United States Office of Water (WH-550D) EPA/570/9-90/008
Environmental Protection Washington DC 20460 April 1990
Agency
Manual for the
Certification of
Laboratories Analyzing
Drinking Water
Criteria and Procedures
Quality Assurance
Third Edition
Prepared by
The Laboratory Certification Program Revision Committee
Supersedes EPA/570/9-82/002, October 1982, entitled Manual for the Certification of
Laboratories Analyzing Drinking Water
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Notice
This manual has been reviewed by the Office of Drinking Water and the Office of
Research and Development and approved for publication. The mention of
commercial products does not constitute endorsement by the U.S. Environmental
Protection Agency.
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Acknowledgments
This manual was prepared through the efforts of many individuals, including
representatives from U.S. Environmental Protection Agency program offices and
laboratories, Regional offices, States, and utility laboratories. The principal
contributors are listed below.
Executive Committee, Laboratory Certification Program Revision
J. Cotruvo (ODW) A. Perler (Advisor)
T. Clark (EMSL-CI) P. Berger (Advisor)
R. Booth (EMSL-CI)
Steering Committee, Laboratory Certification Program Revision
P. Berger, Program Manager (ODW)
B. Bathija, Deputy Program Manager (ODW)
H. Brass (ODW)
T. Clark (EMSL-CI)
D. Easterly (EMSL-LV)
G. Englund (Minnesota)
G. Foree (Region VII)
E. Geldreich (RREL)
W. Knight (Region IV)
J. Lichtenberg (EMSL-CI)
C-K. Liu (EMSL-LV)
H. Nash (RREL)
A. Perler (ODW)
D. Pickering (Washington Aqueduct)
I. Pomerantz (ODW)
M. Silver (OGC)
A. Tiedemann (Virginia)
J. Trax (ODW)
N. Wentworth (QAMS)
J. Cole (ODW)
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Implementation Subcommittee
T. Clark, Chairman (EMSL-CI)
B. Bathija (ODW)
P. Berger (ODW)
D. Easterly (EMSL-LV)
G. Hicks (Cincinnati Water Works)
W. Hausler (Iowa)
C. Jones (Region III)
C-K. Liu (EMSL-LV)
C. Ryan (Region I)
P. Ryker (Kentucky)
R. Thomas (EMSL-CI)
J. Winter (EMSL-CI)
A. Wolfgang (Colorado)
Quality Assurance Management Subcommittee
I. Pomerantz, Chairman (ODW)
B. Bathija (ODW)
P. Berger (ODW)
J. Cole (ODW)
R. Graves (EMSL-CI)
D. Pickering (Washington Aqueduct)
C. Ritchey (Region VI)
N. Roberts (Louisiana)
P. Stamp (Region IV)
A. Tiedemann (Virginia)
J. Trax (ODW)
N. Wentworth (QAMS)
J. Westrick (ODW)
Technical and Quality Control Subcommittee
J. Lichtenberg, Chairman (EMSL-CI)
Chemistry Subgroup
G. McKee, Chairman (EMSL-CI)
J. Barron (ODW)
B. Bathija (ODW)
D. Beesley (North Carolina)
J. Blosser (Nebraska)
P. Britton (EMSL-CI)
B. Fleck (Illinois)
M. Gomez-Taylor (ODW)
J. Longbottom (EMSL-CI)
J. Pfaff (EMSL-CI)
R. Thomas (EMSL-CI)
IV
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Microbiology Subgroup
H. Nash, Chairman (RREL)
P. Berger (ODW)
R. Bordner (EMSL-CI)
T. Covert (EMSL-CI)
A. Dufour (EMSL-CI)
E. Geldreich (RREL)
R. Gentry (Region IV)
M. Long (Region V)
D. Reasoner (RREL)
G. Rice (RREL)
P. Ryker (Kentucky)
L. Shadix (ODW)
J. Standridge (Wisconsin)
J. Vasconcelos (Region X)
Radiochemistry Subgroup
C-K. Liu, Chairman (EMSL-LV)
F. Novielli (EMSL-LV)
D. Easterly (EMSL-LV)
R. Cothern (EPA Science Advisory Board)
S. Gold (EMSL-CI)
R. Holloway (EMSL-LV)
D. McCurdy (Massachusetts)
R. Tauer (Region VIII)
G. Uyesugi (California)
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Preface
Since 1978, the U.S. Environmental Protection Agency (EPA) has had a
program for certifying Regional laboratories, principal State laboratories in
primacy States, and local laboratories in non-primacy States performing
drinking water analyses required by regulations issued pursuant to the Safe
Drinking Water Act. This document is the third edition of the manual
describing the program's implementation procedures and technical criteria. It
supersedes the Manual for the Certification of Laboratories Analyzing Drinking
Water, EPA-570/9-82-002 (October 1982).
This revision was necessary to address the increased complexity of the
revised drinking water regulations, clarify Regional responsibilities concerning
State laboratory certification programs, reduce the time a laboratory can be
"provisionally certified," and improve feedback to EPA on how laboratories
perform on a routine basis. This edition is based on an ongoing review of the
laboratory certification program to improve implementation and technical
criteria in light of newly approved methodology and six additional years of
experience with the program.
The document was prepared by a committee chaired by the EPA's Office of
Drinking Water (ODW). Comments from the Regions and States were
solicited and considered at several points in the preparation of this revision.
These included recommendations from a workshop held in April 1987, at
which all Regions and States were invited to share their views about both the
implementation strategy and the technical criteria. Regions and States were
represented on the revision steering committee and its various subcommittees
and subgroups.
The EPA quality assurance program covers all activities relating to data
collection, processing, and reporting. This is managed by the Office of
Research and Development, Quality Assurance Management Staff (QAMS).
This manual represents ODW's implementation of the QAMS program
applicable to laboratories conducting drinking water analyses.
Like the previous edition, this program is not regulatory in nature (except for
analytical methodology and requirements in the primary drinking water
regulations), but rather offers guidance describing the recommended
procedures and criteria for assuring data validity. Laboratories may use
equivalent criteria, if these criteria are approved by the certifying authority.
EPA is currently developing new regulations for laboratory certification and
certain pre-laboratory and post-laboratory activities. The Agency is
undertaking this effort to ensure that all primacy States include in their
certification programs those few basic elements that the Agency regards as
critical to assuring data validity (e.g., certification downgrading procedures,
training of on-site evaluators). EPA does not expect that the recommended
procedures and criteria in this manual will conflict with these forthcoming
regulations.
VI
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Unlike previous editions, this edition is in a loose-leaf format which will allow
EPA to more easily update it from time to time. EPA will furnish revised pages
to each State drinking water administrator and State laboratory director.
Holders of this manual should check with the EPA Region or the State
occasionally to make sure their manual is current.
In conclusion, EPA will use the certification criteria in this manual for
evaluating all laboratories that it certifies (Regional laboratories, principal State
laboratories, and local laboratories in non-primacy States). The Agency will
also use this manual as guidance in determining the adequacy of State
certification programs for local laboratories.
VII
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Contents
Page
CHAPTER I: INTRODUCTION 1
CHAPTER II: RESPONSIBILITIES 3
Office of Drinking Water 3
Office of Research and Development 3
Regional Offices 3
Drinking Water Laboratory Certification Work Group 4
CHAPTER III: IMPLEMENTATION 5
Regional Laboratories and Programs 5
Principal State Laboratories 5
Local Laboratories 6
Other Considerations for Certification 7
Quality Assurance Plan 7
Performance on Routine Water Samples 8
Chain-of-Custody Procedures 8
Requirements for Maintaining Certification Status 8
Criteria and Procedures for Downgrading/Revoking
Certification Status 8
Reciprocity 10
Training 10
Technical Services 11
Reference Samples 11
Early Warning System for Problems with Test
Supplies and Equipment 11
Alternate Analytical Techniques 14
CHAPTER IV: CHEMISTRY 15
1. Personnel 15
2. Laboratory Facilities 16
3. Laboratory Equipment and Instrumentation 16
4. General Laboratory Practices 16
5. Analytical Methodology 16
6. Sample Collection, Handling, and Preservation 17
7. Quality Assurance 17
8. Records and Data Reporting 18
9. Action Response to Laboratory 19
IX
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Contents (continued)
Page
CHAPTER V: MICROBIOLOGY 37
1. Personnel 37
2. Laboratory Facilities 37
3. Laboratory Equipment and Instrumentation 37
4. General Laboratory Practices 40
5. Analytical Methodology 42
6. Sample Collection, Handling, and Preservation 43
7. Quality Assurance 43
8. Records and Data Reporting 44
9. Action Response to Laboratory 44
CHAPTER VI: RADIOCHEMISTRY 59
1. Personnel 59
2. Laboratory Facilities 59
3. Laboratory Equipment and Instrumentation 60
4. General Laboratory Practices 61
5. Analytical Methodology 61
6. Sample Collection, Handling, and Preservation 61
7. Quality Assurance 61
8. Records and Data Reporting 62
9. Action Response to Laboratory 62
APPENDICES
Appendix A: Chain-of-Custody 75
Appendix B: Recommended Protocol for Regions Conducting
On-site Laboratory Evaluations 81
Appendix C: Abbreviations 83
Appendix D: EPA Policy on Third Party Certification 85
Appendix E: Required Analytical Capability for
Principal State Laboratory Systems 87
Appendix F: Additional Contaminants Scheduled for
Future Rules (Rest of the 83) 89
Appendix G: §1445 Unregulated Chemicals to be
Monitored (Listed or Proposed) 91
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Chapter I
Introduction
Public water systems serving at least 25 persons or
having at least 15 service connections must comply
with the Safe Drinking Water Act and the
requirements of the National Primary Drinking Water
Regulations (40 CFR Part 141). Section 1401(1)(D) of
the Act defines a National Primary Drinking Water
Regulation to include "criteria and procedures ... [for]
quality control and testing procedures to insure
compliance ...." 40 CFR Part 142 sets out imple-
mentation requirements.
The regulations at 40 CFR 142.10(b)(4) require a
State that has primary enforcement responsibility
(primacy) to have laboratory facilities available which
have been certified by EPA (see Table 1-1). The
regulations at 40 CFR 141.28 require that all testing
for compliance purposes, except for turbidity, free
chlorine residual, temperature, and pH, be performed
by laboratories certified by the State. This manual is
intended to assist EPA in implementing 40 CFR
142.10(b)(4) by specifying procedures for certifying
principal State laboratories. States with primacy may
also choose to use equivalent, nonidentical criteria
and procedures to those in this manual for their own
certification programs.
Table 1-1. Primacy Requirements for States
To obtain and maintain primary enforcement responsibility
("primacy"), a State must comply with 40 CFR 142 10, which
includes the following two provisions:
"The establishment and maintenance of a State program for the
certification of laboratories conducting analytical measurements of
drinking water contaminants pursuant to the requirements of the
State primary drinking water regulations including the designation
by the State of a laboratory officer, or officers, certified by the
Administrator, as the official(s) responsible for the State's
certification program. The requirements of this paragraph may be
waived by the Administrator for any State where all analytical
measurements required by the State's primary drinking water
regulations are conducted at laboratories operated by the State
and certified by the Agency." (40 CFR I42.l0(b)(3(i))
"Assurance of the availability to the State of laboratory facilities
certified by the Administrator and capable of performing analytical
measurements of all contaminants specified in the State primary
drinking water regulations ..." (40 CFR 142.10(b)(4))
The EPA laboratory certification program extends to
its Regional laboratories, principal State laboratories
in primacy States, and laboratories that perform
analyses under the Safe Drinking Water Act in States
without primacy. Primacy States must have a
certification program for local laboratories if all
analyses are not performed in principal State
laboratories (See Table 1-1). The State certification
program may involve a third party certifier (see
Appendix D).
EPA's Environmental Monitoring Systems Laboratory
in Cincinnati, Ohio (EMSL-CI), is responsible for
determining what certification status is warranted for
EPA Regional laboratories in microbiology and
chemistry. The Environmental Monitoring Systems
Laboratory in Las Vegas (EMSL-LV) has this
responsibility for radiochemistry. Regional certification
officers are responsible for the certification of the
principal State laboratory in each primacy State and
are also responsible for all laboratories in non-primacy
States. Evaluations of all laboratories for
radiochemistry are conducted by EMSL-LV, except
where the Regions have this capability.
Primacy States with certification programs are
responsible for certifying local laboratories, i.e.,
laboratories other than the principal State laboratory.
Under EPA's program, principal State laboratories are
expected to successfully analyze a complete set of
unknown performance evaluation (PE) samples from
EMSL-CI (or EMSL-LV, where applicable) at least
annually and pass an on-site evaluation every three
years. Regional laboratories must successfully
analyze a set of PE samples at least annually for all
regulated contaminants for which they conduct
analyses and pass an on-site evaluation at least every
three years. The criteria in this manual will be used
for the on-site evaluation.
Chapter II describes the responsibilities of each of the
EPA organizations for this certification program.
Chapter III describes how the program operates.
Chapters IV, V and VI cover the technical criteria for
chemistry, microbiology, and radiochemistry,
respectively, used during an on-site evaluation of a
laboratory. Evaluation forms are also included in
Chapters IV, V and VI.
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The appendices include: recommended cham-of- the capability to analyze; a list of not yet regulated
custody procedures; a recommended protocol and contaminants which EPA is scheduled to regulate;
format for conducting on-site laboratory evaluations, and a list of unregulated chemicals which systems
which may be used by the evaluators; abbreviations; must monitor under §1445 of the Safe Drinking Water
EPA's policy on third-party certification; a list of Act.
contaminants a principal State laboratory must have
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Chapter II
Responsibilities
The success of the laboratory certification program
depends upon cooperation among the organizations
responsible for its implementation. Within the Agency,
primary responsibilities for laboratory certification are
shared by the Office of Drinking Water (ODW), the
Office of Research and Development (ORD), and the
Regional Offices. The Drinking Water Laboratory
Certification Work Group (DWLC) is a standing group
that reviews problems and provides guidance.
Office of Drinking Water (ODW)
ODW is responsible for developing and implementing
the national certification program for laboratories that
analyze drinking water samples and for implementing
the Safe Drinking Water Act, including the preparation
of regulations and standards.
Office of Research and Development
(ORD)
EMSL-CI and EMSL-LV share responsibility with
ODW for developing and implementing the laboratory
certification program.
EMSL-CI is the lead organization for managing the
national certification program for laboratories
performing chemical and microbiological analyses. Its
responsibilities include:
• Reviewing EPA Regional certification programs
and conducting on-site evaluations of each
Regional laboratory every three years to determine
whether a change in the certification status is
warranted;
• Preparing and distributing PE samples and quality
control (QC) samples for regulated chemical and
microbiological contaminants (when available) and
calibration standards for organic contaminants, as
appropriate;
• Conducting water supply performance evaluation
studies at least annually for all Regional and
principal State laboratories. Other laboratories may
participate in these studies, if EPA resources
allow, by submitting their requests to the State
laboratory officer(s) for forwarding to EPA;
• Evaluating the resources and personnel available
in each EPA Region to carry out the certification
program;
• Developing and participating in training courses to
support the certification program; and
• Providing technical assistance to EPA and the
States, as required, and participating in DWLC
Work Group activities.
EMSL-LV is the lead organization for managing the
certification program for laboratories performing
radiochemical analyses. Its duties correspond to
those described for EMSL-CI. In addition, at the
request of a Region, EMSL-LV is responsible for
conducting on-site evaluations for radiochemistry of
principal State laboratory systems and, if resources
are available, other laboratories. In these cases,
EMSL-LV will report the results of its inspections to
the responsible Regional Administrator, who will have
final authority to determine certification status.
EPA Regions
The ten Regions oversee progress of the certification
program in the States. The Regions are responsible
for:
• Determining what certification status is warranted
for the principal State laboratory in each primacy
State and the local laboratories in non-primacy
States, including an on-site evaluation of each
such laboratory at least once every three years
(the Regional Administrator or designee is the
certifying authority). Regions will provide the
laboratory with an evaluation report within 45 days
of the on-site evaluation;
• Coordinating EMSL water supply performance
evaluation studies with laboratories in the Region;
• Performing an annual review of State certification
programs and performance evaluation reports and
monitoring the adequacy of State programs for
certifying laboratories, as described below;
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• Providing technical assistance to EPA-certified
drinking water laboratories, as needed;
• Operating the certification program in non-primacy
States; and
• Insuring that the Regional laboratory, if one exists,
is certified and meets the criteria in this manual.
Regions are to monitor the adequacy of State
programs for certifying laboratories by periodically
assessing each program's scope, staffing, policy,
procedures, and effectiveness. The adequacy of
these essential program elements are to be monitored
by:
• Evaluating and acting as approval authority for the
State's certification program. The Region must
review the program plan/regulation (including
program description), responsibilities, organi-
zational structure, staff (including educational
background and experience), scope and
description of the certification process and
certification downgrading criteria and procedures,
and use of PE samples;
• Requesting States to submit an annual program
report that includes program highlights, training
and continuing education efforts, number of on-site
evaluations performed, listing of laboratories
certified by discipline or contaminant, and any
certification downgrading or upgrading actions
along with reasons for those actions;
• Observing selected State on-site evaluations of
local laboratories to allow Regional certification
specialists to evaluate specific elements of the
State certification program;
• Allowing State evaluators to participate in Regional
on-site evaluations of the principal State laboratory
to provide experience for State evaluators; and
• Hosting annual meetings of State certification
officers to discuss program issues, policies, and
problems. Key Regional, EMSL, and Headquarters
personnel should be invited to participate.
In addition to its laboratory certification duties, the
Region has administrative, enforcement, and local
laboratory certification responsibilities in non-primacy
States. Some of these duties may be performed by
the State, but the Region must retain responsibility for
the on-site evaluation of the designated principal
State laboratory. Local laboratories may be evaluated
by the Region, or under a Region-approved program
carried out by a designated principal State laboratory.
In either case, this manual will be the basis for the
on-site evaluations of State and local laboratories
conducted by the EPA Region in non-primacy States.
Drinking Water Laboratory Certification
Work Group
The Drinking Water Laboratory Certification Work
Group is responsible for overseeing the operation of
the national certification program for drinking water
laboratories. This group advises ODW and includes
representatives from ODW, ORD (EMSL-CI, EMSL-
LV, Risk Reduction Engineering Laboratory, and
QAMS), Office of Water Enforcement and Permits,
Regional Offices and States. The Work Group's
responsibilities include:
• Monitoring the certification program and
recommending technical and administrative
revisions to ODW as dictated by experience or
updated information;
• Developing guidance and responding to questions
and comments from the Regions;
• Developing technical and administrative criteria to
support additional certification needs imposed by
future regulations;
• Ascertaining laboratory availability and capability
for future regulatory activities; and
• Making recommendations to ODW on resources
needed to implement the certification program.
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Chapter III
Implementation
EPA Regional Laboratories and
Programs
EMSL-CI is responsible for certifying the Regional
laboratory to perform microbiological and chemical
analyses. It also approves the Regional program for
certifying other laboratories to perform these same
analyses. EMSL-LV has similar responsibilities for
Regions that have radiochemistry capabilities. EMSL-
CI (or EMSL-LV for radiochemistry) must approve the
Regional certification program before a Region can
exercise its authority to certify other laboratories. The
certifying authority resides with the Director, EMSL-
CI, for microbiology and chemistry or with the
Director, EMSL-LV, for radiochemistry, or with their
respective designees.
Certification of Regional Laboratories
In order to be eligible to analyze compliance samples
under the Safe Drinking Water Act, EPA Regional
laboratories must meet the minimum criteria specified
in the manual, pass an on-site inspection at least
once every three years, and satisfactorily analyze an
annual set of PE samples or other unknown test
samples, as specified by regulations or this guidance.
For those Regions certified for radiochemistry,
satisfactory performance on two intercomparison
samples per year is also necessary. EMSL-LV
currently provides intercomparison samples to
laboratories without charge, but this may change in
the future. The EMSLs will use the same criteria and
procedures for certifying Regional laboratories as the
Regions use for principal State laboratories.
Individual(s) Responsible for Certification
Program
Each EPA Regional Administrator or designee will
appoint an individual(s) to coordinate drinking water
certification activities. This mdividual(s) must be
experienced in quality assurance; hold an advanced
degree or have equivalent experience in microbiology,
chemistry, or radiochemistry; and have sufficient
administrative and technical stature to be considered
a peer of the director of the principal State laboratory.
On-Site Evaluation Team
One or more teams must be established by the
Region to evaluate a laboratory in microbiology and
chemistry. Team members must be experienced
professionals and hold at least a bachelor's degree,
(or equivalent education and experience) in the
specific discipline being evaluated. Team members
must complete a laboratory certification course
presented by EMSL-CI and pass the course
requirements.
Development of Regional Plans for Certifying
Local Laboratories in Non-Primacy States
Regions are required to develop plans for certifying
local drinking water laboratories in non-primacy
States. Written plans should include the following:
• Designation of certification official;
• Types and numbers of laboratories to be
evaluated;
• Specific types of analyses to be examined;
• Schedule for on-site evaluations; and
• Plans for providing technical assistance to
laboratories in need of upgrading.
Principal State Laboratories
The principal state laboratory system must have the
capability to analyze every contaminant included in
the drinking water regulations (40 CFR 142.10(b)(4));
however, an individual laboratory that is part of a
principal State laboratory system may be certified for
only one, several, or all the cited analyses. If a
principal State laboratory contracts with another
laboratory, including a laboratory outside the State, to
assume the lead role in analyzing a regulated
parameter (e.g., radiochemical contaminants), that
contract laboratory will, for the purposes of this
manual, be considered part of the principal State
laboratory system. In this case, the contract
laboratory must be certified by EPA, unless the
contract laboratory is in another State, and that State
has certified the laboratory for the contaminants of
interest, with the concurrences of the two affected
EPA Regions.
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The certification process for a principal State
laboratory will begin when the laboratory director or
State certification officer makes a formal request to
the Region. The Regional certification officer may
also initiate a request for certification. This application
may result from the following:
• A request for first-time certification for
microbiology, chemistry, and/or radiochemistry;
• A request for certification to analyze additional or
newly regulated contaminants; and
• A request to reapply for certification after
correction of deficiencies which resulted in the
downgrading/revocation of certification status.
The Region should respond to a formal application for
any of the requests within 30 days, and a mutually
agreeable date and time should be set for the on-site
laboratory evaluation. The recommended protocol for
conducting these evaluations is given in Appendix B.
EPA will only certify laboratories that pass an on-site
inspection (see Chapters IV, V, and VI for inspection
checklists) and satisfactorily analyze performance
evaluation samples (or other unknown test samples
for those contaminants for which it requests
certification).
After the on-site visit and the review of PE sample
results, the Region can classify the laboratory for
each type of analysis according to the following rating
scheme:
• Certified — a laboratory that meets the minimum
requirements of this manual and all applicable
regulatory requirements. The certification shall be
valid for up to three years;
• "Provisionally Certified"—a laboratory that has
deficiencies but demonstrates its ability to
consistently produce valid data; and
• Not Certified—a laboratory that possesses major
deficiencies and, in the opinion of the Regional
Administrator, cannot consistently produce valid
data within specified acceptance limits.
A "provisionally certified" laboratory may analyze
drinking water samples for compliance purposes.
However, in no case should provisional certification
be given if the evaluation team believes that the
laboratory cannot perform an analysis within
acceptance limits. Furthermore, neither "certified" nor
"provisionally certified" status may be granted to any
laboratory that has not met the performance criteria
specified in any National Primary Drinking Water
Regulation.
For laboratories requesting first-time certification or
certification to analyze additional or newly regulated
contaminants, the Region may administratively grant a
laboratory "provisionally certified" status, as specified
in a drinking water regulation, pending an on-site
evaluation. "Provisionally certified" status is granted
only when the Region judges that the laboratory has
both the appropriate instrumentation and trained
personnel to perform the analyses, and that the
laboratory has satisfactorily analyzed PE samples for
the contaminants in question. Regions should perform
an on-site evaluation as soon as possible, but in no
case later than seven months after it has granted the
laboratory "provisionally certified" status.
For those Regions lacking the expertise required to
certify laboratories in radiochemistry, ESML-LV will
conduct on-site inspections.
Local Laboratories
For the purposes of this document, local laboratories
include any State, county, municipal, utility, Federal,
or commercial laboratory, but exclude principal State
laboratories and EPA Regional laboratories. In non-
primacy States, the Regions will certify local
laboratories using the criteria and policies in this
manual.
Only those primacy States where not all drinking
water analyses are conducted at State-operated
laboratories are required to establish a certification
program for local laboratories (see 40 CFR
1422.10(b), Table 1-1.). All States, however, are
encouraged to develop such programs. Certification
can be based either upon criteria contained in this
manual or upon State-developed equivalents that are
in accordance with this manual, as determined by
EPA. In addition, all State certification programs must
require compliance with all related provisions of any
National Primary Drinking Water Regulation. Those
States required by regulation to develop a certification
program must appoint a laboratory certification
officer(s), certified by EPA, as the official(s)
responsible for the State program.
The principal State laboratory system must have the
technical capability to analyze for all regulated
contaminants. If a principal State laboratory system
has the intent and resources to perform 100% of the
analyses for some contaminants, it need not include
certification criteria for those contaminants. But, if the
principal State laboratory system does not perform
100% of the analyses for other contaminants (e.g., it
only analyzes 20% of all total coliform samples), then
the State certification program must include those
contaminants.
For the purpose of certification, Federal laboratories
that analyze compliance samples, and other
laboratories that analyze compliance samples for
Federal facilities, are local laboratories and must,
therefore, be certified by the State or EPA. If
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requested by the State, the Region may carry out
certification activities for Federal laboratories in that
State.
EPA will certify individual laboratories on Federal
Indian lands, if requested by the tribal chairperson, as
resources allow.
EPA operates the certification program for local
laboratories in non-primacy States. The criteria,
procedures, and mechanism EPA uses to certify local
laboratories are the same as those for principal State
laboratories, except that a local laboratory does not
have to possess the capability to analyze every
regulated contaminant.
Other Considerations for Laboratory
Certification
Laboratory Quality Assurance Plan
It is essential that all laboratories analyzing drinking
water compliance samples adhere to defined quality
assurance procedures. This is to insure that routinely
generated analytical data are scientifically valid and
defensible and are of known and acceptable precision
and accuracy. To accomplish these goals, each
laboratory should prepare a written description of its
quality assurance activities (a QA plan). The following
items should be addressed in each QA plan:
1. Sampling procedures;
2. Sample handling procedures;
— specify procedures used to maintain
integrity of all samples, i.e., tracking
samples from receipt by laboratory through
analysis to disposal;
— samples likely to be the basis for an
enforcement action may require special
safeguards (see Cham-of-Custody
procedures).
3. Instrument or equipment calibration
procedures and frequency of their use;
4. Analytical procedures;
5. Data reduction, validation and reporting;
— data reduction: conversion of raw data to
mg/L, picocunes/L, coliforms/100ml_, etc.
— validation: includes insuring accuracy of
data transcription and calculations.
— reporting: includes procedures and format
for reporting data to utilities, State officials,
and EPA.
6. Types of quality control
frequency of their use;
(QC) checks and
— may include preparation of calibration
curves, instrument calibrations, replicate
analyses, use of EMSL-provided QC
samples or calibration standards and use of
QC charts^.
7. Preventive maintenance procedures and
schedules;
8. Specific routine procedures used to determine
data precision and accuracy for each
contaminant measured;
— precision is based on the results of
replicate analyses.
— accuracy is normally determined by
comparison of results with "known"
concentrations in reagent water standards
and by analyses of water matrix samples
before and after adding a known
contaminant "spike."
9. Corrective action contingencies;
— response to obtaining unacceptable
results from analysis of PE samples and
from internal QC checks.
10. Laboratory organization and responsibility;
— include a chart or table showing the
laboratory organization and line authority.
— list the key individuals who are responsible
for ensuring the production of valid
measurements and the routine assessment
of measurement systems for precision and
accuracy (e.g., who is responsible for
internal audits and reviews of the
implementation of the plan and its
requirements).
The QA plan may be a separately prepared QA
document or may incorporate, by reference, already
available standard operating procedures (SOPs) that
are approved by the laboratory director and that
address the listed items. Documentation for many of
the listed QA plan items can be made by reference to
appropriate sections of this manual, to the
laboratory's SOPs, or to other literature (e.g.,
1QC chart for chemistry is explained in Standard Methods for the
Examination of Water and Wastewater, 16th ed., 1985, pp. 25-
32. QC chart for rachochemistry is explained in Handbook for
Analytical Quality Control and Radioactivity Analytjcal
Laboratories, EPA-600/7-77-088, August 1977.
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Standard Methods for the Examination of Water and
Wastewater).
If a particular listed item is not relevant, the QA plan
should state this and provide a brief explanation (e.g.,
some laboratories do not collect samples and thus
are not required to describe sampling procedures). A
laboratory QA plan should be concise but responsive
to the above-listed items (a maximum of five pages is
suggested). Minimizing paperwork while improving
dependability and quality of data are the intended
goals.
Performance on Routine Water Samples
Each EPA Region will develop a strategy to assess
laboratory performance on routine water samples as
part of its certification program for principal State
laboratories in primacy States, and for local
laboratories in non-primacy States. This strategy may
include one or more of the following approaches or
some other approach: (1) send the laboratory a blind
audit sample, (2) perform an unannounced on-site
evaluation, (3) require laboratory to analyze an
unknown sample during the on-site evaluation, or (4)
arrange a split sample program with the laboratory.
Each Region should develop a written plan, approved
by EMSL-CI and concurred in by ODW, that
addresses this issue.
Chain-oi'-Custody Procedures
Certified laboratories, when requested to process a
sample for possible legal action against a supplier,
must use an adequate chain-of-custody procedure.
An example of such a procedure is found in Appendix
A.
Requirements for Maintaining
Certification Status
Periodic Performance Evaluation (PE) Samples
and Other Unknown Test Samples
Certified drinking water laboratories must satisfactorily
analyze PE samples (all concentration levels
provided) or other unknown test samples at least
once annually for each chemical, radiochemical, or
microbiological analyte (when available) for which
certification has been granted. However, in some
cases, EPA will permit certification of a group of
related analytes (e.g., volatile organic chemicals) on
the basis of a limited number of analytes in that
group. If the laboratory does not analyze an analyte in
the PE sample, or other unknown test sample, within
the acceptance limits established by EPA, the
certifying authority must follow the procedure
discussed in the section entitled, "Criteria and
Procedures for Downgrading/Revoking Certification
Status." To maintain certification in radiochemistry,
the laboratory must satisfactorily analyze two
intercompanson samples per year in addition to the
annual set of PE samples. The laboratory should be
able to provide evidence that the person(s) analyzing
any PE sample is a laboratory employee who
routinely analyzes drinking water compliance
samples.
Methodology
Laboratories must use methodologies specified by the
drinking water regulations (40 CFR 141.21 - 141.30,
141.41, 141.42).
Notification of Certifying Authority (CA) for Major
Changes
Laboratories certified by EPA must notify the
appropriate CA (Regional Administrator, or designee,
or the appropriate EMSL), in writing, within 30 days of
major changes in personnel, equipment, or laboratory
location which might impair analytical capability. A
major change in personnel is defined as the loss or
replacement of the laboratory supervisor or a situation
in which a trained and experienced analyst is no
longer available to analyze a particular parameter for
which certification has been granted. The CA will
discuss the situation with the laboratory supervisor
and establish a schedule for the laboratory to rectify
deficiencies. If the CA determines that the laboratory
can no longer produce valid data, the CA must begin
certification downgrading actions, including revoking
certification, when warranted.
On-Site Evaluation
The CA must be satisfied that a laboratory is
maintaining the required standard of quality for
certification. Normally, this will be based upon
recommendation of an EPA on-site evaluation
conducted at least every three years. If the laboratory
undergoes a major change, however, or if it fails a PE
sample or other unknown test sample, the CA should
consider an evaluation sooner.
Criteria and Procedures for
Downgrading/Revoking Certification
Status
Criteria for Downgrading Certification Status
A laboratory will be downgraded to "provisionally
certified" status for a particular contaminant analysis
for any of the following reasons:
1. Failure to analyze a PE sample (or an EMSL-
LV intercomparison sample or any other
unknown test sample) within the acceptance
limits established by EPA. Failure on a PE
sample is defined as a failure on any
concentration provided, unless otherwise
specified by ODW or EMSL-CI for a particular
PE study;
2. Failure of a certified laboratory to notify the CA
within 30 days of major changes which might
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impair analytical capability (e.g., in personnel,
equipment, or laboratory location);
3. Failure to satisfy the CA that the laboratory is
maintaining the required standard of quality,
based upon an EPA on-site evaluation; or
4. Failure to notify the State and/or the public
water system in a timely manner of
unsatisfactory results on water samples,
thereby preventing compliance with Federal
and/or State reporting requirements.
Procedures for Downgrading to "Provisionally
Certified" Status
If a laboratory is subject to downgrading on the basis
of the indicated criteria, the CA will notify the
laboratory director or owner, in writing (by registered
or certified mail), within 14 days. The laboratory
director will review the problems cited and, within 30
days of receipt of the letter, send a letter to the CA
specifying what corrective actions are being taken.
The CA will consider the adequacy of the response
and notify the laboratory by mail, within 14 days of
receipt, of its certification status. The CA will follow
up to insure that corrective actions have been taken.
If a laboratory fails to analyze an unknown test
sample within the acceptance limits established by
EPA, the CA will not downgrade certification if the
laboratory identifies and corrects the problem to the
CA's satisfaction within 30 days of being notified of
the failure. If, after review of the submitted
information, the CA determines that the laboratory
need not be downgraded, then within two months of
this decision, the CA will send the laboratory another
unknown sample containing the failed contaminant
(see Figure 111-1). If the laboratory analyzes this
second unknown sample within the acceptance limits
established by EPA (using the most recent PE
summary statistical compilations from EMSL), the
laboratory will not be downgraded. If the laboratory
fails to analyze this second unknown sample within
the established limits, the CA will downgrade the
laboratory to "provisionally certified" status and notify
the laboratory, in writing, by registered or certified
mail. Laboratories should be downgraded only for the
analyte failed, except where EPA certifies a group of
related analytes based on a limited number of
analytes in that group.
During any phase of this procedure, a laboratory may
request that EPA provide technical assistance to help
identify and resolve any problem.
Once the CA notifies a laboratory, in writing, that it
has been downgraded to "provisionally certified"
status, the laboratory must correct its problem within
3 months for a procedural or administrative deficiency
and 6 months for an equipment deficiency. If the
laboratory was downgraded to "provisionally certified"
status because of a failure to analyze a PE sample
(or other unknown test sample) within the acceptance
limits specified by EPA, the laboratory must correct
its problems and satisfactorily analyze another PE
sample (or other unknown sample) within 2 months of
being notified. A "provisionally certified" laboratory
may continue to analyze samples for compliance
purposes, but must immediately notify its clients of its
downgraded status and provide that information, in
writing, on any report.
Criteria for Revoking Certification Status
A laboratory will be downgraded immediately from
"certified" or "provisionally certified" status to "not
certified" for a particular contaminant analysis for the
following reasons:
1. (For "provisionally certified" laboratories)
Failure to analyze a PE sample (or EMSL-LV
mtercomparison sample or any other unknown
test sample) for a particular contaminant within
the acceptance limits established by EPA (see
Figure 111-1);
2. Failure to satisfy the CA that the laboratory
has corrected deviations identified during the
on-site evaluations within 3 months for a
procedural or administrative deficiency or 6
months for an equipment deficiency;
3. Submission of a PE sample to another
laboratory for analysis and reporting data as its
own;
4. Falsification of data or other deceptive
practices; or
5. Failure to use analytical methodology specified
in the regulations.
Procedures for Revocation
The CA will notify the laboratory, in writing (by
registered or certified mail), of the intent to revoke
certification. If the laboratory wishes to challenge this
decision, a notice of appeal must be submitted in
writing to the CA within 30 days of receipt of the
notice of intent to revoke certification. If no notice of
appeal is so filed, certification will be revoked.
The notice of appeal must be supported with an
explanation of the reasons for the challenge and must
be signed by a responsible official from the laboratory
such as the president/owner for a commercial
laboratory, or the laboratory supervisor in the case of
a municipal laboratory.
Within 60 days of receipt of the appeal, the CA will
make a decision and notify the laboratory in writing.
Denial of the appeal will result in immediate
-------
Cert
i
Unknown Sample
2 Months
i
Pass 1
L Fail
1 ^
Proble
| Re
Acceptable
2 Months
i
Decertified
Fail'
HfirtifiPd ^ n
i
ults
4 1 Month
ults I Unkn
own
nple
2 Months A
r 2 Months T
new Provis
m and > > ^ Cert
pon Not Acceptable .
" i
r
Another
Unknown
Sample
h Month
onally
tied
L
Figure 111-1. Criteria and procedures for certification downgrading under the EPA Program on basis of unsatisfactory PE
samples.
revocation of the laboratory's certification. Once
certification is revoked, a laboratory may not analyze
drinking water samples for compliance until its
certification has been reinstated.
If the appeal is determined to be valid, the CA will
take appropriate measures to reevaluate the facility
and notify the laboratory, in writing, of its decision
within 60 days of the reevaluation.
Reinstatement of Certification
Certification will be reinstated when and if the
laboratory can demonstrate to the CA's satisfaction
that the deficiencies which produced "provisionally
certified" status or revocation have been corrected.
This may include an on-site evaluation, a successful
analysis of samples on the next regularly scheduled
EMSL water supply performance evaluation study, or
any other measure the CA deems appropriate.
Reciprocity
Reciprocity, which is defined as mutually acceptable
certification among primacy States, is strongly
endorsed by EPA as a highly desirable element in the
certification program for drinking water laboratories.
The new, more specific certification process should
instill greater confidence of comparable performance
by laboratories in different jurisdictions. EPA also
believes that a third party certifying agent used by
more than one State should promote reciprocity.
(EPA's policy on third party certification is described
in Appendix D.)
States are encouraged to adopt provisions in their
laws and regulations to permit reciprocity. Even
though ultimate responsibility for reciprocal
certification resides with the primacy States, the
States may ask for the assistance of EPA in cases
involving reciprocity. Such requests should be
submitted to ODW through the Region.
Training
Training is an integral part of the laboratory
certification process for:
1. Personnel conducting on-site evaluations of
laboratories on behalf of either the Regional
Office or a primacy State, and
2. Laboratory analysts and samplers responsible
for microbiological, chemical and
radiochemical measurements.
Each Regional laboratory certification evaluator must
initially pass the laboratory certification training course
for chemistry or microbiology conducted by EMSL-CI.
10
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State and third party evaluators (see Appendix D) are
encouraged to take these courses. Mechanisms for
providing periodic upgrade training for both evaluators
and analysts should be examined by the Regions and
States. EMSL-CI will notify previous course
participants of major updates to their course manual.
Technical Services
Reference Samples
There are four types of EMSL reference samples:
calibration standards, quality control (QC),
performance evaluation (PE), and intercomparison
cross-check samples. EMSL-CI provides QC and PE
samples for all regulated chemical and microbiological
contaminants and residual chlorine and in addition,
provides calibration standards for trace organic
chemicals. EMSL-LV provides calibration standards,
PE, and intercomparison samples for all regulated
radiochemical contaminants. EMSL-CI and EMSL-LV
currently provide these samples without charge, but
this practice may change in the future.
QC samples and standards are provided on request
as part of a laboratory's own quality assurance
activities (see section on laboratory quality assurance
plans). Contaminant concentrations are furnished with
the samples. They serve as independent checks on
reagents, instruments, and analytical techniques; as
an aid for testing or training analysts; or for
determining precision and accuracy within the
laboratory. Although no certification or other formal
EPA evaluation functions result from using these
samples, their routine use is considered fundamental
to a proper laboratory QA plan.
EMSL-CI and EMSL-LV conduct periodic water supply
performance evaluation studies using PE samples as
a requirement for certification. In contrast to QC
samples and calibration standards, contaminant
concentrations are not furnished before analysis.
At the conclusion of each study, the EMSLs prepare
individual reports for each laboratory (indicating data
acceptable) on an analyte-by-analyte and sample-by-
sample basis and send them to the participants. The
certifying authority reviews the data with the
laboratory to identify and resolve problems (QC
samples and calibration standards are useful for this
purpose), and to determine certification status.
In addition to the annual PE sample requirement,
EMSL-LV also requires satisfactory performance in
two intercomparison studies per year.
Intercomparison samples differ from PE samples in
that the former contain only one or two radionuclides
(e.g., radium-226 and radium-228), while PE samples
for radiochemistry are complex mixtures of alpha,
beta, and photon-emitting radionuclides. (The one
exception is the mixed gamma intercomparison
sample, which may contain up to 5 radionuclides.) In
neither case are contaminant concentrations
furnished to the laboratory until after completion of
the study.
Early Warning System for Problems with Test
Supplies and Equipment
A voluntary national system has been established to
(1) identify potential problems with chemical and
microbiological test materials and equipment; (2)
notify the EPA, manufacturers, and users of these
problems; and (3) encourage improvements and
tighter quality control over the products. The
problems are concerned with performance, QA,
specification, design, and labeling of microbiological
media and membrane filters, chemical reagents, and
other supplies, equipment, and instrumentation used
in microbiological and chemical analyses of drinking
water. EMSL-CI has the responsibility for maintaining
a QA program on methodologies and test materials,
and serves as the focal point for identifying and
reporting to the users and the manufacturers
significant problems with such materials. The
following protocol is used:
1. State and local drinking water laboratories or
Regional staff members should report
microbiological and chemical problems by
phone or in writing to the Microbiology Section
(513-569-7319) or the Chemistry Research
Division (513-569-7309), respectively, of
EMSL-CI, EPA, 26 West Martin Luther King
Drive, Cincinnati, Ohio 45268. Forms for
written reports are provided in Figures III-2 and
III-3. A copy of the report should be sent to the
QA officer in the appropriate Region. For
radiochemistry problems, send Figure III-3 to
the Radioanalysis Branch, EMSL-LV, P.O. Box
93478, Las Vegas, NV 89193-3478; or phone
702-798-2136.
2. EMSL-CI/EMSL-LV will record the details of
the problem, including name and location of
the reporting laboratory; product type,
manufacturers, lot/catalog/model numbers and
date received; description of the problem;
specific observations; method of preparation,
and length and conditions of storage for media
or reagents; and data documenting
unacceptable test results.
3. EMSL-CI/EMSL-LV will then describe the
reported problem to the manufacturer, obtain
manufacturing and QA data, and discuss its
significance. Corrections or changes by the
manufacturer will be encouraged.
4. Based on the results of discussions with the
reporter(s) of the problem and manufacturer,
EMSL-CI/EMSL-LV will alert the Regional QA
Officers of possible problems with the product.
11
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Product* Date
Manufacturer
Address
Date Received Expiration Date
Lot No. Cat. No. Model No.
Description of Problem:*'
Name Phone No.
(Person Reporting)
Laboratory/Facility
Address
"Membrane filters, microbiological media, reagents, portable incubators, waterbaths, etc.
"Information should include the length and condition of storage, and the method of preparation for media and reagents. Specific observations,
quality control checks, and data that document unacceptable results are useful in describing the problem.
Send to: Microbiology Section, EMSL-CI, U.S. EPA, 26 W. Martin Luther King Drive, Cincinnati, OH 45268, or phone (513) 569-7319.
Figure III-2. Report of problem with microbiological supplies or equipment.
12
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Product' Date
Manufacturer
Address
Date Received Expiration Date
Lot No. Cat. No. Model No.
Description of Problem:"
Name Phone No.
(Person Reporting)
Laboratory/Facility
Address
"Chemicals, prepared reagents, instruments, etc.
"Information should include the length and condition of storage, and the method of preparation for reagents. Specific observations, quality
control checks, and data that document unacceptable results are useful in describing the problem.
Send to: Chemistry Research Division, EMSL-CI, U.S EPA, 26 W. Martin Luther King Drive, Cincinnati, OH 45268, or phone (513) 569-
7309.
Figure III-3. Report of problem with chemical supplies or equipment.
13
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The QA Officers will alert the appropriate EPA
and State personnel. This system is not
intended to label the media, reagents, or other
materials as unacceptable, but rather to alert
water laboratories that a problem may exist
and to determine if similar problems have been
observed elsewhere.
5. If multiple reports of the same problem are
received, EMSL-CI/EMSL-LV will inform the
manufacturer of a potentially broad-scope
problem and request samples from reporting
laboratories for testing.
6. If the product is unsatisfactory in these tests,
EMSL-CI/EMSL-LV will notify the manufacturer
and the Regional QA Officers who, in turn, will
notify the Regional, State, and local
authorities.
Alternate Analytical Techniques
Although the drinking water regulations at 40 CFR
141.27 currently describe approval of limited alternate
analytical techniques, EPA no longer uses this
procedure and will propose to repeal this regulation.
In its place, the Agency is establishing a two-tiered
system for rapidly adopting new and revised analytical
technology for use by all laboratories. The first tier is
for new methods, significantly revised methods, or
new applications of currently approved methods.
These will be evaluated for equivalency by EMSL and
become candidates for accelerated regulation
development. Through formal proposal, public
comment, and promulgation in the Federal Register,
the list of methods approved for use by the National
Primary Drinking Water Regulations will be amended
accordingly, thus making the changes available to all
laboratories.
The second tier covers improvements to existing
methods which are optional and do not substantially
alter the method. These will be evaluated by EMSL
and become candidates for inclusion in a Federal
Register notice which EPA will periodically issue.
Rather than formally amending the regulations, this
notice will interpret the existing regulatory methods to
include minor optional changes. Analysts may use
these minor changes or continue to use the method
as originally promulgated.
This two-tiered process provides an avenue to
evaluate all methodology changes which would have
been handled under the old limited alternate test
procedures program. The new system makes
changes available to all laboratories and provides for
a more uniform system for compliance determination.
The process and requirements for obtaining EPA
approval for new or revised methods is described in
the document, "Requirements for Nationwide
Approval of New and Optionally Revised Methods for
Drinking Water Monitoring." N. S. Ulmer,
Environmental Monitoring Systems Laboratory,
Cincinnati, OH 45268. To obtain more specific
information, contact EMSL-CI at (513) 569-7453.
14
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Chapter IV
Chemistry
1. Personnel
1.1 Director
A laboratory's volume and scope of services may not
require this position. However, there should be a
person either in this position or an individual available
for consultation meeting the same requirements as
the Director. If the Director is also a supervisor, the
requirements of paragraph 1.2 are also to be met.
1.1.1 Academic training: Minimum bachelor's
degree in science is required. If bachelor's
degree is in a field other than chemistry, the
individual should have the number of credit
hours in chemistry equivalent to a minor in
chemistry.
1.1.2 Experience: Minimum of 2 years of
experience in a water laboratory is required.
1.2 Supervisor
Minimum requirements for the supervisor position are
listed below. If the supervisor is also an instrument
operator, the requirements of paragraph 1.3 are also
to be met.
1.2.1 Academic training: Bachelor's degree in
science that includes the number of credit hours
in chemistry courses required for a major in
chemistry.
1.2.2 Experience: Minimum of 1 year
experience in chemical analysis of water is
required.
1.3 Instrument Operators
Operators for the following instruments are needed:
Atomic Absorption (AA), Ion Chromatograph (1C), Gas
Chromatograph (GC), Gas Chromatograph/Mass
Spectrometer (GC/MS), Inductively Coupled Plasma-
Atomic Emission Spectrophotometer (ICP-AES),
Transmission Electron Microscope (TEM). The
following are minimum standards for these analyses.
1.3.1 Academic training: Bachelor's degree in
chemistry or related field. The analyst need not
have a bachelor's degree if the immediate
supervisor has a bachelor's degree in chemistry
or related field or if the analyst has the number
of credit hours in chemistry courses required for
a major in chemistry.
1.3.2 Specialized training: Satisfactory
completion of a short course in GC/MS, ICP or
TEM offered by equipment manufacturer,
professional organization, university, or other
qualified training facility is essential for these
operators. Specialized training for other
instruments is recommended.
1.3.3 Experience: Minimum of six months
experience in the operation of either AA, 1C,
GC, ICP or TEM. Minimum of 12 months
experience in the operation of the GC/MS. (See
paragraph 1.5.)
1.3.4 Initial qualification: After appropriate
training, it is essential that the analyst
demonstrate acceptable results in the analysis
of an applicable QC or PE sample.
1.4 Other Analysts
The following are required minimum standards for the
analyst position.
1.4.1 Academic training: Minimum of a high
school diploma or equivalent.
1.4.2 Initial qualification: After being trained
in a methods training course or by any qualified
analyst, the person being trained shall
demonstrate acceptable results in the analysis
of an applicable QC or PE sample.
1.5 Analysts and Operators in Training
Data produced by analysts and instrument operators
while in the process of obtaining the required training
or experience are acceptable when reviewed and
validated by a fully qualified analyst or the laboratory
supervisor.
7.6 Waiver of Academic Training Requirement
The certification officer may waive the need for the
specified academic training, on a case-by-case basis,
for highly experienced analysts.
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2. Laboratory Facilities
The laboratory facilities should be clean, have
temperature and humidity adequately controlled in the
instrument areas and have adequate lighting at the
bench top. It is important for the laboratory to have
provisions for the proper storage and disposal of
chemical wastes. Exhaust hoods are required for
preparation, extraction and analysis where applicable.
It is recommended that a minimum of 150 to 200
square feet/laboratory person be available. The
laboratory should contain at least 15 linear feet of
usable bench space per analyst. Workbench space
should be convenient to sink, water, gas, vacuum and
electrical sources free of surges. It is recommended
that the organic and inorganic facilities be separate
rooms. The analytical and sample storage area is to
be isolated from all potential sources of
contamination.
3. Laboratory Equipment and
Instrumentation
The laboratory is only required to have those
instruments that are needed to perform the approved
methods for which certification has been requested.
Those instruments must meet the specifications in
the checklist entitled "Required Equipment and
Instruments for Inorganic and Organic Contaminants".
4. General Laboratory Practices
4.1 General
4.1.1 Chemicals/reagents: "Analytical reagent
grade" (AR) chemicals or better are to be used
for analyses. Consult Standard Methods for the
Examination of Water and Wastewater, 16th ed.,
part 102, pp. 4-6 for more detailed information
on reagent grades. Individual analytical methods
in the approved reference may specify additional
requirements for the reagents to be used.
4.1.2 Laboratory safety: While specific safety
criteria are not an aspect of laboratory
certification, laboratory personnel should apply
general and customary safety practices as a
part of good laboratory procedure. Each
laboratory is strongly encouraged to have a
safety plan as part of their standard operating
procedure. Where safety practices are included
in an approved method, they must be strictly
followed.
4.2 Inorganic Contaminants
4.2.1 Reagent water: The laboratory is to
have a source of reagent water having a
sensitivity value of at least 0.5 megohms (less
than 2.0 micromhos/cm) at 25°C. High quality
water meeting such specifications may be
purchased from commercial suppliers. Quality of
reagent water is best maintained by sealing it
from the atmosphere. Quality checks to meet
specifications above should be made and
documented at planned intervals based on use.
This planned interval should not exceed one
month.
4.2.2 Glassware preparation: Glassware
should be washed in a warm detergent solution
and thoroughly rinsed first with tap water and
then with reagent water. This cleaning
procedure is sufficient for general analytical
needs, but the individual procedures must be
referred to for precautions to be taken against
contamination of glassware. It is advantageous
to maintain separate sets of suitably prepared
glassware for the nitrate, mercury, and lead
procedures due to the potential for
contamination from the laboratory environment.
4.3 Organic Contaminants
4.3.1 Reagent water: Reagent water for
organic analysis is to be free of interferences for
the analytes being measured. It may be
necessary to treat water with activated carbon
to eliminate all interferences.
4.3.2 Glassware preparation: Glassware and
sample bottles should be washed in a detergent
solution and thoroughly rinsed first in tap water
and then in reagent water. Glassware should
have a final organic solvent rinse or must be
baked at 400°C for 30 minutes and then dried
or cooled in an area free of organic
contamination. Glassware should be covered
with organic-free aluminum foil during storage.
Bottles and cap liners, used for collection of
samples for determination of volatile organic
chemicals (VOCs), should be dried at 105°C for
1 hr, sealed, and stored in an area free of
volatile organics.
5. Analytical Methodology
5.1 General
A list of approved methodology for inorganic and
organic contaminants can be found in Tables IV-1 and
IV-2, respectively. In general, all procedural steps in
these methods are considered requirements. Other
methods cannot be used unless approved by the
Agency. Contact the appropriate certifying authority
for an alternate test procedure application. Application
for the use of an alternate method may require
acceptable comparability data. Prepackaged test kits
other than the U.S. EPA-approved DPD and the
FACTS Colorimetric Test Kits are not approved for
use. Recommended methods for inorganic
contaminants that do not require the use of an
approved method are listed in Table IV-3.
16
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5.2 Free Chlorine Residual, Turbidity, pH and
Temperature
Free chlorine residual, turbidity, pH and temperature
measurements need not be made in certified
laboratories, but may be performed by any persons
acceptable to the State. The State should institute a
quality assurance program to assure validity of data
from these measurements.
5.2.1 Methodology: Only the EPA-approved
methodology listed in Table IV-1 can be used
for free chlorine residual and turbidity.
Recommended procedures for pH and
temperature are in Table IV-3.
5.2.2 Sealed liquid turbidity standards
purchased from the instrument manufacturer
must be calibrated against properly prepared
and diluted formazin or styrene divinylbenzene
polymer standards at least every 4 months in
order to monitor for any eventual deterioration.
This calibration is to be documented. These
standards are to be replaced when they do not
meet the criteria listed in Table IV-6. Solid
turbidity standards composed of plastic, glass,
or other materials are not reliable and should
not be used.
5.2.3 If visual comparison devices such as
color wheels or sealed ampules are used for
determining free chlorine residual, the standards
incorporated into such devices should be
calibrated at least every six months. These
calibrations are to be documented. Directions
for preparing temporary and permanent type
visual standards can be found in Method 408E,
Standard Methods, 16th ed., 1985. By
comparing standards and plotting such a
comparison on graph paper, a corrective factor
can be derived and applied to future results
obtained on the now calibrated apparatus.
6. Sample Collection, Handling, and
Preservation
The manner in which samples are collected and
handled is critical for obtaining valid data. It is
essential that a written sampling protocol with specific
sampling instructions be available to sample
collectors and for inspection by the certification officer
(see Appendix A, Chain-of-Custody).
6.1 Rejection of Samples
The laboratory is to reject any sample taken for
compliance purposes not meeting the criteria in
paragraphs 6.2 through 6.6 below and notify the
system/individual requesting the analyses.
6.2 Sample Containers and Preservation
The type of sample container and the required
preservative for each inorganic and organic chemical
contaminant are listed in Tables IV-4 and IV-5,
respectively.
6.3 Maximum Holding Times
Samples must be analyzed within the maximum
holding times listed in Tables IV-4 and IV-5.
6.4 Sample Collection and Transport
When the laboratory has responsibility for sample
collection, handling, and preservation, there needs to
be strict adherence to correct sampling procedures,
complete identification of the sample, and prompt
transfer of the sample to the laboratory.
6.5 Sample Collector
The collector should be trained in sampling
procedures and approved by the State regulatory
authority or its delegated representative.
6.6 Sample Report Form
The sample report form should contain the location,
date and time of collection, collector's name,
preservative added, and any other special remarks
concerning the sample. Indelible ink should be used.
7. Quality Assurance
7.1 General Requirements:
7.1.1 All quality control information is to be
available for inspection by the certification
officer.
7.1.2 A manual of analytical methods and the
laboratory's QA plan are to be available to the
analysts (see Chapter Ill's discussion of the QA
Plan).
7.1.3 Class S Weights or better should be
available to make periodic checks on balances.
A record of these checks is to be available for
inspection. The specific checks and their
frequency are to be as prescribed in the
laboratory's QA plan and the laboratory's
operations manual, if appropriate. This
frequency should not exceed one month.
7.1.4 Color standards or their equivalent such
as built-in internal standards are to be available
to verify wavelength settings on spectro-
photometers. A record of these checks should
be available for inspection. The specific checks
and their frequency are to be as prescribed in
the laboratory's QA plan and the laboratory's
operations manual, if appropriate. The frequency
of these checks should not exceed 6 months.
7.2 Analytical Quality Control
The following are necessary for each analyte for
which a laboratory is certified:
17
-------
7.2.1 The laboratory must analyze PE samples
(when available) at least annually.
7.2.2 At least once each quarter, the laboratory
should analyze a QC sample (EPA QC sample
or equivalent). If errors exceed limits specified,
corrective action is to be taken and
documented, and a follow-up quality control
standard analyzed as soon as possible to
demonstrate the problem has been corrected.
7.2.3 At the beginning of each day that
samples are to be analyzed, a standard curve
composed of at least a reagent blank and three
standards covering the sample concentration
range are to be prepared. These standards
should be from a source different than the
quality control standard used for paragraph
7.2.2.
7.2.4 Calibration for some methods is so time-
consuming that paragraph 7.2.3 is impractical.
For these methods, the standard curve is to be
initially developed as specified m paragraph
7.2.3. Thereafter, at the beginning of each day
on which analyses are performed, this curve is
to be verified by analysis of at least a reagent
blank and one standard in the expected
concentration range of the samples analyzed
that day. All checks should be within the control
limits specified in paragraph 7.2.7 or the system
recalibrated as specified in paragraph 7.2.3.
7.2.5 If the reagent blank specified in
paragraph 7.2.3 (or paragraph 7.2.4) is not
carried through the full analytical procedure,
then some other blank (at least one per day) is
to be carried through the entire analytical
procedure. Results from reagent blanks should
not exceed the laboratory's method detection
limit (MDL); see paragraph 7.2.8.
7.2.6 The laboratory should add a known spike
to a minimum of 10% of the routine samples
(except when the method specifies a different
percentage, i.e., furnace methods) to determine
if the entire analytical system is in control. The
spike concentration should not be substantially
less than the background concentration of the
sample selected for spiking. These checks
should be evenly spaced and one check should
be at the end of the day's analyses. Over time,
samples from all routine sample sources should
be spiked. If any of these checks are not within
the control limits specified in paragraph 7.2.7, a
standard should be analyzed to determine if the
"out of control" condition was due to sample
matrix or system operation. This standard is to
be analyzed through the complete analytical
system. Corrective action is to be taken in
accordance with the laboratory's QA plan.
7.2.7 Until sufficient data are available from the
laboratory, usually a minimum of 15 to 25 test
results on a specific analysis, the laboratory is
to use the control limits, if available, developed
from the mean (X) and standard deviation (S)
relationships in Table IV-6. This Table was
derived from EPA's PE sample data. After
inserting the analytical concentration (c),
including the background concentration (B)
wherever appropriate, into the proper pair of
relationships, compute control limits for
standards as X ± 3(S) and for spike recoveries
as (X-B) ± 3 (S). As sufficient data become
available, the laboratory should develop
traditional QC chart criteria for the various QC
checks specified above (see Chapter 6 of the
Handbook for Analytical QA in Water and
Wastewater Laboratories, EPA-600/4-79-019, or
similar QC reference texts for further
information). Since percent recovery may not be
a constant, the percent recovery data may have
to be separated into concentration intervals
before control limits are calculated for each
interval. If any of these control limits are tighter
than the matching control limits developed from
the relationships in Table IV-6, the laboratory
shall use the tighter criteria. Otherwise, control
limits calculated from the relationships in Table
IV-6 are required. The laboratory should
continue to calculate traditional control limits for
each analyte as additional results become
available.
7.2.8 It is further recommended that the
laboratory periodically determine the MDL in
accordance with the procedure given in 40 CFR
Part 136, Appendix B. This procedure is
available from EPA, Environmental Monitoring
Systems Laboratory, 26 W. Martin Luther King
Drive, Cincinnati, Ohio 45268.
8. Records and Data Reporting
8.7 Laboratory Records
Records of chemical analyses are to be kept by the
laboratory for a minimum of 3 years. This includes all
raw data, calculations, and quality control data. These
data files may be either manual or computer based.
The following information may be available as a
sample data report or summary record:
8.1.1 Date, place, time of sampling,
preservative added and name of person who
collected the sample.
8.1.2 Identification of sample as to whether it is
a routine distribution system sample, check
18
-------
sample, raw or finished water sample, or other 8.1.6 Result of analysis.
special purpose sample.
8.1.3 Date of receipt of sample and date of 9 Action Response to Laboratory
analysis.
8.1.4 Laboratory and person(s) responsible for When the action response is a designated laboratory
performing analysis. responsibility, the laboratory must notify the proper
authority of noncompliance sample results and
8.1.5 Analytical technique/method used, and request resampling from the same sampling point
quality control data. immediately.
19
-------
Table IV-1. Approved Methodology for Inorganic Contaminants
Contaminant
Arsenic
Barium
Cadmium
Chromium
Fluoride
Lead
Mercury
Nitrate-N
MCL
mg/L Methodology5
0.05 Atomic Absorption: furnace
• gaseous hydride
Spectrophotometnc. Silver Diethyl-
dithiocarbamate
Inductively Coupled Plasma
1 Atomic Absorption: direct aspiration
: furnace
Inductively Coupled Plasma
0.01 Atomic Absorption: direct aspiration
: furnace
Inductively Coupled Plasma
0.05 Atomic Absorption: direct aspiration
: furnace
Inductively Coupled Plasma
4 Colonmetnc SPADNS, with distillation
Potentiometnc ion selective electrode
Automated Alizarin fluoride blue, with
distillation
Automated ion selective electrode
0.05 Atomic Absorption: direct aspiration
. furnace
Inductively Coupled Plasma
0.002 Manual cold vapor technique
Automated cold vapor technique
10 0 Manual cadmium reduction
Automated hydrazine reduction
Automated cadmium reduction
Ion selective electrode
Colorimetric Brucine
Ion Chromatography
EPA'
206.2
206.3
206.4
200.7A
208 1
208.2
200.7A
213.1
213.2
200 7A
218.1
218.2
200. 7A
340 1
3402
340.3
239.1
2392
200 7A
245.1
245.2
353.3
353.1
353.2
352.1
300.0
neierenufc! (N
ASTM2
D2972-78B
D2972-78A
D3557-78A or B
D1687-77D
D1179-72A
D1179-72B
D3559-78A or B
D3223-79
D3867-79B
D3867-79A
D992-71
ntJinuu iNumuer)
SM3
301A VII
404A after
B(4)
301A-IV
301A-II or III
301A-II or III
41 3C and A 6
413B6
413E6
301A-II or III
301A-VI
41 9C
605
419D
Other
I-1062-784
129-71W7
380-75WE8
WeWWG/58809
B101110
Residual Disinfectant
Chlorine
Ozone
Chlorine Dioxide
Amperometnc Titration
Ferrous Titnmetnc Method
DPD Colorimetric Method
Leuco Crystal Violet Method
Indigo Method
Amperometnc Method
DPD Colorimetric Method
408C6
408D6
408E6
408F6
410B6
41OC6
Note 1
Selenium
Silver
Sodium
Turbidity
0.01 Atomic Absorption: furnace 270.2
: gaseous hydride 270.3 D3859-79 301A-VII
0.05 Atomic Absorption: direct aspiration 2721 301A-II
: furnace 272 2
Inductively Coupled Plasma 200.7A
Atomic Absorption: direct aspiration 273 1
. furnace 273.2
Flame Photometric D1428-64A 320A
Nephelometric 180 1 214A6
I-1667-784
1 "Methods of Chemical Analysis of Water and Wastes." EPA Environmental Monitoring and Systems Laboratory, Cincinnati, Ohio 45268
(EPA-600/4-79-020) March 1979. Available from ORD Publications, CERI, EPA, Cincinnati, Ohio 45268
2 "Annual Book of ASTM Standards," Part 31 Water, American Society for Testing and Materials. 1978, 1916 Race Street, Philadelphia, PA
19103.
3 "Standard Methods for the Examination of Water and Wastewater," 14th Ed., American Public Health Association; American Water Works
Association; Water Pollution Control Federation, 1975.
4 "Techniques of Water Resources Investigation of the United States Geological Survey, "Chapter A-1, "Methods for the Determination of
Inorganics Substances in Water and Fluvial Sediments," Book 5 (1979, Stock #024-001-03177-9). Available from the Superintendent of
Documents, US Government Printing Office, Washington, DC 20402.
5 For approved analytical procedures for metals the technique applicable to total metals must be used
6 "Standard Methods for the Examination of Water and Wastewater," American Public Health Association et ai., 16th Ed , 1985
7 "Fluoride in Water and Wastewater," Industrial Method 129-71W, "Technicon Industrial Systems, Tarrytown, NY 10591, December 1972.
8 "Fluoride in Water and Wastewater," Technicon Industrial Systems, Tarrytown, NY 10591, February 1976.
9 "Orion Guide to Water and Wastewater Analysis." Form WeWWG/5880, pp 5, 1985 Orion Research Inc., Boston, MA 02129
'0 "The Determination of Nitrite and Nitrate in Water Using Single Column Ion Chromatography," method B-1011, Millipore Corp., Waters
Chromatography Division, 34 Maple Street, Milford, MA 01754.
11 "Determination of Ozone in Water by the Indigo Method," A Submitted Standard Method; Ozone Science and Engineering, Vol. 4, pp 169-
176 Pergamon Press Ltd., 1982.
20
-------
Table IV-2. Approved Methodology for Organic Contaminants
Contaminant
Chlorinated hydrocarbons5
endnn
lindane
methoxychlor
toxaphene
Chlorophenoxys
2,4-D
2,4,5-TP
Total Tnhalomethanes
(TTHM)
MCL
ug/L
0.2
4
100
5
100
10
100
Methodology
Solvent extraction, gas chromatography
Solvent extraction, denvatization
gas chromatography
Purge and trap, gas chromatography
Solvent extraction, gas chromatography
Reference
EPA1
pp. 1-19
pp. 20-35
6
7
(Method Number or Page
ASTM2
D3086-85
D3478-85
SM3
509A
509B
Numbers)
USGS4
0-3104-83
0-3105-83
Maximum Tnhalomethane
Potential (MTP)
Volatile Organic
Contaminants (VOC)
Regulated
benzene
carbon tetrachlonde
p-dichlorobenzene
1,2-dichloroethane
1,1 -dichloroethylene
1,1,1-tnchloroethane
trichloroethylene
vinyl chloride
Unregulated12
5
5
75
5
7
200
5
2
Gas chromatography/mass spectrometry
TTHM after incubation
Purge and trap, gas chromatography
Gas chromatography/mass spectrometry
8.9
10
502.1"
5022"
503.1"
524 11'
524.211
Solvent extraction
Purge and trap, gas chromatography
Gas chromatography/mass spectrometry
504"
502.1"
5022"
503.1"
524.1"
524.2"
1 "Methods for Organochlorine Pesticides and Chlorophenoxy Acid Herbicides in Drinking Water and Raw Source Water," Available from
ORD Publications, CERI, EPA, Cincinnati, Ohio 45268.
2 "Annual Book of ASTM Standards," Volume 11 02, American Society for Testing and Materials. 1916 Race Street, Philadelphia, PA
19103.
3 "Standard Methods for the Examination of Water and Wastewater," 14th Ed., American Public Health Association, American Water Works
Association, Water Pollution Control Federation, 1975.
4 U.S. Geological Survey Techniques of Water—Resources Investigations, Chapter A3, "Methods for the Determination of Organic
Substances in Water and Fluvial Sediments," Book 5, 1983. Available from: Open File Service Section, Western Distribution Branch, Box
25425, Federal Center, Denver, CO 80225.
5 These analytes may be extracted using Bakers Solid Phase Extraction procedure as referenced in the Nation Wide Approval in FR 2-19-88,
Vol. 53, No. 33, pp. 5142.
6 "The Analysis of Tnhalomethanes in Finished Waters by the Purge and Trap Method," Method 501 1, EMSL, EPA, Cincinnati, Ohio 45268.
7 "The Analysis of Tnhalomethanes in Drinking Water by Liquid/Liquid Extraction," Method 501.2, EMSL, EPA, Cincinnati, Ohio 45268.
8 "Measurement of Tnhalomethanes in Drinking Water by Gas Chromatography/Mass Spectrometry and Selected Ion Monitoring," Method
501 3, EMSL, EPA, Cincinnati, Ohio 45268.
9 "Measurement of Purgeable Organic Compounds in Drinking Water by Gas Chromatography/Mass Spectrometry," Method 524, EMSL,
EPA, Cincinnati, Ohio 45268
10 40 CFR 141.30(e)(2)
" "Methods for the Determination of Organic Compounds in Finished Drinking Water and Raw Source Water," September, 1986, EMSL,
EPA, Cincinnati, Ohio 45268
12 The complete list of unregulated volatile organic chemicals can be found in 40 CFR part 141.40
21
-------
Table IV-3. Recommended Methods for Inorganic Contaminants
Reference (Method Number)
Contaminant
Alkalinity
Calcium4
Chloride
Copper
Corrosivity
Nitrite
PH
Residue, total dissolved
Sulfate
Temperature
Methodology
Titrimetnc or Potentiometric
EDTA titrimetnc
Atomic absorption: direct aspiration
Inductively coupled plasma
Potentiometric
Ion chromatography
Atomic absorption: furnace technique
.direct aspiration
Inductively coupled plasma
Langeher Index
Aggressive Index
Spectrophotometric
Automated cadmium reduction
Manual cadmium reduction
Ion chromatography
Potentiometric
Gravimetric
Turbidimetnc
Ion chromatography
Thermometric
EPA1
310 1
215 2
215.1
200. 7A
3000
220.2
220.1
200. 7A
3541
353.2
353.3
3000
150 1
160.1
3754
300.0
ASTM2
D1067-70B
D511-84A
D511-84B
D4327
D1688-84D or E
D3867-85A
D3867-85B
D1293-78A or B
D516-S2A
D4327
SM3
403
311C
303A
407C
429
304
303A or B
2037
418F
41 8C
423
209B
429
212
Others
1-1030-845
A-10006
C400-808
B-10119
1-1750-845
A-10006
'"Methods of Chemical Analysis of Water and Wastes," EPA, Environmental Monitoring and Systems Laboratory, Cincinnati, Ohio 45268
(EPA-600/4-79-020) March 1979. Available from ORD Publications, CERI, EPA, Cincinnati, Ohio 45268.
2"Annual Book of ASTM Standards," Volume 11 01, American Society for Testing and Materials. 1916 Race Street, Philadelphia, PA 19103.
3"Standard Methods for the Examination of Water and Wastewater," 16th Ed., American Public Health Association, American Water Works
Association, Water Pollution Control Federation, 1985
4For approved analytical procedures for metals, the technique applicable to total metals must be used..
5"Methods for the Determination of Inorganic Substances in Water and Fluvial Sediments," Techniques of Water-Resources Investigation of
the United States Geological Survey Books, Chapter Al, 1985, Open file report 85-495 Available from Open-File Services Section, Western
Distribution Branch, US Geological Survey, MS 306. Box 24525, Denver, CO 80225.
6 "Conductivity Detection of Anions Using Single Column Chromatography." Method A-1000, Millipore Corp., Waters Chromatography
Division, 34 Maple Street, Milford, MA 01754.
7"Standard Methods for the Examination of Water and Wastewater," 14th Ed., American Public Health Association, American Water Works
Association, Water Pollution Control Federation, 1975
8 'AWWA Standard for Asbestos-Cement Pipe, 4 in. through 16 in. for Water and Other Liquids," AWWA C400-80, Revision of C400-77,
AWWA, Denver, CO.
9"The Determination of Nitrite and Nitrate in Water Using Single Column Ion Chromatography," Method B1011. Millipore Corp., Waters
Chromatography Division, Milford, MA 01754.
22
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Table IV-4. Sample Collection, Containers, and Preservation for Inorganic Contaminants1 2
Contaminant
Alkalinity
Arsenic
Asbestos
Barium
Cadmium
Calcium
Chloride
Chromium
Copper
Fluoride
Free Chlorine
Residual
Lead
Mercury
Nitrate
Chlorinated
Non -chlorinated
Nitrite
PH
Selenium
Silver
Sodium
Sulfate
Temperature
Total Dissolved
Residue
Turbidity
Preservative3
Cool, 4°C
Cone HN03 to pH
Cool4°C<5
Cone HNO3 to pH
Cone HNO3 to pH
Cone HN03 to pH
None
Cone HNO3 to pH
Cone HNO3 to pH
None
None
Cone HNO3 to pH
Cone HNO3 to pH
Cool4°C
Cone H2SO4 to pH
Cool4°C
None
Cone HNO3 to pH
Cone HNO3 to pH
Cone HNO3 to pH
Cool4°C
None
Cool4°C
Cool 4°C
< 2
< 2
< 2
< 2
< 2
< 2
< 2
< 2
< 2
< 2
< 2
< 2
Container4
PorG
PorG
PorG
PorG
PorG
PorG
PorG
PorG
PorG
P
PorG
PorG
PorG
PorG
PorG
PorG
PorG
PorG
PorG
PorG
PorG
PorG
PorG
PorG
Maximum Holding Time5
14 days
6 months
6 months
6 months
6 months
28 days
6 months
6 months
28 days
Analyze immediately7
6 months
28 days
28 days
1 4 days8
48 hours
Analyze immediately7
6 months
6 months
6 months
28 days
Analyze immediately7
7 days
48 hours
1 The laboratory director must reject any samples, taken for compliance purposes, not meeting these criteria and notify the authority requesting
the analysis.
2 Other holding times can be obtained through alternate approval.
3 If HNO3 cannot be used because of shipping restrictions, sample for analysis of metals may be initially preserved by icing and immediately
shipping it to the laboratory. Upon receipt in the laboratory, the sample must be acidified with cone. HNO3 to pH < 2. At the time of analysis,
the sample container should be thoroughly rinsed with 1:1 HNO3; washings should be added to the sample. A volume correction for these
washings must be made.
4 P = plastic, hard or soft; G = glass, hard or soft.
5 In all cases, samples should be analyzed as soon after collection as possible.
6 These samples should never be frozen.
7 "Analyze immediately" generally means within 15 minutes of sample collection.
8 Ion chromatographic methods using conductivity as the detector cannot be used.
23
-------
Table IV-5. Sample Collection, Containers, and Preservation
for Organic Contaminants1
Contaminants
Chlorinated
hydrocarbons
Chlorophenoxys
TTHMs
VOCs
Preservative
Refrigerate at
4°C as soon as
possible after
collection
Refrigerate at
4°C as soon as
possible after
collection.
Ascorbic acid
and 6N HCI
HCL to pH < 2,
Cool4°C
Container
Glass with foil or
Teflon-lined cap
Glass with foil or
Teflon-lined cap.
Glass with
Teflon-lined
septum
Glass with
Teflon-lined
septum
Maximum
Holding
Time2
14 days
7 days3
14 days
1 4 days
1 If a laboratory has no control over these factors, the laboratory
director must reject any samples not meeting these criteria and
notify the authority requesting the analyses.
2 In all cases, samples should be analyzed as soon after collection as
possible.
3 Well-stoppered and refrigerated extracts can be held up to 30
days.
24
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Table IV-6. Background for Development of Control Limits for the Required Quality Control Program (See 7.2.7)
Analyte
Arsenic
Barium
Cadmium
Chromium
Lead
Mercury
Selenium
Silver
Nitrate-N
Fluoride
Endnn
Lmdane
Methoxychlor
Toxaphene
2,4-D
2,4,5-TP
Chloroform
Bromoform
Bromodichloromethane
Dibromochloromethane
Residual Free Chlorine1
Turbidity1
Total Dissolved Residue
Calcium, as CaCO3
pH1
Alkalinity, as CaCO3
Langelier Index, 20°C1
Sodium
Units
ug/L
ug/L
ug/L
ug/L
ug/L
ug/L
ug/L
ug/L
mg/L
mg/L
ug/L
ug/L
ug/L
ug/L
ug/L
ug/L
ug/L
ug/L
ug/L
ug/L
mg/L
NTU
mg/L
mg/L
units
mg/L
units
mg/L
Application
Concentration
Range
3.56 to 106
41 to 938
1 .6 to 42
12.7 to 127
3.2 to 109
0.72 to 7.5
9.71 to 86.9
3.42 to 103
0.35 to 8.5
0.18 to 2.0
0.13 to 6. 7
0.12 to 5.8
1 .96 to 95
1 .42 to 1 2.8
1.79 to 89.6
1.20 to 73.1
9.06 to 81. 5
12.3 to 84.3
11.1 to 75.1
7.66 to 80.5
0.38 to 1.8
0.35 to 5.0
100 to 610
0.90 to 103
4.00 to 9.2
4.97 to 110
0.74 to 1.0
7.58 to 95
l^OUl 1 IdlC Ul V.
Mean
0.982(c)-o.iO
0.974(0 + 0.52
0.972(0 + 0.14
0.997(0) + 0 11
0.999(C)-I-0.24
0.972(C)
0.993(c)-0.11
0.994(c) + 020
1.008(0 + 0.01
0.988(0 + 0.01
0.971 (c)
0.949(c)
0.927(0 + 0.14
0.968(c)-0.05
0.874(0 + 0 14
0.862(0 + 001
0.980(c)i-030
1.008(0 + 0.49
1.000(c)-0.23
1.004(c)-0.17
0.974(0 + 002
0.946(0+0.07
1.027(C)-1.79
1.002(C) + 0.32
0.987(C) + 0.07
0.976(0 + 0.84
1.045(C)-0.04
0.988(C) + 0.20
yUM^GI III CUIUI 1 O.
Standard
Deviation
0.0693(c) + 0.28
0.0504(C) + 1.93
0.0682(c) + 0.12
0.0567(c) + 0.63
0.0647(0 + 0.59
0.0858(0 + 0.06
0.0985(0 + 0.15
0.0585(0 + 0.29
0.0810(0 + 0.03
0.0290(0 + 0.01
0.138(c)
0.163(0 + 0.01
0.149(0 + 0.03
0.152(0 + 0.15
0.230(0 + 0.13
0 238(C) - 0.05
0.0814(0 + 0.55
0 109(0 + 0.33
0.1 06(c) + 0.03
0 111(c) + 0 16
0.0295(0 + 0.09
0.051 7(c) + 0.05
0.0874(0 + 4.03
0.0443(0 + 0.16
0.01 47(C) - 0.04
0.0133(0) + 1.10
00036(0 + 0.15
0.0396(0 + 0.15
1Not amenable to spiking procedure
25
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Sample Forms for On-Site Evaluation of Laboratories Involved in Analysis of Public Water Supplies-
Chemistry
Laboratory.
Street
City State.
Telephone Number
Survey by
Affiliation
Date
Codes for Marking On-Site Evaluation Forms
S - Satisfactory X - Unsatisfactory U - Undetermined NA - Not Applicable
26
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Laboratory Evaluator_
Location Date
Personnel
Other
Analysts
Position/Title Name Education Level Specialized Present Experience
Degree—Major* Training Speciality
Lab Director
Manager
Supervisor
Instrument
Operator
AA_
TEM_
GC_
ICP_
GC/MS_
1C
"If the major is not in chemistry, list hours of college level courses in chemistry
27
-------
Laboratory_
Location
Evaluator
Date
Laboratory Equipment and Instruments for Inorganic and Organic Contaminants
Item
ANALYTICAL BALANCE:
0.1 mg sensitivity
Stable base
Class S weights
Service contracts
MAGNETIC STIRRER:
Variable speed
TFE coated stir bar
pH METER:
± 0.05 units
Readability ± 0.1 units
Line or battery
Usable with specific ion
electrodes
CONDUCTIVITY METER:
Readable in ohms or mhos
Range of 2 ohms to 2
megohms
Line or battery
HOT PLATE:
Temp, control
CENTRIFUGE:
To 3000 rpm
Option of 4 x 50 mL
COLOR STANDARDS:
To verify wavelengths on
photometers
Should cover 200 to 800
nm
REFRIGERATOR:
Standard laboratory
Explosion proof for organic
storage
DRYING OVEN:
Gravity or convection
Controlled from room to
180°C or higher (±2°C)
To 400 °C for cleaning
organic glass
No. of
Units
EPA Method
Manufacturer
Model
Satisfactory
Yes
No
28
-------
Laboratory Equipment and Instruments for Inorganic and Organic Contaminants (Continued)
Item
THERMOMETER:
Mercury-filled Celsius
1 °C or finer subdivision
To 180°C
Certified by or traceable to
NBS
GLASSWARE:
Borosilicate
Class A volumetric
SPECTROPHOTOMETER:
Range 400 to 700 nm
Band width— not greater
than 20 nm
Use several size and
shape cells
Path length 1 to 5 cm
FILTER PHOTOMETER:
Range 400 to 700 nm
Band width 10 to 70 nm
Use several size and
shape cells
Path length 1 to 5 cm
SPECIFIC ION METER:
Readable & accurate to ±
1 mV
ELECTRODES:
As needed
INDUCTIVELY COUPLED
PLASMA:
Computer control
Background coordination
Radio frequency generator
Argon gas supply
WATER BATH:
Electric or steamed heat
Heat to 100°C
Controllable within 5°C
ION CHROMATOGRAPH:
Conductivity detector
Suppressor column
Separator column
U.V. detector
No. of
Units
EPA Method
206.4-340.1-340.3
245.1-254.2-352.1
353.3-353.2-353.1
409E or F-408G&E
375.4-41 OB&C
Same as above
340.2
200.7-200.7A
245.1-352.1
Pesticides
300.0
300.0
300.0-B1011
B-1011
Manufacturer
Model
Satisfactory
Yes
No
29
-------
Laboratory Equipment and Instruments for Inorganic and Organic Contaminants (Continued)
Item
AMPEROMETRIC TITRATOR
ATOMIC ABSORPTION
SPECTROPHOTOMETER:
Single channel
Single or double beam
Grating monochrometer
Photomultiplier detector
Adjustable slits
Range 1 90 to 800 nm
Readout system:
Response time compatible
with AA
Able to detect positive
interference for furnace
Chart recorder, CRT, or
hardcopy printer
Fuel and oxidant:
Commercial grade
Acetylene
Air
Reagent grade nitrous
oxide
Commercial grade argon
or nitrogen (furnace)
Hydrogen (hydride)
Burner:
Recommended by
manufacturer for the
above gases
Hollow cathode lamps:
Single element preferred
Multiple element
acceptable
EDLs acceptable
Graphite furnace:
Any that will reach
temps required
Background corrector:
Required for furnace
Provision for off-line
analysis
Hydride generator
No. of
Units
EPA Method
408-C
208.1 206.2
213.1 208.2
218.1 213.2
239.1 218.2
272.1 239.2
215.1 270.2
273.1 272.2
206.3 273.2 270.3
Same as above
208.1-239.1
213.1 272.1
215.1 273.1
218.1
206.2 218.2 272.2
208.2 239.2 273.2
213.2 270.2
206.3 270.3
See Atomic
Absorption
See Atomic
Absorption
206.2 208.2 213.2
218.2 239.2 270.2
272.2 273.2
See Atomic
Absorption
206.3
270.3
Manufacturer
Model
Satisfactory
Yes
No
30
-------
Laboratory,
Location
Evaluator
Date
Methodology
Contaminant
Inorganic Arsenic
Barium
Cadmium
Chromium
Fluoride
Lead
Mercury
Nitrate
Selenium
Silver
Organic
Chlorinated
Hydrocarbons
Chlorophenoxys
TTHM
MTP
VOC
Name or
Description of
Method
Reference
(Cite Source and
Method by Number
or Page and Year)
Sample Load
Per Month
Satisfactory
Yes
No
33
-------
Laboratory_
Location
Evaluator
Date
Sample Handling and Preservation
Contaminant
Inorganic Arsenic
Barium
Cadmium
Chromium
Fluoride
Lead
Mercury
Nitrate
Selenium
Silver
Organic
Chlorinated
Hydrocarbons
Chlorophenoxys
TTHM
MTP
VOC
Container Used
(Material and Size)
Preservative Used
Maximum
Holding Time
Satisfactory
Yes
No
34
-------
Laboratory Equipment and Instruments for Inorganic and Organic Contaminants (Continued)
Item
AUTOMATED ANALYSES
SYSTEM:
Sampler
Proportioning pump
Manifold or cartridge
Heating bath
Bath with distilling head
Continuous filter
Colorimeter
ISE detector
Recorder
MERCURY ANALYZER:
Spectrophotometer
Dedicated mercury
analyzer acceptable
Having a mercury hollow
cathode lamp
Absorption Cell:
10 cm quartz cell with
quartz end windows or
1 1 .5 cm plexiglass cell
with I.D. of 2.5 cm
Air Pump:
To deliver flow of at
least 1 L per minute
Aeration tube:
With coarse glass frit
Flowmeter:
To measure air flow of
1 L per minute
Drying Unit:
6-inch tube with 20 g
magnesium
Perchlorate
or
Heating device
No. of
Units
EPA Method
340.3-353.1-353.2
380-75WE
340.3-353.1-353.2
380-75WB
340.3-353.1-353.2
380-75WE
353.1
41 3E (Std Methds)
340.3-353.1
340.3-353.1-353.2
380-75WE
340.3-353.1-353.2
380-75WE
245.1-245.2
245.1-245.2
245.1-245.2
245.1-245.2
245.1-245.2
245.1-245.2
Manufacturer
Model
Satisfactory
Yes
No
31
-------
Laboratory Equipment and Instruments for Inorganic and Organic Contaminants (Continued)
Item
PIPETS AND TIPS:
Microliter capacity with
disposable tips
Sizes— 5 to 100
microliters
Tips should be metal-free
GLASSWARE:
Separatory Funnels
Kuderna Danish (K-D)
concentrators
Water bath for K-D
ARSINE GENERATOR:
A Gutzeit generator or
equivalent
GAS CHROMATOGRAPH:
±0.2°C oven
Temperature control
Recorder, hardcopy
Oven temperature
programmer
GC Detectors
Linearized electron
capture or equivalent
Electrolytic
conductivity
Photoionization
Mass Spectrometer:
Electron-impact
ionization
(70eV nominal)
All-glass enrichment
device
All-glass transfer line
Software to acquire and
manipulate data for only a
few ions
Purge and trap system
No. of
Units
EPA Method
See graphite
furnace method list
Organochlonne
Pesticides
Chlorophenoxys
206.4
All
All
501.1 502.1 502.2
503.1 504 524.1
524.2
Pesticides
Chlorophenoxys
501.2
501.1 502.1 502.2
503.1
501.3 524 524.1
524.2
501.3 524 524.1
524.2
501.1 501.3
502.1 502.2 503.1
524 524.1 524.2
Manufacturer
Model
Satisfactory
Yes
No
32
-------
Laboratory_
Location
Evaluator
Date
Sample Collection
Item
General
Trained Sample Collector
Representative sampling
Complete sample form
Inorganic
Appropriate sampling and
preservation
Overaged samples
discarded
Organic
Appropriate sampling and
preservation
TTHM
Stabilizer added to
same bottle in
laboratory prior to
shipment to site or at
time of sample
collection.
TTHM
Hermetic seal
Overaged samples
discarded
Comments
Satisfactory
Yes
No
35
-------
Laboratory_
Location
Evaluator
Date
Quality Assurance and Data Reporting
Item
QA plan and data
Annual performance
samples analyzed
Methods manual available
Records kept 3 years
pH meter calibration
10% spiked samples
Check sample with each
group of 20 samples
Daily method blank
Daily Calibration
Quarterly QC samples or
Daily calibration check
Organic
TTHM/VOCs field blanks
10% TTHM/VOCs in
duplicate
TTHM/VOCs control
standards
TTHM/VOCs startup test
Source water
blank check
BFB tuning check
Comments
Satisfactory
Yes
No
36
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Chapter V
Microbiology
Note: quality control items are designated as "QC"
and necessitate written records which are to be
retained for five years.
1. Personnel
1.1 Supervisor/Consultant
The supervisor or consultant is a professional
scientist experienced in water microbiology. If a
supervisor is not available, a consultant having the
same qualifications may be substituted. State
laboratory personnel would be a primary source for
consultants.
1.1.1 Academic Training: Minimum of a
bachelor's degree in science.
1.1.2 Job Training: Minimum of two weeks
training from a Federal agency, State agency, or
academic institution in microbiological analysis
of drinking water.
1.2 Analyst (or equivalent job title)
The analyst performs microbiological tests with
minimal supervision.
1.2.1 Academic training: Minimum of high
school education.
1.2.2 Job training: Training in microbiological
analysis of drinking water, acceptable to the
State (or EPA for nonprimacy States), plus a
minimum of 30 days on-the-job training.
Personnel should take advantage of workshops
and training programs available from Federal
and State regulatory agencies and professional
societies.
1.2.3 Experience: At least one year of bench
experience in sanitary, water, milk, or food
microbiology.
2. Laboratory Facilities
Laboratory facilities are clean and temperature and
humidity controlled, and have adequate lighting at
bench tops. The laboratory has provisions for disposal
of microbiological waste. It is recommended that the
laboratory contain 150-200 square feet and 5 to 6
linear feet of usable bench space per analyst.
Laboratory facilities should include sufficient bench-
top area for processing samples; storage space for
media, glassware, and portable equipment; floor
space for stationary equipment (incubators,
waterbaths, refrigerators, etc.); and associated area(s)
for cleaning glassware and sterilizing materials.
While safety criteria are not an aspect of laboratory
certification, laboratory personnel should be aware of
general and customary safety practices for
laboratories. Each laboratory is encouraged to have a
safety plan available.
3. Laboratory Equipment and Supplies
A laboratory may request or contract with another
certified laboratory to conduct specified quality control
testing, e.g., testing the quality of laboratory pure
water (paragraph 4.3.2 in this chapter); calibration of
non-reference weights (paragraph 3.2.2 m this
chapter); and calibration of temperature monitoring
devices (paragraph 3.3.2 in this chapter). The
laboratory conducting the actual quality control test(s)
is to be certified for microbiology and provide copies
of quality control data to the requesting laboratory.
Therefore, the requesting laboratory is not necessarily
required to have equipment, supplies, and materials
to conduct specified quality control tests.
3.1 pH Meter
3.1.1 Accuracy and scale graduations within
±0.1 units.
3.1.2 Use pH buffer aliquot only once.
3.1.3 Maintain electrodes according to
manufacturer's recommendations.
QC 3.1.4 Standardize pH meter each use period
with pH 7.0 and pH 4.0 standard buffer.
QC 3.1.5 Date commercial buffer solution container
upon receipt, and when opened. Discard before
expiration date.
37
-------
3.2 Balance (top loader or pan)
3.2.1 Balance detects 100 mg at a 150 gram
load.
QC 3.2.2 Calibrate balance monthly using Class S
or S-1 reference weights (minimum of three
traceable weights which bracket laboratory
weighing needs) or weights traceable to Class S
or S-1 weights. Calibrate non-reference weights
annually with Class S or S-1 reference weights.
Correction data necessary with S or S-1
reference weights.
QC 3.2.3 Maintain service contract or internal
maintenance protocol and maintenance records.
Maintenance conducted annually at a minimum.
3.3 Temperature Monitoring Device
3.3.1 Use glass/mercury or dial thermometers
graduated in 0.5°C increments or less in
incubator units. Mercury column in glass
thermometers is not separated.
QC 3.3.2 Check calibration of m-use glass/mercury
thermometers annually and in-use dial
thermometer quarterly, at the temperature used,
against a reference National Institute of
Standards and Technology (formerly National
Bureau of Standards) (NBS) thermometer or
one that meets the requirements of NBS
Monograph 150.
QC 3.3.3 Recalibrate continuous recording devices
annually which are used to monitor incubator
temperature. Use same reference thermometer
described in QC 3.3.2.
3.4 Incubator Unit
3.4.1 Incubator unit has an internal
temperature monitoring device and maintains a
temperature of 35° ± 0.5°C. For nonportable
incubators, place thermometers on the top and
bottom shelves of the use area with the
thermometer bulb immersed in liquid. If an
aluminum block is used, culture dishes and
tubes fit snugly.
QC 3.4.2 Record temperature for days in use at
least twice per day with readings separated by
at least 4 hours.
3.5 Autoclave
3.5.1 Autoclave has a temperature gauge with
a sensor on the exhaust, a pressure gauge, and
an operational safety valve. Autoclave maintains
sterilization temperature during the sterilizing
cycle and completes an entire cycle within 45
minutes when a 12-15 minute sterilization period
is used. Autoclave depressurizes slowly to
ensure media do not boil over and bubbles do
not form in inverted tubes.
QC 3.5.2 Because of safety concerns and
difficulties with operational control, pressure
cookers and vertical autoclaves are not
acceptable.
QC 3.5.3 Record date, contents, sterilization time,
and temperature for each cycle. Establish
service contract or internal maintenance
protocol, and maintain records.
QC 3.5.4 Use maximum-temperature-registering
thermometer, heat-sensitive tape, or spore
strips or ampoules during each autoclave cycle
and record temperature. Avoid overcrowding.
QC 3.5.5 Check automatic timing mechanism with
stopwatch quarterly.
3.6 Hot Air Oven
3.6.1 The oven maintains a stable sterilization
temperature of 170°-180°C for at least two
hours. Sterilize only dry items and avoid
overcrowding. The oven thermometer is
graduated in 10°C increments or less, with the
bulb placed in sand during use.
QC 3.6.2 Record date, contents, and sterilization
time and temperature of each cycle.
3.7 Colony Counter
Use colony counter, dark field model, to count
Heterotrophic Plate Count colonies.
3.8 Conductivity Meter
Suitable for checking laboratory pure water. Readable
in ohms or mhos, with a range from at least 2 ohms
to 2 megohms or equivalent micromhos ± 2%. Unit
may be in-line/bench or portable/battery operated.
QC 3.8.1 Conductivity meter is calibrated monthly
with a 0.01 M KCI solution (See Method 120.1
in Methods for Chemical Analyses of Water and
Wastes, 1979, EPA 600/4-79-020 (revised
1983); or Section 205, "Conductvity", pp. 76-
80, in Standard Methods for the Examination of
Water and Wastewater (16th ed.), 1985).
3.9 Refrigerator
3.9.1 Refrigerator maintains a temperature of
1° to 5°C. Thermometer graduated in at least
1°C increments with the thermometer bulb
immersed in liquid.
QC 3.9.2 Record temperatures for days in use at
least once per day.
38
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3.10 Inoculating Equipment
Metal or plastic loops, or wood applicator sticks
sterilized by dry heat. The metal inoculating loops
and/or needles are made of nickel alloy or platinum.
3.77 Membrane Filtration Equipment (if MF
procedure is used)
3.11.1 MF units are stainless steel, glass, or
autoclavable plastic, not scratched or corroded,
and do not leak.
3.11.2 10X to 15X magnification device with
fluorescent light source used to count sheen
colonies.
3,11.3 Membrane filters approved by the
manufacturer for total coliform water analysis.
Approval based on data from tests for toxicity.
recovery, retention, and absence of growth-
promoting substances. Filters are cellulose
ester, white, gndmarked, 47 mm diameter, and
0.45 ym pore size, or alternate pore sizes if
manufacturer provides performance data equal
to or better than the 0.45 urn pore size.
Membrane filters are purchased prestenlized or
autoclaved before use.
QC 3.11.4 Record the lot number and date
received for membrane filters. If the quality and
performance of membrane filters are
questionable, new lot(s) of membrane filters can
be checked by comparing recovery of coliform
organisms against membrane filters from a
previously acceptable lot. (Suggested
procedure: Obtain a natural cohform-positive
water sample or prepare a laboratory water
sample using a pure coliform culture. New lots
of membrane filters are evaluated by passing a
sufficient volume of water sample through a
membrane filter from a new lot and a membrane
filter known to be acceptable so that 30 to 60
coliform colonies are observed on the
acceptable membrane filter after 24 hours
incubation at 35°C. The colony counts on the
membranes are evaluated using the formula:
Critical value* =
A- B - 1
, where
A is the count on the acceptable membrane filter, and
B is the count on the membrane filter from a new lot.
If the critical value is not less than 1.96, the new
membranes should be considered unacceptable.)
Unacceptable membrane filters are returned to the
vendor with a request to replace these with
membrane filters from a different lot number.
Replacement membranes are submitted to the same
comparative procedure. (This comparative procedure
will demonstrate gross differences between the
membranes; other, more stringent comparative
procedures are acceptable).
QC 3.11.5 Check sterility of each lot number of
membranes by placing one membrane in 50 ml
volume of non-selective broth medium (e.g.,
tryptic soy broth) and check for growth after 24
hours incubation at 35° ± 0.5°C.
3.72 Culture Dishes (loose or tight lid)
3.12.1 Use prestenlized plastic or sterilizable
glass culture dishes. To maintain sterility of
glass culture dishes, use stainless steel or
aluminum canisters, or wrap dishes in a heavy
aluminum foil or char-resistant paper.
3.12.2 Incubate loose-lid dishes in a tight-
fitting container, e.g., plastic vegetable crisper,
to prevent dehydration of membrane filter and
medium.
3.12.3 Reseal opened packs of disposable
culture dishes between major use periods.
3.73 Pipets
3.13.1 To sterilize and maintain sterility of
glass pipets, use stainless steel or aluminum
canisters, or wrap individual pipets in char-
resistant paper.
3.13.2 Pipets have legible
not chipped nor etched.
markings and are
"Hald, Statistical Theory with Engineering Applications. John
Wiley and Sons, Inc., New York, NY, 1960, p. 725.
3.13.3 Opened packs of disposable sterile
pipets are resealed between major use periods.
3.74 Culture Tubes and Closures
3.14.1 Tubes are made of borosilicate glass or
other corrosion-resistant glass.
3.14.2 Culture tubes used for Presumptive
Test in the Multiple Tube Fermentation
Technique (MPN) are of a sufficient size to
contain medium plus sample without being more
than three quarters full.
39
-------
3.14.3 Tube closures are stainless steel,
plastic, aluminum, or screw caps with non-toxic
liners. Cotton plugs are not acceptable.
3.75 Sample Containers
3.15.1 Sample bottles are wide mouth plastic
or non-corrosive glass with a non-
leaking ground glass stopper or a cap
with a non-toxic liner which will
withstand repeated sterilization, or other
EPA-approved sample containers.
Capacity of sample containers is at
least 120 ml (4 02.).
3.15.2 Glass stoppered bottle closures are
covered with aluminum foil or char-resistant
paper for sterilization.
3.76 Glassware and Plasticware
3.16.1 Glassware is borosilicate glass or other
corrosion-resistant glass and free of chips and
cracks. Markings on graduated cylinders and
pipets are legible. Plastic items are clear and
non-toxic.
3.16.2 Graduated cylinders for measurement
of sample volumes have a tolerance of 2.5% or
less.
3.16.3 Pipets delivering volumes of 10 ml_ or
less are accurate within a 2.5% tolerance or
less.
4. General Laboratory Practices
4.1 Sterilization Procedures
4.1.1 The times for autoclaving materials at
121 °C are listed below. Except for membrane
filters and pads and carbohydrate-containing
media, indicated times are minimal times which
may necessitate adjustment depending upon
volumes, containers, and loads.
Item
Time
(minutes)
Membrane filters & pads
Carbohydrate containing media
Contaminated test materials
Membrane filter assemblies
Sample collection bottles
Individual glassware
Dilution water blank
Rinse water
10
12-15
30
15
15
15
15
15
4.1.2 Remove autoclaved membrane filters and
pads and all media immediately after completion
of sterilization cycle.
4.1.3 Membrane filter equipment is autoclaved
at the start of the first filtration series of each
day and after each filtration series. A filtration
series ends when 30 minutes or longer elapse
between individual sample filtration.
4.1.4 Membrane filter assemblies may be
exposed to UV irradiation (germicidal lamp,
2537 angstroms) or submerged in boiling water
for approximately two minutes if bacterial carry-
over between individual sample filtration
becomes a problem. (Filter assemblies
submerged in boiling water are cooled to room
temperature before filtering sample.)
4.2 Sample Containers
4.2.1 Add sodium thiosulfate (Na2S203;
Anhydrous, 100 mg/L) to sample containers
before sterilization (0.1 ml_ of 10% Na2S203
solution per 120 ml capacity).
QC 4.2.2 Select at least one sample container at
random from each batch of sterile sample
bottles, or other EPA-approved containers, and
confirm sterility by adding approximately a 25
ml volume of a sterile non-selective broth (e.g.,
tryptic soy, trypticase soy, or tryptone broth).
Incubate at 35° ± 0.5°C for 24 hours and check
for growth.
4.3 Reagent Water
4.3.1 Use only satisfactorily tested reagent
water from stills or deionization units to prepare
media, reagents, and dilution/rinse water for
performing bacteriological analyses.
QC 4.3.2 Test the quality of the reagent water or
have it tested by a certified laboratory to assure
it meets the criteria in the table below.
4.4 Dilution/Rinse Water
4.4.1 Prepare stock buffer solution or peptone
water using reagent grade according to
Standard Methods for the Examination of Water
and Wastewater, 16th edition, p 855.
4.4.2 Stock buffer is autoclaved or filter-
sterilized. Label and date containers. Ensure
stored stock buffer is free of turbidity.
4.4.3 Dilution/rinse water is prepared by adding
1.25 ml volume of stock buffer solution and 5
ml volume of magnesium chloride (MgCI2)
solution (81.1 g MgCI2 • 6 H2O/L) per liter of
reagent water.
QC 4.4.4 Check each batch of dilution/rinse water
for sterility by adding 50 ml of water to a 50 ml
of a double strength non-selective broth (e.g.,
tryptic: soy, trypticase soy or tryptose broth).
40
-------
Parameter
Limits
Frequency
Conductivity
Pb, Cd, Cr, Cu,
Ni, Zn
Total Chlorine
Residual1
Heterotrophic
Plate Count2
Quality of
Reagent Waters
> 0.5 megohms
resistance or < 2
micromhos/cm at
25°C
Not greater than
0.05 mg/L per
contaminant.
Collectively, no
greater than 0.1
mg/L
Nondetectable
< 500/mL
Ratio 0.8-3.0
Monthly
Annually
Monthly
Monthly
Annually
1 DPD Method not required if source water is not chlorinated.
2 Pour Plate Method.
3 Test for bacteriological quality of reagent water (Standard
Methods for the Examination of Water and Wastewater, 16th
Edition p. 835; also Microbio/ogica/ Methods for Monitoring the
Environment, EPA-60078-78-017, p 200). Control water for test is
defined as double distilled water using a glass still.
Incubate at 35° ± 0.5 °C for 24 hours and check
for growth.
4.5 Glassware Washing
4.5.1 Use distilled or deionized water for final
rinse.
QC 4.5.2 Perform the Inhibitory Residue Test
(Standard Methods for the Examination of Water
and Wastewater, 16th edition, p. 834, and
Microbiological Methods for Monitoring the
Environment, U.S. EPA-600/8-78-017 p. 199) on
the initial use of a washing compound and
whenever a different formulation of washing
compound, or washing procedure, is used to
ensure that glassware is free of toxic residue.
4.6 Media—General Requirements
4.6.1 Use of dehydrated or prepared media
manufactured commercially is strongly
recommended due to concern about quality
control. Store dehydrated media in a cool, dry
location and discard caked or discolored
dehydrated media.
4.6.2 Date bottles of dehydrated media upon
receipt and also when initially opened. Discard
dehydrated media 6 months after opening; if
stored in a desiccator, storage is extended to 12
months. Discard dehydrated media that has
passed the manufacturer's expiration date.
QC 4.6.3 For media prepared in the laboratory,
record the date of preparation, type of medium,
lot number, sterilization time and temperature,
final pH, technician's initials.
QC 4.6.4 For liquid media prepared commercially,
record date received, type of medium, lot
number, and pH verification. Discard medium by
manufacturer's expiration date.
4.7 Membrane Filter (MF) Media (needed only if
laboratory conducts MF procedure)
4.7.1 Use m-Endo broth or agar or m-Endo
LES broth or agar in the single step or
enrichment techniques. Ensure that ethanol
used in rehydration procedure is not denatured.
Prepare medium in a sterile flask and use a
boiling water bath or, if constantly attended, a
hot plate with a stir bar to bring medium just to
the boiling point. Do not boil medium. Final pH
7.2 ± 0.2.
4.7.2 Refrigerate MF broth no longer than 96
hours, poured MF agar plates no longer than 2
weeks, and ampouled m-Endo broth in
accordance with manufacturer's expiration date.
4.8 Multiple Tube Fermentation Technique (MPN
or MTF) Media
4.8.1 Double strength lauryl tryptose broth or
lactose broth is used in the Presumptive Test
and single strength brilliant green lactose bile
(BGLB) broth in the Confirmed Test. Dispense
broth medium volume of not less than 10 mL
per tube and autoclave media at 121° C for 12-
15 minutes. Final pH 6.8 ± 0.2 (7.2 ± 0.2 for
BGLB broth).
4.8.2 If MPN media are refrigerated after
sterilization, incubate overnight at 35°C before
use. Discard tubes showing growth and/or
bubbles. Use MPN media prepared in tubes with
loose-fitting closures within one week. Store
broth media in screw cap tubes no longer than
3 months, provided media are stored in dark.
Discard media if evaporation exceeds 10% of
original volume.
4.8.3 Use m-Endo agar, m-Endo LES agar, or
Levine Eosm Methylene Blue (EMB) agar for the
Completed Test although the m-Endo LES agar
is the medium of choice. Dissolve, using a
sterile flask, in a boiling water bath (or direct
heat if constantly attended) to bring medium just
to the boiling point. Do not autoclave. Final pH
7.2 ± 0.2. Medium may be stored refrigerated
for two weeks. If EMB agar is used for
41
-------
Completed Test, either dissolve in a sterile flask
using a boiling water bath (or direct heat if
constantly attended) and bring medium to
boiling point or autoclave medium at 121°C for
12-15 minutes. Final pH 7.1 ± 0.2. Use non-
autoclaved medium on day of preparation; do
not store. Refrigerate autoclaved medium and
use within two weeks.
4.9 Heterotrophic Plate Count (HPC) Medium
Autoclave HPC agar at 121 °C for 15 minutes,
depending upon volume. Final pH 7.0 ± 0.2. Temper
melted agar at 440-46°C before pouring. Hold melted
agar no longer than 8 hours. Do not melt sterile agar
medium more than once.
5. Analytical Methodology
Note: on 12/31/90, significant changes will be made in
this section to conform with the requirements of the
revised total coliform rule.
5.1 EPA Approval
Approved analytical methodology is specified in the
National Primary Drinking Water Regulations.
Alternate methods must have EPA approval.
5.2 MF Procedure
5.2.1 Shake sample vigorously before
analyzing. Sample volumes analyzed by the MF
procedure must be 100 ml_ ± 2.5 ml_.
5.2.2 Confluent growth is defined as bacterial
growth with or without sheen covering the entire
membrane filter. TNTC (too numerous to count)
is defined as greater than 200 total bacterial
colonies on the membrane filter.
5.2.3 Samples resulting in confluent growth or
TNTC with less than five distinguishable sheen
colonies are invalid. Record as "confluent
growth" or "TNTC" with the number of
discernable sheen colonies and request an
additional sample from the same sampling site.
5.2.4 Samples resulting in confluent growth or
TNTC with five or more distinguishable sheen
colonies may be a MCL violation. Report as
"confluent growth" or "TNTC" with the number
of distinguishable sheen colonies.
5.2.5 Verify all sheen colonies for all
unsatisfactory samples (>4 colonies/100 ml_)
regardless of the amount of sheen when the
number of the sheen colonies is 5 or more up to
10/100 ml. When the number of sheen colonies
exceeds 10/100 ml, randomly pick 10 colonies
for verification.
5.2.6 Verify sheen colonies using either single
strength lactose or LTB and then single strength
BGLB media (same media used in MPN
procedure), or EPA-approved cytochrome
oxidase and (5-galactosidase rapid test
procedure.
5.2.7 Adjust initial counts based only upon
verification data.
QC 5.2.8 Conduct MF sterility check at the
beginning and the end of each filtration series. If
controls indicate contamination, reject all data
from affected samples and request immediate
resampling.
QC 5.2.9 Laboratories which conduct the MF
procedure and have two or more analysts
should analyze one known coliform-positive
sample monthly and each analyst should count
the sheen colonies on the same membrane.
The sheen colony counts should agree within
10%.
5.3 MPN Procedure
5.3.1 Conduct MPN Completed Test, quarterly,
on riot less than 10% of all unsatisfactory
samples (> three positive confirmed tubes).
Gram-staining is optional for potable water
samples.
5.3.2 For unsatisfactory samples, adjust the
number of positive confirmed tubes on the basis
of the Completed Test.
5.3.3 If the MPN test is used on water supplies
that have a history of confluent growth or TNTC
by the MF procedure, all presumptive tubes with
heavy growth without gas production are
submitted to the Confirmed Test to check for
coliform suppression.
QC 5.3.4 If no positive tubes result from potable
water samples, perform the MPN procedure,
quarterly, on a known coliform-positive sample.
Confirm the positive presumptive tubes and
perform the Completed Test on all positive
confirmed tubes.
5.4 Minimal Medium ONPG-MUG (MMO-MUG)
Test
5.4.1 When using bulk medium, prepare and
incubate a control for each analysis to
determine whether the medium has been
contaminated. Control should consist of a test
tube with the MMO-MUG medium to which
sterile water has been added.
QC 5.4.2 Check each lot of medium with a total
coliform-positive control (e.g., Klebsiella
42
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pneumonia) and a total coliform-negative control
(e.g., Pseudomonas aerug/nosa).
5.4.3 Incubate at 35° + 0.5°C for 24 hours. A
yellow color in the medium indicates the
presence of total coliforms.
5.4.4 After incubation for 24 hours, if the
sample color is indeterminate using a reference
comparator, reincubate for another four hours
(up to but not more than 28 hours). If the
sample color remains indeterminate, the
laboratory should consider the sample invalid
and request another sample from the same site.
QC 5.4.5 Laboratories are strongly encouraged to
perform parallel testing between the MMO-MUG
Test and another EPA- approved procedure for
enumerating total coliforms for at least several
months and/or over several seasons to assess
the effectiveness of the MMO-MUG Test for the
wide variety of water types submitted for
analysis.
5.5 HPC Procedure
5.5.1 Use the pour plate method to determine
the HPC for potable water samples.
5.5.2 For most potable water samples,
countable plates can be obtained by plating 1.0
ml or 0.1 ml volume of the undiluted sample.
5.5.3 Aseptically pipet sample into bottom of
100 mm x 15 mm petri dish. Add 12-15 ml of
tempered melted (44°-46°C) HPC agar to each
petri dish. Mix the sample and melted agar
carefully to avoid spillage. After agar plates have
solidified on a level surface, invert plates and
incubate at 35° ± 0.5°C for 48 ± 3 hours.
Stack plates in incubator to allow proper air
circulation to maintain uniform incubation
temperature. Do not stack plates more than four
high.
5.5.4 Count colonies manually using a counting
aid such as a Quebec colony counter. Consider
only plates having 30 to 300 colonies in
determining plate count, except for plates
inoculated with 1.0 ml volume of undiluted
sample. Counts less than 30 for such plates are
acceptable. (Fully automatic colony counters are
not suitable because of the size and small
number of colonies observed when potable
water is analyzed for HPC.)
5.5.5 Check each batch of HPC agar for
sterility by pouring initial and final control
plates. Reject data if controls are contaminated.
6. Sample Collection, Handling, and
Preservation
(Applicable to those laboratories that collect samples;
all laboratories are responsible for paragraphs 6.4 and
6.5)
6.1 Sample Collector
Collector is trained in sampling procedures and, if
required, approved by the appropriate regulatory
authority or its designated representative.
6.2 Sampling
Samples must be representative of the potable water
distribution system. Water taps used for sampling are
free of aerators, strainers, hose attachments, mixing
type faucets, and purification devices. Maintain a
steady water flow for at least 2 minutes to clear the
service line before sampling. Collect at least a 100
ml sample volume, allow at least 1/2-inch air space
to facilitate mixing of sample by shaking.
6.3 Sample Icing
Sample collectors who deliver samples directly to the
laboratory should ice samples immediately after
sample collection.
6.4 Sample Holding/Travel Time
Holding/travel time between sampling and analysis is
not to exceed 30 hours. If laboratory is required by
State regulation to analyze samples after 30 hours
and up to 48 hours, the laboratory is to indicate that
the data may be invalid because of excessive delay
before sample processing. No samples received after
48 hours are to be analyzed for compliance. All
samples received in the laboratory are to be analyzed
on the day of receipt.
6.5 Report Form
Immediately after collection, enter on the sample
report form the sample site location, sample type
(e.g., routine, check), date and time of collection, free
chlorine residual, collector's initials, and any remarks.
Also include the date and time of sample arrival at the
laboratory and the date and time analysis begins.
Record additional information as required by the
National Primary Drinking Water Regulations.
6.6 Chain-of-Custody
Follow applicable State regulations pertaining to
chain-of-custody.
7. Quality Assurance
The laboratory prepares and follows a written QA plan
(see Chapter Ill's discussion of QA plans) which is to
be available for inspection by the certification officer.
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8. Records and Data Reporting
Records of microbiological analyses are kept by the
laboratory or are accessible to the laboratory for at
least five years. Actual laboratory reports may be
kept, or data may be transferred to tabular
summaries, provided that the following information is
included:
• Date, place, and time of sampling, name of
persons who collected the sample.
• Identification of sample as to whether it is a
routine distribution system sample, check sample,
raw or process water sample, or other special
purpose sample.
• Date and time of sample receipt and analysis.
• Laboratory and persons responsible for
performing analysis.
• Analytical technique/method used
• Results of analysis. Base results of coliform
analyses on data from Confirmed Test or
Completed Test (for MPN Technique). Base MF
results on initial counts or verified counts.
9. Action Response to Laboratory
Results
9.1 Notification of Authorities
Promptly notify the proper authorities of unsatisfactory
results on the basis of Confirmed Test (for MPN
Technique) or unverified MF coliform data.
9.2 Adjustments in Coliform Counts
Although check sampling is to be initiated on the
basis of MPN Confirmed Test and unverified MF
coliform counts, data used to determine monthly
compliance may be adjusted by using the MPN
Completed Test and/or verified MF results.
9.3 High Concentrations of Non-Coliform
Organisms
Alert proper authorities to the occurrence of high
background levels of non-coliform organisms
observed by the MF procedure, or turbid tubes
lacking gas using the MPN procedure.
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Sample Forms for On-Site Evaluation of Laboratories Analyzing Public Water Supplies—Microbiology
Laboratory_
Street
City.
State
Telephone Number.
Survey by_
Affiliation
Date
Codes for Marking On-Site Evaluation Forms
S - Satisfactory X - Unsatisfactory U - Undetermined NA - Not Applicable
1. Personnel
Position/Title
Laboratory
Director
Supervisor/
Consultant
Professional
(note discipline)
Technician/
Analyst
Name
Time in Present
Position
Academic
Training and/or
Degree
Present
Specialty
Experience
(years/area)
45
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2. Laboratory Facilities
Laboratory facilities clean, temperature and humidity controlled
Adequate lighting at bench top
Laboratory has provision for disposal of microbiological wastes
3. Laboratory Equipment, Supplies, and Materials
3.1 pH Meter
Manufacturer Model_
Accuracy ± 0.1 units
Scale graduation, 0.1 units
Maintains electrodes according to manufacturer's
recommendations
pH buffer solution aliquots used only once
QC Commercial buffer solutions dated when received and
discarded before expiration date
QC Standardize pH meter each use period with
pH 7.0 and 4.0 standard buffer
3.2 Balances (Top Loader or Pan)
Manufacturer Model_
Detects 100 mg at a 150 gram load
QC Calibrate balance monthly using Class S or S-1 reference
weights or weights traceable to Class S or S-1 weights.
If non-reference weights are used, calibrate non-reference
weights with Class S or S-1 reference weights
QC Correction data available with S or S-1 weights
QC Annual service contract or internal maintenance
protocol and record maintained
3.3 Temperature Monitoring Device
Use glass/mercury or dial thermometer in incubator.
Units graduated in no more than 0.5 °C increments
No separation in mercury column
QC Check calibration of glass/mercury thermometers annually
and dial thermometers quarterly at the temperature used
against a reference NBS thermometer or one meeting the
requirements of NBS Monograph 150
46
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QC Recalibrate continuous recording devices used to monitor
incubator temperature annually against a NBS thermometer or
one meeting the requirements of NBS Monograph 150
3.4 Incubator Unit
Manufacturer Model_
Maintains internal temperature of 35° ± 0.5°C
Place thermometers on top and bottom shelves in
use area of non-portable incubators
Immerse thermometer bulb in liquid
Culture dishes and tubes fit snugly in aluminum
block incubator
QC Record temperature twice daily for days in use, with
readings separated by at least four hours
3.5 Autoclave
Manufacturer_ Model_
Temperature gauge with sensor on exhaust
Operational safety valve
Maintains sterilization temperature during cycle
Completes entire cycle within 45 minutes when a
12-15 minute sterilization period is used
Depressurizes slowly to insure media do not boil
over and bubbles do not form in fermentation tubes
QC Record date, contents, sterilization time, and
temperature for each cycle
QC Establish service contract or internal maintenance protocol
QC Heat-sensitive tape, spore strips or ampoules, or maximum
temperature registering thermometer used during each
autoclave cycle
QC Check automatic timing mechanism accuracy with
stop-watch quarterly
3.6 Hot Air Oven
Manufacturer Model_
Hot air oven maintains a temperature of 170°-180°C
Thermometer graduated in no more than 10°C increments
Place thermometer bulb in sand
QC Records include date, sterilization time, and
temperature of each cycle
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3.7 Colony Counter
Manufacturer_ Model_
A dark field colony counter available to count
Heterotrophic Plate Count colonies
3.8 Conductivity Meter
Manufacturer Model_
Suitable for checking laboratory pure water. Readable in
ohms or mhos, has a range of 2 ohms to 2 megohms or
equivalent micromhos ± 2%
QC Conductivity meter is calibrated monthly with a
0.01 M KCI solution
3.9 Refrigerator(s)
Manufacturer Model_
Maintains temperatures of 1 ° to 5°C
Thermometer(s) graduated in 1°C increments or less
Thermometer bulb(s) immersed in liquid
QC Temperature recorded for days in use
3.10 Inoculating Equipment
Metal or plastic loops, or applicator sticks sterilized by dry heat
Metal loops and/or needles are made of nickel alloy or platinum
3.11 Membrane Filtration Equipment, Membrane Filters and Pads
Manufacturer Model,
MF units of stainless steel, glass, or autoclavable plastic
Units do not leak, not scratched or corroded
10 to 15X magnification device with fluorescent light source
Forcep tips without corrugations
Membrane filters from cellulose ester material, white,
gridmarked, 47 mm diameter, 0.45 pm pore size
Alternate pore size used
Membrane filters recommended by manufacturer for
total cohform analysis
Membrane filters and pads are purchased presterilized
or autoclaved before use
QC Record lot numbers of membrane filters and date received
48
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QC Determine sterility of each lot of membrane filters by placing
one membrane filter in non-selective broth medium
3.12 Culture dishes
Use presterilized plastic or sterilized glass dishes
Incubate loose-lid dishes in a tight fitting container
Sterilize glass culture dishes in stainless steel or aluminum
canisters or in heavy aluminum foil or char-resistant paper
Reseal open packs of disposable culture dishes between uses
3.13 Pipets
Sterilize glass pipets in stainless steel or aluminum canisters
or individual pipets wrapped in char-resistant paper
Reseal packs of disposable sterile pipets between
major use periods
Pipets not etched, mouthpiece and tip are not
chipped, graduation markings legible
3.14 Culture Tubes and Closures
Tubes are borosilicate glass or other corrosion-resistant glass
Culture tubes are of sufficient size that medium
plus sample does not exceed 3/4 full
Closures are stainless steel, plastic, aluminum, or
screw caps with non-toxic liner
3.15 Sample Containers
Capacity at least 120 ml_ (4 oz)
Sample bottles are wide mouth plastic with a non-toxic
cap liner, or borosilicate glass with a ground glass stopper,
or other EPA-approved sample containers such as
single-service sterilized plastic sampling bags with
sodium thiosulfate
Cover glass-stoppered bottle top with aluminum
foil or char-resistant paper prior to sterilization
3.16 Glassware and Plasticware
Glass made of borosilicate or other corrosion-resistant glass
Free of chips and cracks
Graduation marks are legible
Plastic items are clear and non-toxic
Graduated cylinders used to measure sample
volume have a 2.5% tolerance or less
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Pipets used to measure sample volumes have a
2.5% tolerance or less
4. General Laboratory Practices
4.1 Autoclave Sterilization Procedures at 121°C
Item Time
Membrane filter and pads 10 min_
Carbohydrate media 12-15 min_
Contaminated test materials 30 min_
Membrane filter assemblies 15 min_
Sample collection bottles 15 min_
Individual glassware 15 min_
Dilution water blanks 15 min_
Rinse water 15 min_
Remove autoclaved MF filters and pads and
all media immediately after sterilization cycle
Membrane filter assemblies are autoclaved at
start of each filtration series
4.2 Sample Containers
Stock 10% sodium thiosulfate solution free of turbidity
Add sodium thiosulfate to sample containers
prior to sterilization
Sterilized sampling bags contain sodium thiosulfate
QC Determine sterility of each lot of sample bottles or presterilized
sample bags by adding non-selective broth, incubating at 35° C
for 24 hours and checking for growth
4.3 Reagent Water
Use reagent water to prepare media, reagents, and
dilution/rinse water
QC Reagent water is tested to assure the following
minimum criteria are met:
Parameter Limits Frequency
Conductivity > 0.5 megohms or monthly
< 2 micromhos at
25°C
50
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Metals—Pb , Cd, Cr, Not greater than annually
Cu, Ni, Zn 0.05 mg/L per con-
taminant. Collec-
tively not greater
than 0.1 mg/L
Total chlorine None detected monthly
residual
Heterotrophic < 500/mL monthly
Plate Count
Bacteriological Ratio 0.8-3.0 annually
quality of
reagent water
4.4 Dilution/Rinse Water
Prepare stock buffer solution or peptone water
according to Standard Methods, 16th Edition, p. 855
Stock buffer autoclaved or filter sterilized, labeled,
dated, and free of turbidity
10% peptone stock solution autoclaved, or filter
sterilized, labeled, dated, and free of turbidity
Prepare dilution/rinse water by adding 1.25 mL volume of
stock buffer solution and 5 ml volume of MgCIa stock solution
per liter of laboratory pure water
Prepare 0.1% peptone water by adding 10 ml of 10%
stock solution per liter of laboratory pure water
QC pH of stock phosphate buffer solution is 7.2 ± 0.2
QC pH of peptone water is 6.8 ± 0.2
QC Check dilution/rinse water for sterility
4.5 Glassware Washing
Use distilled or deionized water for final rinse
QC Perform inhibitory residue test on clean glassware
4.6 Media (General Requirements)
Commercially available dehydrated or prepared media used
Dehydrated media stored in cool, dry location
"Caked" or discolored dehydrated media discarded
Date dehydrated media when received and when
initially opened
Discard dehydrated media that has passed the
manufacturer's expiration date
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Discard opened dehydrated media after 6 months;
if stored in a desiccator, storage is extended to 12 months
QC Media Preparation Records include:
(a) Date of preparation
(b) Type of media
(c) Lot number
(d) Sterilization time and temperature
(e) Final pH
(f) Technician's initials
4.7 Membrane Filter Media
M-Endo or M-Endo LES broth or agar, final pH 7.2 ± 0.2
Dissolution of m-Endo broth or agar and m-Endo agar LES:
(a) Boiling water bath
(b) Hot plate with stir bar, constantly attended
Prepare and store media in sterile flasks
Use only 95% ethanol, not denatured
Refrigerate membrane filter broth no longer than 96 hours
Refrigerate membrane filter poured agar plates
no longer than 2 weeks
Ampouled m-Endo broth refrigerated in accordance
with manufacturer's expiration date
4.8 Multiple Tube Fermentation (MPN or MTF) Technique Media
Lauryl tryptose (lauryl sulfate) broth
Lactose broth
Dispense broth medium in volumes not less than 10 mL/tube
Use MPN media in tubes with loose-fitting closures within
one week
Store MPN media in screw cap tubes no longer than three months;
discard if evaporation exceeds 10% of original volume
Overnight incubation at 35°C of refrigerated sterilized
MPN media
Lauryl tryptose (lauryl sulfate) broth:
Autoclave at 121 °C for 12-15 minutes double strength;
final pH 6.8 ± 0.2
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Lactose broth:
Autoclave at 121 °C for 12-15 minutes, double strength;
final pH 6.7 ± 0.2
Brilliant green lactose bile broth:
Autoclave at 121 °C for 12-15 minutes; final pH 7.2 ± 0.2
Levine's Eosin Methylene Blue (EMB) agar (Completed Test):
Autoclave at 121 °C for 12-15 minutes (store refrigerated
two weeks) or use boiling water bath or direct heat for
dissolution (use same day); final pH 7.1 ± 0.2
m-Endo LES agar (Completed Test)
Prepare medium in a sterile flask using boiling water bath or
direct heat to boiling point; final pH 7.2 ± 0.2
4.9 Heterotrophic Plate Count (HPC) Medium
Temper melted agar (44° - 46°C) before pouring
Melted agar held no longer than 8 hours
Do not melt sterile medium more than once
Autoclave at 121 °C for 15 minutes, time adjusted
depending on volume
Final pH 7.0 ± 0.2
5. Analytical Methodology
5.1 Approved methods used as referenced in 40 CFR 141 "National Primary
Drinking Water Regulations." Alternate methods, if applicable,
have EPA approval
5.2 Membrane Filter Technique
Filter funnels and receptacle sterile at start of series
Shake sample vigorously
Examine 100 ml_ ± 2.5 ml of sample
Rinse funnel by flushing several 20 to 30 - ml portions of
sterile buffered water through membrane filter
Remove MF with a sterile forceps, grasping the area outside
the effective filtering area
Roll MF onto medium pad or agar so air bubbles are not formed
Incubation Conditions:
Total incubation time 22 to 24 hours at 35° ± 0.5°C
Incubate in high humidity or in tight fitting culture dishes
53
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Colony Counting:
Fluorescent light positioned for maximum reflection of
colonies with sheen
Colonies uniformly dispersed over effective filtration area
Coliforms reported as coliform number per 100 mL
Confluent growth—membrane covered with bacterial
growth; TNTC—greater than 200 total bacterial colonies
if reported as confluent growth or TNTC with less than
5 coliforms, request another sample from same
sampling site
if reported as confluent growth or TNTC with 5 or more
coliforms, request check samples
Verification procedure conducted on all unsatisfactory samples
(>4 colonies/100 ml)
Use lactose broth or lauryl tryptose broth and confirm by
BGLB media or EPA-approved rapid test
Adjust initial counts based on verification
QC Conduct MF sterility check at beginning and end of each
filtration series
QC Analysts agree within 10% on the number of sheen
colonies on same membrane filter
5.3 Total Coliform Multiple-Tube Fermentation Technique
Total Coliform Presumptive Phase
Five standard portions, either 10 or 100 ml
Sample shaken vigorously before test
Tubes incubated at 35° ± 0.5°C for 24 ± 2 hours
Examined for gas (any size bubble)
24-hour gas-positive tube submitted to confirmed phase
Negative tubes returned to incubator
Examined for gas at 48 ± 3 hours; positive tubes
submitted to confirmed phase
Total Coliform Confirmed Phase
Presumptive positive tubes shaken gently or mixed by rotating
One loopful or one dip of applicator transferred from
presumptive positive tube to BGLB broth
Incubated at 35° ± 0.5°C; checked at 24 hours for
gas production
54
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Negative tubes reincubated for additional 24 hours;
checked for gas production
Results recorded; MPN value calculated
Total Coliform Completed Test
Completed Test conducted quarterly on not less than 10%
of all unsatisfactory samples (> three positive confirmed
tubes)
Positive confirmed tubes streaked on m-Endo, m-Endo
LES, or EMB agar plates for colony isolation
Incubated at 35° + 0.5°C for 24 ± 2 hours
Growth from coliform colonies inoculated into lactose
or LTB medium, incubated at 35° ± 0.5°C and observed for
gas production within 48 hours
Adjust the number of positive confirmed tubes on the
basis of the Completed Test
5.4 Minimal Medium ONPG-MUG (MMO-MUG) Test
When using bulk medium, each analysis or series of analyses
includes a control consisting of test tube with MMO-MUG
medium to which sterile water has been added
Each lot of medium checked with a total coliform-positive
control and a total coliform-negative control
Tubes incubated at 35° ± 0.5°C for 24 hours and examined
for production of yellow color
If test is indeterminate after 24 hours, the sample
is reincubated for another 4 hours (up to but not more than
28 hours)
If sample color is indeterminate after 28 hours, sample is
invalidated
Parallel testing between MMO-MUG Test and another
EPA-approved procedure for enumerating total coliforms
conducted for several months
5.5 Heterotrophic Plate Count (HPC) Procedure
Pour plate method used to determine HPC
Shake sample vigorously
Volume plated is between 0.1 ml and 1.0 ml
Add agar, tempered to 44°-46°C, and mix agar and sample
Incubate plates in inverted position at 35° ± 0.5 °C for 48
± 3 hours
55
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Do not stack plates more than four high
Count colonies using a Quebec colony counter
Count only plates in countable range, 30-300 colonies
QC Perform sterility check by pouring an initial and final control
plate for each container and/or batch of HPC agar
6. Sample Collection. Handling, and Preservation
6.1 Follow sample procedures described in Standard Methods for the
Examination of Water and Wastewater or Microbiological
Methods for Monitoring the Environment,^.^. EPA-600/8-78-017
6.2 Sample collectors receive training
6.3 Samples representative of distribution system
6.4 Water taps free of any attachments and mixing type faucets
6.5 Water run to waste for at least two minutes
6.6 Sample volume is at least 100 ml with sufficient space for
mixing sample
6.7 Sample report form completed by collector
6.8 Samples iced when carrying samples directly to laboratory
6.9 Record date and time of sample arrival at laboratory and
date and time analysis begins
6.10 Transit time does not exceed 30 hours
If laboratory is required by State regulation to examine
samples after 30 hours and up to 48 hours, data are
indicated as possibly invalid
All samples arriving in laboratory after 48 hours are not
analyzed for compliance use
6.11 Compliance with State chain-of-custody regulations, if required
7. Quality Assurance Program
7.1 Written QA Plan implemented and available for review
7.2 Quality control records maintained for five years
QC 7.3 PE sample is satisfactorily analyzed annually (if available)
8. Data Reporting
8.1 Data entered on the sample report form is checked and initialed
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8.2 Sample report forms are retained by laboratory or State program
for five years
Report forms include identification of sample, date and
time of sample receipt and analysis, laboratory and
person(s) responsible for performing analyses,
analytical method used and results of analysis
Results of analyses
MPN data based on Confirmed or Completed Test and MF
data based on initial or verified counts
9. Action Response by Laboratory
9.1 Notify the responsible authorities of unsatisfactory results
9.2 Notify responsible authorities of check sample results
9.3 Alert responsible authorities to high non-coliform levels in sample
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Chapter VI
Radiochemistry
1. Personnel
1.1 Measurement of Gross Alpha and Gross Beta
Analyst or technician responsible only for the
measurement of gross alpha and gross beta
radioactivities.
1.1.1 Academic training: Minimum of a high
school diploma or its equivalent, plus
specialized training in standards and sample
preparation, instrument calibration, calculations,
and data handling.
1.1.2 Experience: Minimum of 6 months of on-
the-job.
1.1.3 A technician may assist in routine sample
preparation and radioanalytical procedures
provided that such work is supervised and
validated by an analyst with qualifications as
described in section 1.2.
1.2 Measurement of Specific Radionuclides
Analyst responsible for the measurement of specific
radionuclides described in the National Primary
Drinking Water Regulations (NPDWR).
1.2.1 Academic training: Minimum of
bachelor's degree in chemistry, radiochemistry,
radioisotope technology, or equivalent.
1.2.2 Experience1: Minimum of 1 year of
appropriate experience in radiation
measurements and radiochemical procedures.
1.3 Laboratory Supervisor, Manager, or Director
1.3.1 Academic training: Minimum of
bachelor's degree or its equivalent.
1.3.2 Experience1:
experience.
Minimum of 5 years of
security and integrity of the drinking water samples
and analytical data are provided. In addition, a work-
place for wet chemistry operations and for equipment
that is critical to valid measurement of radioactive
contaminants is necessary.
2.2 Location of Instruments
The counting mstrument(s) necessary for
measurement of those radionuclides described in the
NPDWR must be located in a room other than the
one in which samples and standards are being
prepared and in which other types of wet chemical
analyses are being performed. All instruments should
be properly grounded, and a regulated power supply,
either external or internal, should be available to each
instrument.
2.3 Preparation of Standards
In areas where radioactive standards are being
prepared, care must be taken to minimize
contamination of surfaces, other samples and
personnel. Either bench surfaces of an impervious
material covered with adsorbent paper, or trays
(stainless steel, plastic, or fiberglass) lined with
adsorbent paper are acceptable.
2.4 Laboratory Fixtures
The following items are necessary in a laboratory
performing even the most basic radiochemical
measurements (gross alpha and gross beta
radioactivities) for compliance monitoring of drinking
water supplies.
2.4.1 Sink with tap water and connection to the
sanitary sewer system.
2. Laboratory Facilities
2.1 General
The analysis of compliance monitoring samples
should be conducted in a laboratory facility where
1 Each year of college-level training in related scientific fields of
demonstrated equivalency shall be considered equal to 1 year of
work experience. Such a substitution should not exceed one-half of
the required experience.
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2.4.2 Electrical outlets (120V AC grounded).
2.4.3 Source of distilled or deionized water.
2.4.4 Exhaust hood.
2.4.5 For laboratories that are performing wet
chemistry separations that require filtration of a
precipitated fraction of the sample, a vacuum
source (pump or aspirator) should also be
available.
3. Laboratory Equipment and Supplies
The following equipment and supplies are necessary
for the analyses of regulated radionuclides. If a
laboratory is not to be certified for a particular
radionuclide parameter, instruments specified for
analysis of that parameter are not necessary.
3.1 General Instrumentation and Equipment
3.1.1 Analytical balance: Precision, ± 0.1
mg. Minimum scale readability, 0.1 mg.
3.1.2 pH meter or specific ion meter:
3.1.2.1 pH meter: Accuracy, ± 0.5
units. Scale readability, ± 0.1 units.
3.1.2.2 Specific ion meter: Expanded
scale millivolt capability. Readable and
accurate to ± 0.1 mV.
3.1.3 Drying oven or lamp: Gravity
convection type, or infrared drying lamp.
3.1.4 Desiccator: Glass or plastic models,
depending on particular application.
3.1.5 Hot plate: Units with selectable
temperature control for safe heating of
laboratory reagents and samples.
3.1.6 Glassware: Borosilicate type glass. All
volumetric glassware should be marked Class
A, denoting that it meets Federal specifications
and need not be calibrated before use.
3.1.7 Muffle furnace: Automatically controlled
with a chamber capacity of at least 2,200 cc (10
x 9.5 x 23) and a maximum operating
temperature of 1,000°C continuous and 1,100°C
intermittent.
3.1.8 Centrifuge: General purpose table-top
model with a maximum speed of at least 3,000
rpm and a loading option of 4 x 50 ml.
3.2 Radiation Counting Instruments
The types of radiation counting systems needed to
comply with measurements described in the NPDWR
are set forth below:
3.2.1 Liquid scintillation system: A liquid
scintillation system is essential if the laboratory
is to be certified for the measurement of tritium
and/or radon in drinking water samples. The
system needs to be such that the sensitivity will
meet or exceed the requirements of section
141.25 of the NPDWR.
3.2.2 Gas-flow proportional counting
system: A gas-flow proportional counting
system may be used for the measurement of
gross alpha and gross beta activities, radium-
226, radium-228, strontium-89, strontium-90,
cesium-134, and iodine-131 as described in the
reference cited in section 141.25(a). The
detector may be either a "windowless" (internal
proportional counter) or a "thin window" type. A
combination of shielding and a cosmic (guard)
detector operated in anticoincidence with the
main detector should be used to achieve low
background beta counting capability. The alpha
and beta background count of the system
should be such that the sensitivity of the
radioanalysis of water samples will meet or
exceed the requirement of 40 CFR 141.25 with
reasonable counting time (not more than 1,000
minutes).
3.2.3 Alpha scintillation counting system:
For measurement of gross alpha activities and
radium-226, a scintillation system designed for
alpha counting may be substituted for the gas-
flow proportional counter described. In such a
system, a Mylar disc coated with a phosphor
(silver-activated zinc sulfide) is either placed
directly on the sample or on the face of a photo-
multiplier tube, enclosed within a light-tight
container, along with the appropriate electronics
(high voltage supply, preamplifier, amplifier,
timer and sealer).
3.2.4 Low background alpha and beta
counting systems other than a gas-flow
proportional counting system: Such a system
should have a cosmic guard detector operated
in anticoincidence with the signal from the
sample detector, and shielding, such that the
alpha background will not exceed 0.2 cpm and
the beta background will not exceed 2.0 cpm for
a 2 inch diameter counting planchet geometry.
3.2.5 Scintillation cell system: A scintillation
system designed to accept scintillation flasks
("Lucas cells") should be used for the specific
measurement of radium-226 by the radon
60
-------
emanation method. The system consists of a
light-tight enclosure capable of accepting the
scintillation flasks, a detector (phototube), and
the appropriate electronics (high voltage supply,
amplifier, timers, and sealers). The flasks (cells)
needed for this measurement may either be
purchased from commercial suppliers or
constructed by the laboratory.
3.2.6 Gamma spectrometer systems: Either
a sodium iodide, Nal(TI) crystal; a solid state
lithium drifted germanium detector; or a gamma-
X photon detector connected to a multichannel
analyzer is needed if the laboratory is to be
certified for analyses of manmade photon
emitters.
3.2.6.1 If a sodium iodide detector is
used, a cylindrical 7.5 cm x 7.5 cm Nal
crystal is satisfactory. However, a 10
cm x 10 cm crystal is recommended.
The detector should be shielded with a
minimum of 10 cm of iron or
equivalent. It is recommended that the
distance from the center of the detector
to any part of the shield should not be
less than 30 cm. The multichannel
analyzer, in addition to appropriate
electronics, should contain a memory
of not less than 200 channels and at
least one readout device.
3.2.6.2 A system with a lithium drifted
germanium, or a high purity
germanium, or a gamma-X photon
detector may be used for measurement
of manmade photon emitters if the
efficiency of the detector is such that
the sensitivity of the system meets the
minimum detectable activity
requirements cited in 40 CFR 141.25.
These detectors should be shielded
with a minimum of 10 cm of iron or
equivalent. The multichannel analyzer,
in addition to appropriate electronics,
should contain a memory of not less
than 2,000 channels and at least one
readout device.
4. General Laboratory Practices
(None specified)
5. Analytical Methodology
The approved methods indicated in the NPDWR or
EPA-approved alternate methods, are to be used for
drinking water compliance monitoring.
6. Sample Collection, Handling, and
Preservation
Table VI-1 gives critical elements for sample handling
including Preservation, and Applicable Counting
instrumentation.
7. Quality Assurance
7.1 Inspections
Quality control data and records are to be available
for inspection.
7.2 Intercomparison Cross Check Studies
A laboratory needs to participate at least twice each
year in those EPA laboratory intercomparison cross
check studies that include each of the analyses for
which the laboratory is, or wants to be, certified.
Analytical results should be within control limits
described in "Environmental Radioactivity Laboratory
Intercomparison Studies Program -- FY 1981-1982"
(EPA- 600/4-81-004), or in subsequent revisions.
7.3 Performance Evaluation Studies
A laboratory also needs to participate once each year
in an appropriate water supply performance evaluation
(blind sample) study administered by EPA. Analytical
results must be within control limits established by
EPA for each analysis for which the laboratory is, or
wants to be, certified.
7.4 Operating Manuals
Operating manuals and calibration protocols for
counting instruments should be available to analysts
and technicians.
7.5 Maintenance of Records
Calibration data and maintenance records on all
radiation instruments and analytical balances should
be maintained in a permanently bound record.
7.6 Daily Quality Control
The following specifications are included in minimum
daily quality control:
7.6.1 A minimum of 10-percent duplicate
samples should be analyzed to verify internal
laboratory precision for a specific analysis. The
difference between duplicate measurements
should be less than two times the standard
deviation of the specific analysis as described in
EPA-600/4-81-004, Table 3. If difference
exceeds two standard deviations, prior
measurements are suspect; calculations and
procedures should be examined and samples
should be reanalyzed when necessary.
7.6.2 When 20 or more specific analyses are
performed each day, a counting standard and a
background sample should be measured with
each 20 samples. If less than 20 specific
61
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Table VI-1: Sample Handling, Preservation, and Instrumentation
Parameter
Preservative'
Container2
Instrumentation3
Gross alpha
Gross beta
Strontium-89
Strontium-90
Radium-226
Radium-228
Cesium- 134
lodine-131
Tritium
Uranium
Photon emitters
Cone. HCI or HNO3 to pH < 2"
Cone. HCI or HNO3 to pH < 2
Cone. HCI or HNO3 to pH < 2
Cone HCI or HNO3 to pH <2
Cone. HCI or HNO3 to pH <2
Cone. HCI or HNO3 to pH <2
Cone. HCI to pH < 2
None
None
Cone. HCI or HNO3 to pH <2
Cone. HCI or HNO3 to pH <2
P or G
P or G
PorG
P or G
P or G
PorG
PorG
P or G
PorG
P or G
P or G
A, B, or G
A or G
A orG
A or G
A, B, D, or G
A or G
A, C, or G
A or G
E
F
C
11t is recommended that the preservative be added to the sample at the time of collection unless suspended solids activity is to be measured.
However, if the sample must be shipped to a laboratory or storage area, acidification of the sample (in its original container) may be delayed
for a period not to exceed 5 days. A minimum of 16 hours must elapse between acidification and analysis.
2 P = Plastic, hard or soft; G = Glass, hard or soft
3 A = Low background proportional system; B = Alpha scintillation system, C = Gamma spectrometer [Nal(TI) or Ge(Li)]; D = Scintillation
cell (radon) system; E = Liquid scintillation system (section C.2.a), F = Fluorometer (section C.1 i); G = Low background alpha and beta
counting system other than gas-flow proportional.
4 If HCI is used to acidify samples which are to be analyzed for gross alpha or gross beta activities, the acid salts must be converted to nitrate
salts before transfer of the samples to planchets.
analyses are performed in any 1 day, a counting
standard and a background sample should be
measured along with the samples.
7.7 Instrument Performance Charts/Records
Quality control performance charts, or performance
records, should be maintained for each instrument.
7.8 QA Plan
The laboratory should prepare and follow a written QA
plan (see Chapter III, section on QA plan).
8. Records and Data Reporting
8.1 Legal Defensibility
Compliance monitoring activities should be made
legally defensible by the records kept of such
activities.
8.2 Retention of Records
Records of radioanalyses for compliance monitoring
of drinking water supplies are to be kept by the
laboratory for not less than three years. This includes
raw data, calculations, quality control data, and
reports.
8.3 Information to be Recorded
Actual laboratory reports may be kept, or data may be
transferred to tabular summaries provided that the
following information is included:
8.3.1 Date, place, and time of sampling; name
of person who collected the sample.
8.3.2 Identification of sample as to whether it is
a routine distribution system sample, check
sample, raw or process water sample, surface
or ground water sample, or other special
purpose sample.
8.3.3 Date of sample receipt and analysis.
8.3.4 Laboratory and persons responsible for
performing analysis.
8.3.5 Analytical technique/method used.
8.3.6 Results of analysis.
8.4 Computer Programs
Computer programs should be verified initially by
manual calculations and the calculations should be
available for inspection.
9. Action Response to Laboratory
Results
When action response is a designated laboratory
responsibility, the proper authority must be notified
promptly of noncompliance sample results, and a
request must be made for resampling from the same
sampling point.
62
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Sample Forms for On-Site Evaluation of Laboratories Involved in Analysis of Public Water Supplies—Radiochemistry
Laboratory
Street
City State.
Survey By
Affiliation.
Date Telephone No..
63
-------
Laboratory.
Location
. Evaluator.
. Date
Personnel
Position/title
Analyst(s)/
techmcian(s)
Supervisory
analyst
Laboratory
supervisor/
director
Support
(e.g. .electronic
technician)
Name
Academic training
HS BA/BS MA/MS Ph.D.
Present
Specialty
Experience (years and area)
64
-------
Laboratory.
Location
. Evaluator.
Date
Laboratory Facilities
Item
Laboratory
Sink- with tap water
and sanitary sewer
connections
Electrical outlets -
1 20V ac, grounded
Distilled or deionized
water
Exhaust hood
Vacuum source
Counting Room
Separate from wetjChemis-
try, sample and standards
preparation I area
Regulated power
supply
Adequate electrical ground
Available
Yes No
Comments
65
-------
Laboratory.
Location
. Evaluator.
Date
General Laboratory Equipment and Instruments
Item
Analytical balance
pH meter
Specific ion meter
Conductivity meter
Drying oven
Infrared lamp
Desiccator
Hot plate
Muffle furnace
Centrifuge
Fluorometer
No. of
Units
Manufacturer
Model
Age and Condition
66
-------
Laboratory
Location
Date
Evaluator
Thin Window Gas-Flow Proportional Counter
Instrument number
Calibration Standard
Type:
Alpha
Beta
Supplier:
Alpha
Beta
Manufacturer
Counting gas
Model
Window density
(g/cm2)
Calibration frequency1
D W M
Year
Sample changing
Manual Automatic Capacity
Alpha Instrument
Operating voltage cpm
Other
background Be
-------
Laboratory
Location
Date
Evaluator
Low Background Alpha and Beta Counter (other than gas-flow proportional)
Instrument number
Calibration Standard
Type:
Alpha
Beta
Supplier:
Alpha
Beta
Manufacturer
Sample dish
diameter (in.) Qperati
Model Year
Alpha
ng voltage cpm
Calibration frequency1
D W M Other
'Daily, weekly, monthly.
2Quarterly, semiannually, annually
3Good operating but needs repair, not operating
Manual
Sample changing
Automatic
Instrument background
Beta
Operating voltage cpm
Capacity
Gamma
Operating voltage cpm
Service Maintenance frequency2
Q S A Other
Condition3
G R N
Are operating manuals readily available to the operator?
Are calibration protocols available to the operator?
Are calibrations kept in a permanent control chart record?
Are permanent service maintenance records kept on these systems?
Yes n No n
Yes o No D
Yes n No n
Yes D No D
Liquid Scintillation Counter
Instrument number
Calibration Standard
Type:
Supplier:
Manufacturer
Model
Discriminator channels
1 2 3
Calibration frequency1
D W M
Year
Visual
Other
Sample changing
Manual Automatic Capacity
Data readout
Channel printout
1 2 3
External standard
Yes No
Service Maintenance frequency2
OS A Other
G
Refrigeration
Yes No
Condition3
R
N
'Daily, weekly, monthly.
'Quarterly, semiannually, annually
3Good operating but needs repair, not operating.
Are operating manuals readily available to the operator? Yes D No G
Are calibration protocols available to the operator? Yes G NOD
Are calibrations kept in a permanent control chart record? Yes D No a
Are permanent service maintenance records kept on these systems? Yes a No a
68
-------
Laboratory
Location
Date
Evaluator
Alpha Scintillation Counter
Instrument number
Calibration Standard
Type:
Supplier:
Manufacturer
Model
Year
Alpha phosphor location
Photo tube Samples
Calibration frequency1
D W M
Other
Manual
Sample changing
Automatic Capacity
Instrument background
Operating voltage cpm
Service Maintenance frequency2
Q S A Other
Condition3
CRN
'Daily, weekly, monthly.
'Quarterly, semiannually, annually.
3Good operating but needs repair, not operating.
Are operating manuals readily available to the operator? Yes a No 3
Are calibration protocols available to the operator? Yes P No a
Are calibrations kept in a permanent control chart record? Yes a No a
Are permanent service maintenance records kept on these systems? Yes p NOD
Radon Gas-Counting System
System number
Calibration Standard
Type:
Supplier:
Counting Instrument
Make Model Year
Calibration frequency1
D W M Other
Gas-counting cells/system
Manufacturer of gas-counting cells
Service Maintenance frequency2
Q S A Other
Condition9
CRN
'Daily, weekly, monthly.
'Quarterly, semiannually, annually.
3Good operating but needs repair, not operating.
Are operating manuals readily available to the operator? Yes a No a
Are calibration protocols available to the operator? Yes D No u
Are calibrations kept in a permanent control chart record? Yes p No D
Are permanent service maintenance records kept on these systems? Yes D No p
69
-------
Laboratory
Location _
Date
Evaluator
Gamma Spectrometer Systems
Detector System
Calibration Standard
Type:
Supplier:
Type Make
System number
Model
Make Model
Analyze
Calibration frequency1
D W M Other
r System
Year
Year
Service Maintenance frequency2
Q S A Other
Size
Channels
Condition3
G R N
'Daily, weekly, monthly Are operating manuals readily available to the operator? Yes n NOD
2Quarterly, semiannually, annually Are calibration protocols available to the operator? Yes 3 No n
3Good operating but needs repair, not operating Are calibrations kept in a permanent control chart record? Yes 3 No n
Are permanent service maintenance records kept on these systems? Yes a No 3
70
-------
Laboratory
Location —
Date
Evaluator
Sample Handling and Preservation
Parameter
Gross alpha activity
Gross beta activity
Strontium-89
Strontium-90
Radium-226
Radium-228
Cesium-134
lodine-131
Tritium
Uranium
Photon emitters:
a.
b.
c.
d
e.
Container
Used
Preservative
Used
Comments
Satisfactory
Yes No
71
-------
Laboratory
Location _
Date
Evaluator
Methodology
Parameter
Gross alpha
activity
Gross beta
activity
Strontium-89
Strontium-90
Radium-226
Radium-228
Cesium-134
lodine-131
Tritium
Uranium
Photon
emitters
(identify) :
a
b.
c.
d.
e.
Sample Load
per Month
Method1 used. Cite Edition. Year, and Page
EPA APHA ASTM
'Approved Other
HASL-300 Alternate
Satisfactory
Yes No
1 Methods used, other than approved alternate methods, must be referenced in the Drinking Water Regulations (Federal Register)
*Cite approval date
72
-------
Laboratory
Location _
Date
Evaluator
Quality Control
Item
Participation in
intercomparison
(cross check) studies
and performance
(blind) studies
(studies conducted
by EMSL-LV)
Reporting Period:
To
Verification of sample
results by duplicate
sample analysis
Use of quality
control charts or
records
Calibration and
maintenance
records available
Crosscheck Studies
(water) A1 B2
Gross alpha
Gross beta
Sr-89
Sr-90
Ra-226
Ra-228
Tritium
Uranium
1-131
Cs-134
Cs-137
Co-60
Ru-106
Yes
No
Frequency
Performance (Blind)
Studies (Water) A1 B2
Gross alpha
Gross beta
Sr-89 1
Sr-90
Ra-226
Ra-228
Uranium
Cs-134
Cs-137
Co-60
Ru-106
Written QA plan implemented
and available for review
Comments
Satisfactory
Yes No
'Scheduled frequency of participation by the Laboratory, times per year
2Number of acceptable performances (results) in the past year, where an acceptable result is a normalized deviation from the known value of < 3 0 Sigma
73
-------
Laboratory
Location _
Date
Evaluator
Data Reporting
Item
Records kept for 3 years
Actual laboratory reports
Tabular summary
Information included.
Date
Place of sampling
Time of sampling
Person collecting sample
Date of receipt of sample
Date of analysis
Type of analysis
Laboratory and person
responsible
Method(s) used
Results
Comments: system(s) used, frequency, etc.
74
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Appendix A
Chain-of-Custody Evaluations
A. Introduction
Written procedures for sample handling should be
available and followed whenever samples are
collected, transferred, stored, analyzed or destroyed.
For the purposes of litigation, it is necessary to have
an accurate written record which can be used to trace
the possession and handling of samples from the
moment of collection through analysis. The
procedures defined here represent a means to satisfy
this requirement.
A sample is in someone's "custody" if:
1. It is in one's actual physical possession;
2. It is in one's view, after being in one's
physical possession;
3. It is one's physical possession and then
locked up so that no one can tamper with it;
4. It is kept in a secured area, restricted to
authorized personnel only.
B. Sampling Collection, Handling and
Identification
1. It is important that a minimum number of
persons be involved in sample collection and
handling. Guidelines established in standard
manuals for sample collection preservation
and handling should be used (e.g., EPA
NPDES Compliance Sampling Inspection
Manual, MCD 51; Standard Methods for
Examination of Water and Wastewater). Field
records should be completed at the time the
sample is collected and should be signed or
initialed, including the date and time, by the
sample collector(s). Field records should
contain the following information:
a. Unique sample or log number;
b. Date and time;
c. Source of sample (including
location and sample type);
name,
d. Preservative used;
e. Analyses required;
f. Name of collector(s);
g. Pertinent field data (pH, DO, Cl residual,
etc.); and
h. Serial number on seals and transportation
cases.
2. Each sample is identified by affixing a
pressure sensitive gummed label or
standardized tag on the contamer(s) This
label should contain the sample number,
source of sample, preservative used, and the
collector(s') initials. Analysis required should
be identified. Where a label is not available,
the sample information should be written on
the sample container with an indelible
marking pen. An example of a sample
identification tag is illustrated in Figure A-1.
3. The sample container should then be placed
in a transportation case along with the chain-
of-custody record form, pertinent field
records, and analysis request form. The
transportation case should then be sealed
and labeled. All records should be filled out
legibly in pen. The use of locked or sealed
chests will eliminate the need for close
control of individual sample containers.
However, there will undoubtedly be
occasions when the use of a chest will be
inconvenient. On these occasions, the
sampler should place a seal around the cap
of the individual sample container which
would indicate tampering if removed.
C. Transfer of Custody and Shipment
1. When transferring the possession of the
samples, the transferee must sign and record
the date and time on the chain-of-custody
record. Custody transfers, if made to a
sample custodian in the field, should account
for each individual sample, although samples
75
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may be transferred as a group. Every person
who takes custody must fill in the appropriate
section of the chain-of-custody record.
2. The field custodian (or field sampler if a
custodian has not been assigned) is
responsible for properly packaging and
dispatching samples to the appropriate
laboratory for analysis. This responsibility
includes filling out, dating, and signing the
appropriate portion of the chain-of-custody
record. A recommended chain-of-custody
format is illustrated in Figure A-2.
3. All packages sent to the laboratory should be
accompanied by the chain-of-custody record
and other pertinent forms. A copy of these
forms should be retained by the field
custodian (either carbon or photocopy).
4. Mailed packages can be registered with
return receipt requested. If packages are sent
by common carrier, receipts should be
retained as part of the permanent chain-of-
custody documentation.
5. Samples to be transported must be packed
to prevent breakage. If samples are shipped
by mail or by other common carrier, the
shipper must comply with any applicable
Department of Transportation regulations.
(Most water samples are exempt unless
quantities of preservatives used are greater
than certain levels.) The package must be
sealed or locked to prevent tampering. Any
evidence of tampering should be readily
detected if adequate sealing devices are
used.
6. If the field sampler delivers samples to the
laboratory, custody may be relinquished to
laboratory personnel. If appropriate personnel
are not present to receive the samples, they
should be locked in a designated area of the
laboratory to prevent tampering. The person
delivering the samples should make a log
entry stating where and how the samples
were delivered and secured. Laboratory
personnel may then receive custody by
noting in a logbook the absence of evidence
of tampering, unlocking the secured area,
and signing the custody sheet.
D. Laboratory Sample Control
Procedures
Sample control procedures are necessary in the
laboratory from the time of sample receipt to the time
the sample is discarded. The following procedures
are recommended for the laboratory:
1. A specific person must be designated
custodian and an alternate designated to act
as custodian in the custodian's absence. All
incoming samples must be received by the
custodian, who must indicate receipt by
signing the accompanying custody/control
forms and who must retain the signed forms
as permanent records.
2. The custodian must maintain a permanent
logbook to record, for each sample, the
person delivering the sample, the person
receiving the sample, date and time received,
source of sample, date the sample was
taken, sample identification log number, how
transmitted to the laboratory, and condition
received (sealed, unsealed, broken container,
or other pertinent remarks). This log should
also show the movement of each sample
within the laboratory; i.e., who removed the
sample from the custody area, when it was
removed, when it was returned, and when it
was destroyed. A standardized format should
be established for logbook entries.
3. A clean, cry, isolated room, building, and/or
refrigerated space that can be securely
locked from the outside must be designated
as a "custody room."
4. The custodian must ensure that heat-
sensitive samples, light-sensitive samples,
radioactive samples, or other sample
materials having unusual physical
characteristics, or requiring special handling,
are properly stored and maintained prior to
analysis.
5. Distribution of samples to the analyst
performing the analysis must be made by the
custodian.
6. The laboratory area must be maintained as a
secured area, restricted to authorized
personnel only.
7. Laboratory personnel are responsible for the
care and custody of the sample once it is
received by them and must be prepared to
testify that the sample was in their
possession and view or secured in the
laboratory at all times from the moment it
was received from the custodian until the
time that the analyses are completed.
8. Once the sample analyses are completed,
the unused portion of the sample, together
with all identifying labels, must be returned to
the custodian. The returned tagged sample
must be retained in the custody room until
76
-------
permission to destroy the sample is received holding time has elapsed.) The same procedure
by the custodian. is true for sample tags. The logbook should
show when each sample was discarded or if
9. Samples will be destroyed only upon the order any sample tag was destroyed.
of the responsible laboratory official when it is
certain that the information is no longer required 10. Procedures must be established for audits of
or the samples have deteriorated. (For example, sample control information. Records should be
standard procedures should include discarding examined to determine traceability,
microbiological samples after the maximum completeness, and accuracy.
77
-------
Figure A-1 Sample Identification Tag Examples
U.S. EPAREGION
GENERAL CHEMISTRY
Official Sample No.
ui
u
a:
o
n
w
Date and Time
Sampler's Signature Office
Other Parameters:
PH
Cond
TS
DS
SS
BOD2
Turb
Color
Acid
Alk
S04
Cl
F
Cr. + 6
BOD5
U.S. EPAREGION
MICROBIOLOGY
Official Sample No.
LJJ
u
DC
3
0
(fl
Date and Time
Sampler's Signature Office
Tot. Col if
Fecal Colif.
Fecal Strep.
Salmonella
U.S. EPAREGION
PESTICIDES, ORGANICS
Official Sample No
LLJ
CJ
DC
0
W
Dafe and Time
Sampler's Signature Office
Pesticides
PCB's-
Organics:
EPA
Station No.
I Date Time Sequence No
Station Location
BOD
Solids
COD
Nutrients
Metak
Oil and Grease
D.O.
Bact
Other
Samplers:
Grab
rnmp
Remarks/Preservative:
O
78
-------
Figure A-2 Chain-of-Custody Record
Survey
Station
Number
Station Location
Date
Relinquished by: Signature
Relinquished by: Signature
Relinquished by: Signature
Relinquished by Signature
Dispatched by: Signature
Time
Samplers: Signature
Sample Ty
Water
Comp. Grab
pe
Air
Seq No.
No. of
Containers
Received by: Signature
Received by Signature
Analysis
Required
Date/Time
Date/Time
Received by: Signature i Date/Time
i
Received by Mobile Laboratory for Field analysis
Signature
Date/Time
Received for Laboratory by
Date/Time
Date/Time
Method of Shipment:
Distribution
Orig.—Accompany Shipment
1 Copy—Survey Coordinator Field Files
79
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Appendix B
Recommended Protocol for Regions Conducting On-Site Laboratory Evaluations
Before conducting the on-site evaluation, the Region
shall:
• Hold a pre-evaluation conference with appropriate
laboratory and field activity representatives to
establish a schedule that would have a minimum
impact on the laboratory activities.
• Request that a variety of tests be scheduled
during the on-site evaluation.
• Arrange for the laboratory staff to be available
during the on-site visit.
During the on-site visit, the team will:
• Evaluate the procedures and equipment used for
those specific analyses for which the laboratory
has requested certification, using the criteria in
this manual.
• Review the records and written standard operating
procedures for compliance with the required
sampling frequency, sample collection, sample
holding times, and if appropriate, resample
notification.
• Insure that the laboratory has a QA plan in effect
by:
— Determining if the laboratory has written
procedures (QA plan or equivalent) for
conducting its quality assurance program.
— Examining the quality assurance data to
determine if the quality assurance program is
being implemented.
• Complete the on-site checklists and other
evaluation forms during the visit (see Chapters IV,
V, and VI).
• Review the results of the evaluation with the
director of the laboratory, the director of State
water supply activities, and appropriate staff
members. The review should:
— Discuss any deviations in the observed
procedures and records.
— Recommend changes in equipment and supply
needs, staffing requirements, and facility
improvements, if necessary.
— Discuss possible assistance the Region can
provide the laboratory.
Evaluation Report for Principal State
Laboratories and Laboratories in Non-
Primacy States
After an on-site inspection, the evaluation team
should prepare a narrative report and action
memorandum. This report should contain all
information pertinent to the evaluation and also
recommend the certification status for all analyses
evaluated. The report should then be forwarded for
evaluation to the Regional Director of the
Environmental Services Division and the Regional
Director of the Water Division. After considering the
report, they should transmit it to the Regional
Administrator for action.
The Regional Administrator should decide the
certification status of the laboratory within 30 days
and notify the State. The State should be sent the
complete report. If the report indicates that the
laboratory not be given Certified status for an
analysis, the Regional Administrator shall give the
specific reasons.
The narrative report should be attached to each copy
of the completed evaluation form. It should include
the general headings and information listed below.
Title Page
The title page should contain the following:
Title: Report of an on-site evaluation of the
(name of laboratory)
At: (city, State, and zip code)
On: (date)
By: (name, title, organization, and
address of the certification team)
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Certification Status
List either Certified, "Provisionally Certified," or Not
Certified for each contaminant evaluated.
List of Deviations
List each deviation by item number used on the
evaluation checklists. Describe the exact deviation
and recommended changes.
Remarks
Recommend improvements which, while not affecting
certification status, would improve laboratory
operation. Other remarks might include reasons for
failing the on-site evaluation, special recognition for
outstanding performance, and description of unusual
tests.
List of Personnel
List name and title of personnel along with the
individual tests that each normally performs. Also
identify the critical laboratory personnel.
Signature
Team members should sign the report.
Distribution
Copies of this report should be distributed to the
State requesting the evaluation and EMSL-CI or
EMSL-LV. For local laboratories in non-primacy
States, reports should be distributed to appropriate
Regional personnel.
Annually, each Region should submit to ODW a brief
listing of laboratories in the Region having U.S. EPA
or State certification status. The listing should include
the names and location of each laboratory, and its
certification status for all regulated contaminants. In
addition, Regions should notify ODW of all changes in
status soon after they occur so that ODW can
maintain an updated list of certification status.
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Appendix C
Abbreviations
CA—Certifying authority. Regional Administrator for
principal State laboratories and laboratories in non-
primacy States; EMSL-CI and EMSL-LV Regional
laboratories.
CFR—Code of Federal Regulations.
EMSL-CI - Environmental Monitoring Systems
Laboratory in Cincinnati, Ohio (ORD).
EMSL-LV—Environmental Monitoring Systems
Laboratory in Las Vegas, Nevada (ORD).
DWLC—Drinking Water Laboratory Certification Work
Group.
NPDWR—National Primary Drinking Water
Regulations.
ODW-Office of Drinking Water.
ORD—Office of Research and Development.
PE—Performance evaluation.
RREL—Risk Reduction Engineering Laboratory
(ORD)
QA—Quality assurance
QAMS—Quality Assurance Management Staff (ORD)
QC—Quality control
83
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Appendix D
UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
WASHINGTON. D.C. 20460
5
MEMORANDUM
SUBJECT: Third-Party Certification for Laboratories
in Primacy States
i\\
FROM : Michael B. Cook, Directory
Office of Drinking Water
TO : Water Supply Representatives, Regions I-X
Environmental Services Division Directors, Regions I-X
Quality Assurance Officers, Regions I-X
This memorandum reissues and slightly modifies Water Supply
Guidance VII-5, dealing with third-party certification for
laboratories in primacy States. This memorandum should be
retained as Water Supply Guidance VII-5A. No fundamental
difference exists between the two versions; VII-5A merely
clarifies the State's continuing responsibilities.
Under 40 CFR 142.10(b)(3), if a State does not perform all
analytical measurements in its own laboratory, it must establish
and maintain a program for the certification of laboratories as a
condition of receiving and maintaining primary enforcement
authority (primacy). This memorandum notifies States with
primacy that they may contract with other organizations (third
parties) to assist in certifying laboratories for drinking water
analyses.
Several States have asked USEPA its position on third-party
certification agents, i.e., private sector organizations which
wish to operate the certification program for local laboratories
in primacy States.
ODW endorses the third-party concept. This Office will not,
however, pass judgment on any specific third-party program. It
is the responsibility of each primacy State to assess the
qualifications of the third-party and the adequacy of its
program. The State must also retain the responsibility for
overseeing the laboratory certification program. In assessing
whether to choose a particular third-party, the State must
85
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consider, as a minimum, the following features, some of which are
outlined in the Manual for the Certification of Laboratories
Analyzing Drinking Water;
o technical criteria for chemistry, microbiology, and/or
radiochemistry
o use and quality of performance evaluation samples
(unknown) and quality control samples (known)
o frequency of on-site evaluations
o evaluator capability
o willingness to provide technical assistance
o availability of records for review by State
o adequacy of quality assurance program
o criteria for downgrading/revoking certification
It is essential that any third-party program be equivalent
to any previous program operated by the State and approved by
EPA. As stated previously, States employing a third-party to
assist in certification must retain ultimate authority to decide
whether individual laboratories will be certified; this decision
may not be delegated to the third-party.,
The Regions should assist the State and third-party agent to
assure the program is sound. This could include reviewing the
program, helping the State obtain reference samples, and
providing technical assistance. In addition, Regions and States
should be sensitive to potential conflict-of-interest problems
between a third-party inspector and evaluated laboratories. For
instance, inspectors employed by firms that provide analytical
services in the drinking water area should not be put in the
position of passing judgement on their competitors.
86
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Appendix E
Required Analytical Capability for Principal State Laboratory Systems
(As of June 1, 1979)
Volatile Organic Chemicals (40 CFR
141.24)
Trihalomethanes
Chloroform
Bromodichloromethane
Dibromochloromethane
Bromoform
Benzene
Carbon tetrachloride
1,2-Dichloroethane
1,1 -Dichloroethylene
p-Dichlorobenzene
1,1,1 -Trichloroethane
Vinyl chloride
Trichloroethylene
Organics other than VOCs (40 CFR
141.24)
Endrin Toxaphene
Lindane 2,4-D
Methoxychlor 2,4,5-TP
Inorganics (40 CFR 141.23)
Arsenic Mercury
Barium Nitrate-N
Cadmium Selenium
Chromium Silver
Fluoride
Lead
Radionuclides (40
Gross alpha
Gross beta
Radium 226
Radium 228
Tritium
Strontium 89
Strontium 90
Uranium
CFR 141.25)
Gamma radiation
Cesium 134
Cesium 137
Chromium 51
Cobalt 60
Iodine 131
Ruthenium 106
Zinc 65
Microorganisms (40 CFR 141.21)
Total cohforms
1 If principal State laboratories or other laboratprjes
analyze compliance samples for sodium, turbidity,
or §1445 chemicals, they must be certified for these
contaminants.
87
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Appendix F
Additional Contaminants Scheduled for Future Rules
(Rest of the 83 Not in Appendix E)
Volatile Organic Chemicals
o-Dichlorobenzene
cis-1,2-Dichloroethylene
trans-1,2-Dichloroethylene
1,2-Dichloropropane
Ethylbenzene
Methylene chloride
Monochlorobenzene
Tetrachloroethylene
Toluene
1,2,4-Trichlorobenzene
1,1,2-Trichloroethane
Xylenes (total)
Inorganics
Antimony Nickel
Asbestos Nitrite-N
Beryllium Sulfate
Copper Thallium
Cyanide
Radionuclides
Radon
Microorganisms (revised rules effective
December 31, 1990)
Escherichia coli (not part of list of 83)
Fecal coliforms (not part of list of 83)
Giardia (no monitoring required under revised rules)
Heterotrophic bacteria (SPC or HPC)
Legionella (no monitoring required under revised
rules)
Viruses (no monitoring required under revised rules)
Organics (other than VOCs)
Adipates (diethylhexyl)
Alachlor
Aldicarb
Aldicarb sulfoxide
Aldicarb sulfone
Aldrin
Atrazine
Acrylamide
Butachlor
Carbaryl
Carbofuran
Chlordane
Dalapon
1,2-Dibromo-3-chloropropane (DBCP)
2,4-DB
Dicamba
1,2-Dichoropropane
Dieldrin
Dinoseb
Diquat
Endothall
Ethylene dibromide (EDB)
Epichlorohydrin
Glyphosate
Heptachlor
Heptachlor epoxide
Hexachlorobenzene
Hexachlorocyclopentadiene
3-Hydroxycarbofuran
Methomyl
Metribuzin
Oxamyl (vydate)
PAHs (benzo(a)pyrene)
PCBs (decachlorobiphenyl)
Pentachlorophenol
Picloram
Phthalates (diethylhexyl)
Styrene
Simazine
2,4,5-T (silvex)
2,3,7,8-TCDD (dioxm)
89
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Appendix G
§1445 Unregulated Chemicals to be Monitored (Final or Proposed)
40 CFR 141.40 (final rule published July
8, 1987)
Bromobenzene
Bromodichloromethane
Bromoform
Bromomethane
Chlorobenzene
Chlorodibromomethane
Chloroethane
Chloroform
Chloromethane
o-Chlorotoluene
p-Chlorotoluene
1,2-Dibro-3-chloropropane (DBCP)
Dibromomethane
m-Dichlorobenzene
o-Dichlorobenzene
1,1-Dichloroethane
cis-1,2-Dichloroethylene
trans-1,2-Dichloroethylene
Dichloromethane
1,2-Dichloropropane
1,3-Dichloropropane
2,2-Dichloropropane
1,1-Dichloropropene
1,3-Dichloropropene (cis and trans)
Ethylbenzene
Ethylene dibromide (EDB)
Styrene
1,1,2,2-Tetrachloroethane
1,1,1,2-Tetrachloroethane
Tetrachloroethylene
Toluene
1,1,2-Tnchloroethane
1,2,3-Trichloropropane
m-Xylene
o-Xylene
p-Xylene
40 CFR 141.40 (proposed May 22, 1989)
Monitoring is required for the following contaminants if
the State determines the system is vulnerable to
contamination.
Synthetic Organics
Metribuzin
Hexachlorobenzene
Dalapon
Dinoseb
Picloram
Oxamyl (vydate)
Simazine
Glyphosate
Hexachlorocyclopentadiene
PAHs
Phthalates
2,3,7,8-TCDD (Dioxin)
Inorganics
Antimony
Beryllium
Cyanide
Nickel
Aldrm
Dieldrm
2,4-DB
Dicamba
2,4,5-T (silvex)
Carbaryl
3-Hydroxycarbofuran
Methomyl
Butachlor
Metolachlor
Propachlor
Sulfate
Thallium
Monitoring for the following contaminants is at the
discretion of the State.
Ametryn
Aspon
Atraton
Azinphos methyl
Bolstar
Bromacil
Butylate
Carboxin
Chloropropham
Coumophos
Cycloate
Demeton-O
Demeton-S
Diazinon
Dichlofenthion
Dichlorvos
Diphenamid
Ethion
Ethoprop
Ethyl parathion
Famphur
Fenamiphos
Fenarimol
Fenitrothion
Fensulfothion
Fenthion
Fluridone
Fonofos
Hexazinone
Malathion
Merphos
Methyl paraoxon
Methyl parathion
Mevinphos
91
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Disulfoton
Disulfoton sulfone
Disulfoton sulfoxide
EPN
EPTC
Pebulate
Phorate
Phosmet
Prometon
Prometryn
Pronamide
Propazine
Simetryn
Stirofos
Tebuthiuron
Terbacil
Terbufos
Terbutryn
Triademefon
Tricyclazole
Vernolate
Chlorneb
Chlorobenzilate
Chloropropylate
Chlorothalonil
MGK 264
MGK 326
Molinate
Napropamide
Norflurazon
Chlorpyrifos
DCPA
4,4'-DDD
4,4'-DDE
4,4'-DDT
Dichloran
Endosulfan I
Endosulfan II
Endosulfan sulfate
Endrin aldehyde
Etridiazole
BCH-alpha
BCH-beta
BCH-delta
BCH-gamma
cis-Permethrin
trans-Permethrin
Trifluralin
Diquat
Endothall
92
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TECHNICAL RFPORT DATA
(Please read Instructions on the reverse before completing/
1. REPORT NO.
EPA 570/9-90/008
2.
3. RECIPIENT'S ACCESSION NO.
4. TITLE AND SUBTITLE
Manual for the Certification of Laboratories
Analyzing Drinking Water
5. REPORT DATE
April 1990
6. PERFORMING ORGANIZATION CODE
7. AUTHOR(S)
8. PERFORMING ORGANIZATION REPORT NO
9. PERFORMING ORGANIZATION NAME AND ADDRESS
Office of Drinking Water (WH-550D)
US EPA
401 M Street, SW
Washington, DC 20460
10. PROGRAM ELEMENT NO.
11. CONTRACT/GRANT NO
12. SPONSORING AGENCY NAME AND ADDRESS
Same as #9
13. TYPE OF REPORT AND PERIOD COVERED
14. SPONSORING AGENCY CODE
15. SUPPLEMENTARY NOTES
16. ABSTRACT
This manual describes the operational and technical criteria and
-rocedures EPA will use to evaluate a laboratory for its ability to
properly analyze a regulated microbiological, chemical, or
radiochemical drinking water contaminant. The certification program
described in this manual extends to the EPA Regional laboratories,
principal State laboratories in States which have primary enforcement
responsibility (primacy), and to all laboratories that perform analyses
under the SDWA in the few States without primacy. The vast majority
of primacy States have thir own laboratory certification programs.
Although many of them use the EPA's program as presented in this manual,
individual State programs should be contacted to insure equivalency
with State requirements.
This document is the third edition of the manual, and supersedes
EPA 570/9-82-002, of the same title, which was issued in 1982.
17.
KEY WORDS AND DOCUMENT ANALYSIS
DESCRIPTORS
b.lDENTIFIERS/OPEN ENDED TERMS C. COSATI Field/Group
Laboratory
Certification
Safe Drinking Water Act (SDWA)
Water Supply
Drinking Water
Quality Assurance
Sanitary Microbiolo^
Chemistry
Radiochemistry
y
18. DISTRIBUTION STATEMENT
Release to Public
19. SECURITY CLASS (This Report)
Unclassified
21 NO. OF PAGES
88
20. SECURITY CLASS (This page)
Unclassified
22. PRICE
EPA Form 2220-1 (Rev. 4-77) PREVIOUS EDITION is OBSOLETE
'-U S GOVERNMENT PRINTING OFFICE'1990-717-003/28006
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