TMECC
TMECC
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
CO-EDITORS
Name Affiliation
Leege, Philip B. The Philip B. Leege Company, Ltd.
Cincinnati, 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
August 12, 2001 Test Methods for the Examination of Composting and Compost
viii
Acknowledgments
Test Methods for the Examination of Composting and Compost August 12, 2001
ix
Acknowledgments
August 12, 2001 Test Methods for the Examination of Composting and Compost
x
Table of Contents
TABLE OF CONTENTS
01.00 INTRODUCTION
Test Methods for the Examination of Composting and Compost August 12, 2001
xi
Table of Contents
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
August 12, 2001 Test Methods for the Examination of Composting and Compost
xii
Table of Contents
Test Methods for the Examination of Composting and Compost August 12, 2001
xiii
Table of Contents
August 12, 2001 Test Methods for the Examination of Composting and Compost
xiv
Table of Contents
Test Methods for the Examination of Composting and Compost August 12, 2001
xv
Table of Contents
07.00 PATHOGENS
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
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.
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.
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.
TMECC TMECC
Preliminary Draft, 1995 First Edition, 1998
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”.
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.
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
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
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.
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
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
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
Fig 5. Stage IV of the TMECC Project. Round-robin testing through the CAP testing
program.
SPAC Co-Editors
TMECC
Addenda to the USGPO
Release, 2002
USDA Co-Editors
Editor-in-Chief
SSSA Co-Editors
IPSC Co-Editors
TMECC
Addenda to the USGPO
Release, 2002
USDA Co-Editors
CCREF/USCC
Editor-in-Chief
SSSA Co-Editors
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-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
Test Methods for the Examination of Composting and Compost August 12, 2001
01.00-1
Introduction
The Composting Process 01.02
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.
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
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
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 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.
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
Amendments
7. Compost Storing
Finished Products
Second Level Detail Model Turning and and Packaging
Mixing
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 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
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
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
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
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
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
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20
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
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
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
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
02.01-D 02.01-D
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
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 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
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
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
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
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
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
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
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
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 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
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
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
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
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
Test Methods for the Examination of Composting and Compost August 12, 2001
03.01-7
Physical Examination
Air Capacity 03.01
August 12, 2001 Test Methods for the Examination of Composting and Compost
03.01-8
Physical Examination
03.01 Air Capacity
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
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
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
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
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
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
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.
August 12, 2001 Test Methods for the Examination of Composting and Compost
03.02-8
Physical Examination
03.03 Bulk Density
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
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
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.
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
γ lv
γlv
γ sv γ lv γ sv γ sv
θ θ θ
γsl γ sl
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
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
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
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
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 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
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
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
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
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
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
August 12, 2001 Test Methods for the Examination of Composting and Compost
03.06-4
Physical Examination
03.07 Process to Reduce Sharps
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 Methods for the Examination of Composting and Compost August 12, 2001
03.08-1
Physical Examination
Man Made Inerts 03.08
August 12, 2001 Test Methods for the Examination of Composting and Compost
03.08-2
Physical Examination
03.08 Man Made Inerts
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