 Pass approximately 750 cm3 of compost through
10.5 Tween 20™—9.92 µM aqueous solution. Place
a 4-mm sieve to provide at least 600 cm3 of < 4 mm
250 mL of water to a 500-mL volumetric flask. Add
sieved material.
0.0065 g of Tween 20™. Add more water to a final
volume of 500 mL. (optional). 12.2 Blend and thoroughly mix sieved compost.

August 12, 2001 Test Methods for the Examination of Composting and Compost
03.04-8
Physical Examination
03.04 Wettability

12.3 Subdivide the < 4 mm material into separate 50 13.5 Thereafter, measure the height of the meniscus
cm3 samples, weigh and place each sub sample into a every 15 min for up to 3 h, or up to the maximum
forced-air oven preheated to 36°C. Take three separate allowable re-wetting time as dictated by the compost
aliquots of the excess sieved material and determine re-wetting operation.
their average moisture content (as-received compost 13.6 Calculate the mass of water absorbed by the
moisture, at 70±5°C; or consider oven-drying at compost for each time interval and plot mass of water
105°C if rapid analysis is needed. against time, (assume that 1 mL H2O ≡ 1 g H2O).
air inlet
rubber stopper 13.6.1 Validation Step—At the end of the run, weigh
with bore hole to
capillary tube
accommodate
the filtering device and determine the change in weight
capillary tube of the compost due to the absorption of water.
13.6.2 Place filtering device in oven at 70±5°C
burette
overnight and determine the % moisture of the compost
burette (wet weight basis).
clamps
glass sample holder 13.7 If the samples pass this test (re-wet to ~35%
weight used to apply moisture), repeat steps 13.1 through 13.6 with each
pressure on sample
sample pair as they are removed from the drying oven,
compost layer where an acceptable series of moisture contents would
sintered glass
be 0, 5, 10, 20, 25 and 30% moisture. If not, stop the
water level line stopcock
test and proceed to Step 13.9 to evaluate surfactants to
ground glass joint
water level flexible
enhance the wetting characteristics of water.
tubing NOTE A2—If the final % moisture content of the compost is
glass water flask
burette stand greater than 35% the compost is considered to be wet. This
Fig 03.04-A1 Wicking rate of compost apparatus assembly implies that the initial state of the compost was at or above the
wettability threshold. If the final % moisture content is less
NOTE—Samples are run in pairs, removed from the oven at than 35% the compost is not considered to be wet. This implies
regular time intervals (e.g., after 1, 2, 4, 8 24 and 36 h), cooled that the initial state of the compost was below the wettability
to room temperature and individually subjected to the wicking threshold.
rate test. As mentioned, runs of the test are repeated at time 13.8 Determine the wettability threshold of
intervals.
compost—This is the minimum percent moisture (wet
12.4 Determine moisture content of partially dried weight basis) that compost may attain without affecting
compost by oven drying at 70±5°C overnight. its ability to re-absorb moisture. If the percent moisture
13. Procedure for Method A content of compost is greater than 35% the compost is
considered wet. For example, if the initial moisture
13.1 Place 45-50 cm3 of partially dried compost into content is 0% and the compost can be wet to 35%
each of two filtering devices (modified beaker with a moisture at a sufficiently fast rate then 0% moisture is
sintered glass bottom) and weigh. the wettability threshold. The rate at which compost re-
13.2 Press compost sample into a flat slab (height of wets also defines the wettability and this will depend
approximately 1 cm) at constant force (1-10 N, ~1 kg; upon the problem at hand and/or the end use of the
the required mass will vary with bulk density of the compost. Report the time taken to reach 35% moisture.
compost) with a weight of equal diameter to that of the 13.9 Surfactants—Enhance the degree and rate of
filtered sample flask (refer to Fig 03.04-A1 for wetting using a modification of the Method 03.04-B
illustration). This ensures that the compost sample is in Water-Drop Penetration Rate by adding non-ionic
intimate contact with the sintered glass. surfactants to water.
13.3 Start Run—Place the filtering device that is 13.9.1 Follow the procedures outlined for Method
filled with compost on top of the flask and open the 03.04-B.
stopcock of the burette. This is the start of the
experiment, where t=0. If the compost moisture 13.9.2 Return to Step 13.1, but use a water solution
content is above the wettability threshold, the sample containing the wetting agent in place of pure water.
absorbs water; the water meniscus of the burette will 13.9.3 Report type and concentration of surfactant
move down and a corresponding volume of air will used to improve the rate and degree of wetting.
enter the burette via the capillary tube.
13.4 Measure and record the height of the meniscus
every 15 sec for 15 min.

Test Methods for the Examination of Composting and Compost August 12, 2001
03.04-9
Physical Examination
Wettability 03.04

14. Calculations and Corrections for Method A 14.6 Plot mass of water adsorbed against time
14.1 Determine % moisture of as received compost: assuming 1 mL of water is equivalent to 1 g of water.
M = 1 - (ODW ÷ ARW) x 100 Equation 14.1 14.7 Determine wettability threshold of compost. For
14.2 Determine % moisture of partially dried the hypothetical data set example shown in Table
compost: 03.04-A1, the wettability threshold is 15%. Refer to
Table 03.04-A1 for further explanation.
A = 1 - (B ÷ C) × 100 Equation 14.2
14.3 Determine % moisture of compost after wetting: 15. Interpretation of Method A
D = 1 - (E ÷ F) × 100 Equation 14.3 15.1 Re-wetting Dried Materials—If a sample below
14.4 Compare % moisture of compost after wetting its wettability threshold must be rewet, a surfactant at a
with compost of 35% moisture. if ∆DF is greater or concentration below its CMC is used to rewet the
equal to -2 then the compost is wet: sample. The test is repeated using a surfactant solution
to assure that it may be used to re-wet the compost in
∆DF = G - 35 Equation 14.4 question at the desired rate.
14.5 Determine rate of wetting:
15.2 Monitoring Compost Moisture—During the
H= [IR - FR] - [CF × (IR - FR)] Equation 14.5 composting process, the moisture status of the compost
where: must be maintained above the wettability threshold to
ODW = oven dried weight of compost, g, avoid dust problems and to maintain adequate moisture
ARW = as received weight of compost, g, for maintaining biological activity. Table 03.04-A1
M= percent moisture of as received compost, %, illustrates a hypothetical scenario where the wettability
B= oven dry weight of compost that was dried for a threshold was identified to be 15%, given the maximum
period of time, g, allowable time for re-wetting (t = critical).
A= percent moisture of partially dried compost, %,
Table 03.04-A1 Hypothetical data set indicating wettability
C= weight of compost after drying it for a period of threshold of a compost sample given the maximum allowable time
time, g, for re-wetting.
D= percent moisture of re-wetted compost, %
Moisture Content Final Moisture of Time to Rewet
E= oven dry weight of compost in filtering device after of Compost Sample Compost (%) is less than
wetting, g, (%) t=critical
F= weight of compost in filtering device before 30 35 yes
wetting, g,
25 34 yes
H= volume of water absorbed by compost, mL,
20 36 yes
∆DF = difference between percent moisture of rewet
compost and compost of 35%, 15 34 yes
IR = initial burette reading, mL, 10 28 No
FR = final burette reading, mL, and 5 25 No
CF = correction factor, volume of capillary per mL of the 0 20 No
water in burette, mL mL-1.

August 12, 2001 Test Methods for the Examination of Composting and Compost
03.04-10
Physical Examination
03.04 Wettability

Test Method: Wettability. Water-drop penetration Rate Units: min %-1


Test Method Applications
Process Management Product Attributes
Step 1: Step 2: Step 3: Step 4: Step 5: Step 6: Step 7: Safety Market
Feedstock Feedstock Composting Odor Treatment Compost Curing Compost Compost Standards Attributes
Recovery Preparation Screening and Storing and
Refining Packaging
03.04-B 03.04-B 03.04-B 03.04-B 03.04-B

03.04-B WATER-DROP PENETRATION RATE


LOOK—Interference and Limitations, and Sampling Handling received compost (oven dried at 70±5°C for 24 h or at
issues are presented as part of the introduction to this section. 105°C for 1 h or until change in mass is nil).
CONTRIBUTED BY—Dr. Brenda F. Farrell, Edaphos International
18.4 Place bags containing 20 cm3 samples in forced
16. Apparatus for Method B air oven preheated to 36°C.
16.1 Drying Oven—forced air, vented, temperature 18.5 At regular time intervals (e.g. after 0, 1, 2, 4, 8
set at 36°C. 24 and 36 h), sequentially remove each 20 cm3 sample
from the oven and subject it to the water-drop
16.2 Bag—brown paper, # 6, or other drying
penetration test.
container.
16.3 Sieve—4-mm mesh, plastic or stainless steel. 19. Procedure for Method B
16.4 Hamilton Syringe—250-µL. 19.1 Place 6 cm3 of partially dried compost into a set
of three petri dishes and gently flatten the compost
16.5 Petri Dishes—20, glass dim: 5 x 1 cm. slightly with a weighted flat surface.
17. Reagents and Materials for Method B 19.2 Place 3 drops (100 µL volume) of water on each
17.1 Water—type II, deionized 17 M!·cm water, compost sample. Make sure the drops are at least 1 cm
minimum standard. apart.
17.2 Brij 58—71.4 µM aqueous solution. Place 250 19.2.1 Surfactant Solutions—if a dry sample fails to
mL of water to a 500-mL volumetric flask. Add 0.04 g rewet and if the goal is to rewet this material,
of Brij 58. Add more water to a final volume of 500 19.2.1.1 In addition to water drops place 10 (100
mL. (optional) µL) drops of surfactant solution to the surface of the
17.3 Nonidet P-40—282 µM aqueous solution. Place compost. The concentration of the surfactant should be
250 mL of water to a 500-mL volumetric flask. Add at or below the critical micelle concentration.
0.085 g of Nonidet P-40. Add more water to a final 19.2.1.2 Compare the time required for water
volume of 500 mL. (optional). droplets to infiltrate the flattened sample (average of
17.4 Tween 20—9.92 µM aqueous solution. Place ten drops) and the time required for the wetting agent to
250 mL of water to a 500-mL volumetric flask. Add penetrate the surface of compost.
0.0065 g of Tween 20. Add more water to a final 19.2.1.3 Establish which of the surfactants (Tween
volume of 500 mL. (optional). 20, Brij 58, Nonidet P-40) increases the rate of wetting.
17.5 Other Surfactants—Use other suitable non-ionic 19.2.1.4 Repeat runs outlined below using lower
surfactant made up at its critical micelle concentration. dilutions of surfactant to identify the minimum effective
18. Sample Preparation for Method B surfactant concentration.

18.1 Pass approximately 200 cm3 of compost through 19.3 Observe and Record the time required for all
a 4-mm sieve to provide at least 175 cm3 of sieved water drops to penetrate the flattened compost sample.
material. 19.4 Stop the run at 1 h.
18.2 Blend sieved compost together 19.5 Determine the average time for penetration, if
18.3 Subdivide the < 4 mm material into subsamples. time is greater than 1 h, simply report penetration time
Place each 20 cm3 subsample into a bag. Take three to be greater than 1 h.
small subsamples, each from a different sample, to NOTE 1B—this experiment should be conducted in a room
where the humidity and temperature are controlled and or
determine the average moisture content of the as- constant (i.e., air-conditioned).

Test Methods for the Examination of Composting and Compost August 12, 2001
03.04-11
Physical Examination
Wettability 03.04

19.6 Repeat steps 19.1 to 19.5 for pairs of compost 20. Calculations and Corrections for Method B
sub-samples as they are removed from the drying oven 20.1 Determine the average observed time required to
and allowed to cool to room temperature. complete penetration for each pair of samples for each
sample moisture tested:
tavg = [t1 + t2+ ... + tn] ÷ n Equation 20.1
where:
tavg = average time to penetrate compost, min, and
t = time it takes each water drop to penetrate compost,
min,
n = run number, (i.e., 1 through 9).

August 12, 2001 Test Methods for the Examination of Composting and Compost
03.04-12
Physical Examination
03.04 Wettability

03.04 METHODS SUMMARY


21. Report surface tension of water and surfactant solutions; and
temperature and humidity in room during experiments.
21.1 Method 03.04-A Wicking Rate of Compost—
Report wettability threshold of compost, % at tcritical, 22. Precision and Bias
where % is moisture content and tcritical is the maximum 22.1 Method 03.04-A Wicking Rate of Compost—
allowable time for rewetting; actual time required to The precision and bias of this test have not been
rewet compost sample; bulk density of compost; force determined. Data are being sought for use in
added to compress compost (kg); concentration and developing a precision and bias statement.
type of surfactant used to improve wetting, if required;
22.2 Method 03.04-A Water-Drop Penetration
temperature and humidity in room where experiments
Rate—The precision and bias of this test have not been
were conducted; and surface tension of water and
determined. Data are being sought for use in
surfactant solutions.
developing a precision and bias statement.
21.2 Method 03.04-B Water-Drop Penetration
Rate—Report average time required for water drop to 23. Keywords
penetrate compost for each moisture level tested; initial 23.1 absorption; adsorption; sorption; fines;
moisture content of compost; bulk density of compost; hydrophobic; hydrophilic; surface tension; surfactant;
wettability; wettability index

Test Methods for the Examination of Composting and Compost August 12, 2001
03.04-13
Physical Examination
Wettability 03.04

August 12, 2001 Test Methods for the Examination of Composting and Compost
03.04-14
Physical Examination
03.05 Film Plastics

Test Method: Film Plastics. One Method. Units: cm2 m-3


Test Method Applications
Process Management Product Attributes
Step 1: Step 2: Step 3: Step 4: Step 5: Step 6: Step 7: Safety Market
Feedstock Feedstock Composting Odor Treatment Compost Curing Compost Compost Standards Attributes
Recovery Preparation Screening and Storing and
Refining Packaging
03.05-A 03.05-A

03.05 FILM PLASTICS


DISCLAIMERS into filaments. Plastic objects are undesirable
(1) The methodologies described in TMECC do not purport to address all
contaminants in finished composts.
safety concerns associated with their use. It is the responsibility of the
user of these methods to establish appropriate safety and health
3.2 film plastic, n—Shredded sheet plastic, man-made
practices, and to determine the applicability of regulatory limitations inert. The weight of film plastic is insignificant relative
prior to their use. to the bulk weight of as-received compost.
(2) All methods and sampling protocols provided in TMECC are subject to
revision and update to correct any errors or omissions, and to 4. Summary of Test Method
accommodate new widely accepted advances in techniques and
methods. Please report omissions and errors to the U.S. Composting 4.1 Method 03.05-A Film Plastic Surface Area
Council Research and Education Foundation. An on-line submission
form and instructions are provided on the TMECC web site,
Determinations Using Digital Processing—A proposed
http://www.tmecc.org. method using digital scanning and image processing to
(3) Process alternatives, trade names, or commercial products as mentioned quantify the relative surface area of film plastic present
in TMECC are only examples and are not endorsed or recommended by
the U.S. Department of Agriculture or the U.S. Composting Council
per unit volume of compost.
Research and Education Foundation. Alternatives may exist or may be
developed. 5. Significance and Use
COMMENT—This test was devised for use with mixed 5.1 Relative surface area determination of film
municipal solid waste and lawn and garden composts. The plastics, measured in cm2 m-3, can indicate its potential
outlined methods conform to conventional image scanning and
processing protocols. Refer to your digital image processing impact under different compost use scenarios. The
software users’ manual for use instructions. total mass of film plastics relative to bulk compost is
NOTE—Test methods presented in this section of TMECC very small. Error associated with mass determinations
should not be used in place of ASTM methods to certify throughout the process of sieving and drying may mask
degradability of plastics or other degradable materials (e.g., the aesthetic significance of the presence of film
ASTM D6400-99: Standard Specification for Compostable plastics. Also, organic carbon determinations with CO2
Plastics).
detection may be inflated due to the presence of
1. Scope petroleum-based carbon in film plastics.
1.1 This section covers the quantification of film 6. Interference and Limitations
plastics in air-dried composted materials.
6.1 Method 03.05-A Film Plastic Surface Area
1.1.1 Method 03.05-A Film Plastic Surface Area Determinations Using Digital Processing—Image
Determinations Using Digital Processing. processing software must be properly calibrated to
1.2 Values stated in SI units are to be regarded as the avoid inaccurate estimates of film plastics surface
standard. Values given in parentheses are provided for areas.
information only. 6.2 Data are being sought for further development of
2. Referenced Documents a Interference and Limitations statement.
NIH Image 1.61. Public Domain Image Processing 7. Sample Handling
Software for Macintosh™. US National Institute of 7.1 Method 03.05-A Film Plastic Surface Area
Health. http://www.nist.gov/lispix/imlab/labs.html.
Determinations Using Digital Processing—Material
August 2, 1993.
used in this test should represent in-process compost
3. Terminology product at 45-60% moisture (wet weight basis). The
3.1 plastic, n—Any of various organic compounds sample aliquot should be unsieved, as-received.
produced by polymerization, capable of being molded, 7.1.1 Quantity—250 cm3, four replicates, finished
extruded, cast into various shapes and films, or drawn compost.

Test Methods for the Examination of Composting and Compost August 12, 2001
03.05-1
Physical Examination
Film Plastics 03.05

Test Method: Film Plastics. Surface Area Determinations Using Digital Processing Units: cm2 m-3
Test Method Applications
Process Management Product Attributes
Step 1: Step 2: Step 3: Step 4: Step 5: Step 6: Step 7: Safety Market
Feedstock Feedstock Composting Odor Treatment Compost Curing Compost Compost Standards Attributes
Recovery Preparation Screening and Storing and
Refining Packaging
03.05-A 03.05-A

03.05-A FILM PLASTIC SURFACE AREA DETERMINATIONS USING DIGITAL


PROCESSING
LOOK—Interference and Limitations, and Sampling Handling 10.3 Inspect the material remaining on the screen and
issues are presented as part of the introduction to this section.
manually separate film plastics.
CONTRIBUTED BY—Wayne H. Thompson, Edaphos
International 10.4 Determine the surface area of film plastic.

8. Apparatus for Method A 10.4.1 Coat transparent film plastic. Transfer film
plastics into wide-mouth 500-mL bottle. Add
8.1 Sieve—4-mm, plastic, nylon or other durable approximately 50 cm3 of opaque coating agent. Cap
mesh. bottle. Shake vigorously until all transparent film
8.2 Desk Top Computer—with image scanning and plastics are coated. Separate excess coating agent from
processing capabilities. coated film plastics using a sieve.
8.3 Scanner—digital, flatbed, 8-bit gray scale capable 10.4.2 Assemble samples and calibration standard
(minimum). for scanning. Transfer the coated film plastic to a sheet
8.4 Bottle and Cap—wide-mouth, 500-mL or other of clean, white paper. Arrange the coated film plastics.
appropriate container with cover. Do not overlap fragments of film plastics. Cover the
film plastic and paper with clear acetate sheet.
8.5 Paper—opaque, A4 or 8.5×11 in. sheet.
NOTE 2A—Include a sample of known dimension for image
8.6 Acetate Sheet—clear, A4 or 8.5×11 in. sheet. calibration.
8.7 Area Calibration Standard—flat disc of known 10.4.3 Scan assembled sample as an 8-bit gray-scale
area dimension to be scanned as area calibration image. Place the prepared sample sheet face-down
reference with film plastic fragments. onto flatbed scanner. Capture the image as directed by
8.8 Image Processing and Analysis—software (e.g., the scanning software instructions. Save the scanned
Image-J - Image Processing and Analysis in Java. image to a file for further processing.
http://rsb.info.nih.gov/ij/). 10.4.4 Determine surface area of each assembled
9. Reagents and Materials for Method A sample. Using image processing software, import the
captured images of film plastics and convert the image
9.1 Coating Agent—Graphite powder, or other from gray scale to binary (i.e., 0 = black = plastics, 255
suitable translucent material to coat transparent film = white = background).
plastics.
10.4.4.1 Determine area in pixels for each piece of
CAUTION—Graphite powder spills on or near electronic
equipment can create severe complications and cause film plastic on white paper sheet.
equipment failures. 10.4.4.2 Determine area in pixels for sample with
10. Procedure for Method A known surface area.
10.1 Air Dry Sample—Analytically transfer a 1000 10.4.4.3 Sum area in pixels for all fragments of film
cm3 sample aliquot to a paper bag or other permeable plastic on the sheet. Multiply the sum by the area of one
container and air dry for at least two days at 36°C until pixel, cm2.
weight change diminishes to nil. 10.5 Repeat steps 10.4.4.1 through 10.4.4.3 three
3 times for each sheet of prepared samples until
10.2 Press the 250 cm air dried sample aliquot
through a 4-mm sieve. technician proficiency improves and variability
between runs diminishes to nil.
NOTE 1A—Determine cumulative surface area of film plastic
fragments > 4 mm. A 4-mm sieve will allow the flexible 4-mm 10.6 Repeat step 10.2 through step 10.4 for each of
film plastic sections to pass through a sieve without detection. the four 250 cm3 subsample of compost.

August 12, 2001 Test Methods for the Examination of Composting and Compost
03.05-2
Physical Examination
03.05 Film Plastics

11. Calculations for Method A 11.3 Calculate total surface area for 1000 cm3
11.1 Determine Area Conversion Coefficient: sample:
C = !(PSn ÷ AS) ÷ n Equation 11.1 TFP = !(AFP) Equation 11.3
where: where:
C = conversion factor used to convert pixels to cm2, AFP = surface area of film plastic for individual 250 cm3
cm2 per pixel, samples, and
PS = number of pixels occupied by sample with known TFP = total surface area of film plastic in 1,000 cm3
area, sample
AS = area cm2 of sample with known area, and 11.4 Correct Area to Volume Measurement (from
n = replication number (minimum = 3). 1000 cm3 sample volume to 1.0 m3):
11.2 Convert Film Plastic Area Measures from Pixels AT = TFP × 1,000 Equation 11.4
to Area Units, cm2: where:
AFP = PFP × C Equation 11.2 AT = total area of film plastics per cubic meter of
compost, cm2 m-3,
where:
TFP = total surface area of film plastic in 1,000 cm3
C = conversion coefficient to convert from pixels to
sample, and
cm2, cm2 per pixel, from equation 11.1,
1000 = conversion factor for cm3 to m3.
PFP = number of pixels occupied by graphite coated film
plastic, and
AFP = area of graphite coated film plastic, cm3.

Test Methods for the Examination of Composting and Compost August 12, 2001
03.05-3
Physical Examination
Film Plastics 03.05

03.05 METHODS SUMMARY


12. Report precision and bias of this test have not been
determined. Data are being sought for use in
12.1 Film plastic surface area is reported in square developing a precision and bias statement.
centimeters (cm2) per cubic meter (m3) of as-received
compost, cm2 m-3. Report the sample mean and 14. Keywords
standard deviation when three or more samples from 14.1 inerts; plastic; film plastics; image processing;
the same bulk are submitted for analysis. digital imagery; surface area; volume
13. Precision and Bias
13.1 Method 03.05-A Film Plastic Surface Area
Determinations Using Digital Processing—The

August 12, 2001 Test Methods for the Examination of Composting and Compost
03.05-4
Physical Examination
03.06 Glass Shards, Metal Fragments and Hard Plastics

Test Method: Glass Shards, Metal Fragments and Hard Plastics. One Method. Units: % g g-1 compost dw
Test Method Applications
Process Management Product Attributes
Step 1: Step 2: Step 3: Step 4: Step 5: Step 6: Step 7: Safety Market
Feedstock Feedstock Composting Odor Treatment Compost Curing Compost Compost Standards Attributes
Recovery Preparation Screening and Storing and
Refining Packaging
03.06-A 03.06-A

03.06 GLASS SHARDS, METAL FRAGMENTS AND HARD PLASTICS


DISCLAIMERS 3.2 metal, n—Any of a category of electropositive
(1) The methodologies described in TMECC do not purport to address all elements that usually have a shiny surface, are
safety concerns associated with their use. It is the responsibility of the generally good conductors of heat and electricity, and
user of these methods to establish appropriate safety and health
practices, and to determine the applicability of regulatory limitations can be melted or fused, hammered into thin sheets, or
prior to their use. drawn into wires. Typical metals form salts with
(2) All methods and sampling protocols provided in TMECC are subject to nonmetals, basic oxides with oxygen, and alloys with
revision and update to correct any errors or omissions, and to
accommodate new widely accepted advances in techniques and one another. An alloy of two or more metallic elements.
methods. Please report omissions and errors to the U.S. Composting An object made of metal.
Council Research and Education Foundation. An on-line submission
form and instructions are provided on the TMECC web site, 3.3 plastics, n—Any of various organic compounds
http://www.tmecc.org. produced by polymerization, capable of being molded,
(3) Process alternatives, trade names, or commercial products as mentioned
in TMECC are only examples and are not endorsed or recommended by extruded, cast into various shapes and films, or drawn
the U.S. Department of Agriculture or the U.S. Composting Council into filaments used as textile fibers. Objects made of
Research and Education Foundation. Alternatives may exist or may be
developed.
plastic.
NOTE—Test methods presented in this section of TMECC 3.4 sieve, n—A utensil of wire mesh or closely
should not be used in place of ASTM methods to certify perforated metal, used for straining or sifting compost.
degradability of plastics or other degradable materials (e.g.,
ASTM D6400-99: Standard Specification for Compostable 3.5 wet sieving, v—To wash compost and/or inert
Plastics). materials through a sieve with water and to collect
those materials that do not pass through the sieve for
1. Scope
further classification.
1.1 This section covers the quantification of glass
shards, metal fragments and hard plastics in finished 4. Summary of Test Methods
compost. 4.1 Method 03.06-A Glass Shards, Metal Fragments
1.1.1 Method 03.06-A Glass Shards, Metal and Hard Plastics Wet Sieving Technique—A
Fragments and Hard Plastics Wet Sieving Technique. destructive wet sieve technique for rapid quantification
of foreign matter in finished compost.
1.2 Values stated in SI units are to be regarded as the
standard. Values given in parentheses are provided for 4.1.1 A proposed method using a wet sieve technique
information only. is described. Replicated aliquots of as-received
compost are wet sieved to isolate glass shards, metal
2. Referenced Documents fragments and hard plastics. The presence of foreign
ASTM D 2217-85, Standard Practice for Wet Preparation matter relative to a bulk sample of compost material is
of Soil Samples for Particle-Size Analysis and determined and reported as a percentage on dw basis.
Determination of Soil Constants. In Annual Book of
ASTM Standards, Vol. 04.08. (Re-approved 1993). 5. Significance and Use
3. Terminology 5.1 Glass shards (4-mm to 13-mm) can pose a human
and animal hazard with unprotected exposure or
3.1 glass, n—Any of a large class of materials with through direct ingestion. Metal fragments can pose the
highly variable mechanical and optical properties that same hazard, and could be a potential source of trace
solidify from the molten state without crystallization, elements upon interaction with soil. Hard plastic can
are typically made by silicates fusing with boric oxide, be an aesthetic concern and in large quantities may
aluminum oxide, or phosphorus pentoxide, are affect physical properties of a compost-amended soil,
generally hard, brittle, and transparent or translucent, (e.g., soil coloring, heat retention, drainage).
and are considered to be supercooled liquids rather than
true solids.

Test Methods for the Examination of Composting and Compost August 12, 2001
03.06-1
Physical Examination
Glass Shards, Metal Fragments and Hard Plastics 03.06

6. Interference and Limitations 7. Sample Handling


6.1 Interference and limitations for this method have 7.1 Sample Size—1000 cm3, four replicates at 250
not been determined. Information is being sought to cm3 each.
develop a Interference and Limitations statement. 7.2 Sample Preparation—as-received finished
compost.

August 12, 2001 Test Methods for the Examination of Composting and Compost
03.06-2
Physical Examination
03.06 Glass Shards, Metal Fragments and Hard Plastics

Test Method: Glass Shards, Metal Fragments and Hard Plastics. Wet Sieve Units: % g g-1 dw
Technique
Test Method Applications
Process Management Product Attributes
Step 1: Step 2: Step 3: Step 4: Step 5: Step 6: Step 7: Safety Market
Feedstock Feedstock Composting Odor Treatment Compost Curing Compost Compost Standards Attributes
Recovery Preparation Screening and Storing and
Refining Packaging
03.06-A 03.06-A

03.06-A WET SIEVING TECHNIQUE


LOOK—Interference and Limitations, and Sampling Handling 10.5.2 Natural Inorganic Inerts—stones and
issues are presented as part of the introduction to this section.
concretions, and
NOTE—This test should not be used in place of ASTM methods
to certify degradability of plastics or other degradable materials, 10.5.3 Organic Fragments—organic materials that
i.e., ASTM D6400-99: Standard Specification for Compostable are not readily biodegradable such as wood chips,
Plastics. fragments of paper, etc.
COMMENT—This proposed test was prepared by W.H. 10.6 Transfer the recovered and classified inert
Thompson for use with mixed solid waste compost.
materials to clean, tared beakers.
8. Apparatus for Method A 10.7 Oven dry recovered inerts at 70±5°C for 18 h to
8.1 Water Delivery System—2-cm (3/4 in.) rubber, 24 h, until weight change or moisture loss diminishes to
tubing, garden hose or other equivalent . nil.
8.2 Evaporation Dish—four 250-mL beakers, four 10.8 Separate and classify oven-dried inert materials
100-mL beakers, glass. into descriptive categories, (e.g., glass shards, metal
8.3 Sieve—4-mm mesh, 20-cm diameter, plastic or fragments, and hard plastics).
equivalent. 10.9 Determine and record the individual net weight
8.4 Tweezers—sized for extracting ~ 4 mm fragments for each class of inerts, ±0.001 g.
from sample. 10.10 Repeat steps 10.4 through 10.9 for each
8.5 Forced Air Drying Oven—vented, capable of replicate, minimum of three replicates, four replicates
maintaining constant temperature, 70±5°C. are recommended.
8.6 Analytical Balance—capable of weighing 100 g, 10.11 Perform calculations for each class of inert.
accurate to ±0.001 g. 11. Calculations for Method A
9. Reagents and Materials for Method A 11.1 Perform the following calculations for each
9.1 Water—continuous flow source, tap water. replicate. Determine the mean and standard deviation
for each inert class.
10. Procedure for Method A
11.1.1 Inert Content by Type, % w/w:
10.1 Transfer four 250 cm3 aliquots of unsieved Xi = A ÷ B Equation 11.1
finished compost to each of four tared 250-mL beakers.
11.1.2 Total Inert Content, %:
10.2 Determine and record weight of each 250 cm3 n
as-received moist sample aliquot. C= x
i =1
i
Equation 11.2
10.3 Determine and record the sample total solids and
moisture content on a parallel aliquot. where:
X = percent inert by type, % g g-1,
10.4 Wash each replicate sample through a 4-mm
sieve. i = inert type, (e.g., hard plastics, metal, glass, stones,
wood chips, etc.),
10.5 Inspect sieve accepts, wet material remaining on A = oven dry weight of recovered inert, g,
the screen, and separate clearly identifiable inert B = oven dry weight of the 250 cm3 compost sample
materials. aliquot, g, and
10.5.1 Man-Made Inerts—glass shards, metal C = sum of inerts, tally of percentages for all inert
fragments and hard plastics, classes, % w/w.

Test Methods for the Examination of Composting and Compost August 12, 2001
03.06-3
Physical Examination
Glass Shards, Metal Fragments and Hard Plastics 03.06

03.06 METHODS SUMMARY


12. Report 13. Precision and Bias
12.1 Report the following information: 13.1 Percent Glass Shards, Metal Fragments and
12.1.1 Express results for each inert type identified Hard Plastics:
in the compost sample on an oven-dried basis to the 13.1.1 Method 03.06-A Glass Shards, Metal
nearest ±0.1 % g g-1. Fragments and Hard Plastics Wet Sieving Technique—
12.1.2 Express results for the sum of inerts in the The precision and bias of this test have not been
compost on an oven-dried basis to the nearest ±0.1 % g determined. Data are being sought for use in
g-1. developing a precision and bias statement.
14. Keywords
14.1 glass; metal; plastic; inerts; sieve

August 12, 2001 Test Methods for the Examination of Composting and Compost
03.06-4
Physical Examination
03.07 Process to Reduce Sharps

Test Method: Process to Reduce Sharps. Units: %, g g-1 dw


Test Method Applications
Process Management Product Attributes
Step 1: Step 2: Step 3: Step 4: Step 5: Step 6: Step 7: Safety Market
Feedstock Feedstock Composting Odor Treatment Compost Curing Compost Compost Standards Attributes
Recovery Preparation Screening and Storing and
Refining Packaging
03.07 03.07 03.07 03.07

03.07 PROCESS TO REDUCE SHARPS


DISCLAIMERS 1.3 When appropriate, compost product intended for
(1) The methodologies described in TMECC do not purport to address all sale or distribution shall be treated for the effective
safety concerns associated with their use. It is the responsibility of the removal of sharps, including steel sewing needles and
user of these methods to establish appropriate safety and health
practices, and to determine the applicability of regulatory limitations straight pins, stainless steel hypodermic needles, wire
prior to their use. snip ends, and metal shavings.
(2) All methods and sampling protocols provided in TMECC are subject to
revision and update to correct any errors or omissions, and to 2. Summary of Test Methods
accommodate new widely accepted advances in techniques and
methods. Please report omissions and errors to the U.S. Composting 2.1 A suitable laboratory method to detect sharps has
Council Research and Education Foundation. An on-line submission not been devised.
form and instructions are provided on the TMECC web site,
http://www.tmecc.org. 2.2 Recommended Process—Treatment shall take
(3) Process alternatives, trade names, or commercial products as mentioned place after product particle size and texture is reduced
in TMECC are only examples and are not endorsed or recommended by
the U.S. Department of Agriculture or the U.S. Composting Council to a fine, uniform soil-like material - characteristic of
Research and Education Foundation. Alternatives may exist or may be stable to very stable compost and may be by a
developed.
combination of the following provisions:
1. Scope
2.2.1 by subjecting product to magnetic separation
1.1 Sharps are stainless steel hypodermic needles, and devices designed to remove ferrous items after compost
steel sewing needles and straight pins that can pose a curing; and
human and animal puncture hazard with unprotected
2.2.2 by subjecting product to an eddy current device
exposure. Although some of these items can harbor
designed to remove metallic materials after compost
pathogens, possible infection will be eliminated by the
curing following ferrous separation; or
Process to Further Reduce Pathogens (PFRP, US EPA
40 CFR Part 503). Long term, sharps can be oxidized 2.2.3 by sifting cured product through a physical
in soil and introduce trace elements. Sharps are inert separation device, such as an air flotation fluidized bed
material and may be considered as a separate category separator (destoner) equipped with a punched ±2.5 mm
of inerts, (e.g., sharps). round, or equally effective, hole-size deck screen,
designed for removal of stainless steel hypodermic
1.2 The Process to Reduce Sharps (PRS) is a
needles.
recommended process standard drafted by the USCC
Standards and Practices Committee, rather than a 3. Keywords
recommended product standard and is subject to peer 3.1 hypodermic needle; needles; Process to Reduce
review. Sharps; PRS; sharps; straight pins

Test Methods for the Examination of Composting and Compost August 12, 2001
03.07-1
Physical Examination
Process to Remove Sharps 03.07

August 12, 2001 Test Methods for the Examination of Composting and Compost
03.07-2
Physical Examination
03.08 Man Made Inerts

Test Method: Man Made Inerts. One Method. Units: % g g-1 dw


Test Method Applications
Process Management Product Attributes
Step 1: Step 2: Step 3: Step 4: Step 5: Step 6: Step 7: Safety Market
Feedstock Feedstock Composting Odor Treatment Compost Curing Compost Compost Standards Attributes
Recovery Preparation Screening and Storing and
Refining Packaging
03.08-A 03.08-A 03.08-A 03.08-A 03.08-A

03.08 MAN MADE INERTS


DISCLAIMERS 3.3 metal, n—Any of a category of electropositive
(1) The methodologies described in TMECC do not purport to address all elements that usually have a shiny surface, are
safety concerns associated with their use. It is the responsibility of the generally good conductors of heat and electricity, and
user of these methods to establish appropriate safety and health
practices, and to determine the applicability of regulatory limitations can be melted or fused, hammered into thin sheets, or
prior to their use. drawn into wires. Typical metals form salts with
(2) All methods and sampling protocols provided in TMECC are subject to nonmetals, basic oxides with oxygen, and alloys with
revision and update to correct any errors or omissions, and to
accommodate new widely accepted advances in techniques and one another. An alloy of two or more metallic elements.
methods. Please report omissions and errors to the U.S. Composting An object made of metal.
Council Research and Education Foundation. An on-line submission
form and instructions are provided on the TMECC web site, 3.4 plastics, n—Any of various organic compounds
http://www.tmecc.org. produced by polymerization, capable of being molded,
(3) Process alternatives, trade names, or commercial products as mentioned
in TMECC are only examples and are not endorsed or recommended by extruded, cast into various shapes and films, or drawn
the U.S. Department of Agriculture or the U.S. Composting Council into filaments. Objects made of plastic.
Research and Education Foundation. Alternatives may exist or may be
developed. 3.5 wood chips, n—A compost bulking agent or
1. Scope mulching material as chips > 9.5 mm (! in.). Wood
chips with particle size < 9.5 mm are considered to be
1.1 This section covers the quantification of man- compost.
made inert materials in compost.
4. Summary of Test Methods
1.1.1 Method 03.08-A Classification of Inerts.
4.1 Method 03.08-A Classification of Inerts by Sieve
1.2 Values stated in SI units are to be regarded as the Size—Inerts may be classified for each sieve size
standard. Values given in parentheses are provided for fraction. Size fractions can include 50, 25, 16, 9.5, 6.3,
information only. 4 and 2 mm. Inerts are hand sorted and classified for
2. Referenced Documents each size fraction.
2.1 TMECC: 4.1.1 Man-made inert content greater than 4 mm are
Method 02.01-B Sample Sieving for Aggregate Size determined by passing four replicates of 250 cm3 oven
Classification. dried (70±5C°) samples of the compost through a 4-
Method 02.01-C Man-Made Inert Removal.
mm sieve. Material remaining on the sieve is visually
inspected and sorted. Clearly identifiable man-made
Method 03.05 Film Plastics
inerts, including glass, metal, and hard plastic, are
Method 03.06 Glass Shards, Metal Fragments and Hard separated.
Plastics
4.1.2 After the inerts > 4 mm and sharps > 2 mm are
3. Terminology removed, the sample is milled and an aliquot is used for
3.1 glass, n—Any of a large class of materials with heavy metals analysis and other tests that require finely
highly variable mechanical and optical properties that milled sample aliquots.
solidify from the molten state without crystallization,
5. Significance and Use
are typically made by silicates fusing with boric oxide,
aluminum oxide, or phosphorus pentoxide, are 5.1 Glass and metal shards 4-13 mm pose a human
generally hard, brittle, and transparent or translucent, and animal hazard with unprotected exposure or
and are considered to be supercooled liquids rather than through direct ingestion. Metal fragments may pose the
true solids. same hazard, and are a potential source of trace metal
contamination. Hard plastic is an aesthetic concern and
3.2 man-made inerts, n—includes synthetic textiles,
can modify the physical properties of the soil when
plastics, metal objects, and glass.
present in significant quantities.

Test Methods for the Examination of Composting and Compost August 12, 2001
03.08-1
Physical Examination
Man Made Inerts 03.08

5.2 Soil is composed of particles of material equal to 7. Sample Handling


or less than 2 mm in size. Particles larger than 2 mm 7.1 Perform inert screening tests on size-classed
are either gravel or foreign matter. Foreign matter of samples (Method 02.02-B). If elemental analysis will
interest in compost as a soil amendment is man-made be performed on samples following inert classification
inert material greater than 4 mm. Foreign matter and removal, store material in a sealed container at
particle sizes larger than 4 mm is an aesthetic concern, room temperature to minimize sample moisture
possibly a safety concern, and may impact soil physical changes.
and chemical properties.
7.2 The < 9.5 mm fraction is air dried at a
6. Interference and Limitations temperature of 36°C to minimize loss of volatile
6.1 Interference and limitations have not been compounds and elements such as mercury.
determined for this test. Information is being sought to
formulate a Interference and Limitations statement.

August 12, 2001 Test Methods for the Examination of Composting and Compost
03.08-2
Physical Examination
03.08 Man Made Inerts

Test Method: Man Made Inerts. Classification of Inerts. Units: % g g-1 dw


Test Method Applications
Process Management Product Attributes
Step 1: Step 2: Step 3: Step 4: Step 5: Step 6: Step 7: Safety Market
Feedstock Feedstock Composting Odor Treatment Compost Curing Compost Compost Standards Attributes
Recovery Preparation Screening and Storing and
Refining Packaging
02.02-B 02.02-B 02.02-B 02.02-B 02.02-B
02.02-C 02.02-C 02.02-C 02.02-C 02.02-C
03.05-A 03.05-A
03.06-A 03.06-A

03.08-A CLASSIFICATION OF INERTS


LOOK—Interference and Limitations, and Sampling Handling 8.2 Method 02.02-C Man-Made Inert Removal; or
issues are presented as part of the introduction to this section.
8.3 Method 03.05-A Film Plastic Surface Area
8. TMECC Methods: Determinations Using Digital Processing; or
8.1 Method 02.02-B Sample Sieving for Aggregate 8.4 Method 03.06-A Glass Shards, Metal Fragments
Size Classification, and and Hard Plastics Wet Sieving Technique.

Test Methods for the Examination of Composting and Compost August 12, 2001
03.08-3
Physical Examination
Man Made Inerts 03.08

August 12, 2001 Test Methods for the Examination of Composting and Compost
03.08-4
Physical Examination
03.09 Total Solids and Moisture

Test Method: Total Solids and Moisture. One Method Units: % g g-1 wet basis
Test Method Applications
Process Management Product Attributes
Step 1: Step 2: Step 3: Step 4: Step 5: Step 6: Step 7: Safety Market
Feedstock Feedstock Composting Odor Treatment Compost Curing Compost Compost Standards Attributes
Recovery Preparation Screening and Storing and
Refining Packaging
03.09-A 03.09-A 03.09-A 03.09-A 03.09-A 03.09-A 03.09-A 03.09-A 03.09-A

03.09 TOTAL SOLIDS AND MOISTURE


DISCLAIMERS 3. Terminology
(1) The methodologies described in TMECC do not purport to address all
safety concerns associated with their use. It is the responsibility of the
3.1 ash, n—The inorganic matter, or mineral residue
user of these methods to establish appropriate safety and health of total solids that remains when a compost or
practices, and to determine the applicability of regulatory limitations feedstock is combusted at 550°C in the presence of
prior to their use.
(2) All methods and sampling protocols provided in TMECC are subject to
excess air; Fixed Solids, % g g-1.
revision and update to correct any errors or omissions, and to
accommodate new widely accepted advances in techniques and
3.2 biodegradable volatile solids, n—The
methods. Please report omissions and errors to the U.S. Composting biodegradable portion of total solids that volatilizes to
Council Research and Education Foundation. An on-line submission carbon dioxide and other gasses when a compost or
form and instructions are provided on the TMECC web site,
http://www.tmecc.org. feedstock is combusted at 550°C in the presence of
(3) Process alternatives, trade names, or commercial products as mentioned excess air, % g g-1.
in TMECC are only examples and are not endorsed or recommended by
the U.S. Department of Agriculture or the U.S. Composting Council 3.3 fixed solids, n—The inorganic matter, or mineral
Research and Education Foundation. Alternatives may exist or may be residue of total solids that remains when a compost or
developed.
feedstock is combusted at 550°C in the presence of
1. Scope excess air; Ash, % g g-1.
1.1 This section covers the determination of total 3.4 moisture content, n—The liquid fraction
solids and moisture content of feedstocks and (percentage) of a compost or feedstock that evaporates
composts. at 70±5°C, % g g-1.
1.1.1 Method 03.09-A Total Solids and Moisture at 3.5 total solids, n—The solid fraction (percentage) of
70±5°C. a compost or feedstock that does not evaporate at
1.2 Values stated in SI units are to be regarded as the 70±5°C, which consists of fixed solids, biodegradable
standard. Values given in parentheses are provided for volatile solids, and volatile solids that are not readily
information only. biodegradable, % g g-1.

2. Referenced Documents 4. Summary of Test Method


2.1 TMECC: 4.1 Method 03.09-A Total Solids and Moisture at
70±5°C—An aliquot of a well-mixed, as-received, bulk
Method 03.02 Ash.
sample is weighed, oven dried at 70±5°C to steady state
2.2 Other References: and re-weighed. The remaining dry solids fraction
ASTM D 2974-87, Standard Test Methods for Moisture, represents the total solids, and the evaporated fraction
Ash, and Organic Matter of Peat and Other Organic represents percent moisture.
Soils. In Annual Book of ASTM Standards, Vol. 04.08.
(Re-approved 1995). 4.1.1 Total solids and percent moisture of feedstock,
in-process material, and finished compost products are
Cohen, I.R. 1973. Laboratory Procedure for the
Preparation of Solid Waste Related Materials for