United States
Environmental Protection
Agency
A Industrial User Inspection And
Sampling Manual For POTW's
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Industrial User Inspection and Sampling
Manual for POTWs
Prepared by:
The Office of Wastewater Enforcement and Compliance
Water Enforcement Division
U.S. Environmental Protection Agency
Washington, D.C. 20460
April, 1994
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UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
WASHINGTON, D.C. 20460
MEMORANDUM
SUBJECT: Transmittal of the Final Industrial User Inspection and Sampling Manual
FROM: Michael B. Cook, Director
Office of Wastewater Enforcement and
TO: Water Management Division Directors
Regions I-X
I am pleased to provide the final Industrial User Inspection and Sampling Manual.
The manual represents the culmination of almost two years of effort on the part of various
offices within EPA Headquarters, and is the result of substantial comments from the EPA
Regional Water Management Divisions, the Office of Research and Development in
Cincinnati, AMSA members, and other interested parties. We appreciate the extensive
effort in providing comments on the previous two drafts. Your insight significantly
improved the document, and we are confident that the manual will be extremely useful to
POTW inspection and sampling personnel.
The final document includes the second round of comments made by the Regions.
The most significant change made to the document as a result of Regional comment is the
deletion of the discussion on determining compliance with the 4-day average standard under
the Electroplating regulation. The method for determining compliance with the
Electroplating standard may be addressed through a policy paper at a later date. A second
significant change is the deletion of the discussion on determining compliance from sample
results below detection. The reason that we deleted this discussion is that the national work
group addressing this issue has delayed its time frame for making a recommendation on
how to address compliance in these situations. Therefore, any discussion of this matter will
need to wait until the national work group has reached its conclusion.
We are expecting to conduct a mass-mailing of the document to all POTWs with
approved pretreatment programs in late spring or early summer depending on the amount of
time it takes to have the document printed. If you have any questions regarding the manual
or its distribution, please feel free to call Lee Okster at (202) 260-8329.
cc: Cynthia Dougherty
Regional Pretreatment Coordinators
Fred Stiehl - OE
Ken Kirk - AMSA
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POTW Inspection and Sampling Manual Preface
Disclaimer
This manual has been written by the Office of Wastewater Enforcement and Compliance, U.S. Environmental
Protection Agency, and has been peer reviewed both within the EPA and outside of the EPA. This guidance
represents the EPA's recommended procedures to be used by POTW personnel when conducting an inspection
or sampling visit at an industrial user. A failure on the part of any duly authorized POTW official, inspector, or
agent to comply with the contents of the manual shall not be a defense in any enforcement action taken against
an IU, nor shall a failure to comply with this guidance alone constitute grounds for rendering evidence obtained
in the inspection inadmissible in a court of law. Any mention of trade names or commercial products is neither
an endorsement nor a recommendation for use.
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POTW inspection and Sampling Manual Preface
Acknowledgements
This manual was written by the Office of Wastewater Enforcement and Compliance, U.S. Environmental
Protection Agency, under the direction of Lee Okster. The Office of Wastewater Enforcement and Compliance
would like to acknowledge the considerable efforts and cooperation of the following individuals, whose
contribution helped to complete this document successfully: Mr. Paul Marshall (Region VII Retreatment
Coordinator) for use of his checklist for inspecting industrial users; the EPA Regional Pretreatment Coordinators
for insightful comments on the draft document; Mr. Sam Hadeed and members of the Association of Metropolitan
Sewerage Agencies (AMSA) who provided comments on the draft document; Mr. William Potter of the EPA's
Office of Research and Development in Cincinnati; Mr. Jack Stoecker of Brown and Caldwell; and Ms. Nadine
Steinberg of the EPA's Office of Enforcement.
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Table of Contents
Disclaimer i
Acknowledgements ii
List of Tables vii
List of Figures viii
Definitions and Acronyms Used in the Pretreatment Program ix
I. Introduction 1
Inspections and Sampling in the Pretreatment Program 1
Legal Authority and Regulatory Basis for Conducting
Industrial User Inspections and Sampling 2
Purposes for Inspection and Sampling Industrial Users 3
Outline of the Guidance 5
II. Inspecting Industrial Users 6
Introduction 6
Developing and Maintaining an IU Survey 7
Frequency of Inspections and Sampling 7
Types of Inspections 8
Confidential Business Information 9
Responsibilities of the Inspector 11
Inspector's Field Notebook 14
Pre-lnspection Activities 16
- Pre-lnspection Preparation
Review of Facility Background Information
Developing an Inspection Plan
Safety and Sampling Equipment Preparation
Notification of the Facility
Entry to the Industrial User 22
- Legal Basis for Entry
- Arrival for the Inspection
Reluctant to Give Consent
Uncredentialed Persons Accompanying the Inspector
Access to Federal Facilities
Denial of Consent to Enter
Withdrawal of Consent to Enter
Denial of Access to Parts of the Facility
Covert Sampling in Response to Denial of Entry
Conducting an Inspection Under a Warrant 28
Pre-lnspection Checklist 29
Pre-lnspection Observations 29
Information to be Collected During the Inspection 31
On-Site Activities 32
- Opening Conference
- Inspection Procedures
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Table of Contents (cont.)
Physical Plant Review
Self-Monitoring Review
Operations Evaluation
Maintenance Evaluation
Records Review at the Industrial User
Obtaining Copies of Necessary Records
Record Identification Procedures
- Closing Conference
Follow-Up Activities 45
- Inspection Report
Inspection Checklist 48
III. Sampling Industrial Users 53
Introduction 53
Analytical Methods 55
Quality Assurance and Sampling Plan 56
Standard Operating Procedures 58
Pre-Sampling Activities 60
Cleaning and Preparation of Sampling Equipment
Cleaning Procedures for Conventional Pollutants
Cleaning Procedures for Metals
Cleaning Procedures for Oil and Grease
Cleaning Procedures for Organic Analyses
Volatile Organic Compounds
Semi-Volatile Organic Compounds, Organochlorine Pesticides
& PCBs
Cleaning of Automatic Sampling Equipment
Preparing Field Instruments
Ph Meters
Residual Chlorine Meters
Temperature
Dissolved Oxygen
Selection and Preparation of Sample Containers
Type of Sample
On-Site Activities 71
Sampling Location
Sample Collection Techniques
Sample Volume
Sample Preservation and Holding Times
Sample Documentation
Sample Identification and Labeling
Chain-of-Custody
Sample Packaging and Shipping
Quality Control
Safety Considerations During Sampling 79
Physical Hazards
Atmospheric Hazards
Oxygen Deficient Atmosphere
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Table of Contents (cont.)
Explosive Atmosphere
Toxic Atmosphere
- Safety Equipment
Protective Clothing
Traffic Control
Radio
Air Monitoring Devices
Ventilation Devices
Safety Harness and Retrieval System
Respirators
- Confined Space Entry
- Safety Training
Flow Measurement
- Open Channel Flow
Primary Devices
Secondary Devices
- Closed Channel Flow
Quality Assurance and Quality Control
- Quality Control Procedures for Sampling
- Quality Assurance Procedures for Sampling
- Laboratory Quality Assurance and Quality Control
Compliance Issues Related to Industrial User Sampling
- The Use of Duplicate Samples to Evaluate Compliance
- Compliance With Monthly Average Limitations
- Closed Cup Flashpoint Sampling and Compliance
- Frequency of POTW Sampling In Lieu of Industrial User Sampling
- SNC in Situations of Multiple Outfalls
- Violation Date
- Compliance With Continuous Monitoring of pH
Summary
Appendix I - General Industrial Inspection Questions
Appendix II - Industry Specific Questions
Appendix III - General Operations and Maintenance Questions
Appendix IV - Hazard Associated With Specific Industrial Categories
Appendix V - EPA Memorandum The Use of Grab Samples to Detect Violations of Pretreatment Standards.'
Appendix VI - Now Measurement Techniques
Appendix VII - EPA Memorandum, "'Determining Industrial User Noncompliance Using Split Samples"
Appendix VIII - Compliance With Continuous Monitoring of pH
Appendix IX - Example Standard Operating Procedures
Appendix X - Example Sample Tag and Chain-of-Custody Form for Use by POTWs
Appendix XI - List of Regional Pretreatment Coordinators
Appendix XII - List of Available Pretreatment Guidance Documents
Appendix XIII - 40 CFR Part 136 - Tables IA, IB, 1C, ID, IE and II
94
99
104
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List of Tables
Table # and Title Page #
2-1 Procedural Responsibilities of the POTW Inspector 13
2-2 Knowledge and Skills Reguired of Pretreatment Inspectors 15
2-3 Information to Review Prior to the Inspection 18
2-4 "Generic" Elements of an Inspection Plan 21
2-5 Pre-lnspection Checklists 30
3-1 Checklist of Field Sampling Eguipment 61
3-2 Composite Sampling Methods 7 0
3-3 Volume of Sample Reguired for Analyzing Various Industrial Pollutants 107
3-4 Reguired Containers, Preservation Technigues, Holding Times, and Test Methods 109
VI-1 Head-Discharge Relationship Formulas for Nonsubmerged Weirs VI-3
VI-2 Discharge of 90° V-Notch Weir - Head Measured at Weir Plate VI-4
VI-5 Flow Rates for 60° and 90° V-Notch Weirs VI-5
VI-3 Minimum and Maximum Recommended Flow Rates for Cipolletti Weirs VI-7
VI-4 Minimum and Maximum Flow Rates for Free Flow Through Parshall Flumes VI-7
VI-5 Free Flow Values of C and N for Parshall Flume Based on the Relationship Q=CWH." VI-11
VI-6 Minimum and Maximum Recommended Flow Rates for Free Flow Through
Plast-Fab Palmer-Bowlus Flumes VI-13
VI-7 Coefficients of Discharge c for Venturi Meters VI-15
VI-8 Values of K in Formula for Venturi Meters VI-15
VI-9 Advantages and Disadvantages of Secondary Devices VI-17
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List of Figures
Figure # and Title Page #
2-1 Example of a Deficiency Notice 47
3-1 Metals Cleaning Procedures 61
3-2 Atmospheric Constituents 80
3-4 Profile and Nomenclature of Sharp-Crested Weirs 90
3-5 Four Common Types of Sharp-Crested Weirs 91
3-6 Plan View and Cross Section of a Parshall Flume 92
3-7 Free-Flowing Palmer-Bowlus Flume 93
3-8 Configuration and Nomenclature of a Venturi Meter 93
3-9 Electromagnetic Flow Meter 95
VI-2 Nomograph for the Capacity of Rectangular Weirs VI-6
VI-3 Flow Curves for Parshall Flumes VI-8
VI-4 Dimensions and Capacities of Parshall Flumes for Various Throat Widths VI-9
VI-5 Effect of Submergence on Parshall Flume Free-Discharge VI-12
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Definitions and Acronyms Used in the P ret reat me nt Program
1) Accuracy
Accuracy refers to the degree of difference between observed values and known or actual value in the
analysis of wastewater.
2) Act or "the Act"
The Federal Water Pollution Control Act. also known as the Clean Water Act, as amended, 33 U.S.C.
§125 et.seq.
3) Acute Effects
When the effects of an exposure to a pollutant (over a short period of time) cause severe health effects to
humans or other organisms, this condition is said to be acute (compare to chronic below).
4) Baseline Monitoring Report (BMR) [40 CFR 403.12(b)]
All new source industrial users subject to categorical standards must submit a baseline monitoring report
(BMR) to the Control Authority (POTW, State or EPA) at least 90 days prior to the commencement of
discharge. The purpose of the BMR is to provide initial information to the Control Authority including
identifying information, description of existing environmental permits, description of operations, flow
measurements (estimated), and the concentration of pollutants in the waste stream (estimated). Existing
sources were required to submit BMRs within 180 days after the effective date of any applicable
categorical standard.
Batch Process
A treatment or manufacturing process in which a tank or reactor is filled, the wastewater (or solution) is
held or a chemical solution is prepared, and the tank is emptied, resulting in a discrete discharge to the
sanitary sewer. The tank may then be refilled and the process repeated. Batch processes are also used to
clean, stabilize, or condition chemical solutions for use in industrial manufacturing and treatment
processes.
6) Biochemical Oxygen Demand (BOD)
The quantity of oxygen utilized in the biochemical oxidation of organic matter under standard laboratory
procedures for five (5) days at 20° centigrade, usually expressed as a concentration (e.g.. mg/l). BOD
measurements are used to indicate the organic "strength" of wastewater.
7) Biological Treatment
A waste treatment process by which bacteria and other microorganisms break down complex organic or
inorganic (e.g., ammonia) materials into simple, nontoxic, more stable compounds.
8) Blank (Bottle)
Is an aliquot of analyte-free water which is taken through the appropriate steps of the analytic process as
a means of determining if the sampling container is introducing contamination into the sample. For
aqueous samples, reagent water is used as a blank matrix; however, a universal blank matrix does not
exist for solid samples (e.g., sludge), and therefore, no matrix is used.
9) Blank (Equipment)
Is an aliquot of analyte-free water which is taken to and opened in the field. The contents of the blank
are poured appropriately over or through the sample collection device, collected in a sample container,
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POTW Inspection and Sampling Manual Definitions
and returned to the laboratory as a sample to be analyzed. Equipment blanks are a check on the sampling
device cleanliness.
10) Blank (Field)
Is an aliquot of analyte-free water or solvent brought to the field in sealed containers and transported
back to the laboratory with the sample containers and analyzed along with the field samples.
11) Blank (Method)
Is an aliquot of analyte-free water prepared in the laboratory and analyzed by the analytical method used
for field samples. Method blanks are used to test for the cleanliness of reagents, instruments, and the
laboratory environment.
12) Blank (Sample Preservation)
Is an aliquot of analyte-free water (usually distilled water) to which a known quantity of preservative is
added. This type of sample is a means of determining the level of contamination of acid and chemical
preservatives after a period of use in the field.
13) Blowdown
The discharge of water with high concentrations of accumulated solids from boilers to prevent plugging
of the boiler tubes and/or steam lines. In cooling towers, blowdown is discharged to reduce the
concentration of dissolved salts in the recirculating cooling water. Clean "make-up" water is added to
dilute the dissolved solids in the system. Blowdown also includes the discharge of condensate.
14) Categorical Industrial User (CIU)
A categorical industrial user is an industrial user (see ID definition below) which is subject to a
categorical standard promulgated by the U.S. EPA.
15) Categorical Standards (40 CFR 405-471)
Any regulation containing pollutant discharge limits promulgated by the EPA in accordance with Sections
307(b) and (c) of the Act (33 U.S.C. §1317) which apply to a specific category of users and which
appear in 40 CFR Chapter I, Subchapter N, Parts 405-471.
16) Centralized Waste Treatment Facility (CWT)
A public or private facility which treats hazardous and other wastes. These facilities are designed to
handle the treatment of specific hazardous wastes from industry. The waste waters containing the
hazardous substances are transported to the facility for proper storage, treatment and disposal.
17) Chain of Custody
A legal record (which may be a series of records) of each person who had possession of an
environmental sample, from the person who collected the sample to the person who analyzed the sample
in the laboratory and to the person who witnessed the disposal of the sample.
18) Chemical Oxygen Demand (COD)
Chemical oxygen demand is expressed as the amount of oxygen consumed from the oxidation of a
chemical during a specific test (in mg/L). As such, COD is a measure of the oxygen-consuming capacity
of the organic matter present in the wastewater. The results of the COD test are not necessarily related to
the Biochemical Oxygen Demand (BOD) because the chemical oxidant responsible for utilizing the
oxygen may react with substances which bacteria do not stabilize.
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POTW Inspection and Sampling Manual Definitions
19) Chemical Treatment Process
A waste treatment process which involves the addition of chemicals to achieve a desired level of effluent
quality.
20) Chronic Effects
When the effect of a single or repeated exposure(s) to a pollutant causes health effects over a long period
of time in humans or other organisms this is said to be a chronic condition (compare to acute above).
21) Code of Federal Regulations (CFR)
A publication of the United States government which contains all of the finalized federal regulations.
Federal environmental regulations are found in volume 40 of the CFR. and the General Pretreatment
Regulations are found at 40 CFR Part 403.
22) Combined Wastestream Formula (CWF) 140 CFR 403.6(e)l
The combined wastestream formula is a means of deriving alternative categorical discharge limits in
situations where process effluent is mixed with waste waters other than those generated by the regulated
process prior to treatment.
23) Composite Proportional) Samples
A composite sample is a collection of individual grab samples obtained at regular intervals, either based
on time intervals or flow intervals (e.g., every two hours during a 24-hour time span or every 1000
gallons of process wastewater produced). Each individual grab sample is either combined with the others
or analyzed individually and the results averaged. In time composite sampling the samples are collected
after equal time intervals and combined in proportion to the rate of flow when the sample was collected.
Flow composite sampling can be produced in one of two ways. The first method of obtaining a flow
composite sample is to collect equal volume individual grab samples after a specific volume of flow
passes the sampling point. The second manner of obtaining flow composite sample is to vary the volume
of the aliquot collected in proportion to the amount of flow that passed over the time interval which the
sample represents. Composite samples are designed to be representative of the effluent conditions by
reflecting the average conditions during the entire sampling period (compare grab sample).
24) Confined Space
A space which, by design, has limited openings for entry and exit, unfavorable natural ventilation which
could contain or produce dangerous air contaminants (or create an atmosphere of oxygen deprivation),
and which is not intended for continuous employee occupation. A permit may be required under OSHA
to enter a confined space.
25) Conservative Pollu tant
A pollutant found in wastewater that is not metabolized while passing through the treatment processes in
a conventional wastewater treatment plant. Therefore, a mass balance can be constructed to account for
the distribution of the conservative pollutant For example, a conservative pollutant may be removed by
the treatment process and retained in the plant's sludge or it may leave the plant in the effluent.
Although the pollutant may be chemically changed in the process, it can still be detected. Heavy metals
such as cadmium and lead are conservative pollutants.
26) Control Authority 1403.12(a)l
The Control Authority is the jurisdictional entity which oversees the implementation of the National
Pretreatment Program at the local level. Usually, the Control Authority is the POTW with an approved
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POTW Inspection and Sampling Manual Definitions
pretreatment program, but in some cases, the Control Authority may be the State (e.g., Vermont,
Connecticut, Nebraska, Alabama, and Mississippi), or it may be the EJPA (i.e., where there is no local
approved program and the state is not approved to administer the National Pretreatment Program in lieu
of the EPA).
27) Conventional Pollutant
A pollutant which has been designated as conventional under section 304(a)(4) of the Act. These
pollutants include: BOD. TSS, pH, fecal coliform, and oil and grease.
28) Custody
Custody refers to the process whereby the inspector gains and controls possession of a sample, A sample
is in custody if: I) it is in the actual possession, control, and presence of the inspector; or 2) it is in the
inspector's view; or 3) it is not in the inspector's presence, but is in a place of storage where only the
inspector has access; or 4) it is not in the inspector's physical presence, but is in a place of storage and
only the inspector and identified others have access.
29) Dallv Maximum
Is the average value of all grab samples taken during any given calendar day. If only one grab sample
has been taken, that grab sample becomes the daily maximum (as well as the instantaneous maximum
see definition below). If more than one grab sample is taken in a given day, the daily maximum is the
average of all the individual grab samples. A composite sample, by definition, becomes the daily
maximum for the calendar day in which it is collected.
30) Duplicate Sample (Field)
Is a precision check on sampling equipment and sampling technique. At selected stations on a random
time frame duplicate samples are collected from two sets of field equipment installed at the site, or
duplicate grab samples are collected from a single piece of equipment at the site.
31) Duplicate Sample (Laboratory)
A sample which is received by the laboratory and divided (by the laboratory) into two or more portions.
Each portion is separately and identically prepared and analyzed. The results from laboratory duplicate
samples check the laboratory precision.
Wastewater or other liquid - raw, untreated, partially or completely treated - flowing from an ILJ to a
reservoir, basin, treatment process, or treatment plant.
33) EPA
The United States Environmental Protection Agency. The principal environmental regulatory agency
established by the Congress to administer the nation's environmental laws.
34) Existing Source
Any source of discharge, the construction or operation of which commenced prior to the publication by
the KPA of proposed categorical pretreatment standards, which will be applicable to such source if the
standard is thereafter promulgated in accordance with Section 307 of the Act.
35) Grab Sample
A sample which is taken from a wastestream without regard to the flow in the wastestream and over a
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period of time not to exceed 15 minutes.
36; Hazardous Waste (40 CFR 261)
For a waste to be considered a hazardous waste it must first be designated a solid waste. Virtually all
forms of wastes are considered to be solid wastes (including solids, liquids, semi-solids, and contained
gaseous materials) except those expressly excluded under the regulatory definition, e.g., industrial effluent
which is mixed with sanitary wastes in the sewer. For a solid waste to be considered hazardous it must
meet one of two criteria: 1) it has one of the following four characteristics - ignitibility, corrosivity,
reactivity, or toxicity (according to the Toxicity Characteristic Leaching Procedure), or 2) it must be a
listed hazardous waste in 40 CFR 261.31-261.33.
37) Industrial User (IV) 140 CFR 403.3(h)l
An industrial user is any non-domestic source which introduces pollutants into a publicly owned
treatment works (POTW).
Wastewater or other liquid - raw (untreated), partially or completely treated - flowing into a reservoir,
basin, treatment process, or treatment plant.
39; Instantaneous Maximum Discharge Limit
The maximum concentration of a pollutant allowed to be discharged at any time, determined from the
analysis of a grab sample collected at the industrial user.
40) Interference 140 CFR 403.3(i)l
A discharge which, alone or in conjunction with a discharge or discharges from other sources, inhibits or
disrupts the POTW, its treatment processes or operations or its sludge processes, use or disposal; and
therefore, is a cause of a violation of the POTW's NPDES permit or of the prevention of sewage sludge
use or disposal in compliance with the act or any more stringent State or local regulations.
41) Local Limits 140 CFR 403.5(c)l
Effluent discharge limits applicable to industrial users of the Control Authority's system developed by the
Control Authority in accordance with 40 CFR 403.5(c).
42) Monthly Average
The monthly average is the arithmetic average value of all samples taken in a calendar month for an
individual pollutant parameter. The monthly average may be the average of al! grab samples taken in a
given calendar month, or the average of all composite samples taken in a given calendar month.
43) New Source 140 CFR 403.3(k)(l)l
(I) Any building, structure, facility, or installation from which there is (or may be) a discharge of
pollutants, the construction of which commenced after the publication of proposed pretreatment
standards under Section 307(c) of the Act which will be applicable to such source if such standards
are thereafter promulgated in accordance with that section, provided that:
(a) The building, structure, facility, or installation is constructed at a site at which no other
discharge source is located; or
(b) The building, structure, facility, or installation totally replaces the process or production
equipment that causes the discharge of pollutants at an existing source; or
(c) The production or wastewater generating processes of the building, structure, facility, or
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installation are substantially independent of an existing source at the same site. In determining
whether these are substantially independent, factors such as the extent to which the new
facility is engaged ion the same general type of activity as the existing source, should be
considered.
(2) Construction on a site at which an existing source is located results in a modification rather than a
new source if the construction does not create a new building, structure, facility, or installation
meeting the criteria of Section UXb) or (c) above but otherwise alters, replaces, or adds to an
existing process or production equipment.
(3) Construction of a new source as defined under this paragraph has commenced if the owner or
operator has:
(a) Begun, or caused to begin, as part of a continuous on-site construction program;
(i) any placement, assembly, or installation of facilities or equipment; or
(ii) significant site preparation work including clearing, excavation, or removal of existing
buildings, structures or facilities which is necessary for the placement, assembly, or
installation of new source facilities or equipment; or
(iii) entered into a binding contractual obligation for the purchase of facilities or equipment
which are intended to be used in its operation within a reasonable time. Options to
purchase or contracts which can be terminated or modified without substantial loss,
and contracts for feasibility, engineering, and design studies do not constitute a
contractual obligation under this definition.
44) 90-Dav Compliance Rwort 140 CFR 403.l2(d)l
A report submitted by categorical industrial users within 90 days following the date for final compliance
with the standards. This report must contain flow measurement (or regulated process streams and other
streams), measurement of pollutants, and a certification as to whether the categorical standards are being
met.
45) Noncontact Cooling Water
Water used for cooling which does not come into direct contact with any raw material, intermediate
product, waste product, or finished product.
46) HPDES Permit
A National Pollutant Discharge Elimination System permit is the regulatory document issued by either
the EPA or approved State agency. The permit is designed to control the discharge of pollutants from
point sources into waters of the U.S.
47) Pass Through 140 CFR 403.3MI
A discharge which exits the POTW into waters of the United States in quantities or concentrations
which, alone or in conjunction with a discharge or discharges from other sources, is a cause of a
violation of any requirement of the City's NPDES permit, including an increase in the magnitude or
duration of a violation.
48) Periodic Compliance Report 140 CFR 403.12(e)l
A report submitted at least twice annually by each significant industrial user regulated under the local
pretreatment program which indicates the nature and concentration of pollutants in the effluent which are
limited by applicable pretreatment standards. In addition, the periodic report must indicate a record of
measured or estimated average maximum daily flows for the reporting period.
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pH is an expression of the concentration of hydrogen ions in solution. The measurement indicates an
acid solution when the pH is <7 and an alkaline solution when the pH is -7. pH meters typically
measure the pH in the range of 0 to 14. pH reflects the negative logarithm of the hydrogen ion
concentration of the aqueous solution.
50) Physical Waste Treatment Process
Physical wastewater treatment processes include racks, screens, comminutors. clarifiers (sedimentation
and flotation), and filtration, which, through physical actions, remove pollutants from the wastewater.
51) Pickle
An acid or other chemical solution in which metal objects are dipped to remove ov>de scale or other
adhering substances.
52) POTW 140 CFR 403.3(0)1
Publicly Owned Treatment Works. A sewage (or wastewater) treatment v jrks which is owned by a
state, municipality, city, town, special sewer district or other publicly ov .ed or financed entity, as
opposed to a privately owned (industrial) treatment facility. The def- ,
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POTW inspection and Sampling Manual Definitions
regulatory focus in on the control of hazardous waste through a comprehensive system of identification,
tracking, treatment, storage, and ultimate disposal.
59; Receiving Water
A stream, lake, river, ocean, or other surface or groundwater into which treated or untreated wastewater
is discharged.
60) Representative Sample
A sample from a wastestream that is as nearly identical in composition to that in the larger volume of
wastewater being discharged.
61) Sewer Use Ordinance (SUO)
A sewer use ordinance is a legal instrument implemented by a local governmental entity which sets out
all the requirements for the discharge of pollutants into a publicly owned treatment works.
62) Significant Industrial User (SIl) 140 CFR 403.3(01
A significant industrial user is an industrial user (see IU definition above) which is either: 1) a
categorical industrial user; 2) a user which discharges an average of 25.000 gallons per day or more of
process wastewater to a POTW; 3) contributes a process wastestream which makes up 5 percent or more
of the average dry weather hydraulic or organic capacity of the POTW; or 4) is designated significant
industrial user by the POTW
63; Significant Noncompltance (SNC) 140 CFR 403.8(f)(2)(vii)l
An industrial user is in SNC if its violations meet one or more of the following criteria:
(A) Chronic violations of wastewater discharge limits, defined as those in which sixty-six percent or
more of all measurements taken during a six month period exceed (by any magnitude) the daily
maximum limit or the average limit for the same pollutant parameter;
(B) Technical Review Criteria (TRC) violations, defined as those violations in which thirty-three
percent or more of all measurements for each pollutant parameter taken during a six month period
equal or exceed the product of the daily maximum limit or the average limit multiplied by the
applicable TRC (TRC I 4 for BOD. TSS, fats, oil, and grease, and 1.2 for all other pollutants
except pH;
(C) Any other violation of a pretreatment effluent limit (daily maximum or longer term average) that
the Control Authority determines has caused, alone or in combination with other discharges.
interference or pass through (including endangering the health of POTW personnel or the general
public):
(D) Any discharge of a pollutant that has caused imminent endangerment to human health, welfare or to
the environment or has resulted in the PO'I'W's exercise of its emergency authority to halt or
prevent such discharge;
(E) Failure to meet, within 90 days after the schedule date, a compliance schedule milestone contained
in a local control mechanism or enforcement order for starting construction, completing
construction, or attaining final compliance;
(F) Failure to provide, within 30 days after the due date, required reports such as the baseline
monitoring report (see definition above), 90-Day Compliance Report (see definition above), periodic
report (see definition above), and reports on compliance with compliance schedules;
(G) Failure to accurately report noncompliance; and
(H) Any other violation or group of violations which the Control Authorit> determines will adversely
affect the operation or implementation of the local pretreatment program..
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POTW Inspection and Sampling Manual Definitions
64) Sludee
The settleable solids intentionally separated from liquid waste streams during treatment typically under
quiescent conditions, and the unintentional accumulation of solids in tanks and reservoirs associated with
production and manufacturing processes.
65) Slue Discharge 140 CFR 403.8(f)(2)(v)l
Any discharge at a flow rate or concentration which could cause a violation of the prohibited discharge
standards in the General Pretreatment Regulations.
66) Slue Discharge Control Plan 140 CFR 403.8(f)(2)(v)l
A plan designed to prevent the uncontrolled discharge of raw pollutants (or materials, e.g., a dairy spill
of milk may disrupt a small POTW and would have to be reported even though milk is not a "pollutant")
into the POTW. Every Significant Industrial User is required to be evaluated, at least every two years,
for the necessity of instituting such a control plan.
67) Spiked Sample (Field)
A sample of a known amount of a particular pollutant constituent prepared in the field by adding a
known amount of the analyte in question during sampling. This technique identifies potential sample
matrix interference and/or problems with inadequate sample preservation.
63) Spilled Sample (Laboratory)
A sample of a known amount of a particular pollutant constituent prepared in the laboratory by adding a
known amount of the pollutant in question at a concentration where the accuracy of the test method is
satisfactory. Spiked samples check on the accuracy of the analytical procedure.
69) Split Sample (Field)
A sample which is collected and divided in the field into the necessary number of portions (e.g., 2, 3,
etc.) for analysis. Equally representative samples must be obtained in the process. The split samples are
then analyzed by separate laboratories (or the same laboratory) preferably using the same analytical
techniques.
70) Technology-Based Standards
Discharge limits for specific industrial categories established by the Federal EPA based on the use of the
Best Available Technology economically achievable (BAT), the Best Practicable Control Technology
available (BPT), or the Best Conventional Technology available (BCT). Such standards are based on the
cost and/or availability of technology to treat the specific wastestream under consideration.
71) Toxic Pollutant (40 CFR 122 Appendix D)
Those pollutants, or combination of pollutants, including disease-causing agents, which after discharge
and upon exposure, ingestion, inhalation, or assimilation into any organism either directly from the
environment or indirectly by ingestion through the food chain, will, on the basis of information available
to the Administrator of the EPA, cause, death, disease, behavioral abnormalities, cancer, genetic
mutations, physiological malfunctions (including malfunctions in reproduction) or physical deformations,
in such organisms or their offspring. Such pollutants which have been identified as toxic are listed at 40
CFR 122 Appendix D.
72) Water Quality Standards
Water quality standards are provisions of state or federal law which consist of a designated use or uses
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POTW Inspection and Sampling Manual Definitions
for a given water body and associated water quality criteria which must be met in the stream to achieve
these uses. Water quality standards are effluent standards imposed on point sources. These standards
are designed to achieve the water quality criteria established for a given wata body. These standards are
designed to improve and/or maintain the quality of the receiving water, regardless of the cost or
availability of treatment technology.
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I. INTRODUCTION
Inspections and Sampling in the Purposes and Objectives for Inspecting and Sampling
Pretreatment Program 1 Industrial Users 3
Legal Authority and Regulatory Basis for Conducting Outline of the Guidance 5
Industrial User Inspections and Sampling 2
Inspections and Sampling in the Pretreatment Program
The requirements imposed on Industrial Users (lUs) and Publicly Owned Treatment Works (POTWs) by
the National Pretreatment Program have become increasingly complex. The scope and detail of the
pretreatment regulations have expanded at the same time as the control on the discharge from POTWs has
evolved from traditional pollutants (e.g., BOD, TSS, etc.) to water quality-based permit limits and
biomonitoring requirements. In addition, the Federal Sludge Regulation, promulgated on February 19, 1993,
imposes requirements on the POTWs sludge use or disposal practice based on the quality of the sludge the
POTW produces. Due to this increased complexity and the strengthened controls on the POTWs effluent and
sludge, it has become increasingly important for the POTW to be able to assess directly the compliance status
of its I Us. The primary method for a POTW to accomplish this oversight is to use periodic inspections and
sampling at the IU.
This manual is intended to acquaint POTW personnel with the well-established inspection and
wastewater sampling procedures which have been used in the NPDES program for many years. The
information presented will guide the POTW inspector by providing a framework for conducting inspections
and wastewater sampling. The manual assumes that the POTW inspector has a basic knowledge of
wastewater treatment technologies, as well as all applicable Federal. State and local pretreatment
requirements. The information contained in this guidance will serve the experienced inspector as a reference,
while new inspection personnel will find it useful as a logical framework for learning how to conduct
inspections and sampling. This manual is also intended to assist the POTWs legal counsel and lab personnel
as a reference for the legal and technical aspects of pretreatment inspections and sampling activities. This
manual is not intended to provide detailed information on pollution prevention activities. For further
information on pollution prevention, the POTW should consult the following EPA Manual: Guides to
Pollution Prevention: Municipal Pretreatment Programs. October, 1993, EPA/625/R-93/006.
Prior to this manual, in July, 1986, the EPA issued the Pretreatment Compliance Monitoring and
Enforcement (PCME) Guidance document, With the evolution of the Pretreatment Program since that time,
As used in the text and throughout this manual, the term 'inspector' includes all field personnel who collect information that may lead
to or support an enforcement action While the focus of the text is on the conduct of compliance inspection at facilities subject to regulation
by the POTW, the majority of the material is also relevant to other types of compliance/enforcement investigations
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Industrial User Inspection and Sampling Manual Introduction
however, much of the information contained in the PCME Guidance has become outdated. Instead, POTWs
should use the Guidance for Developing Control Authority Enforcement Response Plans (September, 1989),
the Industrial User Permitting Guidance Manual (September, 1989) and this guidance as the principal guides
for implementing their approved pretreatment programs. These three documents are intended to replace the
use of the PCME Guidance because they provide the most current information for POTWs to establish
appropriate pretreatment permitting, compliance monitoring and enforcement procedures.
This document creates a comprehensive and detailed framework for conducting inspections and sampling
at regulated industrial users. Certain elements of this overall framework may not need to be implemented by
each POTW in all cases. For example, where there are few industrial users in the system and each one is
small, the POTW may never encounter issues relating to confidential business information or some of the
safety precautions described in this manual. Nevertheless, each of these items should be considered when a
new industrial user is identified in the POTWs system. For large POTWs with many industrial users which
are complex, it will probably be necessary for the POTW to follow each of the procedures outlined in this
manual.
Legal Authority and Regulatory Bask for Conducting
Industrial User inspections and Sampling
The General Pretreatment Regulations establish the overall framework for implementing an approved
pretreatment program. The Regulations outline the minimum requirements which a POTW must perform to
satisfy the obligation established in its NPDES permit. With regard to inspecting and sampling industrial
users, Section 403.8(f)(1)(v) of the Regulations requires the POTW to have the legal authority to:
"carry out all inspection, surveillance and monitoring procedures necessary to determine, independent of
information supplied by Industrial Users, compliance or noncompliance with applicable Pretreatment
Standards and requirements Representatives of the POTW shall be authorized to enter any premises of
any Industrial User in which a discharge source or treatment system is located or in which records are
required to be kept ... to assure compliance with Pretreatment Standards."
The standard to which POTWs are held for purposes of evidence collection during an inspection or sampling
event is further outlined in Section 403.8(f)(2)(vi):
"Sample taking and analysis and the collection of other information shall be performed with sufficient
care 10 produce evidence which is admissible in enforcement proceedings or judicial actions."
It is important that the inspector keep current on the regulations by reading the Federal Register, the Code of
Federal Regulations, by subscribing to a service which summarizes the EPA regulations, or by consulting on a
regular basis with the POTWs legal counsel.
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Industrial User Inspection and Sampling Manual Introduction
The overall objectives of the General Pretreatment Regulations are to: I) prevent the introduction of
pollutants into POTWs which will interfere with the operation of the plant, including interference with the
desired use or disposal of its municipal sludge; 2) prevent the introduction of pollutants into the POTW which
will pass through the treatment works to receiving streams; 3) improve opportunities to reclaim and recycle
municipal and industrial wastewaters and sludges; and 4) reduce the health and environmental risk of
pollution caused by the discharge of toxic pollutants to POTWs
Ultimately, the POTW must implement an overall compliance monitoring program (i.e.. receiving and
reviewing self-monitoring reports from IDs, and conducting inspections and sampling) that accomplishes the
following objectives: 1) meets the requirements and intent of the General Retreatment Regulations. 3) is
effective and timely in determining compliance with categorical standards, local limits and prohibited
discharge standards, 3) provides representative data required to meet POTW reporting requirements to the
State or EPA. and 4) provides sampling data that would be admissible in court, if such an enforcement action
were to be undertaken by the POTW, State or Federal government.
Inspection and sampling activities form the core of the POTWs compliance monitoring program and
require POTW personnel to enter private property to gather information to assess or determine the compliance
status of the facility. Therefore, these compliance monitoring activities must be performed in accordance with
minimum constitutional protections (e.g., protecting against unreasonable searches and seizures), as well as
other rights and "due process" considerations available to individuals under Federal. State or local law.
Consequently, all POTW representatives, including any authorized agents of the POTW, who enter industrial
facilities should* be familiar with the section of their local ordinance that gives the Inspector (or the POTWs
agent) the authority to enter an industrial user's facility to conduct an inspection or sample the wastcwater. In
addition, each inspector should be familiar with the POTWs standard procedures for entering industrial
facilities, including how to obtain a warrant if entry is denied or withdrawn.
Purposes and Objectives for Inspecting
and Sampling Industrial Users
The purposes and objectives of the POTWs compliance monitoring program (including inspections and
sampling conducted by the POTW) are to:
Verify the completeness, accuracy and representativeness of self-monitoring data from the ID:
Determine compliance with IU permit conditions or Sewer Use Ordinance (SUO) provisions;
Support enforcement actions taken by the POTW against noncompliant It's;
Generate data which can be used by the POTW in its annual report to the Approval Authority;
Determine if the IU has corrected problems identified in the previous inspection:
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Industrial User inspection and Sampling Manual Introduction
Determine potential problems with other statutes or regulations (e.g., OSHA, RCRA);
Evaluate Best Management Practices and pollution prevention measures;
Identify which IDs influence the quality of the POTW's influent, effluent, and sludge quality;
Evaluate the impacts of the POTW's influent on its treatment processes and receiving stream;
Evaluate, the need for revised local limits;
Inform the regulated community of pretreatment requirements;
Maintain current data on each regulated industrial user;
Assess the adequacy of the industrial user's self-monitoring program and the IU permit;
Provide a basis for establishing the sampling requirements of the IU (above the Federal minimum);
Evaluate the adequacy of the IlJ's operation and maintenance activities on its pretreatment system;
Assess the potential for spills and/or slug discharges;
Evaluate the effectiveness of slug discharge control measures;
Gather information for IU permit development;
Evaluate the adequacy of the IlJ's hazardous waste management and disposal;
Evaluate compliance with existing enforcement actions; and
Develop a good working relationship with the IU;
The inspector is the cornerstone of the POTW's compliance monitoring and enforcement of the pretreatment
program. Without the inspector on the scene, processes that violate Federal, State, or local laws would
continue to jeopardize the POTW, the environment, and public health.
For example, industrial waste can cause damage to the POTW's collection system by clogging sewers,
causing corrosion, creating the potential for explosions, and contaminating the POTW's sludge. Toxic wastes
from industry can upset the biological treatment processes which may take months to repair. To protect the
environment, the Pretreatment Program has been designed to prevent pollutants generated at industrial sites
from passing through (see the definition of Pass Through in the Definitions section of the manual) the POTW
into the environment, either through the POTW's sludge or effluent, or by interfering (see the definition of
Interference) with the operation of the POTW Public health is protected by the Pretreatment Program
through the regulation of industrial discharges so that treatment plant and sewer maintenance personnel are
not exposed to toxic or flammable chemicals.
The inspector is usually the only person from the POTW who regularly appears at the industrial user's
facility. The inspector's presence dramatically symbolizes the POTW's role as a responsible public agency
observing the actions of the regulated industry. The knowledge that an inspection could occur unannounced
encourages industrial plant managers to keep their operations in compliance.
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Industrial User Inspection and Sampling Manual Introduction
Outline of the Guidance
The guidance is designed to lead the POTW inspector through the inspection and sampling process in a
step-by-step fashion. The Introduction has laid out the overall framework for conducting site visits at
industrial users. Chapter Two of the manual presents a chronological outline for conducting an inspection at
an industrial user, beginning with the pre-inspection activities, such as the preparation and entry
considerations; and then covers the on-site activities of the inspector, including: pre-inspection observations,
the opening conference or initial meeting at the facility, the records review process, observations and
illustrations, and the closing conference or exit interview conducted by the inspector. Finally, follow up
activities by the POTW (e.g., inspection report writing and enforcement actions) are discussed.
Chapter Three of the manual presents a detailed framework for conducting sampling at the industrial
user. This chapter covers: the objectives of sampling, pre-sampling considerations (e.g.. a sampling plan),
special sampling requirements (e.g., cyanide sampling at Electroplating facilities), analytical methods, use of
automatic sampling devices, flow measurement, and quality assurance/quality control considerations.
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II. INSPECTING INDUSTRIAL USERS
Introduction
Developing and Maintaining an IU Survey
Frequency of Inspection and Sampling
Types of Inspections
Confidential Business Information
Responsibility of the Inspector
Inspector's Field Notebook
Pre-lnspection Activities
Pre-lnspection Preparation
Review of Facility Background Information
Developing an Inspection Plan
Safety and Sampling Equipment Preparation
Notification of the Facility
Entry to the Industrial Facility
Legal Basis For Entry
Arrival for the Inspection
Reluctance to Give Consent
Uncredentialed Persons
Access to Federal Facilities
Denial of Consent to Enter
Withdrawal of Consent
Denial of Access to Parts of the Facility
Covert Sampling in Response to Denial of Entry
6
7
7
8
9
11
14
16
22
Conducting an Inspection Under a Warrant 28
Pre-lnspection Checklist 29
Pre-lnspection Observations 29
Information to be Collected Prior to and During the Inspection 31
On-Site Activities
Opening Conference
Inspection Procedures
Physical Plant Review
Self-Monitoring Review
Operations Evaluation
Maintenance Evaluation
Records Review at the Industrial User
Obtaining Copies of Necessary Records
Record Identification Procedures
Closing Conference
Follow-Up Activities
Inspection Report
Inspection Checklist
32
45
48
INTRODUCTION
This chapter presents a framework to be used by POTW personnel when conducting on-site inspections at
industrial facilities that discharge or have the potential to discharge process wastewater to the POTW. The
principal intent of this chapter is to assist POTW personnel in planning, collecting, and documenting
sufficient information to determine compliance or noncompliance, particularly by all SlUs, with all applicable
Federal, State, and local pretreatment standards and requirements. New POTW inspection personnel are
encouraged to read and understand the material presented in this chapter before beginning any inspection
activities.
This chapter begins with a discussion of general inspection topics such as: developing and maintaining an
industrial user survey; criteria to be used in setting the frequency of inspections and sampling activities; the
types of inspections which can be used by the POTW; how to handle confidential business information; the
general responsibilities of the POTW inspector; and the use of an inspector's field notebook. Once this
groundwork has been laid, a detailed discussion of specific inspection activities follows. The topics covered
in this discussion include: pre-inspection activities; on-site activities; and follow up activities. Also included
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Industrial User Inspection Manual Chapter 2 - Inspecting Industrial Users
at the end of the chapter is an inspection checklist which can be used by the inspector as the basis for the
inspection report.
Each of these activities of the inspection (i.e., general, pre-inspection, on-site, and follow up activities)
are discussed in greater detail in the sections which follow, but first, the need for developing an industrial
user survey is discussed.
DEVELOPING AND MAINTAINING AN INDUSTRIAL USER SURVEY
All permitting, compliance monitoring and enforcement activities which the POTW undertakes are
derived from an accurate identification of the regulated industrial users in the POTW's system. Therefore, it
is imperative that the POTW maintain an up-to-date listing of each IU which discharges to the POTW. Once
this list is established, the POTW should update this information periodically (sources of information and
techniques for updating this information include: checking with the local Chamber of Commerce for new
businesses, reconnaissance drive-throughs of the POTW district by POTW personnel, newspapers, applications
for water service, yellow book advertising, building permits, etc.). For Significant Industrial Users (SlUs), the
POTW is required to update this list annually as part of its Pretreatment Performance Report to the State or
EPA. This list provides the basis for developing a plan for scheduling site visits at SlUs. The schedule for
site visits should be contained in a neutral inspection plan (discussed later in this chapter) which should be
developed by the POTW to guide its conduct of SIU site visits.
FREQUENCY OF INSPECTION AND SAMPLING
The General Pretreatment Regulations require POTWs to inspect and sample each SIU at least once each
year. This frequency was established as a minimum to represent the EPA's expectation for site visits to
facilities with good compliance histories. POTWs should develop a neutral inspection plan (discussed below)
to establish the criteria under which the POTW will conduct site visits at a frequency greater than the once
per year minimum. These criteria should be applied when the POTW schedules routine compliance
inspections for its IU universe. When considering how often to visit an industrial facility, the POTW should
consider (at a minimum) the following criteria:
- The industrial user's potential to adversely affect the POTW's operations (e.g., the type and/or
concentration of pollutants in the lU's discharge);
. The volume and variability of the discharge;
. Available resources and finances;
. The type and reliability of control methods used to achieve compliance;
. The quantity and nature of materials stored or in use and their relative risk of accidental spill;
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Industrial User Inspection Manual Chapter 2 - Inspecting Industrial Users
. POTW problems known or suspected to have been caused by the IU;
. A history of complaints, if any. at the facility;
. The facility's geographic location;
. The compliance history of the user;
. The period of time since the last inspection;
. The imposition of new or additional pretreatment standards and requirements; and
. Special considerations or circumstances such as seasonal production schedules or batch discharges at an
industrial facility.
For example, a large facility with a poor compliance history may be scheduled for monthly site visits.
On the other hand, a significant industrial user with a fairly consistent record of compliance, a cooperative
attitude toward the pretreatment program, and a relatively constant manufacturing process may need to be
inspected only once per year. When establishing an inspector's site visit schedule, adequate time must be
allotted to allow inspectors to prepare for each visit, document their findings in a site visit report, and conduct
other assigned duties.
The POTW should develop procedures to implement a neutral inspection plan for routine inspection and
sampling visits. A neutral monitoring scheme provides some objective basis for scheduling inspections and
sampling visits by establishing a system for setting priorities (whether a complex factor-based, alphabetical, or
geographic system) to ensure that industrial users are not unfairly selected for inspection or sampling. The
selection of which industrial users to inspect must be made without bias to ensure that the POTW can not be
challenged for operating its inspection and sampling program in either an arbitrary or capricious manner.
This plan should be included as part of the POTW's Enforcement Response Plan as well as included in the
POTW's automated tracking system (if available).
TYPES OF INSPECTIONS
Inspection and sampling activities at industrial facilities may be: I) scheduled, based on a neutral scheme;
or 2) on demand, usually in response to a specific problem or emergency situation, such as a spill at the
industry or an upset at the POTW. The POTW may use either of these inspection types when conducting a
site visit at an industrial user, but to satisfy the minimum inspection frequency established by the General
Pretreatment Regulations (40 CFR403.8(f)(2Xv)), the POTW must conduct a routine compliance inspection at
the ID (i.e., not a demand inspection, which may not have sufficient coverage to satisfy the regulatory
requirement).
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Industrial User Inspection Manual Chapter 2 - Inspecting Industrial Users
Scheduled inspections should be conducted according to the POTW's neutral inspection scheme. This
does not mean that the POTW must notify the facility prior to each scheduled inspection. On the contrary, a
routine compliance inspection is most effective when it is unannounced or conducted with very little advance
warning (M>ri;:when determining compliance with pretreatment standards, the ID should be in normal
operation to ensure the representativeness of the samples taken). The neutral inspection scheme should set the
criteria the POTW uses to choose which facilities to inspect, but the schedule for the actual inspection should
remain confidential and may be separate from the neutral plan. Demand inspections are usually initiated in
response to known or suspected violations, usually identified as a result of reviewing a self-monitoring report,
a public complaint, a violation of the POTW's NPDES permit requirements, POTW operating difficulties,
unusual influent conditions at the POTW. or emergency situations (e.g., sewer line blockages, tires, or
explosions) When emergency situations arise in the treatment system (including the collection system),
industrial inspections should be initiated immediately. Sampling is almost always a part of a demand
inspection because the purpose of the inspection is to identify or verify the source of a discharge causing
problems, and to gather information which might be used in a subsequent enforcement action. In some
instances, the POTW may want to notify other appropriate local agencies (e.g., the fire department, State
hazardous waste response team, the EPA. etc.) depending on the nature of the suspicion at the industry.
CONFIDENTIAL BUSINESS IN FORM4 TION
The very nature of inspections involves gaining access to and collecting information that companies
would not ordmariK make available to outsiders. When conducting compliance inspections, the inspector
may have to deal with claims of confidentiality. These claims are authorized under Section 308 of the
Federal Clean Water Act and are explained in the Code of Federal Regulations at 40 CFR Part 2. The
inspector is responsible for following proper security measures when handling inspection data, both while on
the road and in the office. Confidential business information includes trade secrets (including chemical
identity, processes, or formulation) that could damage a company's competitive position if they became
known to the public. Unauthorized disclosure of confidential information could result in criminal sanctions
against the inspector.
Any business being inspected has the right to claim all or any part of the information gathered during the
inspection as confidential. Information collected during an inspection is available to the public unless the ID
takes measures to have the information held as confidential. This information must be held in confidence
from the public, but this information must also be disclosed to the EPA upon request. The Control Authority
may. as a matter of policy, notify the business through the ID permit or by providing the local SUO to the
business of its right to claim confidentiality.
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Industrial User Inspection Manual Chapter 2 - Inspecting Industrial Users
The affected business must assert its claim of confidentiality at the time the information is submitted to
the POTW. If a claim of confidentiality is made after the fact, the POTW should make every effort to honor
such a claim, but is in no position to guarantee that the information has not already been distributed to the
public. The claim of confidentiality must be made in writing and signed by a responsible company official
(e.g., a president, vice president, treasurer, general counsel, or chief executive officer). While the business is
entitled to make a claim of confidentiality on all information which an inspector requests or has access to
while on site, claims of confidentiality should be subject to review by the POTW's counsel. A business may
not refuse (on the grounds that the information is considered confidential or a trade secret) to release
information requested by the inspector. The claim of confidentiality only relates to the public availability of
such data and is not to be used for denying access of a facility to POTW inspectors performing their duties
under State or local law. Confidential business information must not be disclosed to competitors or to any
other person who does not need to have access to the information to evaluate compliance with pretreatment
obligations (e.g., POTW compliance personnel). A determination of confidentiality should be made when
someone from the public requests the information which was claimed as confidential. At that time, the
POTW's legal counsel must determine if the information is. under State law. confidential information. The
POTW must have a process for safeguarding these materials until such a request is made, including having
locked file cabinets, designating responsible officials, etc. Federal law requires that information described as
"effluent data" (defined at 40 CFR Part 2.302(2X0) not be treated as confidential. Effluent data include any
information regarding the nature of the discharge to the sewer system.
In some cases, entry to a facility may be denied based on a claim that there is confidential information at
the facility. In such cases, the inspector should inform the industry of the relevant subsections of the State or
local law regarding confidentiality so that they are clearly understood b> all parties involved. The inspector
should then explain the procedures used by the POTW to keep information confidential. In this instance, it
would be helpful if the POTW had already notified the 1U of its right to claim confidentiality and the Ill's
response (assuming it acknowledges this right and agrees that information must be provided to the inspector
under the expectation that its claim will be honored by the POTW). If the facility representative still refuses
entry, the inspector should not contest the issue but should treat the matter in the same manner as any denial
of entry and follow established procedures for gaining entry (see discussion of Entry to the Industrial Facility
later in this chapter).
To understand claims of confidentiality, an inspector should know the types of information considered
confidential. The federal regulations specifically exclude certain types of information from confidential
treatment. In particular, this "public" information includes all "effluent data." Fffluent data include all
10
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Industrial User inspection Manual Chapter 2 - Inspecting Industrial Users
information necessary to determine the identity, amount, frequency, concentration, temperature, and other
characteristics (to the extent related to water quality) of :
. Any pollutant which has been discharged by the source (or any pollutant resulting from any discharge
from the source) or any combination of these Pollutants; and
. Any pollutant which, under an applicable standard or limitation, the ID was authorized to discharge
(including a description of the manner or rate of operation of the facility).
Effluent data may also include a general description of the location and/or nature of the source of pollutants
to the extent necessary to distinguish it from other sources of pollutants (e.g., a description of the device,
installation, or operation of the source). In general, information which is collected to determine the
compliance status of the industry is not considered confidential. It is the inspector's responsibility to handle
all material claimed as confidential according to established procedures. For more information on
confidentiality and the handling of confidential information, as well as on the right of entry to a facility for
inspections and sampling, the inspector should consult with the POTW's legal counsel.
The inspector should not sign any pledge of secrecy or confidentiality agreements or any agreement
which would limit the POTW's ability to disclose or use the information obtained while inspecting an IU.
Such secrecy agreements are not a precondition of entry to the facility and should not be signed by the
inspector. It is not appropriate for the inspector to determine whether an ILJ's claim of confidentiality is
justified. Once such a claim is made, the information must be kept confidential until a determination is made
by the POTW's legal counsel.
RESPONSIBILITIES OF THE INSPECTOR
The inspector's fundamental mission is to examine the environmental activities of a single regulated
facility. The site visit is the basic element that determines the quality of information available for
determining compliance and taking enforcement actions. The inspector must be knowledgeable about the
requirements that apply to the user (i.e., the industrial user permit, the SUO, and Federal categorical
standards) in order to determine the facility's compliance status. Local pretreatment program inspectors are
responsible for the following areas of conduct:
Legal:
POTW inspectors must conduct all inspection activities within the legal framework established under
State or local law. The inspector must be knowledgeable of the conditions established in the industrial
user permit, the local SUO, applicable National Categorical Standards, local limits, the General
Pretreatment Regulations, and any other applicable State or Local regulations, including any special
requirements regarding entry to the industrial facility.
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Industrial User inspection Manual Chapter 2 - Inspecting industrial Users
Procedural:
POTW inspectors must be familiar with general inspection procedures and evidence collection techniques
to ensure accurate inspections and to avoid endangering potential legal proceedings on procedural
grounds. These inspection procedures should be set forth in the local Enforcement Response Plan and
should address inspections, sampling, flow monitoring, and documenting the results of these activities in a
manner which enables the POTW to produce evidence which is admissible in a judicial action. The
standard sequence of activities for conducting inspections are outlined in detail in Table 2-1. These
procedural considerations are discussed further later in this chapter.
Evidence Collection:
POTW inspectors must be familiar with general evidence gathering techniques because the POTW's case
in a civil or criminal prosecution depends in part on the evidence which the inspector has gathered.
Inspectors must keep detailed records of each inspection. This information will serve when preparing the
inspection report, determining the appropriate enforcement response, and giving testimony in an
enforcement action. In particular, inspectors must know how to:
0 substantiate facts with items of evidence, including: samples, photographs, document copies,
statements from witnesses, and personal observations (but not opinions);
0 abide by chain-of-custody procedures;
0 collect and preserve data in a manner admissible in legal proceedings; and
0 testify in court and administrative hearings.
Inspection and sampling procedures are discussed in detail in this chapter and in chapter three of this
Manual.
The POTW inspector must follow safety procedures, including: dressing appropriately and wearing safety
clothing (e.g., steel toed shoes, hard hats, etc.), maintaining safety equipment in good working order, and
using safety equipment in accordance with any manufacturers specifications or label procedures. In
addition, the POTW inspector should follow the safety procedures established by the industrial user which
is being inspected, unless these procedures prevent the inspector from conducting the inspection.
Professional/Ethical:
POTW inspectors must perform their duties with the highest degree of professionalism. In dealing with
industry representatives, inspectors must be tactful, courteous, and diplomatic. The inspector is the
representative of the POTW, and is often the initial or only contact between the IU and the POTW. A
firm but responsive attitude should encourage cooperation and initiate a good working relationship with
industry. Inspectors should avoid any negative comments regarding any product, manufacturer, or person
while conducting their inspection. Inspectors should not accept gifts, favors, lunches, or any other
benefits under any circumstances. This might be construed as influencing the performance of their duties.
When evaluating the information obtained during the inspection, the facts of the inspection should be
developed and reported completely, accurately, and objectively.
Quality Assurance (QA) Responsibilities:
The inspector must assume the primary responsibility for ensuring the quality of the compliance data
obtained during the inspection. While other organizational elements play an important role in quality
assurance (see the discussion in Chapter 3), it is the inspector who must assure that all effluent data
generated by the POTW and introduced into the inspection file are complete, accurate, and representative
of conditions at the IU. To help the inspector meet these responsibilities, the POTW should develop a
QA Plan that identifies individual responsibilities and documents detailed procedures for ensuring the
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Procedural Respo
Pre-lnspection Preparation:
Establish the purpose and scope of the inspection;
Review all pertinent background information, including the ID permit and the permittee's
compliance tile;
Contact appropriate staff personnel responsible for the permittee: e.g., pretreatment coordinator;
Develop a plan for the inspection;
Prepare an\ documents and equipment necessary for the inspection;
Coordinate >our schedule with the laboratory if samples are to be collected;
Contact responsible part} for transporting samples and for packing'shipping requirements.
Re\ ie\s applicable categorical standards.
. Present official credentials and verbally identify oneself;
Manage denial or withdrawal of entry, if necessary.
Opening Conference or Meeting: (if applicable)
. Discuss inspection objectives and scope;
. Kstablish a working relationship with the industrial user
Facility Inspection:
Conduct visual inspection of the entire industrial facility;
Review industrial user records;
Inspect monitoring equipment and operations;
Review ha/ardous waste records;
Collect samples;
Review laboratory records for QA QC, monitoring data (flow, pH, etc.);
Review laboratory procedures to verify the use of approved methods;
Document inspection activities.
Closing Conference: (if applicable)
. Collect missing or additional information;
. Clarify questions and answers with facility officials;
. Review inspection findings and inform industry officials of follow-up procedures; and
. Issue a deficient-} notice, if appropriate.
Inspection Report:
. Organize inspection findings into a useful, objective evidence package;
. Include all deficiencies and required activities; and
. Prepare the narrative report, checklists, and documentary information, as appropriate.
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Industrial User Inspection Manual ( 'hapter 2 - inspecting Industrial Users
highest quality of sampling from the inspection. The objective of the QA Plan is to establish
standards that will guarantee that data obtained during the inspection or sampling event meet the
requirements of all users of that data (e.g., it must be able to be used by compliance personnel to
determine the compliance status of the facility, and it must be able to be used by the POTW in court
as admissible evidence in an enforcement proceeding). Many elements of QA are incorporated
directly into the basic inspection procedures and may not be specifically identified as QA techniques
by the inspector (e.g.. chain-of-custody procedures). The inspector must be aware that following
established inspection procedures is critical to the inspection program. These procedures should be
developed to reflect the following QA elements:
0 Valid data collection;
° Approved analytical methods;
° Standard data handling and reporting;
° Quality analytical techniques.
When conducting an in-depth inspection at an industrial user, POTW personnel are required to evaluate a
broad spectrum of activities at the facility. In some cases, the level of expertise for this evaluation may
exceed the qualifications of the inspector (e.g., when evaluating if appropriate analytical equipment is used or
conformity with the analytical procedures in 40 CFR 136). In situations where such an evaluation is part of
the inspection, the POTW should make available specially trained or skilled staff (e.g., analytical chemists) to
either assist in the inspection or to train inspectors in their areas of expertise. The POTW inspector should
have the necessary knowledge and skills for conducting effective IU inspections, but these skills and expertise
may be supplemented by other POTW or contractor staff. The general skills and knowledge which POTW
inspectors should have are outlined in Table 2-2.
INSPECTOR'S FIELD NOTEBOOK
providing strong documentary support of discrepancies uncovered in an inspection (e.g., conditions at the
plant are found to be different than described in the permit application, the BMR, slug control plan, etc...) is
one of the inspector's basic responsibilities. The core of all documentation taken by the inspector at the ID is
contained in the inspector's field notebook, which is intended to provide accurate and inclusive documentation
of all inspection activities. It is important for the information contained in the field notebook to relate exactly
to the conditions observed by the inspector at the facility. The field notebook should not contain opinions or
any observations not supportable from the facts of the inspection Normally, field notes will be written in a
field notebook and/or on a prepared report form developed by the POTW (or the inspector may use the
enclosed checklist) to ensure that all pertinent information is collected. The field notebooks used by the
inspector should be bound, to be sturdy enough to last through several inspections, and information should be
recorded in permanent ink. It is important that the information obtained during the inspection be retained in
the inspection notebook for a long time, because the information contained in the notebook might be used in
an enforcement action years later. The POTW's legal counsel should be consulted for advice on preparing
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Industrial User Inspection Manual
Chapter 2 - Inspecting Industrial Users
Pretreatment inspectors should have the following knowledge and skills:
Knowledge of Federal, State and local regulations and requirements.
Know ledge of toxic constituents in industrial waste discharges.
• Knowledge of the Federal Categorical Pretreatment Standards.
• Knowledge of all local limits developed by the POTW.
• Knowledge of industrial processes and where wastestreams are generated.
Knou ledge of spill control procedures.
Know ledge of wastewater treatment technology.
• Know ledge of w astewater sampling methods.
Know ledge of w astewater analytical methods.
Knowledge of flow measuring techniques.
• Know ledge of and ability to identify safety hazards associated with pretreatment control.
• Knowledge of and ability to practice professional ethics.
Abilit) to inspect waste treatment facilities and verify conformance with specifications.
Abilit) to evaluate and select monitoring locations.
Abilit) to deal tactfully and effectively with industry representatives.
• Ability to maintain accurate records and write clear and concise reports.
• Abilit) to read and interpret mechanical construction drawings and pipeline schematics.
• Abilit) to keep confidential information and trade secrets.
• Abilit) to understand other viewpoints and work with industries and other regulatory agencies.
Abilit) to prepare and maintain proper files and documentation on work performed.
Abilit) to understand and carry out procedures on confidentiality developed by the POTW.
notes so that they ma\ be read or introduced as evidence in an enforcement proceeding.
Since an inspector may be called to testify in an enforcement proceeding, it is imperative that each
inspector keep detailed records of inspections, investigations, samples collected, and related inspection
information. The types of information that should be entered into the field notebook include:
. Obsenations: All conditions, practices, and other observations that will be useful in preparing the
inspection report or that will validate evidence should be recorded;
. Documents and Photographs: All documents taken or prepared by the inspector such as the completed
checklists for the inspection report should be noted and related to specific inspection activities.
(Photographs taken at a sampling site should be listed and described).
. Unusual Conditions and Problems: Unusual conditions and problems should be noted and described in
detail, and
. General Information: Names and titles of facility personnel and the activities they perform should be
listed along with statements they have made and other general information. Weather conditions should
be recorded (e.g., raining or clear). This information can be used to determine if storm water is being
discharged to the sanitary sewer. Information about the facility's record keeping procedures should be
noted since it may be useful in later inspections. Information on who was interviewed and what those
individuals said are important pieces of information for the inspector's notebook.
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Industrial User Inspection Manual Chapter 2 - Inspecting Industrial Users
PRE-INSPECTION ACTIVITIES
Pre-inspection activities are crucial for conducting efficient and effective inspections because they provide
a focus for the on-site inspection activities. By carefully planning the inspection activities, the inspector will
not waste time on-site deciding what needs to be accomplished and how to obtain all of the necessary
information. This background work should be completed at the POTW so that inspectors can use their time
efficiently when they arrive at the facility. An inspection and sampling program begins even before the
inspector goes out into the field. A good inspection begins with planning. Generally, a significant amount of
time should be devoted to planning the inspection and on follow up activities to the inspection. Planning
begins with the thought process by which the inspector identifies all activities relating to the inspection, from
its objective (purpose) through its execution (actual conduct) and follow-up. Pre-inspection preparation is an
essential element of conducting high quality inspections. By knowing "why" the facility is being inspected,
"what" should be looked for, "how" it will be found, and "where" attention should be focused, the inspector
will make the most efficient use of field time and ensure that the appropriate information for subsequent
compliance or enforcement purposes is collected. By the time the inspector goes into the field, he or she
should:
. Have a clear idea of the objective for the inspection (e.g., investigation of a reported spill or
complaint, routine compliance inspection, etc.). The objective will define the scope of the inspection
(i.e., the range of activities to be conducted during the inspection). The objective will depend on
what type of inspection is being conducted (i.e., scheduled, or demand);
. Know all applicable program regulations (federal and local), compliance history, and physical layout
of the site to help define the scope of activities the inspector will undertake at the facility;
. Know the Standard Operating Procedures (SOPs) for the type of inspection activities to be conducted
(again, these activities will be determined by the objective of the inspection). It is recommended
that all Control Authorities adopt written SOPs. SOPs are a document or set of documents which
explain, in step-by-step detail, how an inspection should be conducted (e.g., it defines who will be
interviewed; what types of questions will be asked; how a specific type of sample will be collected;
cleaning procedures for sample collection equipment and sample bottles; calibration methods for pH
meters, D.O. meters, and conductivity meters, etc.; identification of the correct equipment, materials
and techniques for conducting the inspection and for collecting, preserving, and documenting
samples and other evidence; and any additional activity which the POTW conducts related to
inspections or sampling). This manual will provide many of the details needed by POTWs to
establish SOPs for their inspection activities; and
. Know the safety plan for protecting all members of the inspection team from potential hazards or
harmful exposures on site.
This section will describe the elements and procedures that go into pre-inspection planning, both those
related to general field activity and the facility inspection itself. In this section, we will concentrate on the
"why" and "what" of pre-inspection planning; detailed discussion of the "how to's" of some of the key
elements of planning (e.g., how to develop a quality assurance plan for samples) will be found in later
chapters.
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Industrial L'ser Inspection Manual C'hapter 2 - Inspecting industrial Users
Pre-Inspection Preparation
Pre-inspection preparation can be broken down into the following activities: reviewing facility
background information; developing an inspection plan; safety and sampling equipment preparation; and
notifying the facility (if appropriate). Each of these will be discussed in turn.
Review of Facility Background Information:
To plan effectively and ensure the overall success of an inspection, it is essential that the inspector
collect and analy/.e any available background information on the candidate facility. By reviewing background
information, the inspector can minimize the inconvenience to the ID caused by requesting information which
has already been submitted. Avoiding this situation increases the regulatory credibility of the POTW. The
inspector must Jet'.- -:,ne the amount of background information necessary for the inspection and in collecting
this information should focus on the characteristics which are unique to the targeted facility, e.g., design and
physical layout, historical practices and compliance status, legal requirements, etc.. The types of information
which might be important for the inspector to review are listed in Table 2-3. A summary of this information
may be kept in a separate file or filed with the final inspection report for each IU so that it is conveniently
available for any subsequent inspection.
The inspector can find the majority of the information described in Table 2-3 in the permit application
and permit of the industrial facility (for a review of permit requirements and application information, refer to
the Industrial User Permitting Guidance Manual September. 1989). the POTW's Industrial Waste Survey, the
BMR and 90 Da> Compliance Reports, Periodic Compliance Reports, and information learned by the
inspector from previous visits at the facility. The industrial user permit should clearly identify all of the
responsibilities and obligations of the industrial user in a single document. The permit should provide
information on all applicable effluent Itmitations (Federal categorical standards, prohibited discharge
standards, and local limits), requirements and restrictions applicable to all discharges from the facility; slug
control plans; monitoring, record keeping and reporting requirements; sampling location; type of samples to
be taken; and required analytical methods (i.e., methods approved in 40 CFR Part 136). The permit
application and BMR should outline the general facility information by describing the facility and providing
site plans and layouts of the process areas and other areas of concern. The application should also include all
contact persons as well as production levels and flow data from the facility. The previous inspection report
for the facilit) will identify areas of concern from the last inspection which required action on the part of the
IU. The inspector should review this report carefully and follow up on any progress in addressing any
problems previously identified.
When the facility to be inspected is a categorical industry, the inspector should review any appropriate
guidance from the U.S. EPA regarding that particular category to become familiar with the specific industrial
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industrial User Inspection Manual Chapter 2 - Inspecting Industrial Users
Table 2-3
Information to Review Prior to the Inspection
General Facility Information:
Previous inspection report(s) (determine if there were any previously identified problems which
needed to be addressed by the ID);
Maps and schematics: showing the facility location, wastewater discharge pipes (i.e.. flow
schematic), and geographic features (e.g.. topography);
Names, titles, and telephone numbers of responsible facility officials;
Any special entry requirements, e.g.. safety equipment (steel toed shoes, hard hats, etc.)
Nature of the IU processing operations and wastewater characteristics:
General layout of the facility;
Production levels - past and present (especially for facilities regulated by production based
categorical standards (e.g., aluminum forming);
Changes in facility conditions since the last inspection or permit application (e.g.. expansion of the
facility);
Water use data;
SID slug control plan;
Raw materials used in production processes;
Location of storage sites for raw materials;
Special permit conditions (e.g., peak flow restrictions, regulation of unusual substances);
Progress toward meeting any applicable compliance schedule;
Sources, volumes, and characteristics of the waste discharges;
Aerial photographs (if available).
Requirements, Regulations, and Limitations:
Copies of all applicable Federal, State and Local regulations and requirements, including any joint
agreements or multi-jurisdictional agreements;
Copy of the industrial user's permit and permit application; and
Any applicable compliance schedule which the industry might be under.
Facility Compliance and Enforcement History-'
Any correspondence between the facility and Local, State or Federal agencies;
Documentation on past violations of permit requirements or compliance schedules (available from
the POTW's data tracking system);
Self-monitoring data and reports;
Post inspection reports;
Past notices of violation (NOV), or other enforcement correspondence between the facility and the
POTW; and
Laboratory capability and analytical methods used by the industrial user's lab (if applicable).
Wastewater Treatment Systems:
Description and design specifications for the wastewater treatment process employed at the
industrial user;
. Process description, specifications, and schematic diagram;
. Available bypasses for existing pretreatment systems (if applicable):
. Type and amount of wastes discharged; and
• Spill control and contingency plans.
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Industrial User Inspection Manual Chapter 2 - inspecting Industrial Users
processes to be inspected. A list of all pretreatment-related guidance documents is found in Appendix XII.
In addition, the inspector should become familiar with the EPA issued Development Documents associated
with each industrial category' to become more acquainted with the manufacturing processes, wastewater
characteristics, as well as treatment technology at these categorical industries.
DevelopinE an Inspection Plan:
The development of a sound inspection plan prior to going on-site is as important to the success of the
POTW's inspection efforts as the on-site activities themselves or the preparation of a high-quality, well-
documented inspection report. Inspection plans should be flexible enough to adapt to unanticipated situations
encountered at the site, but the plan should also be designed as an organized approach to guide the conduct of
the inspection. The basic purpose of the plan is to provide the inspector or inspection team (if appropriate)
with a step-by-step guide to collecting relevant evidence about a facility's procedures and practices that are to
be observed during the inspection. All inspection activities (i.e., its scope) are derived from the inspection's
objective(s) (i.e., why the inspection is taking place). The objective(s), in turn, depend on the reason for
conducting the inspection (i.e.. to conduct a routine compliance evaluation, to follow up on information from
a previous inspection, to investigate a complaint, or in response to an emergency situation). The inspection
plan clarifies each of these areas (the inspection's objective, scope and activities) for each type of inspection.
The basic components of the inspection plan should cover the following areas:
. The purpose of (i.e., reason for) the inspection: a brief history of why the inspection is taking place
and the inspection objectives (i.e., what goal is to be accomplished). This will depend on the type of
inspection taking place.
. The scope of the inspection (i.e., what range of activities need to take place to fulfill the objectives
of the visit (NOTE This may change in the Held, since some of the best evidence may be
unanticipated by the inspector. The inspector must be flexible enough to adapt to new unanticipated
situations in the field);
. The inspection standard operating procedures (SOPs) and associated rationale for these activities
(i.e., which field and analytical techniques will be used to collect what information; what record
keeping systems will be reviewed; which ID personnel will be interviewed; which samples will be
collected; and for each step, why).
. The definition of team task assignments and time scheduling (if applicable);
. Resource requirements (costs and time) based upon the planned activities and time allowances;
. What kinds of evidence should be collected and documented in field log books.
. A Quality Assurance Plan, where necessary; and
. , safety contingency plan, where necessary.
The investment of time required to produce a quality inspection plan is worth the effort because it
constitutes a "walk-through" of the facility for the particular inspection type that should save time and
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Industrial User Inspection Manual Chapter 2 - inspecting Industrial Users
resources during the actual inspection. The inspector must be clear on what questions are appropriate to
address during the inspection, and the plan provides a framework for working through these issues prior to
visiting the site. POTWs should develop standard operating procedures and/or inspection checklists that are
incorporated as part of the inspection plan. The checklist at the end of the chapter can be used for this
purpose, and it can form the basis of the POTW's SOPs for a comprehensive compliance inspection. It is still
important, however, to be clear as to which elements will be the focus of the inspection. Once this plan is
developed for each facility and each type of inspection, it can used for each subsequent inspection without
revision, unless circumstances at the plant change significantly. If there are significant changes at the ID, a
new inspection plan may need to be developed The general components of such a plan are outlined in Table
2-4.
Safety and Sampling Equipment Preparation:
After the background information for an ID has been gathered and reviewed, and a plan for the
inspection has been developed, POTW personnel should review and check the types of equipment which are
necessary to meet the objectives of the site visit. An inspector must carry enough equipment to gather the
necessary information during the inspection. This part of the pre-inspection process involves obtaining and
preparing the equipment necessary for the inspection. The necessary types of equipment may van with the
nature of the ID and the types of activities to be performed by the POTW during the inspection. For
example, if sampling is to be performed during the inspection, sampling equipment, and possibly additional
safety equipment would need to be prepared. All equipment must be checked, calibrated and tested prior to
each inspection. The inspector must also ensure that all materials necessary for the inspection are taken to the
inspection site. Safety procedures and equipment for a facility will be based on past experience at the
facility, or, for new facilities, the facility's response to the POTW's letter requesting such safety information
(such a letter is recommended for all new facilities). Safety requirements must be met to ensure the
inspector's safety and to help ensure that the inspector is not denied entry to the facility or parts of the
manufacturing operations.
Notification of the Facility:
Most inspections will not involve notice to the affected facility. This is especially true when the POTW
has established a working relationship with the IU, and its personnel are known at the facility. Also,
notification should not be given to the facility when illegal discharges or improper records are suspected or
the POTW wants an accurate picture of "normal" operations. The concern that physical conditions may be
altered before the inspection or that records may be destroyed or altered justifies an unannounced visit to the
facility. Likewise, a "demand" inspection (i.e., an inspection conducted as a result of a spill at the IU or
upset at the POTW) can not be planned in advance. The POTW must be ready to conduct these types of
inspections on very short notice and at any time of the day or night.
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Industrial User Inspection Manual Chapter 2 - Inspecting Industrial Users
TaUt2-4
"Generic" Elements of an Inspection Plan
- Objectives (Purpose)
0 What is the purpose of the inspection?
0 What is to be accomplished'!
• Tasks (Scope)
0 What records, tiles, permits, regulations will be checked?
0 What coordination \s ith laboratories, attorneys, other programs (e.g.. solid waste or public health)
is required?
0 What information must he collected?
• Procedures
0 What specific facility processes will be inspected?
0 What procedures will be used?
° Will the inspection require special procedures?
0 Has a QA QC plan been developed and understood?
0 What equipment will be required?
° What are the responsibilities of each member of the team (if applicable)?
• Resources
0 What personnel will be required?
° Has a safet) plan been developed and understood?
• Schedule
° What will be the time requirements and order of inspection activities?
0 What will be the milestones? What must get done vs. what is optional?
In some instances, the 111 may be notified that it has been scheduled for an inspection by the POTW.
The time frame for this notification is up to the POTW. Notification of the ID prior to visiting the facility is
used primarily before inspecting an II' for the first time, so that plant officials are prepared to conduct a tour
of the facility to familiari/e the POTW uith the Ill's operations. If coordination with the IU is necessary for
the inspection (e.g., to ensure that appropriate plant personnel are present), then the POTW may notify the
facility of the exact date of the inspection and request that certain ID personnel be present. This notification
may also inform the POTW of its rights to claim confidentiality of the information obtained during the
inspection, but any confidentiality claim should be reviewed by the POTW's counsel at the time a request for
the information is made by the public (sec the Confidential Business Information discussion earlier in the
chapter for a more detailed discussion of this matter).
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Industrial User inspection Manual Chapter 2 - Inspecting Industrial Users
ENTRY TO THE INDUSTRIAL FACILITY
The POTW's ability to conduct an inspection at a regulated facility stems from its authority to enter the
ILTs premises. Proper, lawful entry onto an inspection site is crucial. Failure to adhere to the requirements
for exercising the POTWs entry authority could jeopardize any enforcement actions, and may subject the
inspector to liability. Any evidence that may have been collected from an inspection where proper entry was
not followed could be ruled inadmissible in an enforcement proceeding because it was obtained unlawfully.
This section discusses the legal basis for entry onto an IlJ's premises. It is always desirable to enter an
Ill's facility with the consent of the plant personnel, but there may be circumstances where such consent is
not granted, or consent to enter particular areas of a facility may be denied. In situations where consent is
denied, or where consent is withdrawn part way through an inspection, it will be necessary to follow certain
procedures to ensure the legality of the inspection. This section covers both of these situations and explains
what procedures should be followed by the inspector when consent is not granted to conduct or continue the
inspection.
Legal Basis for Entry:
The authority to enter an Ill's premises to conduct a compliance inspection comes from State or local law
(usually the local sewer use ordinance). When a POTW is Identified as required to have an approved
pretreatment program, its legal authority is thoroughly reviewed by the HP A or State prior to any "approval"
of that program. An approval from the L:PA or State means that the POTW has the necessary authority under
State and/or local law to implement all facets of its local program, including inspections. Usually, a local law
authorizes the conduct of inspections and vests that authority with the Superintendent of the POTW or their
designated representative. The designated representative is then allowed to enter, inspect, review records and
sample at an industrial facility. If the Superintendent's designated representative (i.e., the POTW inspector) is
allowed to inspect, he or she is usually required to present proper credentials prior to entering the facility. An
inspector's credentials are his or her proof of authority to enter and inspect a facility, and should always be
presented when entering the facility.
There may be times when the POTW may wish to inspect a non-discharging facility (e.g.. if the POTW
suspects that the non-discharging facility has commenced a discharge without a permit, or if the POTW
desires to ensure that no discharge is occurring at the facility). Under these circumstances, the same authority
which allows the POTW to enter the premises of discharging facilities should enable the POTW to gain
access to the non-discharging facility. Of course, if the facility refuses entry, fur whatever reason, the POTW
has the same recourse as with any other facility, i.e., seek a warrant to enter the premises. In this case, the
POTW should follow the Denial of F-ntry procedures outlined in this manual.
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Industrial User Inspection Manual Chapter 2 - inspecting Industrial Users
In some instances, the POTW employs an independent contractor to perform all or a certain aspect of the
inspection or sampling at the industrial facility. POTW personnel should consult with their legal counsel to
ensure that the POTW may, in fact, designate such contractor personnel as inspectors. This designation must
be made in accordance with State or local law. The POTW should be aware that contractors may not perform
functions which are inherently governmental (e.g.. determining compliance, initiating enforcement action,
etc.). All inspectors (whether POTW or contractor) must follow the POTWs written procedures for
inspecting and sampling, and the POTW must be the ultimate authority when compliance determinations are
made or policy decisions which affect the conduct of inspections or sampling.
The right of the government (Federal, State or Local) to enter an industrial facility and the protection
against unlawful entry by the government has been the subject of numerous court decisions. These court
decisions influence the manner in which a POTW inspector may enter a regulated facility. Several decisions
by the Supreme Court pertaining to the right to enter and the use of warrants for entry have bearing on the
POTW inspection process because these decisions define the limitations under which a POTW inspection may
lawfully gain entry to a regulated industry. The principal court case dealing with these issues is Marshall v.
Barlow's, 436 U.S. 307 (1978). Under this decision, the court concluded that where consent for the
inspection was not voluntarily given by the facility, the inspector is required to obtain an administrative
warrant to gain lawful entry. The court held that an inspector is not permitted to enter the non-public areas of
the worksite without either the owner's consent or a warrant.
The court further established the conditions under which a civil or administrative warrant can be issued
by a judge or magistrate. These conditions are: 1) reasonable cause to believe that a circumstance (e.g., a
violation) addressed by a statute or ordinance (for a POTW this would be a State statute and/or local
ordinance) had 2) that the facility to be entered was identified and selected by the POTW based on a pre-
existing administrative plan or scheme for entries. The basis for the "plan" or "scheme" was required by the
court to be "neutral". The message of the court was simply that the government (Federal, State and Local),
through its field agents, cannot "pick on" regulated facilities with subtle harassing techniques or through the
exercise of entry, search, inspection, investigation, or correctional rights or powers. The appropriate exercise
of government authority is not to threaten an industry. This is why it is important that the POTW develop an
inspection plan which is based on "neutral" conditions (e.g., geographical location) and to stick to this plan
when conducting site visits or to conduct the inspection when there is a justified suspicion of a violation.
The procedures which an inspector should follow when entry is denied are discussed in detail below.
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Industrial User Inspection Manual Chapter 2 - Inspecting Industrial Users
There are two important exceptions to the limitations described above. In these two situations, there is a
right to entry without a warrant, as discussed below:
Emergency Situations: such as potential imminent hazard situations, as well as situations where there
is potential destruction of or where evidence of a suspected violation may disappear if time is permitted
to elapse while a warrant is obtained. In an emergency, when there is insufficient time to obtain a
warrant, a warrantless inspection is allowed. The POTW will have to exercise considerable judgment
as to whether a warrant should be served when dealing with an emergency situation. However, even in
emergency situations, the POTW would probably need the assistance of the police, sheriff, or fire
department to gain entry. During the time it takes to get this assistance, a warrant could probably be
obtained if there is close coordination with the POTWs legal counsel.
. "Open Fields" and "In Plain View" situations: Observations by an inspector of things which are in
plain view (i.e., they can be seen by anyone in a lawful position or place to make such observations)
do not require a warrant. For example, an inspector's observations from the public area of a facility or
even from certain private property not normally closed to the public, are also proper and valid.
Further, even when a warrant is obtained for entry, those areas outside of the warrant's scope are also
"in plain view" so long as the warrant permits the inspector to be where they are when they make such
viewing.
The inspector's authority is usually not limited to entering and examining the industry's treatment plant
(effluent sources) alone. The inspector may inspect other areas of the permitted facility as well. The
inspector should consult with the POTWs counsel to ensure a complete knowledge of the local law which
authorizes their activity. Coordination with the POTWs counsel is also important when situations arise
where entry is denied. Under these circumstances it may be necessary to contact the POTWs legal counsel
to gain entry into the facility.
Arrival for the Inspection
The inspector should enter the industrial facility in the following manner to avoid any "unreasonable
search" or procedural problems:
• Arrive during normal business hours, unless it is an emergency situation or if other arrangement have
been made with the industry;
. Enter the facility through the main gate, unless the facility has designated another point for entry;
. Locate the "person in charge" at the facility as soon as possible. Consent to enter the facility must be
given by the owner or operator, or their designated representative. The inspector should learn who this
individual is and develop a working relationship with that person. The inspector may want to have
several industry contacts to grant entry in case the primary contact is not available. As long as the
inspector is allowed to enter, the inspection is considered voluntary and consensual. A clear expression
of consent is not necessary because an absence of an expressed denial is considered consent. If there is
only a guard at the entrance, the inspector should present their credentials (if no credentials are issued
by the POTW a business card should suffice) and suggest that the guard call his or her superior or the
responsible industry representative. The credentials indicate that the holder is a lawful representative of
the POTW and is authorized to perform pretreatment inspections. These credentials are important
documents and should never leave the sight of the inspector.
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Industrial User Inspection A ftinuul Chapter 2 - Inspecting Industrial Users
If the facility provides a blank sign-in sheet, log, or visitor's register, it is acceptable for the inspector to
sign it, as long as there is no restrictive language associated with it. The inspector must not sign any type of
"waiver" or release from liability form that would limit in any way the ability of the POTW to use the
information obtained during the inspection. The inspector must not agree to any such restrictive condition of
entry. In addition, the inspector must not sign any safety or personal harm waiver absolving the facility of
any injury which the inspector may incur while on-site. If the industry insists on such a waiver, the inspector
should politely explain that they cannot sign and request a blank sign in sheet. In some instances, it may be
possible to simply cross out the offensive language before signing, obtain a photocopy and make a note in
your field notebook about it. If the inspector is refused entry because they do not sign the release, they
should leave and immediately report all pertinent facts to their supervisor or. preferably, the POTW's legal
staff. All events surrounding the refused entry should be fully documented, and problems should be discussed
cordially and professionally. Officials at the regulated facility must not be subjected to any form of
intimidation or threats for their failure to allow an inspector entry to the premises. The inspector's authority
to inspect should not be abused, nor should the IL"s right to refuse entry be attacked. Keep in mind that the
inspector is at the facility to conduct an inspection, not to see a specific individual. If the normal contact is
not in, the inspection should not be postponed.
The POTW inspector cannot be required to take a facility's safety training course prior to entry, but if the
company has a relatively short safety briefing that will not interfere with the inspector's ability to complete
the planned inspection, it may be worthwhile to attend.
Reluctance to give consent. The receptiveness of facility officials toward inspectors is likely to vary
from facility to facility. Most inspections will proceed without difficulty. Because monitoring may be
considered an adversarial proceeding to some industries, the inspector's legal authority, techniques, and
competence may be challenged. If consent to enter is flatly denied, the inspector should follow the denial of
entry procedures outlined below. In other cases, officials may be reluctant to give consent for entry because
of misunderstandings of responsibilities (e.g., officials may feel that the inspection is part of an enforcement
proceeding against the company), inconvenience to the firm's schedule, or other reasons that may be resolved
through diplomacy and explanation on the part of the inspector.
One of the typical obstacles encountered by the inspector is a receptionist refusing entry because the
inspector does not have an appointment. In this case, remind the receptionist that you are not there to see a
specific individual but to inspect the facility. If entry is still refused, ask to speak to the environmental
manager or owner of the facility. If that does not work, follow the denial of entry procedures outlined below.
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Another common obstacle is the statement, "There is nobody here who can authorize the inspection." In this
instance, ask to speak to a supervisor, or show the receptionist the section of the sewer use ordinance which
authorizes the inspector's access to the facility. Do not threaten legal action, but clearly state your intent to
inspect. Be professional, assertive and persistent, but if you still cannot gain entry, follow the denial of entry
procedures outlined below.
Whenever there is difficulty in gaining consent to enter, inspectors should tactfully probe the reasons and
work with officials to overcome any problems. In any instance where there is a misunderstanding or conflict
due to the inspection, the inspector must avoid threats, inflammatory discussions, or language which would
deepen the antagonism. The inspector should be aware of their personal safety during such confrontations
and avoid actions which may enrage an individual who is irrational. If the situation is beyond the ability or
authority of the inspector to manage, the inspector should leave and consult with the POTW's legal counsel.
Uncredenlialed persons accompanying the inspector. The consent of the owner or agent in charge
(i.e., industry representative) must be obtained for persons accompanying an inspector to enter a site if they
do not have specific authorization (e.g.. acting as an agent of the POTW). If consent is not given, such
individuals may not enter the premises. If consent is given, these individuals may not view confidential
business information unless officially authorized for access.
Access to Federal facilities requiring security clearances. Certain Federal facilities, including those
with military, intelligence or nuclear-related activities may have special security or access requirements due to
the facility's mission of national security. POTW inspectors have the right to gain access to these facilities to
the same degree they have authority to enter any industrial facility which discharges to their system, but it is
necessary for POTW personnel to comply with any special entry requirements. POTW inspectors must obtain
the appropriate clearances for access to national security information, facilities or restricted areas at Federal
facilities. Where compliance information has been classified, restricted or protected for national security, all
information is to be maintained in accordance with the originating Agency's (e.g.. DOD) requirements. This
information should be treated as confidential business information and protected to the same degree as other
CBI (e.g.. access to this information should be under lock and key with only authorized personnel having
access to the key). The POTW should contact the EPA Regional office (Pretreatment Coordinator - see the
list of Regional Pretreatment Coordinators in Appendix XI) to get information on how to obtain these security
clearances. Obtaining top level security clearances can take up to one year, so you should plan ahead to
avoid unnecessary delays. In the interim, it may be necessary to contact the EPA Regional Office for
assistance in conducting inspections at these facilities.
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Denial of Consent to Enter. If an inspector is refused entry into a facility to conduct their inspection
under an appropriate State or Local law, the following procedural steps should be taken:
• Present Credentials. Make sure that all credentials have been presented to the facility owner or agcnt-
in-charge;
• Tactfully Discuss the Reason for Denial. If entry is not granted, courteously ask why.
Diplomatically probe the reason for the denial to see if obstacles (such as misunderstandings) can be
resolved. If the resolution of these conflicts is beyond the inspector's authority, he or she may suggest
that the facility officials seek advice from their attorneys regarding a clarification of the POTW's
inspection authority and right of entry;
• Carefully Record Observations in Your Field Logbook. All observations pertaining to the denial
should be noted carefully in the inspector's field logbook. Specifically, note the following:
0 Facility name and exact address;
0 Name, title, and authority of the person who refused entry;
0 Name, address, and telephone number of the facility's attorney (if readily available);
° Date and time of refusal;
0 Reason for the denial; and
0 Facility appearance (e.g., neat and orderly, or chaotic);
All of this information will be helpful in case a warrant is sought.
• Avoid Threatening or Inflammatory Statements. Under no circumstances should the inspector
discuss potential penalties or do anything that may be construed as coercive or threatening. For
example, the POTW has the right to ask for a warrant under normal circumstances. Therefore, refusal
to permit entry to conduct the inspection is not likely to lead to any action against the industry,
providing that the refusal was based on the inspector's lack of a warrant and there isn't an emergency
situation as described above. If the inspector were allowed to enter the facility based on a threat of
enforcement liability, it is likely that any evidence obtained through such an inspection would be
deemed inadmissible in an enforcement proceeding.
On the other hand, an inspector may inform the facility representative that he or she intends to seek a
warrant to compel the inspection. However, the inspector should be careful how this statement is
phrased. Do not state: "I will get a warrant." If an enforcement action is brought against this facility
using the information obtained in that inspection, a reviewing court may feel that the above statement
usurped the court's authority to authorize a warrant and may deny the warrant. Even if the company
later consents to the inspection following a statement that the inspector will get a wan-ant, there may be
an issue as to whether consent was coerced. If the inspector decides to make a statement regarding a
warrant, it should be phrased similar to: "1 intend to seek (or apply for) a warrant."
. Leave Premises and Contact Supervisor. If entry is still denied after attempting to resolve the
obstacles, the inspector should leave the premises after obtaining the information noted above in the
field logbook. The inspector should contact his or her supervisor immediately after leaving the
premises, and the supervisor should confer with the POTW's legal counsel regarding the desirability of
obtaining a warrant. The POTWs legal counsel should attempt to resolve the conflict by contacting
the facility's legal counsel prior to obtaining a warrant.
Withdrawal of Consent Durinn an Inspection. Occasionally, a facility may consent to an inspection
and later withdraw the consent while the inspection is in progress. Consent for the inspection may be
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withdrawn at any time after entry has been made. A withdrawal of consent is tantamount to a refusal of
entry. Therefore, the inspector should follow the procedures cited above under "Denial of Consent" unless
the inspection has progressed far enough to accomplish its purposes. All activities and evidence obtained
prior to the withdrawal of consent are valid and may be used in an enforcement proceeding against the
facility.
Denial of Access to Parts of the Facility. If, during the course of the inspection, access to some parts of
the facility is denied, the inspector should make a note of the circumstances surrounding the denial of access
and of the portion of the inspection that could not be completed The inspector should then proceed with the
rest of the inspection and should contact his or her supervisor after leaving the facility to determine whether a
warrant should be obtained to complete the inspection.
Covert Sampling in Response to Denial of Entry. Whenever entry to a facility is denied, a sample
should be obtained at a manhole immediately downstream of the facility, if possible (NOTE: the inspector
should be aware of the potential difficulties with the sample, i.e., are other facilities connected to that part of
the sewer which discharge the pollutants of concern?). This type of sampling, however, may help with any
further enforcement actions or investigations which the POTW may undertake at the facility by uncovering
activities which the industry is attempting to hide. This type of sampling is also effective when a demand
inspection is being conducted because the POTW personnel can then compare the results of sampling from
inside and just outside the plant to see if they match. This can provide evidence of any batches being
dumped prior to entry to the facility.
CONDUCTING AN INSPECTION UNDER A WARRANT
As an alternative to conducting an inspection with the consent of the facility, inspectors may conduct
inspections under a search warrant issued by a magistrate or judge. If a search wan-ant is obtained prior to
the inspection, the inspection may be conducted whether or not the facility officials consent to the inspection.
(NOTE: Under these circumstances, it may be necessary to have the assistance of the police or sheriff to gain
entry. This situation would only occur where the POTW knows that entry will be denied to the inspector).
The Barlow decision from the Supreme Court (discussed earlier), authorizes the issuance of a warrant to
inspect facilities without showing that a violation is probably occurring (probable cause requirement). When
the POTW seeks a warrant, it must show that it has the authority to inspect industrial facilities. Obtaining
such a warrant may be an appropriate part of the pre-inspection preparation process when the POTW suspects
that entry may be denied, either absolutely, or temporarily until processes or records can be altered, or other
actions taken to obscure violations of applicable pretreatment requirements.
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PRE-INSPECTION CHECKLIST
No single list of documents and equipment will be appropriate for each inspection. The majority of the
inspections which the POTW undertakes will be routine annual inspections required by the Federal
Pretreatment Regulations. There ma) be instances, however, such as emergencies (e.g., spills at an IU, or
complaints of problems at an II!). which might require an immediate site visit to assess compliance or
ascertain the situation at the II!. The POTW must be ready to respond to such situations by having all
inspection equipment and documents readily available and ready to go. The checklist outlined in Table 2-5 is
intended to guide and aid the inspector in planning for necessary inspection supplies and activities.
PRE-INSPECTION OBSERVA TIONS
Prior to entering the permittee's facility, the inspector should examine the facility's perimeter. By doing
this, the inspector may detect leaky storage areas and other general housekeeping practices at the plant which
might affect their discharge to the POTW. In addition, the inspector should also evaluate the environmental
conditions near the plant, such as vegetation, odor problems, or direct discharges to streams. It may also be
appropriate to take a sample at a manhole Immediately downstream from the facility (if available) to
determine the nature of the flow from the plant. This type of sampling may indicate problem areas that
require further Investigation. In this situation the inspector will need to know if that manhole is the only
discharge from the facility.
The inspection report form and the field notebook form the basis for the written report made of the
inspection and should onl> contain pertinent information and data. The language used in recording the
inspection information should be objective, factual, and free of personal feelings or terminology. Notebooks
can become an important part of the evidence package used by the POTW in an enforcement action and can
be entered in court as evidence if properly maintained. All of the information developed as a result of the
inspection should be dated so that the inspector can recall the information while writing the inspection report.
This report should be written as soon as possible after the inspection or sampling visit.
The inspector should keep all pertinent information from the inspection in the field notebook, This
information could include sampling measurements, flow measurements, production rates (if they are needed to
determine compliance with any applicable mass based limits), process descriptions, nature of the facility,
cooperativeness of the II,' officials, general housekeeping observations (e.g., how clean or organized is the
facility), and an> other information learned from visiting the site. Representatives from the IU may request
that any or all of the Information collected be treated as confidential business information. The POTW must
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TaHe 2-5
Pre-Inspeciion Checklists
General Equipment:
• Proper personal identification
. Camera
• Film and flash equipment
. Pocket calculator
. Tape measure
. Clipboard
. Waterproof pens, pencils, and markers
. Copy of the local sewer use ordinance
. Field logbook and maps
Sampling Equipment:
• Siphoning equipment
. Weighted bottle sampler
. Liquid waste samplers
Sample bottles/containers (certified clean bottles
with teflon lids)
. Ice chest
. Flow meter (if applicable)
. Preservatives
. Thermometer
Documents and Forms:
. Entry warrant (if applicable)
• Notice of inspection (if applicable)
. Receipt for samples and documents
• Chain of custody for auto samplers
• Copy of ILJ's permit
Safetv Equipment:
• Safety glasses or goggles
• Face shield
• Ear plugs
• Rubber-soled, metal toed, non-skid shoes
• Liquid-proof gloves
• Coveralls, long sleeved
• Oxygen/combustion/H:S meter with alarm
• Air blower with 15 ft. hose
• Safety harness, tripod and hard hat
• Flashlight
• Self-contained breathing apparatus
Emergency Equipment:
. Substance-specific first aid information
. Emergency telephone numbers
. First aid kit with eyewash
Polyethylene bags
Disposal towels or rags
Flashlight and batteries
Pocket knife
Locking briefcase
List of facility contacts
Compass for direction on maps. etc.
pH paper
Evidence tape
Container for contaminated material
Waterproof container labels
Field test kits
Field document records
Vermiculite or equivalent packing
Colorimetric gas detection tubes
pH equipment
Explosimeter (atmospheric testing device)
Tubing, tape and rope
Chain of Custody Forms
Hazardous sample shipping labels
Inspection form checklist
Copy of the local Sewer Use Ordinance
Confined space permit (if applicable)
Plastic shoe covers
Respirators and cartridges
Self-contained breathing apparatus
Manhole hook or pick
Fire extinguisher
Safety ladder (aluminum, chain, or rope)
Safety cones
Warning flags
Particulate masks
Traffic diversion devices
Two-way communication radio
Fire extinguisher
Soap, waterless hand cleaner, and towels
Supply of clean water for washing
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honor this claim until or unless the POTW's legal counsel determines that the information is not confidential.
In some instances it may be possible or necessary to elevate this evaluation process up the judicial ladder to
the state or federal system for final determination
INFORMATION TO BE COLLECTED PRIOR TO AND DURING THE INSPECTION
As mentioned earlier, the types of information that will be collected during an inspection will depend, in
part, on the objective of the site visit. For a comprehensive compliance evaluation and site review most of
the following information should be summarized prior to the inspection and updated during the inspection.
The information discussed in this section is reflected in the checklist questions found at the end of this
chapter, and this discussion should be used in conjunction with the checklist and the checklist instructions.
• Identifying Information: Facility name, site address, mailing address, contact name, title, and telephone
number.
. General Background Information: Applicable categorical standards and local limits, applicable
Standard Industrial Classification (SIC) code(s), number of shifts used, number of employees per shift,
hours of operation, date facility commenced discharge to the sewer, date the categorical process
commenced operation, etc.
. Water Schematic: The schematic for water flow through the facility and the location of all wastewater
discharge lines that flow to the POTW's system, along with major plant features.
. Discharge Schematic: A description of each discharge's (including any batch discharges) amount,
regulated pollutants, frequency, and destination.
. Process Schematic: A description of each process flow from each major product line and process used
within the plant, particularly processes that are subject to Federal Categorical Standards. Reactors,
plating tanks and all types of process tanks can contain chemicals which maybe discharged
periodically. Metal cleaning solutions are a prime example. The amounts, chemical nature, brand
name, and frequency of discharge are all important. In addition, it is important to note how these
wastes are disposed (i.e.. discharged to the POTW or packed in drums as hazardous waste). If
pretreatment of these solutions is practiced (neutralization, etc), this fact should be noted as well as the
method used to determine that the waste has been treated to acceptable levels. General plant
washdown (its frequency and quantity of water used) is also important. In many plants, the washdown
is the largest andor the most significant discharge.
. Pretreatment Systems: A detailed description and appropriate sketches of each existing pretreatment
facility, including operating data, if available.
. List of Pollutants: The list should be divided into two categories: 1) pollutants that come into direct
contact with the water that is discharged to the POTW; and 2) pollutants that do not come into direct
contact with water discharged to the POTW, but which have the potential to enter the wastewater due
to spills, machinery malfunctions, etc.
. Sampling Locations: A list of all sampling locations used at the facility.
. Chemical Storage: The proximity of chemical storage to floor drains and whether floor drains
discharge to storm or sanitary sewers. The volume of all hazardous chemicals encountered should be
listed. Any floor drains should be noted. If the chemicals stored are unknown, note the brand name,
use and chemical supplier and obtain all material safety data sheets for all chemicals used at the plant.
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The supplier's address should be noted in case it is necessary to contact them to obtain the necessary
chemical information.
. Slug Control Plans: A description of all spill control practices used by the IU, including information
on all past spills, unusual discharges, or temporary problems with any of the process units that may
affect the wastewater discharged to the POTW.
. Air Pollution Control Equipment: A description of all air pollution control equipment that may
generate a wastestream, the pollutants that are likely to be found in this wastestream, and the discharge
or disposal method used. In some industries, the effluent from air scrubbing may be the principal
waste source and may contain a wide variety of process chemicals which are not encountered in any
other wastestreams. For example, booths for spray painting sometimes use a water column as a "water
curtain" for fume control.
. Sludge Disposal: A description of how waste residuals (sludge) from the pretreatment operations are
handled, stored, and/or disposed. Many industrial processes such as cleaning, degreasing, grinding, or
chemical pretreatment produce sludge which must be disposed. How this occurs, how often, and the
quantities involved are all important. For example, vapor degreasers are used for cleaning metal in a
wide variety of industrial applications. They almost always produce a sludge and solvent waste, and
are usually water cooled, producing a steady stream of uncontaminated cooling water. The presence of
these devices should always be noted as well as appropriate answers to questions concerning the wastes
associated with them. As is the case with batch discharges, any waste disposal service should be
recorded.
. Boiler Slowdown: A description of the biocide(s) or algicide(s) used in the boiler maintenance
program. The chemicals used in this process may be chemicals of concern, especially for sludge
disposal by the POTW (e.g., molybdenum compounds).
. Operational Problems: A description of any operational problems or shut-downs of pretreatment
facilities since the previous inspection.
• IU Water Bills: The inspector should be familiar with trends in the lU's water consumption and
wastewater production. This information can be obtained by a careful review of the facility's water
bills. A mass balance approach should be taken to pinpoint any areas of water loss or potential bypass.
. Compliance Information: The inspector should review all previous IU compliance sampling data, as
well as all data obtained by the POTW on the facility to be inspected.
. RCRA (i.e.. Hazardous) Wastes: A description of all hazardous waste generated or stored at the site
and the manner of disposal for all such waste, especially any disposal to the sewer.
Each of these areas of a complete compliance evaluation are contained in the checklist which is presented at
the end of the chapter. This checklist should provide the basis of the information collected during the
inspection, unless the scope of the inspection does not require a complete compliance evaluation (e.g., a
response to an emergency situation may require only very specific information and not include the general
information contained in the checklist).
ON-SITE ACTIVITIES
This chapter has thus far addressed the procedures which should be followed when planning and
preparing for the inspection visit at a regulated IU. In doing so, we have covered the "why" and "what" of
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inspections. We nou turn to the on-site activities of the site visit. These activities can be characterized as
the "who." "how ," and "\s here" aspects of conducting inspections and form the core of the inspector's hands-
on activities.
The on-site activities at the facility form the core of the inspection. Once on-site, the inspector is
responsible for developing a complete picture of the lU's manufacturing and process operations, wastewater
treatment operation, compliance activities, and records management. Using the industrial inspection to its
fullest extent will depend upon the abilitv of the inspector to ask the right questions and to look closely in the
appropriate locations w hile on-site. 'Hiis will require inspectors to become thoroughly familiar with industrial
treatment processes. w.'.stew uter sources and treatment technology, as wel I as with correct inspection
procedures and techniques (e.g.. interviewing and observation). The principal goal of the ID inspection is to
gather information that can be used to determine compliance with all applicable requirements, including
permit conditions, regulations, and other State or local requirements.
An industrial pretreatment facility consists of wastewater treatment processes designed to remove
pollutants from wastestreams prior to discharge to the local sewer system. Pretreating these wastes is the
method used b> mam industries to compK \\ith local waste discharge ordinances and permits, and also
federal and state regulations. The sources, amounts, and types of wastes generated at an industrial
manufacturing or processing site depend on the age of the facility, raw materials used, production processes,
and the abilitv to recover or recvcle wastes generated as a result of industrial activity. Some industries
attempt to minimize the different wastestreams by controlling them at the source (i.e.. pollution prevention),
while others gather all wastestreams together for treatment at one central location.
Physical, chemical, and sometimes biological treatment processes are used to separate or remove
pollutants from these wastestreams. Hiese treatment processes should be closely controlled by plant
personnel to produce discharges which are acceptable to the POTW. To ensure that industrial dischargers
meet all applicable requirements, the pretreatment facility inspector must inspect each of the treatment
processes or facilities at any industrial site which has the potential to discharge toxic or hazardous wastes to
the POTW. This section outlines the procedures used in the NPDES program for industrial inspections.
These procedures should be followed bv POTW inspectors when conducting their site visits.
Opening Conference:
Once proper credentials have been presented and legal entry has been established, the inspector can
proceed with the on-site activities of the inspection. If this is the first visit by the POTW to the IU, or if the
management team at the IU has changed significantly since the last inspection, the on-site activities should
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begin with an opening conference with facility officials to outline what will be covered during the inspection,
the purpose of the inspection, and the procedures which will be followed. Once a rapport with facility
officials has been established, subsequent inspections and sampling activities at the ID may not require a
detailed opening conference as described below, or may not require a conference at all. (NOTE: The inspector
should always inquire if any changes have been made at the plant since the last inspection. This can be done
during an official opening conference or it may be done informally at the beginning of the inspection. If
changes have been made which affect the discharge to the POTW, the ID is required to report such changes.
If the IU has not reported such changes, it should be considered a reporting violation and brought to the
attention of appropriate ID officials). The inspector should gauge the level of awareness of the ID officials
with the POTW's role in the pretreatment program, and the inspector should continue opening conferences
until the IU clearly understands th : significance of its responsibilities. The POTW should encourage
cooperation between the facility o ficials and the inspector(s) to ensure that the activities go smoothly. This
section addresses the role of the inspector in the opening conference, along with relevant meeting agenda
topics. This section also describes possible mid-course adjustments which might be needed as a result of the
information discussed during the opening conference.
The opening conference establishes a forum for exchanging information between the POTW inspector and
facility personnel. This information exchange should focus on the inspection, but it does not need to be
limited to the inspection itself. The inspector should use the following principles when conducting the
opening meeting:
. Gain an early rapport;
. Start the meeting on a positive and professional note;
. Prepare and use any supprting information that will enhance the discussion (e.g., a copy of the local
regulations or statute authorizing the inspection, pollution prevention materials or technology transfer
information which might allow the IU to operate more efficiently). If you can provide the IU with
information which it might find useful, the inspector will be viewed as a resource and not a
burden on (he facility;
. Acknowledge that the inspection may disrupt daily facility routines, but assert that reasonable efforts
will be made to minimize such disruption;
• Listen carefully and be willing to answer the facility official's questions, but do not permit yourself to
be maneuvered into bending POTW policies/procedures or overstepping your authority in an attempt to
accommodate facility representatives. For example, facility representatives will be understandably very
curious about how they are performing vis-a-vis the requirements of the pretreatment program Do not
forget that the inspector's primary objective is to inspect the facility for compliance with discharge
requirements. The inspector is not there as a consultant to solve technical problems for the company,
but if through the inspector's experience or technical expertise the inspector can describe how similar
problems have been handled successfully, the inspector may be able to help the industry solve its
problem. Be cautious about giving advice. The inspector should not "advise" the IU on how it could
come into compliance. Such information, if followed, could be used as a defense in a future
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enforcement proceeding. The 1U has the primary responsibility to ensure compliance. It is the
inspector's job to evaluate the IU based on the requirements established in its permit or in the local
sewer use ordinance. It is not the inspector's job to tell the IU how to come into compliance.
A cooperative working relationship developed during this opening meeting can set the tone for the rest of
the inspection. It can also be used as the foundation for strengthening ties between the POTW and its
regulated industries. If approached properly, the opening conference provides an ideal opportunity for the
inspector to function as a public relations liaison and educator. The inspector should ensure that he or she
provides tactful assistance before, during and after the inspection, but does not provide information which the
IU can use as a defense in a later enforcement action. During the opening conference, the inspector should
attempt to cover the following topics with the facility officials:
• Inspection Objectives: By informing facility officials of the purpose and scope of the inspection, it
may help to avoid misunderstandings and facilitate the work of the inspector.
• Order of the Inspection: If the inspector also discusses the order in which the inspection will be
conducted, it will eliminate wasted time by allowing officials at the IU the time to make any requested
records available.
• Meeting Schedules: The inspector should schedule meetings with key IU personnel (perhaps
beforehand) to allow facility officials adequate time to spend with the inspector during the inspection.
It is important that a facility representative accompany the inspector during the inspection, not only to
answer questions about the facility and to describe the plant and its operating processes, but also for
safety and liability considerations. If these needs are discussed prior to the inspection, it allows the IU
an opportunity to make someone available.
. Permit Verification: The inspector should verify the pertinent sections of the IU permit, e.g., name and
address of the facility, discharge points, and proper use of the Combined Wastestream Formula (if
applicable).
• Safety Requirements: The inspection should verify which safety requirements (if any) are required at
the facility, to ensure that appropriate preparations were made.
• Photographs: Photographs are a useful tool for documenting inspection information, and may prove
useful in any enforcement proceedings against the facility. Facility officials, however, may object to
the use of cameras on their property (especially Federal military facilities or defense contractors). If a
mutually acceptable solution can not be reached, and if photographs arc considered essential for the
inspection, the inspector should conclude the inspection without photographs and consult the POTW's
legal counsel for additional information. If facility officials request that photographs be considered
confidential, as with any other information so identified, the POTW is obliged to comply with this
request pending further legal determination. When taking photographs it may be useful for the
inspector to use a camera which takes pictures with the dates imprinted on the photograph. This can
prove useful when storing and retrieving photographs for enforcement purposes. Also, when taking
pictures, it is often useful to include reference objects in the photograph to judge the distance and size
of objects. This creates a more substantial picture of the scene and may be useful when pursuing an
enforcement action.
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Inspection Procedures:
Physical Plant Review
When an inspector performs an industrial facility site review, his or her primary areas of investigation
include the facility's pretreatment units, monitoring equipment, and production processes. The purpose of a
facility site review is to examine the permittee's premises for problem areas and to verify existing POTW file
information on the IU. This overall review allows the inspector to gain a feeling for the facility being
inspected and to review areas that may indicate problems with plant operations or effluent limitations. In
particular, the inspector should focus attention on areas of the lU's premises where regulated pollutants are
produced, pumped, conveyed, treated, stored or recorded. This type of facility site review requires that the
inspector understand fully the wastewater treatment processes used at the industrial facility and how each
process fits in with the overall treatment scheme. The objectives of this type of comprehensive review are to:
. Evaluate the flow of raw water used for production culminating in wastewater discharged to the
POTW, the facility's water consumption and distribution usage, and the hydraulics of the facility's
drainage and collection system;
. Understand the flow of raw materials and any additives used in production as well as all end-products;
by-products; and other liquid, gaseous, and solid wastes resulting from the production process;
. Assess the conditions of the facility's current treatment processes and operations;
. Evaluate the wastewater characteristics (only possible if the inspector samples the effluent);
. Evaluate the lU's operation and maintenance activities;
. Check the completeness and accuracy of the lU's performance/compliance records (e.g., production
levels, results of self-monitoring, etc.); and
. Determine if the treatment units are being operated as efficiently as possible.
In the course of the site visit, the inspector should become more knowledgeable about the facility, including
areas that may indicate problems with effluent limits and overall operation and maintenance of the facility. It
is to the inspector's advantage to conduct the facility review as soon as possible upon entering the facility.
This prevents the permittee from altering any problem areas. After completing the preliminary discussions
with the plant officials, the inspector is ready to tour the facility. During the plant tour, the inspector should
be alert to and inquire about any of the following areas:
. Vital treatment units out-of-service for repairs. (The inspector should determine when the units were
taken out of service, the type of failure experienced, and when the units will be put back in service).
. Any unusual equipment or operations such as special pumps, floating aerators in diffused air systems,
chemical feeders, construction, temporary structures, or any rigged systems intended to correct
operational problems;
. Adequate safeguards to prevent the discharge of untreated or inadequately treated wastes during
electrical failures;
• Any evidence of spills an&or leaks, including proper storage of chemicals, which may enter the sewer
(the inspector should ask questions of the employees to see if they are familiar with any rquired spill
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Industrial User Inspection Manual Chapter 2 - Inspecting Industrial Users
or slug control measures at the plant and to determine if the 11! provides any training on safety or slug
control measures)
• Unauthorized discharge points and or bypasses, channels, or other areas likely to experience overflows.
(The inspection should determine if spills or unauthorized use has recently occurred as a result of
facility staff attempting to correct operational problems; and
• Disposal of collected screenings, slurries, sludges, or other by-products of treatment. (These materials.
including waste\vater should be disposed of in a manner so as to prevent the materials from entering
navigable waters or their tributaries);
One of the principal areas which the inspector should evaluate is the level of production at the facility.
Industries frequently make production changes because of advances in technology and the availability of new
products. Therefore, during the tour of the facility, the inspector should inquire whether the permittee has
made any changes to: production processes; raw material usage; amount of finished product; water use; waste
treatment processes; and other such changes.
The inspector should also inquire whether the permittee has modified any production process that would
change the pollutant loading to the POTW, and whether the POTW had been notified of such changes. This
is especially critical if the industry has limitations which are based on the combined wastestream formula
(CWF). The inspector must assess the impact which any changes in the discharge of wastewater will have on
any existing limits based on the CWF. Finally, the inspector must ensure that any increases in wastewater
flow is not used as dilution to meet any applicable pretreatment limits. If dilution is suspected at an industrial
facility, the inspector should trace each plumbing line to determine where it originates and where it goes.
This may be very time intensive, but it is the only way to accurately assess the existence of dilution at the
facility, since it is unlikely that dilution lines will show up on any schematics that the company provides.
The inspector should verify any changes in production processes or pollutant loadings and include the results
in the Inspection Report prepared alter the inspection.
In addition, the inspector should check the appropriateness of monitoring locations, the existence,
condition and calibration of the permittee's self-monitoring equipment (both field and laboratory), and the
facility's maintenance program for this equipment. During the physical "walk through" of the facility, the
inspector should observe all areas which have current or potential problems. Each, of these observations
should be carefully documented in '.he inspector's field notebook because of their potential sensitivity during
an enforcement proceeding. It is often useful when trying to understand the industrial facility's process to
follow the process in a sequential order of production.
Self-Monitoring Review:
The site review at the industry should include an examination of the permittee's self-monitoring program.
To perform this review thoroughly, it is the inspector's responsibility to be familiar with the monitoring
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industrial User inspection Manual Chapter 2 - Inspectinn Industrial Users
requirements contained in the facility's permit and with any correspondence which may have modified or
replaced sampling points or analytical procedures. The inspector should also be thoroughly familiar with all
approved test methods and the specified sample holding times and preservation techniques, or in the case of a
complex array of methods, the inspector should have a reference list available of the approved methods for
those samples required by the permit. (See Table 3-4 in Chapter 3 for an overview of appropriate holding
times and analytical methods for various pollutant parameters).
There are two objectives of the self-monitoring review: 1) confirm that sampling and flow measurement
equipment are provided as required in the permit and that they are being operated, calibrated and maintained
properly; and 2) confirm that the analytical test methods used to evaluate pollutants or parameters specified in
the ID permit conform with the EPA's regulations at 40 CFR Part 136. When conducting the self-monitoring
review, the inspector should:
. Verify that flow measurement devices are in use (if required) and are adequate to handle the expected
ranges of flow rates;
. Verify that samples are taken at the locations prescribed in the ID permit;
. Verify that the sampling location specified in the permit is adequate to provide a representative sample
of the regulated discharge;
. Verify/determine that the appropriate limits arc being applied at the specified sampling locations;
. Verify that the frequency of sampling is performed in accordance with the permits requirements and
that this frequency is adequate for the nature of the facility;
. Verify that samples are collected and preserved in accordance with 40 CFR Part 136;
. Verify that samples are analyzed within the holding times and analyzed according to approved test
methods in 40 CFR Part 136;
. Verify that appropriate procedures are used by the industrial user when the IU pulls its own sample
(i.e.. observe the IU pulling a routine compliance sample), and observe the IU when it conducts its
measurements of flow and/or pH (it should be a common practice for the inspector to pull a pH sample
and compare the results with the IU;
. Verify that QA/QC procedures used by the IU in its self-monitoring program are adequate; and
. Check all sampling, monitoring, and laboratory equipment to verify that all equipment is in working
order and has been operated, maintained and calibrated (including O&M and calibration logs) correctly.
Operations Evaluation.
The operating factors at the facility which might affect plant performance range from qualitative factors
such as the skills and aptitudes of the operators (e.g., process knowledge and general aptitude), to physical
deficiencies in laboratory equipment or a lack of flexibility in process equipment. The evaluation of operation
activities must focus on wasteuatcr treatment, and laboratory analysis. This evaluation should be based on
the following topics:
. Policies and Procedures;
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Industrial User Inspection Manual Chapter 2 - inspecting Industrial Users
• Staffing and Training;
• Health and Safety; and
• Management controls.
Appendix 111 presents the basic review questions that an inspector should ask to evaluate the operation and
maintenance activities at the facility,. These questions are detailed and comprehensive, and it is probably not
necessary to cover all of these points with each inspection. The POTW should make sure that these areas are
covered during the course of the Ill's permit cycle (e.g.. if the lU's permit is issued every three years, the
POTW should cover the operation and maintenance questions at least every three years, unless there are
suspected problems at the plant which relate to the operation and/or the maintenance of the facility. NOTE:
The permit issuance cycle should never exceed five years).
Policies and Procedures. Written operating procedures and standard reference texts enable the operator of
the process lines or wastewater treatment equipment to achieve efficient plant operation. The operations
manual prepared for the facility is the most important reference that an inspector should review when
evaluating plant policies and procedures. Other reference materials which should be available relating to the
operation of the facility include: manufacturer's literature, publications by professional organizations (e.g..
the Chemical Manufacturer's Association), and EPA publications.
Staffinn. Hven the best engineered facility cannot perform to its potential without a sufficient number of
capable and qualified staff. Staff interviews are an important component of this evaluation, and the questions
outlined in Appendix III can be used to ascertain the quality of the operations at the facility. The inspector
should make an attempt to interview the individual in charge of overall operation at the facility, the chief
operator (if different), specific unit process operators, and the laboratory staff.
Health and Safety. At all times, safe operating procedures should be followed by the regulated facility's
personnel. Employees must be trained in emergency shut-down, fire control, and spill response procedures, as
well as in the use of safety equipment. Each of these areas can adversely affect the nature of the discharge to
the POTW by allowing unregulated or uncontrolled amounts of pollutants to enter the POTW's system. The
authority for such an evaluation is found at 40 CFR 403.8(0(2Xv) which requires an evaluation of each SIU
for the need to adopt a slug control plan. The inspector should also verify that the Material Safety Data
Sheets required by the Right-to-Know law are readily available at the facility. This law also requires a
written hazard communication program (including notification to the POTW, which is also covered by the
General Pretreatment Regulations), and labeling of chemicals (to ensure that incompatible chemicals are not
stored together, e.g., cyanide compounds stored with acid compounds).
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Industrial User Inspection Manual Chapter 2 - Inspecting Industrial Users
Management Controls. Monitoring practices are a good indicator of both the emphasis placed on
operations and the operator's understanding of process controls. Factors affecting a facility's monitoring
capabilities are:
. The sampling program;
. Performance testing;
. Analytical capabilities; and
• Record keeping practices.
An effective process control program is essential to a treatment facility's optimal performance. However,
process control cannot be quantified easily by the inspector, therefore, in most cases, the inspector must rely
on discussions with plant personnel (e.g., operators) to supplement available records and the technical
evaluation. Again, the questions outlined in Appendix III can be used to evaluate the quality of the facility's
operations.
Maintenance Evaluation:
Facility maintenance directly affects the ability of the facility to run efficiently and to comply with its IU
permit. There are two types of facility maintenance which should be conducted at the plant:
. Preventative Maintenance: Reduces the facility operating costs by eliminating breakdowns and the
need for corrective maintenance. It improves the facility's reliability by minimizing the time the
quipment is out of service. It increases the useful life of the treatment and process equipment, thus
avoiding the need for costly premature replacement which may cause an interruption of wastewater
treatment at the facility. Each of these items, if adequately addressed, reduces the possibility of
compliance problems at the facility. Therefore, it is important that the inspector evaluate these areas to
ensure compliance with all applicable program requirements. AND
. Corrective Maintenance: Returns the malfunctioning equipment to operation. This has compliance
implications because the malfunctioning equipment may be in a treatment process necessary for
compliance with the pretreatment program requirements. Therefore, the inspector should evaluate the
procedures the facility uses to identify and correct instances of malfunctioning equipment.
The principal areas of concern for both the operations and maintenance evaluation are: staffing and training,
planning and scheduling, and management control (i.e., records systems and inventory control). Only well-
trained, competent staff can be expected to perform adequate physical inspections, repairs, and preventative
maintenance. Wastewater facility maintenance is complex and requires a variety of skills. Because many of
these skills are not readily available, an ongoing training program is essential. The pluming and scheduling
of maintenance is also essential for effective preventative and corrective maintenance. Ensuring that an
adquate plan and schedule is in place is an important task for the inspector. A detailed records system is the
basis of any maintenance program. Records are used to establish the maintenance histories of equipment.
diagnose problems, and anticipate (and thereby avoid) equipment failure, making records an effective tool for
preventative maintenance. A central inventory of spare parts, equipment and supplies should be maintained.
The extent of the inventory should be adequate to avoid process or treatment interruptions. A maintenance
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industrial User Inspection Munual Chapter 2 - Inspecting Industrial Users
cost control system should he an integral part of every wastewater treatment facility at the IU. Evaluating
costs in this manner serves to control expenditures and can be used as a baseline for future budgets. This will
help ensure that all necessary process and treatment equipment is operated continuously and effectively,
thereby ensuring that the regulated facility operates within the limits specified in its permit.
Records Review at the Industrial User
The General Pretreatment Regulations require Significant Industrial Users (SIU) to submit reports at least
twice per year on the nature and concentration of pollutants in their discharge and the flow from the plant to
the POTW. Each SIU is required to maintain records of all the information obtained from their monitoring
activities for a period of at least three years. However, many ItJs, as well as many POTWs, maintain records
for at least five years to coincide with the statute of limitations on penalties. These records contain a variety
of information which may be useful to ascertain the facility's compliance status with its permit requirements.
Examining these records is a key part of the inspection process for the POTW.
Records and files may be stored in a variety of information retrieval systems, including written or printed
materials, computer or electronic systems, or visual systems such as microfilm and microfiche. Conducting
an effective records review is an important investigative skill for the POTW inspector, but it is an art that is
developed largely through experience and practice. No set of instructions can prepare an inspector for the
variety of records and record keeping systems they are likely to encounter. This process can be difficult
because of the complexity of the industrial processes being regulated and the infinite variety of record
keeping systems which can be used to document how these processes are operated and maintained This
complexity makes it difficult for the inspector to achieve his or her goal, i.e., to verify or determine whether
or not a facility is in compliance with its applicable permit requirements.
The POTW inspector should review the ILJ's permit prior to conducting the inspection (it may even be
useful to have a copy of the permit along on the inspection) to determine the facility's record keeping
requirements. Throughout the inspection, the facility's operations should be compared with the permit to
verify that required permit activities are correct, current, and complete. Some of the information needed to
verify the permit can be obtained during the opening conference and compared with the facility permit. This
general information may include: correct name and address, correct name of the facility contact, number and
location of discharge point(s) to the POTW, and the facility's principal products and production rates (what
there are production based standards in place).
The inspector should check for records which will verify that proper notification was made by the facility
to the POTW if: 1) discharges have changed from those stated in the ID permit (e.g., additional discharges,
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Industrial User Inspection Manual Chapter 2 - Inspecting industrial Users
or significant increase in flow), 2) a permit violation has occurred (e.g.. the permittee is required to notify the
POTW within 24 hours of becoming aware of an effluent violation and to resample the discharge within 30
days), 3) any discharge of a hazardous material (as defined in 40 CFR 261) has occurred from the IU (NOTE:
This notification must be sent to the POTW, the U.S. EPA Regional Waste Management Division Director,
and the State hazardous control authorities), or 4) a bypass has occurred. These record keeping requirements
are outlined in the federal regulation at 40 CFR 403.12. The inspector should also check to ensure that the
appropriate records are being kept for a minimum of three years. These records will likely include many of
the following types of information:
• Sampling and Analysis Data:
0 Dates, times, and location(s) of sampling;
0 Sampling techniques (e.g., grab or composite) and analytical methods used;
0 Results of the analyses;
0 Dates of the analyses; and
0 Name(s) of analysis and sampling personnel.
. Monitoring Records:
0 Self-monitoring reports (if applicable), including flow, pollutant parameters, etc. as required by the
permit; and
0 Original charts for continuous monitoring instrumentation and bench sheets for analyses.
. Laboratory Records:
0 Calibration and maintenance equipment and schedule;
0 Calculations (e.g.. bench sheets or books); and
0 QA/QC analysis data.
. Facility Operating Records:
0 Daily operating log;
0 Summary of all laboratory tests run and other required measurements (if applicable);
0 Chemicals used (e.g., pounds of chlorine per day. etc.);
0 Weather conditions (temperature, precipitation, etc.);
° Equipment maintenance schedules; and
0 Sludge/RCRA disposal records and waste hauling manifests.
. Slug Control Plan (if applicable);
0 When required, a properly completed Slug Control Plan should be available to the inspector.
The inspector should document all records review activities and should note all inadequacies,
discrepancies, or other problems disclosed or discovered during this review. Any identified problems may
warrant a more intensive investigation. This decision should be made by the inspector in conjunction with
POTW officials.
A primary objective of the records review at the industrial user includes a comparison of the bench sheet
data and laboratory report summaries to the values reported on the self-monitoring reports submitted by the
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industrial User inspection Manual Chapter 2 - Inspecting Industrial Users
facility. This evaluation is critical to determine if all data are correctly summarized on the self-monitoring
reports received by the POTW.
As mentioned above, the IU is required to keep complete and accurate sampling records, and a failure to
do so is a violation of the Federal Pretreatment regulations. The POTW should treat this failure to keep
records as a violation and respond with the appropriate enforcement response, as identified in its Enforcement
Response Plan. A review of facility records must determine if the IU is complying with the sampling and the
record keeping requirements of the General Pretreatment Regulations contained in its ID permit. In particular,
the inspector should verify that the IU is keeping the following records for all samples: the date and time for
each sample, the date(s) of each analysis, the exact place the sample was taken (i.e., location of the sample
point), the analytical techniques/methods used for all samples, the name of the person who took each of the
samples, the name of the person who performed the analysis, and the results of each of the analyses.
Obtaining Copies of Necessary Records:
When copies of records arc necessary the ID must make these records available in accordance with 40
CFR 403.12(o). The inspector must consider how to retrieve and store the required records. The following
outline may be useful in determining the appropriate means of accessing and securing certain records.
• Written or printed records generally can be photocopied on-site. Portable photocopy machines may be
available to the POTW inspector, but in the absence of this equipment, inspectors should be authorized
to pay a "reasonable" price for the use of facility copying quipment.
0 At a minimum, all copies made for or by the inspector should be initialed and dated for
identification purposes (see identification details below).
0 When photocopying is impossible or impractical, close-up photographs may be taken to provide
suitable copies.
• Computer or electronic records may require the generation of hard copies. Arrangements should be
made at the time of entry or during the opening conference for these copies. Photographs of computer
screens may provide adequate copies of these records if no other means are available.
• Visual systems (microfilm and microfiche) may have photocopying capacity built into the viewing
machine, which can be used to generate copies. Photographs of the viewing screen may provide
adequate copies if hard copies can not be generated.
Record Identification Procedures:
Immediate and adequate identification of the records reviewed by the inspector is essential to ensure a
legally binding custody process which ensures the admissibility of the records in court. If an inspector is
called to testify, he or she must be able to identify positively each particular document and state its source
and the reason for its collection. This identification can be accomplished by initialing, dating, numbering, and
entering each of the records in the inspector's notebook under the facility's name.
. Initialing/Dating: Each inspector should develop a unique system for initialing and dating the
records and copies of records so that he or she can easily verify their validity. This can be done by
initialing each document in a similar position, or by another method, at the time of collection. Both
the original and the copy should be initialed in the same fashion. All record identification notations
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Industrial User Inspection Manual Chapter 2 - Inspecting Industrial Users
should be made on the back of the document. The inspector must be able to identify positively that
he or she so marked the document.
. Numbering: Each document or set of documents substantiating a suspected violation(s) should be
assigned an identifying number unique to that document. The number should be recorded on each
document and in the inspector's field notebook.
. Logging: Documents obtained during the inspection should be entered in the field notebook by a
logging or coding system. The system should include the identifying number, date, and other
relevant information, such as: the reason for copying the material (i.e., the nature of the suspected
violation); the source of the record (i.e., type of file, individual who supplied the record); and the
manner of collection (i.e., photocopy, other arrangement).
The originals of each document must be returned to the proper person or to their original location, and
related records should be grouped together for ease of reference. Confidential business records should be
handled according to the special confidential provisions discussed earlier in this chapter.
Closing Conference:
To achieve the most effective results from the compliance inspection, the inspector must communicate the
results of the inspection promptly to the facility's management and/or operating personnel. The inspector's
discussion, however, should be limited to the specific findings of the site visit. If appropriate, the findings
should be compared with the industrial user's permit requirements, consent decrees, administrative orders,
an&or other enforcement actions. Even though a discussion of the inspection findings is important, certain
precautions are essential when conveying this information. The inspector should keep the following
guidelines in mind when presenting any findings from the site visit.
• The inspector should be cautious about discussing the compliance status or any legal enforcement
consequences with the industrial user representatives or with facility operating personnel. On the
other hand, if there are violations which are clearly identified during the inspection, and the inspector
is confident that those violations are "actionable", then the inspector should bring these violations to
the attention of the IU representative. This should be done in writing, either through a Notice of
Violation (NOV) or Deficiency Notice (DN) (see Figure 2-1 for an example form for the deficiency
notice).. The inspector's purpose is to call attention to and explain the violation but not to predict
the consequences or penalties that may occur beyond the NOV/DN.
. The inspector should refrain from recommending a particular consultant or consulting firm, or any
particular treatment system, even if asked to do so. Inspectors should tell the permittee's
representative to contact a professional society or approved listing for advice on how to come into
compliance with all applicable permit requirements.
A deficiency notice identifies existing or potential problems specific to the permittee's self-monitoring
program. Issuing a deficiency notice on-site or after the site visit provides a swift and simple method for
improving the quality of the data submitted by the industrial user. This type of notice allows the inspector to
assign formal responsibility to the permittee, and to track each stage of the compliancdenforcement process
with respect to the lU's self-monitoring program. This notice is designed to alert the facility to deficiencies
in their self-monitoring activities and to assist the industrial user in complying with its permit
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Industrial User Inspection Manual Chapter 2 - Inspecting Industrial Users
FOLLOW UP ACTIVITIES
Follow up activities from the inspection are necessary because this is how the information from the
inspection is translated into an action by the POTW (e.g., an enforcement action or decision to modify the
IL"s permit). The POTW has the primary responsibility to ensure compliance with all applicable pretreatment
requirements, and the inspection is an important mechanism for achieving this goal. Once the inspection has
been completed, the inspector must summarize his or her findings in a report (a standard form for this repot-t
should be developed by the POTW) so that inspection findings can be admitted in court. The POTW may
also choose to use the inspection checklist at the end of the chapter as the basis of its inspection report
format. This report should be placed in the Ill's file for future reference as background material for
subsequent inspections.
Every POTW should have systematic procedures for tracking industrial user problems, including
permanent records of all problems kept in office tiles or computers. In this way, the information can be
reviewed at any future date. If the inspector took effluent samples as part of the site visit, the results of these
tests should be placed into the POTW's compliance tracking system (either manual or, preferably, automated)
and appropriate action (as defined in the POTW's Enforcement Response Plan) should be taken if a violation
is detected. It is in the POTW's best interest to conduct timely follow-up activities with the IU so that any
identified problems can be addressed before they get out of control. Such follow-up activities will usually
include some form of enforcement action, perhaps even formal enforcement action for significant violations.
Inspection Report
Once the inspection has been completed, the inspector should review his or her notes to identify areas
which may require follow-up activities. The notes from the inspection should be organized into a report
format. This is one of the most important points of the whole inspection procedure, yet it is often ignored
The need to write a clear and concise report which contains pertinent information to be used as a basis for
future permitting, compliance, and enforcement decisions cannot be stressed enough. This chapter has
outlined in detail the procedures for collecting and substantiating the information which should be used to
prepare the inspection report.
The report accomplishes three objectives: I) it organizes and coordinates all information in a
comprehensive, usable manner for use by the POTW's compliance personnel, 2) it clearly identifies areas
which require follow up activity, and 3) it provides significant background information on the facility which
can be reviewed prior to conducting subsequent inspections at the facility. The quality of this report will, to a
large degree, determine how effective these follow up activities will be at the facility. The preceding sections
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Industrial User Inspection Manual Chapter 2 - inspecting Industrial Users
have detailed the procedures for collecting and substantiating the inspection information. Once organized, this
material should be translated into a report format developed by the POTW.
The information in the inspection report must be presented in a clear, concise, and well-organized
manner. The information must be objective and factual; the report should not speculate on the ultimate result
of the inspection findings (i.e.. anticipate any enforcement action), but should stick with the facts as identified
by the inspector. Of particular importance in the report are the following items:
. Accuracy: The information in the report must be factual and based on sound inspection practices.
Observations in the report must be the verifiable result of firsthand knowledge so that compliance
personnel can depend on the report's accuracy when determining appropriate follow-up action (if
any).
. Relevancy: The information in the report must be relevant to the compliance status of the facility.
Irrelevant facts and data will clutter the report and may reduce its clarity and usefulness. Personal
comments and opinions must be avoided.
. Comprehensiveness: All information pertinent to the industrial user's compliance status should be
organized as a complete package. Documentary support (e.g.. photographs, statements, sample
results, etc.) accompanying the report should be referenced clearly so that anyone reading the report
will get a complete, clear overview of the situation at the facility. The more comprehensive the
evidence, the better and easier is the task of the compliance personnel when taking an action.
Each report should contain the following elements: the report form (developed by the POTW); supplementary
narrative information; copies of the completed checklist (an example of a checklist is provided at the end of
this chapter); and documentary support (e.g., photographs or sketches).
The contents of the report should be comprehensive (i.e., should include all pertinent observations from
the inspection), but the report should focus on supporting or explaining the information provided in the
inspector's notes. The narrative of the report should be a concise, factual summary of the observations and
activities undertaken during the inspection, organized in a logical, legible manner, and supported by specific
references to accompanying documentary support.
All documentation that is produced or collected by the inspector to provide evidence of suspected
violations should be included in the inspection report. This type of documentation may include: the
inspector's field notebook, statements, photographs, drawings and maps, printed matter, mechanical
recordings, and copies of records. In general, the types of information contained in the report should reflect
the type of information collected during the inspection.
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Industrial User Inspection Manual Chapter 2 - Inspecting Industrial Users
FIGURE 2-1
EXAMPLE DEFICIENCY NOTICE
DEFICIENCY NOTICE PERMI'ITEE NAME AND ADDRESS
Pretreatmcnt Program Administered
by the (POTW Same)
PERMITTEE REPRESIMA IIVI (Receiving this noiw/TJTLI- III Permit No
During the compliance inspection carried out on (dale) the deficiencies noted below were found Additional areas
of deficiency ma> be brought to jour attention following a complete review of the Inspection Report and other information on file
with the (Same of POTH*)
DEFICIENCIES
MONITORING LOCATION (Describe)
FLOW MEASUREMENT (Describe)
SAMPLE COLLECnON/HOI.DING TIM I- (Describe)
SAMPLE PRESERVATION (Drscnhf)
ANALYTICAL METHODS (Inscribe)
RECORD KEEPING (Describe)
OTHER SELF-MONITORING DCMCILN'CILS (Describe)
ADDITIONAL COMMENTS
REQCESTED ACTION • Your menuon to Che corrvcuofi of the dcficiencia noted i£>o>c d requccted Receipt of the description of the correcrjve •ctx>ru ukea will
W ootuid^nd in the detennirutioa of the need for further Admirmtnlive or l^yij Action Your mponie cui eirjier be tubmined with vour next periodic compliance report or
H diracud by the intpector Queltxx>i rrgudm) thu notice miy be directed to • (/I'TV i Xatut}
INSPECTOR'S SIGNATURF. INSPECTOR'S ADDRESS/PHONE POTW S ADDRESS DATE
INSPECTOR'S PRINTED NAME
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Checklist Questions for POTW Inspectors
I. General Inspection Information:
Date of inspection. IMS! imped I on diite
inspected by. Last impeded h\-
Type of inspection? Demand Scheduled
Did the previous inspection identify areas which the II) was required to correct ' (Y \l
What areas were identified'.'
What progress has the IU mude in correcting the identified deficiencies '
Persons present during the inspection
Name
1.
2.
Title
Affiliation
II. General Facility Information
Industry name.
Site
address:
SIC cadets)
Mailing
Permit on file' (}'-'\i
f-'ax »• ( )
Phone ft: ( >
Phone #• f )
Industry contacts fw/ titles)
I.
2.
Applicable categorical standards.
(e.g.. 413, 433, 425, etc.)
Pollutants covered by local limits:
(e.g.. Cd Cr. Cu, Pb. A'/. Zn)
Are local limits technically based'' (Y/N)
Number of employees.
Number of shifts per day.
Hours of operation per day.
Work days per week.
Manufacturing processes used.
Planned changes to the plant
Changes since lust inspection Production level.
Use of raw materials
Amount of finished product.
Did the facility report any changes identified above to the POTW lY. \ \.-ti
- 48 -
Uric/ facility description
Seasonal production " ( Y. \)
Product(s) produced
Amount of finished product
Rav> materials used.
h.mplovee showers on
site'' (Y.\>
Si'heduicd shutdown
periods ' (Y \l
When'
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General Instructions for Using the Checklist
General:
The checklist is intended to be used by POTW inspectors as a field guide when conducting
site visits at industrial users. The checklist is intended to encompass the scope of a routine
compliance inspection. If the POTW inspector follows the checklist questions, all necessary
compliance information should be obtained during the site visit. Some of the information contained in
the checklist may not change (e.g., industry name, SIC codes, etc.), but the POTW inspector should
continue to gather the information in case of a change which might affect the discharge of pollutants
to the POTW (e.g., a new SIC code might indicate a new industrial process which may discharge
additional pollutants to the POTW). The checklist may be altered by the POTW to meet its specific
needs, but the checklist, either as presented or altered, should form the basis of the inspection report
prepared by the POTW.
I. and H. General Inspection Information and General facility Information:
The inspector should obtain basic identifying information about the IU when conducting the
site visit, including: industry name; standard industrial classification code number(s) (NOTE: there may
be more than one SIC code for a given facility); site address and mailing address (the two are often
different); as well as any industry contact names, fax and phone numbers, and titles. This
information will facilitate routine communication with the industry. The inspector should also check
to see if a copy of the IU permit is on file at the IU. If it is not, this may be an indication that the IU
does not understand or realize its obligations under the local pretreatment program. The inspector
should provide a brief description of the facility (i.e., type of operation, how long in business, nature
of the products produced, length of time in business, etc.) and probe the nature of the facility's
applicable limits (both categorical standards and local limits).
The nature of the business operation should be understood by the inspector. Therefore, the
inspector should cover: how may employees the facility has (and the trend of employment over time);
the number of shifts per day; the hours of operation each day; the number of work days per week;
whether there is any seasonal production schedule; the nature of the products and the amount
produced and raw materials used in the process; as well as a description of the manufacturing
processes used. It is important for the inspector to track any changes in the plant's operation,
including any changes in the items listed above. This information provides a history of the
manufacturing process and will aid in future inspections at the facility.
The inspector should evaluate the lU's efforts at operation and maintenance of its pretreatment
facilities and storage areas since this will affect the discharge of pollutants from the facility.
Therefore, there are checklist questions pertaining to these issues. Production data is included and is
especially important in situations where production based limits are in place for the IU. A final area
of general investigation is the compliance status of the facility and a note of any enforcement actions
which have been taken for the current noncompliance (past, resolved actions need not be mentioned).
The inspection report should track the progress of any IU in meeting imposed compliance deadlines,
and the checklist reflects this.
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n. General Facility Information (continued)
Date the facility commenced discharge to the POTW:
Current long-term average production rate: (if applicable)
Is the facility currently in compliance? (Y/N)
If not in compliance, what action has been taken ?
Comments:
Are O&.M schedules available at the facility?
Are there O&M policies and procedures ?
Is OA.M training/certification adequate?
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J. Water Usage and Wastewater Production
I. WATER USAGE
SOURCE AVG. FLOW (gpd) METERED (Y/N) ? Comments.
Water Company
Private Well
TOTAL
2. WASTE WATER PRODUCTION
WASTE WATER GENERATING PROCESS AVG FLOW BATCH OR
CONTINUOUS'
BATCH MEASURED TRL4TED REGULATED
FREQUENCY ESTIMATED (Y'Ni POLLUTANTS
OUTFALL *
C.
D.
E.
F. Contact cooling water
SUBTOTALS
G. Boiler blowdo\vn/Make up
H. Evaporation (loss)
I. Non-contact cooling
J . Lawn maintenance/Irrigation (loss)
K. Sanitary (loss)
L- In product/Shipped (loss)
M. Other
TOTAL
Number of outfalls to the POTW Total
Regulated
Number of outfalls to surface waters
All outfalls accounted for? WIN)
N.A
N'A
N-'A
Chemicals used in boiler blowdown.
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///. Water Usage and Wastewater Production
To calculate the amount of wastewater discharged to the sewer, the inspector must obtain data
on incoming water and water consumption. The inspector should request the following information
from the IU regarding the Ill's operation: water bills for the most recnt 12 months; documents
showing incomping water from other sources (e.g., well); discharge flow meter totalizer charts or
readings for the same 12 month period (if flowmeter is present); and production process flow meter
totatlizer charts for the 12 month period (if flowmeter is present). The inspector should understand
clearly all water use and wastewater production at the IU, and the checklist is designed to allow the
inspector to account for all such water use/loss and wastewater production. The chart should be
copied and expanded if there are additional sources of wastewater at the facility. In addition, the
inspector should check for such illegal activities as: piped or hosed connections which bypass a
sampling point; any signs of dilution, such as rinses running during non-processing times which may
be inadequately substituting for pretreatment; and any diversions of wastewater flow around the
pretreatment system. One of the main reasons for establishing this water balance is to be able to
compare water usage and wastewater production from one inspection to the next to determine if
additional processes are being employed by the facility.
In addition, the inspector should evaluate the number of outfalls from the facility and identify
if there are any unregulated outfalls in use. Any potential for by-pass needs to be investigated as
soon as possible to ensure that the POTW is not receiving pollutants of a kind or an amount which it
can not handle. Also, the inspector should be aware of the chemicals which are being used as
biocides in the boiler blowdown because some of these chemicals may interfere with the operation of
the treatment plant or interfere with the POTW's final sludge use or disposal (e.g.. molybdenum
compounds).
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IV. Monitoring, Record Keeping and Reporting
I. Monitoring
Flow
Permit
Sampling
Location
Industry
Sampling
Location
Permit
Limit
Permit
Sampling
Frequency
Industry
Sampling
Frequency
Permit
Sampling
Method (metals)
Industry Sampling Permit Sampling
Method (metals) Method
(CN. phenol. O&G,
pH>
Industry Sampling
Method
(CN, phenol, O&C',,
pHl
Discrepancies between permit requirements and industry practice for Sampling location? (Y/N)
Sampling frequency') (Y/N)
Sampling method? (Y/N)
Are the permit requirements appropriate for. Sample location(s)? (Y'N) If no. explain.
Permit limit(s) ~> (Y/N) If no, explain
Sample method? (Y/N) If no, explain.
Sample frequency"* ( Y'N) If no, explain.
What changes, if any, ure needed in the permit 7
Samples analyzed according to 40 CrR 136' Are samples preserved according Part 136^ Samples analyzed within required holding times 9
Samples token during periods of process discharge only7 Samples analyzed in-house or contract'.' Is required unulytical certification used?
2. Record Keeping
All information kept for 3 years'' All required information available, current and complete? Are all sample results included in the lU's report'*
3. Reporting
Did the facility report results of any more frequent sampling in the last reporting period? If so. were all results reported"*
POTW notified of all violations w/i 24 hours7
Do sample results match what is reported by the industry'' Are there any violations which were not reported to the POTW?
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IV. Monitoring, Record Keeping and Reporting
It is crucial for the inspector to evaluate the lU's monitoring, record keeping and reporting
practices because this information forms the basis of the POTW's regulation of the industry. If the
IU is not monitoring correctly or if the samples are not analyzed using the required procedures, the
information derived from that monitoring can not be used to establish compliance. Likewise, if the
facility does not keep records, the POTW can not know the conditions at the facility during the
reporting period. It is necessary for the inspector to compare the results of sampling to the actual
reported values to ensure that there are no discrepancies. If a discrepancy is found, the cause should
be determined at once.
In the first section the inspector should compare the industry's practice with the permit
requirements for the following: sampling location (which must be specified in the permit, e.g.,
location 001 with a schematic indicated this location), sampling frequency (e.g., monthly, twice per
year, etc.), and sampling method (i.e., grab or composite) for metals and organics. Each of these
items should be specified in the permit, and the facility must abide by the requirements established in
the permit for these items.
In addition, the inspector must determine if the current permit conditions for the facility are
adequate to control the discharge to the sewer. The checklist questions are designed to give the
inspector a comprehensive overview of the IU's monitoring, record keeping and reporting procedures.
If there are any problems, the source of the problem should be determined as soon as possible.
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V. Wastewater Treatment Systems
Does the industry treat its process wastes prior to discharge to the POTW
I/treatment is in place, complete the following information. (If no treatment, go to the next section)
Are any treutment units out of service:? (Y/N) Inadequate system in place to correct a problem? (Y/N)
Unauthorized discharge points in service? (Y/N) Unauthorized bypasses in place'' (Y/N)
Treatment type. Date originally installed.
Modified since installation'.' Describe.
Design flow (gpd).
Actual flo w (gpd)
Operating Schedule
Hours per day. Days per week
FTEs needed to operate.
Clarifier volume.
Description of overall condition.
Treutment (hutch or continuous)?
Discharge (batch or continuous)'
Reagents used, (include usage rate] if
Effluent filtration media (if applicablei
Has the system experienced operational/upset problems since the last inspection' If yes, describe
VI. Sludge Generation/Waste Disposal
If the fad lity generates sludge or hauls regulated wastes, please complete the following information. (If "01. go to next section)
Sludge dewatering method. Moisture content. Amount generated (55 gal Disposal method.
bbl/mu).
Sludge Storage (bbls)
Sludge hauleris)
Shipment frequency.
Disposal location(s) :
Manifests available?
Hazardous Sludge Generated? (Y/N/NA)
Manner of Hazardous Waste Disposal.
Are hazardous waste manifests available':'
Hazardous Waste Discharged to tk POTW7 (Y/N/NA)
If not, verify manner of hazardous waste disposal.
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V. Wastewater Treatment Systems
The wastewater treatment system at the IU must be operated and maintained in a manner
which allows the system to prevent the discharge of pollutants in excess of the Ill's permit limits.
The treatment system is at the heart of the ID's ability to control its discharge of pollutants.
Therefore, it is necessary for the inspector to spend some time to evaluate the treatment system's
condition and use/operation. The inspector should check for the following items: equipment
maintenance record keeping or lack of preventative maintenance; instrument calibration frequency;
critical spare parts inventory; inadequate detention time or inadequate mixing in the pretreatment
tanks; improper chemical dosage; impoper meter settings; stale chemical use; and current operational
status. (NOTE: not all of these items are contained in the checklist, but should be noted in the
comment section at the end of the checklist).
Vi. Sludge Generation/Waste Disposal
How the IU handles its solid waste is an indication of its commitment to the .proper handling
of all its wastes, liquid or otherwise. The inspector should examine the lU's sludge disposal methods
to ensure that no sludge from the treatment system is being discharged to the sewer (except in
accordance with a permit). If the facility produces hazardous wastes (e.g., electroplating sludge), the
inspector should verify where the waste is being ultimately disposed. Make sure that each applicable
box is filled in (Y/N'NA stands for Yes, No, and Not Applicable).
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VIL Combined Wastestream Formula/Permit Limits
Can flow he measured at all sampling locations'.' Are flows measured at each sampling location?
What type of measuring device is used?
Are dilution wastestreams present at the sample location? Is the C'WF used at the facility':'
How are the flows determined' Is the facility using dilution to meet its effluent Iimits3
Should the facility he using the combined wastestream formula?
Are there any new flows which need to be considered in the application of the combined wastestream formula?
Are there any dilution flows which have not been accounted for?
VIII. Chemical Storage
What chemicals are used ut the facility.' Can chemicals reach floor drains if spilled:?
Is chemical containment needed?
How often are floors washed'' What chemicals are used?
How often is equipment washed7 What chemicals are used?
Does the facility have a slug control program ?
Has the facility had any past slug discharges? Amount of water used in washdowns (gals).
IX. Production/Process Areas .of the Industrial User
Are wastestreams separated at the facility? (Y/N) Arc incompatible materials separated? (Y/N)
Do floor drains/troughs lead to the PO7W? (Y/N) Are temporary hoses in place as part of production ?
Are pipes labelled/color coded for easy identification? Is a piping diagram available al the facility?
Attach a schematic of production, wafer flow, wastewater production, and a stepwise description of the production
process at the facility.
Attach a stepwise description of the chemicals used and/or discharged during production.
Overall Inspection Comments
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VII. Combined Wastestream Formula/Permit Limits
If the CWF is being used to calculate alternative discharge limits, the flow of each waste
stream must be known and measurable. The inspector should ensure that flow can be measured at all
necessary points and that flows are being measured correctly at all locations. The inspector will need
to evaluate any dilute streams being discharged to the sewer and whether these streams are being used
to meet any permit limits. Dilution streams for purposes of the CWF include: sanitary wastewater,
boiler blowdown. non-contact cooling water or blowdown, deionizer backwash, cooling tower
bleedoff condensate, and rainwater/stormwater. If it appears that dilution or unregulated streams are
being co-mingled with regulated streams prior to treatment, then the inspector should initiate the
procedure to have the permit changed and new limits applied (as well as initiating any applicable
enforcement action as dictated by the POTW's Enforcement Response Plan). In addition to dilution
streams, the inspector should check for any unregulated streams at the facility. Unregulated
wastestreams for purposes of the CWF include: any wastestream which is not currently regulated by
a categorical pretreatment standard and does not meet the definition of a dilute stream. Determining
such unregulated wastestreams requires a familirity with the categorical industry in question, and
probably will require some research into the Development Document issued by the EPA. Refer to the
EPA Guidance Manual on the use of the combined wastestream formula which is listed in Appendix
XII.
VIII. and IX. Chemical Storage and Production/Process Areas of the Industrial User
II is important for the inspector to trace the use of all process (and non-process) chemicals
which may be discharged to the sewer. Areas of spill containment, floor drains, and the
manufacturing process should be examined to determined which chemicals are (or can) find their way
into the sewer. The inspector should verify that incompatible chemicals (e.g., strong acids and bases,
or chemicals which may interact to form toxic compounds) are not stored near each other in the event
of a spill. It is best for the inspector to follow the chronological sequence of the production process
in the step wise sequence of production to comprehend the activities at the plant. (NOTE: Do not
allow the 1U contact to "control" the inspection or the sequence of the inspection. How the inspection
is conducted is up to the inspector alone). Once the inspector understands the operation at the
facility, a schematic of the production/manufacturing process, water use and wastewater production,
and a stepwise description of all chemicals used or discharged during production should be developed
and compared on subsequent inspection visits.
The inspector should also check the production area for the following conditions: excessive
drag-out and/or spillage from plating lines; excessive water on the floor and its entry points to the
sewer system; and labelling of all tanks used in the production process.
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General Inspection Comments (cont.)
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III. SAMPLING INDUSTRIAL USERS
Introduction
Analytical Methods
Quality Assurance and Sampling Plan
Standard Operating Procedures
Pre Sampling Activities
Cle;
nng am
eanmg
eanjng
eanmg
eanin
Prep ration of Sampling Equipment
^rocedures tor Conventional Pollutants
rocegures _.__
3rocedures for Oil and Grease
.._-0 Procedures for Organic Analyses
Volatie Organic Compounds
, Sera-Volatile Organic Compounds,, etc.
Cleaning,.of Automatic Sampling Equipment
Preparing Tield Instruments
Residual Chlorine Meters
Temperature
n Dissolved Oxygen. .
Selection and Preparation of Sample Containers
Type of Sample
On-site Activities
ins Location , .
Dllection Techniques
e Volume. , ,,.
e Preservation and Holding Times
e Documentation
. e Identification and Labelling
..jn-of-Custo.dy
imp e Packaging and Shipping
'uahty Control
53
55
56
Safety Considerations During Sampling
79
71
Physical Hazards
""---'lencHaj
" pci
Explosive Atmosphere '
Atmospheric Hazards
Oxygen Deficient Atmosphere
Exoioi
Toxi
xic Atmosphere
Safety Equipment .
Protective Clothi
.'rotective uotnin
Traffic Control
Radio . . .
Air Momtonng Devices
Ventilation Devices
Safety Harness and Retneval System
Coniinea Space Entry
Safety Training
Flow Measurement
. Channel Flow
-jmary Devices
Secondary Devices
el Flow
Quality Assurance and Quality Control
94
Compliance Issues Related to Industrial User Sampling 9 9
Summary 104
INTRODUCTION
An effective local pretreatment program must include the ability to collect and analyze wastewater
samples such that laboratory results are of high quality, defensible and able to support the two primary goals
of the Pretreatment Program. The first goal is to determine the Impact of Industrial wastes from a particular
industry or group of industries on the Publicly Owned Treatment Work's (POTW) collection and treatment
system, including the impact on treatment plant operations, sludge management (including final use or
disposal), and receiving stream quality. The second goal is to evaluate compliance by all industrial users
with applicable pretreatment standards and requirements. In addition to these primary objectives, the POTW's
sampling and analysis program is designed to satisfy one or more of the following program objectives:
Verity the quality of self-monitoring data;
Verify chat sampling location(s) specified in the permit are adequate;
1 Verify compliance with daily maximum effluent limits (local limits or categorical standards);
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Industrial User Sampling Manual Chapter 3 - Sampling industrial Users
Support enforcement actions;
Support local limits development; and
Support permit development/reissuance and revision
These objectives can only be supported if the data produced by sampling are adequate. The quality of
the data resulting from the POTW's sampling activities can be ensured by using the following procedures and
techniques: collecting representative samples; maintaining the integrity of samples through proper handling
and preservation; adhering to appropriate chain-of-custody and sample identification procedures; and
practicing adequate quality assurance and quality control activities. This chapter outlines each of these areas
in detail.
Sampling and analysis of wastewater can be done independently or in conjunction with a compliance
inspection visit, and can be performed by the same or different POTW personnel. If sampling and analysis
are performed independently and by POTW personnel different from the inspection personnel, it is strongly
recommended that the sampling personnel familiarize themselves with the procedures and guidelines used by
the inspection personnel. Chapter Two of this manual provides a recommended framework for conducting
inspections at regulated lUs. Sampling, just like inspections, can be announced or unannounced. The goal of
your sampling visit will determine whether the industry is notified. As with inspections, routine compliance
sampling should be conducted based on a "neutral" scheme (see discussion in Chapter 2). These routine
compliance sampling visits should be unannounced. Sampling visits which are in response to known or
suspected problems or in response to a complaint should also be unannounced so that the facility does not
have time to alter any of its activities.
In the pretreatment program, the vast majority of sampling will be routine compliance evaluation
sampling mandated in 40 CFR 403.8. In these situations, it is necessary for the POTW to ensure that the
sampling data collected will be of a quality sufficient for the POTW to draw a proper conclusion about the
compliance status of the facility and to ensure that the data will be viewed as credible evidence substantiating
the POTW's position should an enforcement action be pursued. This is the fundamental objective of any
sampling carried out for compliance and enforcement purposes, and even, perhaps, when developing local
limits, since the basis for these limits must be justifiable and defensible. Rut there may be situations where
other types of sampling may be used by the POTW. This sampling can be conducted for a variety of reasons
(e.g., operation or maintenance evaluations). These sample objectives would not involve as comprehensive a
set of procedures as a compliance sampling visit, which results in evidence that may be used in court. If a
sample is to be used for other than compliance evaluation purposes, it need not comply with the strict
requirements of compliance sampling (i.e., to obtain results which are admissible in court). However, if a
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Industrial User Sampling Manual Chapter 3 - Sampling Industrial Users
sample is obtained using approved sampling and analytical procedures, then the results of the sampling must
be reported to the POTW
This chapter presents a detailed and comprehensive framework to be used by POTW sampling personnel
when conducting sampling and flow measurements at regulated industrial users. The purpose of the chapter is
to familiarize POTW inspectors with proper sampling procedures and to establish consistent procedures for all
POTWs with approved local programs. The goal of this chapter is to assist POTW personnel in planning and
conducting sampling activities at industrial facilities which discharge to the POTW. The chapter is divided
into six sections to accomplish these objectives: analytical methods, quality assurance and sampling plan,
standard operating procedures, pre-sampling activities, on-site sampling activities, safety considerations during
sampling, flow measurement, and quality assurance and quality control. In addition to these sections, this
chapter presents a concluding section on Compliance Issues Related to Sampling and Analysis. This section
discusses specific compliance issues related to the POTWs and ILTs compliance monitoring program and
provides recommendations for handling certain compliance information. POTW sampling personnel are
encouraged to read and understand the material presented in this chapter before beginning any sampling
activities.
ANALYTICAL METHODS
The National Pretreatment Program requires that samples be analyzed using the approved methods listed
in 40 CFR 136 (40 CFR 403.l2(gX4)). The methods in 40 CFR 136 are derived from five different sources:
(I) Methods for the Chemical Analysis of Water and Wastes, F.PA-600/4-79-020, revised March, 1983; (2)
Standard Methods for the Examination of Water and Wastewater, (specified edition); (3) ASTM; (4) Methods
for Analysis of Inorganic Substances in Water and Fluvial Sediments • USGS; and (5) additional sources.
Not all methods listed in each of these documents are approved in 40 CFR 136. Therefore, the POTW (and
IU) must use the methods listed in Part 136 or apply for an alternative method. POTWs and lUs can apply
for such an alternate test procedure if they believe that a method not listed in 40 CFR 136 is a better method
of analysis and can prove that the proposed method of analysis is comparable to the method listed in 40 CFR
136. This alternate method must be approved by the EPA if the results are to be used to comply with 40
CFR 403.12(gX4). The POTW is not allowed to grant this variance in analytical methods. The application
and approval procedures for instituting an alternative analytical method are outlined in 40 CFR 136.4 and
136.5
Choosing the appropriate analytical method for the samples collected is an important task. If more than
one method is listed for a parameter (which is common), the method which is chosen should be based on the
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Industrial User Sampling Manual Chapter 3 - Sampling Industrial Users
effluent limit in the permit, Sewer Use Ordinance, and/or Federal Categorical Standard. An example of how
to choose the correct analytical method can be illustrated using the pollutant parameter lead. Lead can be
analyzed using HPA methods 200.7, 239. I, and 239.2. For our example, let's assume that the established
eflluent limit for lead is 15 ug I. The detection limit for lead using EPA method 200.7 is 42 ug/1. The
detection limit for lead using EPA method 239.1 is 100 ug/'l. The detection limit for lead using EPA method
239.2 is I ug I. Methods 200.7 and 239.1 should not be used because the detection limit for the method is
higher than the permit limit. Therefore, any results reported, even a non-detect, could be viewed as an
excursion from the permit limit. The appropriate method of analysis in this example is EPA method 239.2.
and this method should be specified to the analytical laboratory. (NOTF: the actual detection limits for these
methods will vary with different matrices). In addition, laboratories must establish their own method
detection limits using Appendix B to 40 CFR 136 - Revision 1.1 1. In addition, the impact of sample dilution
and elevated detection limits should be evaluated by the POTW If a sample must be diluted to get one or
more analytes on-scale within the linear range of the calibration curve, the detection limit for any non-
detected parameter must be elevated accordingly. For example, if a detection limit for analyte A was 10 ug/'l
and a sample was diluted 1:4 to get another analyte on-scale, then the detection limit for analyte A in that
sample must be elevated to 40 u& I. The POTW must be aware of this situation when evaluating the
appropriate detection limits and analytical methods for sample analysis.
QUALITY ASSURANCE AND SAMPLING PLAN
A fundamental step in setting the objective(s) of a sample collection effort is to establish clearly the
ultimate use of the data. Refore sampling at an industrial user, the inspector should understand clearly the
data needs (i.e., for what purpose will the data be used, e.g.. compliance determination) and the data quality
objectives of the site visit (e.g., a compliance determination will require data which are admissible in court).
When the data resulting from the sampling become available, it is crucial that it be possible to assess the
quality and utility of the data in meeting the sampling objective. Once the inspector understands the needs
and objectives of the site visit, a complete and comprehensive quality assurance and sampling plan can be
developed. The plan should be documented in written form and completed prior to initiating any sampling
activities. This plan ensures that each sampling effort goes through a careful thought process before it is
undertaken. The U.S. EPA Quality Assurance Management Staff (QAMS) has developed documents which
will be useful to the POTW when developing their QA and Sampling Plans. It is recommended that POTWs
contact their U.S. EPA Regional QAMS or QA Managers for copies of model QA and Sampling Plans to use
as guidance in preparing their own plans. At a minimum, the QA and Sampling Plan should include the
following elements:
. Sampling Location^): Sampling locations should include all outfalls that appear in the lU's permit.
Due to accessibility, needs, and objectives of the sampling, and/or safety hazards, the sampling
location specified in the permit may not be adequate. Therefore, locations other than those specified
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Industrial User Sampling Manual Chapter 3 - Sampling Industrial Users
int he lU's permit may need to be sampled. The number of samples at each location should also be
specified in the Ill's permit. In addition, the inspector should sample any outfalls which are not
included in the lU's permit because they may represent illegal bypasses or other illegal discharges.
Type o/Sample: The type of sample depends on the parameters to be measured and/or the discharge
characteristics (e.g., batch discharge). This information may be specified in 40 CFR 136 and should
be specified in the ILTs permit.
Type of Flow Measurement: The type of flow measurement is dependent on the flow rate, the
condition of the wastewater, and the variability of the discharge. Flow measurements are necessary to
determine the mass loadings of a discharge. The adequacy of the permittee's flow measuring device
should be verified at the time of sampling.
. Parameters for Analysis: The ID permit should specify the pollutant parameters to be monitored by
the permittee, and these parameters should be specified as either mass- or concentration-based
discharge limits, These parameters must 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 if new or
added sources of wastewater are evident. If new processes or products have been introduced in the
plant, additional sampling will help provide the basis for necessary permit modifications. (NOTE: The
IIJ is required to notify the POTW in advance of any substantial change in the discharge from the
facility. Failure to do this, as discovered during the inspection or sampling visit, should be addressed
with an appropriate enforcement response as specified in the POTW's Enforcement Response Plan).
. Sample Volume: The volume of sample collected depends on the type and number of analyses to be
conducted. The volume of the sample obtained should be sufficient to perform all the required
analyses (including laboratory QA/QC and repeat analyses) plus an additional amount to provide for
any split samples that may be required. A summary of required sample volumes for various pollutants
is provided in Table 3-3 at the end of this chapter, but it is still best to check with the individual
laboratory to determine the sample volume which it requires.
. Type of Sample Containers: The selection and preparation of sample containers are based on the
parameters to be measured and wastewater characteristics. Required containers are specified in 40
CFR 136 and are summarized in Table 3-4.
. Sample Preservation Techniques: To preserve samples correctly, the appropriate chemicals must be
used and temperature control must be ensured. Preservation techniques and maximum allowable
holding times are specified in 40 CFR 136 and are summarized in Table 3-4 at the end of this chapter.
. Sample Identification Procedures: Each container should have an acceptable identification label so
that the sample can be tracked accurately and an uninterrupted chain-of-custody can be maintained.
. Sample Packaging and Shipping: Once a sample is collected, it must be delivered to the laboratory
for analysis within the prescribed holding time. The manner of packaging and shipment must be
addressed through the sampling plan.
. Safety Concerns: Sampling personnel should have complete information on any relevant plant safety
regulations and safety procedures to be followed during on-site sampling activities.
. Hazardous Waste: Samples of potentially hazardous waste; samples with extremely high or low pH;
and samples that may contain toxic, volatile, or explosive substances will required special handling.
DOT regulations for shipping these types of wastes must be followed.
. Chain-of-Custody Procedures: Procedures for chain-of-custody must be followed for all samples
collected by the POTW. and standard chain-of-custody forms should be used for this purpose (see
Appendix X for an example Chain-of-Custody form).
. QA/QC Procedures: To ensure that the data collected are valid, systematic checks must be conducted
to verify that the sample results are sufficiently accurate and precise to evaluate the compliance status
of the facility being sampled.
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Industrial User Sampling Manual Chapter 3 - Sampling Industrial Users
Several of these items must be coordinated with the lab. Therefore, the inspector should contact the lab
in advance of any sampling to discuss the sampling plan and QA/QC procedures, to allocate lab time, and
obtain sample identification numbers and field trip blanks.
Once the sampling plan is developed, it should be followed when conducting sampling at the industrial
users regulated by the POTW's approved pretreatment program. The procedures in the plan should be
followed closely to ensure that all the information collected can be used for its intended purpose. This is
especially critical when the sampling data is to be used for compliance evaluation (which accounts for the
majority of the data collected by the POTW). However, in certain situations, the inspector may be forced to
alter some items in the plan due to uncontrollable circumstances at the industrial user. The inspector has
discretion to change some items in the QA Plan if. in the opinion of the inspector, circumstances at the
facility warrant such a change. Whenever, possible, however, the elements in the QA Plan should be
followed.
STANDARD OPERATING PROCEDURES (SOPS)
Once the sampling plan has been established, the POTW should develop specific standard operating
procedures (SOPs) for on-site sampling activities. SOPs can be a document or sef of documents which
explain, in step-by-step detail, how sampling will be conducted by the POTW. The SOP developed by the
POTW should include all elements of sampling, including:'
• Sample Documentation: Documentation is an integral part of any pretreatment program. The
validity of the samples collected and the data obtained both in the field (e.g., pH and flow) and in the
laboratory (i.e., chemical analyses) is ensured through documentation and record keeping. All the
information documented must be complete and accurate. Failure to maintain records and
documentation according to set procedures could result in these documents being deemed inadmissible
as evidence in court. The POTW should include the following records in their SOP:
Field Data Record - The Field Data Record is the primary sampling information document and
should include: the sample site identification; the type of sample taken; sampler identification;
settings on the sampler; results of field analyses; flow information (where applicable), and any
additional information related to the site or effluent characteristics.
Field Documentation Log - The Field Documentation Log is used to record which sites are
sampled each day, and any violations, conversations or other notable occurrences during the
sampling visit.
Field pH Calibration Log - The Field pH Calibration Log is used to record the calibration of the
field pH meter during the sampling event. The field pH meter must be calibrated at each site
prior to measuring the pH of the effluent. Calibration and slope should be checked, adjusted as
necessary, and recorded, along with the temperature of the buffer.
Flow Meter Calibration Log - The Flow Meter Calibration Log is used to record program
information for the flow meter and water level calibration from the initial value shown on the
flow meter to the actual measured water level.
1 The discussion of Standard Operating Procedure elements was taken from the "Standard Operating Procedures
Manual: Pinellas County Sewer System Industrial Monitoring Program, " January, 1989.
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pH Meter Calibration (Laboratory) - The laboratory should maintain its own notebooks to record
equipment calibration. When the laboratory pH meter is used, it must be calibrated. The
discussion of how to calibrate the meter should be included in the SOP under the calibration
procedures section. Once the meter is calibrated, the results should be recorded in the
(laboratory) pH Meter Calibration Log Book.
- pH Calibration/Spike Checklist • The pH Calibration/Spike Checklist is used to record the date
and time of field pH meter calibration, calibration data, results and true value for the known
sample, and to document the buffer and fill solution changes.
Chain-of-Custody Form - The Chain-of-Custody Form includes sample collection information
(i.e., who collected the sample, when the sample was collected, what type of sample was
collected, and who received the sample after the initial sample was taken), types of analyses to be
run by the lab, preservation technique used, and a space for the lab personnel to sign with the
date and time the sample was received by the lab.
. Chain-of-Custody: The overall success of a sampling program (whether by the POTW or the
industry) depends on its ability to produce valid data through the use of accepted sampling procedures
and protocols, and its ability to substantiate such data through documentation. The success of
documenting samples depends on the faithful use of chain-of-custod> forms by all involved personnel.
The SOP should include the chain-of-custody form.
. Safety: The SOP should outline the many safety precautions which must be followed both at the
office and in the field. Industrial monitoring, by its very nature, adds additional hazardous situations
to those existing in any field sampling situation. All safety procedures should be outlined in the SOP.
• Cleaning: Sampling equipment, grab and composite collection containers, sample bottles, and tubing
should be cleaned at a specified frequency outlined in the SOP. All cleaning procedures should also
be included in the SOP.
. Maintenance: Maintenance activities ensure the constant reliability of sampling equipment, including
flow meters. The SOP should outline a maintenance schedule for all equipment related to sampling.
. Calibration: Calibration of field and lab equipment is crucial to the continued reliability of the
sample results obtained from sampling. A regular schedule of calibration should be included in the
SOP and should be adhered to strictly. This calibration should include flow meters, pH meters, and
any other equipment requiring calibration, as recommended in the manufacturer's specifications.
• Sampling Preparation: Sampling preparation is the most important part of a successful sampling
event. Standard sampling checklists should be included in the SOP and should outline all sampling
preparation procedures.
. Types of Samples/Sample Methodoloev: There are two basic types of samples: grab and composite.
The ID permit should establish the sample type, and this sample type should be used by the POTW
when collecting samples.
• Field Analyses: Certain measurements are typically performed in the field (e.g.. flow, pM, and
temperature). Detailed procedures for conducting these analyses should be included in the POTW's
SOP.
Each of these areas is discussed in greater detail later in this chapter, and a copy of the Pinellas Count) SOP
is included as Appendix IX. Each POTW should review its SOPs to ensure that all necessary areas arc
covered in adequate detail using Appendix IX as a guide.
Once the SOPs are written, they should be followed closely. Any deviation from a SOP may create
potential problems or weaknesses in a subsequent enforcement action taken by the POTW against a
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noncompliant industrial user. If the POTW establishes clearly identified SOPs and follows those procedures
when conducting on-site sampling activities, it is unlikely that an industry could challenge the results of the
POTW's sampling results. If circumstances arise in the field which make it unrealistic or physically
impossible for the SOPs to be followed, the inspector should document any deviation from the written SOPs
and the reason for the deviation.
PRE-SAMPLING ACTIVITIES:
The success of each sampling task hinges on adequate preparation. Because POTW personnel may not
be familiar with the facility to be sampled, a sampling plan should be developed prior to going out into the
field. Once the POTW sampling plan is in place for a particular industrial user, inspection personnel should
follow the plan when conducting on-site sampling. Inspection 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 (e.g.. pH), the necessary instruments should also be included. Equipment must be checked prior to
going into the field to ensure accurate operation and calibration. In addition, a review of necessary safet>
equipment should be made and the inspector should be aware of any potential hazards at the facility. The
inspector and plant staff should discuss any unusual circumstances and formulate a plan for dealing with them
in advance of the site visit.
A checklist of field sampling equipment should be used to ensure proper preparation. An example of
such a list is outlined in Table 3-1. When the type of waste to be sampled is known ahead of time, the list
can be narrowed to the actual pieces necessary for the specific sampling required.
Cleaning and Preparation of Sampling Equipment
The cleaning and preparation methods for sampling equipment will vary depending on the parameters
being sampled. This section addresses the cleaning and preparation of sample collection vessels and/or
sample bottles for conventional pollutants (TSS, BOD, fecal colifonm, oil and grease and pH), metals, and
organic pollutants. Many vendors now sell precleaned sample bottles with varied cleaning specifications. It
is recommended that a bottle blank be run when analyzing the samples to verify that the bottles are not a
source of sample contamination. One bottle blank is recommended per LOT number.
Cleaning Procedures for Conventional Pollutant Parameters (BOD and TSS only):
When sampling for the conventional pollutants BOD and TSS, it is necessary to clean the sample bottles
and/or collection vessels prior to each sampling visit. The recommended cleaning procedure involves: (I) a
detergent wash, (2) tap water rinses, and (3) deionized water rinses. This procedure forms the basis for
almost all further cleaning procedures required for other pollutant parameters when preparing sampling bottles
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Table 3-1
Checklist of Field Sampling Equipment
Sampling Equipment:
. Container for contaminated material
. Waterproof container labels
. Ambient air monitor
• Field document records
• Vermiculite or equivalent packing
. Thermometer
• Colorirnetric gas detection tubes
. pH equipment
• Eixplosimeter (atmospheric testing device)
• Tubing, tape and rope
• Field sampling logs
. Sample shipping forms (w lab phone PS)
. Graduated cylinder
• Preservatives (e.g., nitric acid and NaOH)
• Siphoning equipmenl
• Weighted bottle sampler
• Liquid waste samplers
. Auger, trowel, or core sampler
• Scoop sampler
. Sample bottles/containers (certified clean
bottles)
• Ice chest
• Flow meter (if applicable)
• Preservat ives
• Chain-of-custody forms
• Custody seals and tags
• Strapping tape
• Field test kits (pH, etc.)
. Automatic or composite sampler
or vessels.
Cleaning Procedures for Metals Sampling:
When preparing for metals analysis, it is necessary to preclean the sample bottles and or vessels (either
purchased precleaned or cleaned manually). The cleaning procedures for preparing sample bottles for metal
analyses is provided in 40 CFR 136, Appendix C, Section 8 (ICF method 200.7) [NOTK: This method is not
applicable for atomic absorption analysis], along with the documentation on the analytical method in Methods
for Chemical Analysis of Water and Wastes,
1983. The cleaning process for metals
sampling and analysis is outlined in Figure 3-
Figure 3-1 Metals Cleaning Procedures
Chromic acid may be used to remove
organic deposits on glassware. If chromic
acid is used, extreme care must be taken to
ensure that the glassware is thoroughly rinsed
to remove all traces of the chromium. It is
recommended that chromic acid not be used
for cleaning sampling bottles if chromium is
one of the parameters being analyzed.
Use the following procedures when cleaning sampling
bottles and/or vessels for metals sampling and analysis:
1) Detergent wash
2) Tap water rinses
3) (1:1) Nitric acid rinse
4) Tap water rinses
5) (1: I) Hydrochloric acid rinse
6) Tap water rinses
7) Deionized distilled water rinses.
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Cleanine Procedures for Oil and Crease:
The approved method of analysis for Oil and Grease is gravimetric extraction (Standard Methods for the
Examination of Water and Wastewater, 17th edition, 1989. method 155208 or Methods for Chemical
Analysis of Water and Wastes, 1983. method Ml3.1). When sampling for oil and grease, it is necessary to
use a wide mouthed glass jar, which has been rinsed with the solvent used in the extraction process.
Currently, freon is used as the solvent in this process. A substitute for freon is currently being researched and
may result in an alternative analytical method. The cleaning method for oil and grease is the following: (I)
detergent wash; (2) tap water rinses: and (3) solvent rinse. It is recommended that the sample bottles have a
teflon-lined cap. If this is not possible, there should be either aluminum foil or cut teflon pieces which cover
the areas where the bottle and the cap meet. The teflon or aluminum foil used must also be prepared,
following the same cleaning procedures as the sample bottle.
Cleanine Procedures for Oreanic Analvsis:
Volatile Organic Compounds
Generally, the glassware used to collect volatile organic samples is precleaned. When glassware needs to
be cleaned, the procedure in 40 CFR 136 may be followed. EPA method 624 states that the vials and the
septa must be cleaned as follows: (I ) detergent wash; (2) tap water rinses; (3) distilled water rinses; and (4)
drying at I05°C.
Semi-volatile Organic Compounds, Organochlorine Pesticides, and PCBs
Semi-volatile organic samples should be collected in amber bottles according to 40 CFR 136, Methods
625 and 1625. Organochlorine pesticides and PCB samples should also be collected in amber bottles
according to 40 CFR 136. Method 608. If amber bottles are not available, the samples must be sheltered
from the light The sample bottles (including cap liner, either teflon or foil) and the collection vessels for
semi-volatile organic compounds, Organochlorine pesticides, and PCBs must be cleaned by the following
procedure: (I ) detergent wash; (2) tap water rinses; (3) distilled water rinses; (4) solvent rinse (method 625
lists acetone or methylene chloride); and (5) drying. If one or more of the samples'is being collected in a
sampling vessel, the sampling vessel must be cleaned for all parameters. Examples of this include:
• Sampling for conventional pollutant analysis and metals analysis: the collection vessel must be
detergent washed and then acid washed (following the steps for metals cleaning listed above).
• Sampling for metals analysis and semi-volatile organic analysis: the collection vessel must be acid
washed (following the steps above) and then solvent rinsed. The initial steps in the semi-volatile
organic cleaning do not need to be repeated in this case (only the solvent rinsing), since they were
already done in the metals cleaning procedure.
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Cleaning of Automatic Sampling Equipment:
Generally, the sampler tubing and inner parts of the sampler (e.g., distribution arm, S-tube, and
compressed silicon tubing) which come into contact with the effluent are cleaned using the following
procedure: (1) detergent wash, (2) tap water rinses, and (3) distilled water rinses. If the sampler is to be used
to collect semi-volatile organic and/or organochlorine pesticide and PCB samples, additional cleaning is
required. 40 CFR 136, Methods 625 and 608, respectively, states that the automatic sampler must be as free
as possible of contaminants in the Tygon tubing and any other potential source of contamination. One
suggestion for the replacement of Tygon sampler tubing is the use of teflon tubing. These methods also state
that if the sampler has a peristaltic pump, a minimum length of compressible silicon rubber tubing may be
used. Before it is used, the compressible silicon tubing must be cleaned using the following procedure: (1)
methanol rinse, and (2) distilled water rinses. If the sampler used has an S-tube, it must be cleaned b>
following the same procedure as for the sample bottles for semi-volatile organic compounds, organochlorine
pesticides, and PCBs. As an alternative, some POTWs may prefer to replace tubing prior to each use of the
automatic sampler.
Preparing Field Instruments
The most common parameters tested in the field are: pH, residual chlorine, temperature, and dissolved
oxygen. For these four parameters, 40 CFR 136 states that they must be analyzed immediately. 'ITie term
"analyze immediately" means that the parameter should be analyzed wilhin 15 minutes of the sampling.
These analytical parameters cannot be preserved, and therefore, must be analyzed in the field. The electronic
and photometric instruments used to monitor these different parameters should be checked prior to leaving the
office. The instruments should be in good condition, have charged batteries, be calibrated, and have all
appropriate standards already made. If an instrument is calibrated in the office prior to going into the field, if
must be recalibrated once you reach your sampling location.
pH Meters:
In the field. pH samples are analyzed using a portable pH meter. The meter may either analyze
individual samples or do continuous readings with a recorder (e.g., strip chart), ptl meters must have a
minimum of two point calibration (see EPA method 150.1 section 7). (NOT! : If there are separate
manufacturer's specification for calibration, these procedures must be followed. Otherwise, use the
procedures outlined in the remainder of the paragraph). The pH meter should be calibrated using two fresh
buffer solutions. The buffers that are used to perform the calibration should bracket the expected pH range of
the wastewater that is being sampled and should be at least 3 SU or more apart. If the buffer solutions are
bought already made, it is important to note their shelf life and dispose of buffers when their expiration date
has passed. A log book with calibration information for the pH meters should be maintained. This allows
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the inspector to track when a pM probe needs to be changed or when batteries start to fail. Remember, the
meter must he recalibrated once the sample location is reached.
Residual Chlorine Meters:
The manufacturer's specifications should be followed for calibration. Portable spectrophotometric, DPD
meters are an approved method of anal)sis listed in 40 CFR 136. Other instruments, such as portable
amperometric titrators, can also be taken into the field to detect low levels of chlorine (100 ug/1). The
permits limit, local limit, or Sewer l.'se Ordinance limit will determine the appropriate method of analysis.
Temperature:
A mercury-tilled thermometer, a dial type Celsius thermometer, or a thermistor must be used to make a
temperature determination. The measuring device used must be routinely checked against a National Institute
of Standards (MS I') traceable thermometer. Hi is check should be recorded in a calibration log book with the
date, both temperature readings (reference and actual), and any correction which was made to the temperature
measuring device. l"he calibration log book could be an important document in an enforcement case, if
temperature violations were noted during the inspection.
Dissolved Oxygen:
Dissolved oxygen measurements can be taken either using the Winkler or the electrode method, If the
Winkler method is used, the samples must be fixed (preserved) on-site. stored in the dark, and analyzed
within eight hours. JO CFR 136 requires that if the electrode method is used, the sample must be analyzed
immediately (see Table 3-4 at the end of the chapter for a summary of this information). Prior to each
sampling, the D.O. meter should be calibrated. The manufacturer's specifications for calibration should be
followed. Generally, the D.O. meter is calibrated to a solution of known D.O. concentration (usually
saturated) or to moist air. A calibration record should be maintained (including date, D.O. readings, any
adjustments, date a new probe is added, etc.). If a membrane electrode is used, great care should be used
when the membrane is being changed to avoid trapping air bubbles under the membrane. Trapped bubbles
will result in inaccurate D.O. readings.
Selection and Preparation of Sample Containers
The selection and preparation of sample containers must be made prior to going out into the field.
Sample containers must be made of chemically resistant 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 (i.e.. SOPs). If either type of sample container is acceptable and available, the inspector
should use plastic containers since they are less likely to break POTWs should develop specific acceptance
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criteria (i.e., chemical\parameter concentration) for each type of sample container to be used. An example of
such criteria (as well as sample container preparation procedures) may be found in the U.S. EPA document
"Specifications and Guidance for Contaminant-Free Sample Containers," EPA 540/R-93/05 1, December, 1992.
Although this document was prepared for solid waste applications, it gives an idea of the types of
requirements POTWs should have for sample containers. Sample containers, preservatives, and holding times
are specified in Table 3-4 and in 40 CFR 136.
Glass sample bottles are required when collecting samples for organic priority pollutants, oil and grease,
and phenols, while plastic sample bottles are most often used for Biochemical Oxygen Demand (BOD), Total
Suspended Solids (TSS), metals, and nutrients. Containers with wide mouths are recommended to facilitate
the transfer of samples from the sampler to sample containers (for automatic samplers). In addition, the
container must be large enough to contain the required volume for laboratory analysis. The inspector should
use dark containers for samples that contain constituents which will oxidize from exposure to sunlight (e.g.,
iron cyanide which oxidizes to hydrogen cyanide).
Container lids and closure linings must also be intact so they do not interfere with the pollutant
parameters to be measured. Most containers have tight, screw-type lids. Plastic containers are usually
provided with screw caps made of the same material as the container, so cap liners are usually not required.
Glass containers usually come with rigid plastic screw caps. Liner materials may be polyethylene,
polypropylene, neoprene, or teflon.
The inspector should make sure that all sample containers are clean and uncontaminated. The general
cleaning procedure for a sample container was outlined previously and should be followed whenever samples
are taken. All tubing and other sampling system parts must be scrubbed with hot water and detergent, rinsed
several times with tap water, and then rinsed with distilled or deionized water. Further rinsing with acetone is
advised only when the type of tubing (e.g., teflon) is not susceptible to dissolution by the solvent. In most
cases, the container should be rinsed three times with the wastewater to be sampled before the sample is taken
(NOTE: Except when sampling for oil and grease, volatile organic compounds, and coliform bacteria. In
these situations, the sample container should not be rinsed with the wastewater prior to sampling). 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. Table 3-4 outlines required sample containers, sample preservation and
sample holding times.
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Type of Sample
"I"he type of sampling which will be undertaken at the 1U must be understood clearly prior to going out
into the field and should be outlined in the POTW's Quality Assurance and Sampling Plan and SOP. There
are two basic types of samples: grab samples and composite samples. Each type of sample has distinct
advantages and disadvantages. To obtain a complete characterization of a specific facility's effluent, the two
sample types may be used in combination. However, the inspector must use the appropriate sample type for
compliance monitoring. For determining compliance with all applicable requirements, the inspector must use
the sample method established in the industrial user's permit. (NOIT If the sample method is inadequate the
inspector should take two samples, one with the permit sample method, and the other with the sample method
which the inspector deems more appropriate). In this situation the permit should be modified to reflect the
appropriate method. It is very important that the POTW establish specific procedures for collecting grab and
composite samples. These procedures must be consistent with the EPA guidance on grab versus composite
sampling which was distributed to all POTWs with approved pretreatment programs and all of the EPA
Regional Offices (No It;: See Appendix V for a copy of this guidance). Copies of this policy can be obtained
from the Regional Pretreatment coordinators. Once the POTW has established its procedures for taking grab
and composite samples, the IU permit should be modified to incorporate these specific procedures so that the
1U is held to the POTW's procedures.
A grab sample is an individual sample collected over a period of time not to exceed 15 minutes. Grab
samples are usually taken manually, and the sample volume depends on the number of analyses to be
performed. The sampler must make sure that sufficient volume of sample is taken to conduct all necessary
analytical procedures, including QA QC. Grab samples represent the conditions that exist at the moment the
sample is taken and do not necessaril> represent conditions at an> other time. Grab sampling is the preferred
method of sampling under the following conditions:
• When the effluent is not discharged on a continuous basis (i.e., batch discharges of short duration),
and only when the batch is continuously stirred (i.e.. well-mixed) and the pollutant can be safely
assumed to be uniformly dispersed.
• When sampling wastewater from an electroplating facility regulated under 40 CKR 413, if it has been
demonstrated that the single grab sample is representative of the daily discharge.
• When sampling a facility where a statistical relationship can be established between previous grab
samples and composite data.
• When the effluent is being screened to see if a parameter is present (NOTE: This is only true when
the sample is well-mixed and representative of the discharge).
• When the waste conditions are relatively constant (i.e., are well-mixed and homogeneous) over the
period of the discharge. In lieu of complex sampling activities, a grab sample provides a simple and
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accurate method of establishing waste characteristics.
. When a POTW or State has adopted an instantaneous local limit which is based on grab samples;
. When it is necessary to check for extreme conditions. For example, composite sampling 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. Therefore, composite sampling cannot be
used for pH analyses.
When specific pollutant parameters are immediately affected by biological, chemical, or physical (e.g., pH
sensitive compounds) interactions, or have short holding times, such as pH, temperature, total phenols,
residual chlorine, soluble sulfide, hexavalent chromium, cyanide, volatile organ ics, and dissolved oxygen,
individual grab samples must be taken. Individual grab samples or composite samples (with proper
compositing procedures) may be taken for oil and grease, and cyanide (as described below). The sampler
must be careful in sampling for oil and grease, since these pollutants tend to adhere to the sample container.
Composite samples are samples collected over a period of time greater than 15 minutes, formed by an
appropriate number of discrete samples which are: I) collected at equal time intervals and combined in
proportion to the wastewater flow, or 2) are equal volumes taken at varying time intervals in proportion to the
wastewater flow, or 3) equal volumes taken at equal time intervals. Composite samples are used to determine
the average pollutant concentration during the compositing period. Various methods for compositing samples
are available. Composite samples may be collected individually at equal time intervals if the flow rate of the
sample stream does not vary more than plus or minus IO percent of the average flow rate, or they may be
collected proportional to the flow rate. The industrial user's permit may specify which composite sample
method to use, either time composites or flow-proportional composites. 'ITie compositing methods, all of
which depend on either continuous or periodic sampling, are described below:
• Time Composite Sampline: Composed of constant volume discrete sample aliquots collected at
constant time intervals. This method provides representative samples when the flow of the sampled
stream is relatively constant (i.e.. when the Row does not vary by more than 10% of the average flow
rate over time).
. Flow-Proportional Sampline: There are two methods used to collect a flow-proportional composite
sample. In the first method, the time between samples is constant, and the volume of each sample is
proportional to the flow at that given moment in time (i.e., the volume of the sample varies over time
as the flow changes). This is the preferred method of sampling when taking a manually composited
sample. This method requires that discrete samples be collected over the operating day and then be
manually composited. It is crucial, when using this method, to have accurate flow data continuously
recorded during the sampling period.
The second flow-proportional sampling method involves collecting a constant sample volume for each
volume of wastestream Row (e.g., 200 ml sample collected for every 5.000 gallons of flow) at time
intervals inversely proportional to the stream flow. This is the preferred method when taking
composite samples using an automatic sampler. This method is based on taking a sample after a set
amount of wastewater has been discharged. This method provides representative samples of all
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wastestreams when the flow is measured accurately. In the other method, the sample is collected by
increasing the volume of each aliquot as the flow increases, while maintaining a constant time interval
between al iquots.
A composite sample should be collected over a workday. If a facility operates and discharges 24 hours
per day, then the composite sample should be taken as a 24-hour composite (either flow proportional or time
composite). If a facility operates 24 hours per day but only discharges wastewater for six hours, a six hour
composite sample should be collected. In general, composite samples should be collected to assess
compliance with Categorical Standards and local limits, as long as the limits are daily, weekly, or monthly
averages, except for those parameters listed above which must be taken by grab sample. If the POTW is
using an automatic sampler with discrete sample containers, the inspector should keep track of any sample
bottles which are empty and seek an explanation from the IU for all empty sample bottles from the composite
sampler.
Appendix V contains the EPA memorandum, "The Use of Grab Samples to Detect Violations of
Pretreatment Standards." This memo explains in greater detail when it is appropriate to use grab samples for
determining the compliance status of industrial users with categorical standards and local limits.
As stated earlier, some pollutant parameters should be collected as grab samples, but may be collected as
composite samples, if specific sampling/preservation techniques for each parameter are followed. Those
parameters which may be a grab or a composite sample are oil and grease, and cyanide. Each of these is
discussed in turn below.
OH and Grease
Method 5520B in Standard Methods for the Examination of Water and Wastewater. 17th edition, is an
approved method of analysis for oil and grease and is listed in 40 CFR 136. Standard Methods states that a
representative sample shall be collected in a wide-mouthed glass jar that has been rinsed with a solvent. It
also proceeds to explain that composite samples should not be taken due to the potential losses of grease on
the sampling equipment. This concept applies only to samples which are collected using automatic samplers.
Oil and grease samples may be composited, if the following steps are taken:
. The compositing vessel is made of glass and has been precleaned and rinsed with the solvent to
remove the detergent film.
• The sampling jar is made of glass and has been precleaned and rinsed with the solvent to remove the
detergent film.
• Collect the sample directly into the sample jar and properly preserve the sample with HCI or HjSO, to
a pH<2. Pour the sample into the compositing vessel. After each additional sample is added to the
collection vessel, the pH should be re-checked and adjusted if necessary. Preserve the sample in the
compositing vessel by cooling to 4°C and holding at a pH<2. When taking the pH, it is recommended
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that the pH paper or probe not be put directly into the sample. To make sure that equal volumes of
each sample are taken, mark the outside of the sampling jar. Repeat this process for the compositing
period.
When the compositing is finished, both the compositing vessel, which has the sample in it, and the
sampling jar must be submitted to the laboratory for analysis. The entire volume in the compositing
vessel must be sent to the laboratory, a smaller sample may not be taken from this vessel. The sample
jar is sent to the laboratory to allow the oil and grease which has adhered to the side of the container
to be extracted and included as part of the sample which is analyzed.
This compositing procedure must be approved by the EPA prior to its use for determining compliance with
oil and grease pretreatment standards, but is available subject to approval by the FPA Regional Office.
Cvanidc (Total)
EPA methods 4500-CN-C, D. or E are approved methods from Standard Methods. I Th edition, which are
listed in 40 CFR 136. Most of the sampling guidance to date has recommended that total cyanide samples be
collected as grab samples (see Grab Sample memo in Appendix V). A manual composite for total cyanide
may be collected if the following steps are followed. (NOTE: 'The first 12 steps must be followed to preserve
a grab sample, even if it is not being composited).
I) Collect a grab sample into either a glass or polyethylene sample bottle.
2) Check for oxidizing agents (e.g., chlorine). If oxidizing agents are not present, then go to step #6.
3) If oxidizing agents are present, add 0.6g of ascorbic acid (see NOTE below).
4) Repeat steps 2 and 3 until no oxidizers are present.
5) Add one additional dose of ascorbic acid.
6) Check the sample for sulfides by placing a drop of the sample on a piece of lead acetate test paper
which has been moistened with acetic acid buffer solution (pH 4). If the lead acetate test paper is
darkened, sulfides are present. If sulfides are not present, go to step I 1.
7) If sulfides are present, add cadmium nitrate powder.
8) Repeat steps 6 and 7 until the moistened lead acetate test paper no longer darkens.
9) Add one additional dose of cadmium nitrate powder.
IO) Filter the sample to remove the sulfides which have precipitated out of the solution. The filtrate
then goes to step 1 1.
11) Preserve with NaOH to a pH>12.
12) Pour the sample into a compositing vessel. After each additional sample has been individually
preserved (steps 1-1 1), add it to the compositing vessel. The pH of the composite should be re-
checked and adjusted as needed. The sample in the compositing vessel must remain preserved at
4°C and at pH>12. When taking the pH, it is recommended that the pH paper or probe not be put
directly into the sample. To ensure that equal volumes of each sample are taken, mark the outside
of the sampling jar. Repeat this process for the compositing period.
(NOTE: 40 CFR 136.3, Table II, footnote 5 explains that if residual chlorine is present, rhe sample must be
treated with 0.6g of ascorbic acid. Footnote 6 to this table also states that if sulfides are present in the
sample, it must be analyzed within 24 hours. It continues to explain that samples can he tested for the
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Chapter 3 - Sampling Industrial Users
presence of sulfides using l*-'ad acetate paper. If sulfides ure present, cadmium nitrate powder should be
added until a negative spot lest is obtained with the lend acetate paper. The sample should then be filtered
and \iiOH he added l<> a />// -12 v u According to 40 CFR 136 3. checking and preserving for sulfides
allows a holding lime oj 14 days rather that 24 hours if sulfides are present and not treated.
40 ( 'f-'K 136 3 Table IB slates thut Standard Methods for the Examination of Water and Wastewater.
l~th edition - methods 4500-C\-C, D, E, and G are approved analytical methods for cyanide analyses. The
preservation techniques for these samples are explained in the analytical methods. When conflicts arise, the
information stated in 40 ( 'f-'R 136.3. TAble II supersedes the preservation technique in the analytical method
.\()TK the preservatives in 40 CFR 136 are not the same as those stated in Standard Methods).
This process of compositing a total cyanide sample is very resource intensive. Therefore, it is not
recommended for routine compliance sampling for cyanide. Table 3-2 lists the advantages and disadvantages
of each compo-.iiinj; sampling method. Either manual or automatic sampling techniques can be used. If a
sample is composite.., manually, sample manipulation should be minimized to reduce the possibility of
contamination. 'I"he inspector must use the sampling method specified in the permit, but if the sampling
method is inadequate, the inspector should pull a sample using the permit method and the method which is
deemed more appropriate
Method
Time Composite
Constant sample
\ olume, constant time
inter\ al bet\v een
samples.
Flow Proportional
Composite
• Constant sample
\ olume. time
interval between
samples proportional
to stream flow
• Constant time
interval between
samples, sample
volume proportional
to total stream flow
at time ot sampling.
Table 3-2
Composite Sampling Methods
Advantages
Minimal instrumentation
and manual effort.
Requires no flow
measurement.
Minimal manual effort.
Minimal
instrumentation.
Disadvantages
May lack
representativeness
especially for highly
variable flows.
Requires accurate flow
measurement reading
equipment.
Samples must be
manually composited.
Discrete samples must
be taken. Chance of
collecting samples
which are too small or
too large for a given
composite volume.
comments
Widely used in both
automatic samplers and
manual handling.
Widely used in
automatic as well as
manual sampling
Used in automatic
samplers and widely
used as manual
method.
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ON-SITE ACTIVITIES
Once the sampling plan has been established and pre-inspection activities have been completed, the focus
of the inspection turns to the on-site activities performed by the inspector. This section outlines the
procedures which POTW inspectors should follow when conducting on-site sampling at their industrial users.
As with inspections, in many cases the first thing the sampler will do is conduct an opening conference with
the IU representatives. Where the POTW has developed a working relationship with the II-' or where there
are suspected violations, the sampler should proceed immediately with sampling and then conduct a closing
conference as necessary.
Sampling Location
The first step in preparing to sample is to verify that the sample location is appropriate. l"he III permit
must specify the sampling location for compliance sampling (40 CFR 403.8(fX2)(iii)). This sampling location
must be representative of the actual discharge from the facility. When conducting a compliance sampling site
visit, the inspector should use the sample location specified in the industrial user's permit. If the sample
location specified in the 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 believes is most representative, samples should he
collected at both sites. The reason for the conflict should be thorough ly documented for later resolution by
the POTW. If necessary, the permit must be amended to reflect the correct sampling location(s).
The Federal Categorical Standards apply at the end-of-process (or at the end of treatment, if treatment
exists), unless the standard specifies a different location to collect the sample (e.g.. in 40 CFR 4.33 Metal
Finishing, the sample location for cyanide is after the cyanide destruct system prior to dilution with other
streams). If process effluent is mixed prior to treatment with unregulated wastestrcams or dilution water or if
local limits apply at a different point, the combined wastestream formula (CWF) or flow weighted average
(FWA) formula must be used (40 CFR 403.6). Samples under this circumstance would be taken after
treatment. If the samples are being taken to determine compliance, all associated flows must be measured
The inspector should always collect samples from a sampling location or locations that reflect the total
regulated effluent flow (i.e., is representative). Convenience and accessibility are important considerations,
but are secondary to the representativeness of the sample. The most representative samples will he drawn
from a wastewater depth where the flow is turbulent and well mixed and the chance of solids settling is
minimal. Depending on the sampling location, ideally, the depth of sample collection should he 411 to 60
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percent of the wastestroam's depth. Stagnant areas must be avoided as well, particularly if the wastewater
contains immiscible liquids or suspended solids. To avoid contamination, the inspector should take care to
collect samples from the center of the flow with the opening of the sampling device or container facing
upstream. Wide channels or paths of flow may require dye testing to determine the most representative
sampling site. If dye testing is inconclusive, multiple samples may need to be collected by cross sectional
sampling.
Sample Collection Techniques
To obtain a representative sample, sampling must be conducted where wastewater is adequately mixed.
Ideally, a sample should be taken in the center of the flow where the 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 should be cautious when collecting samples near a weir because solids tend to collect upstream and
floating oil and grease accumulate downstream.
Samples can be collected either manually (grab or composite) or with automatic samplers. The following
general guidelines apply when taking samples:
• Take samples at the site specified in the industrial user permit (andor at the site selected by the
inspector to yield a representative sample if the inspector concludes that the site specified in the
permit is not appropriate)
• Use the sampling method (grab, or composite) required by the IIJ permit. If the permit sampling
method is inappropriate (e.g.. if it calls for composite sampling for pH), then the inspector should note
this in his her field notebook and take two samples: one using the permit method and one using the
method deemed most appropriate by the inspector. Samples of certain pollutant parameters may not
be taken by automatic samplers, but must be taken by manual grab samples. These parameters
include: dissolved oxygen, residual chlorine. pH, temperature, oil and grease, fecal coliforms,
purgeable organics, and sulfides.
Avoid collecting large nonhomogeneous particles and objects.
• Collect the sample facing upstream to avoid contamination.
Do not rinse the sample container with the effluent when collecting oil and grease and microbiological
samples, but till the container directly to within 2.5 to 5 cm from the top.
Fill the container completely if the sample is to be analyzed for purgeable organics, dissolved oxygen,
ammonia, hydrogen sulfide. free chlorine, pH, hardness, sulfite. ammonium, ferrous iron, acidity, or
alkalinity.
• Collect sufficient sample volume to allow for quality assurance testing. (NOTH: Table 3-4 provides a
guide to numerous sample volume requirements but additional volume may be necessary for QA
testing)
When taking a grab sample, the entire mouth of the container should be submerged below the surface of
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the wastestream. 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.
Sample Volume
The volume of samples collected depends on the type and number of analyses needed. This will be
determined by the parameters to be measured and the requirements of the analytical laboratory being used.
Sample volume must be sufficient for all analyses, including QA/QC and any repeat analyses used for
verification. Laboratory personnel should be contacted for the sample volume required to complete all
analyses, since the lab is in the best position to estimate the necessary volume of sample. Individual,
minimum composite portions should be 100 mis. 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 40 ml for pH and volatile organic
determinations to 1,000 ml or more for BOD, oil and grease, and settleable solids. The inspector should
always collect more than the minimum sample volume to allow for spillage and laboratory reruns. Table 3-3
lists minimum volume requirements for various parameters.
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 requires that the sample be analyzed immediately or that it be preserved or fixed to minimize
changes in the pollutant concentration or characteristics between the time of collection and analysis. Because
immediate analysis is not usually possible, most samples are preserved regardless of the time of analysis.
This preservation mast take place as soon as possible after collecting the sample. This means thar
preservation must take place in the field (see 40 CFR 136.3). The most common procedures used for
preserving samples include icing, refrigeration, pH adjustment, and chemical fixation. When chemical
fixation is used, the chemical preservative must be added before the samples are transferred to the laboratory.
Likewise, refrigeration should be supplied immediately upon taking the sample. For many samples, if
preservatives are not appropriately used, bacteria can quickly degrade certain pollutant constituents (e.g.,
phenols and phosphorous). Other constituents may volatilize (e.g.. cyanide and sulfides) or may react to form
different chemical species (e.g., hexavalent chromium). Proper preservation and holding time for each
parameter is essential for the integrity of the monitoring program. (See Table 3-4 and refer to 40 CFR Part
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136).
Problems may be encountered, however, when N-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 the compositing in addition to preserving the aggregate sample before shipment to the laboratory.
Preservation techniques vary depending on the pollutant parameter that is to be measured; therefore, the
inspector must be familiar with the 40 CFR Part 136 preservation techniques to ensure proper sample
handling and shipment. It is important to verify that the preservation techniques for one parameter do not
affect the analytical results of another parameter in the same sample. If there is this possibility, then two
discrete samples should be collected and preserved independently. Sample preservation should be provided
during compositing, generally by refrigeration to 4°C (or icing) [><)IK: See 40 CTR 136.3 Table II.
Footnote 2.]
Refrigeration is the most widely used preservation technique because it has no detrimental effect on the
sample composition and does not interfere with any analytical methods. Refrigeration requires that the
sample be quickly chilled to a temperature of 4°C, which suppresses biological activity and volatilization of
dissolving gases and organic substances. This technique is used at the start of sample collection in the field
and during sample shipment, and continued until the sample is analysed by the laboratory Sample
temperature should be verified and recorded by the inspector. This is particularly important if the analytical
results are to be used in an enforcement action.
In addition to presenation 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. (NOIK: Some parameters have separate holding times from the time of sample collection to
extraction preparation and from extractionpreparation to analysis). A wastewater sample becomes a sample
when the first aliquot is collected. At that point, holding time limitations begin A detailed list of
presenation methods and holding times appears in Table 3-4 at the end of this chapter. These sample
preservation procedures and holding times were selected by the E-PA because they, retard sample degradation
and minimize monitoring costs by extending holding times as long as possible.
Sample Documentation
Since many 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, including all chain-of-custody forms. If required, the following
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information should also be documented in the field record:
• Unique Sample or Lon 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 their field
records.
• Date and Time of Sample Collection: The date and time 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 (Facility Name and Address): The name and address of the facility being
sampled should be recorded as well as 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 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 Method: Any preservatives (including the amount) added to the sample should be
recorded. The method of preservation (e.g.. refrigeration) should be indicated.
• Analysis Required: All parameters for which the sample must be analyzed should be specified.
• Field Analysis: Field measurements must be recorded at the time that the analysis is completed
Examples of analyses which must be conducted and recorded in the field include: pH, temperature.
dissolved oxygen, residual chlorine, and sulfites. Field analyses should be treated the same as any
other sample, i.e.. the sampler must record the date of the sample, type of sample, name of the
sampler, chain of custody, etc.
. Flow: If flow is measured at the time of the sampling, the flow measurement must be recorded. If
the sample is to be used to determine compliance, flow must be measured.
• Production Rates: Information on products manufactured and production rates should be included
since many effluent limitations are based on production rates.
• Date, Time and Documentation of Sample Shipment: The shipment method (e.g.. air, rail, etc.) as
well as the shipping papers or manifest number should be recorded.
• Comments: This refers 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.
Each of these items must be recorded by the POTW inspector when conducting site sampling, but this
information should also be kept by the industrial user when it conducts its required self-monitoring. This
information should be available for review by the POTW when conducting an on-site inspection or sampling
visit.
Sample Identification and Labeling
Fiach sample must be accurately and completely identified. At the time a sample is collected, a
waterproof, gummed label and a waterproof tag which is able to withstand field conditions should be attached
to the sample container. This label and tag are necessary to prevent any misidentification of samples, since it
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provides the laboratory with relevant information for analysis, such as: the name of the sample collector, the
sample identification number, the date and time of sample collection, the location of the sample collection, the
preservatives used, the type of sample (grab or composite) and the identification of the parameters to be
analyzed. Sample identification, therefore, is a crucial part of chain-of-custody. Sample tags should be used
as part of the chain-of-custody process because they can be removed after the sample has been transported to
the lab and placed in the evidence file for that sample while labels are usually discarded with the sample.
The tags can then be used as evidence in an enforcement proceeding The sample identification procedures
should be incorporated into the POTW's Quality Assurance and Sampling Plan (see p 56 for a further
discussion of the plan).
Sample seals or cooler seals (i.e., seals placed around a cooler with similar samples inside) 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 contain the collector's name, the date and time of sample collection and the sample
identification number. Information on the seal must be identical to the information on the label and tag. In
addition, the seal must be attached so it must be broken to open the sample container or gain access to the
sample container in the case of a cooler seal. Caution should be observed to assure that glue on the sample
seals and tag wires does not contaminate samples, particularly those containing volatile organics and metals.
Chaln-of-Custody Procedures
Once an appropriate sample has been obtained and the sample collection methods 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
(see Definition section for a definition of "custody"). Chain-of-custody procedures are a critical aspect in
monitoring industrial users, and these procedures should be incorporated into the POTW's Quality Assurance
and Sampling Plan (see p. 56 for a further discussion of the plan). The chain-of-custody record allows an
accurate step-by-step recreation of the sample path, from its origin through its final analysis in the laboratory.
Every sample needs to he accompanied by a chain-of-custody tag which is properly signed and transferred to
each person in the chain, from the original sampler to the final person involved in analyzing the sample.
Some of the information that needs to be addressed in chain-of-custody are:
. Name of the person collecting the sample;
. Sample identification number(s);
. Date and time of sample collection;
. Parameters to be analyzed;
. Location of sample collection; and
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. ,.»».,. and signature(s) of all persons handling the samples in the field and in the laboratories.
To ensure that all necessary information is documented, a chain-of-custody form should be developed by
the POTW. An example of such a form used by the EPA is found in Appendix X. Chain-of-custody forms
should be preprinted on carbonless, multipart paper so that 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 wilt 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 till in the appropriate section of the
chain-of-custody record. Finally, the person or group at the POTW responsible for permitting and/or
compliance and enforcement should receive a copy of the completed chain-of-custody from, particularly if the
sample results are to be used for enforcement purposes.
Chain-of-custody records are crucial if the 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 during shipment. 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.
Therefore, all compliance samples taken at an industrial user should follow chain-of-custody procedures.
Sample Packaztne and Shipping
After the samples are properly labelled, they should be placed in a transportation case along with the
chain-of-custody form, pertinent field records, and analysis request forms. 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 should be placed in a waterproof bag, envelope or airtight sample
bottle and taped to the inside lid or other appropriate place inside the transported container to prevent
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tampering or breach of custody. Shipping containers should also be sealed to prevent tampering. Sample
Packaging and Shipping considerations should be included in the POTWs Quality Assurance and Sampling
Plan (see p. 56 for a further discussion of the plan).
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 Waste Materials Regulations (49 CFR Parts 171 -177). Air shipment of
hazardous waste materials may also be covered by requirements of the International Air Transport Association
(1ATA). Before shipping a sample, the inspector should be aware of. and follow, any special shipping
requirements. Special packaging and shipping rules apply to substances considered hazardous as defined by
1ATA rules. Wastewater samples are not generally considered hazardous materials (see Footnote #3 in Table
3-4).
Oualit\ Control
Control checks should be performed during the actual sample collection to determine the performance of
sample collection techniques. In general, the most common monitoring errors are caused by improper
sampling, improper preservation, inadequate mixing during compositing, and excessive holding time. The
following samples should be used to check the sample collection techniques:
• Duplicate Samples (Field): Duplicate samples are collected from two sets of field equipment installed
at the site, or duplicate grab samples are collected from a single piece of equipment at the site. These
samples provide a precision check on sampling equipment and techniques.
• Equipment Blank: Is an aliquot of analyte-free water which is taken to and opened in the field. The
contents of the blank are poured appropriately over or through the sample collection device, collected
in a sample container, and returned to the laboratory as a sample to be analyzed. Equipment blanks
are a check on the sampling device cleanliness.
Field Blank: Is an aliquot of analyte-free water or solvent brought to the field in sealed containers
and transported back to the laboratory with the sample containers. The purpose of the trip blank is to
check on sample contamination originating from sample transport, shipping and from site conditions.
• Preservation Blanks: Is an aliquot of analyte-free water (usually distilled water) to which a known
quantity of preservative is added. Preservation blanks are analyzed to determine the effectiveness of
the preservative, providing a check on the contamination of the chemical preservatives.
The quality control measures taken by the POTW should be included in the POTWs Quality Assurance and
Sampling Plan (see p. 56 for a further discussion of the plan). Quality control is discussed in greater detail
later in this chapter. This full discussion includes a review of laboratory as well as sampling quality
assurance and quality control techniques.
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SAFETY CONSIDERA TIONS DURING SAMPLING ACTIVITIES
Inspection and sampling activities are often carried out under hazardous situations. In developing the
sampling plan, the inspector should not include sampling locations which pose a threat to health or safety, It
is recommended that sampling and inspection teams include at least two people for safety purposes. Under
known hazardous conditions, a two-person team should be mandatory. The sampling team should use all
required safety equipment and protective clothing. Appendix IV lists specific hazards which are associated
with various industrial facilities. The inspector should use this appendix as a reference when conducting
sampling activities at any of the listed industries.
Continuous education is essential to a successful safety program. The inspector should be familiar with
the 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, training in confined space entry and rescue
procedures should be required. In addition, a permit for confined space entry is now required under OSMA,
and the permit must be obtained prior to field personnel entering a confined space. 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 presence of other gases. 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.
In general, the potential hazards that POTW personnel will encounter while performing inspection or
sampling at industrial users can be divided into two areas: physical hazards and atmospheric hazards. The
ability to recognize these hazards and follow proper procedures will eliminate most accidents.
Physical Hazards
A sampling location can present several potential hazards. Sampling activities are often carried out in
locations that meet the criteria set forth in the definition of confined space. A confined space is defined as a
space having limited means of entry or exit which is subject to a deficiency of oxygen, and the accumulation
of toxic or combustible gases. Such locations include manholes, pumping stations, wetwells. storm drains,
and water meter vaults.
Care must be exercised when removing manhole covers and entering manholes or other confined spaces.
Manhole covers should be opened and removed with a properly designed hook. Manhole covers should never
be opened with fingers. An acceptable tool can be made from 3/4 hex or round stock. Two inches of one
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end should be bent at a right angle and the opposite end should be formed into a handle wide enough for
placement of both hands. The two inch hook can be inserted into one of the holes in the cover and lifted by
straightening the legs. Improper lifting of a manhole cover may result in back injury. Caution must be
exercised when lowering and lifting sampling equipment. A sampler is much heavier when it is full and is
sometimes difficult to lift. Tools should be lowered into and lifted out of the manhole in a bucket to prevent
the tools from falling on someone below.
Generally, the top of a manhole is flush with the surrounding surface. Therefore, a person entering the
manhole may not have anything to hold on to for support, ladders and steps leading into manholes and other
types of confined spaces are subject to corrosion and may not be well maintained. These structures should be
examined prior to entry. If there is any doubt regarding the soundness of the manhole steps, a portable ladder
should be used. Other physical hazards in a confined space include the following: excessive depths;
excessive flow; poor visibility; wet'slippery surfaces; harmful animals, insects or organisms (spiders, snakes,
bacteria); protruding or sharp objects; and falling objects. Other physical hazards are listed in Appendix IV.
Atmospheric Hazards
Atmospheric hazards are comprised of three primary types: oxygen deficient atmospheres;
explosive, flammable atmospheres; and toxic atmospheres. These types of hazards require air monitoring and
ventilation before entering a manhole or other confined space. Air monitoring equipment is discussed later in
this chapter.
Oxygen Deficient Atmosphere:
The minimum OSHA requirement for oxygen concentration in the atmosphere is 19.5%. A Self-
Contained Breathing Apparatus is necessary to enter an atmosphere with less than 19.5% oxygen. The
oxygen enriched atmosphere, which exists when the oxygen concentration is greater than 25%. is also
considered hazardous because of its ability to support combustion.
Normal air consists of the gases listed in Figure 3-2. Other gases,
Q Volume suc^ as nitr°gen and carbon dioxide, which are harmless under
normal conditions, may build up in confined spaces in quantities
Nitrogen 78.09% ,.,-,,
~ 20 0507 large enough to displace the oxygen necessary to support life.
Argon 0.93% When the concentration of oxygen in the atmosphere falls to 10-
Carbon Dioxide 0.03%
16%. a person will expenence shortness of breath. Loss of
consciousness will occur at a 6-10% oxygen concentration and
Figure 3-2 Atmospheric Constituents
death will occur rapidly when the concentration of oxygen falls
below 6%.
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industrial User Sampling Manual Chapter 3 - Sampling Industrial Users
Explosive Atmosphere:
Gasoline is the most common flammable liquid found in the sewer system. The major source of gasoline
is leaking underground storage tanks and accidental discharge or spills. Gasoline is lighter than water,
enabling it to float on top of the wastestream, and the vapors spread out in the collection system. It takes a
very small amount of gasoline to generate an explosive atmosphere in a confined space.
Methane is the most common flammable gas encountered in the sewer system. Methane gas is the
product of waste decomposition and is the primary component of natural gas. A leak in a natural gas pipe
may result in the gas seeping into the collection system. Methane is lighter than air, which allows it to
collect at the top of a confined space.
Toxic Atmosphere:
There are various guidelines for assessing chemical hazards in the atmosphere. The Threshold Limit
Values (TLVs) are guidelines developed and published by the American Conference of Governmental
Industrial Hygienists (ACGIH) to be used for identifying and controlling potential hazards. One form of the
TLS - the time weighted average (TWA} - refers to the vapor phase concentration a worker may be exposed
to for an eight hour day or 40 hour work week without chronic or acute health effects. TLV-TWA numbers
are sometimes used to calculate IU discharge screening levels for volatile organic compounds. The EPA has
issued a guidance document entitled "Guidance to Protect POTW Workers from Toxic and Reactive Gases
and Vapors," (HPA 812-B-92-001). This document should be used to evaluate the potential for exposure to
toxic atmospheres and necessary steps for avoiding contact with such atmospheres.
Hydrogen sulfide (H2S) is the most common gas found in the collection system. The gas, which is
formed by anaerobic decomposition of organic matter, is heavier than air and tends to collect at the bottom of
an enclosed space. At low concentrations, hydrogen sulfide has an odor of rotten eggs, at higher
concentrations, however, the olfactory system becomes impaired and the gas cannot be detected by smell.
The TLV-TWA for hydrogen sulfide is 100 ppm. At higher concentrations of H2S, damage can occur to the
eyes, nervous system, and respiratory system. A caustic solution (sodium sulfide) is formed when the gas
comes into contact with moist tissue, such as in the eyes and respiratory tract, which causes the irritation and
danger from the chemical. At concentrations of 500-1,000 ppm the respiratory system is paralyzed and death
will occur.
Hydrogen cyanide gas may be generated when cyanide salts react with an acidic wastestream. Cyanide
salts are often found in plating baths and metal finishing facilities. The gas causes death by preventing the
transfer of oxygen within the bloodstream.
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Chlorine (Cl.) gas may be encountered at plating facilities where it is used for cyanide destruction.
Aside from the irritating odor, chlorine gas is corrosive in the presence of moisture. It combines with
moisture in the lungs and the respirator) system to form hydrochloric acid. Pulmonary edema (fluid in the
lung may occur at SO ppm and at 1,000 ppm death occurs rapidly.
Carbon monoxide (CO) is another gas that is generated in a collection system from anaerobic
decomposition of organic materials. Asphyxiation occurs from exposure to this gas because the hemoglobin
of the blood has 300 times more affinity for carbon monoxide than for oxygen. Carbon monoxide combines
with hemoglobin to form carboxy hemoglobin. As a result, blood cells with CO cannot transport ox\gen to
body tissues, and death occurs.
Toxic vapors also present a hazard to inspectors and sampling personnel. Vapors are the volatile form of
substances that are normally in a solid or liquid state. Chlorinated solvents used in degreasing or photoresist
developing operations generate vapors that may accumulate in the collection system. Some of the vapors
have an anaesthetic effect when inhaled. In addition, the vapors are generally heavier than air causing oxygen
in a confined space to be displaced which may create an oxygen deficiency in that space.
Safety Equipment
Recognizing the physical and atmospheric hazards associated with sampling and inspections is important.
Simply acknowledging the hazards, however, does not guarantee safe working conditions. An employer is
obligated to provide safely equipment and to establish a training program for employees. 'The important thing
to remember is that the responsibility for using the equipment and following safety procedures rests with the
individual inspector. The following discussion will acquaint the inspector with proper safety techniques,
Protective Clothing:
Protective clothing is an important aspect of safety, and the guidelines presented below should be
followed when conducting inspections and sampling at industrial users.
• Hard Hat - All persons entering a confined space are required to wear a hard hat. A full strength hard
hat with a brim and chin strap provides protection from head injuries.
• Coveralls - A person's skin should be covered as much as possible to prevent scrapes and cuts and to
avoid skin contact with hazardous substances.
. Gloves - Hand protection is necessary when collecting and/or handling wastewater samples. In
addition to preventing absorption of hazardous chemicals through the skin, gloves will protect the
hands from cuts and scratches.
• Shoes - Rubber-soled, non-skid, steel-toed shoes and boots must always be worn in or around a
confined space. Safety shoes are designed to protect against impact and/or hazardous chemicals.
. Ear Plugs - Ear plugs should be worn when working in areas with high noise levels (e.g.. general
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manufacturing areas). This equipment will protect the inspector from the cumulative effects of loud
noises in the work place.
• Safety Goggles - Safety goggles are necessary during inspections and sampling to prevent eye contact
with hazardous substances. Contact lenses are often prohibited around some industrial processes such
as plating operations, if a hazardous substance comes into contact with a person's eye through
splashing or exposure to mists or vapors, that substance may become trapped behind the lens where it
would be difficult to flush out and could cause severe eye damage.
. Safety Vests - Safety vests are necessary warning devices in areas with vehicle traffic.
Traffic Control:
Traffic diversions are necessary when inspecting and/or sampling in areas subject to vehicle traffic. For
protection of Ihe public as well as employees, Ihe devices musl be installed immediately upon arrival al Ihe
site and musl nol be removed until Ihe work is completed. The following devices may be used to route
Traffic away from an open manhole.
. Warning Devices - Relating/flashing lighls and arrow boards should be placed belween Ihe work area
and oncoming traffic to alert drivers and pedestrians.
. Barricades - A vehicle or heavy piece of equipmenl should be placed belween Irafflc and Ihe working
area. II should nol, however, interfere wilh Irafflc.
. High-Levcl Warning Flag/Cones - Should be used to route Iraffic through a job-site. Flagmen should
be used whenever possible and musl wear reflective doming, such as safely vesls, hard hals, and
safely shoes.
Radio:
A Iwo-way radio is Ihe mosl effective way to maintain conlacl wilh a main office. A sampling learn
should make radio conlacl upon arrival and departure from each sampling location. Sampling sites are often
located in unpopulated areas; Iherefore, il is importanl lhal Ihe radio be kepi in working order in Ihe evenl il
is necessary to call for help. If an accidenl should occur, Ihe rescuer musl call for help before any assistance
is given to Ihe victim
Air Monitorine Devices:
Before sampling in a confined space, tests should be done for: (I) explosive gases; (2) the presence of
toxic gases; and (3) oxygen deficiency. The mosl effective melhod for delecting Ihese conditions is wilh an
almospheric monitor. The gas detectors discussed below are Ihe mosl commonly used for almospheric
monitoring
. Single Purpose Detector - Designed to delecl specific gases, such as carbon monoxide, melhane, or
hydrogen sulfide. These gases are commonly presenl in collection systems and confined spaces.
Single detection unils or lubes are available for measuring gases lhal are less common.
. Dual Purpose Detector - Capable of delecting lack of oxygen and explosive conditions in an area.
• Combination Detector - Capable of delecting a lack of oxygen, explosiviry and Ihe presence of toxic
gases. 'I"his type of meter provides maximum protection by delecting Ihe presence of all Ihree hazards.
Hydrogen sulfide and carbon monoxide are Ihe gases usually measured because Ihey occur mosl
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frequently in a collection system
The atmosphere in a confined space can change suddenly; therefore, a detector that continuously
monitors the atmosphere is recommended. In addition, detectors should be equipped with an audible and
visual alarm which is activated in response to specific hazardous conditions or a low batter), thus eliminating
the need for taking the time to read a dial or gauge.
It is important to remember that using an atmospheric tester does not ensure safe conditions. Gas
detectors are only one source of information pertaining to a potentially hazardous situation. Most gas
detectors are designed to test for common gases such as hydrogen sulfide, and are not effective for detecting
less common substances such as trichloroethylene vapors. There are test kits available for detecting the less
common gases. The kits consist of a bellows-type pump and glass tubes containing an indicator chemical
which are sealed at the ends until they are used. The indicator chemical in the detector tube is specific to a
particular contaminant or group of gases. A predetermined volume of air is drawn through the tube and the
contaminant reacts with the indicator chemical, producing a color change that can be compared to a color-
calibrated chart to determine an approximate concentration.
When measuring explosivity. gas meters measure the percentage of the Lower-Explosive Limit (LEL) of
a calibration gas. which is usually methane. Gases are combustible throughout a range of air mixtures. The
meters do not differentiate between gases, but only indicate explosivity relative to the calibration gas. The
range begins with the LEL, which is the lowest concentration of a combustible gas or vapor in air that is
necessary to support combustion. The explosive range extends upward to the Upper Explosive Limit (UEL)
which is the maximum concentration that will support combustion. If the concentration of gas is below the
LEL, there is insufficient fuel to support ignition. Alternatively, if the concentration is above the UEL, there
is insufficient oxygen to support combustion. These limitations in the atmospheric monitoring equipment
emphasize the need for constant ventilation and awareness of potential hazards. (NOTE: Combustible gas
meter alarms are usually set a point well below the LEL of the gas or atmosphere being measured)
Ventilation Devices:
Few confined spaces have adequate natural or mechanically induced air movement, and in most spaces, it
is necessar> to remove harmful gases or vapors by ventilation with a blower or fan. The most common
method of ventilation uses a large flexible hose attached at one end to a blower with the other end lowered
into the space. The blower will push fresh air into the space to purge the area of hazardous substances. The
blower allows the fresh air to enter the space at the lowest point possible. Because the atmosphere in a
confined space can change quickly, ventilation should be continuous.
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Safety Harness and Retrieval System:
Any entry into a confined space must always be performed by a team consisting of at least two people.
A standby person must be stationed outside of the confined space and must remain in visual and radio contact
with the person inside. All personnel required to enter the confined space must wear a safety harness. A full
body parachute type harness with a lifeline attached at the shoulders is recommended. This type of harness
will keep a body vertical and prevent a limp body from falling out when being pulled out of an area.
The lifeline should be attached to a retrieval system which includes a fall arrest mechanism. This type of
safely system works in a similar manner as an automobile safely belt where a centrifugal locking mechanism
is activated when a fall occurs. If a rescue attempt is necessary, this type of retrieval system eliminates the
need to enter the space. Approximately one half of all fatalities that occur in confined spaces are unplanned
rescue attempts where a worker instinctively rushes into the confined space to assist an injured co-worker.
The retrieval system should be purchased from a reputable manufacturer or authorized distributor as
complete systems, including, repair, and training for proper use. Most components of a retrieval system must
meet certain manufacturer specifications and substitution of these components may result in liability for
personal injury.
Safely equipment must be maintained and inspected on a regular basis. A safety harness and rescue rope
should be examined for the following: frayed strands of fibers, cuts or tears, chemical damage, decay, and
kinks or extreme stiffness. Visual inspection of this equipment should be made prior to each use, and formal
procedures should be implemented for periodic inspection and maintenance.
Respirators:
The primary function of a respirator is to prevent exposure to hazardous atmospheres. It is important to
choose a respirator based on the job to be performed and the potential hazards to which an employee may be
exposed. The basic types of respirators are:
. Air Purifying - Masks which filter dangerous substances from the air; and
. Air Supplying - Devices which provide a supply of safe breathing air from a tank.
An air-purifying respirator will remove particles of dust and light concentrations of gas or vapors, but it will
not protect against heavy gas concentrations. In addition, this type of respirator provides no oxygen other
than what is filtered through the mask. Air-purifying respirators include the following types:
. Gas and Vapor Respirators - Contaminated air is passed through charcoal which traps gases and
vapors.
• Paniculate Respirator - Contaminated air is passed through a filter for removal of particles.
. Powered Air-Purifying Respirator - A blower passes contaminated air through a device which removes
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Industrial User Samp line Manual Chapter 3 - Sampling industrial Users
. Testing. All confined spaces must be tested prior to entry.
. Evaluation. Tests must be evaluated for oxygen level, explosivity, and potentially toxic substances.
Sampling personnel should also consider necessary safety equipment.
• Monitoring. The atmosphere in a confined space is subject to change. Therefore, the area should be
continuously monitored during the sampling activities.
Rescue procedures must be developed for each type of confined space that may be encountered by the
sampling personnel. A written record of training and safety drills should be kept. Rescue procedures should
be practiced frequently enough to ensure proficiency in any necessary rescue situations. In developing a
successful training program, the POTW is encouraged to call on other agencies (e.g., local fire and rescue
department) with expertise in any of the areas described above.
FLOW MEASUREMENT
Pollutant limits in the industrial user's permit are often expressed in terms of mass loadings to the POTW
(e.g.. OCPSF categorical standards). To determine a mass loading and thereby evaluate compliance with the
permit limits, it is necessary for the inspector to obtain accurate flow data. "Flow measurement" is the
commonly used term for this process, and this section briefly describes the types of devices and procedures
used to measure flow. For further information, the inspector should consult two other EPA guidance manuals,
the 1988 NPDES Compliance Inspection Manual and the 1981 NPDES Compliance Flow Measurement
Manual. In situations where flow measuring devices such as those described in the following sections are not
available, the POTW may need to rely on the use of water consumption records at the facility. However,
when a mass loading needs to be determined for assessing compliance, the POTW should have the ability to
assess directly the flow at the facility during the sampling event, Relying on water consumption records
when determining compliance with mass-based limits is not an acceptable practice and should nor be used by
the POTW.
Open Channel Flow
Open channel flow, where the flow occurs in conduits that are not full of liquid, is the most prevalent
type of flow at industrial user discharge points regulated by the pretreatment program. Partially full pipes that
are not under pressure are classified as open channels as well. Open channel flow is measured using both
primary and secondary devices (as described below).
Primary Devices:
Primary devices are calibrated, hydraulic structures installed in the channel so flow measurements can be
obtained by measuring the depth of liquid at a specific point in relationship to the primary device. Weirs and
flumes are examples of primary devices.
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Industrial User Sampling Manual Chapter 3 - Sampling Industrial Users
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 3-4 shows a profile of a sharp-crested weir and indicates the
appropriate nomenclature. Four common types of sharp-crested weirs are shown in Figure 3-5. 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 the
Palmer-Bowlus Flume.
Figure 3-6 presents a sketch of the Parshall Flume, identifying its different parts. In the Parshall Flume,
the floor level of the converging section is higher than the floor of the throat and diverging section. The
Flume operates on the principle that when water flows through a constriction in the channel, a hydraulic head
is produced that is proportional to the flow. Flumes are good for measuring open channel waste flow because
they are self-cleaning. Sand and suspended solids are unlikely to affect the device's operation.
A Palmer-Bowlus 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 at 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 the manufacturer's data a»'e consulted, and it is difficult to measure manually the height of water above
the step at an upstream point. The dimensions of each Palmer-Bowlus Flume are different. Therefore, the
manufacturer's data must be consulted to establish a relationship between the head and the discharge rate.
Figure 3-7 contains a sketch of a free-flowing Palmer-Bowlus Flume.
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
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POTW Inspection Manual
Chapter 3 - Sampling Industrial Users
K = AfPROX. 0.1"
K
•- m
POINT TO
awr«
i
or
45"
V
STRAIOMT I
INLET RUN | I
SHARP - CHESTED WEIR
HEIR CREST
MINIMUM
DI SCHARGE LEVEL
FOR FREE FALL
FREE FALL
cww&WKsr
WEIR
Figure 3-4
Profile and Nomenclature of Sharp-Crested Weirs
(Taken from NPDES Compliance Inspection Manual, EPA, May 1988)
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Crest Length
1
L
Hmax
2Hmax
Minimum
Suppressed (Without End Contractions)
Rectangular Weir
2Hmax L
Minimum Crest Length
.• .v:: < :: i •. •
Hmax
2Hm«x
•Minimum • .• • •: • •.
• .• - ~ .- .**.-.*..-...*'
Trapezoidal (Cipolletti) Sharp-Crested Ueir
2Hma»
Minimum
1 .
L
Crest Length
-Hmax
2Hm«x
Minimum
led (With tnd Cuntr^clions)
live t^ntjuUr Wi-ir
2Hmax
Minimum
2Hmax
Hmax
•
V-Notch (Triangular) Sharp-Crested Ueir
Four Common Types of Sharp-Crested Weirs
(Taken from NPDKS Compliance Inspection Manual, KI*A, May 1988) 91
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POTW Inspection Manual
Chapter 3 - Sampling Industrial Users
Section
M
Water
Surface
B
ty
I
r
Dt»*ril«t
L
0 Level Floor |
Subm«ro«d Flow
Free Flow
g o t & -
4 Zero Reference
- Level for
and
Figure 3-6
Plan View and Cross Section of a Parshall Flume
(Taken from NPDES Compliance Inspection Manual, EPA, May, 1988)
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POTW Inspection Manual
Chapter 3 • Sampling industrial Users
Flow
Water Surface
Three:
Upstream
Depth
Small Jump
Should Occur
In This Region
. Downstream
Depth
••••>:•:••••••:•:• •••>"•:
Preferred Head
Measuring Point
D = Conduit Diameter
Figure 3-7
Free-Flowing Palraer-Bowlus Flume
(Taken from NPDES Compliance Inspection Manual, EPA, May 1988)
THROAT
INLET SECTION SCCT10
PlU DIA
H16N
MfSSUt
TA?
OUTLCT UCTfO*
LOW fRCSSUHC TAP
TMOAT OIA.
Configuration and Nomenclature of a Venturi Meter
(Taken from NPDES Compli»«c» Inspection Manual, EPA, May 1988)
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Industrial User Sampling Manual Chapter 3 - Sampling Industrial Users
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 categories:
• A non-recording type with direct readout (e.g., a staff gauge) or indirect readout from fixed points
(e.g., a chain, wire weight, or float); or
• A recording type with either digital or graphic recorders (e.g.. float in well, float in flow, bubbler,
electrical, or acoustic).
Closed Channel Flow
Closed channel flow is normally encountered between treatment units in a wastewater treatment plant and
after lift stations, where liquids an&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 3-8. 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.
Hlectromagnetic flow meter operation is based on the fact that the voltage induced by a conductor
moving at right angles through a magnetic field will be proportional to the velocity of that conductor as it
moves through the field. In the case of the electromagnetic flow meter, the conductor is the stream of water
to be measured, and the magnetic field is produced by a set of electromagnetic coils. A typical
electromagnetic flow meter is shown in Figure 3-9.
QUALITY ASSURANCE/QUALITY CONTROL (QA/QC) PROCEDURES
Quality Assurance and Quality Control are tools which are necessary to maintain a specified level of
quality in the measurement, documentation, and interpretation of sampling data. To produce evidence which
is admissible in an enforcement action, QA and QC procedures are necessary both in the field (during
sampling) and in the laboratory. The QA/QC procedures used in the field are separate from those used in the
laboratory, but both are crucial for obtaining reliable data. Both laboratory and field QA/QC are discussed in
this section. QA'QC procedures are used to obtain data that are both precise (degree of closeness between
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POTW Inspection Manual
Chapter .? - Sampling Industrial Users
INSULATING
LINER
ELECTRODE
ASSEMBLY
MAGNET COILS
STEEL METER
BODV
POTTING COMPOUND
Figure 3-9
Electromagnetic Flow Meter
(Taken from NPDES Compliance Inspection Manual, EPA, May 1988)
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Industrial User Sampling Manual Chapter 3 - Sampling Industrial Users
two or more samples) and accurate (degree of closeness between the results obtained from the sample analysis
and the true value that should have been obtained). By following QA/QC procedures, the POTW's
confidence in the validity of the reported analytical data is increased.
All data generated or used by the POTW must be of known, defensible, and verifiable quality. This
includes data which are generated through self-monitoring at the industrial facility. Therefore, the ID should
also have QA QC procedures in place to ensure the adequacy of the data submitted as part of its periodic
compliance report (son : All inspections, and the data obtained as a result of the inspection, have the
potential to be used in an enforcement proceeding and should be treated as potential evidence to be admitted
in court).
QA is the program functions specified to assure the quality of measurement data while QC is the process
of carrying out those procedures stated in the QA program The QA program should be general while QC
activities are specific. Also, the specific QC procedures used to assure data of good quality should be
specified in the Quality Assurance and Sampling Plan developed for individual sampling events (e.g., the use
of duplicate samples in the field). A QA program has two primary functions. First, it is designed to monitor
and evaluate continuously the reliability (i.e., accuracy and precision) of the analytical results reported by
each industrial user. 'This is how the quality of the data received from the IU is judged for acceptability.
Second, QA should control the quality of the data to meet the program requirements. A QC program is
designed to ensure the routine application of procedures necessary for the measurement process to meet
prescribed standards of performance (e.g., through instrument calibration and analysis of reference unknowns).
A program describing the schedule for calibration is QA, while the actual calibration procedures are QC.
QA/QC functions fit into two categories, field procedures and laboratory procedures. Each of these items
is discussed in greater detail in the subsections which follow.
Oualitv Assurance Procedures for Sampling
A QA program for sampling equipment and for field measurement procedures (for such parameters as
temperature. DO, pH, and conductivity) is necessary to ensure data of the highest quality. The inspector
should recognize the importance of implementing quality assurance in sample collection to minimize such
common errors as improper sampling methodology, poor sample preservation, and lack of adequate mixing
during compositing and testing. Again, each of these activities should be a part of the POTWs SOP. so that
all POTW sampling personnel are familiar with the proper sampling procedures. Quality assurance checks
will help the inspector determine when sample collection techniques are inadequate for the intended use of the
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data. A field quality assurance program should contain the following elements:
• The required analytical methodology for each regulated pollutant; special sample handling procedures;
and the precision, accuracy, and detection limits of all required analytical methods.
• The basis for selecting the analytical and sampling method. For example, each analytical method
should consist of approved procedures. Where the method does not exist, the QA plan should state
how the new method will be documented, justified, and approved for use.
• The number of analyses for QC (e.g., the percentage of spikes, blanks, or duplicates), expressed as a
percentage of the overall analyses, (e.g., one duplicate sample per IO samples) to assess data validity.
Generally, the QA program should approximate IS percent of the overall program, with 10 percent
and 5 percent assigned to laboratory QC and field QC respectively. The QA plan should include
shifting these allocations or decreasing these allocations depending on the degree of confidence
established for collected data.
• Procedures to calibrate and maintain field instruments and automatic samplers.
. A performance evaluation system which allows sampling personnel to cover the following areas:
Qualifications of personnel for a particular sampling situation;
Determining the best representative sampling site;
Sampling techniques, including the location of sampling points within the wastestream, the choice
of grab or composite samples, the type of automatic sampler, special handling procedures, sample
preservation procedures, and sample identification.
Flow measurement, where applicable.
Completeness of data, data records, processing, and reporting.
Calibration and maintenance of field instruments and equipment.
- Use of QC samples, such as field duplicates, or splits to assess the validity of the data.
Training of all personnel involved in any function affecting data quality.
By following these QA procedures, the inspector can ensure the proper quality data from the industrial user.
Quality Control Procedures for Sampling
Sampling QC begins with calibration and preventative maintenance procedures for sampling equipment.
The inspector should prepare a calibration plan and documentation record for all field sampling and analysis
equipment. A complete document record should be kept in a QC logbook, including equipment
specifications, calibration date, and calibration expiration data, and maintenance due date. All of these
activities should be reflected in the POTW's Standard Operating Procedures (see the beginning of the chapter
for a discussion of SOPs). The sampler should keep in mind that field analytical equipment should be
recalibrated in the field prior to taking the sample. In addition to calibration procedures, the person
conducting field sampling should complete the various types of QC samples outlined on page 77.
Personnel conducting sampling should be well-trained in the use, cleaning, calibration, and maintenance
of all instruments or samplers used. Automatic sampler tygon tubing, bottles, and the sampler itself should be
cleaned prior to each sampling event. Automatic samplers should be calibrated for sample quantity, line
purge, and the timing factor, if applicable. This calibration can and should be checked in the field to verify
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draw. 'I~he manufacturer's directions should be reviewed and followed for cleaning and calibrating all
equipment.
Laboratory Quality Assurance/Quality Control
Laboratory QA/QC procedures ensure high-quality analyses through instrument calibration and the
processing of control samples. The precision of laboratory findings refers to the reproducibility of results. In
a laboratory QC program, a sample is analyzed independently (more than once) using the same methods and
set of conditions. Precision is estimated by comparing the measurements. Accuracy refers to the degree of
difference between observed values and known or actual values. The accuracy of a method ma> be
determined by analyses of samples to which known amounts of a reference standard have been added,
Four specific laboratory QA procedures can be used to determine the confidence in the validity of the
reported analytical data, duplicates, blanks, splits, and spiked samples. Each of these are described below:
• Duplicate Samples (Laboratory): Laboratory duplicate samples are samples which are received b>
the laboratory and divided (by the laboratory) into two or more portions. Each portion is separate!)
and identical!) prepared and analyzed. Duplicate samples check for precision. These samples provide
a check on sampling equipment and sampling techniques.
• Method Blanks: Method blanks are samples of analyte-free water that are prepared in the laboratory
and analyzed by the analytical method used for field samples. The results from the analyses are used
to check on the cleanliness of reagents, instruments, and the laboratory environment.
• Split Samples (Field): Field splits are collected and divided in the field into the necessary number of
portions (e.g.. 2, 3, etc) for analysis. Equally representative samples must be collected in this process.
and then the samples are usually sent to different analytical laboratories. Field splits allow the
comparison of analytical techniques and procedures from separate laboratories. Sampling personnel
should exercise caution when splitting samples to avoid producing large differences in TSS. All
widely divergent results should be investigated and the cause identified. NOTE: Oil and grease
samples cannot be split due to the nature of the pollutant.
• Laboratory Spiked Samples: These samples provide a proficiency check for the accuracy of
analytical procedures. A known amount of a particular constituent is added to separate aliquots of the
sample or to distilled/deionized water at a concentration where the accuracy of the test method is
satisfactory. The amount added should be coordinated with the laboratory.
Laboratory QA/QC procedures can be quite complex. Often, the analytical procedures specify QA/QC
requirements for calibration, interference checks (for ICP analyses), control samples, spiking (including the
method of standard additions), blank contaminant level, and instrument tuning. Accuracy is normalls
determined through the analysis of blanks, standards, blank spikes, laboratory control samples, and spiked
samples. Precision is determined through the comparison of duplicate results or duplicate spiked results for
organic analysis. For more information on laboratory QA/QC, the POTW should contact their Regional
Quality Assurance Management Staff or Quality Assurance Manager.
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industrial User Sampling Manual Chapter 3 - Sampling Industrial Users
The methods used by in-house or contract laboratories to analyze industrial user samples must be
methods which are EPA approved under 40 CFR 136 and thus are acceptable to a court of law as the most
reliable and accurate methods of analyzing water and wastewater. Although some field test kits are useful as
indicators of current conditions (and, thus, may be used for process control considerations), they are not
appropriate for sampling that is conducted to verify or determine compliance. If non-EPA approved methods
are used for analysis, it is likely that the data will be considered inadmissible as evidence. When choosing a
contract lab. POTWs should obtain and review a copy of the lab's QA/QC plan.
Compliance Issues Related to Sampling and Analysis
The compliance monitoring program of the POTW (i.e., the process of receiving 1U self-monitoring
reports, and conducting inspections and sampling at regulated industrial users) is a crucial aspect of the local
pretreatment program. The compliance monitoring program forms the basis of the information the POTW
must use to enforce the federal and local requirements established as part of the POTW's approved
pretreatment program. The purpose of this manual has been to ensure the ability of the POTW to use the
information gained in compliance monitoring (e.g., through proper chain-of-custody, sample QA/QC, and
legal entry procedures). We now turn to certain specific issues of how the POTW should use this information
to determine the compliance status of its industrial users after it has been appropriately gathered. For
example, we have already discussed certain laboratory QA/QC measures. These measures are necessary to
ensure the validity and reproducibility of the sample. One of these measures is the use of duplicate samples,
but how should the POTW determine compliance from these samples if their results are different (e.g., one
shows compliance and the other shows noncompliance)? This issue and others like it are addressed in this
section of the manual. The POTW should follow the procedures and information outlined in this section
when establishing the compliance status of their IDs.
The Use of Duplicate Samples to Evaluate Compliance
In the previous section, the use of duplicate samples (both field and laboratory) was discussed as a means
of determining if the sample collection and laboratory analyses are adequately precise for compliance
determination. In most cases, if proper QA/QC procedures are followed, the analyses from the duplicates
should be very close together. This indicates that the sample collection technique is sufficiently precise and
that the lab has a high degree of precision in its analysis of samples. If the duplicate sample results are very
close to one another (i.e., within the QC range established by the laboratory) but one is above the limit and
the other is below the limit, the POTW should average these results together to determine the compliance
status of the II,'. Remember, this can only be done if the sample results are within the QC range of the
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Industrial User Sampling Manual Chapter 3 - Sampling Industrial Users
laboratory
In other cases, the analytical results from the duplicate samples, even though pulled from the same
sample (or a simultaneous second sample), may yield significantly different analytical results. If this happens,
the POTW needs to make a judgment as to whether the sample can be used for determining the compliance
status of the IU (e.g.. for determining SNC). If duplicate samples produce significantly different analytical
results, the POTW should follow the procedures outlined below:
Investigate the Analytic Methodology. The POTW should review the procedures used by the
laboratory personnel when analyzing the sample to ensure that all steps were followed properly. The
POTW should also evaluate the nature of the samples themselves and whether the samples may be
responsible fur contributing to any analytical discrepancies (e.g., duplicate samples of very high
concentration, i.e.. requiring significant dilutions, may produce high relative percent differences which
may be due to sampling techniques in the field, sampling of the aliquot in the laboratory, dilution
technique, or a combination of these factors). POTWs must be aware of this situation when
evaluating whether any duplicate sample results may be used for determining compliance.
• Check the Analytic Time Sequence. Very often the sample analysis for duplicate samples is done
sequentially. This is especially true when the sample analysis requires the use of GC/MS equipment.
In these situations, it is possible to have the sample analyses far apart in time. If this happens, the
sample holding time may be exceeded. If this happens, the sample which was analyzed after the
holding time is not valid, and a new sample must be taken. Even if the sample holding time has not
been exceeded, it is possible that two analyses from the same sample will produce different results if
they are far enough apart in time. Therefore, make sure that all duplicate samples are analyzed as
close together as possible to ensure sample integrity through the entire analytic process. If the sample
has not exceeded its allotted holding time, the POTW can re-analyze two new samples from the
original sample collection vessel to obtain valid duplicate results.
. Check the Laboratory Equipment. The POTW should make sure that all glassware is properly washed
and rinsed to make sure that it is clean and free of contaminants. Dirty glassware can cause
interference with the sample analysis. In addition, make sure that all lab equipment is properly
calibrated, operzted and maintained. This should ensure consistent sample results.
• Review the Sampling Methodology. It is possible that a duplicate sample, if taken as two discrete
samples, will have very different characteristics. For example, when taking a duplicate sample for oil
and grease, it is usualK necessary to take two discrete samples because it is not possible to split an oil
and grease sample. When the two samples are taken, the sampler may not take each sample in exactly
the same way (e.g.. one sample may skim the top of the wastestream and the other may be taken from
the bottom of the wastestream). This can produce two radically different samples, even though they
were taken at the same time from the same place. If duplicate samples are taken from the same
sample collection vessel, make sure that the sample is well mixed and homogeneous so that each
sample is as close as possible to each other.
. Check the Laboratory QA/QC. xhe laboratory and sampling QA/QC procedures should be reviewed
when duplicate samples produce different analytical results. The lab should check to see if blank and
spike sample analyses give appropriate results. If the blanks and/or spikes do not produce expected
values, it is highly likely that there is a problem with the analytical procedures. If the blanks and
spikes indicate analytic problems, it may be necessary to discard the sample and disregard the results
when determining the compliance status of the industrial user.
If the source of the discrepancy is identified, the POTW should run another analysis from the same
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Industrial User Sampling Manual Chapter 3 - Sampling industrial Users
sample batch (this is one good reason to take an adequate sample amount when in the field) making sure to
avoid the mistakes on the original duplicate sample.
The POTW also has the option of sending the sample in question to an independent laboratory. This
"referee" laboratory can serve to give impartial analysis of the sample so that the sample results can be used
to evaluate compliance. If the POTW chooses this option it should keep in mind that while the "referee?
laboratory will give independent results, it will not necessarily give the "right" result. The POTW should
evaluate the referee lab in terms of the equivalency of its analytical procedures, QA/QC etc., in relation to 40
CFR 136 as well as equivalency to the POTW's and/or the lU's lab.
Compliance with Monthly Average Limitations
POTWs are faced with the issue of how to assess an appropriate penalty for various types of violations
of the local pretreatment program. In evaluating this situation, the POTW should follow the reasoning of the
courts when assessing the number of violations which accrue as a result of a violation of a monthly average.
In Chesapeake Bay Foundation v. Gwaltney of Smithfield Ltd. 791 F.2d. 304 (4th Cir. 1986) a violation of the
monthly average was deemed to be a violation of each of the days of the month (not necessarily operating
days). The court reasoned that the language in the Clean Water Act "strongly suggests that where a violation
is defined in terms of a time period longer than a day, the maximum penalty assessable for that violation
should be defined in terms of the number of days in that time period." (Id at 314). This means that if there is
a violation of a monthly average, the largest penalty assessable is the maximum penalty authority of the
POTW (which should be, at a minimum, 1.000 dollars per day) multiplied by the number of days in the
month of violation. This is not necessarily the penalty which the POTW will impose on the IU, but it is the
maximum amount which the POTW may legally assess.
There has been some confusion on the part of some POTWs as to how many samples are required to
demonstrate a violation of a monthly average. At a minimum, the POTW needs only one valid sample from
the month to assess compliance with the monthly average. If the POTW has only one sample from an IU in
the six month reporting period and that sample is in violation of the monthly average, the maximum liability
the IU faces for that effluent violation in that six month period is the maximum penalty authority of the
POTW multiplied by the number of days in the month the sample was taken. This process should be used by
the POTW when evaluating the appropriate penalty amount to assess in situations where the POTW's
Enforcement Response Plan indicates the need to assess a penalty.
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Industrial User Sampling Manual Chapter 3 - Sampling Industrial Users
Closed Cup Flashpoint Sampling and Compliance
The General Pretreatment Regulations at 403.5(bXO require that no discharge to a POTW shall "create a
tire or explosion hazard in the POTW." The regulation further explains this requirement by setting a closed
cup flashpoint limit of 140°F (60°C) on wastestreams discharged to the POTW. Since this prohibitive limit is
an instantaneous limit, the POTW must use a grab sample to evaluate compliance with the closed cup
flashpoint requirement.
The POTW should monitor the ID's wastestream periodically for the potential of creating a tire hazard,
but this frequency should be based on the nature of the wastestream. If the POTW has reason to believe that
the IU has a strong notential to create a tire hazard, monitoring for the closed cup flashpoint should be
conducted regularly If the POTW has no reason to believe that the IU poses a fire hazard, minimum closed
cup flashpoint monitoring can be done. At a minimum, the POTW should evaluate the Ill's potential to
cause pass-through or interference, as well as the ILf's potential to violate any of the prohibitive discharge
limits, at least once every permit cycle (e.g., every five years if the !U's permit duration is five years long).
Frequency of POTW Sampling In Lieu of industrial User Sampling
The General Pretreatment Regulations allow for the POTW to take over the periodic sampling and
analysis activities for the industrial user. When the POTW chooses to exercise this option, the IU is not
required to submit the periodic sampling report required in 403.12(e). The General Pretreatment Regulations
also require POTWs to "inspect and sample the effluent from each Significant Industrial User at least once a
year." (403.8(0(2Xv)). The purpose of this inspection and sampling is to provide information, independent
of the IU, on the compliance status of the SIU. If the POTW is already conducting the periodic sampling for
the IU, however, the POTW is already evaluating compliance independent of the IU. Therefore, if the POTW
is conducting the required sampling for the IU under 403.12, the POTW is satisfying the 403.8 requirement of
annually sampling the IU. The POTW is still required to inspect each SIU annually, but the POTW would
only be required to conduct two sampling events at the IU, as required by 403.12.
The General Pretreatment Regulations require lUs to notify the Control Authority and conduct follow-up
sampling if the previous sample taken by the IU indicates a violation. The notification to the Control
Authority must be conducted within 24 hours of becoming aware of the violation, and the results of
resampling must be submitted to the Control Authority within 30 days. If the POTW is conducting the
sampling for the IU, however, there is no regulatory requirement for the POTW to resample after detecting a
violation. As a matter of policy, though, we strongly recommend that the POTW conduct the required repeat
sampling, or require the IU to conduct the repeat sampling, because this provides further information on the
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industrial User Sampling Manual Chapter 3 - Sampling industrial Users
nature of the ILJ's impact on the treatment plant and may provide further support in an enforcement action
taken by the POTW for effluent violations.
SNC in Situations With Multiple Outfalls
POTWs often encounter situations where industrial users have multiple outfalls (i.e.. connections to the
collection system) from the same categorical process line, and the question has been raised of how the POTW
should evaluate such situations for the purpose of determining the compliance status of the facility, especially
with respect to SNC. When the POTW encounters a multiple outfall situation, compliance with applicable
standards should be determined in the following manner.
Multiple outfall situations can arise in three ways: I) multiple categorical operations with multiple
outfalls, 2) a single categorical operation with multiple outfalls, and 3) a wastestream regulated by local limits
with multiple outfalls. Each of these circumstances are discussed below. If an industrial user has several
outfalls to the POTW from separate categorical operations, each of these outfalls and each pollutant parameter
per outfall must be evaluated separately for the purpose of determining whether the facility meets the criteria
for Significant Noncompliance. For example, if the IU has three outfalls from three separate categorical
operations and each outfall is regulated for chromium, cadmium and zinc, and any of the data from each
separate outfall exceeds either the chronic or TRC criterion, then the IU meets the criteria for SNC and
should be published in the newspaper by the POTW. When evaluating the compliance status of the IU keep
in mind that the IU must be evaluated on a categorical operation-by-categorical operation, parameter-by-
parameter, and outfall-by-outfall basis. However, if the IU has more than one outfall from the same
categorical operation (e.g., several lines from the same metal finishing operation), the POTW should treat
those different categorical operations as a single, aggregate line for purposes of determining compliance. For
example, if a metal finisher discharges categorical process wastewater generated from different categorical
operations in the same process line through two different sewer connections (without any intermediate
treatment), compliance with the categorical standard should be determined by using a flow weighted average
of the two lines. Finally, the POTW should be aware of how to evaluate compliance in situations where local
limits control the nature of the discharge and there is more than one discharge point to the POTW. If there is
more than one discharge point to the POTW which is regulated by a local limit (even if the separate outfalls
come from the same process line), then the facility must meet the local limit at the end of each pipe.
Likewise, the federal prohibitive standards in 403.5 must be met for each discharge point to the POTW no
matter where the discharge point is derived.
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Industrial User Samplinz Manual Chapter 3 - Sampling Industrial Users
Violation Dare
If a sample taken at an IU indicates a violation, the date of the violation is the date the sample was
taken, not the date the sample was analyzed in the laboratory. For a long-term composite sample, the date of
violation is the date the Samplexmmcdnapletdd.a sampler is placed at an industrial user at
SAM on Tuesday and picked up at SAM on Wednesday (the following day), but the sampler stopped taking
samples at 5PM Tuesday, the date of violation is 5PM Tuesday (not SAM Wednesday). (NOTK: In this
example, the required holding time for this sample would commence at SAM on Tuesday). This can be
important when the POTW goes to apply the rolling quarters method for determining SNC (as outlined in the
EPA Memorandum "Application and Use of the Regulatory Definition of Significant Noncompliance for
Industrial Users," September 9. 1991). When tracking the compliance status of each IU, the POTW should
have an automated system which tracks the date each sample was taken at each IU regulated by the POTW.
Compliance With Continuous Monitoring ofpH
The question of how to determine compliance with a pH limit when there is continuous monitoring has
often been raised by POTWs. The EPA has formally responded to this question in a letter to the State of
New Jersey. This letter is provided in Appendix VIII for your reference. The underlying concern of how to
determine compliance with continuous monitoring centers on the length of time allowed for pH to be out of
compliance with the limit. POTWs have been placed in the situation of having to determine what is an
acceptable amount of time to be out of compliance under a continuous monitoring scheme, and many POTW
have turned to the federal regulations at 401.17 to provide the answer. Part 401 .17 addresses the allowed
excursions for pH when applied to facilities which discharge directly to a receiving water. The question has
been asked whether or not this same excursion policy should be adopted for facilities which discharge to the
sanitary sewer. In general, POTWs may apply an excursion policy (although not necessarily the one found at
40 CFR 40 1. 17), with three important restrictions. First, the POTW may not allow an industrial user to
discharge waste below a pH of 5 (403.5(bX2)) unless the POTW is specifically designed to accommodate
such waste. Second, a POTW may not grant a variance from a categorical standard for an upper pH limit, if
such an upper limit exists in the standard. Finally, a POTW may not grant a waiver from a local pH limit if
the waiver would cause pass through or interference at the plant. If the POTW observes these restrictions, it
can establish a policy of allowing the pH discharge of a facility to go outside the range established in the
limit without the facility incurring any enforcement liability. If a POTW establishes a policy allowing pH
discharges outside the established range, the POTW should document such a policy in the POTWs
Enforcement Response Plan, Sewer Use Ordinance, or IU permit to ensure the enforceability of the policy.
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Industrial User Sampling Manual Chapter 3 - Sampling Industrial Users
Summary
This chapter discussed the procedures and protocols which should be used when sampling the effluent
from industrial users or when observing a permittee's self-monitoring procedures. The need for a sampling
plan and for coordinating with the laboratory performing the analyses were stressed in order to promote
consistency between samplers and to ensure that laboratory requirements are met during all sampling events.
The chapter also emphasized 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 to establish the validity of each sample result
should violations be identified that lead to an enforcement action. The chapter further explained several
instances in which special sampling requirements must be followed. Finally, this chapter 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.
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POTW Inspection Manual Chapter 3 - Sampling Industrial Users
Table 3-3
Volume of Sample Requited for Analyzing Various Industrial Pollutants
(Associated Water and Air Resource Engineers, Inc., 1973
Handbook for Monitoring Industrial Wastewater. U.S. EPA Technology Transfer
Analytical Tests Volume of Sample1 (ml)
PHYSICAL
Color and Odor 100 to 500
Corrosivity: flowing sample
Hlcctrical Conductivity' 100
pH. electrometric' 100
Radioactivity' 100 to 1.000
Specific gravity' loo
Temperature' flowing sample
Toxicity' 1,000 to 20,000
Turbidity' 100 to 1,000
CHEMICAL
Dissolved Gases:
Ammonia', NH,' 500
Carbon Dioxide' 200
Chlorine' 200
Hydrogen1 1,000
f Jydrogen Sulfide' 500
Oxygen' 500 to 1,000
Sulfur dioxide' 100
Miscellaneous
Acidity and alkalinity loo
Bacteria, iron 500
Bacteria, sulfate reducing 100
Biochemical Oxygen Demand (BOD) 100 to 500
Chemical Oxygen Demand (COD) 50 to 100
Chloroform extractable matter 1,000
Detergents 100 to 200
Hardness 50 to 100
Hydrazine 50 to loo
Microorganisms 100 to 200
Volatile and filming amines 500 to 1.000
Oil and Grease 3,000 to 5,000
Organic Nitrogen 500 to 1,000
Phenolic compounds 800 to 4,000
pH, colorimetric IO to 20
Polyphosphates loo to 200
Silica 50 to 1,000
Solids, dissolved 100 to 20,000
Solids, suspended 50 to 1,000
Tannin and Lignin loo to 200
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POTW Inspection Manual Chapter 3 - Sampling Industrial Users
Table 3-3
Volume of Sample Required for Analyzing Various Industrial Pollutants (cont)
Anal&al Tests: Volume of Sample (ml)
Cations:
Aluminum, AF" . . loo to 1.000
Ammonium'. NH,' . . 500
Antimony, Sb"' to Sb loo to 1,000
Arsenic, As"' to As""' 100 to 1,000
Barium, Ba" loo to 1,000
Cadmium. Cd* 100 to 1,000
Calcium, Ca" 100 to 1,000
Chromium, Cr"* to Cr*"*' loo to 1,000
Copper, Cu" 200 to 4.000
Iron', Fe" to Fe'" 100 to 1.000
Magnesium, Mg" 100 to 4,000
Manganese, Mn" to Mn " 100 to 1,000
Mercury, Hg' to Hg" loo to 1,000
Potassium, K' loo to 1,000
Nickel, Ni" loo to 1,000
Silver, Ag' loo to 1,000
Sodium, Na' 100 to 1,000
Strontium, Sr" 100 to 1,000
Tin, Sn"' to Sn"" 100 to 1,000
Zinc, Zn" 100 to 1,000
Anions:
Bicarbonate, HCO, . 100 to 200
Bromide, Br' . 100
Carbonate, CO,' 100 to 200
Chlorine, CI~ 25 to 100
Cyanide, Cn' 25 to 100
Fluonde, Fl 200
Hydroxide, OH' 50 to loo
Iodide, I 100
Nitrate, NO; IO to 100
Nitnte, NOf 50 to 100
Phosphorous, ortho, PO,', HPO4', H:PO, 50 to 100
Sulfate, SO/, HSO,' 100 to 1,000
Sulfide, S-, HS' 100 to 500
Sulfite. SO,", HSO," 50 to loo
' Volumes specified in this table should be considered as guides for the approximate quantity of sample
necessary for a particular analysis. The exact quantity used should be consistent with the volume
prescribed in the standard method of analysis, whenever a volume is specified.
2 Aliquot may be used for other determinations.
' Samples for usntable constituents must be obtained in separate containers, preserved as precribed,
completely filled, and sealed against all exposure.
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POTWInspection Manual
Chapter 3 - Sampling Industrial Users
Table 3-4
Required Containers, Preservation Techniques, Holding Times, and Test Methods
(Excerpt from 40 CFR PM 136 Tab& I and II)
EPA Tar Method
(1979)
Pollutant Parameter
BACTERIAL TESTS
Colifonn, Fecal and Total
Fecal Streptococci
INORGANIC TESTS
Acidity
Alkalinity
Ammonia
BOD
BOD. carbonaceous
Bromide
Chemical Oxygen
Demand
Chloride
Chlorine, total residual
Color
Cyanide, total and
amenable to chlorination
Fluoride
Hardness
Container"'
P,G
P,G
P,G
P,G
P,G
P,G
P,G
P,G
P,G
P,G
P,G
P,G
P,G
P
P,G
Preservative aJ)
Cool to 4°C
0.008% NajSjO,""
Cool to 4°C
0.008% NajSjO,""
Cool to 4°C
Cool to 4°C
Cool to 4°C
H3SO< to pH<2
Cool to 4°C
Cool to 4°C
None required
Cool to 4°C
HSO, to pH<2
None required
None required
Cool to 4°C
Cool to 4°C
NaOH to pH>12
0.6g ascorbic acid'"
None required
HNO, to pH<2,
H2SO, to pH<2
Maximum
Holding Time1"
6 Hours
6 Hours
14 days
14 days
28 days
48 Hours
48 Hours
28 Hours
28 Hours
28 days
Analyze
immediately
48 Hours
14 days (6)
28 days
6 months
[unless otherwise
noted)'"1
Standard Methods
15th Ed.: 908
Standard Methods
15th Ed.: 910
305.1
310.1
350
405.1
Standard Methods
16* Ed.:507(5.e.6)
320.1
410
325
330
110
335
340
130
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POTW Inspection Manual
Chapter 3 - Sampling Industrial Users
Table 3-4 (Conk)
Required Containers, Preservation Techniques, Holding Times, and Test Methods
(Excerpt from 40 CFR Part 136 Table I and II)
EPA Tat Mtthod
(I 979)
M otherwise
noted)
Parameter
Hydrogen Ion (pH)
TKN. organic nitrogen
METAL!?"
Hexavalent Chromium
Mercury
Metals, (except above)
Nitrate
Nitrate -nitrite
Nitrite
Oil and Grease
Organic Carbon
Orthophosphate
Phosphorous
Dissolved Oxygen
Probe
Wmkler
Phenols
Container™
P.G
P.G
P,G
P.G
P.G
P.G
P.G
P.G
G
P.G
P.G
G bottle/top
G bottle/top
G
Preservative**
None required
Cool to 4°C
H2SO4 to pH<2
Cool to 4°C
HNO' to pH<2
HNO' to pH<2
Cool to 4°C
Cool to 4°C
H:SO4 to pH<2
Cool to 4°C
Cool to 4°C
H2SO4 to pH<2
Cool to 4°C. HCI or
H2SO4 to pH<2
Filter immediately
Cool to 4°C
None required
Fix on-site and
store in the dark
Cool to 4°C
H2SO4 to pH<2
Maximum
Holding Time(t>
Analyze
immediately
28 days
24 Hours
28 days
6 months
48 Hours
28 days
48 Hours
28 days
28 days
48 Hours
Immed. analysis
8 Hours
24 Hours
(unit
150.1
351
218.4
245
(Vane
352.1
353
354
413
415
365
360
420
Phosphorous (elemental) G
Cool to 4°C
48 Hours
Note
(16)
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POTW Inspection Manual
Chapter 3 - Sampling industrial Users
Table 3-4 (Cent.)
Required Containers, Preservation Techniques, Holding Times, and Test Methods
(Excerpt from 40 CFR Part 136 Table I and II)
EPA Test Method
(1979)
ss otherwise
noted)
Parameter
Phos. (total dissolved)
Residue, total
Residue, filterable
Residue, nonfilterable (TSS)
Residue, settleable
Residue, volatile
Silica
Specific conductance
Sulfate
Sulfide
Sulfite
Surfactants
Temperature
Turbidity
ORGANIC TESTS'"
Purgeable halocarbons
Container"'
P,G
P.G
P,G
P,G
P,G
P,G
P
P,G
P,G
P.G
P,G
P.G
P.G
P.G
G, tcrton
lined
septum
Preservative11*
Cool to 4°C
H2SO4 to pH<2
Cool to 4°C
Cool to 4°C
Cool to 4°C
Cool to 4°C
Cool to 4°C
Cool to 4°C
Cool to 4°C
Cool to 4°C
Cool to 4°C add
zinc acetate plus
NaOH to pH>9
None required
Cool to 4°C
None required
Cool to 4°C
Cool to 4°C
0.008Na2S2O'0)
Maximum
Holding Time*4*
28 days
7 days
7 days
7 days
48 Hours
7 days
28 days
28 days
28 days
7 days
Analyze
immediately
48 Hours
Analyze
immediately
48 Hours
14 days
(unit
365
160.3
160.1
160.2
760.5
160.4
370.1
120.1
575
576
577
425. 1
170.1
180.1
601 0
Apper
1984)
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POTW Inspection Manual
Chapter 3 - Sampling Industrial Users
Table 3-1 (ConL)
Required Containers, Preservation Techniques, Holding Times, and Test Methods
(Excerpt from 49 CFR Part 136 Table I and II)
Parameter
Purgcablc Aromatic Hydrocarbons
Acrolein and acrylonitrile
Phenols
Benzidines'''
Phthalate esters"
Nitrosamines"
Polychlorinated Biphenyls"
Nitroaromatics and
isophorone' '''
Polynuclear aromatic hydrocarbons"
Contained"
G, teflon-
lined
septum
G, teflon-
lined
septum
G, teflon-
lined cap
G, teflon-
lined cap
G. teflon-
lined cap
G, teflon-
lined cap
G. teflon-
lined cap
G, teflon-
lined cap
G. teflon-
lined cap
Preservative™
Cool to 4°C
0.008% NajS2O,(M
HCI to pH 2'"
Cool to 4°C
0.008% NajSjCV"
Adjust pH/4.5"0)
Cool to 4°C
0.008% NajSA'"
Cool to 4°£
0.008% NajSjO,'"
Cool to 4°C
Cool to 4°C
Store in the dark
0.008% NihSz
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POTW Inspection Manual
Chapter 3 - Sampling Industrial Users
Tab&? 3-4 (Cent.)
Required Containers, Preservation Techniques, Holding Times, and Test Methods
(Excerpt from 40 CFR Part 136 Tab& I and II)
Parameter
ORGANIC TESTS (cont.)""
Haloethers""
Chlorinated Hydrobarbons'
.do
TCDD (2,3,7,8-Tctrachlordibenzo-p-
dioxin)""
PESTICIDES TESTS
Organochlorine pesticides""
RADIOLOGICAL TEST
Alpha, beta, and radium
KEY
(1)
(2)
EPA Method
[19791
Maximum (unless
Container"' PratrvativJ1^ Hold Tlme{t) otherwise
noted)
G, teflon-lined Cool to 4°C 7 days until 611 (40 CFR
cap extraction; 40 136 Appendix
days after A, 1984)
extraction
G, teflon-lined
cap
G, teflon-lined
cap
Cool to 4°C
a. aas%
Na,S,0,(5)
EBB! to 4°E
0.0087.
NajSjO,'"
7 days until
extraction; 40
days after
extraction
7 days until
extraction; 40
days after
extraction
612 [40 CFR
136 Appendix
A, 1984)
613 [40 CFR
136 Appendix
A, 1984)
G, teflon-lined
cap
P,G
Cool to 4°C 7 days until 608 [40 CFR
pH 5-9"" extraction; 40 136 Appendix
days after A, 1984)
extraction
HNO, to pH<2 6 months
Meth. 900-903
(17)
(3)
Polyethylene (P) or Glass (G)
Sample preservation should be performed immediately upon sample collection. For composite chemical
samples, each aliquot should be preserved at the time of collection. When use of an automatic sampler
makes it impossible to preserve each aliquot, then chemical samples may be preserved by maintaining
at 4°C until compositing and sample splitting is completed.
When any sample is to be shipped by common carrier or sent through the United States mail, it must
comply with the Department of Transportation Hazardous Materials Regulations (49 CFR Part 172). The
person offering such material for transportation is responsible for ensuring such compliance. For the
113
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POTW Inspection Manual Chapter 3 - Sampling Industrial Users
Table 3-4 (Conk)
Required Containers, Preservation Techniques, Holding Times, and Test Methods
(Excerpt from 40 CFR Part 136 Table I and II)
preservation requirements of this table, the Office of Hazardous Materials. Materials Transportation
Bureau, Department of Transportation has determined that the Hazardous Materials Regulations do not
apply to the following materials: hydrochloric acid (HCI) in water solutions at concentrations of 0.04%
by weight or less (pH about 1.96 or greater); nitric acid (HNO,) in water solutions at concentrations of
0.15% by weight or less (pH about 1 .62 or greater); sulfuric acid (H2SO4) in water solutions at
concentrations of 0.35% by weight or less (pH about 1.15 or greater); and sodium hydoroxide (NaOH)
in water solutions at concentrations of 0.80% by weight or less (pH about 12.3 or less).
(4) Samples should be analyzed as soon as possible after collection. The times listed are the maximum times
that samples may be held before analysis and still be considered valid. Samples may be held for longer
periods only if the permittee, or laboratory, has data on file to show that the specific types of samples
under study are stable for the longer time and has received a variance from the Regional Adminstrator
under §136.3(e). Some samples may not be stable for the maximum time period given in the table. A
permittee, or monitoring laboratory, is obligated to hold the sample for a shorter period of time if
knowledge exists to show this is necessary to maintain sample stability and integrity.
(5) Should only be used in the presence of residual chlorine.
(6) Maximum holding time is 24 hours when sulfide is present. Optionally, all samples may be tested with
lead acetate paper before pH adjustments to determine if sulfide is present. If sulfide is present, it can
be removed by the addition of cadmium nitrate powder until a negative spot test is obtained. The sample
is filtered, then NaOH is added to raise the pH to 12.
(7) Samples should be filtered immediately on-site before adding preservative for dissolved metals.
(8) Guidance applies to samples to be analyzed by GC, LC, GC/MS for specific organic compounds.
(9) Sample receiving no pH adjustment must be analyzed within 7 days of sampling.
(10) The pH adjustment is not required if acrolein will not be measured. Samples for acrolein receiving no
pH adjustment must be analyzed within 3 days of sampling.
(11) When extractable analytes of concern fall within a single chemical category, the specified preservation
and maximum holding times should be observed for optimum safeguarding of sample integrity. When
the analytes of concern fall within two or more chemical categories, the sample may be preserved by
cooling to 4°C, reducing residual chlorine with 0.008% sodium thiosulfate. storing in the dark, and
adjusting the pH to 6-9; samples preserved in this manner may be held for 7 days before extraction and
for 40 days after extraction. Exceptions to this optional preservation and holding time procedure are
noted in footnote (5) (re: the requirement for thiosulfate reduction of residual chlorine and footnotes (12).
(1 3) (re: the analysis of benzidine).
(12) If 1,2-diphenylhydrazine is likely to be present, adjust the pH of the sample to 4.0 ±0.2 to prevent
rearrangement of the benzidine.
(13) Extracts ma> be stored up to 7 days before analysis if storage is conducted under an inert (oxidant-free)
atmosphere.
114
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POTW inspection Manual Chapter 3 - Sampling Industrial Users
Table .M (Cent)
Required Containers, Preservation Techniques, Holding Tunes, and Test Methods
(Except from 40 CFR Part 136 Table I and II)
(14) For the analysis of diphenylnotrosamine, add 0.008% NajSjO, and adjust pH to 7-10 with NaOH within
24 hours of sampling
(15) The pH adjustment may be performed upon receipt of the sample at the laboratory and may be omitted
if the samples are extracted within 72 hours of collection. For the analysis of aldrin, add 0.008%
Na,S:O,.
(16) K.F. Addison and R.G. Ackman, "Direct Determination of Elemental Phosphorous by Gas-Liquid
Chromatography," Journal of ChromatOKraohy, 47 (3): 421-426, 1970.
(17) Reference: "Prescribed Procedures for Measurement of Radioactivity in Drinking Water" EPA-600/4-80-
032 (1980 Update) U.S. EPA, August, 1980.
(18) This list does not represent an exhaustive list of all approved test methods. When determining the
appropriate analytical method, always refer to 40 CFR Part 136. NOTE: See Appendix XIII for details
on 40 CFR Part 136.
115
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POTW Inspection Manual
Chapter 3 - Sampling Industrial Users
Table 3-4 (ConL)
Required Containers, Preservation Techniques, Holding Times, and Test Methods
(Excerpt from 40 CFR Part 136 Table I and II)
Parameter
ORGANIC TESTS (cont)""
Haloethers*
Chlorinated Hydrobarbons'
(in
Container*
G, teflon-lined
cap
G, teflon-lined
cap
Preservative™
Cool to 4°C
Cool to 4°C
0.008%
TCDD (2,3,7,8-Tctrachlordibcnzo-p- G, teflon-lined
dioxin)"" cap
PESTICIDES TESTS
Organochlorine pesticides'"' G, teflon-lined
cap
RADIOLOGICAL TEST
Alpha, beta, and radium P,G
KEY
Cool to 4°C
0.008%
Cool to 4°C
pH 5-9"»
Maximum
Hold Tlmew
EPA Method
(1979)
(unless
otherwise
noted)
7 days until 611 (40 CFR
extraction; 40 136 Appendix
days after A, 1984)
extraction
7 days until 612 (40 CFR
extraction; 40 136 Appendix
days after A, 1984)
extraction
7 days until 613 (40 CFR
extraction; 40 136 Appendix
days after A. 1984)
extraction
7 days until 608 (40 CFR
extraction; 40 136 Appendix
days after A, 1984)
extraction
HN03 to pH<2 6 months
Meth. 900-903<17)
(1) Polyethylene (P) or Glass (G)
(2) Sample preservation should be performed immediately upon sample collection. For composite chemical
samples, each aliquot should be preserved at the time of collection. When use of an automatic sampler
makes it impossible to preserve each aliquot, then chemical samples may be preserved by maintaining
at 4°C until compositing and sample splitting is completed.
(3) When any sample is to be shipped by common carrier or sent through the United States mail, it must
comply with the Department of Transportation Hazardous Materials Regulations (49 CFR Part 172). The
person offering such material for transportation is responsible for ensuring such compliance. For the
113
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POTW Inspection Manual Chapter 3 - Sampling Industrial Users
Table 3-4 (Cent.)
Required Containers, Preservation Techniques, Holding Times, and Test Methods
(Excerpt from 40 CFR Part 136 Table I and II)
preservation requirements of this table, the Office of Hazardous Materials, Materials Transportation
Bureau, Department of Transportation has determined that the Hazardous Materials Regulations do not
apply to the following materials: hydrochloric acid (HCI) in water solutions at concentrations of 0.04%
by weight or less (pH about 1.96 or greater); nitric acid (UNO,) in water solutions at concentrations of
0.15% by weight or less (pH about 1.62 or greater); sulfuric acid (H2SO4) in water solutions at
concentrations of 0.35% by weight or less (pH about 1.15 or greater); and sodium hydoroxide (NaOH)
in water solutions at concentrations of 0.80% by weight or less (pH about 12.3 or less)
(4) Samples should be analyzed as soon as possible after collection. The times listed are the maximum times
that samples may be held before analysis and still be considered valid. Samples may be held for longer
periods only if the permittee, or laboratory, has data on file to show that the specific types of samples
under study are stable for the longer time and has received a variance from the Regional Adminstrator
under §136.3(e). Some samples may not be stable for the maximum time period given in the table. A
permittee, or monitoring laboratory, is obligated to hold the sample for a shorter period of time if
knowledge exists to show this is necessary to maintain sample stability and integrity
(5) Should only be used in the presence of residual chlorine.
(6) Maximum holding time is 24 hours when sulfide is present. Optionally, all samples may be tested with
lead acetate paper before pH adjustments to determine if sulfide is present. If sulfide is present, it can
be removed by the addition of cadmium nitrate powder until a negative spot test is obtained. The sample
is filtered, then NaOH is added to raise the pH to 12.
(7) Samples should be filtered immediately on-site before adding preservative for dissolved metals.
(8) Guidance applies to samples to be analyzed by GC, LC, GC/MS for specific organic compounds.
(9) Sample receiving no pH adjustment must be analyzed within 7 days of sampling.
(10) The pH adjustment is not required if acrolein will not be measured. Samples for acrolein receiving no
pH adjustment must be analyzed within 3 days of sampling.
(11) When extractabte analytes of concern fall within a single chemical category, the specified preservation
and maximum holding times should be observed for optimum safeguarding of sample integrity. When
the anatytes of concern fall within two or more chemical categories, the sample may be preserved by
cooling to 4°C, reducing residual chlorine with 0.008% sodium thiosulfate, storing in the dark, and
adjusting the pH to 6-9; samples preserved in this manner may be held for 7 days before extraction and
for 40 days after extraction. Exceptions to this optional preservation and holding time procedure are
noted in footnote (5) (re: the requirement for thiosulfate reduction of residual chlorine and footnotes (12),
(13) (re: the analysis of benzidine).
(12) If 1,2-diphenylhydrazine is likely to be present, adjust the pH of the sample to 4.0 ±0.2 to prevent
rearrangement of the benzidine.
(13) Extracts may be stored up to 7 days before analysis if storage is conducted under an inert (oxidant-free)
atmosphere.
114
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POTW Inspection Manual Chapter 3 - Sampling Industrial Users
Table 3-4 (Cent)
Required Containers, Preservation Techniques, Holding Times, and Test Methods
(Excerpt from 40 CFR Part 136 Table I and II)
(14) For the analysis of diphenylnotrosamine, add 0.008% Na^SjO, and adjust pH to 7-10 with NaOH within
24 hours of sampling.
(15) The pH adjustment may be performed upon receipt of the sample at the laboratory and may be omitted
if the samples are extracted within 72 hours of collection. For the analysis of aldrin, add 0.008%
Na,S:O,.
(16) K.F. Addison and R.G. Ackman, "Direct Determination of Elemental Phosphorous by Gas-Liquid
Chromatography," Journal of Chromatographv, 47 (3): 421-426, 1970.
(17) Reference: "Prescribed Procedures for Measurement of Radioactivity in Drinking Water" EPA-600/4-80-
032 (1980 Update) U.S. EPA, August, 1980.
(18) This list does not represent an exhaustive list of all approved test methods. When determining the
appropriate analytical method, always refer to 40 CFR Part 136. NOTE: See Appendii XIII for details
on 40 CFR Part 136.
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Appendix I
General Industrial Inspection Questions
-------
General Industrial Inspection Questions
GENERAL QUESTIONS
A. Usage of Chemicals, Cleaners, and Location of Drains
1. Check the proximity of any chemical storage areas to floor drains. What kind of chemicals are
stored? Chemicals might include, paint, thinner, solvents, etc. Are the chemicals stored in a way that
they could reach the floor drains if spilled?
2. Check the floor washdown procedures (frequency, water usage, detergents). What is the frequency
(daily, periodical) of the washdown? Are high pressure sprays used? Are detergents used? How is
the wash water disposed?
3. If floor drains are sealed, do employees have access?
4. Check for the use of detergents and chemical cleaners for equipment washdown. Acids (e.g.,
muriatic, sulfuric, phosphoric, acetic, etc.), surfactants, caustic soda, soda ash, and phosphates are
commonly used as cleaners. How are these materials stored? How are working concentrations of
chemical prepared, and who prepares them?
B. Cooline Waters
1. Are there any sources of uncontaminated cooling water in the plant? Are there any sources of
recirculated or once-through cooling waters? What is the disposal method of the cooling water?
2. If contact cooling water is used, is it treated in any way before discharge? What contaminants would
be in the water? Are conditioning chemicals added to cooling waters?
3. Is there any water cooled machinery used by the facility? What contaminants would be in the water?
What is the volume and how is the cooling water disposed?
C. Solvents
1. Does the facility use any solvents or degreasing agents?
2. Are any solvent wastes handled separately from the other cleaning solution wastes?
3. Is there any batch pretreatment prior to discharge?
4. How are any residual materials, sludges at the bottom of the tank disposed?
5. Is there a solvents management plan to reduce solvent waste at the facility?
6. If solvents are used, are they redistilled on-site? Does this process generate uncontaminated cooling
water? Where is it discharged?
D. Boiler Discharge
1. Check the frequency and volume of any boiler blowdown Check on the usage of additives to the
boiler make-up waters. Do the additives contain any metals or priority pollutants?
2. What types of boiler pretreatment is used (e.g., ion exchange, chemical addition, etc.)? Are there any
boiler wastes generated?
3. What is the frequency and volume of boiler blowdown?'
4. Is the waste stream acting as a dilution stream at a process monitoring point?
5. Are there air pollution control devices which use water? How is the water disposed>
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POTW Inspection and Sampling Manual Appendix I
E. Discharge Locations and Sampling Points
1. Are the facility's domestic and process wastewaters segregated?
2. What method is used to determine domestic and process discharge volumes?
3. Are dilution streams accounted for at the monitoring point?
4. Does the facility have a sampling point available which is representative of the process wastewaters
discharged?
F. Food Processing
I What are the products processed at the facility? What is the production rate?
2. Does the facility use flow equalization prior to discharging into the sewer? Does the facility have
any provisions to respond to a produce spill into the wastewater system?
3. Does the facility generate any byproducts which have associated wastewaters?
4 Is there any coloring added to the product? Is there any treatment for removal of the color?
5 Check for the usage of chemical cleaners for equipment washdown. Acids (e.g., muriatic, acetic,
sulfuric. and phosphoric), surfactants, caustic soda, soda ash, and phosphates are commonly used as
cleaners. How are these materials stored and used?
6 Check the floor washdown procedures. Are equipment and floors washed down with water?
7 What is the water consumption rate of the operation (total gallons per day and the number of pounds
of product or pounds of material processed)? How much water is generated by or incorporated into
the product?
8 What percent of water use is recycled? Does this include any uncontaminated water (for
refrigeration, machinery, etc.)? NOTE: Single pass cooling water is common in food processing and
should be checked or verified.
9 What kind of containers does the facility use to package the product? Are containers made on-site?
Are they washed or sterilized?
10 Are acidic and caustic solutions used and when are pH samples taken by the facility?
G. Pretreatment
1 What kind of treatment systems does the facility have in place for each of the various types of
process wastewaters discharged? What chemicals are added? How often are monitoring equipment
calibrated?
2. Are any of the process wastewaters subject to National categorical pretreatment standards? If so, are
dilution waste streams accounted for during monitoring?
3 Does the facility combine its waste from the various sources prior to treatment or discharge? Is the
combined wastestream formula applicable? If so, are proposed waste stream volume determination
method accurate?
H Radioactive Materials
1 Determine the maximum quantity of each radionuctide used, stored, and discharged at the facility
Does the storage area have adequate spill control?
2. How are liquid and solid radioactive wastes being disposed?
3. Are the> being hauled away? If so, what is the name of the hauler and what is the destination of the
waste?
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POTW Inspection and Sampling Manual Appendix I
4. Are they being discharged to the sanitary sewer? If so, how often and what are the maximum
concentrations in Curies?
5. Obtain a copy of the industrial user's radioactive user's license(s).
6. Obtain a copy of any protocols for handling radioactive materials at the facility.
7. Obtain a copy of any logs pertaining to radioactive discharges.
I - 3
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Appendix II
Industry Specific Questions
-------
Industry Specific Questions
Adhesives and Sealants:
I. What is the product manufactured at the facility? Are the adhesives water-based or organic solvent base
materials0 What kind of binder material is used?
2. Are there any product washing operations? Are reactor vessels washed down between batches0 Is water
or a solvent used? Would these wastes be discharged to the sewer? What is the frequency and volume of
washing operations?
3. Check the general questions on solvents listed below.
4. Check the usage of cooling waters. See general questions on cooling waters listed below.
Aluminum Forming:
1. What is the production rate of this facility in terms of mass of aluminum or aluminum alloy processes per
year? Is there an accurate method for determining off-lbs from individual processes?
2. What are the forming processes at the facility? Is there a waste stream generated from any air pollution
control unit present?
3. What kind of metal forming lubricating compounds are used? Is water recycling feasible?
4. How often are the lubricant-wastewater emulsions changed and discharged?
5. Is there a continuous overflow from quenching water baths? What is the disposal method for the quench
waters?
6. Is any casting done on site? If yes, see questions under Metal Refineries and Foundries listed below
7. Are any solvents used as part of the cleaning processes? Refer to the general questions on Solvents.
8. Are wastewaters from desmutting and deoxidizing pretreated before discharge to the sewers? What volume
is discharged?
9. Are there any metal finishing processes (anodizing, chemical conversion coatings, coloring, dyeing, chemical
sealing, chemical or electrochemical brightening, or etching) done on site? If yes. refer to questions under
Electroplating and Metal Finishing listed below.
Auto Repair and Paint Shops:
I. Do the paint booths use a water curtain? If so, how often is it discharged? How is the bottom sludge
disposed? Are water conditioning chemicals used?
2. Check the paint spray gun cleaning procedures and the method of disposal of any cleanings. Are employees
trained, supervised, and rewarded to paint efficiently, thus reducing contaminants to the sewer?
3. How does the facility dispose of old unwanted paint?
4. Is there any other disposal of any chemicals at this site? What is the disposal method?
Auto Parts and Suppliers: Wholesale and Retail
\. If floor drains are present, is there any storage of oils, paint, ami-freeze, transmission and brake fluids, or
any other fluids within the proximity of the drains? What is the quantity of fluids stored?
2. Check the location and manner of storage of batteries and battery acid.
3. Check for used crankcase oil and return facilities.
4. Check for any machining or repair. See Auto Repair questions.
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POTW Inspection and Sampling Manual Appendix II
Auto Repair (Mechanical) - Engine and Transmission Work
1 Look for drains under service bays. What is the destination of the drain?
2 Identify the location of any gas/oil interceptors or separators. What kind of unit is it and what is the general
operating condition of the unit?
3 Check on the use of solvents and parts degreasers. Check the general questions on solvents.
4. Check for the storage of fluids such as oil. transmission fluid, brake fluid, and anti-freeze.
5. Check on the quantity and method of waste oil storage and the manner and location in which it is disposed.
Auto Wash
\ Check for any system for water reuse or reclamation such as settling tank.
2 If a settling tank exists, check how the sludge from it is handled and by whom, what is the ultimate disposal
method?
3. Check what types of cleaners are used. Do any specialty cleaners such as tire cleaners contain solvents?
Do waxes contain solvents? If yes, check the general questions on solvents.
4 Check for an oil and grease separator on the discharge line.
5 Check for the storage of any liquids near the floor drains.
6. Check and identify the water consumption level.
7 Can the facility handle trucks? If so, what kinds of materials might be contained in the trucks and what the
washwater contamination from those materials?
Bakeries - Retail
\ Check the washdown and cleanup procedures.
2. Check the storage of cleaning agents.
.1. Check the storage of baking ingredients.
4 Check the quantity of deep fry grease generated. Note how it is disposed.
5 Check for the presence of any grease interceptor. Describe the size and general condition of the unit How
often and b\ whom is it serviced? How is the grease disposed?
Battery Manufacturing
I. What is the production rate of the facility (number of units manufactured, amp per hour output, etc.)?
2 What is the primary reactive anode material (cadmium, calcium, lead, Icelandic, lithium, magnesium,
nuclear, /inc) used for the batteries produced at the facility?
3. What volume of wastewater from electrodeposition rinses, scrubber bleed off and caustic removal is
discharged to the sewer?
4 Are depolari/crs used in the manufacturing process? What type? What is the final disposal method of these
materials''
5. What kind of electrolytes does the facility use? Check the general questions on Usage of Chemicals,
Cleaners and Location of Drains.
Beverages
I. Check the general questions on Food Processing.
II-2
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POTW Inspection and Sampling Manual Appendix 11
Blueprinting and Photocopying
1. Check to see if they do any offset printing (related questions).
2. What type of blueprinting machines are being used? With some, the total ammonia is totally consumed
while other will have spent ammonia solution to dispose.
3. Js there a significant amount of ammonia stored? Check the floor drains.
4. Check the usage of other cleaning agents and solvents. Are there any chemicals of concern'.'
Canned and Preserved Fruits and Vegetables
1. Check what detergents and techniques are used in washing fruits and vegetables before rinsing.
2. In addition to checking the water usage for washing, rinsing, and cooling, check to see if water is also used
for conveyance and the amounts used.
3. Is peeling done chemically (i.e., caustic soda, surfactants to soften the cortex)? Is there any discharge from
the peeling operation?
4. Check the floor washdown procedures. Are equipments and floors washed down with water?
5. Does the facility have a grease and soiids recovery system? Is there any other pretreatment before
discharge? Describe the system. How often is monitoring equipment calibrated?
6. Are there any processing brines used by the facility? How are these brines disposed of? Check the kind
of treatment given the brines prior to discharge to the sewer.
7. How are the larger remains of processed fruit and vegetables disposed (ground up and flushed down the
sewer? used as byproducts?)?
8. Check the refrigeration system for possible leaks.
9. Are there any fungicides or other similar chemicals used in the processing? Are they discharged to the
sewer?
10. Check the general questions on Food Processing.
Coil Coating (Including Canmakins)
1. What is the average square footage of metal sheeting processed at the facility (either on a daily or annual
basis)?
2. What is the base metal processed (aluminum, galvanized steel, and/or steel)?
3. Check the general questions on solvents.
4. What sort of conversion coating is used at the facility (chromating, phosphating, complex oxides)?
5. What solvents are used to control viscosity?
6. Is there a continuous overflow from quenching water baths? What is the disposal method from the quench
waters?
Canmaking (in addition to the questions above)
1. What kind of metal forming lubricants does the facility use?
2. What is the volume of rinse waters discharged to the sewer? Have the wastewaters been characterized?
Eating Establishments: (Restaurants)
I. Check for the presence of any grease interceptor. Describe the size and general condition of the unit. How
often and by whom is the unit serviced? How is the grease disposed?
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POTW Inspection and Sampling Manual Appendix II
2. How does the facility dispose of spent cooking grease?
3. How does the facility dispose of edible garbage material?
4. Check what types of janitorial cleaners are used. How are they stored?
5. Does the facility use an automatic dishwasher? Approximately how may hours per day does it operate?
What is the discharge temperature and the water consumption rate? Is the dishwasher connected to any
grease interceptors?
6. How may sinks does the facility have and how are they used?
7. How are grill cleaning residuals disposed?
Electric Services
Steam Electric Power Generation
1. Are the plants run on coal, oil, or gas?
2. What is the source of condenser cooling water (e.g., city, river, wells)? Are there any water treatment
chemicals added by the facility? How is the cooling water disposed?
3. What is done with the waste oils?
Substations
1. Check the location of any floor drains.
2. Is there any contact cooling water discharge?
3. Look for signs of leaking transformer oil and to where it would go if leakage occurred. Look for a label
on the transformer for the identification of PCBs. What percentage of PCBs are in the oil?
Electronic Components
1. What is the product that is manufactured at this facility?
2. Does the facility use any solvents or degreasing agents? If yes. check the general questions under Solvents.
3. Does the facility use any cooling water? Check the general questions under Cooling Waters.
4. Does the facility have a clean air room for which is must scrub air? Are there any chemical wastes
generated from the scrubber0 How is the waste disposed?
5. Does the facility conduct any electroplating activities? Check the questions under Electroplating and Metal
Finishing.
6. Is there any water recycle.reuse within the plant? Does the plant employ pretreatment for the recycle
streams?
7. Does the facility employ any photographic processes?
8. Check the general questions under Solids Disposal.
Electroplating and Metal Finishing
I. Try to determine the quantity of plating done by the facility in terms of surface area (sq. ft., etc.) plated.
2. How often does the facility change its cleaning solutions, both acidic and alkaline cleaners? What is the
volume for each change and how is the old material disposed? Is there any batch pretreatment prior to
discharge'1 How are any residual materials, i.e., sludges, at the bottom of the tank disposed?
3. Does the facility use any solvents or degreasing agents0 If yes, check the general questions under Solvents.
4. Does the facility use any cooling water? If yes, check the general questions under Cooling Waters.
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POTW Inspection and Sampling Manual Appendix II
5. What types of chemicals make up the plating baths? Is cyanide used in the plating operations? Is there any
chromium used? Is there any ammonium persulfate used in an etching process? Are employees aware of
water conservation'drag out?
6 How often are plating bath solutions changed? What is the volume for each change and how is the old
material disposed? Is there any batch pretreatment prior to discharge? How are any residual materials at
the bottom of the tank disposed?
7. Is there any water recycle reuse within the plant? Does the plant employ any pretreatment for the recycle
streams?
8. If masking is employed, are photographic processes involved (circuit boards)?
9. Are there metal finishing operations (e.g., machining, grinding, coloring, brightening, etc.) associated with
the plating operations?
10. If metal coloring is present, are organic dyes used?
11. Check the plumbing of the process wastewater from the plating room to the pretreatment system or sewers.
Are floor drains in the plating room directed to the pretreatment units? Are floors washed down regularly?
How much water is used and discharged? Where is the discharge location for dilution streams9
12. Does the facility use running water systems for rinsing? Are the units set up for countercurrent flows? Are
any still or dead rinses used? Check if the rinsewaters are pretreated prior to being discharged.
13. Has the facility been checked against any interconnections of the public water supply with process lines
(cross connections)? Are there backflow preventers in place?
14. Check the general questions under Solids Disposal.
Explosives
1. What are the products manufactured at this facility?
2. Does the facility blend these products into end-use products?
3. is ammonium nitrate used in the product and if so, how is it monitored for in the wastewater?
4. Does the facility have a disposal area for obsolete, off-grade, contaminated, or unsafe explosives and
propellants?
5. Are the products produced for private sector usage or military usage? Are there any security clearances
necessary to enter the facility?
6. Check the general questions for Solids Disposal.
Fiberglass Insulation
1. What methods are used to bind and cool the glass after is has been drawn into fibers? What wastes are
generated from this phase? Are these wastes pretreated prior to being discharged to the sewer?
2. What method is employed for collecting the glass fibers (i.e., wire mesh conveyors, flight conveyors, etc.)?
What methods are used to clean the conveyors or any glass fibers? Is this process shut down or in service
while being cleaned? What type of cleaning agent is used? Is the wastewater discharged to the sewer?
3. Are wet air scrubbers used? Is wastewater discharged to the sewer? Is the wastewater treated prior to
discharge (e.g., sedimentation for paniculate matter)?
4. How are any backings applied (heat, adhesives, etc.)?
Fuel Oil Dealers
I. Record storage capacity (above ground and underground).
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POTW Inspection and Sampling Manual Appendix II
2. Are the above ground storage and the loading areas diked or bermed? Is there any leakage or spillage access
to storm or sanitary sewers?
3. Are any oils or fuels stored inside the building? Note the proximity of floor drains to these areas.
4. What types of absorbent is used for spills? How much is stored for immediate availability? Note the
proximity of the material to any floor drains
?. Does the facility have a spill prevention plan? Do employees receive spill plan training?
Funeral Services
\. Check what kind of chemicals are used and how they are stored. What is the storage proximity to the floor
drains?
2 Check how much formalin is used for embalming. What percentage of usage is discharged to the sewer?
Mow much blood is discharged per day? Are there any other chemicals involved in the embalming process?
3. Check the washing and cleaning procedures at the embalming table What kind of detergents and
disinfectants are used?
4. How are infectious wastes disposed?
Gasoline Service Stations
I. Check the location of any floor drains. Look for drains under service bays. What is the destination of the
drain0
2. Identify the location of any gas/oil interceptors or separators. What kind of unit is it and what is the general
operating condition of that unit?
3. Check what kind of chemicals are used and how they are stored. Chemicals might include fluids such as
oil, transmission and brake fluids, anti-freeze, or solvents. What is the proximity of the storage area to floor
drains'.'
4. Check the quantity and method of waste oil storage and the manner and location in which it is disposed.
Is there a waste oil recepticle (drum or tank)?
5 Check the disposal method used for radiator flushing.
Gum and Wood Chemicals Manufacturing
\. What volume of product is produced on a yearly basis?
2 If gum resin, turpentine, or pine oil are produced, what is the volume of process wastewater from stripping,
vacuum jet stream condensates, and unit washdown?
3 If tall oil resin, pitch, or fatty acids are produced, what is the volume of wastewater form the acid treatment
system, overflow from the evaporative cooling system, process washdowns and quality control lab wastes'.'
4. Check the general questions on Cooling Water.
5. If essential oils are produced, what is the volume of contaminated condensate that is discharged from the
batch extraction of oil of cedarwood?
6 If rosin derivatives are produced, what is the volume of wastewater from the water of reaction; sparge
stream, if used; and the vacuum jet stream?
Hospitals
\. Note the general layout of the facility (e.g., types of labs, equipment, morgue, laundry, food services, etc.).
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POTW Inspection and Sampling Manual Appendix II
2. C'heck what kind of chemicals are used and how they are stored. What is the storage proximity to the floor
(drains'?
3. Any special procedures used for handling infectious or hazardous wastes? Identify the mode of disposal and
names of any haulers of such wastes.
4 What are the types and quantities of cleaners and germicides utilized in cleaning procedures?
5 Disposal of spent photoprocessing chemicals (i.e., fixen) from X-ray departments?
5 See general questions on Radioactive Materials.
Inorganic Chemicals
\. What is the product that is manufactured at this facility?
2. Arc any brine muds generated by the facility's production or inorganic compounds? Do these brines contain
any known heavy metals? How are these brine muds disposed?
3. Does the facility generate any air scrubber wastewater? What is the chemical quality of this water and how
is it disposed?
4. Are any cyanide (CM) compounds generated by the facility? Are the CN wastestreams segregated and/or
pretreated prior to discharge?
5. Check the general questions under Cooling Waters.
6. Check the general questions under Solids Disposal.
Laundries
1. Is dry cleaning done? If so, what is the solvent used?
2. Is sludge generated? What is the disposal method?
3. If solvents are used, are they redistilled on-site? Does this process generate uncontaminated or contaminated
cooling water? Where is it discharged? What is the discharge volume?
4. Do washers have lint traps and settling pits?
5. What is the temperature of the effluent? Is a heat exchange system used?
6. Arc printers rags, shop rags, or other industrial materials cleaned?
7. What types of detergents and additives are used? What is the pH of the effluent? How are chemicals
added?
8. Are laundry trucks maintained and washed on-site? If so, how are the waste oils, etc. handled? Are there
any floor drains leading to the sewer in the vicinity of the vehicle wash or vehicle storage area?
9. Is there any loss of water as a result of evaporation? What is the estimated volume of the loss?
10. What is the water consumption at the facility? What is the source of the water used at the facility?
Leather Tanniny and Finishing
I. What method is used to preserve the received hides? (Note, hides preserved with salt will result in a high
dissolved solids count in the effluent).
2. What types of skins and/or hides are tanned? (Note, if sheepskins or goatskins are tanned, there will be a
separate solvent or detergent degreasing operation.)
3. Is hair saved or pulped (i.e., chemically dissolved)? (Note: in a save hair operation with food recovery of
hair, the contribution to the effluent strength is substantially lower that in pulp hair operations).
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POTW Inspection and Sampling Manual Appendix II
4. Is deliming accomplished by treating with mild acids or by bating? What is the destination of these waters?
5. What types of tannin are used? (Note: chrome and vegetable tannins are the most common. A combination
of tannins may also be used).
6. Are chemicals stored near floor drains? (This is a very appropriate question to ask since many liquid
chemicals are used in the leather tanning industry).
7. Are tannins recycled and/or chemically recovered? What happens to this wastewater?
8. Are any pretreatment units employed? What is the calibration of monitoring equipment?
9. If sludge is generated, how is it disposed?
10. Check the general questions under Cooling Waters.
Lumber and Building Materials: Retail
\. Check for the storage of paint, thinner, and other solvents, adhesives, roofing materials, etc.
2. Does the facility mix paint? Is the paint mixing dry or does it involve water? Check the nearby sinks for
evidence of water usage. How is the waste paint disposed?
3. Are cutting oils used and are they water soluble?
4. Are hydraulic oils used?
5. Would any of these oils ever be discharged to the sewer?
Machine and Sheet Metal Shops
1. What type of product is manufactured?
2. What kind of material is machined?
3. Are cutting oils used and are they water soluble?
4. Are hydraulic oils used?
5. Would any of these oils ever be discharged to the sewer0
6. Are any degreasing solvents or cleaners used? What are the chemical make up and/or brand names of the
degreasers and how are they used? How are the spent degreasing chemicals or sludge disposed? Is
degreasing rinse water discharged to the sewer?
7. Is there any water cooled equipment such as a vapor degreaser or air compressor? What is its discharge
frequency and volume?
8. Is any painting done on the premises? How are waste thinners or paints disposed? Is a water curtain used
for control of solvents entering the air and is contaminated water discharged?
9. Is any type of metal finishing done, such as anodizing, chromating, application of black oxide coating or
organic dye'1 What are the chemicals used, volumes consumed, and destinations of the finishing chemicals0
10. What is the water consumption at the facility?
11. Are there any pretreatment units, traps, etc.?
Meat Products/Poultry Products
I. What type of livestock are slaughtered and/or processed?
2. What are the principal processes employed?
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POTW Inspection and Sampling Manual Appendix II
3. What methods are used to dehair? Is the hair recovered from the wastewater stream?
4. Does the facility cure hides? What brine solution is used specifically (i.e., sodium chloride)? Are hides
cured in vats? Are vats ever discharged to the sewer? What is the frequency and volume of such
discharges0
5. What are the by-product processes?
6. Is rendering practiced at the plant? How (i.e., catch basins, grease traps, air flotation, etc.)? How often are
the systems cleaned out?
7. What methods are used for clean-up operations? What detergents are used (i.e., caustic, alkaline, etc.)?
8. Which wastestreams, if any (i.e., uncontaminated water) bypass all treatment and discharge directly to the
sewer?
9, If poultry processing is done, how are the feathers removed? How are they disposed? How are chicken
parts disposed? How is blood disposed?
Metal Heat Treating Shops
1. What kinds of metal are heat treated?
2. What fluids are used for quenching metals? Are these ever discharged to the sewer?
3. Are sludge ever removed from the quenching tanks? How are the sludge disposed?
4 Is any of the metal cleaned before or after heat treating? Are any degreasing solvents or cleaners used and
how are they used9
5. Are there any water cooled quenching baths, vapor degreasers, or other equipment? Where are they
discharged? What volumes are discharged?
6 What is the water consumption?
Metal Refineries and Foundries
1. What is the product that is manufactured at the facility?
2. Does the facility use any solvents or degreasing agents? Check the general questions under Solvents.
3 Does the facility use any cooling water? Check the general questions under Cooling Waters.
4. Is there any water recycle/reuse within the plant? Does the plant employ any pretreatment for the recycle
streams?
5. Does the facility have a spill prevention plan developed? Does the plan include spills to the sewer of highly
acidic or caustic materials?
6. Check the general questions under Solids Disposal.
Nursing Care Facilities
1 Food service (se Restaurant questions).
2. Any chemical usage (e.g., lab facility)?
3. Janitorial chemicals - usage, destination, and storage or germicides and disinfectants.
Organic Chemicals
1. Are processes batch or continuous?
2. If batch processes are used, how frequent is clean-up and how are wastes disposed0
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POTW Inspection and Sampling Manual Appendix II
3. Are waste disposal services or scavengers used? If so, are they licensed? Which wastes are hauled?
4. What types of solvents are stored in bulk?
5. Check the points for the discharge of cooling water. Check general questions under Cooling Waters.
6. Is there water in contact with catalysts used at the plant (e.g., in cleaning catalyst beds)?
7. List all products and raw materials.
8. Are there laboratories for research and for product testing? How are laboratory wastes disposed?
9. Is the water used in boiler feed or in processing pre-created? How are laboratory wastes disposed?
10. Are storage areas near drains leading to the sewer?
II. Are there any chemical reaction or purification techniques, such as crystallization, filtration, or
centrifugal ion, which produce wastewater and/or sludge wastes? What is the destination of these
wastestreams and/or sludge?
12. Are there any pretreatment units at the facility?
13. Is deionized water used, how is it generated (on-site)? Are columns regenerated on-site? Does the facility
use acids or caustics? Is there a discharge from the deionization process? Where does the discharge go?
14. Is a water tower used? What is the frequency and volume of the discharge? Where does the discharge go?
Are any additives such as chromates used by the facility?
Paint and Ink Formulation
\. What types of inks are made (i.e., oil-based or water-based)?
2. What types of paints are manufactured (i.e., water-based or solvent-based)?
3. What are the pigments made of?
4. Are extenders used?
5. Are any solvents used? Check the general questions under Solvents.
6. What are the resin types?
7. What other ingredients are used in formulating the product?
8. Is there any discharge to the sewer system (washdown and/or bad batches)? Are any chemicals used to
clean product equipment?
9. Are there any floor drains in chemical storage and mixing areas?
10. Is there a scavenger service? If yes, for which wastes?
II. Is there on-site disposal of solids by burial? If not, where do the solids go?
12. Check the general questions on Cooling Waters.
Paper Mills
I. What are the products manufactured at the plant?
2. Which specific chemicals are used in the process?
3. Is pulp bleached? If yes, what is the process and what chemical are used?
4. Are any chemicals manufactured on-site (e.g., chlorine dioxide, hypochlorites, etc.)? Are any chemicals
discharged from these operations?
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5. Are recovery streams (white water recycle, cooking liquor regeneration, cooling water reuse, etc.)?
6. Where is cooling water used in the plant (e.g., condensers, vacuum pumps, compressors)? Where is it
discharged?
7. Describe the types of fillers, coatings, finishes, etc., in paper making.
8. What happens to bad batches or liquids in case of equipment failure? Are they discharged to the sewer?
9. On the average, how much water is consumed in the process of making paper? What is the source of the
water?
Paving and Roofing
Tar and Asphalt
I. Does the wastewater from wet air scrubbers used on the oxidizing tower discharge directly to the sewer?
Is it treated and recycled?
2. What method(s) are used to control the temperature or the oxidizing tower (i.e., water)? Is this waste
discharged or recycled?
3. What treatment methods are used to remove suspended solids or oil from the water (i.e., catch basins, grease
traps, sedimentation, oil skimmers)?
4. Is water or air used to cool asphalt products? If water, is il contact or noncontact? If contact, is this water
discharged directly to the sewer or does it undergo treatment? (Note: mist spray used alone causes the
largest amount of solids present in wastewater.)
5. Check the general questions under Cooling Waters.
6. Are any solvents used? Check the general questions under Solvents.
Pesticides
\. Does the facility manufacture or blend pesticides at this location?
2. What pesticides are manufactured or formulated at the facility? What volumes of product is produced on
a yearly basis?
3. Check the chemical storage areas.
4. How arc chemical containers rinsed? Is the rinse water discharged to the sewer?
5. What is the volume of wa-tewater from the final synthesis reaction or the dilution water step used directly
in the process?
6. Check the procedures for floor and/or equipment washes.
7. Check the general questions under Solids Disposal.
Petroleum Refining
1. What are the processes employed by the facility and what is the throughput (in barrels per day) of each of
the following processes:
Topping: The term includes basic distillation processes;
Cracking: The term cracking includes hydrocracking, fluid catalytic cracking, and moving bed catalytic
cracking processes;
Petrochemical: This includes the production of second generation petrochemicals (i.e., alcohols, ketones,
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POTW Inspection and Sampling Manual Appendix II
cumene, styrene, etc.), first generation petrochemicals, and isomerization products (i.e., BTX, olefms,
cyclohexanes, etc.); and
Lube: This term includes hydrofining, white oi! manufacturing, propane dewaxing. solvent extractions
and dewaxing, naphtenic lubes, phenol extraction, SO, extraction, etc.
2. Identify the location of any oil interceptors or separators. What kind of unit is it and what is the general
operating condition of the unit?
3. Does the facility employ any biological treatment prior to discharging to the sewer9
4. Are there any controls in place for phenols, sulfides, hexavalent chromium, and/or ammonia? How does
the facility dispose of any spent caustic which it might generate?
5. Is storm water runoff isolated from the sewer discharge? How is the contaminated storm water runoff
disposed? Does the facility have a NPDES permit for stormwater?
6. Check the general questions for Cooling Waters.
7. Check the general questions for Sludge Disposal.
Pharmaceuticals Manufacturing
1. What type of processes are used to manufacture the product (e.g., fermentation, biological, or natural
extraction, chemical synthesis, mixing/compounding and formulation).
2. If processes include fermentation and/or chemical synthesis, are these continuous or batch discharge?
3. If chemical synthesis is involved, what processing steps (crystallization, distillation, filtration, centrifugal ion.
vacuum filtration, solvent extraction, etc.) produce wastewater? Are these wastewaters discharged to the
sewer system?
4. What types of solvents are used? Check the general questions on Solvents.
5. Is raw water intake purified? If yes, by what method (e.g., ion exchange, reverse osmosis, water softening,
etc.)0 What types and volumes of wastes are generated? What is the frequency of discharge?
6. What is done with the spent beer generated by fermentation?
7. Check the general questions on use of cleaners and location of drains.
8. Is there any chance of spills or batch discharges?
9. Check the usage of cooling waters. See general questions on Cooling Waters.
10. Is there a research lab in the plant? What are the wastes generated by the facility0 How are they
controlled?
Photographic Process
\. Determine what type of chemistry is used. This is important because some of the chemicals may be toxic
while others are not.
2. What types of films are developed? Are prints made? Give an estimate of how much total processing is
done per day. How may automatic processors are utilized and long are they in operation per day?
3. What chemical brands are used? What type of process chemistry is used: C-41, E-6, CP-30, etc.? What
are the names of each chemical used in the process? What are the volumes used? Which chemicals are
discharged to the sewer? Do any of the chemicals contain cyanide?
4. What is the square footage of the material being processed?
5. Is silver recover, practiced? Is bleach regeneration practiced, and if yes, is it done within the lab? What
are the processes and wastes involved? Does the silver recover)' system have a maintenance schedule?
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POTW Inspection and Sampling Manual Appendix II
6. What is the wastewater flow from each of the photographic processing operations? Does the rinse water
on the processors run continuously or does it shut off when film is not being processed? How often are the
processors cleaned and the chemicals changed? How often, if ever, are these chemicals discharged to the
sewer? What chemicals, if any, are used to clean the processor rollers and trays? Are there any floor drains
where the chemicals are mixed or stored?
7. Is there any type of pretreatment or pH control?
8. What is the frequency of silver recovery maintenance?
9. What is the water consumption of the facility?
Plastic and Synthetic Materials Manufacturing
I. What is the product that is being manufactured?
2. What are the raw materials used, including any accelerators and inhibitors? Are there any known toxics
(such as cyanide, cadmium, or mercury) utilized in manufacturing the product?
3. What type of polymerization process is employed? Does the process use a water or solvent suspension?
What are the wastes generated from the process? What are the possible contaminants0 How are the wastes
disposed?
4. Are there any product washing operations? Are reactor vessels washed down between batches? Is water
or a solvent used? Would these wastes be discharged to the sewer?
5. Check the usage of cooling water. Check the general questions on Cooling Waters.
Porcelain Enameling
\. What is the square footage of material enameled at the facility on annual basis?
2. How is the base metal prepared for enameling?
3. Is any electroplating done on-site? If yes, check the general questions on Electroplating and Metal Finishing.
4. What coating application method is used?
5. Check the general questions under Usage of Chemicals, Cleaners and Location of Drains
Some of the following questions may apply and others may not; experience will be the best judge. The SIC
number for offset and silkscreen printing is 2732 and letterpress is 2751. other types of printing are listed in the
27XX group.
1. Note the kind of printing done (i.e., offset, letterpress, silkscreen, or other types of printing).
2. If offset printing is done, is film processing and plate developing done in the shop?
3. If film processing is done, is an automatic film processor used or are trays used? Does the processor's rinse
water run continuously or does it shut off after processing is completed? How often are the processor's
chemical tanks cleaned out and what volume is discharged to the sewer? How much developer, fixer, and
stop batch (if applicable) are used and are these discharged to the sewer? Is silver reclamation practiced?
Is cyanide used at all for further reducing of negatives? Are phototypositors used, and if yes, what
chemicals are discharged?
4. If plate development is done, what type of plates are used? If they are aluminum plates, are they developed
with a subtractive color key additive developer? What are the names of the developers, and what quantities
are used? Is the developed washed off the plates to the sewer or wiped off with a rag0 Where do the rags
go? How may plates are developed?
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POTW Inspection and Sampling Manual Appendix II
5. If paper plates are used, what Jypt of processor is employed and what are the names, volumes, and
destination of the chemicals used? If a silver process is used, is silver reclamation practiced?
6. In the press room, what type of fountain solution is used and would this ever be discharged during normal
use or cleanup operation? What type of solvent is used to clean the presser and how is this applied? Would
this solvent ever be discharged or does it become associated with the rags? Are these rags washed on the
premises or are they picked up by a commercial laundry? What is the name of the laundry? Are there any
floor drains where the solvent or ink is stored? Are any of the presser waters cooled? Are there any waste
oils from the presser?
7. If letter press printing is done, is old lead type smelted in the shop, and if yes, are the molds water cooled0
What type of solvent is used to clean the presser and type? Check the general questions on Solvents
8. Is silkscreen printing done? What kind of photosensitive coating is used and what volume of coating is
used? What kind of developer is used and is it discharged? Is a solvent or other cleaner used to clean the
screen after printing? Check the general questions for Solvents. Are the screens used over again for making
new stencils or are they thrown away?
9 If a different type of printing is done, what kind is it and what are the names and volumes of the chemicals
used? Are these discharged to the sewer? Are the screens used over again for making new stencils or are
they thrown away?
10. Check the general questions under Cooling Waters.
Rubber Processing
Synthetic or Natural
1. What are the products manufactured at the facility?
2. Is the rubber natural or synthetic? If synthetic rubber is used, is it polymerized on-site and would it he a
water or solvent suspension? Is there a discharge associated with the process?
3. What are the ingredients of the rubber, including all additives? What kind of anti-tack agents are used'.'
Are any known toxics used at the plant?
4. Are there any waste oils from rubber mixers or other processes which required disposal, and if \es, how are
they disposed0
5. What type of forming process is used? Is cooling water used? Check the general questions on Cooling
Waters.
6. Is there any wastewater associated with the curing process (e.g., steam condensate) and what would the
contaminants be in the water?
7. Is rubber reclaimed, and if yes, what types of processes are used? Are any chemical agents used and how
are spent agents disposed?
8. Are any final coatings applied to the rubber, paint, plastics, etc.? Are there any wastes or wastewater
associated with the process and how are they be disposed?
9. Does the plant have air pollution control equipment? Does it use water as a scrubbing medium and is this
discharged?
10. Check the general questions under Cooling Waters.
Schools and Universities
General
1. Cafeteria (see Restaurant questions).
2. Janitorial chemicals (usage, destination and storage).
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POTW Inspection and Sampling Manual Appendix II
Junior High and High Schools
1. Labs (chemical usage and disposal).
2. Art department (note any agents disposed to the sewer and their amounts - e.g., paint thinners).
3. Wood'metal shop (refer to questions under Woodworking Shops.
Universities
1. Is a map of the campus available to inspectors?
2. Can a master list of chemicals used on campus be provided? Which chemicals are used most?
3. Is there an organized waste chemicals pickup program? How many pickups per year? How many gallons
picked up per year? Are there any central storage locations?
4. Are radioactive materials handled on campus? If yes, in what capacity? Are any wastes generated which
are discharged to the sewer?
5. Any photo developing facilities on campus? Any printing facilities?
6. Any prototype PC board work in the electronics labs on campus?
7. How are pathogenic organisms disposed?
8. Any pretreatment facilities?
9. Has study been done to account for all water uses at the university (e.g., cooling water, lab wastes, cooling
tower and boiler blowdowns, etc.)? What is the total campus population, including support staff?
10. Are there any floor drains near liquid chemical storage areas?
Scrap and Waste Materials
1. Is there any processing of the material (e.g., welding or smelting)?
2. Check the general questions under Cooling Waters.
3. Describe oil storage, including capacity. Is there a potential for discharge to the sewer?
4. Is there any other liquid storage or reclamation?
Soap and Detergent Manufacturing
General
1. Are only soaps manufactured, detergents, or both? Classify the plant.
2. Is there any cooling water used? Refer to the general questions under Cooling Waters.
3. How are the liquid materials stored? Are there floor drains nearby leading to the sewer?
4. Are air scrubbers used? Is water used? Caustics?
5. In product purification steps, how are filter backwashes handled?
Soap
1. What is the basic process employed for manufacturing soap (e.g., batch kettles)? What amount for fatty acid
neutralization? Other?
2. Is process batch or continuous? If batch, what is the frequency and volume of reactor cleanout?
3. Is waste soap from processing sewered?
4. Are defoamers added prior to sewer discharge?
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POTW Inspection and Sampling Manual Appendix II
5. Are perfumes and additives used? If so, what are they?
Detergent
1. What are the additives used in the product?
2. How are the spray drying towers cleaned?
Steam Supply and Noncontact Cooling
Steam Supply
1. Is the system high or low pressure steam?
2. Check the general questions under Boiler Discharges.
3. Is major cleaning and maintenance done? How often?
4. Are ion exchange systems used for boiler feed water? If yes, whal types of wastes are generated0
Noncontact Cooling Water
1. Are cooling towers used? If yes, what are the chemical additives?
2. How frequently are towers blown down? Where does the blowdown go?
3. Are closed system ever by-passed? Under what circumstances?
Sugar Processing
1. Are both liquid and crystalline sugar produced?
2. What type of system exists for "sweet water" recovery?
3. Are ion exchange systems used? If yes, what are the backwashing systems likely to produce as wastes?
How frequent is the backwash?
4 Are trucks or other heavy equipment maintained? Washed? Any floor drains leading to sewers? Any traps?
5. What bulk chemicals are stored and how? (Examples are acids used in liquid sugar production).
6. What happens to filter sludges in the plant? What type of filter aids are used?
7. Is cooling water used? Refer to the general questions on Cooling Waters.
8. From the cleaning of the equipment, what wastes are sewered and what wastes are recycled through the plant
(e.g., filters, evaporation plans screens, etc.)
Textile Mills
I. What are the products manufactured at the mill? What is the approximate production of the mill?
2. What types of fibers are used in the fabric?
3 Does the raw fiber require cleaning before spinning and weaving?
4. Are the fibers or fabrics scored, mercerized, fulled, carbonized or bleached? What chemicals and rinsing
operations are used and what is the destination of these wastes?
5. Is any kind of sizing applied, and if yes, what kind is it?
6. Is desizing practiced and what are the chemicals used? Are these chemicals discharged to the sewer?
7. Is dye applied to fabrics? What are the types and chemical constituents of the dyes and are the spent dye
solutions and rinse waters discharged to the sewer?
8. Are any antistatic agents applied to synthetic fibers before spinning and weaving operations? Would these
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POTW Inspection and Sampling Manual Appendix II
be removed from the fabric and subsequently enter the wastewater discharged to the sewer?
9. Are any further finishing operations practices such as printing or application or various coatings?
10. What is the volume of wastewater generated by each chemical process?
11. Are there any methods of pretreatment employed before discharge of wastewater to the sewer?
12. Check the general questions for Cooling Waters.
13. Any liquids stored near floor drains leading to the sewer?
Veterinary Services
I. Check on chemical (including alcohol, germicides, pesticides, cleaners, and medicines) usage and storage.
Refer to the general questions under Usage of Chemicals, Cleaners.a nd Location of Floor Drains.
2. Are detergents used and discharged for animal washing baths? Are there any hair clogging problems?
3. What is done with excreta material for any animals boarded?
4. Are there any special procedures taken for infectious wastes?
Woodworking Shops
1. Check chemical usage at the facility (e.g., look for solvents, thinners, paints, stains, cutting oils, adhesives,
etc.). Check the general questions under Solvents.
2. Check the general questions under Usage of Chemicals, Cleaners, and Location of Drains.
3. How are brushes cleaned? Are any spray guns used? If yes, how are they cleaned?
4. Are cutting oils discharged?
5. Is any cooling water used? Check the general questions under Cooling Waters.
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Appendix III
General Operations and Maintenance Questions
-------
Operations and Maintenance Questions for Industrial Users
Policies and Procedures:
General Questions:
Yes No N'A I. Is there a formal or informal set of policies for facility operations?
2. Do policies address any of the following:
Yes No N/A • Remaining in compliance?
Yes No N.'A • Maintaining process controls?
Yes No N/A • Quality control?
Yes No N/A • Preventative maintenance?
Yes No N'A 3. Is there a set of standard procedures to implements these policies?
Yes No N'A 4. Are the procedures written or informal?
5. Do the procedures consider the following areas?
Yes No N'A • Safety?
Yes No N'A • Emergency?
Yes No N'A • Laboratory?
Yes No N-'A • Process control?
Yes No N/A • Operating procedrues?
Yes No N'A • Monitoring?
Yes No N'A • Labor relations?
Yes No N/A • Energy conservation?
Yes No N/A • Collection system?
Yes No N'A • Pumping stations?
Yes No N/A • Treatment processes?
Yes No N/A • Sludge disposal?
Yes No N/A • Equipment record system?
Yes No N/A • Maintenance planning and scheduling?
Yes No N/A • Work orders?
Yes No N A • Inventory management?
Yes No N/A 6 Are the procedures followed?
Organization:
Yes No N/A 1. Is there an Organizational Plan (or Chart) for operations?
2. Does the plan include:
Yes No N/A • Delegation of responsibility and authority?
Yes No N/A • Job descriptions?
Yes No N/A • Interaction with other functions (such as maintenance)?
Yes No N/A 3. Is the Plan formal or informal?
Yes No N/A 4. Is the Plan available to and understood by the staff?
Yes No N/A 5. Is the Plan followed?
Yes No N/A 6. Is the Plan consistent with policies and procedures?
Yes No N/A 7. Is the Plan flexible (i.e., can it handle emergency situations)?
8. Does the Plan clearly define lines of authority and responsibility in such areas as
Yes No N/A • Laboratory?
Yes No N/A • Process control?
Yes No N/A • Instrumentation?
Yes No N A • Sludge disposal?
Yes No N/A • Collection system?
Yes No N/A • Pumping stations?
Yes No N'A • Monitoring practices?
Yes No N/A • Mechanical"7
III - 1
-------
POTW Inspection and Sampling Manual Appendix 111
Yes No N/A • Electrical?
Yes No N/A • Buildings and grounds?
Yes No N/A • Automotive?
Yes No N/A • Supplies and spare parts?
Staffing:
Yes No N/A 1 Is there an adequate number of staff to achieve the policies and procedures established in the
plan?
Yes No N/A 2. Are staff members adequately qualified for their duties and responsibilities by demonstrating:
Yes No N/A • Certification?
Yes No N/A • Qualification?
Yes No N/A • Ability?
Yes No N/A • Job performance?
Yes No N'A • Understanding of treatment processes?
Yes No N'A 3. Is staff effectively used?
Yes No N'A 4. Has the potential for borrowing personnel been considered?
5. Are training programs followed for:
Yes No N'A • Orientation of new staff?
Yes No N/A • Training new operators?
Yes No N/A • Training new supervisors?
Yes No N'A • Continuing training of existing staff?
Yes No N'A • Cross training?
6. Which of the following training procedures are used?
Yes No N/A • Formal classroom?
Yes No N/A • Home study?
Yes No N'A • On-the-job training?
Yes No N'A • Participation in professional conferences or organizations?
Yes No N'A 7. Does the training program provide specific instruction for the following operations and
maintenance activities?
Yes No N/A • Safety?
Yes No N'A • Laboratory procedures?
Yes No N'A • Treatment processes?
Yes No N A • Instrumentation?
Yes No N'A • Equipment troubleshooting?
Yes No N'A • Handling personnel problems?
Yes No N'A • Monitoring practices?
Yes No N'A • Handling emergencies?
Yes No N'A • Mechanical?
Yes No N A • Electrical?
Yes No N/A • Automotive?
Yes No N'A • Building maintenance?
Yes No N'A • Inventory control?
Yes No N'A 8. Does management encourage staff motivation?
Yes No N/A 9, Does management support its first-line supervisors?
10. Is staff motivation maintained with:
Yes No N'A • Encouragement for training?
Yes No N''A • Job recognition?
Yes No N'A • Promotional opportunities?
Yes No N'A • Salary incentives?
Yes No N'A • Job security?
Yes No N/A • Working environment?
Ill - 2
-------
POTW Inspection and Sampling Manual
Appendix HI
Operations:
Yes
Yes
Yes
Yes
Yes
Yes
Yes
Yes
Yes
Yes
Yes
Yes
Yes
Yes
Yes
Yes
No
No
No
No
No
No
No
No
No
No
No
No
No
No
No
No
N
N
N
N
N
N
N
N.
N,
N.
N.
N.
N.
N.
N.
N.
A
;A
;A
'A
A
A
A
A
A
A
A
A
A
A
A
A
1.
2
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
14.
15.
16.
Maintenance:
Yes
Yes
Yes
Yes
Yes
Yes
Yes
Yes
Yes
Yes
Yes
Yes
Yes
Yes
Yes
Yes
Yes
Yes
No
No
No
No
No
No
No
No
No
No
No
No
No
No
No
No
No
No
N.
N'
N'
N
N
N'
N/
N
N'
N.'-
N/
N/
N-'
N/
N/
N/
N-
N/
A
A
A
A
A
A
A
A
A
A
A
A
A
A
A
A
A
A
1.
2
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
14.
15.
16.
17.
18.
Management Cont
Yes
Yes
Yes
Yes
No
No
No
No
N'
N/
N'
N'
A
A
A
A
1.
How are operating schedules established?
Do schedules attempt to attain optimum staff use?
Are line supervisors inculded in manpower scheduling?
Are staff involed in and/or informed of manpower planning?
Is there sufficient long-term planning for staff replacement and system changes'*
Are there procedures in manpower staffing for emergency situations?
7. How are process control changes initiated?
8. How do process control changes interct with managment?
9. How effectively are laboratory results used in process control?
10. Are there emergency plans for treatment control?
Is there an effective energy management plan? Is the plan used?
To what extent are operations personnel involved in the budget process?
Do budgets adequately identify and justify the cost components of operations?
Are future budgets based on current and anticipated operating conditions?
Do operating and capital budget limits constrain operations0
16. Can budget line items be adjusted to reflect actual operating conditions?
Are maintenance activities planned? Is the planning formal or informal0
Does the facility have sufficient management controls to affect realistic planning and
scheduling? If the controls exist, are they used?
Are operating variables exploited to simplify maintenance efforts?
To what extent are the supply and spare parts inventories planned in conjunction with
maintenance activities?
Have minimum and maximum levels been established for all inventory items?
Does the facility have a maintenance emergency plan?
1st he maintenance emergency plan current? Is the staff knowledgable about emergency
procedures?
Does a plan exist for returning to the preventative maintenance mode following an
emergency?
Are preventative maintenance tasks scheduled in accordance with manufacturer's
recommendations?
Is adequate time allowed for corrective maintenance?
Are basic maintenance practices (preventative and corrective) and frequencies reviewed for
cost-effectiveness?
Do the management controls provide sufficient information for accurate budget preparation?
To what extent are maintenance personnel involved in the budget process?
Do budgets adequately identify and justify the cost components of maintenance?
Are future budgets based on current and anticipated operation and maintenance conditions0
Do maintenance and capital budget limits constrain preventative maintenance (equipment
replacement and improvement)?
Does the maintenance department receive adequate feedback on cost performance?
Can budget line items be adjsuted to reflect actual maintenance conditions?
Are current versions of the following documents maintained:
• Operating reports?
• Work schedules?
• Activity reports?
• Performance reports (labor, supplies, energy)?
- 3
-------
POTW Inspection and Sampling Manual Appendix III
Yes No N'A • Expenditure reports (labor, supplies, energy)?
Yes No N'A • Cost analysis reports?
Yes No N A • Emergency and complaint calls?
Yes No N A • Process control data, including effluent quality?
Yes No N A 2 Do the reports contain sufficient information to support their intended purpose?
Yes No N A 3. Are the reports usable and accepted by the staff?
Yes No N A 4. Are the reports being completed as required?
Yes No N A 5 Are the reports consistent among themselves?
Yes No N A 6. Are the reports used directly in process control?
Yes No N A 7. Are the reports reviewed and discussed with operating staff?
Yes No N A 8. What t>pes of summart reports are required?
Yes No N A 9. Io whom are reports distributed and when?
Management Controls (Maintenance):
I Does a maintenance record system exist? Does it include:
Yes No N A • As-built drawings'.'
Yes No N A • Shop drawings?
Yes No N A • Construction specifications?
Yes No N A • Capital and equipment inventory0
Yes No N A • Maintenance history (preventative and corrective)?
Yes No N A • Maintenance costs'1
Yes No N'A 2. Is the base record system kept current as part of daily maintenance practices?
Yes No N A 3. Is there a work order system for scheduling maintenance? Is it explict or implicit?
4. Do work orders contain the following:
Yes No N'A • Date0
Yes No N A • Work order number?
Yes No N'A • Location0
Yes No N A • Nature of the problem?
Yes No N A • Work requirements0
Yes No N'A • Time requirements?
Yes No N A • Assigned personnel?
Yes No N A • Space for reporting work performed, required supplies, time required, and cost summary0
Yes No N A • Responsible staff member and supervisory signature requirements?
Yes No N A 5. When emergency work must be performed without a work order, in one completed afterward?
Yes No N A 6 Are work orders usable and acceptable by staff as essential to the maintenance program? Are
they actually completed?
Yes No N A 7 Is work order information transferred to a maintenance record system?
Yes No N A 8 Does a catalog or index system exist for controlling items in inventory?
Yes No N A 9. Are withdrawal tickets used for obtaining supplies from the inventory?
Yes No N A 10 Do the tickets contain cost information and interact well with inventory controls and the work
order system'.'
Yes No N A II Is the cosl and activity information from work orders aggregated to provide management
reports'.'
Yes No N A 12. Is this information used for budget preparation?
Yes No N A 13. Is the maintenance performance discussed regularly with staff?
Yes No N A 14. How is the cost of contract maintenance or the use of specialized assistance recorded?
Yes No N A 15. Are safeguards and penalties adequate to prevent maintenance cards from being returned
without the work being done?
Yes No N A 16. Is the pre\entati\e maintenance record checked after an emergency equipment failure0
III - 4
-------
Appendix IV
Hazards Associated with Specific
Industrial Categories
-------
Hazards Associated With Specific Industrial Categories
Industry
Electroplating
Metal Finishing
Chemical
Blending
Manufacturing
Semiconductor
Manufacturing
Kilp. Paper and
Paperhoard
Manufacturing
Battery
Manufacturing
Physical
Cluttered areas
Sloppy housekeeping
Wet floors'loose hoards
Healed plating baths
High amperage in plating
baths
Slipper, floors
• Slippery floors
• Steam heated tanks
• Moving equipment (fork
lifts)
. Heat from steam curing
of pasted plates
• Spills of washwaier
• Exposure to lead metal
particles during anode
production
Atmospheric
• Flammable vapors
« Exposure to chlorine
• Sulfur dioxide vapors
• Cyanide vapors
• Alkaline vapors mist
• Acid vapor/mist
• Leaking mixing or
blending equipment
Exposure to freon and
chlorinated solvents
Exposure to:
- Ammonia I pulping
process)
- Chlorine (bleaching
process)
Arsenic fumes
Corrosive
• Corrosive chemicals
used in plating
pn>cess
• Heavy metal baths
• High voltage
« Exposure to
chemicals due to
leaking equipments
• Exposure to acids
{hydrofluoric and
fluoroboncl
• Exposure to caustic
soda I pulping
process)
Suggested
Protective Gear
• Safety glasses
• Neoprene gloves
• Boots
• organic vapor/gas mask
• Ear plugs
• Safety glasses
« l-alcx gloves
• Dust and mist mask
• Boots
Exposure to sulfunc
acid vapors.
Lead fumes
Acid vapors
• Exposure to sulfunc
acid I pickling and
bleaching process)
• Safety glasses
• Boots
• l~atex gloves
• l^ad fume mask
• Organic vaporgas
mask
I.c.ithei Tanning
Iron and Steel
Manufacturing
• Slippery floors
• Moving equipment in
wringing operation
• Hot ovens
. Hot baths
. Particulates
• Moving equipment
. Slippery floors
Industrial
1 jundnes
Aluminum
Formers
• Healed equipment
• Slippery floors
• Moving machinery
• Exposure to:
- sulfunnc acid
- chromium
• cyanide
- napthalene
- phenol
- pentachlorphenol
• Exposure to toxic
vapors from hot baths
• Exposure to toxic
vapors from solvents
• Metal particulars
• Exposure to vulture
and hydrochloric
acids (acid pickling)
« Nitric acid
• Caustic solutions
Electrical and • Wet floors
Semiconductors • Loose hoards
• Acid vapors'mist.s
« Ammonia vapors
• Alkaline vapors
• • Metal fumes
• Freon chlorinated
solvents
• Borane gas
• Chlorinates
« Aromatic solvents
• Hydroflounc acid
• Fluoroboric acid
• Safety glasses
. Bts
• l.atcx gloves
• Metal fume mask
• Organic vapor mask
• Safety glasses
• Boots
• l.atex gloves
• l.ead fume mask
« Organic vapor mask
-------
Metal Molding
and Casting
Nonferrous
Metals
Organic
Chemicals
Soap and
Detergent
Welding
• Tripping hazards
• Hot liquid metals
• Tapping hazards
• Bum danger from hot
metals
Tripping hazards
Pharmaceutical • Tripping hazards
Slippery floors
Electric shock
Bums
Radiant energy/light.
Metal paroculates
Degreasing solvents
Cyanide gas
• Organic vapors/mists
• Phenols
• Ammonia
formaldehyde
• Chlorine
• Hypochlonte solvents
• Plastic monomers
• Radioactiviie materials
• Biological materials
Detergent dust
Exposure to toxic
fumes
Potential for explosions
caused by sparks.
• Cyanide liquid
Monomers
Acidic or alkaline
solutions
High pH
Slippery oils
• Safely glasses
• Boots
• Latex gloves
• Hard hat
• Metal fume mask
• Safety glasses
• Boots
• Latex gloves
• Hard hat
• Organic vapor/gas
mask
• Safety glasses
• Boots
• Rubber gloves
• Organic vapor/gas
mask
• Safety glasses
. Boots
• Ear protection
• Latex gloves
• Dust mask
• Safety glasses
• Boots
• Latex gloves
• Paniculate mask
-------
Appendix V
EPA's Policy on Grab Samples vs.
Composite Samples
-------
UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
WASHINGTON, D.C. 20460
XT I 1992
X»MOP»NDUM
WATfM
SUBJECT:
FROM:
The Use of Grab Samples to Detect Violations of
Pretreatment Standards
Michael B. Cook, Direct
Office of Wastewater En
Frederick F. Stiehl
Enforcement Counsel
br Water (LE-134W)
TO:
ance (WH-546)
- X
Water Management Division Directors, Regions I
Environmental Services
Division Directors, Regions I - X
Regional Counsels, Regions I - X
The primary purpose of this Memorandum is to provide
guidance on the propriety of using single grab samples for
periodic compliance monitoring to determine whether a violation
of Pretreatment Standards has occurred. More specifically, the
Memorandum identifies those circumstances when single grab
results may be used by Control Authorities, including EPA, State
or publicly owned treatment works (POTW) personnel, to determine
or verify an industrial user's compliance with categorical
standards and local limits. Please be aware that the concepts
set out below are applicable when drafting self-monitoring
requirements for industrial user permits.
REGULATORY BACKGROUND
The General Pretreatment Regulations require Control
Authorities to sample all significant industrial users (SIUs) at
least once per year [see 40 CFR 403.8(f)(2)(v)]. In addition,
the Regulations, at 40 CFR 403.12(e), (g) and (h) require, at a
minimum, that all SIUs self-monitor and report on their
compliance status for each pollutant regulated by a Pretreatment
Standard at least twice per year unless the Control Authority
chooses to conduct alj. monitoring in lieu of self-monitoring by
its industrial users.
1 The POTW should conduct more frequent sampling and/or
require more frequent self-monitoring by an industrial user if
deemed necessary to assess the industry's compliance status (e.g.,
a daily, weekly, monthly or quarterly frequency as appropriate).
-------
- 2 -
The Regulations, at 40 CFR 403.12(g) and (h), also specify
that pollutant sampling and analysis be performed using the
procedures set forth in 40 CFR Part 136. Part 136 identifies the
proper laboratory procedures to be used in analyzing industrial
vastevater (including the volume of wastevater necessary to
perform the tests and proper techniques to preserve the sample's
integrity). However, with certain exceptions, Part 136 does not
specifically designate the method to be used in obtaining samples
of the wastewater. Rather, section 403.12(g) and (h) require
sampling to be "appropriate" to obtain "representative" data;
that is, data which represent the nature and character of the
discharge.
DISCUSSION 07 BASIC SAMPLIMO TYPES
Sampling may be conducted in two basic ways. Both types of
sampling provide valid, useful information about the processes
and pollutants in the wastewater being sampled. The first is an
"individual grab sample." An analysis of an individual grab
sample provides a measurement of pollutant concentrations in the
wastewater at a particular point in time. For example, a single
grab sample might be used for a batch discharge which only occurs
for a brief period (e.g., an hour or less). Such samples are
typically collected manually but are sometimes obtained using a
mechanical sampler.
The second type of sample is a "composite sample."
Composite samples are best conceptualized as a series of grab
samples which, taken together, measure the quality of the
wastewater over a specified period of time (e.g., an operating
day). Monitoring data may be composited on either a flow or time
basis. A flow-proportional composite is collected after the
passage of a defined volume of the discharge (e.g., once every
2,000 gallons). Alternatively, a flow-proportional composite may
be obtained by adjusting the size of the aliquots to correspond
to the size of the flow. A time-proportional composite is
collected after the passage of a defined period of time (e.g.,
once every two hours).
Generally, composite samples are collected using a
mechanical sampler, but may also be obtained through a series of
manual grab samples taken at intervals which correspond to the
wastewater flow or time of the facility's operations. In some
cases, composite data is obtained by combining grab samples prior
Mechanical samplers may not be used to sample for certain
pollutants (e.g., those which could adhere to the sampler tubing,
volatilize in the sampler, or pollutants with short holding tiroes).
-------
to transmittal to a laboratory. At other tines, the samples
remain discrete and are either combined by the laboratory prior
to testing or are analyzed separately (and mathematically
averaged to derive a daily maximum value).
DETERMINING APPROPRIATE COMPLIANCE SAMPLING METHODS
EPA policy on appropriate compliance sampling types has been
articulated in several pretreatment guidance manuals and
regulatory preambles, and continues to be as follows:
A. Compliance with C»tegoric»i St*n^*rrts
• Most effluent limits established by categorical standards
are imposed on a maximum daily-average and a monthly-average
bases. Generally, vastewater samples taken to determine
compliance with these limits should be collected using
composite methods.
There are exceptions to the general rule. Composite
samples are inappropriate for .certain characteristic
pollutants (i.e., pH and temperature) since the composite
alters the characteristic being measured. Therefore,
analysis of these pollutants should be based on individual
grab samples. Alternatively, continuous monitoring devices
may be used for measuring compliance with pH and temperature
limits. Any exceedance recorded by a continuous monitoring
device is a violation of the standard.
Sampling wastewater from electroplating facilities
regulated under 40 CFR Part 413 may be conducted using
single grab samples [(assuming that the grab samples are
representative of the daily discharge for a particular
facility); see also preamble discussion at 44 Fed. Reg.
52609, September 7, 1979]
A series of grab samples may be needed to obtain
appropriate composite data for some parameters due to the
nature of the pollutant being sampled. Examples of this
situation include:
Daily maximum discharge limits are controls on the average
wastewater strength over the course of the operating day. They are
not intended to be instantaneous limits applied at any single point
during that operating day.
-------
- 4 -
Sampling for parameters which nay be altered in
concentration by compositing or storage. These
pollutants include pH-sensitive compounds (i.e., total
phenols, ammonia, cyanides, sulfides); and volatile
organics such as purgeable halocarbons, purgeable
aromatics, acrolein, and acrylonitrile.
Sampling for pollutants with short holding tines such
as hexavalent chromium and residual chlorine; and
Sampling for pollutants which may adhere to the sample
container or tubing such as fats, oil and grease.
Individual analysis for these parameters ensures that
all the material in the sample is accounted for.
B. Compliance with T-T.C*! Limits
Local limits may be established on an instantaneous,
daily, weekly or monthly-average basis. The sample type
used to determine compliance with local limits should be
linked to the duration of the pollutant limit being applied.
Compliance with instantaneous limits should be
established using individual grab samples. Exceedances
identified by composite sampling are also violations.
Compliance with daily, weekly or monthly average
limits should be determined using composited sampling
data, with the same exceptions noted in A, above.
Measurements of wastewater strength for non-
pretreatment purposes (e.g., surcharging) may be
conducted in a manner prescribed by the POTW.
GRAB SAMPLING AS A SUBSTITUTE FOR COMPOSITE SAMPLING
EPA is aware that a number of Control Authorities currently
rely on a single grab sample to determine compliance,
particularly at small industrial users, as a way of holding down
monitoring costs. It is EPA's experience that the process
activities and wastewater treatment at many industrial facilities
may not be sufficiently steady-state as to allow for routine use
4 Certain pH-sensitive compounds can be automatically
composited without losses if the collected sample is only to be
analyzed for a sinale oarameter. Additionally, a series of grab
samples may be manually composited if appropriate procedures are
followed.
-------
- 5 -
of single grab results as a substitute for composite results.
Therefore, the Agency expects composited data to be used in most
cases. However, there are several circumstances when a single
grab sample may be properly substituted for a single composite
sample. These situations are:
Sampling a batch or other similar short term discharge,
the duration of which only allows for a single grab
sample to be taken;
Sampling a facility where a statistical relationship
can be established from previous grab and composite
monitoring data obtained over the same long-term period
of time; and
Where the industrial user, in its self-monitoring
report, certifies that the individual grab sample is
representative of its daily operation.
Except for these circumstances, Control Authorities should
continue to use composite methods for their compliance sampling.
GRAB SAMPLES AS A COMPLIANCE SCREENING TOOL
Control Authorities may consider using grab samples as a
compliance screening tool once a body of composite data (e.g.,
Control Authority and self-monitoring samples obtained over a
year's time), shows consistent compliance. However, in the event
single grab samples suggest noncompliance, the Control Authority
Grab sampling may provide results that are similar to
composite sampling. See for example, a March 2, 1989, Office of
Water Regulations and Standards (OWRS) Memorandum to Region IX
describing the results of a statistical analysis of sampling data
from a single industrial facility. These sampling data included
both individual grab and flow-proportional, composite sampling
obtained during different, non-overlapping time periods. After
reviewing the data, OWRS concluded that the composite and grab
sample data sets displayed similar patterns of violation for lead,
copper, and total metals. In fact, the analyses did not find any
statistically significant difference in the concentration values
measured between the grab and composited data. Furthermore,
additional statistical tests of the two data sets indicated that
the means and variances for each pollutant were similar. The
statistical conclusion was that the plant was judged to be out of
compliance regardless of what data were analyzed.
-------
- 6 -
and/or the industrial user should resample using composite
techniques on the industrial users effluent until consistent
compliance is again demonstrated.
Control Authorities may also rely on single grab samples, or
a series of grab samples for identifying and tracking slug
loads/spills since these "single event" violations are not tied
to a discharger's performance over time.
Any time an SIU's sample (either grab or composite) shows
noncomplianca, the General Pretreatment Regulations, at 40 CFR
403.12(g)(2), require that the SIU notify the Control Authority
within twenty four (24) hours of becoming aware of the violation
and resample within 30 days. Furthermore, EPA encourages Control
Authorities to conduct or require more intensive sampling in
order to thoroughly document the extent of the violation(s). Of
course, the use of grab samples should be reconsidered in the
event the SIU changes its process or treatment.
fUXXARY
The collection and analysis of sampling data is the
foundation of EPA's compliance and enforcement programs. In
order for these programs to be successful, wastewater samples
must be properly collected, preserved and analyzed. Although the
Federal standards and self-monitoring requirements are
independently enforceable, Control Authorities should specify, in
individual control mechanisms for industrial users, the sampling
collection techniques to be used by the industry. Generally,
pretreatment sampling should be conducted using composite methods
wherever possible, to determine compliance with daily, weekly or
monthly average limits since this sampling technique most closely
reflects the average quality of the wastewater as it is
discharged to the publicly owned treatment works. Grab samples
should be used to determine compliance with instantaneous
limits. There are circumstances when discrete grab samples are
also an appropriate, cost effective means of screening compliance
with daily, weekly and monthly pretreatment standards.
6 Where grab samples are used as a screening tool only (i.e.,
consistent compliance has been demonstrated by composite data), the
results should not be used in the POTW's calculation of significant
noncompliance (SNC).
7 When POTWs choose to allow the SIU to collect single grab
samples, the POTW should draft the SIU's individual control
mechanism to clearly indicate that grab samples are to be obtained
thereby preventing any uncertainty at a later date.
-------
- 7 -
In summary, there are limited situations in which single
grab sample data may be used in lieu of composite data. Assuming
adequate quality control measures are observed, analyses of these
grab samples can indicate noncompliance with Federal, State and
Local Pretreatment Standards and can form the basis of a
successful enforcement action. Grab sampling can also be useful
in quantifying batches, spills, and slug loads which may have an
impact on the publicly owned treatment works, its receiving
stream and sludge quality.
Should you have any further comments or questions regarding
this matter, please have your staff contact Mark Charles of OWEC
at (202) 260-8319, or David Hindin of OE at (202) 260-8547.
cc: Frank M. Covington, NEIC
Thomas O'Farrell, OST
Regional and State Pretreatment Coordinators
Lead Regional Pretreatment Attorneys, Regions I - X
Approved POTW Pretreatment Programs
-------
Appendix VI
Flow Measurement Techniques
-------
Flow Measurement Techniques and Inspection
Procedures:
Basic Hydraulic Calculations
The relationship between flow rate (Q), the average velocity (V). and the cross-sectional area of the flow
(A) is given by the following equation:
0 ^ VA
where: Q - flow in cubic feet per second
V = the velocity in feet per second
A = the cross-sectional area in square feet
To convert flow in cubic feet of water per second to flow in gallons of water per minute, the following
proportionality is used:
cubic feet x 7.48 gallons water x 60 seconds . gallons
second cubic foot of water minute minute
To convert from cubic feet per second to million gallons per day, mulitply the number of cubic feet per second
by 0.6463. The cross-sectional area of the pipe is described by the equation: A 1 4 n d:, where d is the
diameter of the pipe in feet.
Flow Measurement Devices
Flow data may be collected instantaneously or continuously. Instantaneous flows must be measured when
samples are taken so that the pollutant concentration can be correlated to the flow data. In a continuous flow
measurement system, flow measurements are summed to obtain a value for the total flow to verify IU permit
compliance.
A typical flow measurement system consists of a flow device, a flow sensor, transmitting equipment, a
recorder, and a totalizer. Instantaneous flow data can be obtained without using such a system. The primary flow
device is constructed to yield predictable hydraulic responses related to the rate of wastewater or water flowing
through the device. As previously mentioned, examples of such devices include weirs and flumes, which relate
water depth (head) to flow, Venturi meters, which relate differential pressure to flow; and electromagnetic flow
meters, which relate induced electric voltage to flow. In most cases, a standard primary flow device has
undergone detailed testing and experimentation and its accuracy has been verified.
Flow is measured by many methods; some are designed to measure open channel flows, and others are
designed to measure flows in pipelines. A complete discussion of all available flow measurement methods, their
supporting theories, and the devices used are beyond the scope of this manual. The most commonly used flow
measurement devices and procedures for inspecting them are described in this Appendix.
VI - 1
-------
POTW Inspection and Sampling Manual Appendix VI
Primary Devices:
Weirs. A weir consists of a thin vertical plate with a sharp crest that is place in a stream, channel, or
partly tilled pipe. Figure 3-4 (in Chapter 3) shows a profile of a sharp-crested weir and indicates the appropriate
nomenclature. Four common types of sharp-crested weirs are shown in Figure 3-5. This figure illustrates the
difference vetween suppressed and contracted rectangular weirs as well as illustrates Cipoletti (trapezoidal) and
V-notch (triangular) weirs.
To determine the flow rate, it is necessry to measure the hydraulic head (height) of water above the crest
of the weir For accurate flow measurements, the crest must be clean, sharp, and level. The edge of the crest
must not he thicker than 18 inch. The rate of flow over the weir is directly related to the height of the water
(head) above the crest at a point upstream of the weir where the water surface is level. To calculate the discharge
over a weir, the head must first be measured by placing a measuring device upstream of the weir, at a distance
or at least 4 times an approximate measurement of the head. A measurement can be taken at the weir plate to
approximate the head. However, if this measurement is used to calculate the discharge, this value will provide
onl\ a rough estimate of the discharge. Therefore, when evaluating compliance with mass-based permit limits,
it is essential that a more refined method of determining flow be used.
I"he head-discharge relationship formulas for nonsubmerged contracted and suppressed rectangular weirs,
Cipolletti weirs, and 90° V-notch weirs are provided in Table Vl-l. Discharge rates for the 90-degree V-notch
weir (when the head is measured at the weir plate) are included in Table VI-2. Flow rates for 60- and 90-degree
V-notch weirs can be determined from the nomograph in Figure VI-1. Minimum and maximum recommended
flow rates for Cipolletti weirs are provided in Table VI-3. Figure VI-2 is a nomograph for flow rates for
rectangular weirs using the Francis formulas.
Parshall Flume: The Parshall Flume is composed of three sections: a converging upstream section, a
throat or contracted section, and a diverging or dropping downstream section. When there is free fall out of the
throat of a Parshall Hume, no diverging downstream section is required. It operates on the principle that when
open channel water Hows through a constriction in the channel, it produces a hydraulic head that is proportional
to the flow. The hydraulic head is used to calculate the flow. Flow curves are shown in Figure VI-3 to determine
free flow through 3 inches to 50 feet Parshall flumes.
Hie Parshall flume is good for measuring open channel flow because it is self-cleaning. Therefore, sand
or suspended solids are unlikely to effect the operation of the device. The flume is both simple and accurate.
The flume si/e is given by the width of the throat section. Parshall flumes have been developed with throat
widths from I inch to 50 feet. The configuration and standard nomenclature for Parshall flumes is provided in
Figure 3-6 Strict adherence to all dimensions is necessary to achieve accurate flow measurements. Figure VI-4
VI - 2
-------
Table VI-1
Head-Discharge Relationship Formulas for Nonsubmerged Weirs'
(Taken from NPDES Compliance Inspection Manual, EPA, May 1988)
Weir Type
Rectangular
Francis
formulas
Contracted
Q - 3.33 {L - 0.1nH)Hl.S
Suppressed
Q = 3.33 L Hi-5
Remarks
Reference
Approach velocity King
neglected 1963
Q • 3.33 [(H + h)1.5-hl-5](L - U.lnH) Q = 3.33 L[(H + h)l.$ - hi.5] Approach velocity King
considered 1963
Cipolletti Q - 3.36? L Hi-5
Q - 3.367 L (H + h)1.5 - hi.5
V-notch
Formula for .Q » 2.50 H?-^
90* V-notch
only
Q- 3.01 H 2.48
0 • discharge in cubic feet per second
H = head in feet
NA = not applicable
H^ * head in feet at weir plate
n - number of end contractions
NA
NA
NA
NA
Approach velocity King
neglected 1963
Approach velocity EPA
considered 19/3
Not appreciably Kiig
affected by 191 3
approach velocity
Head measured at EM and
weir plate Peterson 19/9
L ' crest length in feet
h = head in feet due to the approach velocity
V * approach velocity
g * gravity (32.2 ft/sec?)
•Selection of a formula depends 0*1 its suitability and parameters under consideration.
VI-3
-------
Table VI-2
Discharge of 90* V-Notch Weir - Head Measured at Weir Plate
(Taken fron: NPDES Compliance Inspection Manual, EPA, May 1988)
Head@
Weir
in
Feet
0.06
0.07
0.08
0.09
0.10
0.11
0.12
0.13
0.14
0.15
0.16
0.17
0.18
0.19
0.2U
0.21
0.22
0.23
0.24
0.25
0.26
0.27
0.28
0.29
0.30
0.31
0.32
0.33
0.34
0.35
0.36
0.37
0.38
0.39
0.40
0.41
0.42
0.43
0.44
0.45
FLOW
RATE
in
CFS
0.003
0.004
0.006
0.008
0.010
0.013
0.016
0.019
0.023
0.027
0.032
0.037
0.043
0.049
0.056
0.063
0.070
0.079
0.087
0.097
0.107
0.117
0.128
0.140
0.152
0.165
0.178
0.193
0.207
0.223
0.239
0.256
0.273
0.291
0.310
0.330
0.350
0.371
0.393
0.415
HEADP
WEIR
in
FEET
0.46
0.47
0.48
0.49
0.50
0.51
0.52
0.53
0.55
0.55
0.56
0.57
0.58
0.59
0.60
0.61
0.62
0.63
0.64
0.65
0.66
0.67
0.68
0.69
0.70
0.71
0.72
0.73
0.74
0.75
0.76
0.77
0.78
0.79
0.80
0.81
0.82
0.83
0.84
0.85
FLOW
RATE
in
CFS
0.439
0.463
0.488
0.513
0.540
0.567
0.595
0.623
0.653
0.683
0.715
0.747
0.780
0.813
0.848
0.883
0.920
0.957
0.995
1.034
1.074
1.115
1.157
1.199
1.243
1.287
1.333
1.379
1.426
1.475
1.524
1.574
1.625
1.678
1.730
1.785
1.840
1.896
1.953
2.012
HEAD?
WEIR
in
FEET
0.86
0.87
0.88
0.89
0.90
0.91
0.92
0.93
0.94
0.95
0.96
0.97
0.98
0.00
1.00
1.01
1.02
1.03
1.04
1.05
1.06
1.07
1.08
1.09
1.10
1.11
1.12
1.13
1.14
1.15
1.16
1.17
1.18
1.19
1.20
1.21
1.22
1.23
1.24
1.25
FLOW
RATE
i n
CFS
2.071
2.140
2.192
2.2i>5
2.318
2.382
2.448
2.514
2.582
2.650
2.720
2.791
2.863
2.936
3.010
3.085
3.162
3.239
3.317
3.397
3.478
3.556
3.643
3.727
3.813
3.889
3.987
4.U76
4.166
4.2S7
4.349
4.443
4.538
4.634
4.731
4.829
4.929
5.030
5.132
5.235
EQUATION Q - 3.01 Hw'«4° where Hw is nead is in feet at the weir and 0 is
cubic feet per second
\l - -t
-------
24
20
18
16
14
12
10
y
8
7
6
3-
4-
«
3-
•
t-
•
-7000
J -600O
•WOO
-4000
m
•3000
i
t
r2000
•
:
*f
r 1000
^800
-800
m
m
»4OO
? J300 <
K ^
" E**V : ><
"S K!^ • v
"I /^ ^I0° r
:* 1 E"
. uj • •
< _ * .
;l
f*0
R
1
r»
r8
f-8
•
»4
»
•1
r4000 ,24
r3900 :
i .
' • 2C
i-2000 r
f r '•
\ *
* *
rKJOO I H
^BOO :
r ^,j
- 800
» r
-400 r»
• ^
— L~TO r*
k *
* ' DO ^*
^ ^80 :
& r 2 "8
• * 3 •
«:«0 ,-4
W '
I -30 o -
. « „
» -20 -3
: 5
i *'.
rIO
it
r "2
f«
7
- 4
• •
»3
i »
rt
J
rL3
• I
Figure VI-1
Flow Rates for 60* and 90* V-Notch Weirs
(Taken from NPDES Compliant* Inspection Manual, EPA, May 1988)
vi-5
-------
H
ta
If
O
9?
3 "•
n
I*
2 »
?.«
^^ **
i G0
-"?
m <;
r^ ^™"* XZ) j^D ^ CC
X "^i v% ^v
O O • • «/•
-» -* <»
^6 OJ OJ ^3 ^A
3 o « • —•
O. O CO CO ^ O
3 CO CO O 3
O r» *
o T --> i— «* -n
3 fit I— I •• I
r» O I CO a*
-> e* o -^ 3
o> «» • ro n
o a. ro -»•
o «t
3 -»
1 >^-» —•
—• cs> -»
X ^
-^ I C -%
r» -O O
7 OT9 T
•^^ i
?s *
SD
oo
00
r\>
z i— o
HUM
I
3* -«i — -«i Q.
o. «-» ua «-» o
T3 (b
(» T
IV CO)
f^ ^ O "J"
r» -*• O 3
-> 3
» o. o
c
r>
3
b
K 9
5 O
<•
0
00090^0 o o
LENGTH OF NEIR, L. IN FEET
p
8
2
GALLONS PER MINUTE TO BE SUBTRACTED FROM FLOW FOR CONTRACTED HE|R
WITH TMD END CONTRACTIONS = (0.66 H5/2) (450)
^^°?5 "--S8885i§
UI_
HEAD IN INCHES
DISCHARGE. IN GALLONS PER MINUTE
8 $ 38S8
«K
o
g § s §§g§si
2
S S SSSS5
g
rt
DISCHARGE. Q. IN CUBIC FEET PER SECOND
-------
Table VI-3
Minimum and Maximum Recommended Flow Rates for Cipolletti Weirs
(Taken from NPDES Compliance Inspection Manual, EPA, May 1988)
Crest Minimum Maximum
Length, Minimum Flow Rate Maximum Flow Rate
ft. Head, ft. MGO CFS Head, ft. MGD CFS
1
1.5
2
2.5
3
4
5
6 0.2 1.17 1.81 3.0 67.8 105.0
8 0.2 1.56 2.41 4.0 139.0 214.0
10 0.2 1.95 3.01 5.0 243.0 375.0
0.2
0.2
0.2
0.2
0.2
0.2
0.2
0.195
0.292
0.389
0.487
0.584
0.778
0.973
0.301
0.452
0.6U2
0.753
0.903
1.20
1.51
0.5
0.75
1.0
1.25
1.5
2.0
2.5
0.769
2.12
4.35
7.60
12.0
24.6
43.0
1.19
3.28
6.73
11.8
18.6
38.1
66.5
Table VI-4
Minimum and Maximum Flow Rates for Free Flow Through Parshall Flumes
(Taken from NPDES Compliance Inspection Manual, EPA, May 1988)
Throat
Width,
W
1
2
3
6
9
1
1-1/2
2
3
4
5
6
8
10
12
in.
in.
in.
in.
in.
ft.
ft.
ft.
ft.
ft.
ft.
ft.
ft.
ft.
ft.
Minimum
Head, Ha
ft.
0.07
0.07
0.10
0.10
0.10
0.10
0.10
0.15
0.15
0.20
0.20
0.25
0.25
0.30
0.33
Minimum
Flow
MGO
0.003
0.007
0.018
0.035
0.059
0.078
0.112
0.273
0.397
0.816
1.00
1.70
2.23
3.71
5.13
Rate
CFS
0.005
0.011
0.028
0.054
0.091
0.120
0.174
0.423
0.615
1.26
1.55
2.63
3.45
5.74
7.93
Maximum
Head, Ha
ft.
0.60
0.60
1.5
1.5
2.0
2.5
2.5
2.5
2.5
2.5
2.5
2.5
2.5
3.5
4.5
Maximum
Flow
MGO
0.099
0.198
1.20
2.53
5.73
10.4
15.9
21.4
32.6
43.9
55.3
66.9
90.1
189
335
Rate
CFS
0.153
0.306
1.86
3.91
8.87
16.1
24.6
33.1
50.4
67.9
85.6
103
139
292
519
VI- 7
-------
JOOO .
2000 f
C'i
4 OOO
1.000.000 :
•00.000 -
•OOAOO -
soo.ooo -
«00.000 -
JOO.OOO -
200.000 (-
100.000 -
•o.ooo -
•O.OOO -
so.ooo -
4O.OOO -
30.000 -
20.000 -
IO.OOO -
•ooo -
»ooo p-
iOOO -
«ooo -
JOOO -
2OOO -
5»M
'OOO ^
•OO p
«oo r
»oo -
400 -
JOO -
200 K
K)0
to
•0
»o
40
JO
20
iO -
Figure VI-3
Flow Curves for Parshall Flumes
(Taken from NPDES Compliance Inspection Manual, EPA, May 1988)
v;. a
-------
VI -9
ft . I*. f t . In. rt
a 4 i 7 i
0*2 n 1
1 t 4 » 1
2 • 1 fl 1
•Cquoli 1 cu (1 p. i
IB. ft. IB rt . IB
T I .07
.» , . . .1
4n 2 • 1 Jy
24 7j 2 <
4 4 l»j 1 •
toe
ft IB. rt . IB ft. IB. ft. IB rt. In IB IB rt IB. ft
J 4f> 020 10 00 ) 1 }« 5
J llj J 030 JO 00 ) 1 If *
In ft !• in IB
j T
* i a 2 )
1 I I 2 J
f r«*-f low
C«B«city
( S*c Mid-root •)
HiBi-
0
0
e
0.
o
e
0
i
i
i
i
}
.•)
•1
•»
11
.IS
41
.«!
1
t
i
.0
J
*•»»-
BtiB:
1
I
1
It
14
>J
SO
*7
It
101
121
1 J»
.»
.»
.»
.1
.«
.1
4
.»
t
.1
.4
)
LOBO:
V
A
1*
B
C
D
E
T
Width of fluK throat.
Lo«jth of side wall of cowerfinf section.
Distance bade trtm end of crest to we point.
Axial length of convctpng section.
Width of dounstraa* end of fluv.
Width of upstream end of fline.
Depth of UUK.
L*tf th of tlt*t thrat.
G Axial Length of diverging section.
H Length of side wll of the diverting section.
K Difference in elevation between lower end of OUK and crest.
N Length of «w
-------
POTW Inspection and Sampling Manual Appendix VI
provides Parshal) flume dimensions for various throat widths and Table VI-4 provides the minimum and
maximum flow rates for free flow through Parshall flumes.
For free, nonsubmerged flow in a Parshall flume of throat and upstream head (H. in feet), the discharge
relationship for flumes of 8 feet or less is given by the general equation: Q = CWH,", where Q = flow. Table
VI-5 provides the values of C, n, and Q for different sizes (widths) of the Parshall flumes. Nomographs, curves,
or tables are readily available to determine the discharge from head observations. Flow through a Parshall flume
may also be submerged. The degree of submergence is indicated by the ratio of the downstream head to the
upstream head (Hh'H,) which is the submergence ratio. Hb is the height of water measured above the crest. The
flow is submerged if the submerged ratio is:
• Greater than 0.5 for flumes under 3 inches;
Greater than 0.6 for flumes 6 to 9 inches;
Greater than 0.7 for flumes 1 to 8 feet; and
Greater than 08 for flumes larger than 8 feet.
If submerged conditions exist, the inspector should apply a correction factor to the free flow determined using
the relationship Q CWH". These correction factors are shown in Figure VI-5 for different sizes of the Parshall
flume.
Palmer-Bowlus Flume. The Palmer-Bowlus flume is also composed of three sections: a converging
upstream section, a contracted section or throat, and a diverging downstream section (see Figure 3-7). The
upstream depth of the water (head) 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 the manufacturer's data are consulted, since it is difficult to manually
measure the height of water above the step at an upstream point. The dimensions for Palmer-Bowlus flumes are
not standardized as they are for Parshall flumes. Therefore, no standard flow equation exists. Instead, rating
curves are provided by the manufacturers of these flumes to relate the head to the discharge rate.
The flume must be installed with a minimum channel slope downstream to maintain critical flow through
the flume and prevent the flume from becoming submerged. A small jump or rise in the water surface below the
throat indicates that critical flow through the flume has probably occurred and submerged conditions exist.
Accurate flow measurements can usually be obtained with upstream depths that are up to 95 percent of the pipe
diameter Table VI-6 provides a table of the maximum slopes recommended for installation of Palmer-Bowlus
flumes The advantages of this type of flow measurements device are: easy installation, insignificant head loss,
and self-cleaning.
VI - 10
-------
Table VI-5
Free Flow Values of C and N for Parshall Flume
Based on the Relationship Q = CWHan
(Taken from NPDFS Compliance Inspection Manual, EPA, May 1988)
Flume Throat, W
1
2
3
6
9
1
1.5
2
3
4
5
6
7
8
1n
1n
1n
1n
1n
ft
ft
ft
ft
ft
ft
ft
ft
ft
0.338
0.676
0.992
2.06
3.07
4 W *
1.55
1.55
1.55
1.58
1.53
1.52:
Max. Q cfs
0.15
0.30
1.8
3.9
8.9
16.1
24.6
33.1
50.4
67.9
85,
103,
121,
139.5
Where:
W • Flume throat width
Q « Flow (cfs)
C - Constant
H • Head upsteam of the flume throat (feet)
n « Constant
* « W should be represented 1n feet to calculate C
VI- 11
-------
100
*» Width of flume
90
•o
SUBMERGENCE,
• 0 90
, IN PERCENT
100
Figure VI-5
Effect of Submergence on Parshall Flume Free-Discharge
(Taken from NPDES Compliance Inspection Manual, EPA, May 1988)
VI - 12
-------
Table VI-6
Minimum and Maximum Recommended Flow Rates for Free Flow
Through Plast-Fab Palmer-Bowlus Flumes
(Taken from NPDES Compliance Inspection Fvianuai, EF/», Ma/ 1SSS)
D Maximum Slope
Flume for
Size, Upstream,
(1n.) Percent
6 2.2
8 2.0
10 1.8
12 1.6
15 1.5
18 1.4
21 1.4
24 1.3
27 1.3
30 1.3
Minimum
Head
(ft.)
0.11
0.15
0.18
0.22
0.27
0.33
0.38
0.44
0.49
0.55
M1 nimum
Flow
MGD
0.023
0.048
0.079
0.128
0.216
0.355
0.504
0.721
0.945
1.26
Rate
CFS
0.035
0.074
0.122
0.198
0.334
0.549
0.780
1.12
1.46
1.95
Maximum
Head
(ft.)
0.36
0.49
0.61
0.73
0.91
1.09
1.28
1.46
1.64
1.82
Maximum
Flow
MGD
0.203
0.433
0.752
1.18
2.06
3.24
4.81
6.70
8.95
11.6
Rate
CFS
0.315
0.670
1.16
1.83
3.18
5.01
7.44
10.4
13.8
18.0
VI - 13
-------
POTW Inspection and Sampling Manual Appendix VI
Venturi Meter. The Venturi (differential pressure) meter is one of the most accurate primary devices for
measuring flow rates in pipes The Venturi meter is basically a pipe segment consisting of an inlet section, a
converging section, a throat, and a diverging outlet section as illustrated in Figure 3-8. The water velocity is
increased in the constricted portion of the inlet section resulling in a decrease in the static pressure. The pressure
difference between the inlet pipe and the throat is proportional to the square of the flow. The pressure difference
can easily be measured with great accuracy, resulting in an accurate flow measurement. One of the advantages
of the Venturi meter is that it causes insignificant head loss.
The formula for calculating the flow in a Venturi meter is as follows:
Q - cKd:: Vh - h:
Where: Q = volume of water, in cubic feet per second
c ; discharge coefficient, obtain from Table VI-5
h1 pressure head at center of pipe at inlet section, in feet of water
h: pressure head at throat, in feet of water
K - constant which relates d, to d, for Venturi meters. Values for K can be
obtained from Table VI-8 or calculate according to the following formula:
Where: d; - throat diameter, in feet
d, - diameter of inlet pipe, in feet
Electromagnetic Flowmeter The electromagnetic flowmeter operates according to Faraday's Law of
Induction the voltage induced by a conductor moving at right angles through a magnetic field will be proportional
to the velocity of the conductor through the field. In the electromagnetic flowmeter, the conductor is the liquid
stream to he measured and the field is produced by a set of electromagnetic coils. A typical electromagnetic
flowmeter is shown in Figure 3-9. The induced voltage is transmitted to a converter for signal conditioning. The
meter may be provided with recorder and totalizer using electric or pneumatic transmission systems. This type
of flowmeter is useful at sewage lift stations and for measuring raw wastewater flow or raw or recirculated sludge
How.
Electromagnetic flowmeters are used in full pipes and have many advantages, including: accuracies of
±1 percent, a wide flow measurement range, a negligible pressure loss, no moving parts, and rapid response time.
However, the> are expensive and buildup of grease deposits or pitting by abrasive wastewaters can cause errors.
Regular checking and cleaning of the electrodes is necessary. The meter electronics can be checked for proper
operation with devices especially made for this purpose. The meter should be checked at least annually. The
calibration of an electromagnetic flow meter can not be verified except by returning it to the factory or be the
VI - 14
-------
Table V!-7
Coefficients of Discharge c for Venturi Meters
(Taken from NPDES Compliance Inspection Manual, EPA, May 1988)
Throat ve'iocivy, ft. per sec
Diameter of
Throat, 1n. 3 4 5 10 15 20 30 40 50
1 0.935 0.945 0.949 0.958 0.963 0.966 0.969 0.970 0.972
2 0.939 0.948 0.953 0.965 0.970 0.973 0.974 0.975 0.977
4 0.943 0.952 0.957 0.970 0.975 0.977 0.978 0.979 0.980
8 0.948 0.957 0.962 0.974 0.978 0.980 0.981 0.982 0.983
12 0.955 0.962 0.967 0.978 0.981 0.982 0.983 0.984 0.985
18 0.963 0.969 0.973 0.981 0.983 0.984 0.985 0.986 0.986
48 0.970 0.977 0.980 0.984 0.985 0.986 0.987 0.988 0.988
Table VI-8
Values of K in Formula for Venturi Meters
(Taken from NPDFS Compliance Inspection Manual, EPA, May 1988)
d2
0.20
0.21
0.22
0.23
0.24
0.25
0.26
0.27
0.2fi
0.29
0.30
0.31
0.32
6.31
6.31
6.31
6.31
6.31
6.31
6.31
6.32
6.32
6.32
6.33
6.33
6.33
0.33
0.34
0.35
0.36
0.37
0.38
0.39
0.40
0.41
0.42
0.43
0.44
0.45
6.34
6.34
6.35
6.35
6.36
6.37
6.37
6.38
6.39
6.40
6.41
6.42
6.43
0.46
0.47
0.48
0.49
0.50
0.51
0.52
0.53
0.54
0.55
0.56
0.57
0.58
6.45
6.46
6.47
6.49
6.51
6.52
6.54
6.54
6.59
6.61
6.64
6.66
6.69
0.59
0.60
0.61
0.62
0.63
0.64
0.65
0.66
0.67
0.68
0.69
0.70
0.71
6.72
6.75
6.79
6.82
6.86
6.91
6.95
7.00
7.05
7.11
7.17
7.23
7.30
0.72
0.73
0.74
0.75
0.76
0.77
0.78
0.79
0.80
0.81
0.82
0.83
0.84
7.37
7.45
7.53
7.62
7.72
7.82
7.94
8.06
8.20
8.35
8.51
8.69
8.89
VI - IS
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Table VI-9
Advantages and Disadvantages of Secondary Devices
(Taken from NPDES Compliance Inspection Manual, EPA, May 1988)
Device
Hook gauge
Stage board
Pressure measurement
a. Pressure bulb
b. Bubbler tube
Float
Dipper
Ultrasonic
Advantages
Common
Common
Since no compressed air
1s used, source can be
linked directly to
sampler
Self-cleaning, less
expensive, reliable
Inexpensive, reliable
Quite reliable, easy
to operate
No electrical or
mechanical contact
Disadvantages
Require training to
use, easily damaged
Needs regular
cleaning, di fflcult to
read top of meniscus
Open-Ings can clog,
expensive
Needs compressed air
or other air source
Catches debris,
requires frequent
cleaning to prevent
sticking and changing
bouyancy, and corroding
hinges
011 and grease foul
probe causing possible
sensor loss
Errors from heavy
turbulence and foam,
calibration procedure
1s more Involved
than for other devices
vi. 17
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POTW Inspection and Sampling Manual Appendix VI
dye dilution method. Secondary devices are the devices in the flow measurement system that translate the
interaction of primary devices in contact with the fluid into desired records or readouts. They can be organized
into two types:
Nonrecording type with direct readout (e.g., a staff gauge) or indirect readout from fixed points
(e.g., a chain, wire weight, or float); and
Recording type with either digital or graphic recorders (e.g., float in well, float in flow, bubbler,
electrical, and acoustic).
The advantages and disadvantages of various secondary devices are provided in Table VI-9.
Flow Measurement System Evaluation
The current strategy for assessing compliance by industrial users in the Pretreatment Program depends
heavily on the Ill's submittal of self-monitoring data. When the POTW inspector is on-site, he or she should
evaluate the lU's flow measurement system and techniques if there are any effluent limitations (local limits or
categorical standards) which are mass-based. The flow measured during the compliance inspection should verify
the flow data submitted by the IU as part of its periodic report to the POTW, support any enforcement action that
may be necessary, and provide a basis for reissuing or revising the ILJ's permit.
The POTW inspector must check both the lU's flow data and the flow measurement system to verify the
lU's compliance with mass-based categorical standards or local limits. When evaluating the flow measurement
system, the POTW inspector should consider and record his or her findings on the following:
• Whether the system measures the entire discharge flow.
• The system's accuracy and good working order. This will include a thorough physical inspection of
the system and comparison of the system's readings to those obtained with calibrated portable
instruments.
• The need for new system equipment.
• The existence or absence of a routine calibration and maintenance program for flow measurement
equipment.
If the lU's flow measurement system is accurate to within ±10 percent, the inspector is encouraged to use
the installed system. If the flow sensor or recorder is found to be inaccurate, the inspector should determine
whether the equipment can be corrected in time for use during the inspection. If the equipment cannot be repaired
in a timely manner, the portable flow sensor and recorder used to assess the accuracy of the ILTs system should
be used for the duration of the inspection. If nonstandard primary flow devices are being used by the IU, the IU
should provide data on the accuracy and precision of the method being employed.
For flow measurement in pipelines, the inpsector may use a portable flowmeter. The inspector should
select a flowmeter with an operating range wide enough to cover the anticipated flow to be measured. The
VI - 17
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selected flowmeter should be tested and calibrated before use. The inspector should select the site for flow
measurement according to the permit requirements and install the selected flowmeter per the manufacturer's
specifications. The inspector should use the proper tables, charts, and formulas as specified by the manufacturer
to calculate the flow rate.
Four basic steps are involved in evaluating the lU's flow measurement system.
• Physical inspection of the primary device;
• Physical inspection of the secondary device and ancillary equipment;
• Flow measurement using the primary/secondary device combination of the IU; and
• Certification of the system using a calibrated, portable instrument.
In the following section, procedures are presented for inspecting the more common types of primary and
secondary devices, for measuring flow using common permanent and portable systems, and for evaluating flow
data. It must be emphasized that the number of primary/secondary device permutations is limitless. Therefore,
it is not feasible to provide procedures for all system configurations, when system other than those discussed are
encountered, the inspector is strongly encouraged to consult the manufacturers for advice before preparing a
written inspection procedure.
Primary Device Inspection Procedures
The two most common open channel primary devices are sharp-crested weirs and Parshall Flumes.
Common sources of error when using these devices include:
• Faulty Fabrication - The weirs may be too narrow or not "sharp" enough. Flume surfaces may be
rough or critical dimensions may exceed tolerances or throat walls may not be vertical.
• Improper Installation - The weirs and flumes may be installed to near pipe elbows, valves, or other
sources of turbulence. The devices may also be out of level or out of plumb.
• Sizing Errors - The primary device's recommended applications may not include the actual flow range.
• Poor Maintenance - The primary devices corrode and deteriorate and debris or solids may accumulate.
Sharp-Crested Weir Inspection Procedures
• Inspect the upstream approach to the weir
- Verify that the weir is perpendicular to the flow direction.
- Verify that the approach is a straight section of conduit with a length at least 20 times the
maximum expected head of liquid above the weir crest.
- Observe the flow pattern in the approach channel. The flow should occur in smooth stream
lines without the velocity gradients and turbulence.
- Check the approach, particularly in the vicinty of the weir, for acculated solids, debris, or oil
and grease. The approach musl not have any accumulated matter.
• Inspect the weir
- Verify thai the crest of the weir is level across the entire conduit traverse.
- Measure the width of the weir crest. The edge of the weir crest should be no more than 1/8-
inch thick.
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POTW Inspection and Sampling Manual Appendix VI
- Make certain the weir crest corresponds to zero gauge elevation (zero output on the secondary
device).
- Measure the angle formed by the top of the crest and the upstream face of the weir. This
angle must be 90 degrees.
- Measure the chamfer on the downstream side of the crest The chamfer should be
approximately 45 degrees
- Visually survey the weir-bulkhead connection for evidence of leaks or cracks which permit
by-pass.
- Measure the height of the weir crests above the channel floor. The height should be at least
twice the maximum expected head of liquid above the crest.
- Inspect the weir for evidence of corrosion, scale formation, or clinging matter. The weir must
be clean and smooth.
- Observe flow patterns on the downstream side of the weir. Check for the existence of an air
gap (ventilation) immedialley adjacent to the downstream face of the weir. Ventilation is
necessary to prevent a vacuum that can induce errors in head measurements. Also ensure that
the crest is higher than the maximum downstream level of water in the conduit.
- Verify that the nappe (see Figure 3-4) is not submerged and that it springs free of the weir
plate.
- If the weir contains a V-notch, measure the apex angle. The apex should range from 22.5
degrees to 90 degrees. Verify that the head is between 0.2 and 2.0 feet. The weir should not
be operated with a head of less than 0.2 feet since the nappe may not spring clear of the crest.
Parshall Flume Inspection Procedures
• Inspect the flume approach.
- The flow pattern should be smooth with straight stream lines, be free of turbulence, and have
a uniform velocity across the channel.
- The upstream channel should be free of accumulated matter.
• Inspect the flume
• The flume should be located in a straight section of the conduit.
- Flow at the entrance should be free of "white" water.
- The flume should be level in the transverse and translational directions.
- Measure the dimensions of the flume. Dimensions are strictly prescribed as a function of
throat width (see Figure 3-6 for critical dimensions).
- Measure the head of liquid in the flume and compare with the acceptable ranges in Figure 3-6.
• Inspect the flume discharge
- Verify that the head of water in the discharge is not restricting flow through the flume. The
existence of a "standing wave" is good evidence of free flow and verifies that there is no
submergence present.
- Verify whether submergence occurs at or near maximum flow.
Paltner-Bowlus Flume Inspection Procedures
• Inspect the flume approach as outlined above (these flumes are seldom used for effluent flow
measurement).
• Inspect the flume.
- The flume should be located in a straight section of the conduit.
- The flow at the entrance should be free of any "white water."
- Observe the flow in the flume. The profile should approximate that depicted in Figure 3-7.
- The flume should be level in the transverse direction and should not exceed the translational
VI - 19
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POTW Inspection and Sampling Manual Appendix VI
slope in Table VI-1 at the end of the Appendix.
- Measure the head of water in the flume. The head should be within the ranges specified in
Table VI-1.
• Inspect the flume discharge
- Verify that free flow exists. Look for the characteristic "standing wave" in the divergent
section of the flume.
Venturi Meter Inspection Procedures
• Verify that the Venturi Meter is installed according to the manufacturer's specifications.
• Verify that the Venturi Meter is installed downstream from a straight and uniform section of pipe.a
t least 5 to 20 diameters, depending on the ratio of pipe to throat diameter and whether straightening
vanes are installed upstream. (Installation of straightening vanes upstream will reduce the upstream
piping requirements).
• Verify that the pressure measuring taps are not plugged.
• Calibrate the Venturi Meter in place by either the volumetric method or the comparative dye dilution
method to check the manufacturer's calibration curve or to develop a new calibration curve
Secondary Device Inspection Procedures
Common sources of error in the use of secondary devices are:
• Improper Location - The gauge is located in the wrong posilion relalive to the primary device.
• Inadequate Maintenance - The gauge is not serviced regularly.
• Incorrect Zero Settings - The zero setting of the gauge is not the zero point of the primary device.
• Operator Frror - There is human error in the reading.
Specific inspection procedures follow.
Flow Measurement in Weir Applications
• Determine that the head measurement device is positioned 3 to 4 head lengths upstream of the weir.
• Verify that the zero or other point of the gauge is equal to that of the primary device.
The inspector should use an independent method of measuring head, such as with a yardstick or carpenter's rule
(be sure to measure at least 4 (-!„„ upstream and convert to the nearest hundredth of a foot). To determine flow
rate, use the appropriate head discharge relationship formula (see Table VI-2).
Flow Measurement in Parshall Flume Applications
Flow Measurement - Free-Flow Conditions
• Determine the upstream head (H,) using a staff gauge.
- Verify the staff gauge is set to zero head. A yardstick or carpenter's rule can be used for this
- Verify the staff gauge is at the proper location (two-thirds of the length of the converging
section back from the beginning of the throat).
Read to the nearest division the gauge division at which the liquid surface inlersects the gauge.
- Read H, in feet from the staff gauge.
VI - 20
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POTW Inspection and Sampling Manual Appendix VI
• To determine the flow rate, use Table VI-3 in the units desired, or use tables published in flow
management standard references, or calculate using the coefficients in Table VI-4.
Flow Measurement - Submerged Flow Conditions
Generally, it is difficult to make field measurements with submerged-flow conditions. In cases when
measurements can be obtained (using a staff or float gauge), the procedures listed below should be followed:
• Determine the upstream head using a staff or float gauge.
- Read to the nearest division and, at the same time as for H,,, the gauge division at which the
liquid surface intersects the gauge.
- Calculate H, from the gauge reading.
• Determine the downstream head (Hb) using a staff or float gauge.
- Hb refers to a measurement at the crest.
- Read to the nearest division, and at the same time as for H., the gauge division at which the
liquid surface intersects the gauge.
- Calculate Hh from the staff reading.
• Determine the flow rate
- Calculate the percent submergence [Hh/H.J x 100
- Consult Table VI-XXX
When a correction factor is obtained, use H, and find the free-flow from Figure VI-XXX.
- Multiply this free-flow value by the correction factor to obtain the submerged flow.
The inspector may use an independent method of measuring head, such as a yardstick or carpenter's rule at the
proper head measurement point. Due to the sloping water surface in the converging section of a flume, it is
essential that the proper head measurement point be used.
Flow Measurement in Palmer-Bowlus Flume Applications
• Obtain head measurements as in the Parshall Flume application, using the secondary device. The head
is the height of the water above the step. The total depth upstream of the step is not the head.
• Refer to the manufacturer-supplied discharge tables to convert head measurements to flow data.
Palmer-Bowlus flumes, unlike Parshall Flumes, are not constructed to rigid dimensional standards.
The inspector must not use discharge tables supplied by other manufacturers.
Verification
Most flow measurement errors result from inadequate calibration of the flow, totalizer and recorder. If
the inspector has determined that the primary device has been installed properly, verification of the lU's system
is relatively simple. The flow determined from the inspector's independent measurement is compared to the flow
of the lU's totalizer or recorder. The inspector's flow measurements should be within 10 percent of the ILJ's
measurements to certify accurate flow measurement. Optimally, flow comparisons should be made at various
flow rates to check the system's accuracy.
VI - 21
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POTW Inspection and Sampling Manual Appendix VI
When the Ill's permit requires daily average flow to be measured by a totalizer meter, the inspector
should verify that the totalizer is accurate, i.e., properly calibrated. This can be done during a period of steady
flow by reading the totalizer and at the same time starting a stop watch. The stop watch should be started just
as a new digit starts to appear on the totalizer. After ten to thirty minutes, the totalizer should be read again, just
as a new digit begins to appear, the stop watch is read. By subtracting the two totalizer readings, the total flow
over the measured time period can be obtained. The flow rate in gallons per minute can be calculated by using
the time from the stop watch. This flow rate should be compared to the flow determined by actual measurement
of the head made at the primary device at the time interval. The calibration of the totalizer should be considered
satisfactory if the two flows are within 10 percent of each other, when the actual measured flow is used as the
known value, or divisor, in the percent calculation.
VI -22
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Appendix VII
EPA's Policy on Split Samples
-------
UNfTED STATES ENVIRONMENTAL PROTECTION AGENCY
WASHINGTON, O.C. 20440
JAN2I
OFfKX Of WATM
MEMORANDUM
SUBJECT: Determining Industrial User Compliance Using Split Samples
FROM: Richard G. Kozlowski, Director
Enforcement Division
TO: Mary Jo M. Aiello, Acting Chief
Bureau of Pretreatment and Residuals
This memo is a response to your letter of September 30, 1991, where you requested
written clarification regarding the use of split samples for determining industrial user (IU)
compliance under die Pretreatment Program. Specifically, you requested g"M«nce on how to
use the data from split samples for determining IU compliance in situations where split
samples yield different analytical results. The fundamental question posed by your inquiry is
whether all analytical results must be used when evaluating the compliance status of lUs and
how to use those results for determining compliance. In situations where split samples exist
and both samples were properly preserved and analyzed* POTWs should evaluate compliance
with applicable Pretreatment Standards in the manner described below.
When evaluating the m»«pii«iM>» status of an industrial user, the POTW must use all
samples which were obtained through appropriate sampling wbniqwf and analyzed in
accordance with the procedures established in 40 CFR Pan 136*. The Environ*""!"!
Protection Agency (EPA) has consistently encouraged Publicly Owned Tre*««*fn Works
(POTWs) to periodically split samples with industrial users as a method of verifying the
quality of the monitoring data. When a POTW splits a sample with an IU, me POTW must
use the results from each of the split samples.
A legitimate question arises, however, when a properly collected, preserved and
analyzed split sample produces two different analytical results (e.g., one which inrt«c? IPS
compliance and the other shows noncompliance, or where both indicate either
noncompliance but the magnitudes are substantially different). In these instances, questions
arise regarding the compliance status of the IU, and what should be done to reconcile die
results.
1 See Memorandum, 'Application md UK of the Regulatory Definition of Significau Noacompliance for
Indusoul Users.' U.S. EPA. September 9. 1991.
-------
There is inherent variation in all analytical measurements, and no two measurements
of the same tnalyte (even when drawn from the same sample) will produce identical results.
When a split sample is analyzed using appropriate methods, there is no technical basis for
choosing one sample result over the other for determining the compliance status of a facility.
Since this is the case for all split samples which have been properly analyzed, the POTW
should average the results from the split and use the resulting average number when
determining the compliance status of an IU. Using the average of the rwo sample results
avoids the untenable situation of demonstrating compliance and noncompliance from the same
sample.
If the split sample produces widely divergent results or results which are different over
a long period of time, then the cause of the discrepancy between the analytical results should
be reconciled. When this happens, the POTW should investigate Quality Assurance and
Quality Control (QA/QC) procedures at each laboratory involved For example, the POTW
could submit a spiked sample (i.e., a sample of known concentration) to the laboratories
involved (preferably blind) to determine which laboratory may be in error.
In situations where one or both of the analytical results is determined to be invalid,
there are compliance and enforcement consequences. If one of the analytical results is
determined to be invalid, the average value for that sample is also invalid. In this situation,
the value for this sample should be the value of the sample which was not determined to be
invalid (e.g., if the Ill's results are determined to be invalid, the POTW should use its sample
for assessing compliance, and vice versa). If both samples are determined to be invalid, the
averaged result from thai sample should be discarded and not used for compliance assessment
purposes. In either case, the POTW must recalculate the compliance status of the IU using
all remaining valid sample results.
In summary, whenever split samples are taken and both are properly preserved anu
analyzed, the POTW should avenge the results from each sample and use the averaged value
for determining compliance and appropriate enforceuxnt responses. Where the sample results
are widely divergent, the POTW should instigate QA/QC measures at each of the analytical
laboratories to determine the cause of the discrepancy. If one or both of the samples are
invalid, the POTW must r?rtlnt|M» the compliance status of the IU using all .valid results.
If you have any further questions regarding these questions, please feel free to call me
at (202) 260-8304. The staff person familiar with these issues is Lee Okster. Lee can be
reached at (202) 260-8329.
cc: Cynthia Dougherty
Regional Pretrea"n"it Coordinators
Approved State Pretreatment Coordinators
BUlTelliard
-------
UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
WASHINGTON, D.C. 20460
APR I 2 1993
OFFCCOF
WATER
Mr. Harold R. Otis
Chairman, Split Sampling Task Force
Greater Fort Wayne Chamber of Commerce
826 Ewing Street
Fort Wayne, IN 46802-2182
Re: Using Split Samples to Determine Industrial User Compliance
Dear Mr. Otis:
In response to your letter of January 12, 1993, and your phone conversation of
February 9, 1993, with Lee Okster, I am providing a further discussion of the issues
surrounding the use of split samples to determine industrial user (IU) compliance with
Pretreatment Standards. In your letter and your phone conversation, you requested
clarification from the Environmental Protection Agency (EPA) on three issues. First,
you requested a firm definition of what constitutes "widely divergent results" when
comparing split sample results. Second, when a publicly owned treatment works
(POTW) splits a sample with an IU, you inquired whether a POTW must use the
industrial user's data to determine compliance with pretreatment standards. Finally, you
requested written authorization from the EPA to incorporate the language from our
existing guidance memorandum on split samples into the Rules and Regulations of the
Water Control Utility for the City of Fort Wayne.
What are Widely Divergent Results?
As you are aware, the EPA issued a memorandum on January 21, 1992, entitled
"Determining Industrial User Compliance Using Split Samples." The "widely divergent
results" criterion established in this memo is to be used as an indication that a problem
exists with the laboratory analysis. We did not include an indication of what constitutes
"widely divergent" in our memorandum because the amount of "normal" analytical
variability depends on the pollutant parameter being tested and the method being used
to analyze the sample. With appropriate QA/QC, this "normal" analytical variability is
small. In general, though, metals analyses have a smaller variation than organics
analyses, but the magnitude of the variability depends on the pollutants being tested.
Therefore, no hard and fast rules exjst for determining what is widely divergent. This
determination is left to the discretion of the local authority.
Pnnted on flecvc'efl Paoer
-------
Must the POTW Use AU Sample Results?
In the January. 1992, memorandum we state that "the POTW must use all samples
which were obtained through appropriate sampling techniques and analyzed in
accordance with the procedures established in 40 CFR Part 136." The memo further
states "[w]hen a POTW splits a sample with an IU; the POTW must use the results from
each of the split samples."
The POTW is required to sample the IU at least once per year to determine,
independent of information supplied by the IU, the compliance status of that facility. If
the POTW does not wish to be in a position of comparing its own data with the IU when
it samples the lU's discharge, it is not required to split its samples with the IU.
Furthermore, we do not recommend that the POTW use a split sample with the industry
to satisfy its annual sampling requirement. The POTW should pull its own sample so
that it has data which are truly independent of the lU's results.
The POTW also has the primary responsibility to ensure compliance by the IU
with all applicable pretreatment standards and requirements. One way the POTW can
satisfy its requirement to ensure compliance is to split a routine sample taken by the IU.
If a POTW splits a routine sample taken by the IU, it must use the lU's data, in
conjunction with its own, to determine the compliance status of the facility (assuming all
of the data are sampled and analyzed appropriately). We encourage POTWs to split
samples in this manner to verify the lU's data. In a similar fashion, if the POTW
chooses to split its own sample with the IU, it must use all of the data to determine the
compliance status of the facility (assuming all of the data are appropriately analyzed).
When the POTW splits a sample with an IU (whether it is a routine sample by
the IU or an annual sample by the POTW) the POTW has the responsibility to
determine whether the lU's results from the split sample are valid. Where an lU's
results are different than the POTW's, the burden is on the IU to show that all
preservation, chain-of-custody, and analytical and QA/QC methods were followed. If the
IU cannot make this showing, then the analytical results from the IU should be discarded
when determining the compliance status of the facility. If the IU establishes that it
followed all appropriate procedures, then the POTW should review its own QA/QC
program. If both the IU and POTW have followed appropriate procedures, and there is
still a wide divergence, then follow-up sampling should be conducted. If follow-up
sampling consistently shows IU noncompliance, or if the POTW is otherwise satisfied
with the validity of its own results, it should proceed to follow its enforcement
procedures.
Authorization From the EPA
In regard to your final request, the City of Fort Wayne has the authority to
incorporate these procedures into its Rules and Regulations without any authorization
from the EPA. As long as the City has the minimum legal authorities to implement its
- 2 -
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approved program, it has satisfied its requirements under the Federal regulations. As
always, the City is encouraged to adopt the EPA's Pretreatmcnt Guidance whenever
possible.
I hope this letter responds to your questions and concerns. If you have any
further questions, please feel free to call me at (202) 260-8304 or you can call Lee at
(202) 260-8329.
Sincerely yours,
.
ichard G. KozlowsKi, Director
Water Enforcement Division
U.S. Environmental Protection Agency
cc: Cynthia Dougherty
Regional Pretreatment Coordinators
Approved State Pretreatment Coordinators
-3 -
-------
Appendix VIII
Compliance with Continuous Monitoring of pH
-------
UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
WASHINGTON, D.C. 20460
MAT t 3 1993
OFFICE OF
WATER
Mary Jo M. Aiello, Chief
Bureau of Pretreatment and Residuals
Wastewater Facilities Regulation Program (CN 029)
New Jersey Department of Environmental
Protection and Energy
Trenton, NJ 08625-0029
Dear Ms. Aiello:
Thank you for your letter of January 25, 1993, to
Jeffrey Lape of my staff regarding the New Jersey Department of
Environmental Protection and Energy's (the Department) proposed
policy on waivers from pH limits applicable to industrial
discharges to Publicly Owned Treatment Works (POTWs). Subject to
the qualifications stated below, your proposed policy is
consistent with the federal regulations.
Your letter relates to the application of 40 CFR 401.17,
which allows facilities that employ continuous pH monitoring to
exceed certain pH limits one percent of the time. Your letter
correctly notes that 40 CFR 401.17 applies only to discharges to
surface waters, but inquires whether an analogous policy could be
applied to discharges to POTWs.
We believe an analogous policy could be applied to
discharges to POTWs,,, subject to several restrictions. First, the
federal pretreatment regulations contain a specific prohibition
against discharges with a pH below 5.0, from which no waivers are
allowed unless the treatment works is specifically designed to
accommodate such discharges (40 CFR 403.5(b)f2)). Your letter
correctly acknowledges that, except for such specifically
designed treatment works, waivers below this minimum limit would
not be consistent with federal regulations. Second, although
federal pretreatment regulations do not include an upper pH limit
applicable to all discharges, some categorical pretreatment
standards do so. Waivers from the requirements of those
categorical standards would not be allowed unless expressly
permitted by the standards themselves.
Third, a POTW may not grant a waiver from a local limit if
such waiver would cause pass through or interference. Since
local limits are based on considerations at each POTW, it would
not be appropriate to institute a waiver of local limits that
applies statewide regardless of conditions at individual POTWs.
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-2-
So long as POTWs act consistently with their obligations not to
allow pass through or interference, however, they might implement
waivers that apply either more or less frequently than the 1% you
propose. Of course, if it wishes, the State could cap all
waivers at 1% and thereby be more stringent than Federal law,
which requires no cap.
We note that, if a POTW wishes to provide waivers from pH
limits that are technically-based and are part of the POTW's
Approved Pretreatment Program, the POTW will have to modify its
Approved Pretreatment Program accordingly. The Department should
consider for each POTW whether the adoption of this policy is a
"change to local limits, which result in less stringent local
limits" and therefore requires a formal modification under 40 CFR
403.18(c)(1)(ii), or whether it constitutes a clarification of
the POTW's existing local limits.
I hope that this response addresses your concerns. If you
have any questions or would like to discuss this further, pleas*
call m* at (202) 260-5850 or Louis Eby at (202) 260-2991.
Sincerely,
/
C. DoughertyCX>ire
-------
Appendix IX
Example Standard Operating Procedure
-------
STANDARD OPERATING PROCEDURES MANUAL
PINELLAS COUNTY SEWER SYSTEM
INDUSTRIAL MONITORING PROGRAM
JANUARY 19S9
-------
TABLE OP CONTENTS
SECTION
1.0 INTROnuCTTON L
2.0 noCUM*NTATTON 2
2.I FIELD DATA RECORD 2
2.2 FIELD DOCUMENTATION LOG 2
2.3 FIELD pH CALIBRATION LOG 2
2.4 FLOW METER CALIBRATION LOG 2
2.5 pH METER CALIBRATION - LABORATORY 3
2.6 pH CALIBRATION/SPIKE CHECKLIST 3
2.7 CHAIM-OF-CUSTODY FORM 3
2.8 SAMPLI STORAGE FORM 4
2.9 ISCO CONTROL LOG 4
2.10 CONTAINER CONTROL LOG 4
3.0 CHATM OF rn«TnrW 5
3.1 FIELD DATA RECORD 5
3.2 EQUIPMENT DOCUMENTATION 3
3.3 SAMPLI COLLECTION ;
3.4 SAMPLE TRANSPORT .:
3.5 TRANSFER OP CUSTODY
3.8 SAMPLING QUALITY COKTROL .:
-------
TABLE OP CONTENTS (CONTINUED)
?AGZ
4.1 CLEANING • 3
4.2 TRA7FXC 14
4.3 SAMPLING .;
4.3.1 safety Clothing 15
4.3.2 Opening Manholee -.3
4.3.3 Lifting and Moving 16
5.1 ISCO SAMPLER -
5.2 TUBXNO . 3
5.2.1 Dairies .3
5.2.2 Metals .3
5.2.3 Organic* ;:
5.3 COMTAIMEM ; :
5.3.1 Compoeite Jug« ;:
5.3.2 Oi«crete Saaple Bottles :.
5.3.3 Saaple Container* ::
6.0
6.1 ISCO SAMFLEM
6.2 PLOW M1TU
6.3 BATTERIES
6.4 pH METER
-------
TABLZ OF CONTENTS (CONTINUED)
SECTION.
7.0 CALIBRATION 24
7.1 FLOW METER 24
7.2 pH METER 24
7.2.1 Pi«ld Calibration 24
7.2.1.1 Corning pH m«tar 24
7.2.1.2 Orion pH matar 25
7.2.2 Laboratory Calibration 25
8.0 SAMPT.TNG P?»P>»VTTON 25
9.0 TYPM OF SAMPTTS/MTTHODOTOGY 21
9.1 GRAB SAMPLES 2?
9.2 COMPOSITE SAMPLES : :
10.0 FI^T.n AHATYAVfl ;L
11.0 PouTPHTirr S*T-UP ::
11.1 ACTUATOR ::
11.2 FLOW METER : :
11.3 WATER METERS :5
11.4 GRAB SAMPLER
11.3 ZSCO SAMPLER :;
11.S.I Composite Saaplas
11.5.2 S«quantial Saaplac
12.0 INOUSTRTAT. VAH M\TNTTNANC^ ANF> SUPPT-Y
12.1 MAINTENANCE
12.2 SUPPLY
-------
TABLE OF CONTENTS (CONTINUED)
FOPM*
FORK 1
FORM 2
FORM 3
TABLI 1
TABLE 2
TABU 3
FIELD DATA RECORD
CHAIN-OF-CUSTODY FORM
VEHICLE MAINTENANCE SCHEDULE
DAIRY SAMPLING CHECKLIST
METAL/CYANIDE SAMPLING CHECKLIST
INDUSTRIAL VAN Ihv^
PACE
6
11
42
27
21
43
FICUR1 1
WATER METERS
37
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1.0 INTRODUCTION
The Pinellas County Sewer System (PCSS) , Industrial Monitor:.-.?
Program, is responsible for monitoring industrial discharges to
the sewer system. There are four primary goals in industrial
monitoring: to protect worker health and safety, to prevent
inhibition to the wastewater treatment facilities (WWTF), to
control the quality of effluent discharged from the WWTF, and to
limit sludge contamination. This Standard Operating Procedures
Manual (SOPM) explains the procedure* used to collect samples of
industrial wastewater, including all quality control (QC)
protocols, equipment cleaning and maintenance, and safety
cons iderations.
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2.0 DOCUMENTATION
Documentation is an integral part of any p r e t r e a t m e n t
program. The validity of samples collected and data obtained both
in the field and the laboratory is ensured through documentation
and record keeping. All information must be complete and
accurate. Record management and methodology must be consistent
throughout the program to support the validity of data gathered.
Failure to maintain records and documentation according to set
procedures could result in these documents being inadmissible as
evidence in court. In addition to the Field Data Record, which is
the primary sampling information document, there are logs for
equipment calibration, maintenance, chain-of-custody, and
cleaning.
2.1 FIELD DATA RECORD
The Field Data Record includes sample site identification,
type of sample, sampler and battery identification, settings on
the sampler, results of field analyses, flow information (where
applicable), and any additional information related to the site or
effluent characteristics.
2.2 FIELD DOCUMENTATION LOG
The Field Documentation Log is used to record which sites are
sampled each day, and any violations, conversations, or notable
occurrences during the sampling event.
2.3 FIELD pH CALIBRATION LOG
The Field pH Calibration Log is used to record calibration of
the field pH meter during the sampling event. The field pH meter
is calibrated at each site prior to measuring the pH of the
effluent. Calibration and slope are checked, adjusted as
necessary, and recorded, along wit the temperature of the buffer.
2.4 FLOW METER CALIBRATION LOG
The Flow Meter Calibration Log is used to record program
information for the flow meter and water level calibration from
the initial value shown on the meter to the actual measured
water level.
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2.5 pH METER CALIBRATION - LABORATORY
The laboratory maintains their own notebooks to record
equipment calibration. When the laboratory pH meter is used, it
must be calibrated as discussed in Section 7 , and the results
recorded in the (laboratory) pH Meter Calibration Log Book.
2.6 pH CALIBRATION/SPIKE CHECKLIST
The field pH meter is calibrated in the laboratory on a weekly
basis. The buffers and internal fill solution are also changed at
this time. Once a month, an EPA known sample for pH is checked
after meter calibration in order to verify the accuracy of the pH
meter. The pH C a I i b r a t i o n/S p i ke Checklist is used to record the
date and time of field pH meter calibration, calibration data,
results and true value for the known sample, and to document the
buffer and fill solution changes.
2.7 CHAIN-OF-CUSTODY FORM
When samples are brought in to the laboratory for analyses,
they must be logged in and received by the laboratory personnel.
The C h a i n - o f-C u s t o d y Form includes sample collection information,
types of analyses to be run, preservation, and a space for the
laboratory personnel to sign with the date and time the sample was
received by the laboratory. Any comments which may be important
for the analysts to know prior to running the sample, or in
reviewing the results of analyses, are also included on this
form. A more detailed discussion of the C h a i n - o f-C u s t o d y Form is
presented in Section 3.5.
There will occasionally be samples collected which need to be
sent to an outside laboratory for analyses, either for
confirmation of a number, or for analysis of parameters which we
cannot do in-house. The laboratory is responsible for filling out
additional C h a i n - o f-C u st od y Forms for sending shipments to an
outside laboratory. The C h a i n - of-C u s t o d y Form (discussed above)
will still be used by sampling personnel, with the addition of a
statement that the samples are to be sent to an outside
laboratory. The laboratory documents all shipment information on
the Custody Form.
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2.8 SAMPL1 STORAGE FORM
When a sample is in violation of applicable limits, it is
saved for evidence. The caps are sealed off with tap* prior to
long-term storage. The Sample Storage Fora is used to record all
saaplee which are currently b«ing stored, as well as holding tiaes
and disposal datas for those samplas.
2.9 ISCO CONTROL LOG
It is crucial to the integrity of the samples collsctad that
all equipment used in sample collection be clean and free of
contamination. Those parts of the sample equipment which do not
come into contact with the wastewater are cleaned with soap and
water for sanitary reasons. Any piece of equipment which will
come into contact with the wastewater must be cleaned according to
the procedures outlined in Section S. The ISCO Control Log lists
the ISCO number/ the site at which the sampler was used, the
date(s) used, the date cleaned, the cleaning method used, and the
initials of the personnel cleaning the equipment.
2.10 COMTAXND COWTROL LOO
The container(s) used to collect the sample must also be
cleaned thoroughly and that cleaning documented. Actual sample
bottles are cleaned by the laboratory according to their quality
assurance protocols. Composite and sequential bottles are cl«an«d
by Program personnel, according to the procedures outlined in
Section 3. The Container Control Log lists the container number,
the site at which the container was used, the date(s) used, the
date cleaned, the cleaning method used, and the initials of the
personnel cleaning the container.
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3.0 CHAIN-OF-CUSTODY
The overall success of a monitoring program depends on its
capability to produce valid data through the use of accepted
sampling procedures and protocol, and its ability to substantiate
such data through documentation. This begins with properly
trained personnel and continues with sampling preparation, the
sampling event, transfer of sample custody, laboratory analyses,
equipment cleaning and data management. The importance of this
concept is realized when sampling data is used as evidence in
court against non-compliant Industrial Users.
3.1 FIELD DATA RECORD
The Field Data Record is a permanent record of the information
gathered during the sampling round. An example of the Field Data
Record is included as Form 1. The sheet should be accurate,
legible and complete. INFORMATION RECORDED SHOULD NEVER BE
FALSIFIED. A few points to consider:
1) When identifying the facility sampled, record the complete
name of the industry and street address. This line also
includes the Industry Login Code.
2) The description of the sample site location (point where
sample is actually taken) should be concise.
3) The last name of each person from PCSS that is actively
participating in the sampling round is recorded by that
person for Day 1. If the same people are present the next
day, they place their name or initials by Day 2. If a
different person is present, he records his name by Day
2. It is preferable that sampling personnel remain
consistent throughout the round to assure continuity.
4) Monitoring is considered unscheduled unless the industry
is notified of a specific date and time that they will be
sampled, in which case it would be a scheduled event.
Surcharge sampling is marked as such. A sample would be
considered a demand sample if it were taken in response to
a complaint or an emergency situation. A sample will
either be a grab, a composite, or a sequential sample.
5) When collecting samples for metals analyses, a deionized
(Dl) water blank is collected using the tubing and ISCO to
be used at that site. This will confirm that the
equipment was not contaminated at setup. The time
collected is also noted.
-------
PINELLAS COUNTY SEWER SYSTEM
INDUSTRIAL MONITORING PROGRAM
FIELD DATA RECORD
Facility Stapled:
Facility Address:
Sample Sits Location:
Parsons Sampling: n,-v 11
Type Monitoring: [] Scheduled
UGrab []
Blank Lab Number:
Sample Lao Number:
Login Code:
n-v 2)
[ ] Unscheduled [] Demand [] Surcharge
-Hr Composite [] _ -Hr' Sequential
Time Collected:
1) ISCO I.D. I: Actuator Used: [] Y«»
2) ISCO Battery I:
3) Sample Interval (minutes/gallons):
4) Suction line: Length (ft) Diameter (in) []3/8" "1/4"
3) Mode: UTlma []Flow
6) Volume Selector: Volume per sample ml.; Head feet
7) Volume, of Measured Grab: ml.
Date: / /
Date: / /
Liters. Number of Containers:
Battery I.D.I:
Time: : Date:
Time: : Date:
TTM* OF
Initial: _ :
Final j _ :
Volume) Collected z
Flov Meter I.D.fs
Initial:
Finals
Total gallons used:
nit
IC\ U
/
/
/
Initials
/
/
Dairiest
Metalst
Cyanidei
v. Organic*s
Oil ft Grease: [] Sulfurie Acid
Other i
(] Chilled [] sulfurie Acid
U Witric Acid (Cd
U Sodium Hydroxide
[] Sodium Thioaulfate
Split sample received
Date
Duplicate Sample Collected: (] Yes [] No Lab Number:
Record Reviewed:
-------
6) Each sample receives a lab number. This number, when
complete, always has eight digits. The first two digits
refer to the year, as in "87-, the second two digits
refer to the month, and the third pair to the day. The
last two digits are assigned by the lab when the saaplts
are checked in and are known as the sequence number. A
sample collected on March 13, 1987, with sequence nunrtr
05, would raad 87031305. If a fiald blanJc is collected.
it is also assigned a lab number, and recorded on the
Field Data Record.
7) It is important to record the ISCO ID number. If there
is any question as to the cleaning procedure used or t.-.a
cleanliness of the equipment, it can easily be traced
back to the Cleaning Documentation Log.
8} ISCO settings must be recorded completely. In sost
cases, sample intervals will be set every 15 minutes for
timed composites. Gallons are used for flov composites
Time or Plow must be indicated. If any settings are not
applicable, they should be marked as such. "Volume of
Measured Grab* is the actual volume collected when usi.-.g
the recorded ISCO settings.
9) Time of sampling is important to note. On a regular
monitoring basic, 24-hour composite samples are collects!
after the last sample interval, and before the 24th
hour. Example: Sample interval is every 15 minutes, a.-.i
the initial sample is at 9:00 as. The sampler is to re
pulled after the 8:45 am sample is collected. Note:
This applies also to an 8-hour, 12-hour, 16-hour, etc.
composite. Composite samplee may be collected and
composited over any time or flow interval, depending -p = -
the purpose of the sampling.
10) when a flov meter is used, the time of flov meter
reading* and total flow is to be recorded along with t:-.«
flov meter identification. Plow meter settings are
recorded along with calibration information in the Flew
Mater Calibration Log. If a flow meter is not used, --..3
section is to be crossed out.
11) Data valuem resulting from analyses performed in the
field are to be recorded accurately and neatly, and
initialed after test completion. This area is extr«=«.
important, as pH and temperature violations could rts~.-.
in the issuance of citations.
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12} The preaervativee which are added to each sample
container must. be marked off, along with the paraaetars
to be analyzed. If th« preservative/parameter is not
listad, it should be apacifiad.
13) If an industry raquaata a "split* (a portion of our
sample for thair own analytical purpoaaa), make aura to
hava the paraon receiving tha sample aign and data tha
Fiald Data Racord.
14) Any unusual oceurrancaa ahould ba racordad undar tha
Coamenta aection, along with tha data, tima and duration.
15) Arv conversations with industry personnel that would ba
of interest are documented in the Field Documentation Leg
and referenced in the Coamenta section.
16) For every 10 samples collected, one duplicate aample la
taken. If laae than 10 aamplee are collected, one
duplicata aample is still collected. When a duplicata
aample ia taken at a site, the lab number ia recorded on
tha Fiald Data Record for that site.
It is important that all field recorda ba completed uaing
black waterproof pan. If errora are aada, corractiona should ba
aada by drawing a single line through tha error, and entering t^.a
correct information. Such correctiona should ba initialed and
dated. Undar n<* "<*^"mjiancja ahould a statement be crossed out
so that the information is not legible.
3.2 ZQUIPMWT DOCUMWTATIOK
Proparly claanad, maintained and handlad aqulpmant will halp
ansura tha Intagrity of tha Monitoring Program. Documentation :•
vital to support thaaa afforta, aapacially in tha avant of
litigation. Documentation is discuaaad la faction a. Proper
cleaning tactmiguea ahould ba implemented according to tha
analyses ta> ba performed. This involves tha ZICO head itself,
tubing, aajamls) containara and any other equipment that may coae :
contact vitfc tha vaatevatar diacharge at tha sampling point.
Tubing ia sita specific to alleviate tha poeaibility of cross
contamination, for proper aquipaent cleaning techniques and uae
of sample containara aaa Section 3.
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3.3 SAMPLE COLLECTION
One* a sample is collected, precautions oust be taken to
ensure sample validity and security. It is possible that the
sample collected sight be in violation and the data could be used
in court. THIS SHOUTn ALWAYS B* K^PT IN MIND.
Every sample collected, regardless of type, should be handled
in the same manner. Once a sample is collected, the following
procedures should be used:
1) Sample containers must be flushed with a portion of t.u.e
effluent sample prior to filling. In the case of
containers with preservatives, i.e., cyanide and volatile
organic sample*, this step is omitted.
2) Sample should be veil agitated (to prevent settling) ar.d
then poured into the sample container, filling to about
1/2 inch from the top (See specific instructions for
purgeable organic samples). If filling more than one
sample container from a composite jug, make sure to shaxe
the jug before each pour to prevent settling.
3) Field tests on a 24-hour composite sample are taken frca
the sample remaining after all sample containers are
filled. If collecting a grab sample for laboratory
analysis, field tests are taken on a separate portic.- ;f
the same grab. The sample container is filled complete./
to the top, and then a small portion is poured into a
separate container for field analysis.
4) Field tests on the initial and final grab samples that
are collected when conducting 24-hour composite sampI.-?
arei taJcen from grab samples collected immediately pnsr
to the initial sample in the composite round and
immediately after the final sample.
5) Sample containers should be labeled with:
- Industry login code for sits at which sample is
collected.
- Type) of sample collected (grab or 24-hr composite)
- Data sample collected, written as process number.
- Type) of preservative added to sample, i.e., HN03,
R3S04.
- Initials of sampling personnel.
6) Sample should be properly preserved, and sample pH
checked to confirm that pH is adjusted appropriately
7) Sample should be placed on ice.
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3.4 SAMFL1 TRANSPORT
One* the samples ars in the van, it is important to talcs every
precaution to make aura that the samples are secure. Whan away
from the van, sake sure it is leapt locked. If away for an
extended parted of time, tha coolar should b« tapsd shut and
initialsd in such a manner that tampering would ba notad. Tha
samples must ba leapt in sight, or in a sscurs place, at all tiaas.
3.S TRANSFER Of CUSTODY
Whan delivering the samples to the laboratory, they should ba
placed on the central counter by the sink. The Chain-Of-Custody
Form should be filled out. When the Fora is completed, the lab
personnel must sign in the samples. At this point, the
responsibility for the custody of the samples is transferred to
the lab. An example of the Chain-of-Custody Form is included as
Form 2, and an explanation of the information to be completed is
provided below.
1) SOURCIs Type of location sample was collected from, i.e.,
industry, POTW, transmission system.
2) COLL1CTXD BYi Identification of personnel involved with
sampling.
3) DATlt Date that sample was collected. If it is a 24 hour
composite sample, the date the sampler was set up is tha
sample date.
4) DBLXVBR1O BY: Personnel that delivered samples to the
lab.
S) DAT!: Date saaples are signed in.
6) TZXIt Tim« samples are signed in.
7) PUMBVATXVBs Circle letter for preservative(s) used.
S) UCUVBil Bit Lab personnel receiving sample accepts
transfer by signing.
9) OATlt Data lab personnel receives sample.
10) TXMlt Time that lab personnel signs in sample.
11) PROCXSa MUMBOt This is a six digit number, the first two
digits refer to tans year, as in *•?•, the second two
digits refer to the sonth, and the third pair to the
day. A sample collected on March 13, 19t7 would be
process number S70313.
10
-------
?" 3M "7
INDUSTIUAZ, UAATI PVOGftAM
CHAIM-OF-CUSTODY FOHH
SOOUCt: Industry PftZStXVATXVZ:
COLLZCTtO BY: OATI:
^ZLIVtJllD BYJ OATIl TIM1: H,SO.
WCEI'/TO BY: OATH TIXlJ H*0,
PROCMS MUNB0I M*0l
Otft«r
Tim
TYW
*no J0^]
n -p/i
VI
Turtei^itv MTD
Con M/l
TCX* *B/1
CU
Pb
Ml
ka
ZB ao/1
m ••/!
T •
PAO1 NO.
COO(OC«lltO«14
11
-------
12) SEQUENCE NUMBER: This i» * two digit number assigned by
the lab which, combined with the process number,
completes the sample lab number.
13) DESCRIPTION: Five-digit Industry login code.
14) TIME: Tim* sample is taken (use military time). If it :.s
a 24-hour composite sample, put down times for the
initial and final samples.
15) TYPE: Type of sample, i.e., grab or 24-hour composite.
16) PRESERVATIVE: Letter(e) Indicating preservative(s) used.
17) PARAKETERSt Mar* squares with a yellow felt tip marker,
indicating tests to be run on sample. Blank spaces are
provided to request additional test(s). This space is
most commonly used when shipping samples to an outside
laboratory.
18) Field pa information is transferred from the Field Data
Record. This includes initial, final and sample pH.
19) Cyanide or other test kit number* arc to be placed
directly under the column that they correspond to.
3.6 SAMPLING QUALITY CONTROL
Control checks should be performed during the sampling round
to ensure proper sampling and cleaning techniques. Thee*
documented checks; can also be used as supportive evidence in
court.
A sample blank is run at each sample site, where metal or
organic samples are collected, at the beginning of the -sampling
round as a QC check on the equipment being used at that site. Dl
water is pumped through the ISCO sampler and tubing, and preserved
in the same) manner as the sample. This ensures that any
contamination of the equipment or lab chemicals will be detected.
Blanks are not run for biological samples (BOO, solids).
Split sample* are sometimee taken by industries that PCSS
monitor*. A split sample is a portion of a sample collected by
PCSS which is given to the industry for testing. That portion of
the sample is then analysed by the industry or sent out to a
private laboratory. Comparison of the data is useful in
identifying discrepancies in analytical methodologies. Duplicate
samples are also collected and analyzed for at least ten percent
of the samples collected as* a check on our laboratory.
-------
4.0 SAFETY
There are many safety precautions which must be followed both
at the office and in the field. Industrial monitoring, by its
very nature, adds additional potentially hazardous situations to
those existing in any field sampling situation. On the job safety
can be broken down into three broad categories: cleaning,
traffic, and sampling. Safety hazards associated with doing
chemical analyses in the field are discussed in the Hach Portable
Laboratory Procedures Manual.
4.1 CLEANING
The major hazard associated with cleaning sampling equipment
and containers is the use of chemicals. Nitric acid, hydrochloric
acid, and/or acetone are used in cleaning certain types of
equipment. The hazards come from 1) mixing the acid/DI water
solution, and 2) using the solution for cleaning.
Acid, when mixed with water, creates fumes which may be
hazardous if inhaled, and can cause irritation to the eyes, nose
and throat. Acid can cause skin burns if it is spilled on the
skin. This can occur during mixing or cleaning. Upon working
with acid, rubber gloves, a rubber apron and goggles should be
worn. Acid solutions should always be prepared under the hood
with the vent fan turned on. It is also advisable to wear rubber
boots when cleaning, to protect your feet and lower legs from
spilled acid, as well as to keep them dry.
NOTE : ALWAYS ADD ACID TO WATER - NEVER ADD WATER TO ACID.
Acetone is used to clean equipment that is used for collecting
organic samples. It is extremely flammable and ignitable.
Acetone is incompatible with nitric and sulfuric acids and should
not be used where these acids are present. While the primary
hazard is ignition, acetone is also a skin and mucous membrane
irritant. Gloves and a respirator with organic vapor cartridges
must be worn when working with acetone. Goggles must be worn to
protect against any possible splashing.
PREVENT OR AVOID ALL IGNITION SOURCES.
13
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Other hazards associated with cleaning are the potential for
slipping on wet ground, and strains from lifting and moving
equipment. Lifting and moving equipment will be discussed under
sampling. Slipping, tripping or falling are problems which can
occur during any activity, and can be prevented by wearing proper
footwear (good fit and condition) and by using extra caution in
areas of potential hazards.
4.2 TRAFFIC
All County employees who are authorized to drive a County
vehicle are required to take a driving safety course. In addition
to following safe driving techniques, wearing seatbelts and
observing traffic laws, there are other concerns related to
working on or near the road and/or parking lots. The county
requires that cones be placed
in front of
lots.
and/or
The
behind
the
vehicle whenever it is parked.
parking in a heavily trafficked
hazard lights should be used in
has to work on or near the road
proximity, a safety vest must be
blocked off with cones and/or
More cones may be advisable when
area. When parking on the road,
addition to cones. If an employee
or where cars may pass in close
worn and the work area should be
barricades. Before leaving the
site, the area should be checked to ensure that everything was
reloaded into the van, and a circle-of-safety check should be
performed (walk around vehicle, look under, and check area).
4.3 SAMPLING
Because sampling is conducted at industrial locations, often
in confined or remote areas, there are so many potential hazards
which must be recognized. Hazards associated with sampling
include; working around unfamiliar chemicals/equipment; handling
contaminated wastewater; lifting and moving equipment; and opening
and/or entering manholes and flumes. A list of the safety
equipment kept in the industrial van is included below:
acid-sill pads
eye-wash station
first aid kit
goggles
I atex gloves
safety cones
barricades
f i re exti ng u i sher
gas/vapor detector
hard hats
respi rators
safety vests
14
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4.3.1 Safety Clothing
Steal to* shots or boots must be worn at all times when
sampling. Steel toes arc protection against manhole lids and
flume doors or sampling equipment dropping on your feet. They car.
also be of aid in moving equipment or knocking a manhole cover
back on. Steel toes are especially important when accessing an
industrial facility's process or pretreatment area where you are
unfamiliar with the layout, equipment used, and associated
hazards.
If it is necessary to enter a manhole/flume, you must wear a
hardhat to protect yourself against falling objects (manhole
cover/flume door). A hardhat is also protection against injuries
to the head from bumping into the walls or roof of the manhole or
flume. A respirator with the appropriate cartridges should also
be available anytime you enter a manhole/flume (see Confined Space
Policy).
Glove* must be worn at all tiaes when sampling. This is not
only to protect yourself from contamination by the effluent being
sampled, but also to protect the sample from contaaination by oils
or dirt on your hands.
Goggles may be worn to protect against splashing or fumes, if
the situation warrants it.
4.3.2 Opening Manholes
Opening manholes and flumes have SOB* common hazards. Fuzes
and/or gases aay accumulate within the manhole, and possibly could
overcome) someone opening the lid. The cover* of manholes and
flumes should always be opened slightly and alloved to vent prior
to opening them completely. A vapor/gas detector probe should be
inserted through the opening to check the quality of'the air in
the manhole/flume. If the probe indicate* the presence of
hazardous gases, a respirator should be worn while working near
the manhole. The gas detector should be kept on as long as ar.yc-.a
is working near the manhole. Be sure to stand upwind of the
opening so any releases will be blown away from you. Manhole
covers are) usually very heavy and unwieldy. Opening them can te
dangerous. Possible injuries include: catching your hands or
feet undsr th« cover; hitting your lags or fsat with the hook if
it slips loos* of ths cover; falling in; or being overcome by
fumes.
-------
The proper procedure for opening a manhole is to first pry the
aanhole cover open slightly with the manhole hook. The manhole
cover has a small indentation where the hook can be inserted and
used to pry the cover up. Some manholes have a larger opening and
you will be able to slide the hook completely under the edge of
the cover. If not, use a screwdriver, alter- nating with the
hook, to pry the lid up until you can slip the manhole hook all
the way under. Use the hook to slide the manhole cover free of
the rim, so that it is ajar. Test the quality of the air as
discussed above. Allow the manhole to vent for several minutes
before opening further. Use the hook to drag the cover off the
manhole, making sure that your hands and feet are clear.
4.3.3 Lifting and Moving
Do not attempt, to lift or move anything that is uncomfortably
heavy, i.e., causes you to strain yourself. Pinellas County
policy requires that two people work together to lift anything
that weighs over SO pounds. Be sure to practice safe lifting
procedures i bend your knees and use your legs and arm* to support
the weight, not your back.
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5.0 CLEANING
ISCO samplers, composite and sequential collection containers,
sample bottles, and suction tubing are cleaned specific to the
parameters to be analyzed. Equipment which door not come into
contact with the effluent (ISCO base and cover, flow meter, etc.)
is either wiped off or washed with soapy water and rinsed well
with tap water.
Cleaning must be done near a source of potable water (a spigot
with a hose) and should be done in sunlight, when possible, to
facilities drying. ISCO sampler, tubing and container cleaning
must be documented in the appropriate log books.
5.1 ISCO SAMPLER
Two types of ISCO samplers are used, Model 1680 and Model
2710. ISCO Model 2710 does not have a control panel plate, and
does not use a discharge tube: the sample collection tubing
extends all the way through the ISCO head into the base. The
following procedures are used to clean the ISCO samplers:
1 ) Clean two 3-gallon polyethylene jugs, fill one jug with
tap water and fill the other jug with soapy water.
2) The sampler should be completely assembled, i.e.: the
base, head, and head cover are all connected, and a
charged battery installed. Remove the head cover.
3) Leave the auction line attached to the sampler and wipe
off the auction line with a sponge, using soapy water.
Rinse the suction line off with tap water.
4 ) Place the end of the suction line into the jug containing
soapy water. Turn the pump to "Forward", and pump at
least 2 liters of soapy water through the sampler.
5 ) Remove the suction line from the soapy water. Place the
end of the line into the jug containing tap water and
thoroughly rinse (use at least 2 liters). Make sure that
there is no detergent residue remaining in the tubing.
Pull the end of the suction line out of the jug, turn the
pump to "Reverse" (this purges the line) until the line
is free of water, and then turn the pump to "Off".
17
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6) Disconnect the suction line at the white polyethylene
connector barbs. Wipe the barb connected to the sampler
clean, or replace if necessary (there are extras in the
van).
7) Disconnect the battery. With a soapy sppnge, wash down
the ISCO head and carefully rinse it, being sure not to
get the control panel vet. Wipe off the control panel
with a slightly damp paper towel or cloth, and then wipe
it dry with a clean paper towel.
NOTE: THE CONTROL PANEL IS SENSITIVE TO MOISTURE AND OTHER
THAN THIS MILD CLEANING, THE CONTROL PANEL MUST BE
KEPT DRY AT ALL TIMES TO AVOID DAMAGE TO THE
CIRCUITRY.
8) Remove the head from the base. Wash the base and head
cover with soap and water. Rinse clean with tap water
and let dry.
9) After all parts are dry, reassemble the sampler (base,
head, control panel plate-black ISCOs only, head cover)
and store in the shed.
10) If the ISCO sampler is to be used for collecting metals
samples, follow the cleaning procedures outlined below
for metals tubing.
5.2 TUBING
5.2.1 Dairies
Tubing to be used for dairy sampling (or other biological
analyses) should be soaked in a composite jug with soapy water and
bleach for at least 24 hours after use, or replaced if necessary.
The tubing should then be cleaned with soap and water again, and
thoroughly rinsed with tap water, followed by a Dl water rinse.
5.2.2 Metals
Tubing to be used for metals or cyanide sampling should be
acid washed and then rinsed with Dl water as detailed below:
1 8
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1) Get the styrofoam cooler from the shed that holds four
2-liter containers: two clear containers labeled "ACI2"
(1:3 HN03:H20) and two brown containers Labeled "DI
water". The cooler should also contain a length of
tubing with a connector barb on one end. This tubir.g is
used as an extension to the discharge tube/hose when
cleaning.
2} In the laboratory, prepare the acid solution in one of
the clear containers, filling it first with 1500 al DI
water, and then adding 500 ml HN03. 7111 both brown
containers with 01 water (you may want to fill an acid
washed composite jug with 01 water and use this to refil
your brown 01 water containers as they are emptied).
Keep the OZ water containers capped when they are not
being used for rinsing to avoid acid contamination.
CAUTION: U«« *XTR*Tffi CAR* WTTTN WORKTNG WITH ACTD. IT WI"
WUPN. GOGGT.v.q. GTOVTS, AH« AM APRON SHOUT n 3?"
AT A". TTM»*.
3) Release ths ISCO head from ths bass of ths sampler and
placs it on ons of ths PVC stands. Attach ths discharge
tubs extension to the discharge tubs on ths underside :?
ths ISCO head and place the end of ths extension into t.-.a
empty acid container. Turn ths pump to "Forward". ?--t
ths end of ths suction lins in ths full acid solution
container and pump the acid through ths sampler. «>.tr-
ail ths acid has passed through, pull ths end of the
suction lins from the acid container and hold it above
the eampler head, allowing any residue in ths tubing to
be- pumped through. Turn the sampler to "Off*. Repeat
this sequence. Cap both acid containers. Disconnect t.-.a
discharge tubs extension and store in ths cooler.
4) Turn ths pump to "Forward", then put ths end of the
suction lins in one of the brown OZ water containers.
Pump two full containers of OZ wstsr through ths sampler
allowing it to run onto ths ground. Hold ths tubir.g
abovs ths sampler head as discussed above to ensure tr.it
ths tubing is flushed completely through. Turn the
sampler to "Off1*.
5) Disconnect ths suction lins at ths whits polyethylene
connsctor bsrb, and connect ths two ends of ths sucticr.
lins together. Hang the line in ths storsgs shed ur.ti.
ready to uss.
6) Re-assemble the ISCO and store in the shed.
-------
7) Empty the used acid solution out in the laboratory sinJc;
flush with copius amounts of water. Rinse the containers
with OZ water and cap. Store the empty acid and OZ water
containers in the styrofoam cooler. Replace the cooler
in the storage shed.
5.2.3 Organics
Teflon tubing must be used for collecting organic samples, and
should be cleaned according to the procedures outlined below:
1} Wash the exterior of the tubing with soap and water, and
rinse thoroughly with tap water. Pump at least 2 liters
of soapy water through the tubing, followed by a tap
water rinse until no detergent reeidue remains.
2) Pump 2 liter* of OZ water through the tubing.
3) Pump aa interference free redistilled solvent such a*
acetons or methylene chloride through the tubingr stop
the sampler when the tubing is filled with the solvent.
Cap the ends of the tubing and allow it to soaJe for 10 -
IS minute*. Flush the solvent through the tubing until
it is completely purged. Place the tubing under the
laboratory hood with the vacuum on and allow to dry
thoroughly.
5.3 COHTJUKXRJ
5.3.1 Composite Jugs
Composite jugs should be cleaned in the same) parameter-
specific manner as the) tubing. "Dairy" jugs should be soap and
water washed, soeJcsd with soap and bleach for at least 24 hours,
soep and water washed again, and rinsed out thoroughly with OZ
water.
"Metal9 lugs should be acid washed with a 1:3 solution of
KNO3, and triple rinsed with ox water.
20
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5.3.2 Discrete Sampl« Bottles
Each set of discrete sample bottles consists of 28 500-ai
bottles which are to bm used when conducting sequential sampling.
These bottles should be acid-washed as outlined below:
1) Soap and water wash, followed by-a tap water rinse.
2) Rinse with a 1:1 solution of HN03/ followed by a triple
rinse with 01 water.
5.3.3 Saaple Containers
Saaple containers used for collecting metal saaples are
prepared by the laboratory according to standard methods. 2a.-/
and other biological saaples are collected in cubitainers, whicn
are rinsed with effluent prior to filling, and are disposed of
after use. Cyanide and organic saaples are collected in bottles
which are supplied and prepared by an outside laboratory.
21
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6.0 MAINTENANCE
6.1 ISCO SAMPLERS
Change desiccants weekly, or more frequently if needed (ISCO
Model 1680). The desiccant face should be blue. If the blue is
faded, or is turning to pink or white, it is time to Change the
desiccant. Unscrew the desiccant cartridge from the sampler and
replace the desiccant as discussed below:
1) Take the cartridges into the laboratory. Inside the
laboratory oven, there are two beakers with colored
desiccant. Using insulted gloves, take the beakers out
of the oven.
2) Unscrew the top of the cartridge and pour the old
desiccant into the least filled beaker. Pour fresh
desiccant into the cartridge, screw the top on, and put
the beakers, as well as the cartridge, back in the oven.
3) Remove the cartridge after the face is a rich blue color
(approximately 5 minutes), let it cool, and screw it back
into the sampler.
Other maintenance for the ISCO includes routine checks of the
base, head and cover for cracks, and checking/repairing the seal
on the control plate cover. The pump housing should be opened and
lubricated once a month, and the tubing checked for cracks. The
locks and cables should also be cleaned and lubricated to prevent
rusti ng.
6.2 FLOW METER
Flow meter desiccants also need to be changed weekly. There
are two plastic desiccant cartridges on the outside of the flow
meter, and one metal desiccant cartridge inside the cover.
Replacement metal cartridges are kept in the laboratory oven. The
whole cartridge should be replaced - DO NOT OPEN. The desiccant
from the exterior plastic cartridges should be emptied into the
least filled beaker from the laboratory oven and refilled with
fresh desiccant. DO NOT HEAT THE PLASTIC CARTRIDGES IN THE OVEN.
Place the cartridges back in the flow meter.
22
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6.3 BATTERIES
Batteries should be kept fully charged. The batteries should
be kept hooked up to the chargers when not in use. Return the
batteries to the chargers after each use. When a battery is
plugged into a charger, it should be labeled with the data and
time plugged in. Always use the batteries that have been charged
for the longest time first. Keep batteries clean and dry.
6.4 pH METER
There are two types of pH meters used: Orion and Corning.
The maintenance procedures for both meters are similar, but
cleaning procedures should be checked in the appropriate pH probe
manual prior to use.
The protective cap that comes with the pH electrode should be
kept filled with pH 7 buffer between measurements. The reference
buffer solutions in the field pH kit should be changed weekly.
The solution level in the pH probe should be maintained above
the internal element at all times. The fill solution should be
changed when erratic readings or slow response/stabilization is
observed. After being refilled, the electrode should be allowed
to soak in pH 7 buffer before being used again.
If the readings continue to be slow/erratic, the ceramic
junction may be clogged. This may be tested by wiping off the
electrode tip and observing it after an hour of air drying. A
failure of KC1 crystals to appear at the junction indicates a
clogged junction. If the junction is clogged, soak the pH probe
in a warm solution of Dl water. If the junction still does not
function properly, it must be replaced (Corning meter only).
Instructions for replacing the ceramic junction are presented in
the pH meter manual.
Another cause of slow/erratic readings is build-up on the
glass bulb or ceramic junction of the probe. This may cause
interference in the measurements. Check the pH probe manual for
proper cleaning solution depending upon the cause of the build-up.
23
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7.0 CALIBRATION
7.1 FLOW METER
The flow meter should be calibrated at the sampling site as
part of the setup activities. After programming the flow meter
(see setup instructions), there are two calibrations which must be
dons. The bubbler tube should be adjusted to put out one bubble
per second. The adjustment knob is located on the outside of the
flow meter, near the bubbler tube outlet. The water level should
also be checked and calibrated, if necessary. Set the meter
readout to level. Check the actual water level in the flume.
Adjust the flow meter level readout to match the actual water
level.
7.2 pH METER
The pH meter is calibrated once a week in the laboratory. The
pH meter is also calibrated in the field at each site, prior to
taking a pH reading. The procedure for calibrating the meter is
the same in the field and the laboratory, but the documentation
varies, and the buffers are replaced during the weekly laboratory
calibration.
7.2.1 Field Calibration
7.2.1.1 Corning pH meter
Rinse the pH probe and the thermometer with Dl water, and
shake the excess water off. Place the probe in buffer 7 and wait
for the readout to stabilities. At the same time, check the temp-
erature of the buffer, and adjust the pH meter temperature dial to
that temperature. Once the meter has stabilized, write down the
initial reading in the pH calibration log book. Also fill in the
date, time, location, and buffer temperature. Calibrate the meter
to 7.00 using the calibration dial, and record the reading in the
log book. Turn the meter off. Remove the probe and thermometer
and rinse with Dl water. Shake the excess water off. Place the
probe in buffer 4 or buffer 10 and allow to stabilize. Once the
meter stabilized has stabilized, write down the initial reading in the log
book. If the reading varies from 4.00 (or 10.00) by greater than
0.04, slope the meter to exactly 4.00 (or 10.00) using the small
screwdriver in the slope hole at the bottom of the meter. Record
the reading in the log book. If sloping was necessary, rinse off
the probe and recheck the meter with buffer 7 as above, to be sure
that the calibration held. If it did not, repeat the procedures
above until the meter returns to 7.00 (±0.02).
24
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7.2.1.3 Orion pH meter
At the beginning of each day, an overall meter check should be
performed. With the shorting plug in, and no probes attached,
turn the meter on with the "type of measurement" selector in the
mV position. mV should read 0. How the selector to Temperature,
and check that it is reading 25.0. If not, use the scroll button
to correct the temperature and press Enter. Move the selector to
pH 0.01. Press ISO, and check that the reading is 7.00. if not,
correct as above and press Enter. Press the Slope button and
check that the reading is 100. Correct as necessary. Press the
Sample button and check that pH is reading 7.00 ±0.05. Correct as
necessary. The meter is now ready for calibration.
Rinse the pH and temperature probes with Dl water, and shake
the excess water off. Place the probes in buffer 7. Move the
selector to pH .01. Turn the pH motor on, and press the "ISO"
button. The readout should show 7.00. Press the "CAL" button.
The readout will flash from ".1." to the pH value. Wait for the
readout to stabilize. Once the meter has stabilized, write down
the initial reading in the pH calibration log book. Press the
Enter button, and record the pH that the meter is calibrated to.
Also fill in the data, time, and location. Remove the probes and
rinse with Dl water. Shake the excess water off. Place the
probes in buffer 4 or buffer 10 and allow to stabilize. The
readout will flash from ".2." to the pH value. Once the meter has
stabilized, write down the initial reading in the log book. Press
the Enter button, and record the sloped value in the log book. If
buffer 4 or 10 were off by more than 0.1, rinse off the probes and
recheck the meter with buffer 7 as above, to be sure that the
calibration held. If it did not, repeat the procedures above
until the meter returns to the calibrated value for buffer 7.00 (±
0.02). Move the selector to temperature, and record the buffer
temperature in the log book.
7.2.2 Laboratory Calibration
Get the pH/Standard Calibration Check Sheet. Change the
buffers in the field pH meter kit and mark the Check Sheet
accordingly. Replace the internal fill solution in the pH probe.
Calibrate the field pH meter as described above, logging the
information onto the Check Sheet. This laboratory calibration
should be done once a week, and/or before each sampling round to
verify the accuracy and operation of the pH meter. Once a month,
a pH sample with a known value is measured with each pH meter.
This chock confirms that the pH meter is functioning properly at
pH values other than the buffers.
25
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8.0 SAMPLING PREPARATION
Sampling preparation is the most important part of a
successful sampling event. Careful attention must be given to
both equipment and handling in order to collect a valid sample.
Sampling site(s) and type(s) of samples will determine the
equipment needed and the method of collection. Standard sampling
checklists are included as Tables 1 and 2. Sampling preparation
procedures are as follows:
Day before the sampling round:
1) Go over the sample checklist and the site specific data
sheet to determine what will be used for each site.
2) Check the van to make sure it is properly stocked. Load
into the van:
-Properly cleaned ISCO samplers, site specific tubing
and composite jug/sequential bottles;
-Site specific equipment;
-Proper sample containers (metals, cyanides,
cubitainers, etc.); and
-Flow meters, if needed.
3) Change the buffers and calibrated the pH meter.
Day of the sampling round:
Load into the van:
-Charged batteries, one for each ISCO plus a backup,
-Ice for ISCO bases (approx. 1/2 cooler per sampler),
-Ice to chill samples (if picking up samples that
day).
26
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TABLE 1
DAIRY SAMPLING CHECKLIST
Data:
Sites to be sampled:
ISCO Sampler(s) #
battery(s) #
desiccant(s) in good condition
site specific tubing with weights
12 liter composite container(s) (dairy)
ISCO Flow Meter(s) #
battery(s) #
desiccant(s) in good condition
program box
pH meter calibrated w/fresh buffer
coo ler(s) w/ice #
cubitainers for samples #
Dl water (lowboy)
latex gloves
Sulfuric acid (for acid kit)
field data sheets
field notebook
grab sampler
ISCO stand
camera with film
27
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TABLE 2
METAL/CYANIDE SAMPLING CHECKLIST
Data:
Sitaa to be stapled:
.ISCO Saapler (coapoaita or diacrete) I
.battery (a) I
_deesicant(a) in good condition •
.actuator* I
.•ita apacific tubing
.aerving piata baa*
.diacrata bottlaa (glaaa or plaatic) I
.12 lltar coapoeite containar(a) (acid-washed)
.ISCO flov Katar(a) I
_batt«ry(«) I
.daaaicajit(a) in good condition
program box
^ matar calibrated w/fraah buffar
_DI vatar for blanks
_coolar(a) w/ica *
_acid-waahad bottla(a) for blanks t
_«cid-waahad bottla(a) for aaaplas I
_DI vatar (lowboy)
.latax glovaa
.Nitric acid (for acid kit)
_fiald d*t* ahMta
.fiald notebook
.grab aaxplar
.I9CO at*nd
.camarm with film
.cyanidav kit (a) *
sites to b« tested!
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9.0 TYPES OF SAMPLES/METHODOLOGY
There are two basic types of samples: grab and composite.
The method of collection is determined by flow, sampling location
and analyses to be performed. Obtaining a representative sample
should be of major concern.
9.1 GRAB SAMPLES
A grab sample is defined as "an individual sample collected
over a period of time not exceeding 15 minutes". A grab sample is
collected when:
1) Setting up a sampler is not feasible due to flow or site
arrangement.
2) There is unusual flow of short duration.
3) The flow is not continuous (batch discharge).
4) Waste characteristics are relatively constant.
5) Analytical parameters require a grab sample: i.e.,
pH, cyanide, organics, oil and grease, sulfides,
temperature, and residual chlorine.
A grab sample can be taken either manually or with an
automatic sampler. To obtain a manual grab sample; a clean grab
container, sample container, and a sampling pole are needed. The
grab and sample containers must be properly cleaned according to
test specifications. The grab container is attached to the pole
and lowered into the wastestream. The sample container is then
rinsed with the effluent to be sampled. This is known as
"seeding". The container is then filled with effluent. Several
grabs might be needed to fill the sample container completely. It
is important to remember that in order for a sample to be
considered a grab, it must be collected within a 15 minute time
frame.
An automatic sampler is used to obtain a grab sample where
pipes or "cleanouts" are used as sampling sites. In most cases,
the diameter of the pipe prevents easy access, allowing only a
tube to be placed into the flow. To obtain a grab sample in this
manner, follow procedures for obtaining a pH grab sample for a
24-hour composite with an automatic sampler. See Section 11 for
instructions on setting up the equipment.
19
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9.2 COMPOSITE SAMPLES
A composite sample is made up of a number of individual grab
samples which are combined based on either time or flow. A time
composite sample consists of equal volume grab samples collected
at equal time intervals. A flow composite sample may consist Of
equal volume grab samples taken at varying time intervals; samples
of variable volume ( in proportion to flow) collected at equal time
intervals; or one sample continuously collected proportional to
flow. A composite sample is taken when:
1) Determining average pollutant concentrations during the
compositing period.
2) Calculating mass/unit time loadings.
The use of an automatic sampler with a composite base
simplifies implementing this type of collection. In the event of
a timed composite, the sampler can be programmed with the desired
time interval. For a flow proportional composite, a flow meter
can be used in conjunction with the sampler (provided that the
sampling site is constructed for this type of sampling). In the
event of industrial batch discharges at varying time intervals, an
actuator should be used. See Section 11 for instructions on
ratting up the equipment.
If an automatic sampler is not available, grab samples can be
collected and manually composited. (NOTE; IN ANY MANUAL
COMPOSITING METHOD. SAMPLE MANIPULATION SHOULD BE MINIMIZED TO
REDUCE THE POSSIBILITY OF CONTAMINATION).
A second type of compositing is known as "sequential"
sampling. This type of compositing consists of a series of
individual grab samples collected into different bottles. The
ISCO sequential base holds 28 500-ml bottles. Depending on sample
volume, from one to four grab samples can be composited into each
of the bottles, at time intervals programmed into the sampler.
This type of sampling is valuable in isolating discharge values
that may vary over a period of time or from one batch discharge to
another. It is also useful in situations where chemical
constituents at a particular time are of interest.
If sequential sampling is to be done manually, procedures for
grab sampling can be followed. An automatic sampler may also be
used with a sequential base (ISCO Model 1680 only). See Section
11 for instructions on setting up the equipment.
30
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10.0 FIELD ANALYSES
Two types of measurements are routinely performed in the
field: pH and temperature. These tests are dorm in conjunction
with one another on the initial and final grabs, and on the
composite sample during the 24-hour composite sampling event.
The pH and temperature are also measured on a portion of the grab
sample during a grab sampling event. Other analyses may be
conducted in the field for special investigations/projects.
These analyses are performed using a Hach portable laboratory.
During composite sampling, the "pH grab" is usually collected
in a graduated cylinder at the beginning and end of the sampling
want. The cylinder should be rinsed out three times with Dl
water, and then seeded with effluent before collecting the pH
grab. The pH can then be measured directly from the cylinder.
The pH of a grab sample is measured off of a separate portion
of the sample. The grab container should be seeded with effluent
before being used to fill the sample container; the sample
container should also be seeded with effluent before filling. The
sample container should be filled to the top, and then a portion
of the sample should be poured into a separate 25-ml container for
pH measurement. The cylinder or pH container should be rinsed out
three times with Dl water after the pH grab is analyzed and
disposed of.
The pH meters used in the field are stored in cases which
contain the following supplies:
1) 1 pH meter.
2) 1 pH probe.
3) 1 thermometer or temperature probe.
4) Buffers - 4, 7 and 10.
5) 1 slope adjustment screwdriver (Corning only).
6) A supply of paper towels.
To obtain a pH measurement, the following procedures are used
1) Connect the probe(s) to the meter.
2) Remove the cap from the pH probe; rinse the probe and the
thermometer (or temperature probe) with Dl water.
3) Calibrate the meter following instructions in Section 11.
31
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4) After meter calibration, rinse the pH probe and the
thermometer/temperature probe with Dl water and place in
the sample solution.
5) Turn the meter on to start stabilization; read the
thermometer and make the temperature adjustment (Corning
only). Record the temperature on the Field Data Record.
When using the Orion meter, it is generally faster to
check the pH first, and check the temperature afterwards
(switch steps 5 and 6).
6) Let the pH reading stabilize; remember to periodically
stir the sample with the probe. Record the results on
the Field Data Record.
7) If the pH value is out of compliance, recheck the buffer
7 solution to verify proper calibration.
8) Rinse the pH probe and the thermometer/temperature probe
with Dl water and store properly.
9) Pour the pH sample back into the wastestream, unless the
pH value is out of compliance. If the pH value is out of
compliance, take the sample in to the laboratory/contact
person so that they may check the pH value themselves.
32
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11.0 EQUIPMENT SETUP
11.1 ACTUATOR
At some sitar where there is intermittent flow, it may be
advisable to use an actuator. The actuator has an open electronic
circuit, which is "closed" by the water when there is flow. When
the circuit closes, it sends a signal to the sampler to collect a
sample. Once the programmed time interval between samples passes,
the ISCO is in the "ready" position and waits for a signal from
the actuator. If there is flow at that time, the circuit will be
closed; a signal will be sent and a sample will be collected. I f
there is no flow, the ISCO will remain in the "ready" position
Until the actuator circuit is again closed by the recurrence of
flow. To use the actuator:
1) Connect the actuator and the sampling hose to a firm
support (such as a short piece of PVC pipe) so that the
end of the actuator is resting on the bottom of the
manhole or flume floor in a vertical position. Be sure
the hole in the aids of the plastic cap at the and of the
actuator is not covered and is open in the direction
affluent flow will be coming from (facing upstream). The
tubing should be positioned so that the end of the tubing
is slightly above the floor (about 1/4-inch).
2) Attach the actuator to the battery by putting the control
box clamp over the top of the battery and pressing down
firmly until it clamps on.
3) Set the switch on the actuator control block to
"Toggle/Reset".
4) Set the ISCO switch to time (not flow).
5) Plug the actuator into the flow meter rocket on the ISCO
head next to the battery socket; you are ready to start
sampling or proceed with the ISCO setup.
11.2 FLOW METER
The settings on the ISCO flow meter will vary with site
characteristics. Be sure you have the programming data for your
site, or the flow meter manual which has all the program settings.
33
-------
Settings for sites which we currently monitor using a flow meter
are listed in front of the Flow Meter Calibration Log. To set up
the flow motor:
1) Hook up the battery.
2) Hook up the bubbler tube.
3) Set the program disk by inputting the device number
(based on width of flume and maximum expected depth of
flow) and the scaling constant (determined by the device
number). Use the scaling constant for gallons per
minute. The scaling constant equals, the flow at the
maximum expected depth, and is expressed in the format
"#.##". If the maximum flow is greater than 9.99 or less
than 1.00, an exponent will be included in the scaling
constant (i.e., #.## ± 1).
4 ) Place the program disk into the flow meter.
5 ) Turn the flow meter on.
6 ) Adjust the bubble rate from the bubbler tube to one
bubble per second.
7 ) Adjust/calibrate the flow level. Set the meter readout
to level. Measure the actual flow level. Unlock the
calibration knob and adjust the level on the readout to
match the actual flow level. Relock the calibration
knob.
8 ) Set the recorder mode/span. This determine the span
(total level variation) that will show up on the recorder
paper. Generally, you want the average flow level to be
near the center of the page.
9 ) Set the flow meter to purge every 60 minutes, except in a
flow with lots of fats or solids, than set it for 30
minutes. "Purge" causes a burst of air to be blown out
through the bubbler tube, thereby clearing any
obstructions from the and of the bubbler tube.
10) The sampler initiation signal sends a signal a to the ISCO
for way 10, 100, or 1000 gallons oi effluent that flow
part the bubbler tube. The ISCO will be set to take a
sample after it receives a certain number of signals.
For example, the flow meter signals every 10
34
-------
gallons, and th« ISCO saaplas avary 10 signals, aqjualir.g
one sampla avary 100 gallons, or it can signal avary ICO
gallons and sample avary signal aquallng ona saapla avary
100 gallons. If thara is an axponant in tha scaling
constant (V) / multiply/divide tha saapler initiation
signal by that axponant. For axaaple, if thara is an
axponant of +1, satting tha saaplar initiation signal at
10 will rasult in a signal baing sant avary 100 gallons.
Tha flow raading on tha total flow dial is also to ba
multipliad/dividad by tha axponant in tha scaling
constant.
11) Sat tha chart spaad at ona inch par hour.
12) On tha display knob, tha bottom satting is calibrata
racordar 0. This will mova your racordar pan to tha
bottom of tha paga. Manually mova tha papar and saa
where tha pan writas. If it is not on tha 0 lina,
unscrew thai knob holding tha pan and adjust tha pan's
position up or down. Recheck this until tha pan linas up
avanly on 0. RalocJc tha knob holding tha pan. Reset tha
display Knob to laval.
13) Boole up tha connact cabla to tha flow matar and to tha
ISCO saaplar.
11.3 WATZX XTTZM
Watar attars ara usad to aatiaata tha flow at facilitias whare
effluent flow aaasuramant is not practical or possibla. Flow data
is necessary in ordar to calculata contaminant/organic loading
based on measured concentrations; this data is than usad as a
basis for surcharge fees, aaas balance eolations, and/or tha
combined wastestream formula.
Hater meter readings should be taken as close as poasibla to
the samei time) each day so aa to ba raprssentative of a 24-hour
period. imeaUafS may also be taken at the beginning and and of
the montsswos* monthly average and total flows, or at the beginning
and end •£ a* sampling period of variable duration (i.e.,
operatioassv.boors, only) for special loading studiee.
Therm arm- two types of watar maters which may be encountartd
in the field. One type usaa a sarias of dials, while the othar
has e digital readout with tha Last digit(s) being determined by
single exterior dial. The numbar of fixed O's at the and of t.w.a
digital readout indicates tha value of the exterior dial (1, :a.
-------
100) . Figure 1 illuatratea theae two types of meters. It is
important to taJca accurate readings. Whan a valua is about to
change, it may appaar to ba the highar valua, vhlia it is actually
naar tha top of tha lovar valua. For example, on a digital
raadout, tha "4" in "49" may appaar to ba a "5" bacausa tha "4"
has almost rollad up and tha "5" is almost in its nav position.
Tharafora, meters should ba raad from right to Laft, or lowast to
hlghast placamant, ao that tha valua of tha lovar digit may give
an indication of tha valua of tha highar digit. Anothar
considaration vhan raading a multiple-dial matar is which dial is
"first", or "lowast". This dial will ba marked in soma way, and
will ganarally ba moving at a fastar rata than tha othars.
11.4 GRAB SAMPLER
Grab samplaa may ba collactad manually or by using an ISCO
sampler. Tha manual aamplar ia a pola with two clampa usad to
hold tha collection bottla. Placa tha coll act ion bottle in tha
clamp a, and tighten until anug. Dip the bottle into the flow,
facing upstream, and rinse (or seed) it several times with
affluent. Redip the collection bottle and pour the effluent
collected into your sample container. Seed the aample container
with this effluent, and then continue to collect grabs until tha
sample bottle is full. When collecting grab samples from a
holding tank (as opposed to a stream-flow) , follow the same
procedures as above, except that tha collection bottle should ba
dipped into the flov upside down and then turned so as to collact
affluent from belov the surface. Depending upon the size and
characteristics of the tank, it may be necessary to use graba from
several different locations and depths of the tank in order to
obtain a representative sample.
NOTl: x caxm ajm*r.» MAY «* coT.T.»rr*Tj nv»f. A proton or TTM»
OP
when collecting a grab sample with the ISCO, connect properly
cleaned tubing to the sampler, and then turn the ISCO to
"Forward0. Pump enough effluent through the ISCO to fill the
sample bottle-, rinse the bottla with this affluent, and then
refill the sample container. Turn the ISCO to "Reverse" to purge
the line when you are finiahad sampling.
-------
y
900
•00
1000
100
200
700
300
600
400 y
500
FIGURE 1. WATCH METZKJ
37
-------
11.3 ISCO SAMPLER
The ISCO is an automatic sampler composed of a base, which
holds the sample collection container(») and ice; the head, which
is the control unit; and a cover to help keep the h«ad dry. It
operatae by utilizing a peristaltic pump to draw effluent up
through a length of tubing extending from the ISCO to the flow,
and discharges this effluent into the collection container(«) in
the base of the ISCO. The ISCO is designed to collect two typ«s
of samples: composite and sequential. Sequential samples can
only be collected with ISCO Model 1610.
For composite samples, ISCO Model 1610 uses a discharge tube
that extends to the middle of the heed so as to discharge to a
container with a center opening. Por sequential sampling, a short
discharge tube is used to feed the sample into the appropriate
discrete container through a distribution funnel (see Sequential
Sampling). Glass discharge tubes are used when collecting metal
or organic samples. To set up an ISCO sampler:
1) Open the manhole, flume, cleanout cap, etc. to access the
flow following the procedures outlined in Section 4
(Opening manholes/flumes).
2) Attach a battery to the ISCO.
3) Attach the site specific tubing.
4) If collecting metal or organic samples, run some 01 water
through the tubing and rinse the sample blank container:
then collect a OZ water blank.
5) Set up the actuator or flow meter, if necessary, but do
not connect thai cable to the ISCO.
«) Lower the tubing into the flow, setting it up with a
weight or pel* as necessary.
7) S«% thai ISCO controls for the tubing length and diameter
(3/t or 1/4-inch).
I) Set the ZflOO controls for the desired volume to be
collected at the appropriate head feet for the site.
9) Por ISCO Model 1«SO, put the sampler on "Auto", set the
time interval to next sample to "000*, and collect a
"measured grab". Por Model 2710, press Manual Sample.
This will allow you to see how much volume will be
33
-------
collected with each grab. If the volume is higher or
lower than you wish to collect, reset the volume and/or
head feet and collect another measured grab until you
collect the desired volume.
10) collact another grab (approximately 400 ml) in the
graduated cylinder to use for pH analysis.
11.5.1 Composite Samples
For composite sampling, a long discharge tube should be used
vita a piece of polyethylene tubing attached to the end (Model
1680) . The tall base, ZSCO head and cover are used.
11) Place the composite jug (with lid on) in the base and
pack with ice; remove the lid from the jug.
12) Put the ZSCO heed on the base, making sure the discharge
tube feeds into the composite jug.
13) Set the toggle switch to disable (Model 1610 only) .
14) Set the interval to next sample at "2" or "3*, then set
the time setting to the desired composite time interval
(15, 20 or 30 minutes) or the number of signals if usi.-.g
a flow meter.
15) Lock the ZSCO, and position it where it will remain for
the composite duration (suspended in the manhole, lowere
into the flume, or located away froa traffic/ activity
areas) .
MOTZ: «• «tJ*£ Vnn QMrnv» TH»
11.5.2 Sequential Staples
For MqosoitiAl sampling, you must use ZSCO Model 1610. A
short diaeharge) tub* should be used with no tubing attached.
distribution funnel should be attached to the bottom of the
using the center bolt to hold it in place. The black serving
plate (with 2i hole* in it) should be placed over the bottles
the base.
11) Use the shorter "discrete1* base that has 28 bottles w
are held in place by a stainless steel metal circle.
-------
12) Pack tha cantar of tha discrata baa* with ica; rsmova th*
lida from tha bottlaa.
13) Sat tha toggla switch to normal or anabla.
14) Hold tha manual advanca button on tha ZSCO until tha word
'•Standby" appaars in tha small hola in tha baaa of tha
ISCO haad, than prass manual advanca again ona tima so
that tha numbar "I1* appaars in tha hola.
15) Put tha ISCO haad on tha baaa.
16) Sat tha aviteh for numbar of bottlaa par aampla, or
numbar of aaaplaa par bottla aa appropriata for tha
sampling raquiramanta .
17) sat tha intarval to naxt sampla at "2" or "3", than
changa tha tima satting to tha daairad tima intarval or
numbar of flow aignala.
It) Lock tha ISCO, and position it vhara it will remain for
tha sampling duration (suspandad in tha manhola, lowarad
into tha flumaj, or locatad away from traffic/ activity
araaa) .
NOTIt «« *UP» KOU 0»«mv* TH»
TH*
40
-------
12.0 INDUSTRIAL VAN MAINTENANCE AND SUPPLY
12.1 MAINTENANCE
The industrial van is serviced by Pinellas County Fleet
Maintenance (PCFM) every six months or 5000 miles, whichever comes
first. PCFM does a complete vehicle inspection, and changes
fluids and filters, as necessary. The industrial van is also
taken to PCFM for repair if the drivers' routine checks indicate
any problems. The van is checked by the drivers for fluid level,
tire pressure, light and horn function, and proper operation on a
routine basis. The Vehicle Maintenance Schedule is included as
Form 3. Per trip mileage is also recorded and turned in monthly.
12.2 SUPPLY
The industrial van is kept stocked with the supplies and
equipment that are commonly used or that may be necessary in an
emergency. These supplies include: first aid and safety equip-
ment, at least one sampler, sampling accessories, miscellaneous
tools, paperwork, Dl water and disinfectants. The complete van
inventory checklist is included as Table 3. Many of the items on
the list are kept in the van at all times, others are depletable
(i.e., gloves, Dl water). The van is checked and restocked, as
necessary, at the end of each sampling rum and/or prior to going
out in the field.
4 1
-------
FORM 3
VEHICLE MAINTENANCE SCHEDULE
INSPECTION ITEM JAN FEB MAR APR MAY JUN JUL AUG SEP OCT NOV DEC
FLUIDS:
OIL
STEERING
BATTERY
TRANSMISSION
RADIATOR
WIPER
LIGHTS:
HEADLIGHTS
TAIL LIGHTS
BRAKE LIGHTS
TURN SIGNALS
HAZARD LIGHTS
TIRES:
AIR PRESSURE
TREAD/APPEARANCE
OPERATION:
HORN
BRAKES
WIPERS
TRANSMISSION
OTHER:
NOTE: Check off items inspected; use an asterisk(*) to indicate items
needing repair. Report any needed repairs immediately.
vehicle: 881221
42
-------
TABLE 3
INDUSTRIAL *rAN INVENTORY CHECKLIST
.acid praservation kit
.acid-washed tubing
.actuator
alcohol
.as-built»
.battery booster cable
.batteries for pH meter
.bubbler tubing
.buckets
.calibration log books (flow meter, pa meter)
.claape and ZSCO hardware
.cubitainera
,01 water for 9 gallon container
.extension cord*
flashlight
.flow meter connector cablee
flow meter manual
flow meter auppliee (paper/pene)
flume depth measurer
foot pump
.graduated cylinder
.hand wash
.incident documentation log
industrial sampling sheets
.inflatable line blocker
,ISCO SAMPLZK (1)
.ladder (20 ft. extension)
.latex gloves
.manhole hook
.manhole «pid«n (2)
.metal sampling bottle*
.mileage sheets)
iso. bottle*
ise. paperwork (accident forme, etc.)
?ape» towels
and ball point pens
.rope>
.strainers and weights
.suspension cables
.taps (electrical, filaaant, fluoreecent, masking)
.thermometers
.tool box
.volatile organic bottlae
.volt-oha meter
.work gloves
43
-------
Appendix X
Example Sample Tag and Chain-of-Custody Form for Use by POTWs
-------
NPDES Compliance Monitoring Inspector Training: SAMPLING
EXAMPLE SAMPLE TAG
ENVIRONMENTAL PROTECTION AGENCY
OFFICE OF ENFORCEMENT
NATIONAL ENFORCEMENT INVESTIGATIONS CENTER
BUILDING 53, BOX 25227, DENVER FEDERAL CENTER
DENVER, COLORADO 80025
\y
EPA
Project Code Station No.
Station Location
MoVDay/Year
Time
Samplers: (Signature)
Designate:
Comp. Grab
Remarks:
Q)
CT
CO
01
CO £
§1
I!
" £
<*
Pes
7 9 2 £
5
g *
_ a
8 9
CO =
o> £. u
3 5» 5>
a i 5
0)
o
O 5
O Q)
•< » «
0) ** -^
3 ?>. O 2
a c g
TJ O CO CO
2" O 2L O
* o a; o
-------
United States 3. Sample Number 5. Task Number
Environmental Protection
Agency
4. Inspection Number
Chain-of-Custody Form
1. Inspector Name and Address 6. Sample Description
7. Sample Date 8. Sample Time 9. Duplicate Requested?
( )Yes ( )No
2. Inspector Signature 10. Sample Location
11. Analysis/Testing Required
Laboratory
Date Received
Received By
Sent Via
Sample Condition
Condition of Seals
Units Received
Storage Location
Assigned By
Assigned To
Delivered By
Date Delivered
Number of Units Received
Units Analyzed
Date Seal Broken
Date Received
Resealed By
Storage Location
Date Results of Analysis
Issued to the POTW
Remarks:
-------
Instructions for the Use of the Example Chain-of-Custody Form
1. Enter the Inpsector's Name and POTW's (or the POTW's office) address.
2. Sign the Chain-of-Custody Record Form.
3 & 4. Each inspection and sampling event should he identified with a unique number to track the information
from the inspection.
5. Task numbers are used when the POTW uses contractors to perform inspections. Inspectors may
disregard this space.
6. Describe the sample, including: si/e, container, contents (e.g., 8 oz. bottle of electroplating effluent).
7 & 8. List the date (7) and time (8) the sample was taken at the facility.
9. Indicate if duplicate (or splits) were performed al the time of sampling.
10. Enter the name and address of the facility and the sample location identification number.
11. List all required analytic tests (e.g., Cd, Cr, Ni, and Zn testing).
-------
Appendix XI
List of Regional Pretreatment Coordinators
-------
Regional Pretreatment Coordinators
REGION I
(CT. ME. MA. NH. RI. & VT)
Mark SpinaU (WCM-2103)
U.S. EPA - Region I
JFK Federal Building
Boston, MA 02203
Phone: (617) 565-3554
Fax: (617) 565^940
REGION II
(NJ. NY. Puerto Rico & VI)
Virginia Wong (2WM-WPC)
U.S. EPA - Region II
26 Federal Plaza, Room 825
New York, NY 10278
Phone: (212) 264-1262
Fax: (212) 264-9597
REGION m
(DE. DC. MD. PA. VA. & WV)
John LovtU (3WM-52)
U.S. EPA - Region III
841 Chestnut Street
Philadelphia, PA 19107
Phone: (215) 597-6279
Fax: (215) 597-3359
REGION IV
(AL.FL.GA.KY.MS.NC.SC.&TN)
Al Herndon (FPB-3)
U.S. EPA - Region IV
345 Courtland Street, N.E.
Atlanta, GA 30365
Phone: (404) 347-3973
Fax: (404)347-1797
REGION V
(IL. IN. Ml. MN.OH. &WI)
MattGtuckman (5 WQP-16J)
Implementation Coordinator
U.S. EP A-Region V
77 W. Jackson Blvd.
Chicago, IL 60604
Phone: (312)886-6089
Fax: (312) 886-7804
Mike Mikulka (WCC-15J)
Enforcement Coordinator
U.S. EPA - Region V (WCC-15J)
77 W. Jackson Blvd.
Chicago, IL 60604
Phone: (312) 886-6760
Fax: (312)886-7804
REGION VI
(AR. LA. NM. OK.
-------
Appendix XII
List of Available Pretreatment Guidance Documents
-------
This appendix provides a comprehensive list of documents available from the U.S.
EPA. To obtain any of these documents, please contact either of the following references:
U.S. EPA Water Resources Center
(202) 260-7786
Please reference the EPA Identification Number provided in the following
table when ordering through the Water Resources Center.
The National Technical Information Service
U.S. Department of Commerce
5285 Port Royal Rd.
Springfield, VA 22161
(800) 553-6847
Please reference the NTIS number provided in the following table when
ordering through NTIS.
Document Safes Desk: (703) 487-4650
General Information: (703) 487-4600
Customer Services: (703) 487-4660
Document Identification: (703) 487-4780
-------
Title
1 Guidance la Protect POTW Woricers From Toilc and Reactive Gases and Vapors
Model Prrtrf4tmoil
NtitiOMl PretreAtmnt Program - Report le Cmfftu (519 R/port)
Control of si^) Lodjiln^ la POTWs - Guiiincf \MniwI
Suyylmntal Manual on ike Develofmenl tiul \mplmmMim of Loc«l
PRELIM Vrrsfon 4.0 Uxrs Gkliie
Guidance Manual for pOTWs to Calculate ttif Economic Btncftt of Uoncompliancc
limiUlions Uider ike prdrttilmnl Program
8 industrial User pernittitifl Guidance Manual
9 Aluminum, Coffer, and Nonienou Mclals Forming and Melal Ponders Prelriealmenl Standards
10 Guidance for Develffinfl Control Authority Enforcement Rtifonse Plans
1 1 Guidance Manual for Preventing interference at POTWs
12 Guidaict Manual for Zattery MjUiufiictiiriiifl Prelrealmenl Standard!.
13 Guidance Manual on l\\e Developnenl and Imflemenlion of local Discharge limits Under the Pretreatment Program
14 Guidance Manual for the identification of Hazardous Wastes Delivered to POTWs In Truclr, Rail, or Otilcaltd PifC
15 Environmental Rr^nlntuw and Technology - The Haliona! Prelreatment program
16 Guidance Manual for leathr Tanning and Finishing PrrtrMtmoit Standards
17 Guidance Manual for the Use of Production-Based Standards and the Combined Wasiestream Formula
18 Guidance Manual for iron and Sled Manufacturing Pretrtalmenl Standards
19 RCRA Information on Hazardous Wastes for PkiWv Owned Treatment Works
ID Guidance Manual for pr^riitum and Revm ft Removal Credit Ayflications
2! Guidance Manual for Implementing the Total Toxic Orgies ITTO) Prelrtalment Standard
22 Guidance Miinkdl tor Electroplating and Metal finishing pretrcalment Slankirds
23 Guidance Manual tor nly, Paper, ,ind rape^oard and ZuiUr's Tapir and Board MiUs Prelreatment Standards
24 Procedures Manual tor Reviewing ,1 POTW pretreatmenl Program submission
Year
1992
1992
1991
1991
1991
1991
1990
1989
1989
1989
1987
1987
1987
1987
1986
1986
1985
1985
1985
I<>85
1985
1^84
1984
1983
EPA Document it
EPA 812/B-92/OOJ
EPA 833/B-92/003
EPA 505/2-91/001
EPA 21W-4O01
EPA 2IW-4OO2
EPA 21 W-4003
EPA 833/B-89/001
EPA83J/B-89/2O1
EPA 833/B-89/2OI
EPA 833/5-87/200
EPA 833/B-87-2O2
EPA 625/ I 0-86/005
EPA 833/B-85/201
EPA 833/B-85/2O2
tTA 83i/B-85/200
EPA 44O/I -85 /009.M
PB93- 209-880
-------
Appendix XIII
40 CFR Part 136 - Tables IA, IB, 1C, ID, IE and II
-------
§ 136.3
§ 136.3 Identification of test proce-
dures.
(a) Parameters or pollutants, for
which methods are approved, are listed
together with test procedure descrip-
tions and references in Tables IA, IB,
1C, ID, and IE. The full text of the ref-
erenced test procedures are incor-
porated by reference into Tables IA, IB,
1C, ID, and IE, The references and the
sources from which they are available
are given in paragraph (b) of this sec-
tion. These test procedures are incor-
porated as they exist on the day of ap-
proval and a notice of any change in
these test procedures will be published
In the FEDERAL REGISTER. The dis-
charge parameter values for which re-
ports am required must be determined
40 CFR Ch. 1(7-1-93 Edition)
by one of the standard analytical test
procedures incorporated by reference
and described in Tables IA, IB, 1C, ID,
and IE, or by any alternate test proce-
dure which has been approved by the
Administrator under the provisions of
paragraph (d) of this section and §§ 136.4
and 136.5 of this part 136. Under certain
circumstances (§ 136.3 (b) or (c) or 40
CFR 401.13) other test procedures may
be used that may be more advan-
tageous when ouch other test proce-
dures have been previously approved by
the Regional Administrator of the Re-
gion in which the discharge will occur,
and providing the Director of the State
in which such discharge will occur doer
not object to the use of such alternate
test procedure.
Environmental Protection Agency
TABLE IA. - LIST OF APPROVED BIOLOGICAL TEST PROCEDURES
314
3 1 5
-------
TABLE 1B.—Itsror
APWWVED INOHOAMC TEST Pnoceoufcs—CondnuBd
ABTM UBQ8'
OMhod No. or MB*)
17* Ed.
OMr
11. Bramid*. mgA;
12. Cadmunv—ToM*. moA;
AA dtr*d MpMMn * ..
OC*»
320.1
M3.1 2111 B or C.
»13J 31138
. '200,7 .._ 2120 B
D12*6-«O (1M) .
OBH7-BO (A or B) ...
M126-66 p.B44.«
1-313S-BS or t-3136-
Bt.
wa£jii"l~~~~.
3667-BOC.
OCP. or
TMnutt (EOT A)
U. Cite-'~~iout
215.1 3111 B ....".." »
a00.7» 3120 B _ .._
06M-«Bj. MB*.' 0
216J 3BOO-C*. D
•210 B -
MOM 34.
MOM 34.
16. Own
V
16 CNond*. mgA-
TfcrMMnc (•***
or (Mvcurtc r*raM). or
CotorMMnc. mdnuct or ..
4iai ..._
4102 «
410.3 ....
410.4
(220 B
1-3660 or ._ V73.46I p. 17»
13 or 14.
1-3661-16 .
17. CMorin*—TaM rwjduM. mpA. TMnMrtc
OTBVC^ end point 0fBci — — ~ _ _...™.._,
Back «n«on MMT «nd port •>. or" u u u ".
If L«^XA«iT / L. DPO " " — 1..._.".". —„..
16. Orannum VI itmti M. inpl\_ 0.46 mkran iiraion Mn»»j by
326J
326.1 or 328.2
330.1 ....»
330 J ».».
4800-06
4800-OC .
I.. M12-BKB1
..". 0612-tBIA)
. . 0612-BXC)
M1BV46 .
l-1164-BS .
M167-4V .
>-21l7-«6 .
S30J
330^'
4600-OD . . . .
4600-O B
4600-OC _..
4600-O 0 '„„
D1263-7BIB) (1BH)
2111 A._..
II. OiroMum-ToM*. ntgV; dtoMon* WtoMd by
AAtfnMl
AA J»-
M232-t6 .
M230-46 .
DCP». or
V<*«m*try".or
211.1 2111 B 01tt7-BKO)
211X3 3111 c ,
21tv2 3112B
•aOO.7 3120 B
D41IO-BI
09667-WC
MM 16.
307B."
•I74J7
MOM 34.
- V
AA IWIMO* _________________________________ ...... - ......
ICP. or ................... _ ........ - ........ _________ ........ - ........ _ ........ .
21 Color pMrttfti ratal i**» or doMMM »«.|««nq». lu*.
3600-Cr 0
21t.lorC 3111 B (A or B)
jjjj 3113B
200.7* 3120B
01BT-B«4A)
D41K-BI
ColarimMrtc (AOM1. or
(PMVHfn Cflb^O.or""...."!."
V 4v»*v*w«rArV ...... - ....... «.
22. Copp«r— ToM*. maA. OpMlon'
1101
1102 ~~
2120 E
2120 B
tijOC
MHO-BS
p. 37..
MBK16.
_. SlIIBorC 01BBKBO IA or B) _. »-»»7O-B» or I-SI71- >f74J7 * D 37
»A lumao*
OCP««. or ___________
ColorttK«rle (t*oa#no(r»), or
•2B0.7
3U3 B
3120 B
3600-CwO
D41IO-BI
23. Oye»Hd» -ToM.
CO
to oMortnflbton. npyi^
•» M0O,
by •MMMc or 336.1
4600-CN-C
4800-04-0
4600-CN-i
4600-CN-O.
M03B-BKA)
(-4100-M
No»34.
OS it.
P.B.*
26. BuortO* ToM. moA.
krkraj«dMMk>r«t<
EKCMO*. nvnuri or
3402 .
4600-F-C
D117KBWB).
M.OoM-TeM*.
AAdnK»M0
340.1 .
340J .
4600-F-O
4600-F-E
Dl17t-BO(A) (IBM)
I-4327-1B
231.1 . Sill B
OCP
27. IMdn«n TOM. M CtCQ,. n^L
Auto
NaMM
TimiwMc (IOTA), or C* ptu* MB • *M»
K*y oaupM |«Mm« or AA dk«*
I3md33).
26 Hydroojtii Ian (pM). pH M*
E*c*x»«»«ne. m»i»»mni. or
130.1
by Indue- 1302
180.1 .
2340c
4600-H.' .
D11
01299-64 |A or B) MaBB-t6
(1B90).
21
AA drao Hp««fc)n or
AA Iwnto* _
Iron-ToM'. mg^L. O^Mton<
... 3111 B
... 236.1. _ 311lBorC- - - 010BKBO (A or ft) ._. 1-3311-66.
236 1
236J
-------
TABLE 1B.—UST OF APPROVED INORGANIC TEST PROCEDURES—Continued
unM «nd mMxx*
EPA in
239.2
17» E«J.
ASTM
U80S'
3113 B
3120 B .
Cotonmcirtc (^ftcncnffwoAno) ...
3V »Q«*J«M Mkagin—ToM. (w N).
3600-F* 0 01099-90(0) .
4600-N org B a c ... 3690-94(A) ..
r
EWcrad*
361.3 4600-NH, E D3690-9MA) .
361.3.. 4600-NH, c D3890-89IA)
361.3..-. 4600-NH,FaO
361.1 — 4600-NH, H _ - _. 1-4661-79'.
361.2 - - 03690-99(8)
_ _ D3690-9XA) _
8*n»«*»TMMd btook Upotti. or -
Pt\ Am* k. _
32. L«d—TOWM. moA; *amai« Ufamta by
AA *•<* Mp**on» _ _ 239.1 31118 or c ._ 03689 90 (A or B) ...
M*mte» _ _ _ __ _ _ 239.2 3113 B -
tCP~ _ «200.7 3120 B _ - _.
DCP» _ _ _ _ 04190-99 -
vmumify". a _ _ _ _ _. _ D3669-90(C)
J2 Cotortmwrtc (O»ttan«) _ _ _ . MOO-Pb 0 - ...
03 33. fcWarmtum-ToWM. mpl; OlBMton • tetouta by
AA drtcl Mpm*on » _ _ __ 242.1 3111 B
CP
200.7 •
t Towi'. moA, Hoi««on' toiooad by
3120 B.
0611-99(8)
(-3447-86
2411 3111 Bore
. 2412 3113 B .......
woo.7 3120 B
SeOO^ng D . 0611-77IA)
.... 0969-90 (A or B)
1-3464-96 .
DCP». a _ _ _ — _ _ D4190-M
Colorlnwtne (PwoJtoW). a _.. 3600-t*> 0 ..... 0899 9«(A) (19991
Otiv
36. Mvoury-TQM«. moA.
CoW wpor, mtnuM Or ..
36. >«a<>»T>-Towi'. moA; mo.mnn«tD9o»nd by
AA »m«o» _
DCP . "
246.1
246-2
..... 3112 B
03223-96
1-3463-96 .
NOW 34.
Not* 22
. 973.49'
"974.27.
NOW 34.
974.27»
MM* 94
•974.27
MM* 34
•980203
249.1 ..... ........ 31110.
246.2 ___ „ 3113 B
200.7 •"!...."! 3120 B ~,
1-3490-96 .
37 N)0«t Towiy mo/L. Hpuioi «
249.1
_ 249.2 "
«P- '200.7 .
OCP««. a _
31119 or c 01
3111 B -
3120 B -
_. 04190-99
(AorB)
977.22'
Mot* 34
Not* 14.
9
?
§
Cotonmcktc QWjBkadnwi .........
39. M»«M (M HI. moA.
CetorkwW (BruoM «uM*| or
(•M pvmwn 39 «nd 40)
39. N» •»»•»• (• N). moA.
C9dmk»i *duc*on.
d or
o
N Mnui MMW N 362.1
.71 - -
40. MM. (M N). moA. V
or
(0*»o9M«or.)
41. 01 and armi ToM
3813 4600-NO.E.... 03897-90(8).-
3632 4600-NO, F 03967-90(A) -.
363.1 4600-NO, M
.._.... . n,«Li^7
384.1- - - - 4*00-NOi B ------ 01264-67
moA.
' ConttuMon or oittMon ....'.
43. Orgvyc nfrogvi (» N). mgd.
TOM KJOIOWX N (P»muWi 31)
(•* P).
„ -------------- 413.1 ------ 6620 B ...... --------- ---------------------
416.1 ---- 6310-8 ..... ------------ 02879-96 (A or B)
973JO*. 4190". p.
29'
NOW 28.
973.47 >. P. 14.»
4900-P E
0616-99(A)
... 31110 ....
46. OdMum—ToM«. "OA- OOMton* tato««d by
ToM«. moA; Oginon' WtoMd by
Of
H(C)(199B)r... M678-79* -
M679-79>_
97186.*
973J6*
973.46B.'
p.827.-«
-... B-829.'*
NOW 34.
NOW 27.
90. PKoM«oru»—Tow). ">gA_.
: KM rcduoMn. or.
396.2 48W-P-BJ
39Uor396J 4600-P-E -
398.1 4900-P-F _
am.4
0616-9B(A).
NOW 27.
NOW 2*.
97346.'
_I. 973J«.«
81. P«*«*iv-Tow)«. m«A; CXg«Nar« Mtowwl by
62.
AA lunwot
DCP ......... -
- 286.1 3111B .—
-«,:*.«,„ 2B6.2
289.1 3111 B
200 7»
NOW 34.
.t-3930^96 973iS.«
FWrrw pholor
^irf'.'a ....!ZIZ!L...-~ - !Z."....r.'.'."".™!.. 3600-K D . .......1.1 D1429-B2
-------
TABLE IB.—Orr of APPROVED INOAOANK; TEST Pnrxcoufcs—Conttnutd
HMmnp* (MMwtf No. or Peg*)
ATTVI U8O8» 0«wr
63 "II»»UI-TOM. rntfU Or«*nw«tc. 103-108'.- _ 160J 2640 6 1-3760-66 .-
64 f\ 7 •? f " *. mpA. Ork»lmi»x. 160* . . . . _ _. 160 ._ _.. 2640-C . _ _ _ _ MT60-66
66 T -•« HUT * e B«««or '
AA aV*CI Mprchon _ 27J.1 ....... 3111B Or C I-3720-66 .._ 97327 •. p 37 «
AAfcnwc* 723 3113B _ _ _
CoMnrrwwc ( M u m ) - _ _ - 3198."
•CP « - _ _.... 2oD.7. _ _ _ _ _ _
_ "„ '_ ~....~1 Not* 34
3111 B - 1-3736-68 .
3120 B -
ri™'Z!~.'-l".'"l'"l"! Not* 34
_ .. 3600-NkD . - D1426-6ZW
_ 1106...... 01128-6HA).. - M790-68 973.40"
375 i _ _ _ _ _..
. or _ _ 378.3 ."!....".. 4BOO-6O. -» C or 0 _ 0616-62(A) (1B66) - - 926*1»
378.4 - 0616-61 - _ 4aC.Q
66. SuNd* (M S). mgrt.
Tftwwtnc («x»w). or _ _ _... 376.1 . ..- 4600-6 « E .-
Cmomiwini. (m+ti^x Out} .._ 3762 4600-6 ' 0 - .
67 SuMto (m SO.). mgA..
TUnrrwmc (KX»n»«0*H) ...... . . 377.1 4600-6O, > B D1336-64-2n F _ _ Now 33.
I tor Qwmul Afwrf»n ol WMr and WkMI'. EnOamwiM Pratodon Agtncy. DrA-M - • UMtanng ByMmt LJCxntory-Cinanrwt (EMSL-CO. EPA-600>4-7»-O20.
/Bkjny. M.±. •> •. 1N»Bd> tar AiwiyM ot »»OrJ»HC BubMniM to WMr kfid rV^I StOiwnkl.' U.S. P»p»f»iwn» ol tw Inwnor. T*cfnf>Mt ol WMr n»oure» ^ - V
Ip/AiwIVMOltw I'amiaiuii 0»06M«I Atwy^wiOiiiiWII.'uwlydijiwnu^.16t<«d- (1690). __^_ _
fn o> ViW MflflipB vw Miflpii) 9 not BHV^O bvofv p^ootH^nA. A QntBpiiQn p^ovpw tt fWQ^fto ID voiuunv tutpttiQtG mttt^tt vtf to dwnroy t
i *Cf CnVWCti AM^rVii of WnMr soo WMVM, *•*• too 1913. U*^A (••cho^ 4.1.3), n ft MDOTOUA ooctton uttno fwrtc flcio- A
t (Melon 4.1.4) to inMinU. howwwr. tw cnttiM inouU b* Okukorwd twl tw mH itamt-r rrwy not tufto* tor •) Mmpwt Iyp4».
' " ' > twl «l «v vc .T» v ban* b* broken M twl tw nwM • m « nwckv* MM In to** MuMcnt. tw
i»«0b* •nftortd. I to »i(ia«rj la «raw*
<4Boroui jgMlar • to b* piMiiiU nwtang etrwtn twl • no »nw dOM tw •*!**» go 10 trjnttt. SimptH conMUng Mrg* •mounte ol orgmc mMriM «rauM MO birwM by tw tugor-
om ol tw anpN>» lunwot fccntnqjk. mdudKwy aouct*> Minn. >t ««i M 11 ,.* x tor evwn MnwnM tuti « mwrac. tw nopw nwiM. nwn>*y. MWnwn. «id
opprowoo r>t»iwc«» k rjMranl tion tw obox*. tw EPA proo*x ol *• umpi*. tw nlmnM prxwXn tor ttW) nwM* mud
M tolOMd Svnpw rlyawuii •kpnxm or gn«nM turrwo*)
•no CP irwryMt pmtMd tw Mnpto toMHn to b* •wrynd nwM tw tolOHM oriwrw.
«. rw* • low COO (00)
b • IWT«) irwwiwrtn mn i >
c • oatorWM "W no Vtnj*M*» ooor «nd
a • ol on* kqud ptWM end »M ol [nrfciMi or •u*p*nd*d nw>*r totomng •.•».•>!•
•Th« mi w>i ol IMfiad 200 7. "mduevvxr f^t^^nttmt Atomc EKWWOTI V / v.. * K. Md»md tar Tnm Ewm«nt A/wty*« ol *•» ma V«MWI.~ • gw«n • atw>da C o< tw pvl
136
-------
•Th*l
•on • not requrad N comperataVy data on .*>> •/ >.-; eMuent temple> ar* on oompany «• >c «^c— m* im» praWranary dMBekon atop * not neoeetery hovever.
«• be required to raeoN* any concmame*
Automated Electrode metiod. InduetneJ Method Number 379-75 WE. deMd February 19. 1976. (Bran 4 Luebb* fTechncon) AutoAnoyter N. Bran 4 LueOD* Anarymg Tacrv
inc.. Elmetord. M.Y. 10623
pprovea metiod a tiat c**d m 'Matiuut tor Datermmatuii ol tnorganc Subetanoet m Water and fluvie> S*d>nant|-. USOS TWM. Boo* 6. Chapter A1 (1979)
can HaaonaJ Standard on photographc nueemu Eieuemt. Apr. 2. 197& AvecaMe trom ANSI. 1430 Broadway. Ne» Yorv. iff 10018
Analytical Metioot Approved and Cited by tie Unaed Statee Enwonmenm Ptutecton Agency.' Supplement to t>e FMeenti Edajon ol Standard Hatmji tor fte Ejumnaaon
r (196H
d*m«»K) (CftOO.) mud not M cortuMd •• »x nd»on« BOO, t**i wf«Ji m»«iur»» TOMI BOO ' Th« aadBtor ol to rar
. bol mu«t b* mcAJbtd to r«pon r« C8OO, pwn«**r A a«c««»J» vtioM p«rm« r*qu»M r«porlng ti* tnrJIbcnal BOO, m«y not JM *
dt>« tor npotng r<« fWiAt Only m««n ( d»cn«rg«r-» p«nni >p«cilinjy MJta* C0OO, • niquirtd. can tt* n»in» back tfrakon mama «• b* u»«d to ravnv
••Onon n«iiai;f Inetucaon Manual. iTcpJual O
tor tieOnon raartm eotonne matvad muet be Oenved uetng t reagent War* and tiree da
ftt
Ot Moda
97-70. 1977. Own
ilanl «OU>
mnMor in tic proo*-
. 040 Mjmivial Onva. CamtrMga. MA 0213B Tfta c««>a>m gnpri
rn. oontanng OJ. 1 0 and 50 ml 0.00281 N pmani^n iudila'100 ml toMon. ra-
"The tpprovad matiod »tiat gtad " Bemdard Mctiodi tor tie Enarnnaton ot Water and Waiiaixnr. I4gi EdBon. 1976
•« Hal oral Cound of tie Paper Induety tor A» tnd Stream Improvement. (Inc.) Tecnmcal Bt*»t»' 253. OcmiiOer t97i
••Cooper. BWUOK* r* Matiuo. Metiod 8606. Hach Handbook ot Water Anetytto. 19T9. HaO> ChemceJ Company. P O Bo> 3M. Lovetend CO 80637
•«After tie manual iliHilun to tompHHd. tie eutoanatvzar mamtoidt n EPA Matxjd* 336.3 (cyende) or 420J (phenoli) arc 0mpMed by cortnecang tie nuamon ane dwcey to «te
aampler Whan uang tie memtotd Mtup *hoMi m Method 336.3. tie butter 63 thouW be replaced wXX tie bufler 7.6 tound In Metwd 3362
' Ityuogwi on IpH) Automated Eteetrod* Method, mduenel Metiod Number 378-75WA. October 1976. Bran 4 Luebb* (Techracon) AutoAnetyier N Bran 4 Luatoe Anan/zng TecrV
ogm. me , EkneVvd. N.Y. 10523
•tton. i.iOPr , >tf»-y •» Method. Metiod •006. 1980. Hech Chemcal Company. P.O Bw 38B. Lovetand. CO 80S37
»Manganae*. Penodat* Ondeton MeHxx). Matmu BOX. Maen Hendtxx* ol WaMmaur Aneryx, 1979. ptget 2-113 and 2-117. Hach ChemceJ Company. Lovetand. CO 80637.
"Wertft*. n.L . el «. •MertiOut tor Anah/M ol Orgarac Subetanoet n Water.' Techraque* o< Water-Reeourcet Inveeiigation of tie U.S. Oentngrai Survey. Book 5. ChapMr A3. (1972
1987) p 14
Nntt*. Motad 8607. Hech ChemceJ Company. P.O Boi 388. Loveiend. CO 80637
The approved metxxl • Otea r Standard Me«ioJi tor tt* Eiamnaaon at Weter er«3 Weetewater. 14*1 Ednxm Th«
are grven on pp 576-61 of tie 14» Edaxxi Method 510A tor dMIaaon. Method S106 trx *>•
\
»R.F Actttan VK) R.O Ackmw. "Oncl OMvmrMkon of El«rn*nt« PtmprXym
tncOxxt* tor •<• irxryM ol (Xv n nduMn*! «K»l»i»a>ri M conotntr
-jj-"-jj- .-._. ... . . _._.
pM o< IO.QtO.2. T>w «p-
S10C tor •
nt ol
.
auch a* tie brorrude and chtohdc are rctatr ay raakJUt m raagemt euch at rutx add but are r
Theretor*. tor levett ol »tver above 1 mp/L. 20 ml ol temple tnould be dtutad to 100 mL u, addng 40 mL each ol 2 M Nt\SrO. end NaOH Standard! thoutd b* prepared «i tie tame
procedure, or Metxid
Chromelograpriy." Journal of Cnrorrat.. ^t,y. tol 47. No 3. pp 421-426. 1970.
and atjov* are nadeojate where etver enett at an i
KXuttt n an aqueout butter ol todum tNOcuMatc and codium hvdro>Me to pH ol 12
For krv*a> y arver below 1 mg/Ctie epproMd metxxt it uh*lackxy
*<>Th* appro,ad method • tiat c*ed r. Sundard Metiudt tor tne Exammation ol Water and Warturetti. 15th Ednon
>' The approved method « tiat Oted n Standard MeBiuJi tor tie Eumnaton oi Water and Wattenratar. 13* Ed*on
• Sjevent. M H. Fck*. J F . and Smoot. OF -water TimperafeA—mttuerrtal Facxn. F«M Maaturement and D*» Piamnabon"
x * ol
P
US O*oiaox« Survey. Booh 1. Chapter 0V '975
"Zjnc Z«eon Method. Matxx] 8009. Hacti HanoKXik ol Water Ana>yM. 1979. page* 2-23' and 2-333. Hacti ChameaJ Comply. Uivatand. CO 80637
••"Oiraci Current Puum* (DCP) Optcat Emxaian St ' u^itK MetVx) tor Trace Element* An**/** of Water and Watt** Herod ACS0029.' 1805 n*. .r? 1991. R«on Inttrumeno.
toe . 32 Commerot Center. Cherry H* Onv*. Oarrvart. MA 01923
MPreowon and recovery etaMmanu tor tie atonvc abeorpton ana aapcrakon and graphite lumace matnodt. erx) tor *e vJ uvrX*urritc SOOC method tor arcane arc provided n
append^ 0 oi tx* pan need. 'Pracwon end Recovery Statement* tor Hetrm.1i tor Maaumq Mcurf
"'Ctoeea veual »*cro»»a»* Ogetton ol Want alir Samplei tor Detemwiekon ol MeWi'. CEM Corporabon.
AvaMX* Irom tr* CEM Corporation
PO Boi 200. »Htiei.». Norm Caroana 26'06-0200. Apm 16. 1902
TABLE 1C.—Usr OF APPROVED TEST PROCCDURES FOR NON-PESTIODE ORGANIC COMPOUNDS
oc
OCXS
MPVC
Standard meffxxn I7ti
Ed
ASTM
OtW
2 ncanapf*tr>y4vnf
) Acrtean
4. Anthracene
8. BanMr>*
T flt ll.Vt
• laniiXilfyiwie
12 §anio(fc)iiii»ai»oi'oati)nj*LiiOc
23 4-CMD*&-4 -Trff^r^ vl
J*. Cntorabanzene " -
IS. Clajiietieii* _
M. 2-G4\»*. jT^t^lr./ atier -
fj Cia^aJOiiii
It Chto>oi> /^arM
18 2~Ontonx ^4t V«-vj
31 4-CMPVti' /VK. .ft e»er
33. Cnryaana
99 pajarti*Hc,h)afttifccari*
34 DUv'ivw'4^6rr^ ~^
36. 1. t-Otcraamjaiuane
3* t J-Ocntorijtianiene
8. i. 4^tcntoraeeniane
M ""tilfiujfcjromafun*
40 i. t-0>cHuiue«'ane
«1 l.2-OcNoroe»«ne ..
610
_ 610
803
803
„ 610
._ 802
610
.._ 610
610
•10
_ 810
. . _ 804
611
_ 611
•06
•01
•01
801
._ _ 611
801
_ 804
_ 801. 603
•m
•01
601
_ _ 801
_ _ 812
•04
en
._ 610
610
•01
_ •01.802.612
601.602.61}
a01.803.6l2
. . 601
«1
«01
•25.1826
•25.1*24
•604. 1624
• •24. 1824
•26.1626
•24. 1824
••25.1625
•26. 1828
•26. 1826
•26.1826
•26.1626
•26.1625
•28. 1826
826.1825
•26.1826
•26.1626
•24. 1624
•24. 1824
(94. 1824
•26.1626
•24, 1624
•26.1825
824.1624
•24. 1824
824. 1824
824. 1824
824. 1624
•25.1625
825. 1825
Ot. 1825
•25.1625
825. 1625
•24, 1624
•24.625.1825
8M.62&KB&
•26.1824.1625
625 162$
•24. 1624
624. 1624
6tO 8410 8. 6440B
610 64106.64408
04867-87
D4687-87
610
610
805
610
610
610
610
610
610
610
905
64'OB.6440B 0*867-«r
8210 B. 8220 B
6410 B. 6440 B 0*867-67
•410 0 6440 B 04667-87
•410 B 6440 B O4867-87
64108. 6440 B 0*667-87
6410 B. 6440 B Oe867-87
6410B
6410 B
8410 B
64108, 8230 B
•2108.62308
8210 B. 8230 B
8210 B. 8230 B
641Q a
6230 B, 6410 B
6410 B. 6420 B
8210 B. 8220 B
62308
6210 B. 8230 B
8210 B. 8230 B
6210 B. 8230 B
8210 B 6230 B
6410 B
6410 B. 6420 B
6410B
6410 6, 6440 B O4667-87
6410 B. 6440 B 04867-87
621Q 6 6230 B
641Q B 6230 B. 8220 B
641Q B. 6230 B. 8220 B
6410 B. 8230 B
6220B
6410 B
•Z30B
6230 B. 6210 B
•230 0. 6210 B
Note 3. p!
Not. 3. pi» Not* 6.
p. 8102
NOH3.
Not* 3. P IX
Not*, p 130
-------
TABLE 1C.—UST OF APPROVED TEST PROCEDURES FOR NON-PESTKSOE OROAMC COMPOUNDS—ConUnuw)
EPA lilMlUli NM«bO» '
oc
OCMB
MPCC
42. 1. 1
«lnn»-1.2-G~U*
44, 2.
47.
4B. OMhyl p
4B. 2, I C .
BO. OMB*
(1 r*MM>l
B*. OMvooy
Bl 2. VOMMphonol
(4. 2. +OMOMOT*
(B. 1. (-OMVMOUn* .
M.
B01
B04
B01
Boi
B01
B06
KM
BOB
BOB
BOB
BO*
BOB
BOB
CM. 1124
BM. IBM
BM. MOS
BM. IBM
BM. IBM
BM. IBM
BM. IBM
BM. 1BM
BM. IBM
BM. IBM
BM. IBM
tOt. IBM
BM. IBM
BM. 1BM
Ed.
... B230 a B210 B
.... B230 B, B210 B
.... BOO B, B410 B
ITtl
ATTM
OBMr
B2HO.V10B
BZJOB. 910 B
B410 B
B420 B. B410 B
B410 B
B410 B
(410 B
B420 B. B410 B
B410 B
B410 B
7VPW-101B
T7. PCBV1J21
TB.PC»-m2
PO-124B
B2. P»-12BO
BJ. P»
KB tat IBM ...... ....... B220 A 010 B
«10 BM. 1BM BIO B410 B. B440 B
*10 BM, IBM BIO B4(0 B, BMO 0
112 BM. 1«S .............. *410B
(12 BM. i«H .............. B410 B
B12 »BM. IBM ........... B410 B
(16 BM IBM ..... .. ....... (410 B
tlO BM. IBM 010 B410 B. (440 B
BOB BM IBM B410 B
B01 K4 IBM Z."Z. BHO B
KM BM. IBM .............. B420 B. B410 B
HO BM. IBM BIO B410 B, B440 B
BOB BM. IBM ...... . ..... B410 B
KM BM. IBM ....... . ..... B410 B, B420 B
KM BM. IBM ..... ______ B410 B. B«20 B
B07 BM. IBM ........ ..... B410 B
(07 4M IBM ...... B410B
107 IBM. IBM ...... ....... B410 B
111 BM. IBM ...... ______ B410 B
BOB BM ...... ....... B410 B
BOB BM -...- ....... B410 B
BOB BM ..... . ....... BtlOB
BOB BM IILJIIIIII *410 *
BOB BM I ____ Illllll
•"• "* ----- ....... **10i
BOB BM IILJM «410 B. BBX B
KM BM. IBM llll..__llll B410B. BB30B
(10 BM. IBM OBCB410 B. 6440 B
NOM1. p.130No»6.
M102.
D4BS7-B7
D4B97-B7
MB67-B7
O4BB7-B7
Mm 3. p.110
O4B67-B7
MOM 3. M3
Now 3. M3
NOM 3. p.43
MOM 2. p.«
MmJ. p.4S
Now a p 43
Now 3 p 140
B420B.I410B
010 B410B.B440B
CMBB7-B7
»*oli»,p,l$a
BHOB,BI10B
BtJOB,Bt10B
Bt10B,BZ20B
B410 •
B110B.BB30B
..... «10 B, BBK B
Bt10B,Bt30B
B»10§,BBJOB
(410B.M40B
(210B.B230B
•J.1.1.1-TrWA.4.f%n«
w
. aiau mn-i-i~T ~i~r -i'ij- *-* r~l*" -- 'i - *• — " f — "
iio»».'». <««n twy •* MOOT « b* pxwm. t» prMmd
vtf OM by M UnBM
tor MM** M BM tnd 100% tor hodi IBM tn) 1BM) <
ot «ry pranol* Hto outoMt »• twntng *"•».
Mmplw to «or*o» wd
tor Ml
Ntm 1>i«* Mmng
m |u> ..... tjMiil •> in Intorlnt IrM Mton OTTI • raquo* tor
-------
$136.3
I AMrw
2.
3.
4.
5 Akvnw
a Aanpho* nw«iyl
40 CfR Ch. I (7-1-93 EdMon)
TABLE 1 D.—UST OF APPROVED TEST PROCEDURES FOR PESTICIDES'
EPA nwnod iw«to«r
FPA,, Standard ma«v .__. °*"r
EPA od»i7»-TP (Stow)
88.
88. Ti
m. Trthnftn
QC
QC
TLC
n c
n c
n c
OC
OC
n c
OC
OC
OC
QC
OCMS
QC
8830B4C
•640 B
•640 B
BOB BB30B4C
B2S 6410 B
8630 B
03086-90
NOM a p. 104; NOM 6. p
964
NOM 3. p. 28. NOM 4. p W
NoM 3. p. 28.
NoM 3. p 7
NOM 3. p. 83. NOM 6. p
368.
NOM 3. p 83. NOM 6. p
388.
NOM 3. P 63; NoM 6. p.
868.
NoM 3. p 104. NOM 6. p
864
NOM a p 94; NOM 6. P
860
NoM 3. P 83. NOM 6. p
388.
NoM 3. P 104; NoM 6. p
384,
NoM 3, p 83. NOM 6. p
888.
NoM S. p. 7
NoM 3. p 104. NOM 6. p
964
NOM 3. p 116. NOM 4. p
38.
NoM 3. p. 118
NoM 3. p 83. NOM 6. p
BBB.
NOM 3. P 7. NOM 4. P 30
Mm 3. p. 7.
. AddMonal paatodM may b* tound
.-o* KM
TabM IDNoM*
' raaacldai am MMd n 1m MDM by common nama tor ffw o&fi-k u of tw raodi
infer TabM 1C. «_jt. w PruMcaon Agancy. ^«pM»«iai. 1978. Trxa EPA niMraanri ndudaa tunlayar J»«.
«1«afiooi tor AnaryM al Organc «•' n WaMr and RuMri SadMianM.- TacnmojuM ol \
•am al IM UA OMtoaat Straw. Book 8. OwpMr A3 (1987)
• Th* mMwd mn b* «>Mnd*d to maUM a-BHC. 4-BMC. i
»to MMI. IM»Drt 808 • «M
I. •ndtmJMn 1. and •ndrln. HOMMT. «Mn My «n>
326
327
-------
TAKE IE.—LOT OF ARROWED RMMUXHCAL TEST PROCEDURES
p. 71
709 D1SSO-S1
70ft OS4S9-70
70S DM64-7*
TMtoK
< / \ ftiandtmstor'*
PMMCSM ASM*. Auul 1«0.
•n^wTliU MrEm*. Eygwfc-Si
ioan.fi IBIK
H^OH H-
«•»•» •HTMjy. VBHS^rr-Ml ne^aw* rv-^r * iiv*«y»
*Ths9 Mflbflst iDIMvt OM O> 71 PRSBBHWH BHlV VH dhMsVCfJ Pty^flH
(b) The full texts of the methods from
the following references which are
cited in Tables IA, IB. 1C. ID, and IE
are Incorporated by reference into this
regulation and may be obtained from
the sources identified. All costs cited
are subject to chance and must be veri-
fied from the Indicated sources. The
full texts of all the test procedures
cited are available for Inspection at the
Environmental Monitoring Systems
Laboratory. Office of Research and De-
velopment, U.S. Environmental Protec-
tion Agency, 36 Weet Martin Luther
King Dr., Cincinnati, OH 46388 and the
Office of the Federal Register, room
B301. 1110 L Street, NW., Washington,
DC 30408.
RBTBUNCn. SOURCES. CO6T8, AND
TABLE CITATIONS:
(1) The full text of Method* 691613.
CM, 836,1634. and 1826 are printed ia ap-
pendix A of this part 136. The full text
for determining the method detection
limit when using the test procedures Is
given In appendix B of this part 136.
The full text of Method 300.7 1* printed
KI • ppdDdllc of this part 136. Cited in:
Table IB. Note S; Table 1C, Note 2; and
Table ID, Note 2.
(2) "Microbiological Methods f o r
Monitoring the Environment. Water
and Wastes." U.S. Environmental Pro-
tection Agency. EPA-«00/8-7S-017, 1978.
Available from: ORD Publications.
CERI, U.S. Environmental Protection
Agency. Cincinnati. Ohio 46366. Table
IA. Note 2.
(3) "Methods for Chemical Analysis
of Water and Waste*." U.S. Environ-
[r.A ji*,.»itiA Pioltcion Acjsjncy
mental Protection Agency. EPA-600/4-
79-030, Much 1979, or "Methods for
Chemical Analysis of Water &nd
Wastes." U.S. Environmental Protec-
tion Agency, BPA-flOO/4-78-030. Revised
March 1963. Available from: ORD Publi-
cations. CERI. U.S. Environmental
Protection Agency. Cincinnati, Ohio
4S368. Table IB. Note 1.
(4) "Methods for Benzidlne.
Chlorinated Organic Compounds.
Pentachlorophenol anc Pesticides in
Water and Wastewater. ' U.S. Environ-
mental Protection Agency, 1979. Avail-
able from: ORD Publications. CERI.
U.S. Environmental Protection Agen-
cy. Cincinnati, Oh 10 46368. Table 1C,
Note 3; Table D. Note 3.
(6) "Prescribed Procedures for Meas-
urement of Radioactivity in Drinking
Water," U.S. Environmental Protec-
t i o n Agency. EPA-600/4-80-032. 1980.
Available from: ORD Publication*
CERI, U.S. Environmental Protection
Agency, Cincinnati, Ohio 46381. Table
IS. Note 1.
(6) "Standard Methods for the Exam-
ination of Water and Wastewater."
Joint Editorial Board, American Public
Health Association, American Water
Works Association, and Water Pollu-
tion Control Federation. 17th Edition.
198. Available from: American Public
Health Association, 1016 Fifteenth
Street, NW., Washington, DC 30036.
Coat: 390.00. Tables IA. IB. and IE.
(7) Ibid. 15th Edition. I860. Table IB.
Note 30; Table ID.
(8) Ibid. 14th Edition, 1975. Table IB.
Notes 17 and 27.
(9) Ibid. 13th Edition. 1971. Table IB.
Note31.
(10) "Selected Analytical Methods
Approved and Cited by the United
States Environmental Protection
Agency," Supplement to the 15th Edi-
tion of Standard Methods for the Ex-
amination of Water and Wastewatar.
1961. Available from: American Public
Health Association. 1015 Fifteenth
Street NW., Washington. DC 30036. Coat
available from publisher. Table IB,
Note 10; Table 1C, Note 6; Table ID,
Note 6.
(11) •'Annual Book of Standards-
Water." Section 11. Parts 11.01 and
11.01, American Society for Testing and
Materials. 1991.1916 Race Street, Phila-
delphl*. PA 19103. Cost available from
publisher. Tables IB. 1C. ID. and IE.
(12) "Methods for Collection and
Analysis of Aquatic Biological and
Microbiological Samples." edited b y
Brltton. L.J. and P.E. Oreason, Tech-
niques of Water Resources Investiga-
tions, of the U.S. Geological Survey.
Book 5. Chapter A4 (1969). Available
from: U.S. Geological Survey. Denver
Federal Center, Box 25425. Denver, CO
80225. Coat: E8.25 (subject to change).
Table IA.
(13) "Methods for Determination of
Inorganic Substances in Water and
Fluvial Sediments." by M.J. Ftshman
and Linda C. Friedman. Techniques of
Water-Reeources Investigations of the
U.S. Geological Survey, Book 6 Chapter
Al (1989). Available from: U.S. Geologi-
cal Survey, Denver Federal Center, Box
26426, Denver, CO 80236. Coat: J108.75
(subject to change). Table IB. Note 2.
(14) "Methods for Determination of
Inorganic Substances in Water and
Fluvial Sediments." N.W. Skougstad
and others, editors. Techniques o f
Water-Resources Investigations of the
U.S. Geological Survey, Book 5. Chap
tar Al (1979). Available from: U.S. Geo-
logical Survey, Denver Federal Center.
Box 26426. Denver, CO 80226. Cost: S10.00
(subject to change). Table IB. Note 8.
(IS) "Methods for the Determination
o f Organic Substances i n Water and
Fluvial Sediments," Wershaw. R.L.. et
al, Techniques of Water-Resources In-
vestigations of the U.S. Geological sur-
vey, Book b. Chapter A3 (1967). Avail-
able from: U.S. Geological Survey,
Denver Federal Center. Box 26426. Den-
ver, CO 80225. Cost: J0.90 (subject to
change). Table IB. Note 94; Table ID,
Note 4.
(16) "Water Temperature-Influentlrl
Factors. Field Measurement and Data
Presentation." by H.H. Stevens. Jr., J.
Flcke. and G.F. Smoot. Techniques of
Water-Reeources Investigations of the
U.S. Geological Survey, Book 1. Chap
t«r Dl. 1975. Available from: U.S. Geo-
logical Survey, Denver Federal Center.
Box 2M25. Denver, CO 80225. Cost: $1.60
(subject to change). Table IB, Not* 32.
(17) "Selected Methods of the U.S.
Geological Survey of Analysis of
Wastewaters," b y M.J. Ftohman and
Eugene Brown; U.S. Geological Survey
Open File Report 76-77 (1976) Available
328
329
-------
from: U.S. Geological Survey, Branch
of Distribution, 1300 South Eads Street.
Arlington. VA 22902. Coat: 313.50 (sub-
ject to change). Table IE. Not* 2.
(18) "Official Methods of Analysis of
the Association of Official Analytical
Chemicals", Methods manual, 15th Edi-
tion (1990). Price: SMO.OO. Available
from: The Association Of Official Ana-
lytical Chemists, 2300 Wilson Boule-
vard, Suite 400, Arlington. VA 22201.
Table IB. Note 3.
(19) "American National Standard on
Photographic Processing Effluents."
April 2.1415. Available from: American
National Standards Institute, 1439
Broadway. New York, New York 10018.
Table IB, Note 9.
(X) "An Investigation of Improved
Procedures for Measurement of Mill Ef-
fluent and Receiving Water Color."
NCASI Technical Bulletin No. 253. De-
umber Ml. Available from: National
Council of the Paper Industry for Air
and Strum Improvements, Inc., 280
Madison Avenue, New York, NY 10016.
Cat available from publisher. Table
IB. Note 19.
(21) Ammonia, Automated Electrode
Method. Industrial Method Number
379-75WE. dated February 19, 1978.
Technicon Auto Analyser II. Method
and price available from Technicon In-
dustrial Systems, Tarrytown. New
York 10W1. Table IB, Note 7.
(22) Chemical Oxygen Demand. Meth-
od MOO. Hach Handbook o f Water Anal-
ysis, 1979. Method price available from
Hach Chemical Company, P.O. Box 389.
Loveland. Colorado 80637. Table IB,
Note 14.
(23) QIC Chemical Oxygen Demand
Method, 1978. Method and price avail-
able from Oceanography International
Corporation, 513 Wat Loop. P.O. Box
2980. College Station, Texas 77840.
Table IB, Note 13.
(24) ORION Research Instruction
Manual. Residual Chlorine Electrode
Model 97-70, 1977. Method and price
available from ORION Research Incor-
poration. 840 Memorial Drive. Cain-
bridge, "•-vrhusetu 00138. Table IB,
Note 16.
(26) Blclnchonlnate Method for Cop
par. Method 8608. Hach Handbook o f
Water Analysis. 1979. Method and price
• vdlabie from Hach Chemical Com-
40 CFR Ch. I (7-1-93 EdMon)
pany, P.O. Box 300. Loveland. Colorado
80537. Table IB, Note 19.
(28) Hydrogen Ion (pH) Automated
Electrode Method, Industrial Method
Number 378-75WA. October 1976. Bran &
Luebbe (Technicon) Auto Analyzer II.
Method and price available from Bran
& Luebbe Analyzing Technologies, Inc.
Elmsford, N.Y. 10523. Table IB. Note 21.
(27) 1.10-Phenanthrollne Method
using FerroVer Iron Reagent for Water,
Hach Method 800B. 1980. Method and
price available from Hach Chemical
Company. P.O. Box 369 Loveland. Colo-
rado 80637. Table LB. Note 22.
(29) Pertodate Oxidation Method for
Manganese. Method 8034. Hach Hand-
book for Water Analysis, 1979. Method
and price available from Hach Chemi-
cal Company, P.O. Box 389, Loveland.
Colorado 80637. Table IB. Note 23.
(29) Nitrogen. Nitrite—Low Range.
Dlasotiiatlon Method for Water and
Wastewater. Hach Method 8607, 1979.
Method and price available from Hach
Chemical Company. P.O. Box 389,
Loveland, Colorado 80637. Table IB.
Note 26.
(30) Zlncon Method for Zinc. Method
8009. Hach Handbook for Water Analy-
sis. 1979. Method and price available
from Hach Chemical Company, P.O.
Box 389, Loveland. Colorado 80637.
Table IB, Note 33.
(31) "Direct Determination of Ela
mental Phosphorus b y Gas-Liquid
Chromatography." by R.P. Addlson and
R.O. Ackman, Journal o f Chroma-
tography. Volume 47. No. 3. pp. 421-426,
1970. Available in most public libraries.
Back volumes of the Journal of Chro-
matography are available from
Elsevier/North-Holland, Inc.. Journal
Information Centre, 52 Vanderbilt Ave-
nue. New York, NY 10164. Cost avail-
able from publisher. Table IB, Note 28.
(32) "Direct Current Plasma (DCP)
Optical Emission Spectrometric Meth-
od for Trace Elemental Analysis of
Water and Wastes", Method AE8 0029.
1986-Revlsed 1991. Plson Instruments.
Inc., 32 Commerce Center, Cherry Hill
Drive, Danvers. MA 01923. Table B.
Note 34.
(33) "Closed Vessel Microwave Dlges-
Lion of Wastewater Samples for Deter-
mination of Metals, CEM Corporation.
P.O. Box 200. Matthews. North Carolina
38108-0200. April 18.1992. Available from
Envtroni.irJ f hotacHon Agency
the CEM Corporation. Table IB, Note
36.
(c) Under certain circumstances the
Regional Administrator or the Director
in the Region or State where the dis-
charge will occur may determine for a
particular discharge that additional
parameters or pollutants must be re-
ported. Under such circumstances, ad-
ditional test procedures for analysis of
pollutants may he specified by the Re-
gional Administrator, or the Director
upon the recommendation of the Direc-
tor of the Environmental Monitoring
Systems Laboratory—Cincinnati.
(d) Under certain circumstances, the
Administrator may approve, upon rec-
ommendation by the Director, Envi-
ronmental Monitoring Systems Lab-
oratory—Cincinnati, additional alter-
nate test procedures for nationwide
use.
(e) Sample preservation procedures.
container materials, and maximum al-
lowable holding times for parameters
cited in Tables I A. IB. 1C. ID. and IE
are prescribed in Table II. Any person
i 136.3
may apply for a vu-lance from the pre-
scribed preservation techniques, con-
tainer materials, and maximum hold-
ing times applicable to samples taken
from a specific discharge. Applications
for variances may be made by letters
Cc the Regional Administrator in the
Region in which the discharge will
occur. Sufficient data should be pro-
vided to assure such variance does not
adversely affect the Integrity of the
sample. Such data will be forwarded.
by the Regional Administrator, to the
Director of the Environmental Mon-
itoring Systems Laboratory—Cin-
cinnati. Ohio for technical review and
recommendations for action on the
variance application. Upon receipt O f
the recommendations from the Direc-
tor of the Environmental Monitoring
Systems Laboratory, the Regional Ad-
ministrator may grant a variance ap
plicable to the specific charge to the
applicant. A decision to approve or
deny a variance will be made within 90
days of receipt of the application by
the Regional Administrator.
TABLE II—REQUIRED CONTAMERS. PRESERVATION TECHNIQUES, AND HOLONG TIMES
Mumum hofckng «m«.
1-4 CoMorm. fee* *tf to* P
b£ kx». «T*M
14. BttLliw* oryg»n rjvntnd. cvto-
r+cmnum
1ft Ctstond*
21 Orrtw
23-24. Cyoruotx tott and Mn«*b8» to
U*JV JV«V
25 Ruortdsi
2t. |M>iiu*m. ion (OH)
31. 43. Nfridtf il and orpanc rt»ctf*n
•to."'
1B.Ct«omMiiVI ilililililllilililili
36 Hfcrowy
3 6-B 10 12 13.19 20 22 2S. 29 30 32-
34. 3S. 37. 46. 47. 51. 62. SS-aO. S2. a.
70-72. 74. 76 MMto. Map! dMOmun VI
39 NT J* . V
40 H»»
41 R md QTMM (
42. Ogmc OHbon f
•• 0.*-.' - yu% iiiiil .._ _ .Ill 1
. a „
Q
Q
Q
o
Q
Q
O
o
o
a
o
Q
Q
o
o II .Jllllll
.0
a
a
o
.0
j
» Q
il a III! .11111
Caoi. 4-c. o oas% Mb&o,> ...
do
Cool 4"C
Cool. 4*C H,SO. 10 pH<2
Cool 4*C
Cool. 4-c _
Coal 4*C H}3O« to pH<2
Non* r«Qjitf«d
Cool. 4-C. NBjQH to pK>-12.
O.eg Mooftic «CBd >.
Non* r*Q>v8)d
HNOt *0 pH<2 HiSO* to pHc2
Man* r*qurad
Coo*. 4-C. H^O, to pH<^
HNOi to pH<2
Cool 4%
Cool 4-c. H|3O*t to pH<2
Cool 4*C
Cool to 4~C. frO or H)SOu to
pHSO. la
pM<2.
Rkw IflT V X. Cool 4X III
6hom.
Do.
Do
4* tan
2SdM.
4SHOW*.
2S dfewft
Do
44 tan
I4o*y*.*
28d*vm
6 rnonMk
2Sd*v*.
• mon*w
4 6
48houn
Da.
330
331
-------
I no
TAKf
40 C» Ch. I (7-1-93 EdMon)
-_U CONTAMERB, PRESERVATION TEOtlQUES. AND HOUNNQ TltfES—Conlnusd
Ri an •*• ond «on •> dork
Coal. 4-C. MrfO. ID pH<2 ...
Cool. 4-C -
Coal. 4-C. H4O. to pH<3 ...
Coal. «•€
• ham.
2S dor*
4Stam.
is-ao. A 2*-as. M-CT. ss-4». 46-47.
66. 66. Hi 88. 88-66. §7
a T
Cool. 4-C. 0406% NbjSiOK* : 14«Bj*.
Cool. 4«pHto4-ftM.
Cool. 4-C. (
72-74. r~
78-82. PC*>"
»4. M.
1.2 ft. 8-12. 32. 33. 6S. 66. 64. 88. 64. 88.
16.16. 21. 31. 76.1'. /* ." _ _.'
28. 38-37. m - a 81. CT \ ~
Cool 4%.
Cool. 4-C.
.--- coot.4-c,ojoot%NbACv.
,& _ Cool. 4*C. pM J-S'«
P. a HNOi to pH<2
Do.
Do.
Da
Da
Da
i g loll IJNbjtc odd S4400 to MMr raMto« • A - _ d 0.18ft by MbM I
___«??jMOJ * Mtor MkioM* m A - , ol 036% by •QtoM or ton IpH QftoU 1.1< or grioin. ond
—-•- i in*toS«oOM)»i»^or ontanritoi :..x. t - _ ol 0X160% b* MioM or tool «pH obou 12JO or tow).
•8""P'" *"**bo o»o)»iido> too*• poooHoo*orooSoaton. Tbo8M4*Modor*•»mo.*«u« MM* tiol lomptoi moy
bft iHtM LMBSMBB •M8888fe«ste SMka fdfl 8^ MM^bBr^H^rt b^rfM It^bSBW^*^ OB^U *— ai^arf fcii LJ^UB^ ••^•^HtWi 4^b*u M MbA «^M^^8B^^ tfw 4^*M^6rw6jM
•^ >^>M« IP^MW SV^^fRBBBl SVm 8BB* 8^ «AV^81V8W ^8B8D. Q^6V6|JBBJB| PfBBBM D8I HsjBH 8HV BBllDBf DWOB WV " ••• DsWWWB«8p, V ItfWIWW
tofcorotory. HOB doto on •• to oko* M *o opocAc topoo at n tiln indv oMdV or«
o*««d o «•*•*» bom tio RoatonoJ > / A - ——- I'TTTliI flp-| in Jill 7-
Mod (*on n Mo MMo. A pBBaW or mMtohng totnrotorv. I. obtaMd to bob tio
*»J?*?• •*•»• "~~nr»•*«•*• -"I*•*•*> soofislawtor
tbam
taropM-% ' \ to ordor to doMn*io *
•*•» poaiSB itm m nogalxo opd tool b) ol
NoQM is odOod to pH 12.
332
trJS PtotacNon Ag«ncy
«mt » i\i>y
no pH oo)uoknonl muot bo onoty
botoro •ddnou -
C. arOCMS
.
n ooy* a* Mmpkng.
S 134.5
no pH «V«ttn«ni not bo
Tho pM oikJOMonl • not roojivod < ocrotom •• no) bo mooMOd. SompM tor ocrota
onoJyiod ••nto S doyi ol Hmptng.
"fthon tio ortoUoMo onolytot ol ooncom tol »«t»» i unoK chomcoi coloonr». f»« .
tor opojmtfn Mtoguord ol Mrnpto mogrtv. \OBIOII tio onoryMs or uunuorn i
bo prooorvod by cookng to 4-C. roduang roMduol cMarmp««h
i pH to 6-«. »on«itoi prooorvod • tio onoty»» ol Bonn-
.
TtM dM. and Muotng tw pH to 6-«.
tor* ortooon ond tar tody O*ft o*or omattn. EKaataru to
« toanoto 5 (r» tio roqi*omonl tor
*^« l>dtotx ./A.Afeira • »oly to bo pFiiiiH. oO)uol «to pH ol tio MmpM to 40*0.2 to prooon
upto7o^y»botoi«orMty*««Mor«o^iloanauctodundoronnoi1 (7
.--.J 1 1 <
P*I?Tho pM MiuoMwil moy b
72 haun ol oofciaT Farlio
pH to 7-10
icnri roDMpt ol tio tobarotory ond «oy bo
oidrtn. oddl-
[38 FR aru. Oct. 16. 1973. u unondod at 41 FR 53711. DM. 1. 1976; 40 FR 433S1. 432M. 433W.
Oct » 19M: 50 FR 691. 692. 696. Jan. 4. 19K; 61 W. 236*3. Juno 30. 19W; 62 FR 33643. 8«pt. 3.
1867; 66 FR 24634. JUDO 16. 1980: 66 FR 33440. Auc 16. 1980; 66 FR 60769. Oct. I. 1901: 67 FR 41133.
Sopt. 11. 1992)
far •Itamato U*t
p* a eir ••*••.
(a) Any penon m*y apply to the Re-
gional Administrator in t h e Region
where the dlacharve occurs for ap-
proval of an alternative test procedure.
(b) When the discharge for which an
alternative test procedure Is proposed
occurs within a State having a permit
program approved pursuant to section
403 o f the Act. the applicant shall sub-
mit his • ppllcatlon to the Regional Ad-
ministrator through the Director of
the State agency having responsibility
for issuance of NPDES permits within
such State.
(c) Unless and until printed applica-
tion forma are made available, an ap-
plication for an alternate test proce-
dure may be made by letter in trip
llcate. Any application for an alternate
test procedure under this paragraph (c)
shall:
(1) Provide the name and address of
the responsible person or firm making
the discharge (if not the applicant) and
the applicable ID number of the exist-
ing or pending permit. Issuing agency,
and type of permit for which the alter-
nate test procedure is requested, and
the discharge aerial number.
(2) Identify the pollutant or param-
eter for which approval of an alternate
testing procedure Is being requested.
(3) Provide justification for using
testing procedures other than those
specified In Table I.
(4) Provide a detailed description of
the proposed alternate test procedure.
together with references to published
studies of the applicability of the alter-
nate teat procedure to the effluents in
question.
(d) An application for approval of an
alternate test procedure for nationwide
use may be made by letter in triplicate
to the Director. Environmental Mon-
itoring and Support Laboratory. Cin-
cinnati. Ohio 46968. Any application for
an alternate test procedure under this
paragraph (d) shall:
(1) Provide the name and address of
the responsible person or firm making
the application.
(2) Identify the pollutanUs) o r
parameter®) for which nationwide ap-
proval of an alternate testing proce-
dure Is being requested.
(3) Provide a detailed description of
the proposed alternate procedure, to-
gether with references to published or
other studies confirming the general
applicability Of the alternate test pro-
cedure to the pollutant(s) o r
parameters) in waste water discharges
from representative and specified
Industrial or other categories.
(4) Provide comparability data for
the performance of the proposed alter-
nate test procedure compared to the
performance of the approved test pro-
cedures.
(38 FR 28760. Oct. 16. 1973. a* unended at 41
FR 52785. Dec. 1. 1976]
| 1S&6 Approval ot alternate test pro-
cedure*.
(a) The Regional Administrator of
the region in which the discharge will
occur has final responsibility for ap-
333
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40 CFR Part 136
Tables IA, IB, 1C, ID, IE
and
Table II
and shall state the tall name. address.
and telephone number of the person
giving notice.
(c) Identification of ctntntel. All no-
tice* • hrll include the name, addreM.
and telephone number of the legal
counsel. If any. representing the person
giving notice.
I1M.1S TlEtlx« of BoCkw.
No action may be commenced under
section 1449(aXl) or (aX2) until the
plaintiff has given each of the appro-
priate parties sixty day* notice of in-
tent to file tuch an action. Actions
concerning injection wells disposing of
hazardous waste which allege jurisdic-
tion solely, under section TOOKc) of the
Resource Conservation and Recovery
Act may proceed immediately after no-
tice to the appropriate parties.
PART 136-GU1DEUNES ESTABLISH-
ING TEST PROCEDURES FOR THE
ANALYSIS OF POLLUTANTS
8*0.
136.1 Applicability
136.2 Definitions.
136.3 Identification at test procedures,
138.4 Application for alternate test proce-
dure*.
138.5 Approral of alternate Met procedures.
APPENDIX A TO PART 138— MSTHODS roR OR-
GANIC CHEMICAL ANALYSIS or MUNICIPAL
AND INDUSTRIAL WASTEWATER
APPENDIX B TO PART 136— DkruiriiON AND
PROCBDUU POR TUB DETERMINATION OP
THm METHOD Dm i nON LMIT— RKVUION
1.11
AmNDa C TO PART 186— INDUCTIVELY Cov-
PLSD PLASMA— ATOMIC EMISSION SPBC-
TROMBTR1C METHOD POR TRACT BLEMBMT
ANALYSIS OP WATER AND WASTES METHOD
300.7
APPENDIX D TO PART 136— PRECISION AND RE-
COVERY STATEMENTS POR METHODS POR
MEASURING METALS
AUTHORITY: &a. an. SOKh). am and aoi(a).
Pub. L, 96-217. 91 Stat. 1606. et s»q. (83 U.8.C.
1161. et s»q.) (the Federal Water Pollution
Control Act Amendment* of 1972 a* amended
by the Clean Water Act of 1977).
The procedures prescribed herein
shall, except as noted in 1136.5, be used
to perform the measurements indicated
whenever the waste constituent speci-
fied is required to be measured for
(a) An application submitted to the
Administrator, or to a State having an
approved NPDBS program for a permit
under section 408 of the Clean Water
Act of 1977. as amended (CWA). and/or
to reports required to be submitted
under NPDES permits or other re-
quests for quantitative or qualitative
effluent data under parts 123 to 125 of
Title 40. and,
(b) Reports required to be submitted
by discharges under the NPDES estab-
lished by parts 124 and 125 of thlr chap
ter. and.
(c) Certifications Issued b y States
pursuant to section 401 of the CWA. as
unended.
[3s FR 287M. Oct. is. 1978, as amended at «
FR 43280. Oct. 26. 19M]
I ISA! DeftettkMM.
As used in this part, the term:
(a) Ad means the Clean Water Act of
1977, Pub. L. 95-217. 91 Stat. 1666, et req.
(33 U.8.C. 1161 et req.) (The Federal
Water Pollution Control Act Amend-
ments of 1972 as unended by the Clean
Water Act of 1977).
(b) Administrator means the Adminis-
trator of the U.S. Environmental Pro-
tection Agency.
(c) Regional Admtnittrator means one
of the EPA Regional Administrators.
(d) Director means the Director of the
State Agency authorised to carry out
an approved National Pollutant Dis-
charge Elimination System Program
under wctlon 402 of the Act.
(e) National Pollutant Discharge Elimi-
nation Svitem (NPDES) means the na-
tional system for the Issuance of per-
mits under section 402 of the Act and
includes any State o r interstate pro-
gram which has been approved by the
Administrator, in whole or in part.
pursuant to section 402 of the Act.
(f) Detection limit means the minimum
concentration of an analyte (sub-
stance) that can be measured and re-
ported with a 99% confidence that the
analyte concentration is greater than
sero as determined by the procedure
set forth at appendix B of this part.
[3i FR 26786, Oct. 16, 1973, as amended at «•
FR 4J380. Oct. 26, 19M)
313
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