Soil
Sampling
CRL
Environmental
Corporation
Presentation Overview
Part I:
Basic Sampling Concepts,
Sampling Plan
Part II:
Sampling Design, Sampling
Techniques
Definitions
What is a Sample ?
A portion of a population or lot. It may
consist of an individual or group of
individuals
Comprise of one matrix
For one location and
one sampling event
Definitions
• the degree to which a property or
Homogeneity substance is uniformly distributed
throughout a material.
Heterogeneity • non-uniform throughout an object
• the quantity chosen for the analysis
• Chemical vs. Statistical:
• Statisticians – the number of units in a
Sample Size
4 physical sample
• Chemists – mass, weight, volume of the
physical sample
Definitions
Sampling
• is a process of selecting a portion of material small enough in volume
to be transported conveniently and handled in the laboratory, while
still accurately representing the part of the environment sampled
Representative Sampling
• the process of obtaining a representative sample or a representative
set of samples. (ASTM, D6044-96, 2009)
Sub Sampling
• A portion of material taken from a larger quantity for the
purpose of estimating properties or composition of the
whole sample
Sampling Concepts
Exploratory Sampling goals – (surveillance) provide
preliminary information about the site or material being analyzed.
Monitoring Sampling goals – (assessment)
undertaken for regulatory enforcement or non regulatory purposes;
initiated to provide information on the variation in the specific period,
and specific area.
A Good Sampling Goal follows a sampling protocol that produces a
sample whose chemical/physical measurements of interest are:
•Representative of the entire lot and
•As consistent as possible, with other samples that would be obtained
if the entire sampling protocol could be repeated.
Outline of Generalized Sampling Protocol
Main point program purpose Sub-elements
Analytes of interest Primary and secondary chemical constituents and criteria
for representativeness
Locations Design, construction, and performance evaluation
Sample Collection Mechanism, materials, & methodology
Sample Handling Preservation, filtration, & field control samples
Field Determinations Unstable species and additional sampling variables
Sample storage and transport Preservation of sample integrity
Hazardous Waste Sampling Plan
Protocols
Objective for Information of
the facility/
Sampling establishment
Event
Sampling
Team
Discharge
Sampling Plan Location
Lab Sampling
Management Criteria &
& Data Analysis
Reporting Sampling
Program
& Field
QA/QC
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Types of Sampling
Types of Sampling
Grab or Catch Sampling
is a discrete sample which collected at a
specific location at a certain point in
time.
Soil Sampling
Depth
•Surface soil at a depth of about 20-cm.
• Common sample depth combinations:
• 0-15cm (0-6”) and 15-60cm (6”-24”) or
• 0-30cm (0-12”) & 30-60cm (12”-24”)
•If nutrients leaching and salinity are monitored, sampling
depth is at 60-100cm
•If organic matter and/or pH: 0-15cm (0-6”)
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Types of Sampling
Composite Sampling
is made by thoroughly mixing
several grab samples. It may be
made up of samples taken at
different locations, or at different
points in time.
Composite Methodology
Soil/fill type
- Discrete subsamples that are to be composited must be collected
from the same soil horizon and depth interval
- -Discrete subsamples must be of similar characteristics, for
example particle size and soil type, and from fill of similar origins
14
Composite Sampling
Location of sample points
Location of sample points in
in a 19 sample point plan,
a 7 sample point plan, with
with detail of compositing
detail of compositing design
design
……….Composite Sampling
Composite sampling must not be used:
• Determine the extent of contamination, eg. ESA
• Assessment of occupational health and safety risks in
relation to site remediation activities
• for validation purposes after remediation
• High clay content
• for volatile compounds and semi-volatile such as PAH and
TPH (gas)
• for leachate analysis
• If the site includes fill of uncertain origin or quality
……….Composite Sampling
Composite Sampling with Re-Testing
Sampling Design
(Selection of Sampling Method)
• Probability Sampling
1
• Non-Probability (Authoritative Sampling)
2
• Haphazard Sampling
3
• Search Sampling
4
Simple Random Sampling
Random – Random sampling means that any portion of
the sample population has the same probability of being taken.
It is often used for production operations that are continuous. It
is also used with constraints, such as the collection of a random
sample during the first, middle, and last third of a production lot
that must be analyzed separately to determine if the lot is
homogeneous.
Figure 1: Randomly
located area of residual
contamination within the
sampling circle
Recommended Sample Sizes
Sampling (ft2) Radius of sampling Percent of oil spills Sample Size
circle (ft)
≤ 50 ≤4 32.5 7
51 – 400 4 – 11.3 50.0 19
> 400 > 11.3 17.5 3719
Sampling Design Appropriate conditions Advantages Limitations
for use
Probability Sampling
Simple Random Useful when the Provides statistically Least preferred if
Sampling population of interest is unbiased estimates of patterns or trends are
relatively homogeneous the man, proportions, known to exist and are
and the variability identifiable.
Easy to understand and Localized clustering of
implement sample points can occur
-can calculate the
accuracy of results
Sampling over Space Sampling over Time or Along a Transect
Stratified Random Sampling
Stratified – is a design where the target population is divided into parts or
subregions called strata for the purpose of getting a better estimate of the
mean or total for the entire population. It involves specification of depth,
size, color or some characteristic that must be considered in meeting the
objective of the analysis.
21
Sampling Design Appropriate Advantages Limitations
conditions for use
Probability Sampling
Stratified Most useful for -Ensures more -Requires some
Random estimating a uniform coverage of prior knowledge of
Sampling parameters of wastes the entire target the waste or media
exhibiting high population to define strata and
heterogeneity -Potential for to obtain a more
achieving greater precise estimate of
precision in the mean.
estimates of the -Statistical
mean and variance procedures of
-May reduce costs calculating the
over simple random number of samples,
and systematic the mean, and the
sampling variance are more
-Enables complicated
computation of
22
reliable estimates
for population
Systematic Sampling
Systematic – Systematic samples are collected at predetermined
intervals that are defined in the sampling plan.
- It makes no assumptions about distribution or movement of analytes
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Soil Sampling Methods
24
Figure 1: Location of sampling points in a
7-point grid
The outer boundary of the
contaminated area is assumed to
be 4 feet from the center (C) of
the spill site
Parameters of hexagonal sampling designs for a sampling circle
No. of points Distance between adjacent Radius of smallest circle
points, s (ft) certain to be sampled
7 0.87r 0.5r
19 0.48r 0.28r
37 0.3r 0.19r
25
The outer boundary of
the contaminated area
is assumed to be 10
feet from the center
(C) of the spill site
Figure 1: Location of sampling
points in a 19-point grid
26
Sampling Design Appropriate conditions Advantages Limitations
for use
Probability Sampling
Systematic Useful for estimating spatial Preferred over simple May be misleading if the
Sampling patterns or trends over time random when sample sampling interval is
locations are random aligned with the pattern of
within each systematic contamination, which
block or interval could happen
Practical and easy inadvertently if there is
method for designating inadequate prior
sample locations. knowledge of the pattern
Ensures uniform of contamination
coverage of site, unit, or Not truly random, but can
process be modified through use
May be lower cost than of the random within
simple random sampling blocks design
because it is easier to
implement.
27
Sampling Design
Authoritative (Judgmental Sampling)
Non-
Probability Convenience Sampling
Sampling
Quota Sampling
Consecutive Sampling
Snowball Sampling
Judgmental Sampling
– implements assumptions about movement and distribution
with time, distance (fate and transport)
Sampling Design Appropriate conditions Advantages Limitations
for use
Authoritative Sampling
Judgmental -Useful for generating rough Can be very efficient with -highly dependent on
Sampling estimates of the average sufficient knowledge of expert knowledge of
concentration the site or waste waste
-obtain preliminary generation process -Nonprobability based so
information about a waste Easy to do and explain inference to the general
stream or site population is difficult
-To assess the usefulness of -Cannot determine
samples drawn reliable estimates of
-To screen samples in the variability
field -Statistical measures of
uncertainty cannot be
developed with
authoritative sampling
-human judgment error
Biased Sampling Useful to estimate worst-
case or best-case
conditions (e.g. to identify
the composition of a leak,
spill or waste of unknown
30 composition
Haphazard Sampling
– "any sampling location will do“; encourages taking samples at
convenient locations or times, which can lead to biased estimates
of means and other population characteristics.
- A very homogeneous population over time and space
-This method of selection is not recommended due to difficulty in
verifying this assumption
Search Sampling
-is conducted to locate pollution sources or to find "hot spots" of
elevated contamination
-Useful when historical information, site knowledge, or prior
samples indicate where the object of the search may be found.
Sample Handling Requirements
Parameter Matrix Container & Preservation Holding
Volume Time
Requirement
PCBs/OCPs Soil 100 grams Cool, ≤6oC 14 days/ 40
Amber Glass, teflon- ext.
line cap
Chlorinated Herbicides Soil 100 grams Cool, ≤6oC 14 days/ 40
(2,4-D & 2,4,5-T) Amber Glass, teflon- days upon
line cap extraction
VOCs (THMs, BTEX) Soil 4 oz, zero- Cool, ≤6oC 14 days
headspace Teflon
cap
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Sample Handling Requirements
Parameter Container Minimum Sample Preservation Holding Time
Size
TPH –Diesel 4 oz, clear wide mouth 100 grams Cool, ≤6oC 14 days
(soil) glass,
Teflon cap
TPH-Gasoline 4 oz, clear wide mouth 100 grams Cool, ≤6oC 14 days
(soil) glass,
Teflon cap, zero
headspace
Metals P, G 250 grams Cool, ≤6oC 6 mos.
28 days (Hg)
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Recommended Methods
Description Method
Ignitability EPA 1010 or 1020
Corrosivity EPA 9040 or 1110, 9045C
Reactivity EPA 9010 or 9030
Toxicity TCLP (EPA 1311), SPLP, Elution Test
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Recommended Methods
(Solid and Hazardous wastes)
Description Method
Organics
Pesticides Gas Chromatography EPA 8081/ EPA 8141
PCBs Gas Chromatography (EPA 8082)
VOCs SW 846 Method 8260
SVOCs SW 846 Method 8270
Herbicides Gas Chromatography (Method 8151)
Hydrocarbons Gas Chromatography (Method 8015)
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Recommended Methods
(Sediments, sludge, solid and Hazardous wastes)
Description Method
Heavy Metals (Cd, Cr, Wet ashing with HNO3 & HCl (SW846 Method 3050A) /
Pb) * Flame AAS /* ICP (EPA 6010)
Heavy Metals Wet ashing with HNO3 & HCl (SW846 Method 3050A) /
(As) * Hydride - AAS /* ICP (EPA 6010)
Cold Vapor Technique (AAS)
Hg, total
(SW846 Method 7471A)
CN ISE Method
Hexavalent Chromium Alkaline Digestion (EPA 3060A/EPA 7196A)
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Sample Handling Requirements
Parameters Method Description Mesh Size
Particle Size Analysis Hydrometer Method %sand, %silt, %clay
Organic Matter Content Titrimetry (FAS) method 0.15mm (air dry)
pH Glass Electrode 2 mm (air dry)
Electrical Conductivity (EC) conductivity meter 2 mm (air dry)
Total and available N Titrimetry (Kjeldahl Method) 0.15mm (air dry)
Colorimetry (Ammonium-
Total and available P 0.15mm (air dry)
VanadoMolybdate Method)
Total and available K Flame AAS 2 mm (air dry)
Exchangeable basic cations
-Potassium Flame AAS (By calculation) 2 mm (air dry)
-Sodium Flame AAS (By calculation) 2 mm (air dry)
Flame AAS (By calculation);EDTA
-Calcium Titration 2 mm (air dry)
Flame AAS (By calculation);EDTA
-Magnesium Titration 2 mm (air dry)
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Sample Handling Requirements
Parameters Method Description Mesh Size
Exchangeable acidity Titrimetry 2 mm (air dry)
Exchangeable aluminum ICP 2 mm (air dry)
Medium to fine textured;
Cation Exchange Capacity Ammonium Acetate Method
or, coarse textured (air dry)
Base Saturation, % By computation
Total Elements (As, Cd, Co, Cu,
Flame AAS 2 mm (air dry)
Cr, Fe, Hg, Mn, Mo, Ni, Pb, Zn)
Turbidimetric/ Gravimetry (BaSO4
Total Elements (Sulfur) 2 mm (air dry)
Method)
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Thank you for your kind attention!
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Environmental
Corporation
