Ohio EPA

State of Ohio Environmental Protection Agency

Manual of Ohio EPA

Sludge Program Field Sampling Methods

And

Quality Assurance Practices

Document Revision: 0
Date: 04/08/2009

Division of Surface Water

Document Name: Sludge Program QA Document Revision: 0
Sludge Program Field Sampling Manual Table of Contents Date: 04/08/2009

Table of Contents

Part I: Section Name (SOP): Soil and Soil/Sludge Sampling Page

Soil and Soil/Sludge Sampling 1 of 4

A. Equipment Preparation 1 of 4
B. Sample Collection Procedure 1 of 4
C. Sample Documentation 2 of 4
D. Chain-of-Custody 3 of 4
E. Laboratory Coordination 3 of 4
F. References (additional information) 4 of 4

Appendix 1 1 of 6
Table 1: Parameter, analytical method, maximum holding time, sample
preservation and comments for soil and soil/sludge sampling 2 of 6
Table 1: A Physical Characteristics, Total Nutrients and Dioxin 2 of 6
Table 1: B Total Metals 4 of 6
Table 1: C. Organisms 6 of 6

Part II: Section Name (SOP): Liquid Sludge Sampling

Liquid Sludge Sampling

A. Equipment Preparation 1 of 4
B. Sample Collection Procedure for Liquid Sludge Being Transferred 1 of 4
1. Anaerobically Digested Sludge 1 of 4
2. Aerobically Digested Sludge 1 of 4
3. Thickened Sludge 1 of 4
4. Heat Treated Sludge 2 of 4
C. Sample Documentation 2 of 4
D. Chain-of-Custody 3 of 4
E. Laboratory Coordination 3 of 4
F. References (additional information) 4 of 4

Appendix 1 1 of 6
Table 1: Parameter, analytical method, maximum holding time, sample
preservation and comments for soil and soil/sludge sampling 2 of 6
Table 1: A Physical Characteristics, Total Nutrients and Dioxin 2 of 6
Table 1: B Total Metals 4 of 6
Table 1: C. Organisms 6 of 6

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Table of Contents (continued)

Part III: Section Name (SOP): Cake Sludge Sampling Page

Cake Sludge Sampling

A. Equipment Preparation 1 of 4
B. Sample Collection Procedure for Cake Sludge Being Transferred 1 of 4
1. Dried, Composted, or Thermally Reduced 1 of 4
2. Dewatered: Belt Filter Press, Centrifuge, or Vacuum Filter Press 1 of 4
3. Press: Plate or Frame 1 of 4
4. Drying Beds 2 of 4
5. Composite Piles 2 of 4
C. Sample Documentation 2 of 4
D. Chain-of-Custody 2 of 4
E. Laboratory Coordination 3 of 4
F. References (additional information) 4 of 4

Appendix 1 1 of 6
Table 1: Parameter, analytical method, maximum holding time, sample
preservation and comments for soil and soil/sludge sampling 2 of 6
Table 1: A Physical Characteristics, Total Nutrients and Dioxin 2 of 6
Table 1: B Total Metals 4 of 6
Table 1: C. Organisms 6 of 6

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Section Name (SOP): Part I Soil and Soil/Sludge Sampling Date: 04/08/2009

Part I: Soil and Soil/Sludge Sampling

The type of sampling and analyses are dependent upon factors such as the volume of
sludge produced annually, the type of treatment performed on the sludge, the final use or
disposal of the sludge, and the sludge parameter(s) of concern.

A. Equipment Preparation

A soil sample is best taken with a soil probe or an auger. These tools help to ensure that
an equal amount of soil sample/subsample will be collected to a definite depth at the
sampling site. A spade, a knife, or a trowel can be used to collect thin slices or sections
of soil samples/subsamples. A spade, a knife, or a trowel can also be used to remove soil
from a probe or auger, to break up cores, or to mix grab subsamples for a composite
sample so that any composite subsample removed after mixing is a homogeneous
mixture.

Proper equipment decontamination protocol must be used to ensure that samples are free
from cross contamination. Equipment must be washed with a phosphorus free detergent,
rinsed with distilled water and dried. If a sample must be collected and the on-site
washing of equipment is not possible, push the probe, or use the auger, several times at
the new site and remove any material adhering to the equipment prior to collecting the
samples at the new site.

Soil samples should be collected and placed in a clean plastic pail or box. Individual
grab samples must be thoroughly mixed to provide a homogenous composite subsample
when composite samples are collected.

B. Sample Collection Procedure

Soil samples can be collected at any time. However, samples collected to analyze for
nutrients or metals should be collected prior to spring planting. Soil samples collected to
analyze for other chemicals (e.g., organic chemicals of concern) should be collected after
sludge has been applied to a site. A control (background) uncontaminated sample must
be collected for chemical analyses when chemicals of concern are being evaluated.
Collectors must wear disposable gloves when collecting soil and soil/sludge samples.

A soil probe, an auger, a spade, or a garden trowel can be used to collect a soil sample. A
plastic bucket should be used to collect soil subsamples/samples.

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Each composite sampling should represent an area of from 15 to 20 uniform acres. The
site should be uniform in soil series, slope, drainage and erosion, and fertilizer
application, including sewage sludge, with less than 5 acres of rolling land. In general,
any area that is large enough to spread sludge separately should be sampled separately.

Establish a transect across the widest portion of the field and collect grab subsamples
every 75 to 100 feet; collect a minimum of 15 grab subsamples per 5 acres. Low spots or
other unusual or atypical areas (e.g., a sludge stockpiling location, or an area where lime
or fertilizer was spilled) must be omitted from the sample, or sampled separately. Repeat
the collection procedure on two adjacent parallel transects, each located one-quarter of
the distance between the first, longest transect and the field boundary. Repeat the entire
sampling procedure by sampling three transects perpendicular to the first three transects
sampled. Using this procedure, a total of six transects will be sampled.

Samples should be taken to plow depth, or approximately to an 8 inch depth. Samples

should be collected between rows where row crop acreage is being sampled. Samples
should be collected to the rooting zone of from 3 to 4 inches where pasture grass acreage
is being sampled. All grab subsamples must be broken up and mixed thoroughly to
homogenize the mixture before a composite subsample is removed. The sample should
be transferred to an appropriate container (Appendix1). Sample weight must be at least
10 grams for metals, 10 grams for mercury, 10 grams for nutrients (approximately 100
grams for all inorganic parameter analyses), and 100 grams for organic analyses.
Sediment samples are not preserved. Samples are kept at 4 degrees C.

Analyte sample concentration for sludge and sludge/soil samples is reported as parameter
concentration per unit dry weight. Composite samples provide an average parameter
concentration.

C. Sample Documentation

Sample labels must include the following information:

1. Sampling organization’s name (e.g., DSW),

2. Facility or location name being sampled,
3. Collector(s)
4. Type of sample (i.e., grab, 24 hour composite, etc.),
5. Date and military time (record time as 24 hour time, e.g., 1:00 P.M. is
1300),

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6. Specific sample location (Latitude and Longitude recorded in decimal

degrees – The method used to determine Latitude and Longitude must be
identified), and
7. Sample container number.

A field note book should include all of the above sample information, parameters
analyzed and any special remarks. A sketch showing the location sampled and an
indication where the sample(s) was (were) collected should be included.

D. Chain-of-Custody

All samples submitted for analyses must include a Chain-of-Custody record. A Chain-of-
Custody provides a record of sample transfer from person to person. This document
helps to protect the integrity of the sample by ensuring that only authorized persons have
custody of the sample. The Chain-of-Custody procedure ensures that an enforceable
record of sample transfer has occurred, which is necessary if the sample results are to be
used in a judicial proceeding alleging violations of sludge standards. A Chain-of-
Custody record for each sample’s collection and handling history from the time of sample
collection, sample transport and sample receipt by the laboratory includes the information
listed on the sample container. All personnel handling the sample must sign, date and
note the time of day (military time) on the Chain-of-Custody sheet.

E. Laboratory Coordination

All sampling must be coordinated with the laboratory. The laboratory (DES for the
DSW) must be contacted to ensure proper preparation of the sample(s), required forms
and labeling procedures, and transportation and the drop off procedure.

Analytical parameters, analytical methods, maximum holding times, sample container

type and comments are listed in Appendix 1. Sludge, sediment and soil samples are not
preserved, and are kept at 4 degrees C. Samples are prepared using Ohio EPA Method
400.9 (microwave preparation) using 0.5 to 0.65 g (wet weight) of sample for all
analytical procedures for total metals identified, U.S. EPA Method 200.7 and U.S. EPA
Method 200.8 (ICP and ICP/MS).

Method SW-846 Method 3050 (using an equivalent to 1g dry weight) for any of the
analytical procedures identified when analyzing for Total Metals (Total Arsenic, Total
Cadmium, Total Copper, Total Lead, Total Molybdenum, Total Nickel, Total Potassium,
Total Selenium and Total Zinc) will be used if requested.

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Analytical Method SW-846 is used for DERR samples only. Analytical Method SW-846
will be used for DSW analyses if requested.

Use SW-846 Method 7471 to analyze for Total Mercury in semisolid and solid wastes.
The digestion method is contained in the analytical method procedure.

The procedure for determining Specific Oxygen Uptake Rate (SOUR) in samples is very
sensitive to sample temperature variation and lag time between sample collection and test
initiation. Replicate samples should be taken. SOUR must be calculated based upon the
total solids dry weight rather than on volatile solids.

Aspiration analyses of metals are applicable at moderate concentrations in clean, complex

matrix systems. Inductively Coupled Plasma (ICP) methods are applicable over a broad
concentration range and are especially sensitive for refectory elements. Detection limits
for AA Furnace methods are generally lower than for ICP methods. The analytical
method selected will be determined by sample type and sampling objective(s). Select an
analytical procedure with a laboratory Reporting Limit (RL) below the analyte
concentration objective. Analyte concentrations are reported as concentration per unit
dry weight. Refer to DES’ WEB site for analytical Method Detection Limits (MDLs)
and Laboratory Reporting Limits (RLs).

F. References (additional information)

DSW Permit Guidance 11, detail testing requirements for sewage sludge for land
application.

Congressional Federal Registrar (CFR) 40 CFR Part 503.

Ohio Administrative Code (OAC), Chapter 3745-40.

U.S. EPA. 1989. “POTW Sludge Sampling and Analysis Guidance Document,” August
1989; for U.S. EPA; by Science Applications International Corporation.

U.S. EPA. 1996. “Test Methods for Evaluation Solid Waste (SW-846), Update III”,
December 1996. U.S. EPA, Office of Solid Waste and Emergency Response.

U.S. EPA. 2003. “Control of Pathogens and Vector Attraction in Sewage Sludge,
Revised July 2003. This document is also known as the “White House
Document”.

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Appendix 1

Sludge Program Sampling QA

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Section Name (SOP): Part I Soil and Soil/Sludge Sampling Date: 04/08/2009

Table 1: Parameter, analytical method, maximum holding time and comments for soil and
soil/sludge sampling (a)

A. Physical Characteristics, Total Nutrients and Dioxin

Parameter Analytical Method Holding Time Comments

Container
pH SW-9045 Immediate The sample is mixed with a prescribed
Plastic or glass liquid and the pH is determined with a
probe. Record pH at 25C, or correct
for temperature and report at 25C
Conductivity SW-9050 28 days Record conductivity at 25C, or correct
Cool to 4C for temperature and report results for
Plastic or glass 25C
Total Solids SM-2540 G 7 Days SM-2540 is the recommended Method
Cool to 4C for solid and semi-solid samples.
Plastic or glass
Volatile Solids SM-2540 G 7 Days SM-2540 is the recommended Method
Cool to 4C for solid and semi-solid samples.
Plastic or glass
Specific Oxygen SM-2710 Perform as See text
Uptake Rate See Appendix D soon as
(SOUR) EPA/625/R-92/013 possible
October 1999 Plastic or glass
Soil Phosphorus Bray/Kurtz Test for P 28 days North Central Regional Research,
(P) Mehlich 3 Test for P Cool to 4C Pub. No. 221 (Revised):
Olsen (NaHCO3)P 500ml amber Recommended Chemical Soil test
jar
Total Kjeldahl SM-4500-N organic 28 days TKN nitrogen is the sum of organic
Nitrogen (TKN) Cool to 4C and ammonia nitrogen. Sample
Plastic or glass digestion and distillation are required.
Include or reference in method

a. Method SW846 (Methods 6010B for ICP parameters and Method 6020A for
ICP/MS parameters) are used if requested.

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Table 1: A. Physical Characteristics, Total Nutrients and Dioxin (continued)

Parameter Analytical Method Holding Time Comments

Container
Total Ammonia SM-4500-NH3 7 days All samples must be distilled using
Nitrogen Cool to 4C procedure SM-4500-NH3 B prior to
(NH3-N) Plastic or glass using a listed specific analytical
method.
Total Nitrate SM-4500-NO3 28 days Nitrate nitrogen is the fully oxidized
Nitrogen SW-846 Method 9056 Cool to 4C state of nitrogen. The presence of
(NO3-N) SW-846 Method 9210 Plastic or glass organics may interfere with the
method.
Total Phosphorus SM-4500-P 7 days Pay close attention to the sample
(T-P) Cool to 4C preparation requirements found in
Plastic or glass section 4500-P-B.
Dioxin TTEs U.S. EPA 30 days For liquid or cake samples
Method 1613B Cool to 4C A cake sample is preferred
U.S. EPA Amber glass
Method 1668A Teflon lined lid
Organic GC-MS 14 days
Chemical of Method SW-846 Cool to 4C
Concern Amber glass
Teflon lined lid

a. Method SW846 (Methods 6010B for ICP parameters and Method 6020A for
ICP/MS parameters) are used if requested.

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Table 1: B Total Metals (a,b)

Parameter Analytical Method Holding Comments

Time
Container
Arsenic USEPA 200.7 ICP 6 months See text
(T-As) USEPA 200.8 ICP/MS Cool to 4C
Plastic or
glass
Cadmium USEPA 200.7 ICP 6 months See text
(T-Cd) USEPA 200.8 ICP/MS Cool to 4C
Plastic or
glass
Copper USEPA 200.7 ICP 6 months See text
(T-Cu) USEPA 200.8 ICP/MS Cool to 4C
Plastic or
glass
Lead USEPA 200.7 ICP 6 months See text
(T-Pb) USEPA 200.8 ICP/MS Cool to 4C
Plastic or
glass
Molybdenum USEPA 200.7 ICP 6 months See text
(T-Mo) USEPA 200.8 ICP/MS Cool to 4C
Plastic or
glass
Nickel USEPA 200.7 ICP 6 months See text
(T-Ni) USEPA 200.8 ICP/MS Cool to 4C
Plastic or
glass
Potassium USEPA 200.7 ICP 6 months See text
(T-K) Cool to 4C
Plastic or
glass

a. Ohio EPA sample microwave preparation SOP 400.9 is used for sludge, sediment
and soil metals parameters.

b. Method SW846 (Methods 6010B for ICP parameters and Method 6020A for
ICP/MS parameters) are used if requested.

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Table 1: B Total Metals (continued)

Parameter Analytical Method Holding Time Comments

Container
Selenium USEPA 200.7 ICP 6 months See text
(T-Se) USEPA 200.8 ICP/MS Cool to 4C
Plastic or glass
Zinc USEPA 200.7 ICP 6 months See text
(T-Zn) Cool to 4C
Plastic or glass
Mercury Cold Vapor (manual) 28 days Use SW-846 Method 7470 for
(T-Hg) SW-846 Method 7470 Cool to 4C liquid wastes. Use SW-846
SW-846 Method 7471 Plastic or glass Method 7471 for solid and
AA Furnace SW-846 semisolid wastes. The digestion
ICP procedure is included in the
SW-846 Method 6010 analytical method.
US EPA Method 245.1

a. Ohio EPA sample microwave preparation SOP 400.9 is used for sludge, sediment
and soil metals parameters.

b. Method SW846 (Methods 6010B for ICP parameters and Method 6020A for
ICP/MS parameters) are used if requested.

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Table 1: C. Organisms

Parameter Analytical Method Holding Time Comments

Organism Container
Fecal Coliform SM-9221 E 24 Hours Both procedures are very
Most Probable Number Cool to 4C temperature sensitive. The
Required for Class A Plastic or glass samples must be analyzed within
and recommended for the defined holding times.
Class B, Alternative 1
SM-9222 D
Membrane filter
Salmonella sp. Kenner and Clark 24 Hours Large sample volumes are needed
See Appendix G Cool to 4C due to low concentrations of
EPA/625/R-92/013 Plastic or glass salmonella in wastewater and
October 1999 sludge. More than one procedure
SM-9260 D may be necessary to determine
salmonella presence because of the
large number of salmonella
species.
Enteric Viruses ASTM 48 Hours Concentration of the sample is
Method D 4994-89 Up to 2 weeks necessary due to the presumably
Cool at 0F low numbers of viruses in the
Plastic or glass sample.
Helminth Ova Yanko 1 Month The analyst must be familiar with
See Appendix I Cool to 4C other ova test methods which are
EPA/625/R-92/013 Plastic or glass found in the same document. All
October 1999 ova identified are considered
viable ova.

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Section Name (SOP): Part II Liquid Sludge Sampling Date: 04/08/2009

Part II: Liquid Sludge Sampling

A. Equipment Preparation

A liquid sludge sample is best taken as sludge is being transferred from one vessel to
another. This should be done downstream from a pump that serves to mix the sewage
sludge thoroughly. Other in-vessel sampling options include using a core sampler, a
Sludge Judge, or a sludge nabber.

Proper equipment decontamination protocol must be used to ensure that samples are free
from cross contamination. Equipment must be washed with a phosphorus free detergent,
rinsed with distilled water and dried. Collect three timed, composite subsamples of equal
volume from the top, middle and bottom of the vessel being sampled. Collect a
minimum of 12 subsamples per vessel; four subsamples from each vessel level for each
of the three timed collections.

Collectors must wear disposable gloves when collecting liquid sludge samples. Liquid
sludge samples should be collected and placed in a clean plastic pail and thoroughly
mixed to provide a homogenous composite subsample.

B. Sample Collection Procedure for Liquid Sludge Being Transferred

1. Anaerobically Digested Sludge

The sample should be collected on the discharge side of the positive

displacement pumps.

2. Aerobically Digested Sludge

The sample should be collected on the discharge side of the positive

displacement pumps directly from the digester if batch digestion is used.

Two cautions are in order for collecting aerobically digested sludge. Volatile
organic compounds may purge with escaping air when air entrains in the sample.
And, solids separate rapidly in well-digested sludge when aeration is shut off.

3. Thickened Sludge

The sample should be collected on the discharge side of the positive displacement
pumps.

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Section Name (SOP): Part II Liquid Sludge Sampling Date: 04/08/2009

4. Heat Treatment

The sample should be collected on the discharge side of the positive displacement
pumps after decanting. Care should be taken when sampling heat treated sludge.
There is a high tendency for solids separation, and the high temperature of the
sample (>600C as sampled) can cause problems with some sample containers due
to cooling and subsequent concentration of entrained gases.

For sludge gathered by a Sludge Judge, lower the Sludge Judge to the bottom of the tank.
When the bottom has been reached and the pipe has been filled to the surface level, tug
slightly on the rope as the unit is raised. This sets the check valve which traps the
column of solids and liquid in the Sludge Judge.

For sludge samples collected with a sludge nabber, section the sample space into decision
unit areas (e.g., quadrants, clock face, etc.). Composite equal amounts of bottom, middle
and top sludge from a minimum of 3 areas of each decision unit area for a total of 12 grab
samples.

Sediment samples are not preserved. Samples are kept at 4 degrees C. A composite
sample should contain equal amounts of bottom, middle and top levels of sludge. A
composite sample should produce an average parameter concentration. Percent solids are
used to determine analyte concentrations reported as dry weight concentrations.

C. Sample Documentation

Sample labels must include the following information:

1. Sampling organization’s name (e.g., DSW),

2. Facility or location name being sampled,
3. Collector(s)
4. Type of sample (i.e., 24 hour grab, composite, etc.),
5. Date and military time (record time as 24 hour time, e.g., 1:00 P.M. is
1300),
6. Specific sample location (Latitude and Longitude recorded in decimal
degrees – The method used to determine Latitude and Longitude must be
identified), and
7. Sample container number.

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A field note book should include all of the above sample information, parameters
analyzed and any special remarks. A sketch showing the location sampled and an
indication where the sample(s) was (were) collected should be included.

D. Chain-of-Custody

All samples submitted for analyses must include a Chain-of-Custody record. A Chain-of-
Custody provides a record of sample transfer from person to person. This document
helps to protect the integrity of the sample by ensuring that only authorized persons have
custody of the sample. The Chain-of-Custody procedure ensures that an enforceable
record of sample transfer has occurred, which is necessary if the sample results are to be
used in a judicial proceeding alleging violations of sludge standards. A Chain-of-
Custody record for each sample’s collection and handling history from the time of sample
collection, sample transport and sample receipt by the laboratory includes the information
listed on the sample container. All personnel handling the sample must sign, date and
note the time of day (military time) on the Chain-of-Custody sheet.

E. Laboratory Coordination

All sampling must be coordinated with the laboratory. The laboratory (DES for the
DSW) must be contacted to ensure proper preparation of the sample(s), required forms
and labeling procedures and transportation and the drop off procedure.

Analytical parameters, analytical methods, maximum holding times, sample container

type and comments are listed in Appendix 1. Sludge, sediment and soil samples are not
preserved. Samples are prepared using Ohio EPA Method 400.9 (microwave
preparation) using 0.5 to 0.65 g (wet weight) of sample for all analytical procedures for
total metals identified, U.S. EPA Method 200.7, and U.S. EPA Method 200.8 (ICP and
ICP/MS).

Method SW-846 Method 3050 (using an equivalent to 1g dry weight) for any of the
analytical procedures identified when analyzing for Total Metals (Total Arsenic, Total
Cadmium, Total Copper, Total Lead, Total Molybdenum, Total Nickel, Total Potassium,
Total Selenium and Total Zinc) will be used if requested.

Analytical Method SW-846 is used for DERR samples only. Analytical Method SW-846
will be used for DSW analyses if requested.

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The analytical method selected will be determined by sample type and sampling
objective(s). Select an analytical procedure with a laboratory Reporting Limit (RL)
below the analyte concentration objective. Analyte concentrations are reported as
concentration per unit dry weight. Refer to DES’ WEB site for analytical Method
Detection Limits (MDLs) and Laboratory Reporting Limits (RLs).

Use SW-846 Method 7470 to analyze for Total Mercury in liquid wastes. The digestion
method is contained in the analytical method procedure.

The procedure for determining Specific Oxygen Uptake Rate (SOUR) in samples is very
sensitive to sample temperature variation and lag time between sample collection and test
initiation. Replicate samples should be taken. SOUR must be calculated based upon the
total solids dry weight rather than on volatile solids.

F. References (additional information)

DSW Permit Guidance 11, detail testing requirements for sewage sludge for land
application.

Congressional Federal Registrar (CFR) 40 CFR Part 503.

Ohio Administrative Code (OAC), Chapter 3745-40.

U.S. EPA. 1989. “POTW Sludge Sampling and Analysis Guidance Document,” August
1989; for U.S. EPA; by Science Applications International Corporation.

U.S. EPA. 1996. “Test Methods for Evaluation Solid Waste (SW-846), Update III”,
December 1996. U.S. EPA, Office of Solid Waste and Emergency Response.

U.S. EPA. 2003. “Control of Pathogens and Vector Attraction in Sewage Sludge,
Revised July 2003. This document is also known as the “White House
Document”.

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Section Name (SOP): Part II Liquid Sludge Sampling Date: 04/08/2009

Appendix 1

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Section Name (SOP): Part II Liquid Sludge Sampling Date: 04/08/2009

Table 1: Parameter, analytical method, maximum holding time and comments for soil and
soil/sludge sampling (a)

A. Physical Characteristics, Total Nutrients and Dioxin

Parameter Analytical Method Holding Time Comments

Container
pH SW-9045 Immediate The sample is mixed with a prescribed
Plastic or glass liquid and the pH is determined with a
probe. Record pH at 25C, or correct
for temperature and report at 25C
Conductivity SW-9050 28 days Record conductivity at 25C, or correct
Cool to 4C for temperature and report results for
Plastic or glass 25C
Total Solids SM-2540 G 7 Days SM-2540 is the recommended Method
Cool to 4C for solid and semi-solid samples.
Plastic or glass
Volatile Solids SM-2540 G 7 Days SM-2540 is the recommended Method
Cool to 4C for solid and semi-solid samples.
Plastic or glass
Specific Oxygen SM-2710 Perform as See text
Uptake Rate See Appendix D soon as
(SOUR) EPA/625/R-92/013 possible
October 1999 Plastic or glass
Soil Phosphorus Bray/Kurtz Test for P 28 days North Central Regional Research,
(P) Mehlich 3 Test for P Cool to 4C Pub. No. 221 (Revised):
Olsen (NaHCO3)P 500ml amber Recommended Chemical Soil test
jar
Total Kjeldahl SM-4500-N organic 28 days TKN nitrogen is the sum of organic
Nitrogen (TKN) Cool to 4C and ammonia nitrogen. Sample
Plastic or glass digestion and distillation are required.
Include or reference in method

a. Method SW846 (Methods 6010B for ICP parameters and Method 6020A for
ICP/MS parameters) are used if requested.

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Table 1: A. Physical Characteristics, Total Nutrients and Dioxin (continued)

Parameter Analytical Method Holding Time Comments

Container
Total Ammonia SM-4500-NH3 7 days All samples must be distilled using
Nitrogen Cool to 4C procedure SM-4500-NH3 B prior to
(NH3-N) Plastic or glass using a listed specific analytical
method.
Total Nitrate SM-4500-NO3 28 days Nitrate nitrogen is the fully oxidized
Nitrogen SW-846 Method 9056 Cool to 4C state of nitrogen. The presence of
(NO3-N) SW-846 Method 9210 Plastic or glass organics may interfere with the
method.
Total Phosphorus SM-4500-P 7 days Pay close attention to the sample
(T-P) Cool to 4C preparation requirements found in
Plastic or glass section 4500-P-B.
Dioxin TTEs U.S. EPA 30 days For liquid or cake samples
Method 1613B Cool to 4C A cake sample is preferred
U.S. EPA Amber glass
Method 1668A Teflon lined lid
Organic GC-MS 14 days
Chemical of Method SW-846 Cool to 4C
Concern Amber glass
Teflon lined lid

a. Method SW846 (Methods 6010B for ICP parameters and Method 6020A for
ICP/MS parameters) are used if requested.

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Section Name (SOP): Part II Liquid Sludge Sampling Date: 04/086/2009

Table 1: B Total Metals (a,b)

Parameter Analytical Method Holding Comments

Time
Container
Arsenic USEPA 200.7 ICP 6 months See text
(T-As) USEPA 200.8 ICP/MS Cool to 4C
Plastic or
glass
Cadmium USEPA 200.7 ICP 6 months See text
(T-Cd) USEPA 200.8 ICP/MS Cool to 4C
Plastic or
glass
Copper USEPA 200.7 ICP 6 months See text
(T-Cu) USEPA 200.8 ICP/MS Cool to 4C
Plastic or
glass
Lead USEPA 200.7 ICP 6 months See text
(T-Pb) USEPA 200.8 ICP/MS Cool to 4C
Plastic or
glass
Molybdenum USEPA 200.7 ICP 6 months See text
(T-Mo) USEPA 200.8 ICP/MS Cool to 4C
Plastic or
glass
Nickel USEPA 200.7 ICP 6 months See text
(T-Ni) USEPA 200.8 ICP/MS Cool to 4C
Plastic or
glass
Potassium USEPA 200.7 ICP 6 months See text
(T-K) Cool to 4C
Plastic or
glass

a. Ohio EPA sample microwave preparation SOP 400.9 is used for liquid sludge
metals parameters.

b. Method SW846 (Methods 6010B for ICP parameters and Method 6020A for
ICP/MS parameters) are used if requested.

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Section Name (SOP): Part II Liquid Sludge Sampling Date: 04/08/2009

Table 1: B Total Metals (continued)

Parameter Analytical Method Holding Time Comments

Container
Selenium USEPA 200.7 ICP 6 months See text
(T-Se) USEPA 200.8 ICP/MS Cool to 4C
Plastic or glass
Zinc USEPA 200.7 ICP 6 months See text
(T-Zn) Cool to 4C
Plastic or glass
Mercury Cold Vapor (manual) 28 days Use SW-846 Method 7470 for
(T-Hg) SW-846 Method 7470 Cool to 4C liquid wastes. Use SW-846
SW-846 Method 7471 Plastic or glass Method 7471 for solid and
AA Furnace SW-846 semisolid wastes. The digestion
ICP procedure is included in the
SW-846 Method 6010 analytical method.
U.S. EPA Method 245.1

a. Ohio EPA sample microwave preparation SOP 400.9 is used for liquid sludge
metals parameters.

b. Method SW846 (Methods 6010B for ICP parameters and Method 6020A for
ICP/MS parameters) are used if requested.

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Table 1: C. Organisms

Parameter Analytical Method Holding Time Comments

Organism Container
Fecal Coliform SM-9221 E 24 Hours Both procedures are very
Most Probable Number Cool to 4C temperature sensitive. The
Required for Class A Plastic or glass samples must be analyzed within
and recommended for the defined holding times.
Class B, Alternative 1
SM-9222 D
Membrane filter
Salmonella sp. Kenner and Clark 24 Hours Large sample volumes are needed
See Appendix G Cool to 4C due to low concentrations of
EPA/625/R-92/013 Plastic or glass salmonella in wastewater and
October 1999 sludge. More than one procedure
SM-9260 D may be necessary to determine
salmonella presence because of the
large number of salmonella
species.
Enteric Viruses ASTM 48 Hours Concentration of the sample is
Method D 4994-89 Up to 2 weeks necessary due to the presumably
Cool at 0F low numbers of viruses in the
Plastic or glass sample.
Helminth Ova Yanko 1 Month The analyst must be familiar with
See Appendix I Cool to 4C other ova test methods which are
EPA/625/R-92/013 Plastic or glass found in the same document. All
October 1999 ova identified are considered
viable ova.

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Section Name (SOP): Part III Cake Sludge Sampling Date: 04/08/2009

Part III: Cake Sludge Sampling

A. Equipment Preparation

A cake sludge sample is best taken as sludge is being transferred, usually on conveyors.
If this is not possible, a stockpile sample can be taken using an auger, a probe, or a
shovel. These tools will help to ensure that all depths of the stockpile are represented.

Collectors must wear disposable gloves when collecting cake sludge samples. Cake
sludge subsamples should be collected and placed in a clean plastic pail or box.
Individual grab samples must be thoroughly mixed to provide a homogenous composite
subsample when composite samples are collected.

Proper equipment decontamination protocol must be used to ensure that samples are free
from cross contamination. Equipment must be washed with a phosphorus free detergent,
rinsed with distilled water and dried. Sampling should composite three subsamples of
equal volume from top, middle and bottom of the vessel being sampled for a total of 12
grab samples.

B. Sample Collection Procedure for Cake Sludge Being Transferred

1. Dried, Composted, or Thermally Reduced

Collect a composite sample by sampling the sludge from the material collection
conveyors and bulk containers. Collected an equal volume of sample material
from the top, middle and bottom of all vessels being sampled; collect four
subsamples of the sludge mass at the three depths at four locations. Composite 12
grab subsamples taken at various locations from the conveyor.

2. Dewatered: Belt Filter Press, Centrifuge, or Vacuum Filter Press

Collect a composite sample of the sludge from the discharge chute.

3. Press: Plate or Frame

Collect a composite sample of the sludge from the storage bin. Select four
locations within the storage bin and collect an equal amount of material from each
location. Combine the four subsamples into a composite sample.

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4. Drying Beds

Divide the bed into quarters and grab equal amounts of material from the center of
each quarter. Each subsample should include the entire depth of the sludge
down to the sand. An equal volume of sampled material from top, middle and
bottom of the vessel being sampled should be collected. Combine the four
subsamples into a composite sample.

5. Composite Piles

Collect a composite sample of the sludge directly from the front end loader as the
sludge is being loaded into trucks to be hauled away or stored.

Sediment samples are not preserved. Samples are kept at 4 degrees C. Sediment samples
are not preserved. Samples are kept at 4 degrees C. A composite sample should produce
an average parameter concentration. Analyte sample concentration for sludge cake is
reported as parameter concentration per unit dry weight.

C. Sample Documentation

Sample labels must include the following information:

1. Sampling organization’s name (e.g., DSW),

2. Facility or location name being sampled,
3. Collector(s)
4. Type of sample (i.e., 24 hour grab, composite, etc.),
5. Date and military time (record time as 24 hour time, e.g., 1:00 P.M. is
1300),
6. Specific sample location (Latitude and Longitude recorded in decimal
degrees – The method used to determine Latitude and Longitude must be
identified), and
7. Sample container number.
.

A field note book should include all of the above sample information, parameters
analyzed and any special remarks. A sketch showing the location sampled and an
indication where the sample(s) was (were) collected should be included.

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D. Chain-of-Custody

All samples submitted for analyses must include a Chain-of-Custody record. A Chain-of-
Custody provides a record of sample transfer from person to person. This document
helps to protect the integrity of the sample by ensuring that only authorized persons have
custody of the sample. The Chain-of-Custody procedure ensures that an enforceable
record of sample transfer has occurred, which is necessary if the sample results are to be
used in a judicial proceeding alleging violations of sludge standards. A Chain-of-
Custody record for each sample’s collection and handling history from the time of sample
collection, sample transport and sample receipt by the laboratory includes the information
listed on the sample container. All personnel handling the sample must sign, date and
note the time of day (military time) on the Chain-of-Custody sheet.

E. Laboratory Coordination

All sampling must be coordinated with the laboratory. The laboratory (DES for the
DSW) must be contacted to ensure proper preparation of the sample(s), required forms
and labeling procedures and transportation and the drop off procedure.

Analytical parameters, analytical methods, maximum holding times, sample container

type and comments are listed in Appendix 1. Sludge, sediment and soil samples are not
preserved. Samples are prepared using Samples are prepared using Ohio EPA Method
400.9 Samples are prepared using Ohio EPA Method 400.9 (microwave preparation)
using 0.5 to 0.65 g (wet weight) of sample for all analytical procedures for total metals
identified, U.S. EPA Method 200.7 and U.S. EPA Mehtod 200.8 (ICP and ICP/MS).

Method SW-846 Method 3050 (using an equivalent to 1g dry weight) for any of the
analytical procedures identified when analyzing for Total Metals (Total Arsenic, Total
Cadmium, Total Copper, Total Lead, Total Molybdenum, Total Nickel, Total Potassium,
Total Selenium and Total Zinc) will be used if requested.

Inductively Coupled Plasma (ICP) methods are applicable over a broad concentration
range and are especially sensitive for refectory elements. The analytical method selected
will be determined by sample type and sampling objective(s). If possible, select an
analytical procedure with a laboratory Reporting Limit (RL) below the analyte
concentration objective. Analyte concentrations are reported as concentration per unit
dry weight. Refer to DES’ WEB site for analytical Method Detection Limits (MDLs)
and Laboratory RLs.

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Analytical Method SW-846 is used for DERR samples only. Analytical Method SW-846
will be used for DSW analyses if requested.

Use SW-846 Method 7471 to analyze for Total Mercury in semisolid and solid wastes.
The digestion method is contained in the analytical method procedure.

The procedure for determining Specific Oxygen Uptake Rate (SOUR) in samples is very
sensitive to sample temperature variation and lag time between sample collection and test
initiation. Replicate samples should be taken. SOUR must be calculated based upon the
total solids dry weight rather than on volatile solids.

F. References (additional information)

DSW Permit Guidance 11, detail testing requirements for sewage sludge for land
application.

Congressional Federal Registrar (CFR) 40 CFR Part 503.

Ohio Administrative Code (OAC), Chapter 3745-40.

U.S. EPA. 1989. “POTW Sludge Sampling and Analysis Guidance Document,” August
1989; for U.S. EPA; by Science Applications International Corporation.

U.S. EPA. 1996. “Test Methods for Evaluation Solid Waste (SW-846), Update III”,
December 1996. U.S. EPA, Office of Solid Waste and Emergency Response.

U.S. EPA. 1999. Environmental Regulations and Technology Control of Pathogens and
Vector Attraction in Sewage Sludge. Appendix G, Kenner and Clark.
EPA/625/R-92/013, October 1999.

U.S. EPA. 2003. “Control of Pathogens and Vector Attraction in Sewage Sludge,
Revised July 2003. This document is also known as the “White House
Document”.

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Appendix 1

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Section Name (SOP): Part III Cake Sludge Sampling Date: 04/08/2009

Table 1: Parameter, analytical method, maximum holding time and comments for cake
sludge sampling (a)

A. Physical Characteristics, Total Nutrients and Dioxin

Parameter Analytical Method Holding Time Comments

Container
pH SW-9045 Immediate The sample is mixed with a prescribed
Plastic or glass liquid and the pH is determined with a
probe. Record pH at 25C, or correct
for temperature and report at 25C
Conductivity SW-9050 28 days Record conductivity at 25C, or correct
Cool to 4C for temperature and report results for
Plastic or glass 25C
Total Solids SM-2540 G 7 Days SM-2540 is the recommended Method
Cool to 4C for solid and semi-solid samples.
Plastic or glass
Volatile Solids SM-2540 G 7 Days SM-2540 is the recommended Method
Cool to 4C for solid and semi-solid samples.
Plastic or glass
Specific Oxygen SM-2710 Perform as See text
Uptake Rate See Appendix D soon as
(SOUR) EPA/625/R-92/013 possible
October 1999 Plastic or glass
Soil Phosphorus Bray/Kurtz Test for P 28 days North Central Regional Research,
(P) Mehlich 3 Test for P Cool to 4C Pub. No. 221 (Revised):
Olsen (NaHCO3)P 500ml amber Recommended Chemical Soil test
jar
Total Kjeldahl SM-4500-N organic 28 days TKN nitrogen is the sum of organic
Nitrogen (TKN) Cool to 4C and ammonia nitrogen. Sample
Plastic or glass digestion and distillation are required.
Include or reference in method

a. Method SW846 (Methods 6010B for ICP parameters and Method 6020A for
ICP/MS parameters) are used if requested.

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Table 1: A. Physical Characteristics, Total Nutrients and Dioxin (continued)

Parameter Analytical Method Holding Time Comments

Container
Total Ammonia SM-4500-NH3 7 days All samples must be distilled using
Nitrogen Cool to 4C procedure SM-4500-NH3 B prior to
(NH3-N) Plastic or glass using a listed specific analytical
method.
Total Nitrate SM-4500-NO3 28 days Nitrate nitrogen is the fully oxidized
Nitrogen SW-846 Method 9056 Cool to 4C state of nitrogen. The presence of
(NO3-N) SW-846 Method 9210 Plastic or glass organics may interfere with the
method.
Total Phosphorus SM-4500-P 7 days Pay close attention to the sample
(T-P) Cool to 4C preparation requirements found in
Plastic or glass section 4500-P-B.
Dioxin TTEs U.S. EPA 30 days For liquid or cake samples
Method 1613B Cool to 4C A cake sample is preferred
U.S. EPA Amber glass
Method 1668A Teflon lined lid
Organic GC-MS 14 days
Chemical of Method SW-846 Cool to 4C
Concern Amber glass
Teflon lined lid

a. Method SW846 (Methods 6010B for ICP parameters and Method 6020A for
ICP/MS parameters) are used if requested.

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Section Name (SOP): Part III Cake Sludge Sampling Date: 04/08/2009

Table 1: B Total Metals

Parameter Analytical Method Holding Comments

Time
Container
Arsenic USEPA 200.7 ICP 6 months See text
(T-As) USEPA 200.8 ICP/MS Cool to 4C
Plastic or
glass
Cadmium USEPA 200.7 ICP 6 months See text
(T-Cd) USEPA 200.8 ICP/MS Cool to 4C
Plastic or
glass
Copper USEPA 200.7 ICP 6 months See text
(T-Cu) USEPA 200.8 ICP/MS Cool to 4C
Plastic or
glass
Lead USEPA 200.7 ICP 6 months See text
(T-Pb) USEPA 200.8 ICP/MS Cool to 4C
Plastic or
glass
Molybdenum USEPA 200.7 ICP 6 months See text
(T-Mo) USEPA 200.8 ICP/MS Cool to 4C
Plastic or
glass
Nickel USEPA 200.7 ICP 6 months See text
(T-Ni) USEPA 200.8 ICP/MS Cool to 4C
Plastic or
glass
Potassium USEPA 200.7 ICP 6 months See text
(T-K) Cool to 4C
Plastic or
glass

a. Ohio EPA sample microwave preparation SOP 400.9 is used for cake sludge
metals parameters.

b. Method SW846 (Methods 6010B for ICP parameters and Method 6020A for
ICP/MS parameters) are used if requested.

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Table 1: B Total Metals (continued)

Parameter Analytical Method Holding Time Comments

Container
Selenium USEPA 200.7 ICP 6 months See text
(T-Se) USEPA 200.8 ICP/MS Cool to 4C
Plastic or glass
Zinc USEPA 200.7 ICP 6 months See text
(T-Zn) Cool to 4C
Plastic or glass
Mercury Cold Vapor (manual) 28 days Use SW-846 Method 7470 for
(T-Hg) SW-846 Method 7470 Cool to 4C liquid wastes. Use SW-846
SW-846 Method 7471 Plastic or glass Method 7471 for solid and
AA Furnace SW-846 semisolid wastes. The digestion
ICP procedure is included in the
SW-846 Method 6010 analytical method.
U.S. EPA Method 245.1

a. Ohio EPA sample microwave preparation SOP 400.9 is used for cake sludge
metals parameters.

b. Method SW846 (Methods 6010B for ICP parameters and Method 6020A for
ICP/MS parameters) are used if requested.

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Document Name: Sludge Program QA Document Revision: 0
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Table 1: C. Organisms

Parameter Analytical Method Holding Time Comments

Organism Container
Fecal Coliform SM-9221 E 24 Hours Both procedures are very
Most Probable Number Cool to 4C temperature sensitive. The
Required for Class A Plastic or glass samples must be analyzed within
and recommended for the defined holding times.
Class B, Alternative 1
SM-9222 D
Membrane filter
Salmonella sp. Kenner and Clark 24 Hours Large sample volumes are needed
See Appendix G Cool to 4C due to low concentrations of
EPA/625/R-92/013 Plastic or glass salmonella in wastewater and
October 1999 sludge. More than one procedure
SM-9260 D may be necessary to determine
salmonella presence because of the
large number of salmonella
species.
Enteric Viruses ASTM 48 Hours Concentration of the sample is
Method D 4994-89 Up to 2 weeks necessary due to the presumably
Cool at 0F low numbers of viruses in the
Plastic or glass sample.
Helminth Ova Yanko 1 Month The analyst must be familiar with
See Appendix I Cool to 4C other ova test methods which are
EPA/625/R-92/013 Plastic or glass found in the same document. All
October 1999 ova identified are considered
viable ova.

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