United States
Environmental Protection
Agency
Office Of Water
(EN-338)
21W-4007
August 1990
&EPA
NPDES
Compliance Monitoring
Inspector Training: Sampling
Printed on Recycled Paper
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NPDES COMPLIANCE MONITORING INSPECTOR
TRAINING MODULE
SAMPLING
U.S. ENVIRONMENTAL PROTECTION AGENCY
ENFORCEMENT DIVISION
OFFICE OF WATER ENFORCEMENT AND PERMITS
ENFORCEMENT SUPPORT BRANCH
1990
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NPDES Compliance Monitoring Inspector Training: SAMPLING
DISCLAIMER
This module has been reviewed by the Office of Water Enforcement and Permits, U.S. Environmental
Protection Agency, and approved for publication. This module represents EPA's introductory training on selected
topics related to conducting NPDES compliance inspections. Failure on the part of any duly authorized official,
inspector, or agent to comply with its contents shall not be a defense in any enforcement action, nor shall failure
to comply with this guidance alone constitute grounds for rendering evidence obtained thereby inadmissible in a
court of law. The mention of trade names or commercial products constitutes neither endorsement nor
recommendation for use.
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NPDES Compliance Monitoring Inspector Training: SAMPLING
ACKNOWLEDGMENTS
This document represents an update of a module originally developed in June 1980 by the Enforcement
Division of the Office of Water Enforcement and Permits (OWEP). The module was revised under the direction
of Virginia Lathrop and Gary Polvi of OWEP, with the assistance of many members of the Inspection Materials
Work Group, including Robert Reeves of Region 6. In addition, the Regions conducted extensive reviews and
provided many valuable comments, most of which were incorporated into this module. Science Applications
International Corporation prepared this updated module under EPA Contract Nos. 68-01-7050 and 68-C8-0066,
Work Assignments Nos. El-7, E2-1, E2-8, C-l-34 (E), and C-2-1 (E).
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TABLE OF CONTENTS
Page
FOREWORD vii
1. INTRODUCTION 1-1
1.1 OVERVIEW OF THE NPDES PROGRAM 1-1
1.2 PURPOSE OF THE NPDES COMPLIANCE MONITORING
PROGRAM 1-2
1.3 OBJECTIVES OF NPDES SAMPLING 1-3
1.4 SAMPLING TASKS 1-3
2. SAMPLE COLLECTION 2-1
2.1 IMPORTANCE OF SAMPLE COLLECTION 2-1
2.2 SAMPLING PLAN 2-2
2.3 PREPARATION FOR SAMPLING 2-4
2.4 SAMPLING SAFETY 2-4
2.5 SAMPLING LOCATION 2-5
2.6 SELECTION AND PREPARATION OF SAMPLE CONTAINERS 2-6
2.7 SAMPLE TYPES 2-8
2.8 SAMPLE COLLECTION TECHNIQUES 2-10
2.9 SAMPLE VOLUME 2-14
2.10 SAMPLE PRESERVATION AND HOLDING TIMES 2-14
2.11 SAMPLE DOCUMENTATION 2-16
2.12 SAMPLE IDENTIFICATION AND LABELING 2-17
2.13 SAMPLE PACKAGING AND SHIPPING 2-18
2.14 CHAIN-OF-CUSTODY PROCEDURES 2-18
2.15 SPECIAL SAMPLING REQUIREMENTS 2-20
3. ANALYTICAL METHODS FOR ONSITE ANALYSIS 3-1
4. AUTOMATIC SAMPLERS 4-1
5. FLOW MEASUREMENT 5-1
5.1 IMPORTANCE OF FLOW MEASUREMENT / 5-1
5.2 OPEN CHANNEL FLOW (. 5-1
5.3 CLOSED CHANNEL FLOW \ 5-7
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TABLE OF CONTENTS (Continued)
Page
6. QUALITY CONTROL PROCEDURES FOR SAMPLING 6-1
6.1 QUALITY CONTROL PROCEDURES FOR SAMPLING 6-1
6.2 QUALITY ASSURANCE PROCEDURES FOR SAMPLING 6-2
6.3 LABORATORY QUALITY ASSURANCE/QUALITY CONTROL 6-3
7. SUMMARY 7-1
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LIST OF TABLES AND FIGURES
Table Page
2-1 COMPOSITING METHODS 2-11
Figure
5-1 PROFILE AND NOMENCLATURE OF SHARP-CRESTED WEIRS 5-3
5-2 FOUR COMMON TYPES OF SHARP-CRESTED WEIRS 5-4
5-3 DIMENSIONS AND CAPACITIES OF THE PARSHALL MEASURING FLUMES FOR
VARIOUS THROAT WIDTHS 5-5
5-4 CONFIGURATION AND NOMENCLATURE OF VENTURI METER 5-8
5-5 ELECTROMAGNETIC FLOW METER 5-10
LIST OF APPENDICES
APPENDIX A - GLOSSARY
APPENDIX B - REFERENCES
APPENDIX C - REVIEW QUESTIONS AND ANSWERS ON NPDES SAMPLING
PROCEDURES
APPENDIX D - VOLUME OF SAMPLE REQUIRED FOR DETERMINATION OF THE
VARIOUS CONSTITUENTS OF INDUSTRIAL WASTEWATER
APPENDIX E - REQUIRED CONTAINERS, PRESERVATION TECHNIQUES, HOLDING
TIMES, AND TEST METHODS (EXCERPTED FROM 40 CFR PART 136)
APPENDIX F - EPA ORDER 1440.2 - HEALTH AND SAFETY REQUIREMENTS FOR
EMPLOYEES ENGAGED IN FIELD ACTIVITIES
APPENDIX G - LIST OF FIELD SAMPLING EQUIPMENT
APPENDIX H - SAMPLE IDENTIFICATION LABELS
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LIST OF APPENDICES (Continued)
APPENDIX I - EXAMPLE RECORD OF FIELD SAMPLE DATA AND CHAIN-OF-CUSTODY
RECORD
APPENDIX J - CRITERIA FOR SELECTION OF AUTOMATIC SAMPLING EQUIPMENT
APPENDIX K - QUALITY CONTROL PROCEDURES FOR FIELD ANALYSIS AND
EQUIPMENT
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FOREWORD
This document is one of five training modules developed by the Office of Water Enforcement and
Permits (OWEP), U.S. Environmental Protection Agency (EPA) to introduce the National Pollutant Discharge
Elimination System (NPDES) program to new inspectors. Information in each module provides training to an
inspector unfamiliar with the NPDES program. The modules address the following topics:
• The Overview Module presents an overview of the entire NPDES program and briefly summarizes
different types of inspections conducted under this program
• The Legal Issues Module discusses the legal issues which must be addressed during an inspection
and provides legal information to assist inspectors in performing their duties
• The Biomonitoring Module outlines the principles of biomonitoring and the role of biological
testing in the NPDES program
• The Sampling Procedures Module details procedures to be used when conducting sampling and flow
monitoring
• The Laboratory Analysis Module outlines procedures and information necessary to perform an
effective evaluation of a permittee's laboratory.
The modules are best used in a classroom setting where there is discussion between instructors and
students and where questions can be asked. Yet, they can also stand alone as reference sources. Additional
discussion of the topics covered in these modules appears in the 1988 NPDES Compliance Inspection Manual.
These training modules were developed primarily for in-house training of Regional and State NPDES
inspectors. However, they are available as well to other interested parties such as attorneys, other program
offices, facility owners and operators, and members of the general public.
Regional and State personnel are encouraged to provide EPA Headquarters with suggested changes or
information which they believe would improve these modules. The content of the modules will be updated and
revised periodically. Comments, information, and suggestions to improve the modules should be addressed to
the:
Enforcement Support Branch (EN-338)
Office of Water Enforcement and Permits
U.S. Environmental Protection Agency
401 M Street, S.W.
Washington, DC 20460
VII
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NFDES Compliance Monitoring Inspector Training: SAMPLING
1. INTRODUCTION
1.1 OVERVIEW OF THE NPDES PROGRAM
The Federal Water Pollution Control Act of 1972, as amended by the Clean Water Act (CWA) of 1977
and by the Water Quality Act of 1987, specifies the objectives of restoring and maintaining the chemical,
physical, and biological integrity of the Nation's waters. The CWA provides broad authority to the U.S.
Environmental Protection Agency (EPA) to:
• Establish the National Pollutant Discharge Elimination System (NPDES) program and the National
Pretreatment Program
• Define acceptable pollution control technologies and establish effluent limitations based thereon
• Obtain information through reports and compliance inspections
• Take enforcement actions, both civil and criminal, when violations of the CWA occur.
The NPDES program, mandated by Section 402 of the CWA, regulates the discharge of pollutants from point
sources, such as municipal treatment plants, industries, animal feedlots, aquatic animal production facilities, and
mining operations. In order to discharge, each point source is required to obtain a NPDES permit which
specifies effluent limits, monitoring and reporting requirements,and any other terms and conditions necessary to
protect water quality.
To determine whether these NPDES permit conditions are being met, Section 308 of the CWA authorizes
inspections and monitoring of permittee facilities. Under the authority of Section 308, two types of monitoring
have been established: self-monitoring by the permittee and compliance monitoring by the permit-issuing
agency. According to the CWA, an inspection may be conducted where there is an existing NPDES permit, or
where a discharge exists or is likely to exist and no permit has been issued.
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Compliance with NPDES permit conditions is often monitored by States. Sections 308 and 402 of the
CWA provide for the transfer of Federal program authority to conduct NDPES permit compliance monitoring
to State agencies. Currently, over 75 percent of the States and territories are approved by EPA to implement
State NPDES programs.
1.2 PURPOSE OF THE NPDES COMPLIANCE MONITORING PROGRAM
As mentioned above, each NPDES permit contains specific, legally enforceable effluent limitations and
monitoring and reporting requirements. The purposes of the NPDES compliance monitoring program (and the
various inspections conducted under the program) are to collect information that supports enforcement of the
Water Quality Act by:
• Evaluating the compliance or dischargers with permit limitations
• Assessing compliance with orders or consent decrees
• Furnishing information which supports permitting.
This compliance evaluation involves two aspects: (1) collection of effluent samples by a NPDES inspector
during a Compliance Sampling Inspection (CSI), a Toxic Sampling Inspection (XSI), or a Compliance
Biomonitoring Inspection (CBI); and (2) evaluation of a permittee's self-monitoring procedures during a
Performance Audit Inspection (PAI) or a Compliance Evaluation Inspection (CEI). Under certain
circumstances, the inspection may also evaluates the industrial monitoring and enforcement efforts conducted as
part of a municipality's pretreatment program. This type of inspection is called a Pretreatment Compliance
Inspection (PCI).
To familiarize new NPDES inspectors with proper sampling procedures and to establish consistent
procedures throughout the NPDES compliance inspection program, this module outlines procedures to collect,
preserve, and transport wastewater samples. This module also discusses sampling equipment, methods for
onsite analytical procedures, flow measurement, and quality assurance and quality control procedures.
Appendix A of this module contains a glossary, of terms with which inspectors should be familiar. In addition
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to the discussion in this module, inspectors may also wish to consult the references listed in Appendix B.
Finally, after reviewing the module, each inspector should complete the questions in Appendix C to test his/her
understanding of its contents. Answers to these questions are also provided in Appendix C.
1.3 OBJECTIVES OF NPDES SAMPLING
Data obtained from sampling play a vital role in the NPDES program. Sampling is conducted to
accomplish one or more of the following objectives:
• Determine discharge quality at the time of the inspection
• Determine compliance with effluent limitations and permit conditions
• Collect information for use in permit development
• Assess the quality of self-monitoring data
• Provide a basis for enforcement proceedings in the event such proceedings become necessary.
Whether sampling is used as a part of an enforcement proceeding or to verify or compile data, sampling
activities should always be performed with great care.
1.4 SAMPLING TASKS
To achieve these objectives, one or more of the following sampling tasks must be performed:
• Sample at the location and for the parameters specified in the NPDES permit. Additionally, sample
at locations and for parameters requested by enforcement personnel but not specified in the permit
• Verify accuracy of permittee flow measuring device, either by verifying accuracy of in-plant
equipment or by actual independent flow measurement
• Verify that the sampling location(s) specified in the permit include all of the process and nonprocess
discharges and is adequate to collect a representative sample of the effluent
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• Verify that the permittee collects self-monitoring samples at the location specified in the permit
• Verify that the permittee's sampling and preservation techniques are adequate to ensure the collection
of a representative sample.
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2. SAMPLE COLLECTION
2.1 IMPORTANCE OF SAMPLE COLLECTION
Actual sample collection is an extremely important part of any sampling program. Without proper
sample collection techniques, even the most precise and accurate analytical procedures will produce results
which do not reflect the actual pollutant levels in the facility where sampling is performed prior to the
inspection. Such information includes:
• EPA guidance materials (manuals such as the NPDES Compliance Inspection Manual. Pretreatment
Compliance Monitoring and Enforcement Guidance. Samplers and Sampling Procedures For
Hazardous Waste Streams, and the Handbook for Sampling and Sample Preservation of Water and
Wastewatert may be helpful in developing a sampling plan.
• Thorough knowledge of the Department of Transportation (DOT) shipping regulations applied to the
constituents and preservatives contained in the samples in case any materials must be transported in a
specific manner.
• 40 Code of Federal Regulations (CFR) Part 136, "Guidelines Establishing Test Procedures for the
Analysis of Pollutants."
• NPDES permit and other pertinent information contained in the compliance files.
• Descriptions and photographs of the waste treatment process used, obtained through such materials as
the EPA development documents and prior inspection reports.
• Familiarity with production processes and sources of wastewaters or, in a municipal plant, a
knowledge of the raw waste and treatment systems. (For industrial processes, the EPA development
documents are a good source of information.)
• Knowledge of travel or shipping schedules in the area of the facility to be sampled in case samples
must be shipped to an offsite laboratory.
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2.2 SAMPLING PLAN
Before sampling a discharger for the first time, the inspector should clearly define the data needs and the
data quality objectives. The inspector should, if possible, refer to available file information; consult with the
appropriate compliance, legal, permitting, and laboratory personnel; and walk through the facility to become
familiar with its operation and layout.
Once the inspector understands the needs and objectives of the visit, a complete and comprehensive
quality assurance and sampling plan can be developed. This plan should contain the following items:
• Sampling Locations - Sampling locations should include all outfalls that appear in the NPDES permit.
Due to accessibility, needs, and objectives of the survey, and/or safety hazards, the sampling location
specified in the permit may not be adequate. Therefore, locations other than those specified in the
NPDES permit may need to be sampled. The number of samples to be taken at each location should
be indicated as well.
• Type of Sample - Type of sample depends on the parameters to be measured and/or the discharge
characteristics (i.e., batch discharge). This information is specified in 40 CFR Part 136 and the
NPDES permit.
• Type of Flow Measurement - Type of flow measurement is dependent on the flow rate, condition of
the wastewater, and variability of the discharge. Flow measurements are necessary to determine the
mass loading of a discharge. Flow should be measured or the permittee flow measurement device
should be verified.
• Parameters for Analysis - The NPDES permit specifies pollutant parameters monitoring by the permit
holder; these parameters are given as mass- or concentration-based discharge limitations. These
same parameters will be selected for compliance sampling but other parameters may be chosen as
well, if new processes or products have been incorporated in the plant or new or added sources of
wastewater are in evidence. If new processes or products have been incorporated in the plant,
additional sampling will help provide the basis for necessary permit modifications.
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• Sample Volume - The volume of sample collected depends on the type and number of analyses
necessary, based on parameters to be measured. The volume of the sample obtained should be
sufficient to perform all the required analyses [including laboratory Quality Assurance/Quality
Control (QA/QC) and repeat analyses] plus additional amounts to provide for any split samples that
may be required. A summary of required sample volumes for determination of various constituents
is provided in Appendix D.
• Type of Sample Containers - Selection and preparation of sample containers are based on the r
parameters to be measured and wastewater characteristics. Required containers are specified in 40
CFR Part 136, which is summarized in Appendix E.
• Sample Preservation Techniques - To preserve samples correctly, the appropriate chemicals must be
used and temperature control must be ensured. Preservation techniques and recommended holding
times are specified in 40 CFR Part 136 (see Appendix E).
• Sample Identification Procedures - Each container should have an acceptable identification label so
the sample can be tracked accurately and an uninterrupted chain-of-custody can be maintained.
• Sample Packaging and Delivery Concerns - Once a sample is collected, it must be delivered to the
laboratory for analysis to be conducted within the prescribed holding time. Holding times are
specified in 40 CFR Part 136.
• Safety Concerns - Sampling personnel should have complete information on any relevant plant safety
regulations and safety procedures to be followed during onsite sampling activities. Personnel should
be familiar with EPA Order 1440.2 (see Appendix F).
• Hazardous Waste Concerns - Samples of potentially hazardous effluent or process waste; samples
with extremely high or low pH; and samples that may contain extremely toxic, volatile, or explosive
substances will require special handling. DOT regulations for shipping these types of samples must
be followed.
• Chain-of-Custodv Procedures - Procedures for chain-of-custody must be followed for all samples.
Chain-of-custody forms should be used for this purpose.
• OA/OC Procedures - To ensure that data collected is valid, systematic checks must show that test
results are accurate.
Several of these considerations must be coordinated with the laboratory. The inspector should contact the
laboratory in advance of any sampling to discuss the sampling plan and QA/QC procedures, allocate laboratory
time, and obtain sample identification numbers.
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2.3 PREPARATION FOR SAMPLING
The success of each sampling task hinges on adequate preparation. Because personnel may not be
familiar with the facility to be inspected, the sampling plan should be reviewed prior to going out into the field.
Personnel should be briefed, as well, on all field procedures, particularly safety requirements. The inspector
should make sure that the appropriate sampling equipment is available and in good working order. When
sample analyses are to be performed in the field (such as pH), the necessary instruments should also be
included. Equipment must be checked prior to going into the field to ensure accurate operation and calibration.
In addition, a review of necessary safety equipment should be made and the inspector should be aware of any
hazards. The inspector and plant staff should discuss any unusual circumstances and formulate a plan for
dealing with them during the inspection.
A checklist of field sampling items (see Appendix G) can be used to ensure proper preparation. When
the type of waste to be sampled is known ahead of time, the list can be narrowed to the actual pieces
necessary.
2.4 SAMPLING SAFETY
In developing the sampling plan, the inspector should not sample at locations which pose a threat to
health and safety. Under hazardous conditions, a two-person inspection team is necessary. All required safety
equipment and protective clothing should be used as well. EPA Order 1440.2 (see Appendix F) specifies the
equipment and clothing required for EPA personnel at various levels of exposure.
Extensive and continuous education is essential to a successful safety program. The inspector should be
familiar with hazards associated with sampling in addition to the safety measures to be followed. For example,
if the inspector is required to enter a manhole or other confined space to obtain a sample, training in confined
space entry and rescue procedures is required. Potential hazards in a confined space include toxic gases, such
as hydrogen sulfide, chlorine, and carbon monoxide; or explosive gases, such as gasoline vapors or methane.
In addition, an atmosphere may be hazardous because there is not enough oxygen to support life due to the
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NPDES Compliance Monitoring Inspector Training: SAMPLING
presence of other gases, such as hydrogen sulfide and/or carbon dioxide. A confined space, such as a
manhole, should not be entered until the atmosphere has been tested for sufficient oxygen and the lack of toxic
or explosive gases. Such a confined space should never be entered alone or without a lifeline. The ability to
recognize hazards and to follow proper procedures will eliminate unnecessary accidents.
2.5 SAMPLING LOCATION
The inspector should always collect samples from a representative sampling that reflects total effluent
flow. Convenience and accessibility are important, but are secondary to the representativeness of a sample. A
representative location is where specific conditions or parameters are measured that adequately reflect the actual
conditions of those waters or wastewaters. The most representative samples will be drawn from a depth where
the flow is turbulent and well mixed and the chance of solids settling is minimal. Depending on the sampling
location, the depth may range from a few inches below the wastestream's surface to 40 to 60 percent of the
wastestream's total flow. Stagnant areas must be avoided as well, particularly if the wastewater contains
immiscible liquids or suspended solids. The inspector should take care to collect samples from the center of
the flow with the container facing upstream to avoid contamination. Wide channels or paths of flow may
require dye testing to determine the most representative sampling site. Dye testing involves placing a colored
dye in a wastestream and following the color to the outfall. If dye testing is inconclusive, cross-sectional
sampling may be required.
If the sample location specified in the NPDES permit is not adequate to collect a representative sample,
the inspector should determine an alternative location. This determination should be based on the inspector's
knowledge of the plant itself, the production processes, and the outfalls. If there is a conflict between the
sample location described in the permit and the location the inspector feels is most representative, samples
should be collected at both sites. The reason for the conflict should be thoroughly documented for later
resolution by the permitting authority.
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In addition to sampling effluent, the NPDES permit will often specify that the influent or internal
wastestreams be sampled, particularly when there is a percent removal requirement. Limits on the influent or
internal wastestreams of an industrial facility may be imposed only when exceptional circumstances make such
limitations necessary, such as when:
• The final discharge point is inaccessible (for example, under 10 meters of water)
• The wastes at the point of discharge are so dilute that monitoring is impractical
• Interferences among pollutants at the point of discharge make detection or analysis impossible.
When the permit requires that influent to the wastewater treatment facility be sampled (i.e., where
treatment efficiencies need to be determined), the preferred sample collection locations are those that provide
the best mixing, such as an influent line upflow distribution box from the plant wet well, or a flume throat.
These samples should be collected upstream of any sludge or supernatant recirculation. If samples are taken
from a closed conduit via a valve or sample tap or from a well equipped with a hand or mechanical pump, the
inspector should allow sufficient flushing time to ensure a representative sample, taking into account the
diameter, the length of pipe to be flashed, and the velocity of the flow.
2.6 SELECTION AND PREPARATION OF SAMPLE CONTAINERS
Sample containers must be made of chemically resistent material that does not affect the concentration of
pollutants to be measured. The containers used should be either glass or plastic. For most analyses, the option
of using either glass or plastic sample containers is open, and the selection of the sample container is based on
the organization's operating procedures. It is important that the inspector become familiar with these
procedures. If either type of sample container is acceptable and available, the inspector should use plastic ones
because they are less likely to break.
Plastic sample bottles are usually made of polyethylene; however, containers with teflon bottoms and lid
liners are available. The teflon provides added chemical resistance to strong mineral acids or organic solvents,
although this added chemical resistance is not normally needed. Glass sample bottles are required when
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NPDES Compliance Monitoring Inspector Training: SAMPLING
collecting samples for priority pollutants, oil and grease, and phenols, while plastic sample bottles are most
often used for Biochemical Oxygen Demand (BOD), Total Suspended Solids (TSS), metals, and nutrients.
Containers with wide mouths are recommended to facilitate the transfer of samples from sampler to sample
containers. In addition, the container must be large enough to contain the required volume for laboratory
analysis. The inspector should use dark containers for samples that contain constituents which will oxidize
from exposure to sunlight, such as iron cyanide (which is oxidized to hydrogen cyanide).
Container lids and closure linings must also be intact so they do not interfere with the pollutant
parameters to be measured. Most containers have tight, screw-type lids. Plastic containers are usually
provided with screw caps made of the same material as the container, so cap liners are usually not required.
Glass containers usually come with rigid plastic screw caps. Liner materials may be polyethylene,
polypropylene, neoprene, or teflon.
The inspector should make sure that all sample containers are clean and uncontaminated. The general
cleaning procedure for a sample container is to:
• Wash with hot water and detergent
• Rinse thoroughly with tap water followed by three or more rinses with organic-free water
• Rinse glass containers with an interference-free, redistilled solvent, such as acetone
• Dry in a contaminant-free room.
Precleaned and sterilized disposable containers are available for sampling use. The most commonly used
container of this type is the molded polyethylene cubitainer shipped (nested) to the buyer.
All tubing and other sampling system parts must be scrubbed with hot water and detergent, rinsed several
times with tap water, and then rinsed with distilled or deionized water. Further rinsing with acetone is advised
only when the type of tubing (e.g., teflon) is not susceptible to dissolution by the solvent.
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In most cases, the container should be rinsed three times with the wastewater to be sampled before the
sample is taken. However, some sample containers, such as those used for bacteriological sampling, require
special cleaning procedures. Bacteriological sample containers must be sterilized prior to sample collection.
The inspector should refer to Standard Methods for the Examination of Water and Wastewater and 40 CFR
Part 136 for proper procedures on sample container preparation.
2.7 SAMPLE TYPES
There are two primary types of samples: grab samples and composite samples. Each type has distinct
advantages and disadvantages. To obtain a complete characterization of a specific facility's effluent, the two
sample types can be used in combination. However, the inspector must use the appropriate sample type for
compliance monitoring based on the requirements specified in the NPDES permit.
A grab sample is an individual sample collected over a period of time not exceeding 15 minutes. Grab
samples represent the conditions that exist at the moment the sample is taken and do not necessarily represent
conditions at any other time. Grab sampling is the preferred method of sampling under the following
conditions:
• When the effluent is not discharged on a continuous basis. The true characteristics of a wastestream
may be obtained only when the batch discharge occurs.
• When specific pollutant parameters are immediately affected by biological, chemical, or physical
interactions, such as pH, temperature, chlorine, soluble sulfide, volatile organics, cyanide, and
dissolved oxygen. Individual grab samples should always be taken for oil and grease and when
bacteriological analysis will be performed.
• When the waste conditions are relatively constant over the period of discharge. In lieu of complex
sampling activities, a grab sample provides a simple and accurate method of establishing waste
characteristics.
• When it is necessary to check for extreme conditions. For example, composite samples would tend
to conceal peaks in the pH of a discharge. Extreme acidic and alkaline conditions may cancel each
other out, causing a composite sample to appear neutral.
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In addition, grab samples may be used to determine consistency in an industry's self-monitoring data and
to corroborate results of composite samples.
A composite sample is a sample collected over time, formed either by continuous sampling or by mixing
discrete samples. Composite samples reflect the average characteristics of the wastestream during the
compositing period. Composite samples are used when stipulated in a permit and when:
• Determining average pollutant concentration during the compositing period
• Calculating mass/unit time loadings.
»
Various methods for compositing samples are available. Composite samples may be collected
individually at equal time intervals if the flow rate of the sample stream does not vary more than plus or minus
10 percent of the average flow rate, or they may be collected proportional to the flow rate. The permit may
specify which composite sample to use, either time composites or flow-proportional composites. The
compositing methods, all of which depend on either continuous or periodic sampling, are described below:
• Time Composite Sample - Composed of discrete sample aliquots collected in one container at
constant time intervals. This method provides representative samples when the flow of the sampled
stream is constant. This type of sample is similar to a sequential composite sample (described
below).
• Flow-Proportional Composite Sample - There are two methods used to collect this type of sample.
One method collects a constant sample volume per stream flow [e.g., 200 milliliters (ml) sample
collected for every 5,000 gallons of stream flow] at time intervals proportional to stream flow. This
method provides representative samples of all wastestreams when the flow is measured accurately.
For this reason, it is used most frequently. In the other method, the sample is collected by
increasing the volume of each aliquot as the flow increases, while maintaining a constant time
interval between the aliquots.
• Sequential Composite Sample - Composed of discrete samples composited in individual containers at
constant time intervals or constant discharge increments. For example, samples collected every 15
minutes are composited each hour. The 24-hour composite is made up from the individual 1 -hour
composites. Each of the 24 individual samples is manually flow-proportioned according to the flow
recorded for the hour the sample represents. Each flow-proportioned sample is then added to the
composite samples. The actual compositing of the samples may be done in the field or the
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laboratory. In most cases, compositing in the field is preferable since only one sample container
must be cooled, transported to, and handled in the laboratory. This method of compositing is
frequently used since an automatic sampler can easily collect the individual samples. A vahation of
this method is to collect a constant volume of sample taken at constant discharge increments, which
are measured with a totalizer. For example, one aliquot is collected for every 10,000 gallons of
flow.
• Continuous Composite Sample - Collected continuously from the wastestream. The sample may be a
constant volume which is similar to the time composite, or the volume may vary in proportion to the
flow rate of the wastestream, in which case the sample is similar to the flow-proportional composite.
Table 2-1 lists the advantages and disadvantages of each sampling method. Either manual or automatic
sampling techniques can be used. If a sample is composited manually, sample manipulation should be
minimized to reduce the possibility of contamination.
The inspector must always use the method required by the permit and also weigh advantages and
disadvantages when choosing between the use of grab or composite sampling methods. While grab sampling
allows observation of unusual conditions that may exist during discharge, such as sudden bursts of color or
turbidity, this method is labor-intensive and impractical when sampling is performed at many locations over
extended periods of time. When sampling a large number of locations, the use of automatic samplers is more
practical. Automatic samplers also help reduce human error, specifically in complex sampling activities, such
as flow-proportional sampling, and reduce exposure to potentially hazardous environments. The primary
disadvantage to automatic sampling is the cost of the equipment and maintenance requirements. Many
automatic samplers in use today are electronically controlled and must be sent back to the manufacturer when a
malfunction occurs. There is also a greater possibility of tampering when using an automatic sampler.
2.8 SAMPLE COLLECTION TECHNIQUES
To obtain a representative sample, sampling must be conducted where wastewater flow is adequately
mixed. Ideally, a sample should be taken in the center of the flow where velocity is highest and there is little
possibility of solids settling. The inspector should avoid skimming the surface of the wastestream or dragging
the channel bottom. Mixing of the flow is particularly important for ensuring uniformity. Sampling personnel
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TABLE 2-1. COMPOSTING METHODS
Method
Advantages
Disadvantages
Comments
Time Composite
Constant sample
volume, constant
time interval
between samples
Flow-Proportional
Composite
• Constant sample
volume, time in-
terval between
samples propor-
tional to stream
flow
• Constant time
interval between
samples, sample
volume propor-
tional to total
stream flow at
time of sampling
Minimal instrumen-
tation and manual
effort; requires
no flow measurement
Minimal manual
Minimal
instrumentation
May lack represen-
tativeness especi-
ally for highly
variable flows
Requires accurate
flow measurement
reading equipment;
manual compositing
from flow chart
Manual compositing
from flow chart in
absence of prior
information on the
ratio of minimum
to maximum flow;
chance of collect-
ing too small or
too large individ-
ual discrete
samples for a given
composite volume
Widely used in
both automatic
samplers and
manual handling
Widely used in
automatic as well
as manual sampling-
Used in automatic
samplers and
widely used as
manual method
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TABLE 2-1. COMPOSITING METHODS (Continued)
Method
Advantages
Disadvantages
Comments
• Constant time Minimal
interval between instrumentation
samples, sample
volume propor-
tional to total
stream flow since
last sample
Manual compositing
from flow chart in
absence of prior
information on the
ratio of minimum
to maximum flow;
chance (^collect-
ing either too
small or too large
individual dis-
crete samples for
a given composite
volume
Not widely used in
automatic samplers
but may be done
manually
Sequential
Composite
• Series of
short period com-
posites, constant
time intervals
between samples
• Series of short
period composites,
aliquots taken at
constant dis-
charge increments
Useful if fluctua-
tions occur and
time history is
desired
Useful if fluctua-
tions occur and the
time history is
desired
Requires manual
compositing of
aliquots
Requires flow
totalizer; re-
quires manual
compositing of
aliquots
Commonly used;
however, manual
compositing is
labor intensive
Manual compositing
is labor intensive
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TABLE 2-1. COMPOSITING METHODS (Continued)
Method
Advantages
Disadvantages
Comments
Continuous
Composite
• Constant sample
volume
Sample volume
proportional to
stream flow
flows; minimal
manual effort
Minimal manual
effort, requires
no flow measurement
highly variable
flows
Most representa-
tive especially
for highly variable
sample volume,
variable pumping
capacity, and
power
Requires large
sample capacity;
may lack represen-
tativeness for highly
representative flows
Requires accurate
flow measurement
equipment, large
sample volume,
variable pumping
capacity and power
Practical but not
widely used
Not widely used
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should be cautious when collecting samples near a weir because solids tend to collect upstream and floating oil
and grease accumulate downstream. If the sample is not to be tested for volatile organics or will not be
affected by stripping dissolved gases, mechanical stirring may be used or a stream of air may be introduced
into the wastestream.
When taking a grab sample, the entire mouth of the container should be submerged below the
wastestreatn's surface. A wide mouth bottle with an opening of at least two inches is recommended for this
type of sampling. When using a composite sampler, the sample line should be kept as short as possible and
sharp bends, kinks, and twists in the line (where solids can settle) should be avoided. The sample line should
be placed so that changes in flow will not affect sample collection.
2.9 SAMPLE VOLUME
The volume of samples collected depends on the type and number of analyses needed, as reflected in the
parameters to be measured and the requirements of the analytical laboratory being used. Sample volume must
be sufficient for all analyses, including laboratory QA/QC and any repeat analyses used for verification.
Laboratory personnel should be contacted for the sample volume required to complete all analyses. Individual,
minimum composite portions should be 25 to 100 milliliters, with a total composite volume of 2-4 gallons.
Larger volumes may be necessary if samples are to be separated into aliquots or if bioassay tests are to be
conducted.
Volume requirements for individual analyses range from 25 ml for pH and volatile organic
determinations to 1,000 ml or more for BOD, oil and grease, settleable matter, and temperature determinations.
The inspector should always collect more than the minimum sample volume to allow for spillage and laboratory
reruns. Appendix D lists minimum volume requirements for various pollutant parameters.
2.10 SAMPLE PRESERVATION AND HOLDING TIMES
Preservation techniques ensure that the sample remains representative of the wastestream at the time of
collection. Since most pollutants in the samples collected are unstable (at least to some extent), this instability
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requires that the sample be analyzed immediately or that it be preserved or fixed to minimize changes in the
pollutant concentrations between the time of collection and analysis. Because immediate analysis is not always
possible, most samples are preserved regardless of the time of analysis.
However, problems may be encountered when 24-hour composite samples are collected. Since sample
deterioration can take place during the compositing process, it is necessary to preserve or stabilize the samples
during compositing in addition to preserving aggregate samples before shipment to the laboratory. Preservation
techniques vary depending on the pollutant parameter that is to be measured; therefore, familiarity with 40 CFR
Part 136 (see Appendix E) is essential to ensure proper preservation techniques. It is important to verify that
the preservation techniques for one parameter do not affect the analytical results of another in the same sample.
If this is the case, two discrete samples should be collected and preserved accordingly.
Sample preservation techniques consist of refrigeration, pH adjustment, and chemical fixation.
Refrigeration is the most widely used technique because it has no detrimental effect on the sample composition
and does not interfere with any analytical methods. Refrigeration requires that the sample be quickly chilled to
a temperature of 4°C, which suppresses biological activity and volatilization of dissolving gases and organic
substances. This technique is used at the start of sample collection in the field and during sample shipment,
and continued until the sample it received in the laboratory for analysis. Sample temperature should be verified
and recorded by the inspector. This is particularly important if the analytical results are to be used in an
enforcement action.
In addition to preservation techniques, 40 CFR Part 136 indicates maximum holding times. Times listed
are the maximum times between sample collection and analysis that are allowed for the sample to be considered
valid. The wastewater becomes a sample upon combination of the last aliquot. At that point, holding time
limitations begin. A detailed list of preservation methods and holding times appears in Appendix E of this
module. These sample preservation procedures and holding times were selected by EPA because they retard
sample degradation and minimize monitoring costs by extending holding times as long as possible.
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2.11 SAMPLE DOCUMENTATION
Because sampling reports may be used in enforcement proceedings, the inspector must keep a precise
record of sample collection and data handling. All field records containing these data must be signed by the
inspector at the time of collection. If required, the following information should also be documented in the
field records.
• Unique Sample or Log Number - All samples should be assigned a unique identification number. If
there is a serial number on the transportation case, the inspector should add this number to his/her
field records.
• Date and Time of Sample Collection - Date and time (including notation of a.m. or p.m.) of sample
collection must be recorded. In the case of composite samples, the sequence of times and aliquot
size should be noted.
• Source of Sample. Including Facility Name and Address - This may be obtained from the sample
request form. A narrative description and/or diagram referring to the particular site where the
sample was taken should be included.
• Name of Sampling Personnel - The name(s) and initial(s) of the person(s) taking the sample must be
indicated. For a composite sample, the name(s) of the person(s) installing the sampler and the
name(s) of the person(s) retrieving the sample must be included.
• Sample Type - Each sample should indicate whether it is a grab or composite sample. If the sample
is a composite, volume and frequency of individual samples should be noted.
• Preservation Used - Any preservatives (and the amount) added to the sample should be recorded.
The method of preservation (e.g., refrigeration at 4°C) should be indicated.
• Analysis Required - All parameters for which the sample must be analyzed at the laboratory should
be specified.
• Field Analysis - Field measurements must be recorded at the time that the analysis is completed.
Examples of analysis which must be conducted and recorded in the field include pH, temperature,
dissolved oxygen, chlorine residual, and sulfites.
• Flow - If flow is measured at the time of sampling, the measurement must be recorded.
• Production Rates - Information on products manufactured and production rates should be included
since many effluent limitations are based on production rates.
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• Date. Time, and Documentation of Sample Shipment - The shipment method (i.e., air, rail, or bus)
as well as the shipping papers or manifest number should be noted.
• Comments - Comments refer to all relevant information pertaining to the sample or the sampling site.
Such comments include the condition of the sample site, observed characteristics of the sample,
environmental conditions that may affect the sample, and problems encountered in sampling.
2.12 SAMPLE IDENTIFICATION AND LABELING
At the time that a sample is collected, a waterproof, gummed label or tag should be attached to the
sample container. This label is necessary to prevent misidentification of samples since it provides the
laboratory with relevant information for sample analysis, such as:
• Name of the sample collector
• Sample identification number
• Date and time of sample collection
• Location of sample collection
• Preservatives used.
Sample seals should be used to protect the sample's integrity from the time it is collected to the time it is
opened in the laboratory. The seal should also contain the collector's name, the date and time of sample
collection and a sample identification number. Information on the seal must be identical to the information on
the label. In addition, the seal must be attached so it must be broken to open the sample container. Example
sample identification labels are provided in Appendix H. Caution should be observed to assure that glue on
sample seals and tag wires do not contaminate samples, particularly those containing volatiles and metals.
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2.13 SAMPLE PACKAGING AND SHIPPING
After the samples are properly labeled, they should be placed in a transportation case along with the
chain-of-custody record form, pertinent field records, and analysis request forms. (Chain-of-custody
procedures are covered below.) Glass bottles should be wrapped in foam rubber, plastic bubble wrap, or other
material to prevent breakage during shipment. The wrapping can be secured around the bottle with tape.
Samples should be placed in ice or a synthetic ice substitute that will maintain sample temperature at 4°C
throughout shipment. Ice should be placed in double-wrapped watertight bags to ensure the water will not drip
out of the shipping case. Metal or heavy plastic chests make good sample transportation cases. Filament tape
wrapped around each end of the ice chest ensures that it will not open during transport. Sampling records can
be placed in an envelope and taped to the transportation case to avoid getting them wet in case either a sample
or ice bag leaks. Shipping containers should also be sealed to prevent tampering.
Most samples will not require any special transportation precautions except careful packaging to prevent
breakage and/or spillage. If the sample is shipped by common carrier or sent through the U.S. mail, it must
comply with DOT Hazardous Materials Regulations (49 CFR Parts 171-177). Air shipment of hazardous
materials samples may also be covered by requirements of the International Air Transport Association (IATA).
Before shipping a sample, the inspector should be aware of, and follow, any special shipping requirements.
Special packing and shipping rules apply to substances considered hazardous materials as defined by IATA
rules. Wastewater samples are not generally considered hazardous materials (see Footnote Number 3 in
Appendix E).
2.14 CHAIN-OF-CUSTODY PROCEDURES
Once a sample has been obtained and collection procedures are properly documented, a written record of
the chain of possession of that sample must be made. "Chain-of-custody" refers to the documented account of
changes in possession that occur for a particular sample or set of samples. The chain-of-custody record allows
an accurate step-by-step recreation of the sample path, from origin through analysis. Some of the information
that needs to be addressed in chain-of-custody is:
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• Name of the person collecting the sample
• Sample ID numbers
• Date and time of sample collection
• Location of sample collection
• Name(s) and signature(s) of all persons handling the samples in the field and in the laboratories.
To ensure that all necessary information is documented, a chain-of-custody form should be developed.
An example of such a form used by EPA is found in Appendix I. Chain-of-custody forms should be preprinted
on carbonless, multipart paper so all personnel handling the sample receive a copy. All sample shipments must
be accompanied by the chain-of-custody record while a copy of these forms should be retained by the
originator. In addition, all receipts associated with the shipment should be retained. Carriers typically will not
sign for samples; therefore, seals must be used to verify that tampering has not occurred during shipment.
When transferring possession of samples, the transferee must sign and record the date and time on the
chain-of-custody record. In general, custody transfers are made for each sample, although samples may be
transferred as a group, if desired. Each person who takes custody must fill in the appropriate section of the
chain-of-custody record.
Typically, the chain-of-custody for a sample is as follows:
• Sampling Personnel - The person(s) who takes possession of the sample as soon as it is collected
• Laboratory Personnel - Laboratory personnel, whether from agency laboratories or from an
independent laboratory, will be responsible for the sample from analysis through disposal.
In addition, permit and/or compliance group should receive a copy of the completed chain-of-custody
form, particularly if the sample results are to be used for enforcement purposes.
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Chain-of-custody records are critical if analytical data are to be used in an enforcement proceeding
because they allow such data to be introduced as evidence without testimony of the persons who made the
record. Therefore, it is important that all chain-of-custody records be complete and accurate. To maintain the
sample's integrity, chain-of-custody records must show that the sample was properly collected, preserved, and
analyzed, and was not tampered with. Since it is not possible to predict which violations will require legal
action, it should be assumed that all data generated from sampling will be used in court.
2.15 SPECIAL SAMPLING REQUIREMENTS
In general, most samples are taken using similar techniques. However, the inspector should be aware
that certain parameters require special precautions in sample collection, preservation, and handling.
2.15.1 Bacteriological Sampling
Bacteriological sampling should always be a grab sample collected in a sterilized container, according to
Standard Methods for the Examination of Waster and Wastewater. A 125 ml or larger sample container should
be used to provide a minimum sample volume of 100 ml and adequate mixing space. Unlined caps or ground
glass tops should be used to ensure complete sterilization of the container's closure. Bottles and caps must be
thoroughly cleaned with detergent and hot water and a final deionized water rinse should be performed prior to
use. All traces of detergent must be removed. A test for bacteriostatic or inhibitory residues is described in
Standard Methods for the Examination of Water and Wastewater.
When sampling water containing residual chlorine, a dechlorinating agent such as sodium thiosulfate
should be added to the sample bottle prior to sterilization in an amount to provide an approximate concentration
of 100 milligram per liter (mg/1) in the sample. This can be accomplished by adding 0.1 ml of a 10 percent
solution of sodium thiosulfate to a 125 ml sample bottle. The dechlorinating agent neutralizes any residual
chlorine and will prevent further reaction between bacteria and chlorine.
For bacteriological sampling, the container must be kept unopened until the moment that the sample is
collected. During sampling, the bottle's lower part should be held with the mouth of the bottle facing the
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direction of the current. The stopper or cap should be protected from contamination during sampling and must
be replaced immediately after the sample has been taken. The inspector should fill the sample bottle to within
one to two inches of the top. S/he should not rinse the bottle with the sample. The inspector should never
collect the sample in an unsterilized sample container and then transfer it to a sterile container.
2.15.2 Radiological Sampling
Polyethylene, polyvinyl chloride, or teflon containers are recommended for collecting radioactive samples
because these containers are less adsorbent than glass or metal containers. Since radioactive elements are often
present in submicrogram quantities, a large fraction of the elements may be lost by adsorption on container or
glassware surfaces used in analysis. This loss may, in turn, cause a loss of radioactivity and possibly
contaminate subsequent samples due to reuse of inadequately cleaned containers. Glass bottles are also more
susceptible to breakage during handling than plastic containers.The standard preservation technique for
radiological sampling is acidification to a pH of less than 2.0 with HNO,. However, there are some
exceptions, and the inspector should contact the laboratory before the sample is collected to find out what these
are. Prior to sampling, the area should be surveyed with a beta-gamma survey instrument, such as a Geiger-
Mueller meter. If radiation levels above instrument background are detected, the inspector should consult a
radiation safety specialist to determine appropriate safety procedures.
2.15.3 Metals Sampling
New plastic or glass containers should be used for metals sampling. If previously used containers are
used for metals sampling, they should be washed with 1 + 1 nitric acid and rinsed with redistilled water.
Samples should be preserved with nitric acid at collection time to keep metals in solution and prevent them
from plating out on the container wall. Approximately 5 ml of concentrated, redistilled HNO, should be added
per liter of sample to reduce pH to below 2.0. If only dissolved metals are to be measured, the sample should
be filtered through a 0.45 membrane filter prior to acidification.
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2.15.4 Volatiles Sampling
Analysis of volatile organic substances requires a 40 ml glass sample vial, sealed with a teflon-coated
septum seal. The sample must be collected so there are no air bubbles in the container after the screw cap and
septum seal are applied. Because it is difficult to completely fill the 40 ml bottle directly from the
wastestream, a larger glass bottle that has been appropriately cleaned may be used to grab the sample from the
wastestream; the inspector should then transfer the sample to the 40 ml vial. The sample must be poured into
the vial very slowly to minimize aeration of the sample. If the sample is known to contain residual chlorine,
10 mg of sodium thiosulfate must be added to the empty vial first.
2.15.5 Oil and Grease Sampling
Sampling for oil and grease is unique because the pollutant is immiscible. Oil tends to adhere to the
sampling device; therefore, an oil and grease sample must always be a grab sample taken in a glass container.
A teflon insert should be included in the glass sample container's lid. However, if teflon is not available,
aluminum foil extending out from under the lid may be used. Grab samples for analysis of oil and grease (or
other immiscible pollutants) should not be transferred from the sampling container and must be analyzed
separately to avoid pollutant loss. The sample must be preserved by adding H,SO4 to reduce the pH to less
than 2.0 and then chilled to 4°C.
2.15.6 Cyanide Sampling
Cyanide is very reactive and unstable. Because of its nature, cyanide must be analyzed as soon as
possible after collection. The sample must be taken in a polyethylene or glass bottle. If the sample cannot be
analyzed immediately, it must be preserved after collection with NaOH pellets or a strong NaOH solution to
raise the pH of the sample to 12.0 or above. If residual chlorine is present, 0.6 grams (g) of ascorbic acid is
added to the sample container. A preserved cyanide sample has a maximum holding time of 14 days.
However, the maximum holding time is reduced to 24 hours when sulfide is present. A lead acetate paper spot
test can be done in the field to determine the presence of sulfide. Sulfide can be removed by adding
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cadmium nitrate powder to the sample. If cadmium nitrate is added, the sample must be filtered prior to
adding the NaOH. Preserved samples must be stored in a closed, dark bottle at 4°C.
2.15.7 Organics and Pesticides
Although conventional sampling practices should be followed for these parameters, there are several
special considerations. First, the sample bottle must not be prennsed with the sample before collection.
Second, if grab samples of these parameters are taken, the samples must always be collected in amber glass
containers, one liter to one gallon volume. Composite samples must be collected in refrigerated glass
containers through teflon tubing. Third, if the sample can not be extracted within 72 hours of collection, the
sample's pH may need to be adjusted with sodium thiosulfate. Table II of 40 CFR Part 136 (which is
excerpted in Appendix E) should be consulted to determine the specific preservation method for each group of
organic compounds and pesticides.
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3. ANALYTICAL METHODS FOR ONSITE ANALYSIS
Proper analytical methods are extremely important to a successful sampling program. The inspector
should consult such reference materials as 40 CFR Part 136, EPA's Methods for Chemical Analysis of Water
and Wastes, and Standard Methods for the Examination of Water and Wastewater before beginning any
analytical tests.
Generally, pollutant parameter values should be determined by one of the standard analytical methods
shown in Appendix E. The inspector usually does not analyze the actual collected sample. The exception to
this is analyzing a sample for parameters that cannot be preserved. Measurements of these parameters should
be taken at the beginning of the sampling period so that, if violations or problems are identified, additional
measurements or information may be obtained during the remainder of the inspection. The most common
parameters for which field measurements are conducted are temperature, Dissolved Oxygen (DO), pH, and
chlorine residual. Field analysis of each of these parameters is highlighted below.
• Temperature - Temperature determinations can be made with any good grade mercury filled or
dial-type Celsius thermometer. The dial-type thermometer is preferred over the glass type for field
work because of its durability and ease of reading. All temperature measuring devices must be
calibrated periodically with a precision thermometer traceable to the National Bureau of Standards.
• DO - The electrode method is predominantly used for onsite DO determinations. The sample size
for this type of determination is 300 ml. Most DO probes are temperature-sensitive and have
temperature compensation built in. The DO meter must be calibrated onsite in accordance with the
manufacturer's specifications before any DO measurements are made.
• gH - pH determinations are often conducted during a sampling inspection. The inspector should
arrange to have a pH meter available. The pH meter must be properly calibrated by the use of two
buffers prior to each set of pH measurements. The inspector should be aware of conditions in the
wastestream that may cause inaccurate readings. For example, oil and grease may interfere with
readings (cause a sluggish response by coating the electrodes).
• Chlorine Residual - Chlorine in an aqueous solution is unstable and the concentration will decrease
rapidly. Exposure to sunlight or other strong light, or agitation will accelerate chlorine reduction;
therefore, analysis should begin immediately after sampling. A field colormetric kit such as the
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HACH DRIOO is an approved EPA procedure if the instrument is properly calibrated using
standards to develop a calibration curve.
Conductivity - Specific conductance is a useful method to approximate the total amount of
inorganic dissolved solids. Conventional conductivity devices consist of two or more platinum
electrodes separated by a test solution. The major disadvantage with this type of system is the
possibility of polarization or poisoning (fouling) of the electrodes. Conductivity systems based on
the measurement of inductance or capacitance are also available. The electrodes in these systems
are insulated by a layer of glass or other insulating material. System response is less rapid, but
problems with fouling and polarization are eliminated. Temperature is important in conductivity
measurements. For example, the conductivity of salt water increases 3 percent per degree at 0°C,
and only increases 2 percent per degree at 25°C. Therefore, it is necessary to record temperature
with conductivity measurements or to adjust the temperature of the samples prior to making
conductivity measurements. Most conductivity meters have a manual temperature compensation
feature.
The inspector should always remember that when analysis is performed in the Held, each piece of
equipment should be checked prior to leaving for the sampling site. The inspector should verify that the
equipment is in working order and calibrated and that batteries are properly charged before leaving on the
inspection.
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4. AUTOMATIC SAMPLERS
A wide vahety of automatic samplers are available commercially. Most have the following five
interrelated subsystem components:
• Sample Intake Subsystem - The sample intake gathers representative samples from the sampling
stream. The intake is usually the end of a plastic suction tube. The inside diameter of this tube
should be at least 1/4 inch, which is large enough to lessen chances of clogging but small enough
to maintain velocity and to avoid solids settling. It should also be resistant to physical damage from
large objects in the flow stream. Nonleaching tygon tubing is most often used; however, teflon
tubing must be used when sampling for priority pollutants. The end of this tubing should be fixed
so that its sampling location can be maintained throughout the sampling period. The automatic
sampler should provide for the line purging after each sample is drawn to prevent contamination of
subsequent samples.
• Sample Gathering Subsystem - Automatic samplers provide one of three basic gathering methods:
Mechanical - Mechanical gathering subsystems are usually built into place and include devices
such as cups on cables, calibrated scoops, and paddle wheels with cups. Although these
systems may obstruct the stream flow, they also take into account site-specific considerations,
such as a very high sampling lifts and wide or extremely deep channel flows. Because of the
mechanical nature of the system. These units require periodic inspection and maintenance.
Forced Flow - Forced-flow gathering subsystems are often built into place as permanent
sampling facilities; thus, like the mechanical gathering subsystems, they may obstruct the
stream flow. They also require periodic inspection and maintenance. However, forced flow
subsystems have the advantage of being able to sample at great depths. In addition, because
this gathering system uses air pressure to transport the sample, it may be ideal for sample
collection in potentially explosive environments.
Suction Lift - The suction lift is the most widely used type of sample gathering subsystem due
to its versatility and minimal affect on flow patterns. Suction lifts are limited to 25 vertical
feet or less because of internal friction losses and atmospheric pressure. As with all suction
devices, when the pressure or a liquid that contains dissolved gases is reduced, the dissolved
gases tend to pass out of the solution. Because the gases leaving the surface have entrained
suspended solids, the liquid's surface layer becomes enhanced with suspended solids. To
minimize the concentration effect, at least 100 ml per sampling unit should be collected.
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Sample Transport Subsystem - The sample is usually transported from the sample intake to the
collection bottle by a plastic tube referred to as the sample transport subsystem. The tubing
should be at least 1/4 inch inside diameter to maintain adequate flow and to prevent plugging.
The tubing should be sized so that a velocity of at least two feet per second can be maintained.
Care should be exercised to avoid sharp bends, kinks, and twists in the transport line.
Automatic samplers usually provide a line purge after each sample is collected to ready the
line for the next sample transfer. The inspector should provide clean transport tubing for each
new sample site to prevent sample contamination.
Sample Storage Subsystem - The sample storage subsystem can accommodate either a single
large collection bottle or a number of smaller collection bottles. The total sample volume
storage capability should be at least 2 gallons (7.6 liters); some samplers have a capacity as
great as 5 gallons. To preserve the samples, storage subsystems should also be large enough
to provide space for ice to chill the sample after collection. In addition, preservatives may be
added to the sample bottle(s) prior to sample collection. Samples with individual bottles for
discrete collection are usually equipped with a cassette which rotates to fill the bottle at the
time of sampling. As previously mentioned, whether large composite or discrete samples are
collected, it is necessary to use collection bottles made of the appropriate materials.
Controls and Power Subsystem - The automatic samplers most widely used have encapsulated
solid state controls. This minimizes the effect of the highly unfavorable environments that
may be encountered in the field, such as high humidity and corrosiveness. These units are
also sealed so they may be used with minimum risks in potentially explosive environments. In
addition, sealed units protect the controls if the sampler is accidentally submerged. Samplers
operating from a power supply are more reliable than battery operated models; however, field
conditions often prohibit the use of a power supply. The control units allow selection of time
or flow-compositing method, or continuous sampling method.
Several factors should be considered in selecting automatic sampling equipment. Among these are:
(1) convenience of installation and maintenance; (2) equipment security; and (3) cold weather operation.
Sampling equipment should always be handled carefully and maintained in accordance with the manufacturer's
instructions. Most equipment failures are caused by careless handling and poor maintenance. Equally
important is equipment security, specifically when sampling is done as part of an enforcement proceeding.
Manhole locations where battery-operated equipment may be installed and the cover replaced will aid in
maintaining security. If sampling equipment must be left unattended, the sampler should be provided with a
lock or seal which, if broken or disturbed, would indicate that tampering had occurred.
NOTES:
4-2
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NFDES Compliance Monitoring Inspector Training: SAMPLING
Use of automatic samplers during cold weather presents problems with freezing. Sampler malfunctions
and frozen intake lines are quite common. These problems may be handled by using heat tape or placing the
sampler inside a thermostatically controlled, electrically heated enclosure. In the absence of special equipment,
freezing may be prevented by installing the sampler in a manhole or wet well or by wrapping the sampler with
eight or nine inches of insulation and wind protection. Also, the sampler should be positioned well above the
effluent stream so that the tubing runs in a taut, straight line to prevent liquid from pooling. Criteria for
selecting automatic sampling equipment are listed in Appendix J.
NOTES:
4-3
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NPDES Compliance Monitoring Inspector Training: SAMPLING
5. FLOW MEASUREMENT
5.1 IMPORTANCE OF FLOW MEASUREMENT
Pollutant limits in a NPDES permit are usually specified as a mass loading. To determine a mass
loading and thereby evaluate compliance with permit limits, it is necessary for the inspector to obtain accurate
flow data. "Flow measurement" is the commonly used term for this process. In addition to verifying
compliance with permit limits, flow measurement serves to:
• Provide operating and performance data on the wastewater treatment plant
• Compute treatment costs, based on wastewater volume
• Obtain data for long-term planning of plant capacity.
This section briefly describes flow measurement. For a more detailed discussion, the inspector should refer to
two other EPA guidance manuals, the 1988 NPDES Compliance Inspection Manual and the 1981 NPDES
Compliance Flow Measurement Manual.
5.2 OPEN CHANNEL FLOW
Open channel flow, where the flow occurs in conduits that are not full of liquid, is the most prevalent
type of flow at NPDES-regulated discharge points. Partially full pipes that are not under pressure are classified
as open channels as well. Open channel flow is measured using both primary and secondary devices. These
devices are explained below.
5.2.1 Primary Devices
Primary devices are calibrated, hydraulic structures installed in the channel so flow measurements can be
obtained by measuring the depth of liquid at a specific point in relationship to the primary device. Weirs and
flumes are examples of primary devices.
NOTES:
5-1
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NPDES Compliance Monitoring Inspector Training: SAMPLING
The most common type of weir consists of a thin, vertical plate with a sharp crest that is placed in a
stream, channel, or partially filled pipe. Figure 5-1 shows a profile of a sharp-crested weir and indicates the
appropriate nomenclature. Four common types of sharp-crested weirs are shown in Figure 5-2. The crest is
the upper edge of the weir to which water must rise before passing over the structure. The depth of water
above the crest of the weir is termed the "head." To determine flow rate, the inspector must measure the
hydraulic head. The rate of flow over a weir is directly related to the height of water (hydraulic head) above
the crest. To measure the hydraulic head, a measuring device is placed upstream of the weir at a distance of at
least four times the head. To approximate the head, the inspector can measure at the weir plate. However,
this value will provide only a rough estimate of flow.
The flume is an artificial channel constructed so the wastestream flows through it. The wastestream's
flow is proportional to the depth of water in the flume and is calculated by measuring the head. A flume is
composed of three sections: (1) a converging upstream section; (2) a throat or contracted section; and (3) a
diverging or dropping downstream section. The two principal types of flumes are the Parshall Flume and
Palmer-Bowles Flume.
Figure 5-3 presents a sketch of the Parshall Flume, identifying its different parts and indicating
capacities. In the Parshall Flume, the floor level of the converging section is higher than the floor of the throat
and diverging section. The Flume operates on the principle that when water flows through a constriction in the
channel, a hydraulic head is produced that is proportional to the flow. The Parshall Flume is good for
measuring open channel waste flow because if is self-cleaning. Sand or suspended solids are unlikely to affect
the devices's operation.
A Palmer-Bowles Flume, which may or may not have a constriction, has a level floor in the throat
section and is placed in a pipe for approximately the length of the pipe's diameter. The depth of water above
the raised step in the throat is related to the discharge rate. The head should be measured a distance (d/2)
upstream of the throat where d is the size (width) of the flume. The height of the step is usually unknown until
NOTES:
5-2
-------
K= APPRO X. 0.1
POINT TO MEASURE
HYDRAULIC HEAD, H
20 H
max
A
i
i
or
STRAIGHT
INLET RUN
SHARP - CRESTED WEIR
WEIR CREST
MINIMUM
DISCHARGE LEVEL
FOR FREE FALL
WEIR
n
^
ts
I
a
H
I
= .
i
5
FIGURE 5-1. PROFILE AND NOMENCLATURE OF SHARP-CRESTED WEIRS
-------
I/I
i.
Crest Length
L
Hmax
2Hmax
Minimum
Suppressed (Without End Contractions)
Rectangular Heir
2Hmax
Minimum Crest Length
_ I
-Hmax
2Hmax
Minimum
2Hmax L
Minimum Crest Length
- I _ I
Hmax
2Hmax
Minimum
Trapezoidal (Cipollettl) Sharp-Crested Heir
2Hmax
Minimum
\
7
I
2Hmax
Minimum
V-Notch (Triangular) Sharp-Crested Weir
Contracted (With End Contractions)
Rectangular Weir
FIGURE 5-2. FOUR COMMON TYPES OF SHARP-CRESTED WEIRS
ES C
e Monitoring Inspec
-
§
f
s
>
7
C.
-------
Ul
Ul
Zero Reference
Level for Ha
and
o
I
r*.
§.
B1
H
5
I
CO
FIGURE 5-1. DIMENSIONS AND CAPACITY OF THE PARSHALL MEASURING
FLUMES FOR VARIOUS THROAT WIDTHS
-------
(SI
Ft.
0
0
1
1
2
4
w A |A B c
In. Ft. In. Ft. In. Ft. In. Ft. In.
i 1 fc| 1 ^ 1 607
62 16 l
-------
NPDES Compliance Monitoring Inspector Training: SAMPLING
the manufacturer's data are consulted, and it is difficult to measure manually the height of water above the step
at an upstream point. The dimensions of each Palmer-Bowles Flume are different. Therefore, the
manufacturer's data must be consulted to establish a relationship between the head and the discharge rate.
5.2.2 Secondary Devices
Secondary devices are used in conjunction with primary devices to determine the actual flow passing the
'measuring point. Typically, secondary devices measure the depth of water in the primary device and convert
the depth measurement to a corresponding flow, using established mathematical formulas. The output of the
secondary device is generally transmitted to a recorder and/or totalizer to provide instantaneous and historical
flow data to the operator. Outputs may also be transmitted to sampling systems to facilitate flow proportioning.
Secondary devices can be organized into two broad classes:
• A nonrecording type with direct readout (e.g., a staff gauge) or indirect readout from fixed points
(e.g., a chain, wire weight, or float)
• A recording type with either digital or graphic recorders (e.g., float in well, float in flow, bubbler,
electrical, or acoustic).
5.3 CLOSED CHANNEL FLOW
Closed channel flow is normally encountered between treatment units in a wastewater treatment plant and
after lift stations, where liquids and/or sludges are pumped under pressure. It is also encountered in submerged
outfalls. Flow in closed channels is usually measured by a metering device inserted into the conduit.
Examples of closed channel flow measuring devices are the Venturi Meter and the electromagnetic flow meter.
The Venturi Meter is one of the most accurate primary devices for measuring flow in closed channels. It
is basically a pipe segment consisting of an inlet with a converging section, a throat, and a diverging outlet
section, as illustrated in Figure 5-4. The water velocity is increased in the constricted portion of the inlet
section which results in a decrease in static pressure. The pressure difference between the inlet pipe and the
throat is proportional to the flow.
NOTES:
5-7
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NPDES Compliance Monitoring Inspector Training: SAMPLING
THROAT
INLET SECTION SECTION
PIPE OIA
OUTLET SECTION
HIGH
PRESSUR
TAP
LOW PRESSURE TAP
THROAT OIA.
FIGURE 5-4. CONFIGURATION AND NOMENCLATURE OF VENTURIC METER
NOTES:
5-8
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NPDES Compliance Monitoring Inspector Training: SAMPLING
Electromagnetic flow meter operation is based on the fact that the voltage induced by a conductor moving
at right angles through a magnetic field will be proportional to the velocity of that conductor as it moves
through the field. In the case of the electromagnetic flow meter, the conductor is the stream of water to be
measured, and the magnetic field is produced by a set of electromagnetic oils. A typical electromagnetic flow
meter is shown in Figure 5-5.
NOTES:
5-9
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NPDES Compliance Monitoring Inspector Training: SAMPLING
INSULATING
LINER
ELECTRODE
ASSEMBLY
STEEL METER
BODY
MAGNET COILS
POTTING COMPOUND
FIGURE 5-5. ELECTROMAGNETIC FLOW METER
NOTES:
5-10
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NPDES Compliance Monitoring Inspector Training: SAMPLING
6. QUALITY ASSURANCE/QUALITY CONTROL
Quality Assurance and quality control are tools necessary to maintain a specified level of quality in the
measurement, documentation, and interpretation of sampling data. Quality Control (QC) is a set of procedures
that provides precise and accurate analytical results. Quality Assurance (QA) ensures that these results are
adequate for their intended purposes. QA is intended to increase confidence in the validity of reported
analytical data. As an example of the distinction between quality control and quality assurance, procedures
established to calibrate a piece of field equipment are QC while checking the calibration of the equipment is
QA. QA checks will help the inspector determine when sample collection techniques are inadequate.
A QA program has two primary functions. First, it should continually monitor the reliability (accuracy
and precision) of results reported. This function is the determination of quality. Second, QA should control
quality to meet program requirements for reliability.
6.1 QUALITY CONTROL PROCEDURES FOR SAMPLING
Sampling QC begins with calibration and preventive maintenance procedures for sampling equipment.
The inspector should prepare a calibration plan and documentation record for all field sampling and analysis
equipment. Appendix K summarizes procedures to use for calibrating field equipment. A complete document
record should be kept in a QC logbook, including equipment specifications, calibration date, calibration
expiration date, and maintenance due date. Automatic samplers should be calibrated for sample quantity, line
purge, and timing factor.
The quality of data resulting from sampling activities is dependent on the following major activities:
• Collecting representative samples (see Chapter 2)
• Maintaining the integrity of samples through proper handling and preservation (see Chapter 2)
• Adhering to adequate chain-of-custody and sample identification procedures (see Chapter 2).
NOTES:
6-1
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NPDES Compliance Monitoring Inspector Training: SAMPLING
• Practicing QA techniques in the field (discussed below).
6.2 QUALITY ASSURANCE PROCEDURES FOR SAMPLING
A quality assurance program for sampling equipment and for field measurement procedures (of such
parameters as temperature, DO, pH, and conductivity) is necessary to ensure data of the highest quality. A
field quality assurance program should contain the following documented elements:
• Analytical methodology; special sample handling procedures; and precision, accuracy, and detection
limits of all analytical methods used.
• Basis for selection of analytical and sampling methodology. For example, all analytical methodology
should consist of approved procedures. Where methodology does not exist, the QA plan should state
how the new method will be documented, justified, and approved for use.
• Amount of analyses for QC, expressed as a percentage of overall analyses, to assess data validity.
Generally, the complete quality assurance program should approximate IS percent of the overall
program, with 10 and 5 percent assigned to laboratory QC and field QC, respectively. The plan
should include a shifting of these allocations or a decrease in the allocations depending on the degree
of confidence established for collected data.
• Procedures to calibrate and maintain field instruments and automatic samplers.
• Performance evaluation system which allows sampling personnel to cover the following areas:
- Qualifications of personnel for a particular sampling situations
- Determination of the best representative sampling site
- Sampling technique, including location of the sampling points within the wastestream; the choice
of grab or composite samples; the type of automatic sample; special handling procedure; sample
preservation; and sample identification
- Flow measurement, where applicable
- Completeness of data, data recording, processing, and reporting
- Calibration and maintenance of field instruments and equipment
• Use of QC samples such as duplicate, split, or spiked samples to assess the validity of data.
NOTES:
6-2
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NPDES Compliance Monitoring Inspector Training: SAMPLING
• Training of all personnel involved in any function affecting data quality.
The inspector should realize the importance of implementing QA in sample collection to minimize such
common errors as improper sampling methodology, poor sample preservation, and lack of adequate mixing
during compositing and testing.
6.3 LABORATORY QUALITY ASSURANCE/QUALITY CONTROL
Laboratory QA/QC procedures ensure high-quality analyses through instrument calibration and the
processing of control samples. Precision of laboratory findings refers to the reproducibility of results. In a
laboratory QC program, a sample is analyzed independently (more than once) using the same methods and set
of conditions. Precision is estimated by comparing the measurements. Accuracy refers to the degree of
difference between observed values and known or actual values. The accuracy of a method may be determined
by analyses of samples to which known amounts of reference standards have added.
Four specific QA procedures can be used to increase confidence in the validity of the reported analytical
data: duplicate, blank, split, and spiked samples. They are described below.
• Duplicate Samples - Separate samples taken at the same time and location using duplicate equipment
or one sample pulled and separated into two aliquots for duplicate analysis at the same laboratory.
Duplicate samples check for precision. These samples provide a check on sampling equipment and
sampling techniques. They also indicate the representativeness of the sampling location.
• Blank Samples - Check the contamination of chemical preservatives. A specified quantity of
preservative (equal to that ordinarily added to a wastewater sample) is added to a sample of deionized
water. After laboratory analysis, the value for the blank is subtracted from the sample value to
obtain the actual value. In the case of automatic sampling, the deionized water must be run through
the sampler prior to sample collection and then the appropriate preservative is added.
• Split Samples - Allow the comparison of analytical techniques and procedures from separate
laboratories. Samples are divided into two, or preferably three, segments for analysis in separate
laboratories. Sampling personnel should exercise caution when splitting samples to avoid producing
NOTES:
6-3
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NPDES Compliance Monitoring Inspector Training: SAMPLING
large differences in TSS. All large discrepancies in results should be investigated and the cause
identified.
• Spiked Samples - Provide a proficiency check for the accuracy of analytical procedures. Known
amounts of a particular constituent should be added to an actual sample or blanks of deionized water
at concentrations where the accuracy of the test method is satisfactory. The amount added should be
coordinated with the laboratory.
It is a good practice if each group of samples (or testing batch) contains at least one blank, one standard
duplicate, and one spiked sample (as applicable). When a batch contains more than 10 samples, every tenth
sample should be followed by a duplicate and a spike (as applicable).
NOTES:
6-4
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NPDES Compliance Monitoring Inspector Training: SAMPLING
7. SUMMARY
This module discussed the procedures and protocol used during sampling of a permittee's effluent or
during observation of a permittee's self-monitoring procedures. The need for a sampling plan and for
coordination with the laboratory performing analyses were stressed in order to promote consistency between
inspectors gathering samples and to ensure that prerequisite laboratory requirements are met during all sampling
events. The module also emphasizes the importance of using proper sample collection techniques, including the
selection of an appropriate sample location and sample type, the preparation of sample containers, and the
preservation, labeling, and handling of samples after collection in order to establish the validity of each sample
should violations be identified that lead to enforcement actions.
The module further explained several instances in which special sampling requirements must be followed.
It discussed methods used for onsite analysis of samples for pollutants that cannot be preserved and mentioned
some of the concerns involved with such analyses. Finally, this module described various chain-of-custody and
quality assurance procedures that should be practiced during all sampling events to ensure the accuracy,
integrity, and reliability of each sample and of the corresponding analytical results. Inspectors must conduct all
sampling activities on the premise that each may lead to an enforcement action.
7-1
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NPDES Compliance Monitoring Inspector Training: SAMPLING
APPENDIX A
GLOSSARY
-------
NPDES Compliance Monitoring Inspector Training: SAMPLING
GLOSSARY
Aliquot - Portion of a sample.
Biochemical Oxygen Demand (BOD) - Amount of oxygen used in the biochemical oxidation of organic matter
in a specified time, at a specified temperature, and under specific conditions. Standard test for measuring
the organic strength of a wastestream.
Blank sample • Samples of deionized water with a known quantity of preservative added.
Chain-of-custody - Written record of the possession and handling of the sample, from collection through
laboratory analysis, disposition of the analytical results, and disposal of the unused sample remnants.
Composite sample - Sample composed of two or more discrete samples. The aggregate sample will reflect the
average water quality over the compositing or sample period.
Confined space - Space having limited means of entry or exit and subject to the accumulation of toxic or
combustible gases or to a deficiency of oxygen.
Duplicate sample - Separate samples taken from the same source at the same time for analysis using identical
analytical techniques by the same person.
Grab sample - Sample collected over a time period not exceeding IS minutes. A single sample that represents
the characteristics of the wastestream only at the specific time and location of collection.
Instantaneous measurement - In-situ or grab measurement for such parameters as DO, pH, temperature, and
specific conductance.
Priority pollutants - A list of 126 pollutants, established by EPA, considered hazardous to the environment and
to humans.
Quality Assurance (QA) - Refers to a management/administrative check on procedures and practices used
during sampling and analysis that ensure the accuracy, precision, reproducibility, and representativeness of
reported data.
Quality Control (QC) - Routine application of procedures to control the accuracy and precision of the sampling
and analytical measurement process (as a function of quality assurance). QC of sampling procedures should
include the use of duplicate, spiked, and/or split samples and sample blanks. QC of analytical procedures
should include proper calibration of instruments and the use of appropriate analytical procedures.
Spiked sample - Effluent or blank sample to which a known quantity of substance has been added.
Split sample - Sample that has been divided into two or more containers for analysis by different analysts or
laboratories.
Supernatant - A substance floating above or on the surface of another substance.
Turbidity • Condition in a wastestream caused by the presence of suspended matter resulting in the scattering
and absorption of lightrays.
A-l
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NPDES Compliance Monitoring Inspector Training: SAMPLING
APPENDIX B
REFERENCES
-------
NPDES Compliance Monitoring Inspector Training: SAMPLING
REFERENCES
American Public Health Association, American Water Works Association, and Water Pollution Control
Federation. Standard Methods for the Examination of Water and Wastewater Use the most current,
EPA-approved edition.
Federal Water Pollution Control Act. 33 USC 1251 et seq.. as amended by the Water Quality Act of 1987
P.L. 100-4, February 4, 1987.
"Guidelines Establishing Test Procedures for the Analysis of Pollutants." 40 CFR Part 136. Use the most
current version.
U.S. Environmental Protection Agency. 1979. Methods for Chemical Analysis of Water and Wastes.
Environmental Monitoring and Support Laboratory, Cincinnati, Ohio. EPA-600/4-79-020.
U.S. Environmental Protection Agency. 1981. NPDES Compliance Flow Measurement Manual. Office of
Water Enforcement and Permits, Washington, DC. MCD-77.
U.S. Environmental Protection Agency. 1982. Handbook for Sampling and Sample Preservation of Water and
Wastewater. Environmental Monitoring and Support Laboratory, Cincinnati, Ohio. EPA-600/4-82/029.
U.S. Environmental Protection Agency. 1986. Pretreatment Compliance Monitoring and Enforcement
Guidance. Office of Water Enforcement and Permits, Washington, DC.
U.S. Environmental Protection Agency. 1979. NPDES Compliance Sampling Inspection Manual. MCD-51.
Office of Water Enforcement and Permits, Washington, DC.
U.S. Environmental Protection Agency. 1973. Handbook for Monitoring Industrial Wastewater. Office of
Technology Transfer, Washington, DC.
B-l
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NPDES Compliance Monitoring Inspector Training: SAMPLING
APPENDIX C
REVIEW QUESTIONS AND ANSWERS
ON NPDES
SAMPLING PROCEDURES
-------
NFDES Compliance Monitoring Inspector Training: OVERVIEW
REVIEW QUESTIONS ON NPDES SAMPLING PROCEDURES
1. List at least three objectives of a sampling program.
2. Describe the appropriate conditions for taking a grab sample.
3. Describe the appropriate conditions for taking a composite sample.
4. Grab samples should be taken for which parameters?
5. List the advantages and disadvantages of using an automatic sampler.
6. Describe a "representative" sample location.
7. Where should the sample container be held when taking a bacteriological sample and why?
8. Oil and grease samples should be taken in what type of container?
9. List three sample preservation techniques.
10. List three factors to consider when selecting automatic sampling equipment.
11. What type of sample container is used for volatile organics and how is the container filled?
12. What is the purpose of chain-of-custody procedures?
13. List specific QA procedures for sampling activities.
14. What is the purpose of QA?
C-l
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NPDES Compliance Monitoring Inspector Training: OVERVIEW
ANSWERS TO REVIEW QUESTIONS ON
NPDES SAMPLING PROCEDURES
1. List at least three objective of a sampling program.
• To verify compliance with effluent limitations
• To verify self-monitoring data
• To verify that parameters specified in the permit are consistent with wastewater characteristics
• To support permit reissuance and revision
• To provide basis for enforcement procedures.
[Section 1.3]
2. Describe the appropriate conditions for taking a grab sample.
• Batch dischargers
• Constant waste conditions over a period of discharge
• Extreme conditions exist
• Wastestream is adequately mixed.
[Section 2.7]
3. Describe the appropriate conditions for taking a composite sample.
• To determine average pollutant concentration.
[Section 2.7]
4. Grab samples should be taken from which parameters?
PH
Temperature
Oil and grease
Residual chlorine
Soluble sul fides
DO
Cyanide
Volatile organics.
[Section 2.7]
5. List the advantages and disadvantages of using an automatic sampler.
• Advantages
- More practical for sampling a large number of locations
- Reduces human error in complex sampling activities
- Reduces exposure to potentially hazardous environments
- Requires less labor.
C-2
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NPDES Compliance Monitoring Inspector Training: OVERVIEW
• Disadvantages
- Cost of equipment
- Maintenance requirements.
[Section 2.7]
6. Describe a "representative" sample location.
• Wastestream must be adequately mixed and sample should be taken in the center of the flow, a few
inches below the surface.
[Section 2.5]
7. Where should the sample container be held when taking a bacteriological sample and why?
• At the lower part of the bottle with the mouth of the bottle facing the direction of the current.
• To avoid contamination.
[Section 2.14]
8. Oil and grease samples should be taken in what type of container?
• Glass container with a teflon insert in the lid.
[Section 2.14]
9. List three sample preservation techniques.
• Refrigeration (metals - pH <2)
• pH adjustment (cyanide - pH > 12)
• Chemical neutralization (tecal colifonn - 0.008% NajS20,)
[Section 2.10]
10. List three factors to consider when selecting automatic sampling equipment.
• Convenience in installation and maintenance
• Equipment security
• Cold weather operation.
[Chapter 4]
11. What type of sample container is used for volatile organics and how is the container filled?
• 40 ml glass bottle with a teflon coated septum seal. The bottle must be filled to the top without any air
bubbles.
[Section 2.14]
12. What is the purpose of chain-of-custody procedures?
• To provide an accurate written record that tracks the possession of a sample from origin through
analysis.
[Chapter 7]
C-3
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NFDES Compliance Monitoring Inspector Training: OVERVIEW
13. List specific QA procedures for sampling activities.
• Split samples
• Blank samples
• Duplicate samples
• Calibration plan for sampling equipment.
[Section 6.2]
14. What is the purpose of a QA program?
• To ensure the integrity of a sample.
[Chapter 6]
C-4
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NPDES Compliance Monitoring Inspector Training: SAMPLING
APPENDIX D
VOLUME OF SAMPLE REQUIRED FOR DETERMINATION
OF THE VARIOUS CONSTITUENTS OF
INDUSTRIAL WASTEWATER
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NPDES Compliance Monitoring Inspector Training: SAMPLING
Volume of Sample Required for Determination of
the Various Constituents of Industrial Wastewater
(U.S. Environmental Protection Agency 1973.
Handbook for Monitoring Industrial Wastewater.
Technology Transfer.)
Tests Volume of Sample 1, in ml
PHYSICAL
Color and odor (2) 100 to 500
Corrosivity (2) following sample
Electrical conductivity (2) 100
pH, electrometric (2) 100
Radioactivity 100 to 1,000
Specific gravity (2) 100
Temperature (2) following sample
Toxicity (2) 1,000 to 20,000
Turbidity (2) 100 to 1,000
CHEMICAL
Dissolved Gases
Ammonia (3) 500
Carbon dioxide (3), free CO: 200
Chlorine (3), free C12 200
Hydrogen (3), H2 1,000
Hydrogen sulfide (3), H,S 500
Oxygen (3), 0, 500 to 1,000
Sulfer dioxide (3), free S2 100
Miscellaneous
Acidity and alkalinity 100
Bacteria, iron 500
Bacteria, sulfate-reducing 100
Biochemical Oxygen Demand (BOD) 100 to 500
Carbon dioxide, total CO, (including
CO,-, HCO*-, and free) 200
Chemical Oxygen Demand (COD) (dichromate) 50 to 100
Chlorine requirement 2,000 to 4,000
Chlorine, total residual Cl} (including
OCl, HOC5", NHjCl, NHClj, and free) 200
D-l
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NFDES Compliance Monitoring Inspector Training: SAMPLING
Volume of Sample Required for Determination of
the Various Constituents of Industrial Wastewater
(U.S. Environmental Protection Agency 1973.
Handbook for Monitoring Industrial Wastewater.
Technology Transfer.)
Tests Volume of Sample1, in ml
Miscellaneous
Chloroform, extractable matter 1,000
Detergents 100 to 200
Hardness 50 to 100
Hydrazine 50 to 100
Microorganisms 100 to 200
Volatile and filming amines 500 to 1,000
Oily matter 3,000 to 5,000
Organic nitrogen 500 to 1,000
Phenolic compounds 800 to 4,000
pH, colorimetric 10 to 20
Polyphosphates 100 to 200
Silica 50 to 1,000
Solids, dissolved 100 to 20,000
Solids, suspended 50 to 1,000
Tannin and lignin . 100 to 200
Cations:
Aluminum, A1*J 100 to 1,000
Ammonium (2), NH/ 500
Antimony, Sb*J to Sbfl 100 to 1,000
Arsenic, As+3 to As*5 100 to 1,000
Barium, Ba+2 100 to 1,000
Cadmium, Cd+2 100 to 1,000
Calcium, Cd+: 100 to 1,000
Chromium, Cr*3 to Cr*6 100 to 1,000
Copper, Cu*2 200 to 4,000
Iron (3), Fe+2 and F+s 100 to 1,000
Lead, Pb+J 100 to 4,000
Magnesium, Mg*J 100 to 4,000
Manganese, Mn*2 to Mn*T 100 to 1,000
Mercury, Ng* and Hg*J 100 to 1,000
Potassium, K* 100 to 1,000
Nickel, Ni*2 100 to 1,000
D-2
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NFDES Compliance Monitoring Inspector Training: SAMPLING
Volume of Sample Required for Determination of
the Various Constituents of Industrial Wastewater
(U.S. Environmental Protection Agency 1973.
Handbook for Monitoring Industrial Wastewater.
Technology Transfer.)
Tests Volume of Sample1, in ml
Cations:
Silver, Ag* 100 to 1,000
Sodium, Na+ 100 to 1,000
Strontium, Sr+J 100 to 1,000
Tin, Sn*2 and Sn+4 100 to 1,000
Zinc, Zn*2 100 to 1,000
Anions:
Bicarbonate, HCO, 100 to 200
Bromide, Br 100
Carbonate, CO,' 100 to 200
Chloride, Cl 25 to 100
Cyanide, CN 25 to 100
Fluoride, Fl 200
Hydroxide, OH 50 to 100
Iodide, I 100
Nitrate, NO,2 10 to 100
Nitrite, N02 50 to 100
Phosphate, ortho, PO*..1, HPO,..2, HjPO^ 50 to 100
Sulfate, S042, HS04 100 to 1,000
Sulfide, S2, HS 100 to 500
Sulfite, SO,2, HSO, 50 to 100
(1) Volumes specified in this table should be considered as guides for the approximate quantity of sample
necessary for a particular analysis. The exact quantity used should be consistent with the volume
prescribed in the standard method of analysis, whenever a volume is specified.
(2) Aliquot may be used for other determinations.
(3) Samples for unstable constituents must be obtained in separate containers, preserved as prescribed,
completely filled, and sealed against all exposure.
D-3
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NFDES Compliance Monitoring Inspector Training: SAMPLING
APPENDIX E
REQUIRED CONTAINERS, PRESERVATION
TECHNIQUES, HOLDING TIMES, AND
TEST METHODS
(EXCERPTED FROM 40 CFR PART 136)
-------
REQUIRED CONTAINERS, HtESERVATICN TECHCQUES, AN) HOLDING TIMES
Source: 49 FR 43260 Friday October 26, 1984 40 CFR Part 136
Parameter
BACTERIAL TESTS
Coliform, fecal and total
Fecal streptococci
INORGANIC TESTS
Acidity
Alkalinity
Amnonia
Biochemical oxygen demand
Biochemical oxygen
demand carbonaceous
Bromide
Chemical oxygen demand
Chloride
Chlorine, total residual
Container'11
P,G
P,G
P,G
P,G
P,G
P,G
P,G
P,G
P,G
P,G
P,G
Preservative'2'1'3'
Cool, 4°C
0.006% Ra2S203(5)
Cool, 4°C
0.008% Na2S203(5)
Cool, 4°C
Cool, 4°C
Cool, 4°C
H2S04 to pH<2
Cool, 4°C
Cool, 4°C
None required
Cool, 4°C
HjSO,, to pH<2
None required
None required
Maximum
Holding Time'4 '
6 hours
6 hours
14 days
14 days
28 days
48 hours
48 hours
28 days
28 days
28 days
Analyze imnediately
%
n
1
i.
&
f
H
1*
CO
i
2
o
-------
m
to
REQUIRED CONTAINERS, RESERVATION TECHNIQUES,
Source: 49 FR 43260 Friday October 26
Parameter
Color
Cyanide, total and amenable
to chlorination
Fluoride
Hardness
Hydrogen ion (pH)
Kjeldahl and organic nitrogen
METALS*71
Chromium VI
Mercury
Metals except above
Nitrate*
Nitrate-nitrite
Nitrite
Container* x '
P,G
P,G
P
P,G
P,G
P,G
P,G
P,G
P,G
P,G
P,G
P,G
AM) HOLDING TIMES
, 1984 40 CFR Part
Preservative'21'
Cool, 4°C
(Continued)
136
Maximum
*3) Holding Time* 4)
48 hours
Cool4°C 14 days'6'
NaOH to pH>12
0.6 g ascorbic acid '
None Required
HN03 to pH<2
None required
Cool, 4°C
H2S04 to pH<2
Cool, 4°C
HN03 to pfl<2
BN03 to pH<2
Cool, 4°C
Cool, 4°C
H2S04 to pH<2
Cool, 4°C
28 days
6 months
Analyze imnediately
28 days
24 hours
28 days
6 months
48 hours
28 days
48 hours
1
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n
•o
ance Monitoring Insp
!
H
3
1'
i
2
o
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REQUIRED CONTAINERS
Source: 49
Parameter
Oil and grease
Organic Carbon
Orthophosphate
Dissolved oxygen (probe)
Phenols
Phosphorus (elemental)
Phosphorus, total
Residue, total
Residue, filterable
Residue, nonfilterable (TSS)
Residue, settleable
Residue, volatile
, PRESERVATION TECaffQUES,
FR 43260 Friday October 26
Container* n
G
P,G
P,G
G bottle & top
G
G
P,G
P,G
P,G
P,G
P,G
P,G
AND HOIIHNG TIMES (Continued)
, 1984 40 CFR Part 136
Preservative'2 >r(3)
Cool, 4°C
H2S04 to pH<2
Cool, 4°C
H2S04 to pH<2
Filter imnediately
Cool, 4°C
None required
Cool, 4°C
H2S04 to pH<2
Cool, 4°C
Cool, 4°C
H2S04 to pH<2
Cool 4°C
Cool4°C
Cool4°C
Cool 4°C
Cool4°C
Maxijiun
Holding Tine'41
28 days
28 days
48 hours
Analyze immediately
28 days
48 hours
28 days
7 days
7 days
7 days
48 hours
7 days
1
So
|
TSL
f"
%
2
e
2.
B
a.
.5
ofe
6*
1
H
§;
V)
1
2
0
-------
tn
.U
REQUIRED CONTAINERS
Source: 49
Parameter
Silica
Specific conductance
Sulfate
Sulfide
Sulfite
Surfactants
Temperature
Turbidity
ORGANIC TESTS1 8 '
Purgeables Halocarbons
Purgeable Aromatics Hydrocarbons
, PRESERVAHON TECHNIQUES,
FR 43260 Friday October 26
Container111
P
P,G
P,G
P,G
P,G
P,G
P,G
P,G
G, teflon-lined
septum
G, teflon-lined
septum
AMJHOLDEC TIMES
, 1984 40 CFR Part
Preservative1
Cool 4°C
Cool 4°C
Cool 4°C
Cool 4°C add
Zinc Acetate and
sodium hydroxide
to pH>9
None required
Cool 4°C
(Continued)
136
Maximum
01 Holding Time1 '
28 days
28 days
28 days
7 days
Analyze inroediately
48 hours
None required Analyze imi^xliately
Cool, 4°C 48 hours
Cool 4°C 14 days
0.008% Na2S203(51
Cool 4°C
0.008% Na2S203(5
HC1 to pH 2(9!
14 days
|
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1
2
utoring Inspector Training
• •
V)
2
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KEQUIBED CONTAINERS
Source: 49
Parameter
Acrolein and Acryloni trite
Extractables (phenols)
Benzidenes
Phthalate esters'111
Nitrosamines'11''14'
PCBs111' Acrylonitrate
Nitroararatics and isophorone
Polynuclear aromatic hydrocarbons'111
, PRESERVATION TBOMQUES,
FR 43260 Friday October 26
Container' * '
G, teflon-lined
septum
G, teflon-lined
cap
G, teflon-lined
cap
G, teflon-lined
cap
G, teflon-lined
cap
G, teflon-lined
cap
G, teflon-lined
cap
G, teflon-lined
cap
AND HOLDING TIMES (Continued)
, 1934 40 CFR Part 136
Preservative' 2 ' ' ' 3 '
Cool 4°C
0.008* Na,SJ)'5'
Adjust pH to i5(10)
Cool, 4°C
H2SCv to pH<2
0.008* Na2S203
Cool, 4°C
0.008* Na2S203(5)
Cool, 4°C
Cool, 4°C
store in dark
0.008* Na2S203
Cool, 4°C
Cool, 4°C
0.008* Na2S20
store in the dark
Cool, 4°C
0.008* Na2S20 '
r»#-rv»-v^ •! r\ tns\ /irs»-v
Maximum
Holding Time'41
14 days
7 days (until extraction)
30 days (after extraction)
7 days until
extraction
7 days until
extraction. 40 days after
extraction
7 days until
extraction, 40 days after
extraction(12)
7 days until
extraction. 40 days after
extraction
7 days until
extraction. 40 days after
extraction
7 days until
extraction. 40 days after
avtr-^ftlnn
Z
1
s
0
•o
5'
0
2
IS
S
M
S1
1
O
H
I
3.
(A
1
0
-------
m
REQUIRED CONTAINERS, PRESERVATION TECHNIQUES,
Source: 49 ER 43260 Friday October 26
Parameter
Haloethers'11'
Chlorinated hydrocarbons' '
TOD
PESTICIDES TEST
Pesticides'11'
RADIOLOGICAL TEST
Alpha, beta, and radium
11 'Polyethylene (P) or Glass (G).
Container'1'
G, teflon-lined
rap
G, teflon-lined
cap
G, teflon-lined
r^p
G, teflon-lined
cap
P,G
AM) HOLDING TIMES (Continued)
, 1984 40 CFR Part 136
Preservative'2' f(3)
Cool, 4°C
0.008% Na2S203( '
Cool, 4°C
Cool, 4°C
0.008% Na2S203(5)
Cool, 4°^
H»3 to pH<2
Maxinun
Holding Time'4 '
7 days until
extraction. 40 days after
extraction
7 days until
extraction. 40 days after
extraction 12)
7 days until
extraction. 40 days after
extraction
7 days until
extraction. 40 days after
extraction 12)
6 months
<2 'Sample preservation should be performed imnediately upon sample collection. For composite samples each aliquot
should be preserved at the time of collection. When use of an automatic sampler makes it impossible to preserve each
alinuot. then samples may be preserved by maintaining at 4°C until compositing and sample splitting is completed.
5 Compliance Monitoring Insp
1
H
I
I
>
I
-------
CCNIMNERS, BESEKJKUGN TEONECBES, M> HDUJUG TIMES (Continued)
Source: 49 FR 43260 Friday October 26, 1984 40 CFR Part 136
13'when any sample is to be shipped by conmon carrier or sent through the Uhited States nails, it must comply with the
Department of Transportation Hazardous Materials Regulations (49 CFR Part 172). The person offering such material
for transportation is responsible for ensuring such compliance. For preservation requirements, the Office of
Hazardous Materials, Materials Transportation Bureau, Department of Transportation has determined that the Hazardous
Materials Regulations do not comply to the following materials: Hydrochloric acid (HC1) in water solutions at
concentrations of 0.04% by weight or less (pH about 1.96 or greater); Nitric acid (HN03) in water solutions at
concentrations of 0.15% by weight or less (pH about 1.62 or greater); Sulfuric acid (H2S04) in water solutions at
concentrations of 0.35% by weight or less (pH about 1.15 or greater); and Sodium hydroxide (NaOH) in water solutions
at concentrations of 0.80% by weight or less (pH about 12.30 or less).
u 'Samples should be analyzed as soon as possible after collection. The times listed are the maximum times that samples
may be held before analysis and still considered valid. Samples may be held for longer periods only if the
permittee, or monitoring laboratory, has data on file to show that the specific types of samples under study are
stable for the longer time. Some samples may not be stable for the maximum time period given in the table. A
permittee, or monitoring laboratory, is obligated to hold the sample for a shorter time if knowledge exists to show
this is necessary to maintain sample stability. tt
15'should only,be used in the presence of residual chlorine. Add ascorbic acid, a few crystals at a time, until no
chlorine remains. Then add 0.6 more grams of ascorbic acid for each liter of sample.
(6'Maximum holding time is 24 hours when sulfide is present.
17'Samples should be filtered immediately onsite before adding preservative for dissolved metals. |
(B'Guidance applies to samples to be analyzed by GC, LC, or GC/MS for specific organic compounds. J-
19'Sample receiving no pH adjustment must be analyzed within 7 days of sampling.
(I°'Samples for acrolein receiving no pH adjustment must be analyzed within 3 days of sampling. Optionally, all samples
ray be tested with lead acetate paper before pH adjustments in order to determine if sulfide is present. If sulfide ^
is present, it can be removed by the addition of cadmium nitrate powder until a negative spot test is obtained. The g1
sample is filtered, then NaOH is added to pH 12. 5.
c«
(U)Unen the extractable analytes of concern fall within a single chemical category, the specified preservation and
maximum holding times should be observed for optimum safeguard of sample integrity. When the analytes of concern
fall within two or more chemical categories, the sample may be preserved by cooling to 4°C, reducing residual
chlorine with 0.006% sodiun thiosulfate, storing in the dark, and adjusting the pH to 6-9; samples preserved in this
manner may be held for 7 days before extraction and for 40 days after extraction. Exceptions to this optional 2
preservation and holding time procedure are noted in footnote (5) (re: the requirement for thiosulfate reduction of
residue chlorine) and footnotes (12) and (13) (re: the analysis of benzidine).
-------
REQUIRED ODNLMNERS, FRESHWATICN TEOMQUES, AM) HOLDING TIMES (Continued)
Source: 49 FR 43260 Friday October 26, 1984 40 CFR Part 136
Extracts may be stored up to 7 days before analysis if storage is conducted under an inert (oxidant-free) atmosphere.
'if 1,2-diphenylhydrazine is likely to be present, adjust the pH of the sample to 4.0 + 0.2 to prevent rearrangement
to benzidine.
114'For the analysis of diphenylnitrosatnine, add 0.008% Na2S203 and adjust pH to 7-10 with NaOH within 24 hours of
sampling.
115'ihe pH adjustment may be performed upon receipt at the laboratory and may be omitted if the samples are extracted
within 72 hours of collection. For the analysis of aldrin, add O.OOSK fe2^V
' 8
n
3
3.
2
o
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NPDES Compliance Monitoring Inspector Training: SAMPLING
APPENDIX F
EPA ORDER 1440.2
HEALTH AND SAFETY REQUIREMENTS
FOR EMPLOYEES ENGAGED IN
FIELD ACTIVITIES
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NFDES Compliance Monitoring Inspector Training: SAMPLING
ENVIRONMENTAL
PROTECTION ORDER
AGENCY
1440.2
July 12, 1991
SERVICES - SAFETY
HSftLTH AND SargTf REQUISSyENTS FOR S-gLOYSES ENGAGED
El FIELD ACTIVITIES
1. PURPOSE. This Order establishes policy, responsibilities, and
Tiindatcry requirements for occupational health and safety training
and certification, and cer^paticnal medical monitoring of Agency
enplcyees engaged In field activities.
a. The term "field activities" as used in this Order means EPA
program activities that are conducted by EPA employees outside of
EPA administered facilities. These activities include environmental
and pesticides sampling, inspection of water and wastawater treatment
plants, and hazardous material spills and vasts sits investigations,
inspections, and sampling.
b. The term "health and safety training" means scheduled, formal
or informal training courses, approved and sponsored by EPA and
conducted by EPA or its contracted agents which is designed to develop,
inprove and upgrade the health and safety knowledge of EPA wiployees
involved in field activities.
c. The term "occupational medical monitoring" means surveillance
over the health status of employee* by means of periodic medical exam-
inations or screening in accordance with the Agency's Occupational
Medical Monitoring guidelines.
d. The term "certification" as used in this Order means that the
employee has successfully completed the minimum classroom and field
training requirements for the specified level of training and the Agency
has issued a certificate attesting that the employee met these require-
ments.
F-l
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NPDES Compliance Monitoring Inspector Training: SAMPLING
ORDER
1440.2
July 12, 1981
3. REFERENCES.
a. 29 CFR 1910, Parts 16, 94, 96, 106, 109, 111, 134, 151, 1000,
Occupational Health and Safety Standards.
b. Executive Order 12196, Section 1-201, Sec. (k), Occupational
Kaalth and Safety Programs for Federal Employees.
c. 29 CFR 1960.59(a), Occupational Safety and Health for the
Federal Employee.
d. EPA Occupational Health and Safety Manual, Chapter 7(1).
e. EPA Training and Development Manual, Chapter 3, Par 7(b).
f, Occupational Health and Safety Act of 1971, P.L. 91-596,
Sec. 6.
g. EPA Order en Respiratory Protection (Proposed).
h. 49 CFR, Parts 100-177, Transportation of Hazardous Materials.
i. EPA C.-der 1000.18, Transportation of Hazardous Materials.
j. EPA Order 3100.1, Change 1, Uniforms, Protective Clothing, and
Protective Equipment.
4. BACKGROUND. Field activities are a critical part of most EPA
programs. These activities range fron routine envirormental recon-
naisance sampling, inspections, and monitoring, to entering and working
in envirorments with known and unknown hazards. Since protection
cannot be engineered into the field working situation, the protection
of personnel engaged in field activities involves training employees
in safe operational procedures and the proper use of appropriate personal
protective clothing and equipment.
5. APPLICABILITY. Thia Order applies to all EPA organizational units
which have employees engaged in field activities.
6. POLICY. It is the policy of the Environnental Protection Agency
to carry out its field activities in a manner that assures the pro-
tection of its enpLoyeefl.
—— _
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NPDES Compliance Monitoring Inspector Training: SAMPLING
ORDER
1440.2
July 12, 1981
7. RESPONSIBILITIES.
a. Assistant Administrators, Regional Administrators, Deputy
Assistant Administrators, Laboratory Directors, and Division
Directors. These officials are responsible within their jur-
isdictions for implementing the provisions of this Order and for
budgeting the necessary funds for employee training and certification,
personal protective clothing and equipment, and occupational medical
monitoring programs.
b. Supervisors. Supervisors are responsible for complying with
the requirements of this Order for employee training and certification,
and occupational medical monitoring programs. They will identify
those employees who require training and certification, and occupational
medical monitoring, and assure they receive it to ccmply with the provisions
of this Order and will insure these requirements are properly contained
in position descriptions and job postings.
c. Pnnloyeea. EhipLoyees are responsible for making known upon
request frcm their supervisors the extent of their individual occupation-
al health and safety training and the history of their occupational
medical monitoring participation. Bnployees should notify their
supervisor of any hazardous work situation and make suggestions for
corrective measures. Employees are responsible for applying the knowledge,
skills, and techniques acquired through training in a manner that will
help assure their health and safety and that of fellow workers.
d. Occupational Health and Safety Designeea. The Occupational
Health and Safety Designers are responsible for identifying program
areas that require training and certification, and occupational medical
monitoring; recommending or providing training and certification re-
sources to meet the requirorients of this Order; and maintaining records
of persons receiving training and certification.
e. Office of Occupational Health and Safety. The Director, Office
of Occupational Health and Safety is responsible for establishing policy
and requirements for adequate training-and certification programs for
field activities, developing and maintaining an occupational medical
monitoring program, approving health and safety training and certifi-
cation programs for employees involved in field activities, and for
evaluating the results of these training and certification programs.
F-3
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NPDES Compliance Monitoring Inspector Training: SAMPLING
ORDER
1440.2
July 12, 1981
8. OBJECTIVES.
a. Training and Certification. The objectives of the health and
safety training and certification programs for employees involved in
field activities are:
(1) To assure that EPA employees are aware of the potential
hazards they may encounter during the performance of field activities;
(2) To provide the knowledge and skills necessary to perform
the work with the least possible risk to personal health and safety;
(3) To assure that Agency program goals are acconplished
in as safe and healthful manner as feasible; and
(4) To assure that EPA employees can safely disengage them-
selves fron an actual hazardous situation which :nay occur during a
field activity.
b. Cccupational Medical Moni taring. The objectives of the oc-
cupation; j. Medical Monitoring program are:
(; > To detect any adverse effects of occupational exposure
on the e -iloyees health and to initiate prompt corrective actions
when ind;.w?.ted; and
(2) To assure that employees assigned arduous or physically
taxi.-,, jobs or jobs requiring unique skills are able to perform those
jobs vlthout impairing their health and safety or the health and safety
of ct'iers.
9. T3AJ2JIN3 AND CERTIFICATION RSQUIMMEinS . Bnployees shall not be
permi-ted to engage in routine field activities until they have been
trained aiJ certified to a level cormensurate with the degree of an-
^. hazards.
a. iasic Level . All employees shall be provided a minimxn of
24 hours of health and safety training prior to their becoming in-
waived i-.» normal, routine field activities. The training shall
inclur .-.: but not be limited to classroom instruction in all the
folio/ ing sJsject areas:
F-4
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NPDES Compliance Monitoring Inspector Training: SAMPLING
ORDER
1440.2
July 12, 1981
(1) Employee Rights and Responsibilities;
(2) Nature of Anticipated Hazards;
(3) Qnergency Help and Self-Rescue;
(4) Vehicles - Mandatory Rules and Relations;
(5) Safe Use of Field Equipment;
(6) Use, Handling, Storage, and Transportation of Hazardous
Materials;
(7) Personal Protective Equipment and Clothing, Use and Care;
and
(8) Safe Sampling Techniques.
In addition to classroom instruction, the employee shall accompany
an errployee experienced in field activities and perform actual field
tasks for a mini-nun of three days within a period of three months after
classroom instruction. Employees satisfactorily completing these re-
quirements will receive certification at the Basic Level of training
fron the Occupational Health and Safety Designee at the Reporting Unit.
b. Intermediate Level. All inexperienced employees who are to
work with experienced employees in uncontrolled hazardous waste and
hazardous spill sites investigations or employees engaged in other
activities which at a later date are determined by the Director, Office
of Occupational Health and Safety, to present unique hazards requiring
aiditional training, shall be provided a minimum of 8 hours of additional
health and safety training. This training shall include (in addition
to the Basic Level requirements) but not be limited to the following
subject matter:
(1) Site surveillance, observation, and safety plan development;
(2) Use and decontamination of totally enclosed-protective
clothing and equipment;
(3) Use of field test equipment for radioactivity, explosivity,
and other measurements; and
(4) Topics specific to other identified activities.
In addition to classroom instruction, the employee shall accompany
another employee experienced in hazardous waste and spill site inves-
tigations and/or .cleanup operations and perform actual field tasks
for a minimum of three days within a period of three months after
classroom instruction. The employee should also be able to provide
cn-the-job trai~.ing and instructions to inexperienced employees during
normal, routine field activities (as required above). Employees
satisfactorily completing these requirements will be certified at the
Intermediate Level by the Occupational Health and Safety Designee
at the Reporting Unit.
. _
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NPDES Compliance Monitoring Inspector Training: SAMPLING
ORDER
1440.2
July 12, 1981
c. Advanced Level. All employees who manage uncontrolled hazardous
waste site and spill site monitoring, sampling, investigations, and
cleanup operations shall be provided a minimum of 8 hours additional
health and safety training. The classroom training shall include but
not be limited to (in addition to the Basic and Intermediate Level
requirements), instruction in the following subject areas:
(1) Management of restricted and safe zones;
(2) Rules of Handling the Press and VIP's; and
. (3) Safe Use of Specialized Sampling Equipment.
In addition to classroom instruction, the employee shall accompany
another employee with experience in managing hazardous waste and
spill site investigations or cleanup operations and perform actual
field tasks for a minimum of three days within a three month period
after receiving classroom instruction. After satisfactorily com-
pleting these requirements, employees will receive Advanced Level
certification from the. Occupational Health and Safety Designee
at the Reporting Unit.'
d. General.
(1) An employee may receive certification at the next higher
level by comple*-ing only the additional training requirements if
certified at the next lower level within the previous one-year period.
(2) The Director/ Office of Occupationl Health and Safety*
may certify employees based on an evaluation of previous training,
education, and experience. Recarmendations for this type certifi-
cation should be made to the Director by the Occupational Health
and Safety Designee at the Reporting Unit.
10. FRBJJPCy OF TRAINING. Bnployees at the Basic, Intermediate, and
Advanced Levels shall complete a minimum of 8 hours of refresher
classrocm instruction annually consisting of a review of all subject
areas to maintain their' certification. In addition to the classrocm
instruction, employees shall hav« demonstrated by having performed actual
field tasks that they have sufficient practical experience to perform
their assigned duties in a safe and healthful manner.
11. RBOORD OF TRAINING.
a. A record of the level of training and certification shall
be maintained in the employee's official personnel file.
F-6
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NPDES Compliance Monitoring Inspector Training: SAMPLING
ORDER
•1440.2
July 12, 1981
b. The Occupational Health and Safety Designee shall maintain
a roster of employee training and certification so that a schedule
of annual training can be established.
c. The Occupational Health and Safety Designee shall issue a
certificate to the employee showing the level of training and certi-
fication.
12. OCCUPATIONAL MEDICAL MONITORING REQUIREMENTS. All employees
routinely engaged in field activities which present the probability
of exposure to hazardous or toxic svfcstances, which are arduous or
physically taxing, or which require the use of respiratory protective
equipment shall be included in the Agency's Occupational Medical
Monitoring Program. Employees should not be permitted to engage in
field activities unless they have undergone a baseline medical exam-
ination (as defined in the Agency's Occupational Medical Monitoring
Guidelines), which will show physical fitness and provide a base to
measure any adverse effects their activities may have on these in-
dividuals.
13. SAVPCS PROVISION. Changes in the Act, Executive Order, or EPA
and OST& standards and guidelines which occur after the effective date
of this Order will automatically cone under the purview of this Order
on the effective date of the change.
Full irqal mentation of this Order shall be within one year of its
effective date.
EdwardXJ. Hanley
Director, Office of Management
Information and Support Services
F-7
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NPDES Compliance Monitoring Inspector Training: SAMPLING
APPENDIX G
LIST OF FIELD SAMPLING EQUIPMENT
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NPDES Compliance Monitoring Inspector Training: SAMPLING
LIST OF FIELD SAMPLING EQUIPMENT
Tools
- Multi-Tooled Jack Knife (Swiss Army Type)
- Electrical and Duct Tape
- Tape Measure
- Handheld Range Finder and Level
- Camera/Film
- Flashlight
- Screwdriver
- Adjustable and Vise Grips Wrench
- Pliers
- Plastic Bucket
- Nylon Cord
- Field Notebook with Waterproof Paper
Samplers
- Tubing
- Sample Bottles
- Batteries
- Desiccant
• Flow Measurement Devices
• Meters
- pH Buffer
- Chart Paper
• Sample Containers
• Coolers/Ice
• Preservatives
• Transportation Materials
- Bubblepack Material
- Filament Tape
- Shipping Labels
- Chain-of-Custody Forms
- Water Resistent Marker/Pen
- Analysis Request Forms
G-l
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NPDES Compliance Monitoring Inspector Training: SAMPLING
Protective Clothing
- Hard Hat
- Safety Shoes
- Gloves
- Coveralls
- Reflective Safety Vest
- Safety Glasses/Goggles
- Rain Wear
Safety Equipment
- First-Aid Kit
- Safety Harness and Retrieval System
- Ventilation Equipment
- Meters (Oxygen Content, Explosivity, and Toxic Gas)
- Respirator
- Self-contained Breathing Apparatus (If Appropriate)
G-2
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NPDES Compliance Monitoring Inspector Training: SAMPLING
APPENDIX H
SAMPLE IDENTIFICATION LABELS
-------
NPDES Compliance Monitoring Inspector Training: SAMPLING
EXAMPLE SAMPLE TAG
ENVIRONMENTAL PROTECTION AGENCY
OFFICE OF ENFORCEMENT
NATIONAL ENFORCEMENT INVESTIGATIONS CENTER
BUILDING 53, BOX 25227, DENVER FEDERAL CENTER
DENVER, COLORADO 80025
&EPA
r Project Code
Station Location
|
*
CO
1
o
*
Remarks:
Station No.
Bacteriology
Mutagenicity
Pesticides
Mo-/Day/Year
2.
at
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o
9
tO
Q)
8
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a.
?
c
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sr
Time
Designate: ^
Comp. Grab
Samplers: (Signature)
Organics GC
^
O
at
O
3
$
o
5
1
9
o?
w
9
1
Phenolics
o
8
8
3
I §
i
ij ^
1!
«
1©
9 ""
cn 5
n i
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H-l
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NPDES Compliance Monitoring Inspector Training: SAMPLING
APPENDIX I
EXAMPLE RECORD OF FIELD SAMPLE
DATA AND CHAIN-OF-CUSTODY RECORD
-------
U.S. ENVIRONMENTAL PROTECTION AGENCY
Environmental Services Division
CHAIN OF CUSTODY RECORD
REGION VIII. ONE DENVER PLACE
999 18TH.STREET
DENVER, CO. 80202 2413
PROJ. NO.
PROJECT NAME
SAMPLERS: (Signature)
STAT. NO
DATE
TIME
O
STATION LOCATION
NO.
OF
CON-
TAINERS
REMARKS
8
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&
I1
Relinquished by: (Signature)
Data/Time
Received by: (Signature)
Relinquished by: (Signature)
Date/Time
Received by: (Signature)
Relinquished by: (Signature)
Date/Time
Received by: (Signature)
Relinquished by: (Signature)
Date/Time
Received by: (Signature)
Relinquished by: (Signature)
Date/Time
Received for Laboratory by:
(Signature)
Date/Time
Remarks
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Olilrtftollon Original Aceompanlm SMpnwnt: Flnt Cony to Coordhutor FMd F»M: SKond Copy to ftoprmnutlm of IhipKlcd Faclllly
R8 EPA-014B (4-21-66)
8-15076
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NPDES Compliance Monitoring Inspector Training: SAMPLING
APPENDIX J
CRITERIA FOR SELECTION OF AUTOMATIC
SAMPLING EQUIPMENT
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NPDES Compliance Monitoring Inspector Training: SAMPLING
CRITERIA FOR SELECTION OF
AUTOMATIC SAMPLING EQUIPMENT
1. Capability for AC/DC operation with adequate dry battery energy storage for 120-hour operation at
1-hour sampling intervals.
2. Suitability for suspension in a standard manhole while accessible for inspection and sample removal.
3. Total weight, including batteries, under 18 kilograms (40 pounds).
4. Sample collection interval adjustable from 10 minutes to 4 hours.
5. Capability for flow-proportional and time-composite samples.
6. Capability for collecting a single 9.5 liter (2.5-gallon) sample and/or collecting 400-milliliter (0.11-gallon)
discrete samples in a minimum of 24 containers.
7. Capability for multiplexing repeated aliquots into discrete bottles.
8. One intake hose with a minimum inner diameter of 0.64 centimeters (0.25 inches).
9. Intake hose liquid velocity adjustable from 0.61 to 3 meters per second (2.0 to 10 feet per second) with
dial setting.
10. Minimum lift of 6.1 meters (20 feet).
11. Explosion-proof.
12. Watertight exterior case to protect components in the event of rain or submersion.
13. Exterior case capable of being locked, including lugs for attaching steel cable to prevent tampering and to
provide security.
14. No metal parts in contact with waste source or samples.
15. An integral sample container compartment capable of maintaining samples at 4°C to 6°C for a period of
24 hours at ambient temperatures ranging from -30°C to 50*C.
16. With the exception of the intake hose, capability of operating in a temperature range from -30°C to 50°C.
17. Purge cycle before and after each collection interval and sensing mechanism to purge in the event of
plugging during sample collection and then to collect the complete sample.
18. Field repairability.
19. Interchangeability between glass and plastic bottles, particularly in discrete samplers, is desirable.
20. Sampler exterior surface painted a light color to reflect sunlight.
J-l
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NPDES Compliance Monitoring Inspector Training: SAMPLING
APPENDIX K
QUALITY CONTROL PROCEDURES FOR
FIELD ANALYSIS AND EQUIPMENT
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NPDES Compliance Monitoring Inspector Training: SAMPLING
QUALITY CONTROL PROCEDURES
FOR FIELD ANALYSIS AND EQUIPMENT
Parameter
Dissolved Oxygen
• Membrane
Electrode
Enter the make,
model, and serial
and/or ID number for
each meter in a
logbook.
Report data to
nearest 0.1 mg/1.
Winkler-Azide method
Record data to
nearest 0.1 mg/1.
EH
• Electrode Method
Enter the make,
model, and serial
and/or ID number for
each meter in a
logbook.
Calibrate meter
using manufacturer's
instructions or
Winkler-Azide
method.
Check membrane for
air bubbles and
holes. Change
membrane and KC1 if
necessary.
Check leads, switch
contacts, etc. for
corrosion and shorts
if meter pointer
remains off-scale.
Duplicate analysis
should be run as a
precision check.
Duplicate values
should agree within
±0.2 mg/1.
Calibrate the system
against standard
buffer solutions of
known pH value; (e.g.
4, 7, and 9 at the
start of a sampling
run).
Periodically check
the buffers during
the sample run and
record the data in
the logbook.
Be on the alert for
erratic meter
response arising
from weak batteries,
cracked electrodes,
fouling, etc.
Quarterly
Check instrument
calibration and
linearity using a
series of at least
three dissolved
oxygen standards.
Take all meters to
the laboratory for
maintenance,
calibration, and
quality control
checks.
K-l
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NPDES Compliance Monitoring Inspector Training: SAMPLING
Parameter
pH (Continued)
• Electrode Method
(Continued)
General
Conductivity
Enter the make,
model, and serial
and/or ID number for
each meter in a
logbook.
Daily
Check response and
linearity following
highly acidic or
alkaline samples.
Allow additional
time for
equilibration.
Check against the
closest reference
solution each time a
violation is found.
Rinse electrodes
thoroughly between
samples and after
calibration.
Standardize with KC1
standards having
similar specific
conductance values
to those anticipated
in the samples.
Calculate the cell
constant using two
different standards.
Quarterly
Rinse cell after
each sample to
prevent carryover.
Take all meters to
lab for maintenance,
calibration, and
quality control
checks.
Check temperature
compensation.
Check date of last
platinizing and
replatinize, if
necessary.
Analyze NBS or EPA
reference standard
and record actual
vs. observed
readings in the
logbook.
K-2
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NPDES Compliance Monitoring Inspector Training: SAMPLING
Parameter
Residual Chlorine
Amperometric
Titration
Temperature
Manual
General
Enter the make,
model, and ID and/or
serial number of
each titration
apparatus in a
logbook. Report
results to nearest
0.01 mg/1.
Enter the make,
model, and serial
and/or ID number and
temperature range.
All standardization
shall be against a
traceable NBS or NBS
calibrated thermo-
meter. Reading
shall agree within
"±1°C. If enforce-
ment action is anti-
cipated, calibrate
the thermometer
before and after
analysis. All data
shall be read to the
nearest 1°C. Report
data between 10 and
99CC to two signifi-
cant figures.
Refer to instrument
manufacturer's
instructions for
proper operation and
calibration
procedures.
Check for air spaces
of bubbles in the
column, cracks, etc.
Compare with a known
source if available.
Quarterly
Biweekly: return
instrument to lab
for maintenance and
addition of fresh,
standardize
reagents.
Biweekly: check at
two temperatures
against a NBS or
equivalent
thermometer. Enter
data in logbook.
Temperature readings
shall agree within
±1°C or the
thermometer shall be
replaced or
recalibrated.
Initially and
biannually:
accuracy shall be
determined through-
out the expected
working range of 0°C
to 50°C. A minimum
of three tempera-
tures within the
range should be used
to verify accuracy.
Preferable ranges are:
5-10°C, 15-25°C, and
35-45 °C.
K-3
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NPDES Compliance Monitoring Inspector Training: SAMPLING
Parameter
• Thermistors,
Thermographs,
etc.
Flow Measurement
Automatic Samplers
General
Enter the make,
model, and serial
and/or ID number of
the instrument in a
logbook. All
standardization
shall be against a
NBS or NBS cali-
brated thermometer.
Reading should agree
within ±1°C. If
enforcement action
is anticipated refer
to the procedure
listed above.
Enter the make,
model, and serial
and/or ID number of
each flow measure-
ment instrument in a
logbook.
Enter the make,
model, and serial
and/or ID number of
each sampler in a
logbook.
Check thermistor and
sensing device for
response and opera-
tion according to
the manufacturer's
instruction.
Record actual vs.
standard temperature
in logbook.
Install the device
in accordance with
the manufacturer's
instructions and
with the procedures
given in owner's
manual.
Quarterly
Initially and
biannually:
accuracy shall be
determined through-
out the expected
working range of 0°C
to 50°C. A minimum
of three tempera-
tures within the
range should be used
to verify accuracy.
Preferable ranges
are: 5-10°C, 15-25°C,
and 35-45°C.
Annually: affix
record of calibra-
tion (NBS, manu-
facturer) to the
instrument log.
Check intake
velocity vs. head
(minimum of three
samples), and clock
time setting vs.
actual time interval.
K-4
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