United States Office of Water Enforcement and Permits
Environmental Protection Office of Water
Agency - Washington, DC 20460 August 1990
&EPA
NPDES Compliance
Monitoring Inspector
Training
Sampling
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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 aad 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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NPDES Compliance Monitoring Inspector Training: SAMPLING
TABLE OF CONTENTS
FOREWORD
1. INTRODUCTION
1 1 OVERVIEW OF THE NPDES PROGRAM . .
1.2 PURPOSE OF THE NPDES COMPLIANCE MONITORING
PROGRAM
1.3 OBJECTIVES OF NPDES SAMPLING
1.4 SAMPLING TASKS
SAMPLE COLLECTION
2.1
2.2
2.3
2.4
2.6
2.7
2.8
2.9
2.10
2.11
2.12
2.13
2.14
2.15
IMPORTANCE OF SAMPLE COLLECTION
SAMPLING PLAN
PREPARATION FOR SAMPLING
SAMPLING SAFETY
SAMPLING LOCATION
SELECTION AND PREPARATION OF SAMPLE CONTAINERS
SAMPLE TYPES
SAMPLE COLLECTION TECHNIQUES . .
SAMPLE VOLUME
SAMPLE PRESERVATION AND HOLDING TIMES ...
SAMPLE DOCUMENTATION
SAMPLE IDENTIFICATION AND LABELING ......
SAMPLE PACKAGING AND SHIPPING
CHAIN-OF-CUSTODY PROCEDURES
SPECIAL SAMPLING REQUIREMENTS
ANALYTICAL METHODS FOR ONSITE ANALYSIS
4. AUTOMATIC SAMPLERS
FLOW MEASUREMENT
.1 IMPORTANCE OF FLOW MEASUREMENT
.2 OPEN CHANNEL FLOW
.3 CLOSED CHANNEL FLOW
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NPDES Compliance Monitoring Inspector Training: SAMPLING
TABLE OF CONTENTS (Continued)
6. QUALITY CONTROL PROCEDURES FOR SAMPLING
6.1 QUALITY CONTROL PROCEDURES FOR SAMPLING
6.2 QUALITY ASSURANCE PROCEDURES FOR SAMPLING
6.3 LABORATORY QUALITY ASSURANCE/QUALITY CONTROL
7. SUMMARY
6-1
6-1
6-2
6-3
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NPDES Compliance Monitoring Inspector Training: SAMPLING
. .
LIST OF TABLES AND FIGURES
I . " " "
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Table ' ' j
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2-1 COMPOSITING METHODS
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
5-4 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 j
D .
APPENDIX G - LIST OF FIELD SAMPLING EQUIPMENT
APPENDIX H - SAMPLE IDENTIFICATION LABELS
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NPDES Compliance Monitoring Inspector Training: SAMPLING
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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NPDES Compliance Monitoring Insi»ector Training: SAMPLING
FOREWORD
This document is one of five training modules developed by the Office of Water Enforcement and
Permits (OWED, 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 i
. The Legal Issues Module discusses the legal issues which must be acidised 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 necessaiy 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 NTOES.^^,^ 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: '..-"- i
* * i
Enforcement Support Branch (EN-338)
Office of Water Enforcement and Permits
U.S. Environmental Protection Agency ; .
401 M Street, S.W.
Washington, DC 20460
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Compliance Monitoring
itoring b**r Training:SAMH
1. INTRODUCTION
1.1 OVERVIEW OF THE NPDES PROGRAM
Environmental Protection Agency (EPA) to:
Pretreatment Program
protect water quality.
mspectionsandmomtonngof
NOTES:
f the CWA regulates the discharge of poUutants from point
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the permit-issuing
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NEDES Compliance Monitoring Inspector Training: SAMPLING
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 pretrearment 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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NPDES Compliance Monitoring Inspector Training: SAMPLING
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 lus/her
understanding of its contents. Answers to these questions are also provided in Appendix C.
1.3 OBJECTIVES OF NPDES SAMPLING - v
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:
the parameters specified in the NPDES permit. Additionally, sample
5 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 locations) specified in the permit include all of the process and nonprocess
discharges and iHdequate to collect a representative sample of the effluent
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NFDES Compliance Monitoring Inspector Training: SAMPLING
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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NPDES Compliance Monitoring Inspector Training: SAMPLING
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 Samolle Preservation of Water and
Wastewater) 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, otyaimsd 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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NFDES Compliance Monitoring Inspector Training: SAMPLING
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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NFDES Compliance Monitoring Inspector Training: SAMPLING
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/QQ 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
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-ciiistody 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).
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. I
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.
QA/OC Procedures - To ensure that data collected is valid, systematic checks must show that test
results are accurate.
j
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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NPDES Compliance Monitoring Inspector Training: SAMPLING
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 shouldldso 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 Ins|>ector 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 niost 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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NFDES Compliance Monitoring Inspector Training: SAMPLING
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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OTDES Compliance Monitoring Inspector Training: SAMPLING
costing sanies for priority poUuan*. oil - ». - ^* -« »** -»" " " '
often ujd for Bfcd-M Oxygen Demand (BOD), Tota, Suspended Solids CTSiS), meUls, an
Containers with wide MOUth, are .-.amended MM. the «* - -M- from ^.er «o
Diners, u, addWon, ,he confer ^ be large enough «o c.H.ui. *e reouW vol^» for laboratory
_* Tne inspecu,, should us. M oonuine. for s^ple, M contain cons,iBJ»«s »h,ch .*«*.
torn 6Jposu» u, sunlight, such as iron cyauide (»hi«h is oxidized to hydrogen ^.ride).
Container lids and closure Unings must also be inuct so they do no, interfere with d. poUuUnt
p^eters to be Measured. Mos, confer, have tig.,, screw-type Uds. »*> confers are usuaUy
provided wi* screw caps nude of th. san« ^ria, as d. confer, so cap liners are usuaUy no, re,u,,ed.
Ota. confers usually COM. with rigid pteUc screw caps. Lin- Materials may b. polyethylene,
polypropylene, neoprene, or teflon.
' ^e 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 v^ith organic-free water
. Ri^gtacootria-wilh-ta^^
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) Ifc the buyer.
AU tubing and other sampling system parts must be scrubbed with bo,!r and detergent, rinsed several
times with tap water, and then rinsed with distilled or deionized water. Fu,her rinsing with acetone » adv1Sed
only when the type of tubing (e.g., teflon) is not susceptible to dissolution by the solvent.
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NEDES Compliance Monitoring Inspector Training: SAMPLING
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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Compliance Monitoring ^pector
to corroborate results of composite samples.
Calculating mass/rait time loadings.
.vailable. Composite samples may be collected
no,
«. re two methods used to collect this type of sample.
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NFDES Compliance Monitoring Inspector Training: SAMPLING
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 variation 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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NPDES Compliance Monitoring Inspector Training: SAMPLING
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
l>oth 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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NPDES Compliance Monitoring Inspector Training: SAMPLING
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 of 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 o<5cur 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
NOTES:
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NFDES Compliance
liance Monitoring Inspector Training! SAMPLING
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
NOTES:
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NFDES Compliance Monitoring Inspector Training: SAMPLING
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
wastestream'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
NOTES:
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NPDES Compliance Monitoring Inspector Training: SAMPLING
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, und chemical fixation.
Refrigeration is the most widely used technique because it has no detrimental «ffect on the sample composition
and does not interfere with any analytical methods. Refrigeration requires thalt 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.
I
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 appesurs in Appendix E of this
module. These sample preservation procedures and holding times were selectisd by EPA because they retard
sample degradation and minimize monitoring costs by extending holding times; as long as possible.
NOTES:
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NPDES Compliance Monitoring Inspector Training: SAMPLING
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 hi 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.
NOTES:
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NPDES Compliance Monitoring Inspector Training: SAMPLING
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
i
Location of sample collection i
Preservatives used. I
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.
NOTES:
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NPDES Compliance Monitoring Inspector Training: SAMPLING
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, arid 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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NPDES Compliance Monitoring Insi»ect«r Training: SAMPLING
Name of the person collecting the sample \
Sample ID numbers
Date and time of sample collection
Location of sample collection I
. Name(S) and signature^) 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 fonn 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:
Personnel - The person(s) who takes possession of the sample as soon as it is collected
. T.hnr.tnrv Personnel - Laboratory personnel, whether from agency laboratories or from an
independent laboratory, will be responsible for the sample from analysis through disposal.
i
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 purpose.
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NFDES Compliance Monitoring Inspector Training: SAMPLING
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
NOTES:
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NPDES Compliance Monitoring Inspector Training: SAMPLING
direction of the current. The stopper or cap should be protected from contamuiation 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 container. Glass bottles are also more
susceptible to breakage during handling than plastic containers. The standard pi^servation 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 b* measured, the sample should
be filtered through a 0.45 membrane filter prior to acidification.
NOTES:
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NPDES Compliance Monitoring Inspector Training: SAMPLING
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 HjSO, 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
NOTES:
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NPDES Compliance Monitoring Insi>ector Training: SAMPLING
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 prerinsed 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 collect*! m refrigerated glass
containers through teflon tubing. Third, if the sample can not be extracted within 72 hours of collect, 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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NPDES Compliance Monitoring Inspector Training: SAMPLING
3. ANALYTICAL METHODS FOR ONSFTE 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 MethodsJsrCVmical Analysis of Water
and Wastes. ^ «,.nH.«l Methods fa, ** T^mination of Water and Wastewiitgr 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 collated 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.
. Temoerature - Temperature determinations can be made with any1 good grade mercury filled or
SS^JSlsius ZLmeter. The dial-type thermometer is preferred over the ^glass type for field
work because of its durability and ease of reading. All temperature measunng dev1Ces must be
c^LWnodically 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
tothis type of determination is 300 ml. Most DO probes are temperature-sensitive and have
SmpTir^c^mpensation built in. The DO meter must be calibrated onsite in accordance with the
manufacturer's specifications before any DO measurements are made.
pH - pH determinations are often conducted during a sampling inspection. The inspectoi ^shouW
arrange to have a pH meter available. The pH meter must be properly calibrated by the use of fcv
Z5£ Prior to e^h set of PH measurements. The inspector should be aware of condiUons in the
wf SreTtn^Ly 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 ^"f^^
raoidlv Exposure to sunlight or other strong light, or agitation will accelerate clJonne reduchon,
Srefore Sy^ should begin immediately after sampling. A field colormetnc kit such as the
NOTES:
3-1
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NPDES Compliance Monitoring Inspector Training: SAMPLING
HACK 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 field, 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.
NOTES:
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NPDES Compliance Monitoring Inspector Training: SAMPLING
4. AUTOMATIC SAMPLERS
foUowing five
interrelated subsystem components:
T...V. subsystem -
,.
subsequent samples.
^ suborn- Au^,ic
Provide -. of ^ b^c
cups
systems n«y
into account site-specific
^ chimnel flows. Because of the
2ffis2.- Bering
collection in potentially explosive environments.
NOTES:
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NFDES Compliance Monitoring Inspector Training: SAMPLING
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:
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NPDES Compliance Monitoring Inspector Training: SAMPLING
Use of automatic samplers during cold weather presents problems with freezing. Sampler malfunct.ons
and frozen intake lines are quite common. These problems may be handled bousing heat tape or placmg the
sampler inside a thermostatically controlled, electrically heated,nclosure. In the absence of special e^pment,
freezing may be prevented by installing the sampler in a manhole or wet well or by wrapping the sampler wUh
eight or nine inches of insulation and wind protection. Also, the sampler should b* positioned well above the
effluent stream so that the tubing runs in a taut, straight line to prevent liquid from pooling. Catena for
selecting automatic sampling equipment are listed in Appendix J. |
NOTES:
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Compliance Monitoring Inspector
;. FLOW MEASUREMENT
5.1
OF FLOW MEASUREMENT
.
compliance with permit limits, flow n^ment serves to: _;
. p,^ operating and peHonnance data oQ the waSteWater Ueat.ent plant
. compute treatment costs, based on wastewater volume
. obtain data for long-term planning of plant capacity.
t For a more detailed discussion, the inspector should refer to
^
devices are explained below.
5 2 1 -
flumes are examples of primary devices.
NOTES:
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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. La 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:
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NPDES Compliance Monitoring Inspector Training: SAMPLING
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NPDES Compliance Monitoring Inspector Training: SAMPLING
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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., floalt in well, float in flow, bubbler
electrical, or acoustic).
5.3 CLOSED CHANNEL FLOW
Closed channel flow is normally encountered between treatment units iii 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
IMLET SECT10H .SECT10J
PIPE OIA
OUTLET SECTION
HIGH
PRESSURt
TAP
THROAT OIA
HGURE5-4
. CONFIGURATION AND NOMENCLATURE OF VENTURIC METER
NOTES:
-------
meter is shown in Figure 5-5.
NOTES:
Comptac, Monitoring tope^cr
: SAMPLING
5-9
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NPDES Compliance Monitoring Inspector Training: SAMPLING
INSULATING
LINER
ELECTRODE
ASSEMBLY
MAGNET COILS
STEEL METER
BODY
POTTING COMPOUND
NOTES:
FIGURE 5-5. ELECTROMAGNETIC FLOW METER
5-10
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Compliance Monitong
Insp^or Training: SAMPLING
6. QUALITY ASSURANCE/QUALITY C(
. a .
prides precise
«"»-
validity of report*
r rrr::: sirs--
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for rel»b,hty. ,
1 QUALITY CONTROL PROCEDURES FOR SAMPLIN
'
. Appendbc K
(i.ubiatioll
purge, and timing factor.
(» Ch.p«r 2)
:
NOTES:
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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 15 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 r«producibility 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 sidded.
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. _
nunlicate Samples - Separate samples taken at the same time and location using *&
or one sample pulled and separated into two aliquots for duplicate analysis at the same
DupUca^mples check for precision. These samples provide . ebeck 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 deiomzed
££ ^fL laboratory analysis, the value for the blank is subtracted from the samplevalue to
oS the^tual 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
laboratories. Samples are divided into two, or preferably three, segments for analysis *«*««*
abo^atoriS 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
i.
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 cannoft 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
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NPDES
Compliance Monitoring Inspector Training: SAMPLING
GLOSSARY
Aliquot - Portion of a sample.
the organic strength of a wastestream.
sample - «-*- - ** « ~ "* '
' """>*"'
- s.mp,e «*- °f - - ~ -
quality over the compositing or sample penod.
wm
Confined space - Space having bM means of e,,r, or ext, «,d .oject W the accumulation of toxic o,
combustible gases or to a deficiency of oxygen.
Duplicau sample - Separate samples «. from *,
analytical techniques by the same person.
- - - <*- f°' -** -*
, me^remen, - M- or gran measurement for such
specific conductance.
Priority poUutants - A lis, of 126 poUuUn., e.ubHshe, hy BPA,
to humans.
- DO, PH, KmperaWre, and
-aroo- - *
reported data.
ConW, (00 - Routine appncation
and ualytiol measurement proceK (as
lei tats. QC of .malytical procedure.
Sprmr. B!»! or btat »*& u, which . know, _* of ^stance h* been added.
Sp,i, samp,e - Sample th« has be«n divided into two or more con.iners fo, an** by different analys. or
laboratories.
Supernatant - A subs*..* flying above or on to surfto of »ott,er substance.
Turbidity - Condition in a wasted caused by to presence of suspended r*»e, resulting in ,
and absorption of lightrays.
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NPDES Compliance Monitoring Inspect
APPENDIX B
REFERENCES
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NPDES Compliance Monitoring Insprctor 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, Olu'o. 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. j
B-l
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^SCo.pHance Monitoring ns^ Trainingt
APPENDIX C
REVIEW QUESTIONS AND ANSWERS
ON NPDES
SAMPLING PROCEDURES
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NPDES 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? I
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 sulfides
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 I
- 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 (fecal coliform-0.008 % NajSjOj) i .
[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 Ibe 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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NPDES 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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Volume of Sample 1, in ml
Tests
PHYSICAL 100 to 500
. ,_, . . following sample
Color and odor (/; , 100
Corrosivity (2) ;;; * ' ' ' 100
Electrical conductivity (2.) , ioQ to IJQQQ
PH, electrometnc (2) ' ' ' ' ' ' IQQ
Radioactivity . .-': following sample
Specific gravity (2) , ' 1>000 to 2o,000
Temperature (2) ibo to 1,000
Toxicity (2)
Turbidity (2)
CHEMICAL
p;ocnlved Gases 5QO
. ,-, ' "... 200
Ammonia (3) * " ' '
Carbon dioxide (3), free CO2 . . .
ChlorineO), free Cl, ' ' ' ' . .!
Hydrogen (3),,TS* - ^ " ' ' ' ' ' ". 500 to 1,000
Hydrogen sulfide (3), HJ> ] 10Q
Oxygen (3), 02 .
Sulfer dioxide (3), free bj
100
Acidity and alkalinity .;'.:'.'.'.'.'.'.'.'.'.'''' iw
Bacteria, iron . ' ... 100 to 500
Bacteria, sulfate-reducmg ... v -...:..;...,- 1°° to 5UU
Biochemical Oxygen Demand (BOD) ....
Carbon dioxide, total C02 (including _-.... 5^0 100
2,000.4,000
D-l
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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', in ml
Miscellaneous
Chloroform, extractable matter i QOO
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 4 3j0oo to's.OOO
Organic nitrogen 50Q to 1,000
Phenolic compounds .. . gOO to 4,000
pH, colorimetric 10 to 20
Polyphosphates 100 to 200
silic* 50 to 1,000
Solids, dissolved 100 to 20,000
Solids, suspended 50 to 1 000
Tannin and lignin 100 to 200
Cations:
Aluminum, Al+3 100 to 1,000
Ammonium (2), NH4* 500
Antimony, Sb+J to Sb*5 100 to 1,000
Arsenic, As+s to As*5 . 10Q to 1,000
Barium, Ba+2 100 to 1)000
Cadmium, Cd*2 10Q to 1,000
Calcium, Cd+2 100 to 1,000
Chromium, Cr+3 to Cr+s 100 to 1,000
Copper, Cu+2 2 to 4,000
Iron (3), Fe+2 and F*3 IQO to 1,000
Le^. Pb*2 100 to 4,000
Magnesium, Mg+2 10o.to 4,000
Manganese, Mn*2 to Mn*7 100 to 1,000
Mercury, Ng* and Hg+2 100 to 1^000
Potassium, K* 100 to 1,000
Nickel, Ni+2 ICQ to 1,000
D-2
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NPDES Compliance Monitoring Inspector Training: SAMPLING
H^HM "
Volume of Sample Required for Determination of
the Various Constituents of Industrial Wastewater
m S Environmental Protection Agency 1973.
unhook for ^fnnitnriti? Industrial Wastewafa^
Technology Transfer.)
Volume of Sample1, in ml
Tests
Cations: ;
. ; 100 tO 1,000
Silver, Ag* ' '".'.'. 100 to 1,000
Sodium, Na* .... 100 to 1,000
Strontium, Sr+2 ; 100 to 1,000
. Tin, Sn+2 and Sn+4 10° to 1)00°
Zinc, Zn*2
j.
Anions: ;
;. ...... 100 to 200
Bicarbonate, HCO3" . . . . .i 100
Bromide, Br V '.'..:. 100 to 200
Carbonate, CO,'2 25 to 100
Chloride, Cl" ' ' "//.'. , 25 to 100
Cyanide, CN 200
Fluoride, Fr ".'.'.. i. 50 to 100
Hydroxide, OH" 100
Iodide, I' ".'... 10 to 100
Nitrate, NO,'2 50 to 100
Nitrite, N02- - ' :' . I .' .' 50 to 100
Phosphate, ortho, PO^3, HPO^ , H.PO,. 100 to 1>000
Sulfate, SO/2, HSO/ . , _ 100 to 500
Sulfide, S'2, HS" ' 50 to 100
Sulfite, SO,2, HSO;
S
in
- .
-
ompletely fflW. and sealed against dl exposure.
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NPDES Compliance Monitoring Inspector Training: SAMPLING
APPENDIX E
REQUIRED CONTAINERS, PRESERVATION
TECHNIQUES, HOLDING TIMES, AND
TEST METHODS
(EXCERPTED FROM 40 CFR PART 136)
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NPDES Compliance Monitoring Inspector Training: SAMPLING
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NPDES Compliance Monitoring Lrispectot Training: SAMPLING
APPENDIX F
i
EPA ORDER 1440.2
i
HEALTH AND SAFETY REQUIREMENTS
FOR EMPLOYEES ENGAGED IN
FIELD ACTIVITIES
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NPDES Compliance Monitoring Inspector Training*. SAMPLING
1
ENVIRONMENTAL
PROTECTION
AGENCY
ORDER
1440.2
July 12, 1981
PROTECTIVE SERVICES - SAFETY
HEALTH AND SAFETY REQUIREMENTS FOR EMPLOYEES. eSC
" IN PTrrr> ACTIVITIES " ~
I, PURPOSE. This Order establishes policy, responsibilities, and
mandatary requirements for occupational health and safety training
and certification, and occupational medical monitoring off Agency
employees engaged in field activities. ;
a. The tern "field activities" as used in this Order rowans EPA. -
program activities that are conducted by EPA employees' outside of
EPA administered1 facilities. These activities include eworconental .
and pesticides sanpling, inspection of water and wastewater treatment
plants, and hazardous material spills and waste site 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 SPA or its contracted agents vfcich is desigaed to develop,
improve and upgrade the health and safety knowledge of EPA' .employees
involved in field activities.
c. The term "occupational medical monitoring" means, surveillance
over the health status of employees by means of periodic medical exam-
ination* or screening in accordance with the Agency's Ocicupational
Medical Monitoring guideline*. ;i,
d. The tern -certification" as used in this Order meara that ,
employee has successfully completed the ministun classreon and field
traiSna requirements for the specified level of training and the Agency
has issued a certificate attesting that the employee met these require-
ments. - ^
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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. 00, Occupational
Hsalth 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 on Respiratory Protection (Proposed).
h. 49 CFR, Parts 100-177, Transportation of Hazardous Materials.
i. EPA Ci-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 environmental recon-
naisance sampling, inspections, and monitoring, to entering and working
in environments 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. This Order applies to^^EPA organizational units
which have employees engaged in field activities.
6. POLICY. It is the policy of the Environmental Protection Agency
to carry out its- field activities in a manner that assures the pro-
tection of its eiiployees.
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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 find 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 recuire training and certification, and occupational
medical monitoring, and assure they receive it to comply with the provisions
of this Order and will insure these requirements are1 properly contained
in position descriptions and job postings. ; .
c. Employees. Employees are responsible for making known upon
request from their supervisors the extent of their individual occupation-
al health and safety training and the history of their occupational
medical monitoring participation. Employees should notify their
supervisor of any hazardous work situation and make sucjgestions 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 Designees. Ihe Occupational
Health and Safety Designees are responsible for identifying program _
areas that require training and certification, and occupational medical
monitoring; recoitnending or providing training and certification re-
sources to meet the requiranents of this Order; and maintaining records
of persons receiving training and certification.
e. Office of Occupational Health and Safety. IChe Director, Office
of Occupational Health and Safety is responsible fear 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.
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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 accomplished
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 may occur during a
field activity.
b. occupational Medical Monitoring. The objectives of the oc-
cupation: fc Medical Monitoring program are:
(-: > To detect any adverse effects of occupational exposure
on the a -ioyees health and to initiate prompt corrective actions
when indww?.ted; and
(2) To assure that employees assigned arduous or physically
taxin-- jobs or jobs requiring unique skills are able to perform these
jobs without in^airing their health and safety or the health and safety
of ct'iers.
T3AINING AND CERTIFICATION
Bnployees shall not be
^ « ' 'VT^LL'l .JATfyJ m^W S»Ai^^* AA A>^fc^ A<^fc» * ^^g'w -. -^ ^^_-^-T_~ * *
permi-ted to engage in routine field activities until they have been
trained aid certified to a level commensurate with the degree of an-
'x hazards.
a. iasic Level. All snployees shall be provided a rninimuttof
24 hours of health and safety training prior to their becoming in-
volved i-. normal, routine field activities. The training shall
inclur -i but not be limited to classroom instruction in all the
fbllc-.-ing sifcject areas:
F-4
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Materials;
aoi
ORDER
(1) Bnployee Rights and Responsibilities;
(2) Nature of Anticipated Hazards;
J,l .. LJ«1 « arvl Solf-ReSCUe
(4)
(5)
(6)
1440.2
July 12, 1981
(7)
(8)
Personal Protective B^uipnent and Clothing,, Use and Care;
Safe Sampling Techniques. . ,,'
to
an employee experii
a mininrtm of
instruction.
after
activities *i=h at a laterte are deteOT-n ^e ha2ard3
subject matter:
S!
test e^ent fcr radioeeti.vil.v. ex^osivity,
to other identified
m addition to
ancther anpLoyee e^"IrSiSfa;erfcm acead fiAd tasXs
tigations and/or cleaiup l^*^!i^,a±..fS of three norths after
fofa mini* of three days «^"> %££ gsobe .able to provide
classr«m instruction. ?«J^^ £ ^experienced 4
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ORDER
1440.2
July 12,' 1981
c. Advanced Level. All employees who manage uncontrolled hazardous
waste site and spill site monitoring, sandaling, investigations, and
cleanup operations shall be provided a miniimjn 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 stfcject 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 complefing only the additional training requirements if
certified at the next lower level within the previous one-year period.
(2) The Director, Office of Occupation! Health and Safety,
may certify employees based on an evaluation of previous training,
education, and experience. Recommendations for this type certifi-
cation should be made to the Director by the Occupational Health
and Safety Designee at the Reporting Unit.
10. FRSJJENSY. OF TRAINING. Hnplcyees at the Basic, Intermediate, and
Advanced Levels shall complete a rainimun of 3 hours of refresher
classroom instruction annually consisting of a review of all subject
areas to maintain their' certification. In addition to the classroom
instruction, employees shall have 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. RECORD OF TRAINING. ^
a. A record of the level of training and certification shall
be maintained in the employee's official personnel file.
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ORDER
-1440.2
July 12, 1981
b. The Occupational Health and Safety Designee shall maintain
a roster of employee training and certification S3 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. :
i
12. OCOJPATTONAL MEDICAL MONITORING REQUIREMENTS. All employees
routinely engaged in field activities which present the probability
of exposure to hazardous or toxic svjsstances, 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^
inaticn (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. ' <
:i .
13. SAVINGS PROVISION. Changes in the Act, .Executive Order, or EPA
and OSKV 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 implementation of this Order shall be within, one year of its
effective date.
EdwardKT. Hanley !
Director, Office of Management.
Information and Support Ser«ic
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APPENDIX G
LIST OF FIELD SAMPLING EQUIPMENT
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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
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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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APPENDIX H
SAMPLE IDENTIFICATION LABELS
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EXAMPLE SAMPLE TAG
ENVIRONMENTAL PROTECTION AGENCY
OFFICE OF ENFORCEMENT
NATIONAL ENFORCEMENT INVESTIGATIONS CENTER
BUILDING 53, BOX 25227, DENVER FEDERAL CENTER
DENVER, COLORADO 80025 j
xvEPA
Project Code [Station No
.
Designate:
Comp. Grab
)
o
3
Z
5'
i
CO CO
2. O
a o
CO
y>
H >
0 3.
22 1
X CO
CO
CO
1 ©
CO CD
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D I
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CD
D '
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1
APPENDIX I
EXAMPLE RECORD OF FIELD SAMPLE
DATA AND CHAIN-OF-CUSTODY RECORD
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APPENDIX J
CRITERIA FOR SELECTION OF AUTOMATIC
SAMPLING EQUIPMENT
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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 .fat 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. ;
a, 4'C «o
for a
of
,5. A.
24 hours at ambient temperatures ranging from -30 C to .
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. . I .
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APPENDIX K
QUALITY CONTROL PROCEDURES FOR
FIELD ANALYSIS AND EQUIPMENT
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QUALITY CONTROL PROCEDURES
FOR FIELD ANALYSIS AND EQUIPMENT
Dissolved Oxygen
Membrane
Electrode
Winkler-Azide method
EH
Electrode Method
Enter the make,
model, and serial
and/or ID number for
each meter in a
logbook.
Report data to
nearest 0.1 mg/1.
Record data to
nearest 0.1 mg/1.
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 KCll if
necessary.
Check leads, switch
contacts, etc. for
corrosion and shoits
if meter pointer
remains off-scale.;
Duplicate analysis
should be run as a
precision check. ',
Duplicate values
should agree within
±0.2 mg/l.
Calibrate the system
against standard
buffer solutions of
known pH value; (e.g.,
4, 7, and 9 at thu
start of a sampling
run). i
Periodically check
the buffers during
the sample run and
record the data in
the logbook. j
Be on the alert iFor
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.
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NPDES Compliance Monitoring Inspector Training: SAMPLING
Parameter
pH (Continued)
Electrode Method
(Continued)
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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Parameter
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
99 °C to two signifi-
cant figures.
Refer to instrument
manufacturer's
instructions for
proper operation arid
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 <~
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
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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