vvEPA
United States
Environmental Protection
Agency
Office of Monitoring
and Technical Support
Washington DC 20460
EPA 600/8-78-008
May 1978
Research and Development
Manual for the 6oo878oos
Interim Certification
of Laboratories Involved
in Analyzing
Public Drinking Water
Supplies
Criteria and Procedures
-------
EPA, Publication 600/8-78-008
Manual for the Interim Certification of Laboratories Involved in
Analyzing Public Drinking Water Supplies
ERRATA
(June 1978)
Page 6
FEDERAL FACILITIES
Federal Facilities must comply with all Federal, State and local re-
quirements with respect to the Safe Drinking Water Act. For the purposes
of certification, Federal laboratories which conduct routine monitoring of
public drinking water supplies are to be considered Local Laboratories and
will be certifiable under a State program. The agency with primary enforce-
ment authority, either the State or the Region acting as the surrogate State,
will also be responsible for carrying out the interim certification guidance
contained in this manual and will conduct on-site evaluations of the Federal
facilities. EPA, however will have primary enforcement authority over any
facilities on Indian lands.
Principal Federal Laboratories
While it is the responsibility of States to certify all Federal labora-
tories which analze large numbers of drinking water samples for compliance
purposes, the EPA Region in which the Principal Federal Laboratory is phys-
ically located will conduct on-site evaluations if requested by a State with
primary enforcement responsibility. Requests for this technical assistance
should be made by the States to the appropriate Regional Administrator. EPA
believes that this service may be of benefit to States that do not wish to
certify Federal laboratories.
NOTE:
The Office of Water Supply has been renamed the Office of Drinking Water
-------
UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
WASHINGTON, D.C. 20460
JUL 1 3 1978
THE ADMINISTRATOR
To the Reader:
Section 1401(1) of the Safe Drinking Water Act, Public Law 93-523
defines "primary drinking water regulations" to include "quality control
and testing procedures" to ensure compliance with maximum contaminant
levels. Pursuant to the Act, the National Interim Primary Drinking Water
Regulations, 40 CFR 141 and 142 require that for compliance purposes
''samples" will be considered only if they have been analyzed by a
.laboratory approved by the State except^ that measurements offturbidity)and
(free chlorine residualjmay be performed by any person acceptable to the
State, and the States must maintain a program for certification of
laboratories conducting measurements of drinking water contaminants. This
Interim Certification Manual is intended to effectuate implementation of
those requirements.
This manual describes the Environmental Protection Agency (EPA) interim
water supply laboratory certification program and the technical criteria
which are considered essential to generate valid data. The technical
criteria should be considered as guides for the on-site evaluation; only
the methods and procedures in the Interim Primary Drinking Water
Regulations or otherwise approved by EPA should be considered as mandatory
Jfor interim Certific^ti"" nf fl laboratory. Once the Interim Certification
program has been thoroughly evaluated and subjected to public comment,
regulatibns covering certification may be developed along with the Revised
Primary Drinking Water Regulations.
While the manual is intended for EPA use in approving and certifying
laboratories in a uniform and impartial manner, EPA fully recognizes that
there are many excellent State laboratory certification programs in
-------
operation. This manual is not intended to regulate, impede, or degrade
existing or future State certification programs. States without
certification programs are encouraged to use this manual; States with
equivalent or better certification programs are encouraged to continue and
improve. The EPA welcomes any comments or suggestions which will improve
this manual.
-------
MANUAL FOR THE INTERIM CERTIFICATION OF
LABORATORIES INVOLVED IN ANALYZING
PUBLIC DRINKING WATER SUPPLIES
Criteria and Procedures
September 1977
Prepared by
THE WATER SUPPLY QUALITY ASSURANCE
WORK GROUP
THE U.S. ENVIRONMENTAL PROTECTION AGENCY
WASHINGTON, D.C. 20460
-------
DISCLAIMER
This manual has been reviewed by the Office of Monitoring and Technical Support and the
Office of Water Supply and approved for publication. The mention of commercial products does
not constitute endorsement by the U.S. Environmental Protection Agency.
-------
ACKNOWLEDGMENTS
This manual was prepared through the efforts of many individuals; representatives from me vari-
ous Environmental Protection Agency program offices and laboratories, Regional Offices, as well as
spokesmen for Government agencies and the States. The principal contributors are listed below:
WATER SUPPLY QUALITY ASSURANCE WORK GROUP
T. Stanley, Chairman, OMTS/MTD/ORD
R. Medz, Executive Secretary, OMTS/MTD/ORD
R. Booth, EMSL-CI/OMTS/ORD
R. Bordner, EMSL-CI/OMTS/ORD
L. Dorsey, MDSD/OWHM
E. Geldreich, MERL-CI/OALWU/ORD
C. Hendricks, OWS/OWHM
A. Jarvis, EMSL-LV/OMTS/ORD
R. Johnson, EAD/ORP/OAWM
T. Larsen, WQD/OGC/OA
P. Lawrence, OFA/OA
D. Lyons, ED/OWE/OE
E. McFarren, MERL-CI/OALWU/ORD
W. Oldaker, Region I
D. Olson, ED/OWE/OE
A. Tiedemann, Virginia
J. Winter, EMSL-CI/OMTS/ORD
OFFICIAL OBSERVERS
R. Brazis, FDA
A. Goldin, ORP
R. Hager, ORIO/OA
D. Shedroff, OE/OWE
J. Stevens, OFA
SUBCOMMITTEE FOR IMPLEMENTATION
C. Hendricks, Chairman, OWS/OWHM
L. Dorsery, MDSD/OWHM
T. Larsen, WQD/OGC/OA
D. Lyons, ED/OWE/OE
R. Medz, OMTS/MTD/ORD
A. Shannon, Michigan
D. Shedroff, OE/OWE
J. Stevens, OFA
D. Taylor, Region IV
A. Tiedemann, Virginia
iii
-------
SUBCOMMITTEE FOR CHEMISTRY
R. Booth, Chairman, EMSL-CI/OMTS/ORD
T. Bennett, Region IV
E. Glod, Ohio
E. McFarren, MERL-CI/OALWU/ORD
SUBCOMMITTEE FOR MICROBIOLOGY
E. Geldreich, Chairman, MERL-CI/OALWU/ORD
R. Bordner, EMSL-CI/OMTS/ORD
B. Carroll, Region IV
K. Whaley, Tennessee
J. Winter, EMSL-CI/OMTS/ORD
SUBCOMMITTEE FOR RADIOCHEMISTRY
A. Jarvis, Chairman, EMSL-LV/OMTS/ORD
D. Easterly, EMSL-LV/OMTS/ORD
H. Krieger, EMSL-CI/OMTS/ORD
G. Uyesugi, California
The Water Supply Quality Assurance Work Group gratefully acknowledges the assistance pro-
vided by States, local agencies, other Federal agencies, and many private laboratories who reviewed
and made suggestions for improving this manual.
IV
-------
CONTENTS
Acknowledgments iii
Abstract vii
Chapter I. Introduction k 1
Chapter II. Interim Certification Program 3
Certification in States With Primary Enforcement Responsibility 5
Certification in States Without Primary Enforcement Responsibility 5
Federal Facilities 6
Chapter III. Operational Guidance for EPA Regions 9
Responsibilities 9
Interim Certification of Regions 11
Interim Certification of Principal State Laboratories—Chemistry and Microbiology 12
Interim Certification of Radiochemistry Laboratories 13
EPA's Quality Assurance Program 14
Evaluation Report for Principal Laboratories 15
Chapter IV. Chemistry: Criteria and Procedures for Interim Certification of Laboratories
Involved in Analysis of Public Water Supplies 19
Personnel 19
Laboratory Facilities 20
Laboratory Equipment and Instrumentation Specifications 21
General Laboratory Practices 22
Methodology and Required Equipment 23
Sample Collecting, Handling, and Preservation 23
Quality Control 23
Data Reporting 26
Free Chlorine Residual and Turbidity 27
Action Response to Laboratory Results 28
Sample Forms for On-Site Evaluation of Laboratories Involved in Analysis of Public
Water Supplies 29
-------
Chapter V: Microbiology: Criteria and Procedures for Interim Certification of Laboratories
Involved in Analysis of Public Water Supplies 39
Personnel 39
Laboratory Facilities 40
Laboratory Equipment, Supplies, and Materials 41
General Laboratory Practices 43
Methodology 44
Sample Collection, Handling, and Preservation 45
Quality Control Program 46
Data Reporting 49
Action Response to Laboratory Results 49
Sample Forms for On-Site Evaluation of Laboratories Involved in Analysis of Public
Water Supplies-Microbiology 50
Chapter VI: Radiochemistry: Criteria and Procedures for Interim Certification of Laboratories
Involved in Analysis of Public Water Supplies 67
Personnel 67
Laboratory Facilities 68
Laboratory Equipment and Instrument Specifications 69
General Laboratory Practices 71
Radiochemistry 71
Quality Control 71
Data Reporting 73
Action Response to Laboratory Results 73
Sample Forms for On-Site Evaluation of Laboratories Involved in Analysis of Public
Water Supplies—Radioanalysis 74
Glossary 91
VI
-------
ABSTRACT
Section 1401(1) of the Safe Drinking Water Act (SDWA), Public Law 93-523, defines "primary
drinking water regulations" to include "quality control and testing procedures" to ensure compli-
ance with maximum contaminant levels. Pursuant to the Act, the National Interim Primary Drink-
ing Water Regulations (NIPDWR), 40 CFR 141 and 142 require that for compliance purposes,
"samples" will be considered only if they have been analyzed by a laboratory approved by the State
except that measurement for turbidity and free chlorine residual may be performed by any person
acceptable to the State, and the States must establish and maintain a program for certification of
laboratories conducting measurements of drinking water contaminants. This manual describes evalu-
ation procedures and minimum technical requirements recommended for certifying laboratories
analyzing public drinking water supplies. In addition to identifying requirements that are critical to
the generation of valid data, optional certification requirements have been included as guidance.
In formulating an implementation strategy, EPA fully recognizes that there are many excellent
State laboratory certification programs in operation. EPA is also aware that the capabilities of State
and local laboratories vary greatly, and that a phased implementation program may be necessary to
permit moving toward our goal without creating artificial impediments to the attainment of State
primacy. This manual describes how EPA will carry out a program for interim approval and certifica-
tion of its 10 Regional laboratories and principal State laboratories. States without certification pro-
grams are encouraged to use this program as a model; States with equivalent or better certification
programs are encouraged to continue and improve. EPA welcomes any comments or suggestions
that will improve this manual.
Vll
-------
-------
Chapter I
INTRODUCTION
As of June 24, 1977, all public water systems serving 25 persons or more must conform with
provisions of the Safe Drinking Water Act (P.L. 93-523) and requirements contained in the National
Interim Primary Drinking Water Regulations (40 CFR 141 and 142). In addition to prescribing max-
imum allowance levels and monitoring frequencies for various materials in drinking water, section
141.28 of the Interim Primary Regulations requires that all testing, except for turbidity and chlo-
rine residual, be performed by laboratories approved by either the U.S. Environmental Protection
Agency (EPA) or the States.
This manual is intended to assist in implementation of section 141.28 by providing a mechanism
for approval of laboratories to assure the validity and quality of the data being developed for com-
pliance with the regulations. The ultimate test of a laboratory is the validity and quality of its data.
However, it is also important that certain minimum technical needs be met to assure that the labora-
tory has the necessary facilities and capabilities to consistently produce data acceptable under the
terms of the regulations.
Formal certification of a laboratory under regulatory authority is the preferred approach of a
certification program. However, since the Interim Primary Regulations are already in effect, time
does not permit development of a regulatory approach to laboratory certification. Instead, a phased
approach has been selected. In the first phase, to provide acceptable data for immediate implementa-
tion of the Interim Primary Regulations, Interim Approval will be granted laboratories on an admin-
istrative basis. Later, after an on-site evaluation based on this manual or its equivalent, Interim
Certification will be granted. The major emphasis of this phase is to provide advice and technical
assistance to the laboratories so that they can meet the requirements of Certification.
EPA's certification program calls for on-site evaluation of Principal Laboratories every 3 years
and an annual performance evaluation of all laboratories analyzing public water supplies under the
Safe Drinking Water Act. The annual performance evaluation, which is the most critical part of the
certification program, involves providing water supply laboratories with unknown samples for analy-
sis. If the laboratory fails to perform acceptably on these sample's Jit r^py HP HP.^]^ Certification.
To renew the initial certification at the end of 3 years, a water supply laboratory must pass an-
other on-site evaluation, as well as a review of its quality control program and its annual laboratory
performance records.
EPA will consider developing revised regulations covering the certification of water laboratories
in the future. However, such regulations will not be adopted until the interim program has been
thoroughly reviewed and all elements of the program have been subjected to public comment.
The Office of Water Supply, EPA, which is responsible for implementation of drinking water
regulations, believes that the criteria contained in this manual are appropriate for evaluation of all
-------
water laboratories engaged in analyses relating to the Interim Primary Regulations. However, these
criteria in general should be considered as guides to the on-site evaluation; only the methods and
procedures in the Interim Primary Regulations or otherwise approved by EPA should be considered
as mandatory for Interim Certification of a laboratory.
Chapter II of this manual outlines the Interim Certification Program, while Chapter III de-
lineates responsibilities within EPA and describes how the program will be operated. The next three
chapters cover technical requirements for conducting on-site evaluations of chemical, microbio-
logical, and radiochemical laboratories. Various terms used in the manual are defined in the appen-
dix.
-------
Chapter II
INTERIM CERTIFICATION PROGRAM
Enforcement of the Safe Drinking Water Act and Interim Primary Regulations rests primarily
with the States. To receive primary enforcement responsibility, a State must meet provisions of 40
CFR 142 (see Table II-l). In States not receiving primary enforcement responsibility, called "non-
primacy States," the EPA Regional Office assumes the responsibility. Federal laboratories will be
certified by the agency with primary enforcement responsibility.
A State seeking primary enforcement responsibility must apply to EPA through its Regional
Office. In its application, a State must indicate that it meets the conditions for primacy including
Table 11-1 .—Definition of primary enforcement responsibility
According to 40 CFR 142.10(b) (3) and (4), a State has primary enforcement responsibility if it:
(b) Has adopted and is implementing
adequate procedures for the enforce-
ment of such State regulations, such pro-
cedures to include:
(3) The establishment and mainte-
nance of a State program for the cer-
tification of laboratories conducting
analytical measurements of drinking
water contaminants pursuant to the re-
quirements of the State primary drink-
ing water regulations including the
designation by the State of a laboratory
officer, or officers, certified by the Ad-
ministrator, 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 measure-
ments required by the State's primary
drinking water regulations are con-
ducted at laboratories operated by the
State and certified by the Agency. Until
such time as the Agency establishes a
National quality assurance program for
laboratory certification the State shall
maintain an interim program for the
purpose of approving those laboratories
from which the required analytical
measurements will be acceptable.
(4) Assurance of the availability to the
State of laboratory facilities certified by
the Administrator and capable of per-
forming analytical measurements of all
contaminants specified in the State pri-
mary drinking water regulations.
Until such time as the Agency estab-
lishes a National quality assurance pro-
gram for laboratory certification the
Administrator will approve such State
laboratories on an interim basis.
-------
the designation of a Principal State Laboratory (or laboratories) to be responsible for analysis of all
contaminants covered by the National Interim Primary Drinking Water Regulations.
In cases where the Principal State Laboratory must rely on another laboratory (called a Local
Laboratory) to perform some of the analyses, the State must develop a certification program for
Local Laboratories before primary enforcement responsibility can be granted.
EPA's Environmental Monitoring Support Laboratory in Cincinnati, Ohio (EMSL-CI), will ini-
tiate the national Interim Certification program for water supply laboratories by determining that
EPA's Regional Offices and their laboratories have the capability to carry out the chemistry and
microbiology portions of the program. Once this decision has been made, the Regions are ready to
perform the on-site evaluations required for certification of Principal State Laboratories. In non-
primacy States, the Regions will conduct the evaluations and grant certification to Local Labora-
tories. Since certification of a Principal State Laboratory may affect primary enforcement responsi-
bility, the State must be notified of any adverse action and given the opportunity for a hearing as
provided in 40 CFR 142, National Interim Primary Drinking Water Regulations—Implementation.
Since few if any EPA Regions have the expertise to certify radiochemistry laboratories, the
Environmental Monitoring and Support Laboratory in Las Vegas, Nev. (EMSL-LV), will assume the
same responsibilities that the Regions have for chemistry and microbiology.
The tentative schedule for laboratory certification is shown in Table II-2.
Table II -2.-Tentative schedule for certification of laboratories
Interim Approval Starting June 24,1977
EMSL-Cincinnati grants Interim Approval to Regional certification programs.
Regions grant primary enforcement responsibility to qualified States. In States not qualified, the responsibility
is assumed by the Regions.
States with primary enforcement responsibility grant Interim Approval to Local Laboratories.
Regions with primary enforcement responsibility grant Interim Approval to Local Laboratories.
Interim Certification by December 1978
EMSL-Cincinnati completes on-site evaluations and grants Interim Certification to Regional Laboratories.
Regions complete on-site evaluations of Principal State and Federal Laboratories using this manual.
States with primary enforcement responsibility begin to conduct on-site evaluations of Local Laboratories using
this manual or one prepared by a State.
Regions with primary enforcement responsibility begin to conduct on-site evaluations of Local Laboratories
using this manual.
Certification 1979-19801
All water supply laboratories are certified using this manual or one prepared by a State.
Estimated effective date of National Revised Primary Drinking Water Regulations.
-------
CERTIFICATION IN STATES WITH PRIMARY ENFORCEMENT RESPONSIBILITY
Present Federal regulations regarding laboratory certification in States seeking primary enforce-
ment responsibility (section 142.10(b) (3), (b) (4)) require that the States' laboratory facilities be
certified by EPA and be capable of analyzing all regulated contaminants in drinking water. These
regulations also require that a State with Local Laboratories appoint a laboratory officer(s), certi-
fied by EPA, as the official(s) responsible for the State's certification program. It is highly desirable
that one officer in each State be responsible for the program.
After a State has received primary enforcemeni responsibility, it must request an on-site evalua-
tion of its Principal Laboratory by writing to its EPA Regional Office. The letter should include the
following information:
• Name and location of each facility to be evaluated.
• Name, address, and telephone number of the supervisor, manager, or director for each facil-
ity to be evaluated.
• Specific analysis for which certification is requested.
• A recommended date, not less than 60 days after submission of the request, for the on-site
evaluation.
The on-site evaluation will be conducted in each analysis, and the criteria contained in this man-
ual will be used to determine if a laboratory qualifies for Interim Certification.
State Program for Certification of Local Laboratories
Local Laboratories covered by the State certification program may be any State, county, city,
Federal, utility, or commercial laboratory. Implementation of the State's certification program may
be accomplished on a phased basis with respect to time (Table H-2). However, at a time agreed to
by the Region and the State, but not later than December 1978, the State must begin to conduct
on-site evaluations of Local Laboratories. Certification must be based upon criteria contained in this
manual or State-developed equivalents that contain requirements at least as stringent as those used
in the evaluation of Principal State Laboratories. All laboratories must be certified by October
1980.
Reciprocity
EPA endorses reciprocity as a highly desirable element in the certification program for water
supply laboratories. As implementation of the Safe Drinking Water Act proceeds, EPA encourages
States to adopt provisions in their laws and regulations to permit interstate reciprocity.
CERTIFICATION IN STATES WITHOUT PRIMARY ENFORCEMENT RESPONSIBILITY
In keeping with the provisions of section 141.28, water supply laboratories in States without
primary enforcement responsibility will be certified on an interim basis by the Region. In addition
to its laboratory certification duties, the Region and its laboratory will have administrative, enforce-
-------
ment, and local laboratory certification responsibilities that would normally be performed by the
State. Some of these tasks may be redelegated to the State, but the Region must retain responsi-
bility for 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. Regions will determine if laboratories in a State without a certification program
qualify for certification to perform analyses for a nonprimacy State (the establishment of a fee
schedule is being considered for this type of certification). In any case, this manual shall provide the
basis for the on-site evaluation.
Local Laboratories
Regions will probably have awarded Interim Approval to laboratories having the capability to
analyze drinking water in conformance with the analytical methods cited in the Interim Primary
Regulations or otherwise approved by EPA. As soon as possible thereafter, the Region should begin
to certify the laboratories on an interim basis using this manual. The Regions should first award
Interim Approval to eligible Principal State and Local Laboratories and begin by December 1978 to
conduct on-site evaluations of laboratories. All laboratories must be certified by October 1980.
Reciprocity
Laboratories fully certified by EPA for specific analyses will be acceptable under the Safe
Drinking Water Act in all other jurisdictions where EPA has primary enforcement responsibility.
This de facto reciprocity does not apply to those States which accept primary enforcement respon-
sibility.
te •/***/ '*•***'
FEDERAL FACILITIES 5«2e
Where States have drinking water regulations^Trtually identical to the National Interim Primary
Drinking Water Regulations, States may have jurisdiction over Federal facilities with respect to the
Safe Drinking Water Act. EPA, however, expects to have primary enforcement authority over most
Federal and Indian facilities. For the purpose of laboratory certification, the agency with primary
enforcement authority will also b^-re'sponsible for carrying out the interim certification guidance
contained in this manual and-wlll conduct on-site evaluations of the laboratory facilities.
Principal Federal Laboratories ^ G e
Principal Federal Laboratories that analyze large numbers of drinking water samples from inter-
state water supplies will be evaluated on-site by the EPA Region where the laboratory is physically
located. EPA believes that good policy and reasonable regulatory procedure dictates that samples
analyzed by any Federal laboratory approved by EPA using this manual should be acceptable to •
State certification programs under the Safe Drinking Water Act.
-------
Local Federal Laboratories
Local Federal Laboratories are approved and certified on an interim basis by either the State or
EPA, whichever has primary enforcement responsibility.
-------
-------
Chapter III
OPERATIONAL GUIDANCE FOR EPA REGIONS
This chapter is primarily directed to the 10 EPA Regions and is intended to describe how EPA
will manage its interim certification program for water supply laboratories. A State with Local
Laboratories must maintain a certification program to receive primary enforcement responsibility.
States without certification programs may use this guidance as a model; States are encouraged to
continue to improve current programs that are equivalent to or better than what is described in this
chapter. However, EPA does not anticipate that all State certification programs will be identical to
the one described here.
RESPONSIBILITIES
The success of the laboratory certification program depends on genuine cooperation among the
organizations responsible for implementing the intent of the program and for establishing the proce-
dures and guidelines that will be followed. Within EPA, primary responsibilities for laboratory
certification are shared by the Office of Water Supply (OWS), the Office of Monitoring and Techni-
cal Support (OMTS), and the EPA Regional Offices.
Office of Water Supply (OWS)
OWS is responsible for management of the national certification program for public drinking
water systems and for implementation of the Safe Drinking Water Act, including preparation of
regulations and standards.
Office of Monitoring and Technical Support (OMTS)
OMTS is responsible for developing and implementing an EPA-wide quality assurance program,
including laboratory certification. Actual development and operation of the quality assurance effort
is conducted by the Environmental Monitoring and Support Laboratory in Cincinnati, Ohio (EMSL-
CI), and the one in Las Vegas, Nev. (EMSL-LV).
EMSL-CI has been designated as the national focal point for Interim Certification of water sup-
ply laboratories making chemical and microbiological measurements. It evaluates the resources and
personnel available in each EPA Region, then makes recommendations to the EPA Assistant Admin-
istrator, Office of Research and Development (ORD), on their ability to carry out the national pro-
gram. Should a Region not have the resources or personnel to certify laboratories in each technical
area, it must make arrangement with OMTS. Among tne duties of EMSL-CI are:
-------
• Approve Regional programs to certify Principal State Laboratories and conduct on-site
evaluation of Regional Laboratories at 3-year intervals.
• Conduct annual performance evaluations for all Principal State Laboratories and the Re-
gions. Other laboratories may participate as approved by the Regions/States.
• Review Regional certification program and laboratory performance records annually.
• Review the overall certification program annually.
• Maintain liaison with the Regional Water Supply Divisions regarding the technical assistance
they provide the States.
• Develop and participate in training courses to support the certification program.
• Provide technical assistance as required.
EMSL-CI will renew approval of the Region and its laboratory at 3-year intervals. Renewal crite-
ria include an annual program review, an annual review of laboratory performance records, and the
on-site evaluation of the laboratory conducted every 3 years.
EMSL-LV has been designated as the national focal point for Interim Certification of water
supply laboratories making radiochemical measurements. Its duties correspond with those described
for EMSL-CI. EMSL-LV will assume responsibility for both on-site inspections and performance
evaluations for radiochemistry capabilities of all Principal State Laboratories and other laboratories
not covered by State programs provided resources are available.
EPA Regional Offices
EPA's 10 Regional Offices have primary responsibility for implementing the water supply certi-
fication program. This responsibility includes review, approval, and overview of State laboratories
and certification programs to assure compliance with conditions for assumption of primary enforce-
ment responsibility. Also, the Regions will be responsible for on-site evaluation and certification of
Principal State Laboratories; however, Regional evaluation teams must be certified by OMTS prior
to conducting evaluations. Specific duties of the Regions include:
• Approve State programs to certify local laboratories.
• Conduct on-site evaluations of Principal State Laboratories.
• Coordinate performance evaluations for all laboratories in the Region.
• Participate in the annual review of State certification programs and performance evaluation
reports.
• Provide technical assistance to water supply laboratories that need to be upgraded.
• Operate certification program in nonprimacy States, including Interim Approval and Certifi-
cation of Federal laboratories.
EMSL-LV will renew certification of Principal State Laboratories at 3-year intervals. Renewal
criteria include annual performance records and an on-site evaluation conducted during the year
of renewal.
Water Supply Advisory Committee for Laboratory Certification
An advisory committee will be established to oversee operation of the national certification
program. This committee should include representatives from the Office of Water Supply, Office
of Monitoring and Technical Support. Office of Radiation Programs, Office of Enforcement,
10
-------
Environmental Monitoring and Support Laboratories, Water Supply Research Laboratory, Regional
Offices, and States. This committee will review and advise on program operation, revise and resolve
technical and administrative problems, and revise evaluation and acceptance procedures as dictated
by experience or more current information.
INTERIM CERTIFICATION OF REGIONS
EPA Regions must be certified by EMSL-CI prior to exercising their authority to certify Princi-
pal State Laboratories and Local Laboratories in nonprimacy States. Certification of the Regions
will be based on the availability of a qualified individual to direct the laboratory certification pro-
gram, an on-site evaluation team, and a laboratory capability for conducting all of the analyses
required by the Interim Primary Regulations. In addition, the Regions are required to have a written
plan for certifying Local Laboratories in nonprimacy States. EMSL-CI must approve such labora-
tory certification plans. Certification requirements are discussed below.
Individuals) Responsible for Certification Program
A Regional coordinator of laboratory certification/quality assurance responsible for water sup-
ply must be designated. This individual must be experienced in quality assurance; hold an advanced
degree or have equivalent experience in microbiology, chemistry, or radiochemistry; and have suffi-
cient 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 designated to evaluate a laboratory in microbiology and chemistry.
Team members must be experienced professionals, qualified to certify a laboratory and holding at
le^st a bachelor's degree in the specific discipline. Team members must participate in a"training
course in the proper use of procedures and criteria "for evaluating and certifying laboratories.
Courses include formal lectures on the criteria document, a mock laboratory evaluation, preparation
of an evaluation report, and the participant's recommendations as to certification status for the
mock laboratory evaluated. The performances of the course participants will determine their eligi-
bility for certification.
A representative from the Regional Water Supply Division should be appointed to the evalua-
tion team to evaluate activities outside the direct control of the laboratory that impact the validity
of its data. However, those activities cannot be used for certification purposes.
Only chemists and microbiologists are planned for certification at this time.
Regional Laboratories
Regional Laboratories that may be required to analyze potable water samples under the Safe
Drinking Water Act must meet the minimum requirements in this current manual, pass an on-site
inspection at least once every 3 years, and pass an annual evaluation of performance.
11
-------
Regional Plans for Certification of Local Laboratories
Regions must develop plans for Interim Approval and Interim Certification of Local Labora-
tories and Federal Laboratories in nonprimacy States, as appropriate. Written plans should include
the following:
• Certification official
• Types and numbers of laboratories (identify radiochemical laboratories and provide ad-
dresses)
• Analyses to be covered, including turbidity and, if allowed, chlorine residual
• Schedule for Interim Approvals and on-site evaluations
• Plans for providing technical assistance to laboratories in need of upgrading
EMSL-LV will be responsible for both on-site inspections and performance evaluations of radio-
chemistry laboratories. All plans for Interim Approval and Certification of radiochemistry labora-
tories must be coordinated with EMSL-LV.
INTERIM CERTIFICATION OF PRINCIPAL STATE LABORATORIES-CHEMISTRY AND
MICROBIOLOGY
Interim Certification of Principal State laboratories starts when the State makes a formal request
to the Region stating the type of analysis to be evaluated. The Principal State Laboratory and its
Local Laboratories must have the capability of performing all analyses; however, an individual labo-
ratory which is a part of a principal State laboratory may be certified for only one, several, or all of
the analyses included in the Interim Primary Regulations. A request for certification of a laboratory
for which the Region has jurisdiction should come from the laboratory director. The Region should
respond within 30 days, and a mutually agreeable date and time should be set for laboratory evalua-
tion.
Before conducting the on-site evaluation, the Region shall:
^ Hold a pre-evaluation conference with appropriate laboratory and field activity representa-
tives 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 shall:
Evaluate the procedures and equipment used for those specific analyses for which the labora-
tory has requested certification.
Review the records and written standard procedures for compliance with the required sam-
pling frequency; check sampling program, sample transit time, and resample notices, if ap-
propriate.
Evaluate the Principal Laboratory's quality control program to determine:
—Does the laboratory have a quality control program in effect?
12
-------
\ —Do quality control data show that this program is being implemented?
\ —Do the data show that the laboratory is producing valid results?
>« • Examine and document general procedures including the following items:
—Sampling location guidance
—Sampling procedures
—Sample identification
—Prompt transport of sample to laboratory
—Sample frequency
—Follow-up of positive samples
—Dissemination of data
Note: This information should be obtained by the Water Supply Division's representative on
the team and be included in the narrative report that is forwarded to the State; however,
only those items in the above list for which the laboratory is directly responsible shall affect
certification.
• Complete the on-site evaluation form during the visit.
\ • Review the results of the evaluation with the director of the laboratory, the director of field
activities, and appropriate staff members. The review should:
\
—Discuss deviations in the observed procedures and records.
—Recommend procedural changes in equipment and supply needs, staffing requirements,
and facility improvements, as necessary.
Conclude with a discussion of how the Region can aid the laboratory.
After the on-site visit, the Region can take one of three actions for each analysis involved:
• Certified (interim)—a laboratory that meets the minimum requirements as determined by
the evaluation team using this manual. The certification shall be for 3 years.
• Provisionally certified (interim)—a laboratory that has been given a grace period of up to 1
year to correct deficiencies. In no case should provisional certification be given if the evalu-
ation team believes that the laboratory lacks the capability of performing the analysis.
Laboratories placed in this category must be reevaluated unless they can document in some
other way that the deficiency has been corrected.
• Not certified—a laboratory that does not meet the minimum requirements as determined by
the evaluation team using this manual. A laboratory in this category may appeal to the Re-
gional Administrator by requesting reevaluation by another Regional team or by a team
from another EPA laboratory. Should the reevaluation confirm the "not certified" classifi-
cation, the laboratory must correct the major deficiencies noted and then request reevalua-
tion, or the State can request that another laboratory be evaluated to perform the analysis.
INTERIM CERTIFICATION OF RADIOCHEMISTRY LABORATORIES
Since few if any Regions have the expertise required to certify radiochemistry, EMSL-LV will
assume primary responsibility for both performance evaluation and on-site inspection of radio-
13
-------
chemistry capabilities of Principal Laboratories. When the Region has established plans for on-site
evaluation of State laboratories, it should request an evaluator from the Director, EMSL-LV. Since
manpower resources are limited, the request should be submitted at least 1 month prior to the sched-
uled visit(s). Whenever possible, several tentative dates should be submitted, and several visits sched-
uled within the same time period. If necessary, the radiochemists will carry out their part of the
evaluation independent of the Regional team. In scheduling on-site visits, every effort will be made
to assist and give priority to those Regions with special problems.
If a State, or a Region acting on behalf of a State, is using or plans to use a private laboratory
for all or part of the radioanalysis required by the National Interim Primary Drinking Water Regula-
tions, an on-site evaluation of the private laboratory is necessary. To facilitate visits to a private
laboratory, a written agreement, granting permission to carry out an on-site evaluation, should exist
between the State (or Region) and the laboratory to be evaluated.
All of the State laboratories involved should be urged to participate in all EMSL-LV perform-
ance studies involving analysis of all radionuclides in water for which they wish to be certified.
The procedures used for on-site evaluation of radiochemistry laboratories generally will be the
same as used for chemistry and microbiology. All laboratories will be encouraged to participate in
EPA's quality assurance program.
EPA'S QUALITY ASSURANCE PROGRAM
Documenting the ability of a laboratory to consistently produce valid data is me primary goal
of the certification effort. Quality assurance is the backbone of the entire program. EPA will pro-
vide two types of samples to Regional and Principal Laboratories. Until EPA provides these samples,
Interim Certification will be based on the results of the on-site evaluation and the laboratory's inter-
nal quality control program.
Calibrated Reference Materials and Quality Control Samples
Known-value quality control samples for microbiology and chemistry will be developed and fur-
nished by EMSL-CI directly to Regions and through the Regions to state and local laboratories.
Calibrated radioactive samples will be provided by EMSL-LV. The known-value samples are to be
used by the laboratories as independent checks on reagents, instruments, or techniques; for training
analysts; or for comparative analysis within the laboratory. However, these samples are not intended
to replace routine check samples or standards run as part of an internal quality control program. Al-
though no certification or other formal evaluation function directly results from the use of these
samples, their routine use will provide evidence that an acceptable laboratory quality control program
is in operation. Requests for samples should be made through the appropriate EPA Regional Office.
Performance Evaluation Samples
Appropriate performance evaluation samples will be furnished to all Principal Laboratories as
part of the Interim Certification program. Unacceptable performance will serve as a basis for deny-
ing the laboratory certification. In such cases, however, appropriate technical assistance, as well as
14
-------
additional performance samples, will be provided to the laboratory. Reexamination may be required
if key analysts leave a particular laboratory during the 3-year certification period.
EVALUATION REPORT FOR PRINCIPAL LABORATORIES
A formal narrative report and action memorandum shall be prepared for the Regional Admin-
istrator. This report should contain all information pertinent to the evaluation and also recommend
the analyses for which Interim Certification can be awarded. The report should then be forwarded
for evaluation to the Regional director of laboratory certification/quality assurance and the Re-
gional director of the Water Supply Division. After considering the report, they should transmit it
to the Regional Administrator for his action.
The Regional Administrator should advise the State within 30 days if the laboratory is certified
and forward the complete report to the State. If the report recommends that the laboratory not be
certified for an analysis, the Regional Administrator should give the specific reasons. The State may
appeal to the Region. At that time the Region should arrange for a reevaluation of the laboratory
by another Regional team or a team from another EPA laboratory. A decision should be forwarded
to the Regional Administrator within one month. In the meantime, the Principal Laboratory may
continue to operate on a provisional status. Should the reevaluation support the Regional Admin-
istrator's decision, the data produced by the laboratory will be considered invalid until the labora-
tory has achieved Interim Certification.
The narrative report should be prepared and 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:
Report of an on-site evaluation of the
(name of laboratory)
at (street address)
(city, State, and zip code)
on (date)
by
(name, title, organization,
and address
of the certification team)
15
-------
Introduction
The introduction might read:
The equipment and procedures employed in the bacteriological, chemical, and radiochemical analyses of water
by this laboratory conformed with provisions of the Manual for Interim Certification of Water Supply Labora-
tories, except for the items indicated.
List of Deviations
List each deviation by item number used on the evaluation form; describe exact deviation; rec-
ommend procedural change for compliance with standard procedure.
Remarks
Include comments on procedures, description of unusual tests, or other remarks. If there are no
remarks, delete heading.
Commendation
List any items or persons deserving special commendation. Reserve such commendation for
outstanding performance. If no commendation is appropriate, delete the heading.
List of Personnel
List name and title of personnel along with the individual tests that each normally performs.
Conclusions
Give descriptive conclusion, including recommendation for approval or rejection of results of
the laboratory. Except in unusual circumstances, one of the three conclusions below should apply
to any laboratory.
• Conclusion A—unqualified acceptance; Interim Certification is recommended. Example:
The procedures and equipment in use at the time of this evaluation were in complete compliance with
provisions of the manual for Interim Certification of Water Supply Laboratories. We recommend that the
analytical data be accepted for the following analysis of waters under the Safe Drinking Water Act. (List.)
• Conclusion B—qualified acceptance; provisional certification is recommended if the team
believes that the deviations do not seriously affect the validity of results and that they will
be corrected immediately. This conclusion can be made more restrictive, when necessary, by
the words "pending correction of deviations" or other appropriate wording. Example:
16
-------
The procedures and equipment in use at the time of the evaluation complied in general with the provisions
of the Manual for Interim Certification of Water Supply Laboratories. When the deviations listed are cor-
rected, we recommend that the results be accepted for the following analyses of waters under the Safe
Drinking Water Act. (List.) We suggest that after the listed deviations have been corrected, this laboratory
request another evaluation, or otherwise document their correction.
• Conclusion C—due to the lack of equipment or use of inappropriate techniques, or other
causes, laboratory results are unacceptable. Example:
The procedures and equipment in use at the time of this evaluation showed unacceptable deviations from
the Manual for Interim Certification of Water Supply Laboratories. We recommend that analytical data
from this laboratory not be accepted for the following analysis of waters under the Safe Drinking Water
Act. (List.) We suggest that this laboratory request another evaluation after the listed deviations have been
corrected.
Laboratory Certification
List either certified (interim), provisionally certified (interim), or not certified for each techni-
cal area of analysis performed. The evaluation team must sign the report.
Distribution
Copies of this report should be distributed to the State requesting the evaluation, EMSL-
Cincinnati, and the Office of Water Supply.
17
-------
-------
Chapter IV
CHEMISTRY: CRITERIA AND PROCEDURES FOR
INTERIM CERTIFICATION OF LABORATORIES INVOLVED IN
ANALYSIS OF PUBLIC WATER SUPPLIES
The criteria and procedures contained herein in bold are the minimum requirements considered
essential for laboratories seeking certification for chemical analysis of public water supplies. They
include methodology and required equipment, collecting, handling, and preserving samples, and
quality control. The other items, involving personnel, laboratory facilities, laboratory equipment
and instrumentation specifications, general laboratory practices, data reporting, and action response,
are optional.
Until National Revised Primary Drinking Water Regulations require mandatory certification of
water supply laboratories, all specifications will be considered as guidelines to be used by certifica-
tion officials. At that time, minimum requirements will be essential to certification of laboratories
involved in analysis of public water supplies.
A laboratory that exceeds these requirements is encouraged to maintain and improve its higher
standards for facilities, equipment, instrumentation, and quality control. Upgrading of personnel
should be an ongoing process involving training efforts to ensure continued production of reliable
data.
Minimum requirements are shown throughout in bold.
PERSONNEL1 (OPTIONAL REQUIREMENTS)
Analyst for Routine Tests fall chemical measurements other than organic chemicals)
Requirements for the routine test analyst position are:
• Academic training: Minimum of high school diploma or its equivalent (State certification or
licensing may be considered).
• Experience:2
—Minimum of 2 years of experience in inorganic measurements, including 6 months of on-
the-job training, under direct supervision of qualified analyst, in measurements being con-
sidered for certification.
1 Exceptions will be made for those persons employed by the laboratory and currently doing the required analy-
ses prior to promulgation of the interim regulations provided that within 2 years after June 24, 1977, they receive a
minimum of 2 weeks of additional training in water chemistry.
2 Each year of college-level training in related scientific fields or demonstrated equivalency shall be considered
equal to 1 year of work experience. Such a substitution should not exceed one-half of the required experience.
19
-------
—With no experience, 2 years of on-the-job training, under direct supervision of a qualified
analyst, in measurements being considered for certification.
Analyst for Organic Chemicals
Requirements for the organic chemicals analyst position are:
• Academic training: Minimum of high school diploma or its equivalent.
• Experience:l Minimum of 6 months of experience in measurement of chlorinated hydrocar-
bons and chlorophenoxys and 2 years of experience in gas chromatography.
• Supervision: Supervision by an analyst (also eligible to analyze for organic chemicals) who
has
—A professional degree or its equivalent, with 1 year of course work in organic chemistry.
— 1 year of experience in measurement of organic chemicals by gas chromatography.
Supervisor I Consultant"
Requirements for the supervisor/consultant are:
• Academic training: Minimum of bachelor's degree in chemistry or its equivalent.
• Experience: Minimum of 2 years of experience in measurements being considered for certifi-
cation.
Laboratory Director2
Requirements for the laboratory director are:
• Academic training: Minimum of bachelor's degree in chemistry or its equivalent.
• Experience: Minimum of 5 years of experience.
LABORATORY FACILITIES
Optional Requirement
Laboratory space should be adequate (150 to 200 ft2/person, regardless of test, is recommended).
It should contain approximately 15 linear ft of usable bench space and include the following:
Minimum Requirements
• Sink with hot and cold running water.
• Electricity.
Each year of college-level training in related scientific fields or demonstrated equivalency shall be considered
equal to 1 year of work experience. Such a substitution should not exceed one-half of the required experience.
These positions may not be necessary in smaller laboratories; however, a consultant should be available.
20
-------
• Source of distilled and/or deionized water (depending on parameters measured).
• Exhaust hood or equivalent for analysis of organic chemicals and trace metals.
LABORATORY EQUIPMENT AND INSTRUMENTATION SPECIFICATIONS
(MINIMUM REQUIREMENTS)
Only those instruments should be required that are needed to analyze for the substances for
which the laboratory is being certified, but those instruments should meet the following specifica-
tions. A laboratory doing all of the required analyses should have, or have access to, all of the fol-
lowing equipment with the minimum specifications cited.
• Analytical balance: Should provide sensitivity of at least 0.1 mg.
• Photometer (see Table IV-1 below for instrumentation for individual methods):
—Spectrophotometer: Usable wavelength range, 400 to 700 nm. Maximum spectral band-
width, no more than 20 nm. Wavelength accuracy, 0 ± 2.5 nm. Photometer should be
capable of using several sizes and shapes of absorption cells providing a sample path
length varying from approximately 1 to 5 cm.
—Filter photometer (abridged spectrophotometer): Capable of measuring radiant energy in
range of 400 to 700 nm. Relatively broad bands (10 to 75 nm) of this radiant energy are
isolated by use of filters at or near the maximum absorption of the colorimetric methods.
Photometer should be capable of using several sizes and shapes of absorption cells pro-
viding a sample path length varying from approximately 1 to 5 cm.
• Magnetic stirrer: Variable speed, 120 V, with Teflon-coated stirring bar.
• pHMeter: Accuracy, ± 0.05 units. Scale readability, ± 0.1 units. Laboratories purchasing a
new pH meter are strongly advised to purchase one capable of functioning with specific ion
electrodes (see following item). Unit may be line/bench or battery/portable operated.
• Specific ion meter: Readable and accurate to ± 5 mV. Unit may be line/bench or battery/
portable operated.
• Atomic absorption spectrophotometer: Single-channel, single- or double-beam instrument
having a grating monochromator, photomultiplier detector, adjustable slits, a wavelength
range of 190 to 800 nm, and provisions for interfacing with a strip chart recorder.
• Recorder for atomic absorption: Strip chart recorder having a chart width of 10 in or 25
cm, a full scale response time of 0.5 s or less, 10- or 100-mV input to match the instru-
ment, and variable chart speeds of 5 to 50 cm/min, or equivalent.
• Gas chromatograph (equipped with an electron-capture detector): A commercial or custom-
designed gas chromatograph with a column oven capable of isothermal temperature control
to at least 210° ± 0.2° C. System should be equipped with accurate needle-valve gas-flow
controls, accept 1/4-in glass columns with the option of direct on-column injection. System
must be demonstrated to be suitable for chlorinated hydrocarbon pesticides, with a mini-
mum of decomposition and loss of compounds of interest.
21
-------
Recorder for gas chromatograph: Strip chart recorder having a chart width of 10 in or 25
cm, a full scale response time of 1 s or less, 1-mV (-0.05 to 1.05) signal to match the instru-
ment, and variable chart speeds of 5 to 50 cm/min or equivalent.
Conductivity meter: Suitable for checking distilled water quality. Should be readable in
ohms or mhos, have a range of 2 to 2.5 million ohms or equivalent micromhos ± 1 percent,
and have a sensitivity of 0.33 percent or better. Unit may be line/bench or battery/portable
operated.
Drying oven: Gravity and mechanical convection units with selectable temperature control
from room temperature to 170° C or higher.
Desiccator: Glass or plastic models, depending on particular application.
Hotplate: Large or small units with selectable temperature controls for safe heating of labo-
ratory reagents.
Refrigerator: A standard kitchen type domestic refrigerator for storage of aqueous reagents
and samples. For storing organics and flammable materials, an "explosion-proof type of
refrigerator should be used. When refrigeration is not required, an explosion-proof cabinet
may be used.
Glass-ware: Should be of Pyrex or Kimax type glass, which is more resistant than regular soft
glass to damage by heat, chemicals, and abuse. All volumetric glassware should be marked
Class A, denoting that it meets Federal Specifications and need not be calibrated before use.
Stirred boiling water bath: For ambient temperature to 100°C (with gable lid).
GENERAL LABORATORY PRACTICES (OPTIONAL REQUIREMENTS)
The following constitute requirements for general laboratory practices:
• Prepackaged kit methods: All kit procedures, other than the DPD Colorimetric Test Kit, are
considered as alternative analytical techniques, and procedures described under section
141.27 of the National Interim Primary Drinking Water Regulations are to be followed.
• Calibration intervals for color wheels, sealed ampules, and other visual standards: Labora-
tories utilizing visual comparison devices should calibrate the standards incorporated into
such devices at least every 6 months. These calibrations should be documented. Directions
for preparing temporary and permanent type visual standards can be found in the appropri-
ate sections of "Standard Methods for the Examination of Water and Wastewater," 14th
edition, published in 1975 (or the latest edition published) by the American Public Health
Association. By comparing standards and plotting such a comparison on graph paper, a cor-
rection factor can be derived and applied to all future results obtained on the now calibrated
apparatus.
• Glassware preparation: All glassware should be washed in a warm detergent solution and
thoroughly rinsed first in tap water and then in distilled water. This cleaning procedure is
sufficient for most analytical needs, but the individual procedures should be referred to for
more elaborate precautions to be taken against contamination of glassware. It has been
found advantageous to maintain a separate set of glassware (suitably prepared) for the ni-
trate, mercury, and lead procedures due to the potentiality for contamination from^the
laboratory environment. All glassware used in organic chemical analyses should have a final
22
-------
rinse with nanograde acetone or its equivalent and should then be air dried in an area free of
organic contamination.
Distilled I deionized water: Water having resistivity values between 0.5 to 2.0 megohms (2.0
to 0.5 micromhos)/cm at 25°C is satisfactory. Megohms are related to micromhos in the
following manner:
= micromhos, —: — = megohms
megohms ' micromhos
Excellent quality water has resistivity values exceeding 1.0 megohms/cm (less than 1.0
micromhos/cm) at 25°C. High quality water meeting such specifications may be purchased
from commercial suppliers; laboratories should request a list of quality specifications for
any water purchased. Quality of distilled/deionized water is best maintained by sealing from
the atmosphere. Quality checks should be made at planned intervals and documented.
Chemicals I reagents: "Analytical reagent grade" (AR) chemicals should be used for most
analyses required of water treatment laboratories. Consult "Standard Methods for the
Examination of Water and Wastewater," 14th edition, part 102, pages 5-8, or the latest
edition of this reference, for more detailed information on reagent grades. Individual ana-
lytical procedures in "Standard Methods for the Examination of Water and Wastewater,"
and the EPA's "Methods for Chemical Analysis of Water and Wastes" often specify special
requirements for the reagents to be used.
Laboratory safety: While safety is not an aspect of laboratory certification, evaluators should
point out, on an informal basis, potential safety problems observed during an on-site visit.
METHODOLOGY AND REQUIRED EQUIPMENT (MINIMUM REQUIREMENTS)
Table IV-1 shows minimum equipment requirements, methodology, and references for individual
parameters. Equivalent equipment may be used. All other procedures are considered alternative
analytical techniques as described in 40 CFR 141. Application for the use of alternative methods
may require acceptable comparability data.
SAMPLE COLLECTING, HANDLING, AND PRESERVATION (MINIMUM REQUIREMENTS)
Table IV-2 shows requirements for container types, preservatives and holding times for
individual parameters.
QUALITY CONTROL
Minimum Requirements
The requirements that appear on pages 25-26 are minimum for quality control.
23
-------
Table IV-1.— Minimum requirements—Methodology and required equipment
Parameter
Methodology (unfiltered sample)
Reference
(page number)
Major equipment required (or its equivalent)
SM1
EPA-*
Arsenic3
Barium
Cadmium
Chromium
Lead
Mercury
Nitrate
2
Selenium
Silver
Fluoride
Chlorinated
hydrocarbons:
Endrin
Lindane
Methoxychlor
Toxaphene
Chlorophenoxys:
2,4-D
2,4,5-TP
Atomic absorption; gaseous hydride — 95-96
Atomic absorption 210-215 97-98
Atomic absorption; chelation-extraction 210-215 101-103
Atomic absorption; chelation-extraction 210-215 105-106
Atomic absorption; chelation-extraction 210-215 112-113
Flameless atomic absorption — 118-126
Brucine colorimetric 461-464 —
Cadium reduction - 201-206
Atomic absorption; gaseous hydride — 145
Atomic absorption 210-215 146
Electrode; distillation not required 172-174 65-67
Colorimetric with preliminary distillation 171-172 59-60
174-176
Gas chromatography —
Gas chromatography
Atomic absorption spectrophotometer with recorder
Atomic absorption spectrophotometer with recorder
Atomic absorption spectrophotometer with recorder
Atomic absorption spectrophotometer with recorder
Atomic absorption spectrophotometer with recorder
Atomic absorption spectrophotometer with recorder
or instrument designed specifically for measurement
of mercury
Spectrophotometer or filter photometer
Spectrophotometer
Atomic absorption spectrophotometer with recorder
Atomic absorption spectrophotometer with recorder
Ion-selective electrode and expanded scale
electrometer
Direct distillation apparatus and spectrophotometer
or filter photometer
Kuderna-Danish glassware, gas chromatograph equipped
with glass-lined injection port and electron-capture
detector, and recorder
Kuderna-Danish glassware, gas chromatograph equipped
with glass-lined injection port and electron-capture
detector, and recorder
1 "Standard Methods for the Examination of Water and Wastewater," 13th edition, American Public Health Association, 1971.
^"Methods for Chemical Analysis of Water and Wastes," U.S. Environmental Protection Agency, Office of Technology Transfer, Washington, D.C. 20460,1974.
^Complete method available in: Caldwell, J. S., Lishka, R. J., and McFarren, E. F., "Evaluation of a Low Cost Arsenic and Selenium Determination at Microgram Per Liter
Levels," J. Amer. Water Works Assoc., 65:731 (November 1973).
Methods available from U.S. Environmental Protection Agency, Environmental Monitoring and Support Laboratory, Environmental Research Center, Cincinnati, Ohio
45268.
-------
, 1
Table IV-2.—Sample collecting, handling, and preservation
Parameter
Arsenic
Barium
Cadmium
Chromium
Lead
Mercury
Nitrate
Selenium
Silver
Fluoride
Chlorinated
hydrocarbons
Chlorophenoxys
Preservative2
Cone HNO3 to pH<2
Cone HNO3 to phK2
Cone HNO3 to pH<2
Cone HNO3 to pH<2
Cone HNO3 to pH<2
Cone HNO3 to pH<2
Cone H2SO4 to pH<2
Cone HNO3 to pH<2
Cone HNO3 to pH<2
None
Refrigerate at 4° C
as soon as possible
after collection
Refrigerate at 4° C
as soon as possible
after collection
Container3
PorG
PorG
PorG
PorG
PorG
G
P
PorG
PorG
PorG
PorG
G with foil- or
Teflon-lined cap
G with foil- or
Teflon-lined cap
Maximum
holding
time
6 months
6 months
6 months
6 months
6 months
38 days
14 days
14 days
6 months
6 months
1 month
14 days5
7 days5
1lf a laboratory has no control over these factors, the laboratory director must reject any samples not meeting these criteria and
so notify the authority requesting the analyses.
2|f HNC>3 cannot be used because of shipping restrictions, sample 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 time of analysis,
sample container should be thoroughly rinsed with 1:1 HNO3; washings should be added to sample.
3p = Plastic, hard or soft; G - Glass, hard or soft.
4ln all cases, samples should be analyzed as soon after collection as possible.
Swell-stoppered and refrigerated extracts can be held up to 30 days.
• All quality control data must be available for inspection.
• Laboratory must analyze an unknown performance sample (when available) once per year
for parameters measured. Results must be within the control limits established by EPA for
each analysis for which the laboratory wishes to be certified. If problems arise, appropriate
technical assistance will be provided, and a followup performance sample should be ana-
lyzed.
25
-------
• Minimum daily quality control:
—After a standard reagent curve composed of a minimum of a reagent blank and three
standards has been prepared, subsequent standard curves must be verified by use of at least
a reagent blank and one standard at or near the MCL. Daily checks must be within ±10
percent of original curve.
—If 20 or more samples per day are analyzed, working standard curve must be verified by
running an additional standard at or near the MCL every 20 samples. Checks must be with-
in ± 10 percent of original curve.
Optional Requirements
The following quality control requirements are optional:
• Current service contract is in effect on all balances.
• Class S weights are available to make periodic checks on balances.
• Thermometer certified by the National Bureau of Standards (or one of equivalent accuracy)
is available to check thermometers in ovens, etc.
• Color standards or their equivalent are available to verify wavelength settings on spectro-
photometers.
• Chemicals are dated upon receipt of shipment and replaced as needed or before shelf life has
been exceeded.
• Criteria have been established for a laboratory analyzing supply samples other than its own:
—Laboratory should perform on a known reference sample (when available) once per quar-
ter for the parameters measured. The measured value should be within the control limits
established by EPA for each analysis for which the laboratory wishes to be certified.
—At least one duplicate sample should be run every 10 samples, or with each set of samples,
to verify precision of the method. Checks should be within the control limits established
by EPA for each analysis for which the laboratory wishes to be certified.
—Standard deviation should be calculated and documented for all measurements being con-
ducted.
—Quality control charts or a tabulation of mean and standard deviation should be used to
document validity of data on a daily basis.
DATA REPORTING (OPTIONAL REQUIREMENTS)
Records of chemical analyses sould be kept by the laboratory for not less than 1 year. Enforce-
ment data should be kept for 3 years. This includes all raw data, calculations, quality control data,
and reports.
Actual laboratory reports may be kept. However, data, with the exception of compliance check
samples as detailed in section 141.33(b) of the National Interim Primary Drinking Water Regula-
tions, may be transferred to tabular summaries. The following information should be included:
26
-------
• Date, place, and time of sampling; name of person who collected the sample.
• Identification of sample as to whether it is a routine distribution system sample, check sam-
ple, raw or process water sample, or other special purpose sample.
• Date of receipt of sample and analysis.
• Laboratory and persons responsible for performing analysis.
• Analytical technique/method used.
• Results of analysis.
FREE CHLORINE RESIDUAL AND TURBIDITY
Free chlorine residual and turbidity measurements do not need to be done in approved labora-
tories, but may be performed by any persons acceptable to the State. There is, however, a definite
need for quality control guidelines to be instituted at the State level for these measurements; it is
equally important that systems be in use to assure validity of data for these critical measurements.
If the criteria below are met, the States should be able to approve persons performing the measure-
ments.
Free Chlorine Residual
The following are criteria for free chlorine residual measurements:
• Method: DPD Colorimetric Method, described on pages 129-132 in "Standard Methods for
the Examination of Water and Wastewater," 13th edition.
• Sample preservation: None; analyses must be made as soon as practicable, or within 1 hour.
• Sample container: Plastic or glass.
• Equipment: DPD Colorimetric Test Kit, or spectrophotometer or photometer.
Turbidity
Criteria for measuring turbidity are the following:
• Method: Nephelometric, described on pages 350-353 in "Standard Methods for the Exam-
ination of Water and Wastewater," 13th edition, and on pages 295-298 in EPA's "Methods
for Chemical Analysis of Water and Wastes."
• Sample preservation: None; analyses must be made as soon as practicable or within 1 hour.
• Sample container: Plastic or glass.
• Equipment: Nephelometer
• Calibration of sealed liquid turbidity standards: Sealed liquid turbidity standards purchased
from the instrument manufacturer must be calibrated against properly prepared and diluted
formazin standards at least every 4 months in order to monitor their eventual deterioration.
These standards should be replaced when any major change from the previous calibration
occurs. Solid turbidity standards composed of plastic, glass, or other materials are not relia-
ble and should not be used.
27
-------
ACTION RESPONSE TO LABORATORY RESULTS (OPTIONAL REQUIREMENTS)
When action response is a designated laboratory responsibility, the water plant operator and
State engineer are promptly notified on unsatisfactory sample results, and a request is made for
resampling from the same sampling point.
28
-------
SAMPLE FORMS FOR ON-SITE EVALUATION OF LABORATORIES INVOLVED IN
ANALYSIS OF PUBLIC WATER SUPPLIES
CHEMISTRY (INORGANIC AND ORGANIC)
LABORATORY:.
STREET:.
CITY: STATE:
TELEPHONE NUMBER:
SURVEY BY:.
AFFILIATION:.
DATE:.
29
-------
PERSONNEL
Laboratory
Location
Date
Evaluator
Position/title
Inorganic analyst(s)
Organic analyst(s)
Supervisor/consultant
Laboratory director
Name
Academic
training
HS
BA/BS
Other
Present
specialty
Experience
(years/area)
-------
LABORATORY FACILITIES
Laboratory
Location
Date
Evaluator.
Item
Labspace (cite ft2 /person)
Bench space (linear feet)
Sink (with hot and cold running water)
Electrical services
Distilled water
Deionized water
Exhaust hood
Available
Yes
No
Comments
31
-------
LABORATORY EQUIPMENT AND INSTRUMENTATION SPECIFICATIONS
Laboratory
Location
Date
Evaluator
Item
Analytical balance
Photometers:
Spectrophotometer
Filter photometer
pH Meter
Specific ion meter
Atomic absorption spectrophotometer
Gas chromatograph
Recorders:
For atomic absorption
For gas chromatograph
Conductivity meter
Drying oven
Desiccator
Hot plate
Refrigerator
Glassware
Water bath
Number
of units
Make
Model
Age/condition
32
-------
GENERAL LABORATORY PRACTICES
Laboratory
Location _
Date
Evaluator
Item
Comments
(Where applicable, cite system, quality check, adequacy of procedures)
Prepackaged kits
Calibration intervals
Glassware preparation
Distilled deionized water
Chemicals/reagents
Laboratory safety equipment
33
-------
METHODOLOGY
Laboratory.
Location
Date
E valuator.
Parameter
Arsenic
Barium
Cadmium
Chromium
Lead
Mercury
Nitrate
Selenium
Silver
Fluoride
Chlorinated hydrocarbons:
Endrin
Lindane
Methoxychlor
Toxaphene
Chlorophenoxys
2,4-D
2,4,5-TP
Name or description
of method
Method used (cite page and year)
SM
ASTM
EPA
Other
Number of analyses (frequency)
Daily
Weekly
Monthly
Satisfactory1
Yes
No
1 For use only by certifying authority.
-------
SAMPLE COLLECTING, HANDLING, AND PRESERVATION
Laboratory
Location
Date
Evaluator
Parameter
Arsenic
Barium
Cadmium
Chromium
Lead
Mercury
Nitrate
Selenium
Silver
Fluoride
Chlorinated hydrocarbons
Chlorophenoxys
Container
used1
Preservative
used
Normal
holding
time
Satisfactory2
Yes
No
1P = Plastic, hard or soft; G = Glass, hard or soft.
2For use only by certify authority.
35
-------
QUALITY CONTROL
Laboratory
Location _
Date
Evaluator
Item
Minimum requirements:
Quality control data available for inspection
Use of unknown performance sample
Documented standard curve
Standard curve checked prior to each sample
set
Verification of standards (every 20 samples)
Optional requirements:
Service contract on balances
Use of class S weights
Use of NBS-certified thermometer
Use of color standards
Dating of chemicals
For lab analyzing samples other than its own
Use of known reference samples
Use of duplicate samples
Standard deviation calculations
Quality control charts or tabulations
Done
Yes
No
Freq.
Comments (system used)
Satis.1
Yes
No
1 For use only by certifying authority.
36
-------
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
DATA HANDLING
Laboratory
1 oration
Date
Evaluator
Comments: system(s) used, frequency, etc.
37
-------
-------
Chapter V
MICROBIOLOGY: CRITERIA AND PROCEDURES FOR INTERIM
CERTIFICATION OF LABORATORIES INVOLVED
IN ANALYSIS OF PUBLIC WATER SUPPLIES
The criteria and procedures described herein, shown in bold, are minimum requirements consid-
ered essential for laboratories seeking certification for microbiological analysis of public water sup-
plies. The requirements include laboratory equipment and supplies, laboratory practices, methodology,
sample collection, and certain quality control measures. The other items, involving personnel, facili-
ties, additional quality control procedures, data reporting, and action response, are optional. For a
commercial laboratory to qualify for certification in microbiology, it must process a minimum of 20
potable water samples per month using either the multiple tube procedure or membrane filter test.
Until National Revised Primary Drinking Water Regulations require certification of water supply
laboratories, all specifications will be considered as guidelines to be used by certification officials.
At that time, minimal requirements will be essential to certification of laboratories involved in anal-
ysis of public water supplies.
The minimum requirements must be in compliance, or action must be taken to correct defi-
ciencies prior to certification. A laboratory that exceeds these minimum requirements is encouraged
to maintain and improve those higher standards for facilities, equipment, methodology, and quality
control, as well as to continue the upgrading of personnel through training efforts to ensure routine
production of reliable data.
The required methods of analyses are referenced in "Standard Methods for the Examination of
Water and Wastewater," 13th edition; however, some criteria in this document are more specific and
permit fewer variations than "Standard Methods."
The guidelines for quality assurance procedures are those in EPA's quality assurance program as
cited in the EPA Manual, "Microbiological Methods for Monitoring the Environment" (EMSL EPA
Cincinnati). A valuable source of further detail and background information for the laboratory eval-
uator is available in EPA's "Handbook for Evaluating Water Bacteriological Laboratories" (EPA-
670/9-75-006, August 1976).
Minimum requirements are shown throughout in bold.
PERSONNEL1 (OPTIONAL REQUIREMENTS)
Analyst
The analyst performs microbiological tests with minimal supervision in those specialties for
which he is qualified by education and/or training and experience.
1 Exceptions will be made for those persons employed by the laboratory and currently doing the required analy-
ses prior to promulgation of the interim regulations provided that within 2 years after June 24, 1977, they receive a
minimum of 2 weeks of additional training in water microbiology.
39
-------
• Academic training: Minimum of high school diploma in academic or laboratory-oriented
vocational courses.
• Job training: Minimum of 30 days on-the-job training plus one week of supplementary train-
ing acceptable to the Federal and State regulatory agency or agency responsible for primacy.
Personnel should take advantage of courses available to Federal and State regulatory
agencies.
• Supervision: Supervision by an experienced professional scientist. In the small water plant
laboratory consisting of a single analyst, the services of a State-approved outside consultant
must be available.
Supervisor/Consultant
The supervisor directs technical personnel in the proper performance of laboratory procedures
and the reporting of results. If no technical supervisor is available, a consultant should be available.
• Academic training: Minimum of a bachelor's degree in microbiology, biology, chemistry, or
a closely related field. Exceptions will be made for employees of laboratories that serve
communities with populations of 50,000 or less if they receive at least 2 weeks of additional
training in water microbiology from a Federal agency, State agency, or university.
• Job training: Technical training in water microbiology for a minimum of 2 weeks from a
Federal agency, State agency, or university in the parameter to be tested. Consultant must
have 1 year of bench experience, approved by the State, in total coliform analysis. State
laboratory expertise would be the most desirable source of outside consultation.
• Experience: One year of bench experience in sanitary (water, milk, or food) microbiology.
LABORATORY FACILITIES (OPTIONAL REQUIREMENTS)
Laboratory space should be adequate (200 ft2 and 6 linear ft of bench space per analyst) to
accommodate periods of peak work load. Working space requirements should include sufficient
bench-top area for processing samples; storage space for media, glassware, and portable equipment
items; floor space for stationary equipment (incubators, waterbaths, refrigerators, etc.); and associ-
ated area for cleaning glassware and sterilizing materials. The space required for both laboratory
work and materials preparation in small water plant laboratories may be consolidated into one
room, with the various functions allocated to different parts of the room.
Facilities should be clean, air-conditioned, and with adequate lighting at bench top (100 ft-
candles).
Laboratory safety, which must be an integral and conscious effort in laboratory operations,
should provide safeguards to avoid electric shock, prevent fire, prevent accidental chemical spills,
and minimize microbiological dangers, facility deficiencies, and equipment failures. While safety
is not an aspect of laboratory certification, the evaluation should point out on an informal basis,
potential safety problems observed during an on-site visit.
40
-------
LABORATORY EQUIPMENT, SUPPLIES, AND MATERIALS (MINIMUM REQUIREMENTS)
The laboratory must have available or access to the items required for the total coliform mem-
brane filter or most probable number procedures as listed below.
• pHMeter: Accuracy must be ±0.1 units.
• Balances—top loader or pan: Balance must be clean, not corroded, and be provided with ap-
propriate weights of good quality. Balance must tare out and detect 50-mg weight accurate-
ly: this sensitivity is required for use in general media preparation of 2g or larger quantities.
• Temperature-monitoring devices:
—Glass or metal thermometers must be graduated in 0.5°C increments.
—Continuous temperature recording devices must be sensitive to within 0.5°C.
—Liquid column of glass thermometers must have no separation.
—A certified thermometer or one of equivalent accuracy must be available.
• Air (or water jacketed) incubator/incubator rooms I waterbaths/aluminum block incubators:
—Unit must maintain internal temperature of 35.0° ± 0.5°C in area of use at maximum
loading.
—When aluminum block incubators are used, culture dishes and tubes must be snug-fitting in
block.
• Autoclave:
—Autoclave must be in good operating condition when observed during operational cycle or
when time-temperature charts are read. Vertical autoclaves are not recommended. For
most efficient operation, a double-walled autoclave constructed of stainless steel is sug-
gested (optional).
—Autoclave must have pressure and temperature gauges on exhaust side and an operating
safety valve.
—Autoclave must reach sterilization temperature (121°C) and be maintained during steriliza-
tion cycle: no more than 45 minutes is required for'a complete cycle.
—Depressurization must not produce air bubbles in fermentation media.
• Hot-air oven: Oven must be constructed to ensure a stable sterilization temperature. Its use
is optional for sterilization of glass pipets, bottles, flasks, culture dishes, etc. (optional).
• Refrigerator: Refrigerator must hold temperature at 1° to 4.4°C (34° to 40°F).
• Optical/counting/lighting equipment: Low power magnification device (preferably binocular
microscope with 10 to 15x) with fluorescent light source must be available for counting MF
colonies. A mechanical hand tally can be used for counting colonies (optional).
• Inoculation equipment:
—Loop diameter must be at least 3 mm and of 22 to 24 gauge Nichrome, chromel, or
41
-------
platinum-iridium wire. Single-service metal loops, disposable dry heat-sterilized hardwood
applicator sticks, pre-sterilized plastic, or metal loops may be used (optional).
• Membrane filtration equipment:
—Units must be made of stainless steel, glass, or autoclavable plastic. Equipment must not
leak and must be uncorroded.
—Field equipment is acceptable for coliform detection only when standard laboratory MF
procedures are followed.
• Membrane filters and pads:
—Membrane filters must be manufactured from cellulose ester materials, white, grid-marked,
47-mm diameter, 0.45 jum pore size. Another pore size may be used if the manufacturer
gives performance data equal to or better than the 0.45-jum membrane filter.
—Membranes and pads must be autoclavable or presterilized.
• Laboratory glassware, plastic ware, and metal utensils:
—Except for disposable plastic ware, items must be resistant to effects of corrosion, high
temperature, and vigorous cleaning operations. Metal utensils made of stainless steel are
preferred (optional).
-Flasks, beakers, pipets, dilution bottles, culture dishes, culture tubes, and other glassware
must be of borosilicate glass and free of chips, cracks, or excessive etching. Volumetric
glassware should be Class A, denoting that it meets Federal specifications and need not be
calibrated before use.
—Plastic items must be of clear, inert, nontoxic material and must retain accurate calibration
marks after repeated autoclaving.
• Culture dishes:
—Sterile tight or loose-lid plastic culture dishes or loose-lid glass culture dishes must be used.
—For loose-lid culture dishes, relative humidity in the incubator must be at least 90 percent.
—Culture dish containers must be aluminum or stainless steel; or dishes may be wrapped in
heavy aluminum foil or char-resistant paper.
—Open packs of disposable sterile culture dishes must be reseated between uses.
• Culture tubes and closures:
—Culture tubes must be made of borosilicate glass or other corrosion resistant glass and
must be of a sufficient size to contain the culture medium, as well as the sample portions
employed, without being more than 3/4 full. It is desirable that the fermentation via]
extend above the medium (optional).
—Caps must be snug-fitting stainless steel or plastic; loose-fitting aluminum caps or screw
caps are also acceptable.
42
-------
• Measuring equipment:
-Sterile, glass or plastic pipets must be used for measuring 10 ml or less.
—Pipets must deliver the required volume quickly and accurately within a 2.5 percent toler-
ance.
—Pipets must not be badly etched; mouthpiece or delivery tips must not be chipped; gradua-
tion marks must be legible.
—Open packs of disposable sterile pipets must be resealed between uses.
—Pipet containers must be aluminum or stainless steel.
—Graduated cylinders must be used for samples larger than 10 ml; calibrated membrane
filter funnel markings are permissible provided accuracy is within a 2.5 percent tolerance.
GENERAL LABORATORY PRACTICES (MINIMUM REQUIREMENTS)
Sterilization Procedures
• The following times and temperatures must be used for autoclaving materials:
Material Temperature/Minimum Time
Membrane filters and pads 121 °C/10 min.
Carbohydrate-containing media 121°C/12-15 min.
(lauryl tryptose, brilliant green
lactose bile broth, etc.)
Contaminated materials and discarded 121°C/30 min.
tests
Membrane filter assemblies (wrapped), 121°C/30 min.
sample collection bottles (empty),
individual glassware items
Rinse water volumes of 500 ml to 1,000 121°C/45 min.
ml
Rinse water in excess of 1,000 ml 121°C/time adjusted for volume; check
for sterility
Dilution water blank 121°C/30 min.
Membrane filter assembles must be sterilized between sample filtration series. A filtration series
ends when 30 minutes or longer elapse between sample filtrations. At least 2 minutes of UV light or
boiling water may be used on membrane filter assembly to prevent bacterial carry-over between
filtrations-(optional).
Dried glassware must be sterilized at a minimum of 170°C for 2 hours.
Laboratory Pure Water (Distilled, Deionized, or Other Processed Waters)
• An analyst must test the quality of the laboratory pure water or have it tested by the State
or by a State-authorized laboratory.
43
-------
• Only water determined as laboratory pure water (see quality control section) can be used
for performing bacteriological analyses.
Although processed water may be acceptable for routine chemistry, there is a good chance that
it contains enough of some constituent to be toxic or stimulatory to microorganisms (optional).
Rinse and Dilution Water
Stock buffer solution must be prepared according to "Standard Methods" using laboratory pure
water adjusted to pH 7.2. Stock buffer must be autoclaved or filter-sterilized, labeled, dated, and
stored at 1° to 4.4°C. The stored buffer solution must be free of turbidity.
Rinse and dilution water must be prepared by adding 1.25 ml of stock buffer solution per liter
of laboratory pure water. Final pH must be 7.2 ± 0.1.
Media Preparation and Storage
The following are minimum requirements for storing and preparing media:
• Laboratories must use commercial dehydrated media for routine bacteriological procedures
as quality control measures.
• Lauryl tryptose and brilliant green lactose bile broths must be prepared according to
"Standard Methods"; lactose broth is not permitted.
• Dehydrated media containers must be kept tightly closed and stored in a cool, dry location.
Discolored or caked dehydrated media cannot be used.
• Laboratory pure water must be used; dissolution of the media must be completed before
dispensing to culture tubes or bottles.
• The membrane filter broth and agar media must be heated in a boiling water bath until com-
pletely dissolved.
• Membrane filter (MF) broths must be stored and refrigerated no longer than 96 hours. MF
agar media must be stored, refrigerated and used within 2 weeks.
• Most probable number (MPN) media prepared in tubes with loose-fitting caps must be used
within 1 week. If MPN media are refrigerated after sterilization, they must be incubated over-
night at 35° C to confirm usability. Tubes showing growth or gas bubbles must be discarded.
• Media in screw cap containers may be held up to 3 months, provided the media are stored in
the dark and evaporation is not excessive (0.5 ml per 10 ml total volume). Commercially
prepared liquid and agar media supplies may be used (optional).
• Ampouled media must be stored at 1° to 4.4°C (34° to 40°F); time must be limited to man-
ufacturer's expiration date.
METHODOLOGY (MINIMUM REQUIREMENTS)
The required procedures, which are mandatory, are described in the 13th edition of "Standard
Methods": standard coliform MPN tests (p. 664-668), single step or enrichment standard total
coliform membrane filter procedure (p. 679-683). Tentative methods are not acceptable. All other
procedures are considered alternative analytical techniques as described in section 141.27
44
-------
of the National Interim Primary Drinking Water Regulations. Application for the use of alternative
methods may require acceptable comparability data.
The membrane filter procedure is preferred because it permits analysis of large sample volumes
in reduced analysis time. The membranes should show good colony development over the entire
surface. The golden green metallic sheen colonies should be counted and recorded as the coliform
density per 100 ml of water sample. The following rules for reporting any problem with MF results
must be observed:
• Confluent growth: Growth (with or without discrete sheen colonies) covering the entire
filtration area of the membrane. Results are reported as "confluent growth per 100 ml, with
(or without) coliforms," and a new-sample requested.
• TNTC (Too numerous to count): The total number of bacterial colonies on the membrane is
too numerous (usually greater than 200 total colonies), not sufficiently distinct, or both. An
accurate count cannot be made. Results are reported as "TNTC per 100 ml, with (or with-
out) coliforms," and a new sample requested.
• Confluent growth and TNTC: A new sample must be requested, and the sample volumes
filtered must be adjusted to apply the MF procedure; otherwise the MPN procedure must be
used.
• Confirmed MPN test on problem supplies: If the laboratory has elected to use the MPN test
on water supplies that have a continued history of confluent growth or TNTC with the MF
procedure, all presumptive tubes with heavy growth without gas production should be sub-
mitted to the confirmed MPN test to check for the suppression of coliforms. A count is
adjusted based upon confirmation and a new sample requested. This procedure should be
carried out on one sample from each problem water supply once every 3 months.
SAMPLE COLLECTION, HANDLING, AND PRESERVATION (MINIMUM REQUIREMENTS)
When the laboratory has been delegated responsibility for sample collecting, handling, and pres-
ervation, there must be strict adherence to correct sampling procedures, complete identification of
the sample, and prompt transfer of the sample to the laboratory as described in "Standard Meth-
ods," 13th edition, section 450, p. 657-660.
The sample must be representative of the potable water system. The sampling program must
include examination of the finished water at selected sites that systematically cover the distribution
network.
Minimum sample frequency must be that specified in the National Interim Primary Drinking
Water Regulations, 40 CFR 141.21.
The collector must be trained in sampling procedures and approved by the State regulatory
authority or its delegated representative.
The water tap must be sampled after maintaining a steady flow for 2 or 3 minutes to clear serv-
ice line. The tap is free of aerator, strainer, hose attachment, or water purification devices.
The sample volume must be a minimum of 100 ml. The sample bottle must be filled only to the
shoulder to provide space for mixing.
The sample report form must be completed immediately after collection with location, date and
time of collection, chlorine residual, collector's name, and remarks.
45
-------
Sample bottles must be of at least 120 mi-capacity, sterile plastic or hard glass, wide mouthed
with stopper or plastic screw cap, and capable of withstanding repeated sterilization. Sodium thio-
sulfate (100 mg/1) is added to all sample bottles during preparation. As an example, 0.1 ml of a 10
percent solution is required in a 4-oz (120-ml) bottle.
Date and time of sample arrival must be added to the sample report form when sample is re-
ceived in the laboratory.
State regulations relating to chain-of-custody, if required, must be followed in the field and in
the laboratory.
Samples delivered by collectors to the laboratory must be analyzed on the day of collection.
Where it is necessary to send water samples by mail, bus, United Parcel Service, courier service,
or private shipping, holding/transit time between sampling and analyses must not exceed 30 hours.
When possible, samples are refrigerated during transit and during storage in the laboratory (optional).
If the laboratory is required by State regulation to examine samples after 30 hours and up to 48
hours, the laboratory must indicate that the data may be invalid because of excessive delay before
sample processing. Samples arriving after 48 hours shall be refused without exception and a new
sample requested. (The problem of holding time is under investigation by EPA.)
QUALITY CONTROL PROGRAM
Minimum Requirement
A written description for current laboratory quality control program must be available for
review. Management, supervisors, and analysts participate in setting up the quality control pro-
gram. Each participant should have a copy of the quality control program and a detailed guide
of his own portion. A record on analytical quality control tests and quality control checks on
media, materials, and equipment must be prepared and retained for 3 years.
Analytical Quality Control Tests for General Laboratory Practices and Methodology
Minimum and optional requirements for analytical quality control tests for general practices
and methodology are:
• Minimum requirements:
—At least five sheen or borderline sheen colonies must be verified from each membrane con-
taining five or more such colonies. Counts must be adjusted based on verification. The
verification procedure must be conducted by transferring growth from colonies into lauryl
tryptose broth (LTB) tubes and then transferring growth from gas-positive LTB cultures to
brilliant green lactose bile (BGLB) tubes. Colonies must not be transferred exclusively to
BGLB because of the lower recovery of stressed coliforms in this more selective medium.
However, colonies may be transferred to LTB and BGLB simultaneously. Negative LTB
tubes must be reincubated a second day and confirmed if gas is produced. It is desirable to
verify all sheen and borderline sheen colonies (optional).
-A start and finish MF control test (rinse water, medium, and supplies) must be conducted
for each filtration series. If sterile controls indicate contamination, all data on samples
affected must be rejected and a request made for immediate resampling of those waters
involved in the laboratory error.
46
-------
—The MPN test must be carried to completion, except for gram staining, on 10 percent of
positive confirmed samples. If no positive tubes result from potable water samples, the
completed test except for gram staining must be performed quarterly on at least one
positive source water.
—Laboratory pure water must be analyzed annually by the test for bactericidal properties
for distilled water ("Standard Methods," 13th edition, p. 646). Only satisfactorily tested
water is permissible in preparing media, reagents, rinse, and dilution water. If the tests do
not meet the requirements, corrective action must be taken and the water retested.
—Laboratory pure water must be analyzed monthly for conductance, pH, chlorine residual,
and standard plate count. If tests exceed requirements, corrective action must be taken
and the water retested.
—Laboratory pure water must not be in contact with heavy metals. It must be analyzed
initially and annually thereafter for trace metals (especially Pb, Cd, Cr, Cu, Ni, and Zn). If
tests do not meet the requirements, corrective action must be taken and the water re-
tested.
—Standard plate count procedure must be performed as described in "Standard Methods,"
13th edition, p. 660-662. Plates must be incubated at 35° ± 0.5°C for 48 hours.
—Requirements for laboratory pure water:
pH 5.5 - 7.5
Conductivity Greater than 0.2 megohm as resistivity or
less than 5.0 micromhos/cm at 25°C
Trace metals:
A single metal Not greater than 0.05 mg/1
Total metals Equal to or less than 1.0 mg/1
Test for bactericidal properties of dis-
tilled water ("Standard Methods,"
13th edition, p. 646) 0.8 - 3.0
Free chlorine residual 0.0
Standard plate count Less than 10,000/ml
—Laboratory must analyze one quality control sample per year (when available) for param-
eter^) measured.
—Laboratory must satisfactorily analyze one unknown performance sample per year (when
available) for parameter(s) measured.
Optional requirements:
—Duplicate analyses should be run on known positive samples at a minimum frequency of
one per month. The duplicates may be run as a split sample by more than one analyst,
with each split being a 50-ml sample.
—Water plant laboratories should examine a minimum of one polluted water source per
month in addition to the required number of distribution samples.
—If there is more than one analyst in laboratory, at least once per month each analyst
47
-------
should count the sheen colonies on a membrane from a polluted water source. Colonies on
the membrane should be verified and the analysts' counts compared to the verified count.
—A minimum number of the official water supply samples required for each system should
be analyzed by the State laboratory. For example, systems that are required to have less
than 10 samples examined per month should submit one additional sample to a State
authorized laboratory. Water systems with sample requirements above 10 per month
would submit two additional samples to a State authorized laboratory.
Quality Control Checks of Laboratory Media, Equipment, and Supplies
Minimum and optional requirements for quality control checks of laboratory media, equipment,
and supplies are:
• Minimum requirements:
—pH meter must be clean and calibrated each use period with pH 7.0 standard buffer. Buf-
fer aliquot must be used only once. Commercial buffer solutions must be dated on initial
use.
—Balances (top loader or pan) must be calibrated annually.
—Glass thermometers or continuous recording devices for incubators must be checked year-
ly and metal thermometers quarterly (or at more frequent intervals when necessary)
against a certified thermometer or one of equivalent accuracy.
—Temperature in air (or water jacketed) incubator/incubator room/waterbaths/aluminum
block incubators must be recorded continuously or recorded daily from in-place thermom-
eter^) immersed in liquid and placed on shelves in use.
—Date, time, and temperature must be recorded continuously or recorded for each steriliza-
tion cycle of the autoclave.
—Hot air oven must be equipped with a thermometer calibrated in the range of 170°C or
with a temperature recording device. Records must be maintained showing date, time, and
temperature of each sterilization cycle. It is desirable to place the thermometer bulb in
sand and to avoid overcrowding (optional).
—Membrane filters used must be those recommended by the manufacturer for water analy-
sis. The recommendation must be based on data relating to ink toxicity, recovery, reten-
tion, and absence of growth-promoting substances.
—Washing processes must provide clean glassware with no stains or spotting. With initial use
of a detergent or washing product and whenever a different washing product is used, the
rinsing process must demonstrate that it provides glassware free of toxic material by the
inhibitory residue test ("Standard Methods," 13th edition, p. 643).
—At least one bottle per batch of sterilized sample bottles must be checked by adding ap-
proximately 25 ml of sterile LTB broth to each bottle. It must be incubated at 35 ± 0.5°C
for 24 hours and checked for growth.
—Service contracts or approved internal protocols must be maintained on balances, auto-
clave, water still, etc., and the service records entered in a log book.
48
-------
—Records must be available for inspection on batches of sterilized media showing lot num-
bers, date, sterilization tune-temperature, final pH, and technician's name.
• Optional requirements:
-Positive and negative cultures should be used, and testing should be carried out to deter-
mine recovery and performance compared to a previous acceptable lot of medium.
-Media should be ordered on a basis of 12-month needs. Bottles should be dated on receipt
and when opened initially. Except for large volume uses, media should be purchased in 1 /4-
Ib bottles. Bottles of media should be used within 6 months after opening; however, in no
case should opened media be used after one year. Opened bottles should be stored in a des-
iccator to extend storage time beyond 6 months. Shelf life of unopened bottles is 2 years.
—Testing should be carried out in media and membranes to determine recovery and per-
formance compared to previous acceptable lot.
—Lot number of membrane filters and date of receipt should be recorded.
—Heat sensitive tapes and spore strips or ampoules should be used during steiinzation. Maxi-
mum registering thermometer is recommended.1
DATA REPORTING (MINIMUM REQUIREMENTS)
Where the laboratory has the responsibility for sample collections, the sample collector should
complete a sample report form immediately after each sample is taken. The information on the
form includes sample identification number, sample collector's name, time and da'a of collection,
arrival time and date in the laboratory, direct count, MF verified count, J.'^N completed count,
analyst's name, and other special information.
Results should be calculated and entered on the sample report form to be forwarded. A careful
check should be made to verify that each result was entered correctly from the bench sheet and
initialed by the analyst.
All results should be reported immediately to the proper authority.
Positive results are reported as preliminary without waiting for MF verification or MPN comple-
tion. After MF verification and/or MPN completion, the adjusted counts should be reported.
A copy of the sample report form should be retained either by the laboratory or State program
for 3 years. If results are entered into a computer storage system, a printout of the data should be
returned to the laboratory for verification with bench sheets.
ACTION RESPONSE TO LABORATORY RESULTS (MINIMUM REQUIREMENT)
When action response is a designated laboratory responsibility, the proper authorities should be
promptly notified on unsatisfactory sample results, and a request should be made for resampling
from the same sampling point.
49
-------
SAMPLE FORMS FOR ON-SITE EVALUATION OF LABORATORIES INVOLVED IN
ANALYSIS OF PUBLIC WATER SUPPLIES-MICROBIOLOGY
LABORATORY:.
STREET-
CITY: STATE:
TELEPHONE NUMBER:.
SURVEY BY:
AFFILIATION:.
DATE:.
CODES FOR MARKING ON-SITE EVALUATION FORMS:
S—Satisfactory
U —Unsatisfactory
NA—Not Applicable
50
-------
Laboratory Evaluator.
Location Date
PERSONNEL
The form dealing with personnel can be found on page 52.
LABORATORY FACILITIES
Space in laboratory and preparation room is adequate for needs during peak work periods
(200 ft2 and 6 linear ft of usable bench space per analyst).
Facilities are clean, with adequate lighting (100 ft-candles) and air conditioning.
NOTE: Material on pages 53-65, except where indicated, are minimum requirements.
51
-------
PERSONNEL
Laboratory.
Location
Date
Evaluator
Position/title
Laboratory director
Supervisor/consultant
Professionals
(note discipline)
Technician/analyst
Name
Academic training
HS
BA/BS
§A
MA/MS
AM
Ph.D.
IF©
Present
specialty
5) f\A (^
Experience
(years/area)
•WILY
-------
Laboratory Evaluator
Location Date
LABORATORY EQUIPMENT, SUPPLIES, AND MATERIALS
1. pH Meter
Manufacturer Model
Clean, calibrated to 0.1 pH units each use period; record maintained .
Aliquot of standard pH 7.0 buffer used only once
2. Balance—Top Loader or Pan
Manufacturer Model
Clean. Detects a 50-mg weight accurately (for a general media preparation of.>2-g
quantities)
Good quality weights in clean condition
3. Temperature-Monitoring Devices
Accuracy checked annually against a certified thermometer or one of equivalent
accuracy
Legible graduations in 0.5°C-increments
No separation in liquid column
4. Incubator or Incubator Room
Manufacturer Model.
Sufficient size for daily work load
Uniform temperature maintained on shelves in all areas used (35.0° ± 0.5°C)
Calibrated thermometer with bulb immersed in h'quid and located on shelves in use.
Temperature recorded daily or recording thermometer sensitive to ± 0.5°C
5. Autoclave
Manufacturer Model
Reaches sterilization temperature (121°C), maintains 121°C during sterilization
cycle, and requires no more than 45 min for a complete cycle
Pressure and temperature gauges on exhaust side and an operating safety valve ..
No air bubbles produced in fermentation vials during depressurization.
Record maintained on time and temperature for each sterilization cycle
53
-------
6. Hot-Air Oven
Manufacturer Model
Operates at a minimum of 170 C
Thermometer inserted or oven equipped with temperature-recording thermometer
device
Time and temperature record maintained for each sterilization cycle
Thermometer bulb in sand (optional)
7. Refrigerator
Temperature maintained at 1° to 4.4°C (34° to 40°F)
8. Optical Equipment
Low power magnification device (preferably binocular microscope with 10 to 15X)
with fluorescent light source for counting MF colonies
Colonies counted with a mechanical hand tally (optional)
9. Inoculation Equipment
Sterilized loops of at least 3-mm diameter, 22 to 24 gauge Nichrome, Chromel, or
platinum-iridium wire
or
Disposable dry heat-sterilized hardwood applicator sticks or presterilized loops....
10. Membrane Filtration Equipment
Manufacturer Model
Made of stainless steel, glass, or autoclavable plastic
Nonleaking and uncorroded
11. Membrane Filters and Pads
Manufacturer Model
Filters recommended by manufacturer for water analyses
Filters and pads presterilized or autoclavable
12. Glass, Plastic, and Metal Utensils for Media Preparation
Washing process provides glassware free of toxic residue as demonstrated by the
inhibitory residue test
Glass items of borosilicate, free of chips and cracks
Utensils clean and free from foreign residues or dried medium
Plastic items clear with visible graduations
54
-------
13. Sample Bottles
Wide-mouth hard glass bottles; stoppered or plastic screw-capped; capacity at least
120ml
Glass-stoppered bottles with tops covered with aluminum foil or kraft
paper
Screw-caps have leakproof nontoxic liners that can withstand repeated sterilization
(30 min at 121°C)
Sterile sample bottles contain 10 mg of dechlorinating agent per 100 ml of sample .
14. Pipets
Brand Type
Sterile; glass or plastic; with a 2.5 percent tolerance
Tips unbroken; graduations distinctly marked
75. Pipet Containers
Aluminum, stainless steel
Pipets wrapped in quality kraft paper (char-resistant)
Open packs of disposable sterile pipets resealed between uses.
16. Culture Dishes
Brand Type.
Sterile plastic or glass
Open packs of disposable sterile plastic dishes resealed between uses .
Dishes are in containers of aluminum or stainless-steel with covers or
are wrapped with heavy aluminum foil or char-resistant paper
17. Culture Tubes and Closures
Sufficient size to contain sterile medium and sample without danger of spillage.
Metal or plastic caps; plastic plugs ,
Borosilicate glass or other corrosion-resistant glass
55
-------
Laboratory Evaluator
Location Date
GENERAL LABORATORY PRACTICES
1. Sterilization Procedures
Satisfactory sterilization procedures and/or records ,
Tube broth media and reagents sterilized at 121°C 12 to 15 min
Tubes and flasks packed loosely in baskets or racks for uniform heating and cooling .
MF presterilized or autoclaved at 121°C for 10 min with fast exhaust
MF assemblies and empty sample bottles sterilized at 121°C for 30 min
MF assemblies sterilized between sample filtration series
Rinse water volumes of 500 to 1,000 ml sterilized at 121°C
for 45 min
Dilution water blanks autoclaved at 121°C for 30 min
Wire loops, needles, and forceps sterilized
Total exposure of MPN media to heat not over 45 min
Timing for sterilization begins when autoclave reaches 121°C
Individual glassware items autoclaved at 121°C for 30 min
Individual dry glassware items sterilized 2 hours at 170°C (dry heat)
Pipets, culture dishes, and inoculating loops in boxes sterilized at 170°C for 2 hours.
MPN media removed and cooled as soon as possible after sterilization and stored in
cool dark place (optional)
UV light or boiling water for at least 2 min may be used on membrane filter assem-
blies to reduce bacterial carry-over between each filtration (optional)
2. Laboratory Pure Water
Only laboratory pure water used in preparing media, reagents, rinse water, and dilu-
tion water
Laboratory pure water not in contact with heavy metals
Source: Laboratory-prepared Purchased.
If laboratory-prepared:
Still manufacturer
Deionizer manufacturer
Record of recharge frequency.
Production rate and quality adequate for laboratory needs
Inspected, repaired, cleaned by service contract or in-house service
a. Chemical quality control
Record of satisfactory annual analyses for trace metals
A single metal not greater than 0.05 mg/1
56
-------
Total metals: equal to or less than 1.0 mg/1.
Record of monthly analyses of laboratory pure water
Conductance: >0.2 megohm resistivity or <5.0 microhmos/cm
pH: 5.5-7.5
Standard plate count: <10,000/ml
Free chlorine residual: 0.0
b. Microbiological quality control
Test for bactericidal properties of distilled water (0.8-3.0) performed at least
annually
Testing laboratory Date : Ratio
3. Rinse and Dilution Water
Stock buffer solution prepared according to "Standard Methods," 13th edition.. . .
Stock buffer solution adjusted to pH 7.2
Stock buffer autoclaved at 121°C, stored at 1° to 4.4°C (34° to 40°F) or filter
sterilized
Stock buffer labeled and dated
Stock potassium phosphate buffer solution (1.25 ml) added per liter distilled water
for rinse and dilution water
Final pH 7.2 ± 0.1
4. Media
Dehydrated media bottle kept tightly closed and protected from dust and excessive
humidity in storage areas
Dehydrated media not used if discolored or caked
Laboratory pure water used in media preparation
Dissolution of media complete before dispensing to culture tubes or bottles
MPN tube media with loose-fitting caps used in less than 1 week
Tube media in screw-capped tubes held no longer than 3 months
Ampouled media stored at 1° to 4.4°C and time limited to manufacturer's expira-
tion date
Media stored at low temperatures are incubated overnight prior to use and
tubes with air bubbles discarded
Media protected from sunlight
MF media stored in refrigerator; broth medium used within 96 hours, agar within
two weeks if prepared in tight-fitting dishes
57
-------
5. Lauryl Tryptose Broth
Manufacturer Lot No..
Single strength compbsition, 35.6 g per liter pure water
Single strength pH 6.8 ± 0.2; double strength pH 6.7 ± 0.2
Not less than 10 ml per tube
Media made to result in single strength after addition of sample portions.
6. Brilliant Green Lactose Bile Broth
Manufacturer Lot No.
Medium composition 40 g per liter pure water
Final pH 7.2 ± 0.2
7. M-Endo Media
Manufacturer Lot No.
Medium composition 48.0 g per liter pure water optionally 15 g agar added/1
Reconstituted in laboratory pure water containing 2 percent ethanol (not
denatured)
Final pH 7.2 ± 0.2
Medium held in boiling water bath until completely dissolved
8. Standard Plate Count Agar
Correct composition, sterile and pH 7.0 ± 0.2
Sterile medium not remelted a second time after sterilization
Culture dishes incubated 48 hours at 35° ± 0.5°C
No more than 1.0 ml or less than 0.1 ml sample plated (sample or dilution).
Liquefied agar, 10 ml or more; medium temperature between 44° to 46°C.
Melted medium stored no longer than 3 hours before use
Only plates with between 30 to 300 colonies counted; when 1 ml of undiluted
sample is plated, colony density may be less than 30
Only two significant figures recorded and calculated as standard plate count/
1.0 ml
58
-------
Laboratory Evaluator.
Location Date
METHODOLOGY
Methodology specified in "Standard Methods," 13th edition, or EPA manual
M-Endo broth, M-Endo agar, or Les Endo agar used in a single step procedure ,
In two-step Les M-Endo procedure, MF incubated on lauryl-tryptose-broth-saturated
absorbent pad for 1.5 to 2 hours at 3.5° ± 0.5°C; then on M-Endo broth or Les
Endo agar for 20 to 22 hours at 35° ± 0.5°C
1. Total Coliform Membrane Filter Procedure
Samples containing excessive bacterial populations (greater than 200), confluency,
or turbidity retested by the MPN procedure
Filtration assembly sterile at start of each series
Absorbent pads saturated with medium, excess discarded; or 4.0 ml of agar medium
can be used per culture dish instead of a pad ,
Sample shaken vigorously immediately before test ,
Test sample portions measured and not less than 100 ml
Funnel rinsed at least twice with 20- to 30-ml portions of sterile buffered water
MF removed with sterile forceps grasping area outside effective filtering area.
MF rolled onto medium pad or agar so air bubbles are not trapped
2. Incubation of Membrane Filter Cultures
Total incubation time 22 to 24 hours at 35° ± 0.5°C
Incubated in tight-fitting culture dishes or loose-fitting dishes incubated in high
relative humidity chambers
3. Membrane Filter Colony Counting
Samples repeated when coliforms are "TNTC" or colony growth is confluent, possi-
bly obscuring coliform development and/or detection
Total coliform count calculated in density per 100 ml
Samples containing five or more coliforms per 100 ml are resampled and tested .. .
Low power magnification device with fluorescent light positioned for maximum
sheen visibility
4. Verification of Total Coliform Colonies
All typical coliform (sheen) colonies or at least five randomly selected sheen colo-
nies verified in lauryl tryptose broth and BGLB
Counts adjusted based on verification
All atypical coliform (borderline sheen) colonies or at least five randomly-selected
colonies verified in LTB and BGLB
Counts adjusted based on verification
59
-------
5. MF Field Equipment
Manufacturer Model
Only standard laboratory MF procedures adapted to field application
6. Total Coliform Most Probable Number Procedure
a. Presumptive Test
Five standard portions, either 10 or 100 ml
Sample shaken vigorously immediately before test
Tubes incubated at 35° ± 0.5°C for 24 ± 2 hours
Examined for gas (any gas bubble indicates positive test)
Tubes that are gas-positive within 24 hours submitted promptly to confirm test
Negative tubes returned to incubator and examined for gas within 48 ± 3 hours;
positives submitted to confirm test
Public water supply samples with heavy growth and no gas production con-
firmed for presence of suppressed coliforms
Adjusted count reported based upon confirmation
Adequate test labeling and tube dilution coding (optional)
b. Confirmed Test
Presumptive positive tube gently shaken or mixed by rotating
One loopful or one dip of applicator transferred from presumptive tube to
BGLB
Incubated at 35°C ± 0.5°; checked within 24 hours ± 2 hours for gas production.
Positive confirmed tube results recorded; negative tubes reincubated and read
within 48 ± 3 hours
Unsatisfactory sample defined as three or more positive confirmed tubes
c. Completed Test
Applied to 10 percent of all positive samples each quarter
Applied to all positive confirmed tubes in each test completed
Positive confirmed tubes streaked on EMB plates for colony isolation
Plates adequately streaked to obtain discrete colonies
Incubated at 35° ± 0.5°C for 24 ± 2 hours
Typical nucleated colonies, with or without sheen, on EMB plates selected for
completed test identification
If typical colonies absent, atypical colonies selected for completed test
identification
If no colonies or only colorless colonies appear, confirmed test for that particu-
lar tube considered negative
An isolated typical colony or two atypical colonies transferred to lauryl tryptose
broth
Incubated at 35° ± 0.5°C; checked for gas within 48 ± 3 hours
Cultures producing gas in lauryl tryptose broth within 48 ± 3 hours are consid-
ered coliforms
60
-------
Laboratory Evaluator.
Location : Date
SAMPLE COLLECTION, HANDLING, AND PRESERVATION
Representative samples of potable water distribution system
Minimal sampling frequency as specified in the National Interim Primary Drinking Water
Regulations
Sample collector trained and approved as required by State regulatory authority or its
delegated representative
1. Sample Bottles
Sterile sample bottles of at least 120 ml; able to withstand repeated sterilization....
Ample air space remains after sample collected to allow for adequate mixing
Sodium thiosulfate, 100 mg/1, added to sample bottle before sterilization
2. Sampling
Sample collected after maintaining a steady flow for 2 to 3 min to clear service
line
Tap free of aerator, strainer, hose attachment, water purification, or other devices .
Samples refrigerated when possible during transit and storage periods in the labora-
tory (optional)
3. Sample Identification
Sample identified immediately after collection
Identification includes, water source, location, time and date of collection, and col-
lector's name; insufficiently identified samples discarded
Chlorine residual where applicable
4. Sample Transit Time
Transit time for potable water samples sent by mail or commercial transportation,
not in excess of 30 hours
No sample processed after 48-hour transit/storage
Samples delivered to laboratory by collectors examined the day of collection ....
Data marked as questionable on samples analyzed after 30 hours
5. Sample Receipt in Laboratory
Sample logged in when received in laboratory, including date and time of arrival and
analysis
Chain-of-custody procedures required by State regulations followed
61
-------
Laboratory Evaluator.
Location Date
QUALITY CONTROL
A written laboratory quality control program is available for review.
1. Analytical Quality Control
A record containing results of analytical control tests available for review
a. Verification of MF Colonies
At least five coliforms verified from each positive sample
Sheen colonies in mixed confluent growth reported and verified (optional)
b. Negative Coliform Controls
A start and finish MF control test (rinse water, medium, and supplies) run with
each filtration series
When controls indicate contamination occurred, all data on affected samples
rejected and resampling requested
c. Total Coliform Confirmed Test
Presumptive tubes with heavy growth but no gas production submitted to con-
firmed test to check for suppression of coliforms. Confirmation procedure
carried out every 3 months on one sample from each problem water supply .
d. Duplicate analyses (optional)
Duplicate analyses run on positive polluted samples not to exceed 10 percent
but a minimum of one per month (optional) |
e. Positive Control Samples (optional)
One positive control sample (polluted water) run each month (optional)
f. Colony Counting (If More Than One Analyst in Laboratory) (optional)
Two or more analysts count sheen colonies; all colonies are verified; analysts'
counts compared to verified counts; procedure is carried out at least once per
month (optional) \
g. Check Analyses by State Laboratories (optional)
A minimum of samples, proportional to the local laboratory work load, proc-
essed by State laboratory (see criteria for recommendations) (optional)
62
-------
2. Quality Control of Equipment, Supplies and Media
a. Records
Satisfactory records containing complete quality control checks on equipment,
supplies, and media available for inspection
b. Equipment and Supplies
Service contracts or approved internal protocol maintained on balance, auto-
clave, water still, etc.; service records entered in a log book _
Glass thermometers calibrated annually against a certified thermometer; metal
thermometers checked quarterly _
pH Meters standardized with pH 7.0 buffer _
Laboratory pure water analyzed as described in criteria _
Lot numbers and dates of receipt of membrane filters recorded (optional)
Heat-sensitive tapes and/or spare strips/ampoules used during sterilization (optional)
c. Media Quality Control
Laboratory chemicals of Analytical Reagent Grade _
Dyes certified for bacteriological use _
pH checked and recorded on each batch of medium after preparation and
sterilization _
Causes for deviations beyond ± 0.2 pH units specified _
Media ordered on a basis of 12-month need; purchased in 1/4-lb. quantities,
except those used in large amounts (optional) f
Bottles dated on receipt and when opened (optional)
Opened bottles of routinely used media discarded within 6 months (if stored in
desiccator storage may be extended) (optional)
Shelf life of unopened bottles not in excess of 2 years (optional)
New lots of media quality tested against satisfactory lot using natural water
samples (optional)
63
-------
Laboratory E valuator.
Location Date
DATA REPORTING
Sample information and laboratory data fully recorded
Direct MF counts and/or confirmed MPN results reported promptly
After MF verification and/or MPN completion, adjusted counts reported
One copy of report form retained in laboratory or by State program for 3 years
Test results assembled and available for inspection (optional)
64
-------
Laboratory Evaluator.
Location Date
ACTION RESPONSE TO LABORATORY RESULTS
Unsatisfactory test results given action response and resampled as defined in National
Interim Primary Drinking Water Regulations
State and responsible local authority notified within 48 hours after check samples con-
firm coliform occurrence
All data reported to State and local authorities within 40 days
65
-------
-------
Chapter VI
RADIOCHEMISTRY: CRITERIA AND PROCEDURES FOR (NTERIM
CERTIFICATION OF LABORATORIES INVOLVED IN ANALYSIS OF
PUBLIC WATER SUPPLIES
The criteria and procedures contained herein in bold are the minimum requirements considered
essential for laboratories seeking certification for the radioanalysis of public water supplies. These
include certain laboratory facilities and instrumentation, sample handling and preservation, method-
ology, and quality control. The other items, involving personnel, general laboratory facilities, equip-
ment and instrumentation, practices, data reporting, and action response are optional.
Until National Revised Primary Drinking Regulations require mandatory certification of water
supply laboratories, all specifications, except those associated with the radioanalytical methods
cited in the Federal Register (Vol. 41, No. 133, July 9, 1976), and the instrumentation needed to
make the required measurements will be considered as guidelines to be used by certification
officials. At that time, minimum requirements will be essential to certification of laboratories in-
volved in analysis of public water supplies.
All laboratories, including those that exceed the guidelines and requirements outlined herein,
are urged to maintain and continually improve their personnel, facilities, equipment, instrumenta-
tion, and quality control procedures. To ensure continued production of scientifically and legally
defensible data, an ongoing training program should be an integral part of a laboratory's program.
Minimum requirements are shown throughout in bold.
PERSONNEL1 (OPTIONAL REQUIREMENTS)
Technician or Analyst Responsible for Measurement of Gross Alpha and Gross Beta Activities in
Those Laboratories Being Certified Only for These Measurements
The following requirements are optional for a technician or analyst for measurement of gross
alpha and gross beta activities:
• Academic training: Minimum of a high school diploma or its equivalent, plus at least 2
weeks of specialized training in standards and sample preparation, instrument calibration,
calculations, and data handling.
• Experience: Minimum of 6 months of on-the-job training and experience in routine radio-
chemistry.
1 Exceptions will be made for those persons employed by the laboratory and currently doing the required anal-
yses prior to promulgation of the interim regulations provided that within 2 years after June 24,1977, they receive
a minimum of 2 weeks of additional training in standards preparation, radioanalytical procedures, and quality con-
trol techniques.
67
-------
Supervisory or Senior Analyst for Radioanalytical Procedures Employed in Those Laboratories
Involved in Specific Analyses of One or More of the Radionuclides Described in the National
Interim Primary Drinking Water Regulations
The following requirements are optional for a supervisor or senior analyst for radioanalytical
procedures:
• Academic training: Minimum of bachelor's degree in chemistry, radiochemistry, radio-
isotope technology, or its equivalent.
• Experience:1 Minimum of 1 year of appropriate experience in low-level radiation measure-
ments and radiochemical procedures being considered for certification.
This analyst may be assisted in routine sample preparation and radioanalytical procedures by
one or more technicians with at least the minimum qualifications described in item 1, provided
that such work is directly supervised by the senior analyst.
Laboratory Supervisor, Manager, or Director
The following requirements are optional for a laboratory supervisor, manager, or director:
• Academic training: Minimum of bachelor's degree or its equivalent.
• Experience:l Minimum of 5 years of experience.
LABORATORY FACILITIES
Minimum Requirements
The counting instrument(s) required for measurement of those radionuclides described in the
Federal Register (Vol. 41, No. 133, July 9,1976) must be located in a room other than the one
in which samples and standards are being prepared or in which other types of chemical analyses are
being performed. Temperature of this room must not exceed 27°C. Temperature variation under
normal operating conditions must not exceed 3°C.
All instruments must be properly grounded, and a regulated power supply, either external or
internal, shall be available to each instrument.
In areas where radioactive standards are being prepared, care must be taken to minimize con-
tamination of surfaces and personnel. Either bench surfaces of an impervious material covered with
absorbent paper, or trays (stainless steel, plastic, or fiberglass) lined with absorbent paper are
acceptable.
Optional Requirements
Laboratory space should be adequate (100 to 150 ft2 per analyst is recommended). This space
must contain no less than 15 linear ft of bench space and include the following:
'Each year of college-level training in related scientific fields or demonstrated equivalency shall be considered
equal to 1 year of work experience. Such a substitution should not exceed one-half of the required experience.
68
-------
Sink with hot and cold running water.
Electrical outlets (120 V a.c. grounded).
Source of distilled or deionized water.
Gas supply (natural gas or liquefied petroleum). A propane cylinder with proper attach-
ments may be adequate in laboratories doing limited amounts of analytical work.
Vacuum line, pump, or aspirator.
Exhaust hood.
LABORATORY EQUIPMENT AND INSTRUMENT SPECIFICATIONS
(OPTIONAL REQUIREMENTS)
The instruments listed below are those commonly found in most radioanalytical laboratories.
However, only those instruments needed to prepare and analyze the specific standards and samples
for which the laboratory is being certified are required. Such instruments, when required, should
meet the following specifications:
General Instrumentation and Equipment
The following are specifications for general instrumentation and equipment:
• Analytical balance: Precision, ±0.05 mg. Minimum scale readability, 0.1 mg.
• pH meter or specific ion meter:
—pH meter: Accuracy, ±0.5 units. Scale readability, ±0.1 units. Instrument may be
either line/bench or battery/portable.
—Specific ion meter: Expanded scale millivolt capability. Readable and accurate to
±0.1 mV. Instrument may be either line/bench or battery/portable.
• Conductivity meter: Readable in ohms or mhos, a range of 2 to 2.5 million ohms or
micromhos ±1 percent, and a sensitivity of 0.33 percent or better. Meter may be either
line/bench or battery/portable.
• Drying oven: Gravity convection type.
• Desiccator: Glass or plastic models, depending on particular application.
• Hot plate: Large or small units with selectable temperature control for safe heating of
laboratory reagents and samples.
• 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.
• 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.
• 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.
• Fluorometer: Capable of detecting 0.0005 /xg of uranium.
69
-------
Radiation Instruments
The types of radiation counting systems needed to comply with measurements described in the
Federal Register, Vol. 41, No. 133, July 9, 1976, are set forth below. Only those instruments
needed to analyze for those activities or specific radionuclides for which the laboratory is being
certified are required. Such instruments should meet the following specifications:
• Liquid scintillation system: A liquid scintillation system is required if the laboratory is to
be certified for measurement of tritium in drinking water samples. The system shall be such
that the sensitivity will meet or exceed the requirements of section 141.25 of the Interim
Primary Regulations (FederalRegister, Vol. 41, No. 133, July 9, 1976).
• 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 minimum shielding equivalent to 5 cm of lead must
surround the detector. A cosmic (guard) detector should be operated in anticoincidence
with the main detector. The system shall be such that the sensitivity of the radioanalysis
of water samples will meet or exceed the requirements of section 141.25.
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 photomultiplier tube,
enclosed within a light-tight container, along with the appropriate electronics (high voltage
supply, amplifier, timer, and sealer).
• Scintillation cell system: For the specific measurement of radium-226 by the radon
emanation method, a scintillation system designed to accept scintillation flasks ("Lucas
cells") shall be used. 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) required for this measurement may
either be purchased from commercial suppliers or constructed according to published speci-
fications (Lucas, H. F., "Improved Low-Level Alpha Scintillation Counter for Radon,"Rev.
Sci. Instrum., 28:680, 1967).
• Gamma spectrometer systems: Either a sodium iodide (Nal(Tl)) crystal or a solid state
lithium drifted germanium (Ge(Li)) detector connected to a multichannel analyzer is
required if the laboratory is to be certified for analyses of manmade photon emitters.
If a sodium iodide detector is used, a 7.5 cm X 7.5 cm Nal cylindrical crystal is satis-
factory. However, a 10 cm X 10 cm crystal is recommended. The detector must 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, must contain a
memory of not less than 200 channels and at least one readout device.
A system with a lithium drifted germanium (Ge(Li)) detector may be used for measure-
ment of manmade photon emitters if the efficiency of the detector is such that the sensitiv-
ity of the system meets the minimum detectable activity requirements cited in section
70
-------
141.25. The Ge(Li) detector must be shielded with a minimum of 10 cm of iron or equiva-
lent. The multichannel analyzer, in addition to appropriate electronics, must contain a
memory of not less than 2000 channels and at least one readout device.
GENERAL LABORATORY PRACTICES (OPTIONAL REQUIREMENTS)
The following requirements are optional for general laboratory practices:
• Glassware preparation: All glassware should be washed in a warm detergent solution and
thoroughly rinsed in tap water. A distilled water rinse should follow the tap water rinse.
This cleaning procedure is sufficient for most analytical needs. However, specific analytical
methods may dictate the need for more elaborate procedures for ensuring cleanliness of
glassware.
• Water quality: All water used in preparation of reagents, standards, and samples should
have resistance values between 0.5 and 2.0 megohms (2.0 to 0.5 micromhos)/cm at 25°C.
Excellent quality water has resistance values exceeding 1.0 megohms/cm (less than 1.0
micromhos/cm). If such high quality water is not available in the laboratory, it may be
purchased from commercial suppliers; the laboratory should request a list of quality specifi-
cations for water purchased and periodically check actual quality against these specifica-
tions.
• Chemicals and reagents: "Analytical reagent grade" (AR) chemicals should be used for
most analyses. Consult the 14th edition of "Standard Methods for the Examination of
Water and Wastewater" (published in 1975 by the American Public Health Association)
section 102, page 5-8 (or the latest edition published) for more detailed information on
reagent grades. Individual analytical procedures in "Standard Methods" often specify
special requirements for reagents to be used.
• Storage of radioactive standards and radioactive wastes: There should be an enclosed and
properly labeled area, either within the analytical laboratory or in a separate room, for the
safe storage (in suitable containers) of standards, samples, and radioactive wastes.
• Standards and sample preparation: There should be a designated area within the laboratory
for preparation of radioactive standards and samples. Adequate precautions should be taken
in this area to ensure against radioactive contamination. Provisions should be made for safe
storage and disposal of radioactive wastes and for monitoring of the work area.
RADIOCHEMISTRY (MINIMUM REQUIREMENTS)
Table VI-1 gives the minimum requirements for sample handling including preservation,
methodology, and major instrumentation.
QUALITY CONTROL
Minimum Requirements
Quality control data and records must be available for inspection.
Laboratory must participate at least twice each year in those EPA laboratory intercomparison
71
-------
Table VM.-Sa/np/e handling, preservation, methodology1 and major instrumentation (minimum requirements)
Parameter Preservative2 Container3 Instrumentation4
Gross alpha
Gross beta
Strontium-89
Strontium-90
Radium-226
Radium-228
Cesium-134
lodine-131
Tritium
Uranium
Photon emitters
Concl. HCI or HN03 to pH<25 I
Concl. HCI or HNO3 to pH<25
Cond. HCI or HNO3 to pH<2
Concl. HCI or HNO3 to pH<2
Cond. HCI or HNO3 to pH<2
Concl. HCI or HNO3 to pH<2
Cond. HCI to pH<2
None I
None (
Concl. HCI or HN03 to pH<2 I
Cond. HCI or HNO3 to pH<2 1
»orG
orG
orG
or G
orG
orG
orG
'orG
•%
>orG
'orG
AorB
A
A
A
A, B, or D
A
AorC
A
E
F
C
1 Federal Register, Vol. 41, No. 133, July 9,1976.
2 It 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 con-
tainer) may be delayed for a period not to exceed 5 days. A minimum of 16 hours must elapse between acidification and analysis.
P = Plastic, hard or soft; G = Glass, hard or soft.
4A" Low background proportional system; B = Alpha scintillation system; C = Gamma spectrometer (Nal(TI) or GE(LO);
D = Scintillation cell (radon) system; E = Liquid scintillation system (section C.2.a); F - Fluorometer (section C.l.i).
slf HCI is used to acidify samples which are to be analyzed for gross alpha or gross beta activities, the acid salts must be con-
verted to nitrate salts before transfer of the samples to planchets.
studies that include each of the analyses for which the laboratory is, or wants to be, certified.
Analytical results must be within control limits described in "Environmental Radioactivity Labora-
tory Intercomparison Studies Program—FY-1977" (EPA-600/4-77-001), or in subsequent revisions.
Laboratory must participate once each year in an appropriate unknown performance 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.
Operating manuals and calibration protocols for counting instruments must be available to
analyst(s) and technician(s).
Calibration data and maintenance records on all radiation instruments and analytical balances
must be maintained in a permanent record.
The following specifications are included in minimum daily quality control:
To verify internal laboratory precision for a specific analysis, a minimum of 10-percent
duplicate analyses must be performed. The difference between duplicate measurements
must be less than two times the standard deviation of the specific analysis as described in
EPA-600/4-77-001. If difference exceeds two standard deviations, prior measurements are
suspect, calculations and procedures must be examined, and samples should be reanalyzed
when necessary.
72
-------
• When 20 or more specific analyses are performed each day, a performance standard and a
background sample must be measured with each 20 samples. If less than 20 specific
analyses are performed in any 1 day, a performance standard and a background sample must
be measured along with the samples.
• Quality control performance charts, or performance records, must be maintained.
Optional Requirements
Optional requirements include the following:
• Current service contract should be in effect on all balances.
• Class S weights should be available to make periodic checks on balances.
• Chemicals should be dated upon receipt of shipment and replaced when needed or before
shelf life has been exceeded.
• Electronics technician or service contract should be in effect for instruments.
DATA REPORTING (OPTIONAL REQUIREMENTS)
Records of radioanalyses should be kept by the laboratory for not less than 3 years. This
includes all raw data, calculations, quality control data, and reports.
Actual laboratory reports may be kept. However, all data, with the exception of compliance
check samples as detailed in section 141.33(b) of the National Interim Primary Drinking Water
Regulations, may be transferred to tabular summaries provided that the following information is
included:
• Date, place, and time of sampling; name of person who collected the sample.
• Identification of sample as to whether it is a routine distribution system sample, check sam-
ple, raw or process water sample, surface or ground water sample, or other special purpose
sample.
• Date of receipt of sample and analysis.
• Laboratory and persons responsible for performing analysis.
• Analytical technique/method used.
• Results of analysis.
ACTION RESPONSE TO LABORATORY RESULTS (MINIMUM REQUIREMENTS)
When action response is a designated laboratory responsibility, the water plant operator and
State engineer are promptly notified of unsatisfactory sample results, and a request is made for re-
sampling from the same sampling point.
73
-------
SAMPLE FORMS FOR ON-SITE EVALUATION OF LABORATORIES INVOLVED IN
ANALYSIS OF PUBLIC WATER SUPPLIES-RADIO ANALYSIS
LABORATORY:.
STREET:
CITY: STATE:
SURVEY BY:_
AFFILIATION:.
DATE:.
NOTE: Material on pages 76-89, except where indicated, are minimum requirements.
74
-------
PERSONNEL
Laboratory.
Location
Date
Evaluator
Position/title
Analyst(s)/technician(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/area)
-------
LABORATORY FACILITIES
Laboratory
Location
Date
Evaluator.
Item
Labspace (cite ft2 /person)
Bench space (linear feet)
Sink (with hot and cold running water)
Electrical services
Distilled water
Exhaust hood
Other
Available
Yes
No
Comments
76
-------
LABORATORY EQUIPMENT AND INSTRUMENT SPECIFICATIONS-GENERAL
Laboratory
Location
Date
E valuator
Item
Analytical balance
pH meter
Specific ion meter
Conductivity meter
Drying oven
Desiccator
Hot plate
Glassware
Muffle furnace
Centrifuge
Fluorometer
Number of units
Make
Model
Age
77
-------
COUNTING ROOM FACILITIES
Laboratory
Location
Date
E valuator.
Item
Available
Yes
No
Comments
Satisfactory
Yes
No
Counting area space (total ft2
Counting area isolated from
sample preparation area
Regulated electrical services
Adequate ground available
78
-------
RADON GAS-COUNTING SYSTEM
Laboratory.
Location —
Date
Evaluator.
System number
Counting instrument
Make
Model
Year
Calibration frequency1
D
W
M
Other
f^__ „
oas-c
ounting cells/system
Manufacturer of gas-counting cells
Service maintenance frequency2
Q
S
A
Other
Condition3
G
P
No
Daily, weekly, monthly.
Quarterly, semiannually, annually.
3 Good, operating but needs repair, not operating.
Are operating manuals readily available to the operator? Yes No
Are calibration protocols available to the operator? Yes — No
Are calibrations kept in a permanent control chart record? Yes — No
Are permanent service maintenance records kept on these systems? Yes — No
Satisfactory Yes — No
-------
LIQUID SCINTILLATION COUNTERS
Laboratory.
oo
o
§M*
Instrument number
Location
r>aT"
Evaluator
Sample changing
Manufacturer Model Year
Manual Automatic Capacity
Data readout
Disci imindlor channels • • ••• "• External standard Refrigeration
Channel printout
Vicnal i
123 1 2 3 Yes No Yes No
Calibration frequency1 Service maintenance frequency2 Condition3
D W M Other Q S A Other G P No
'Daily, weekly, monthly.
Quarterly, semiannually, annually.
Good, operating but needs repair, not operating.
Are manufacturer's operating manuals readily available to the operator? Yes No
Is there a calibration protocol available to the operator? Yes — No —
Are calibrations kept in a permanent control chart record? Yes — No —
Is a permanent service maintenance record kept on these instruments? Yes — No —
Satisfactorv Yes — No —
-------
WINDOWLESS GAS-FLOW PROPORTIONAL COUNTER
Laboratory
Location
Date
Evaluator.
Instrument number
Manufacturer
Model
Year
Sample changing
Manual
Automatic
Capacity
00
Counting gas
Sample dish diameter (in)
Instrument background
Alpha
Beta
Operating voltage
cpm
Operating voltage
cpm
Calibration frequency1
W
M
Other
Service maintenance frequency
Other
Condition3
No
Daily, weekly, monthly.
Quarterly, semiannually, annually.
3Good, operating but needs repair, not operating.
Are operating manuals readily available to the operator? Yes — No
Is there a calibration protocol available to the operator? Yes — No
Are calibrations kept in a permanent control chart record? Yes — No
Is a permanent service maintenance record kept on these instruments? Yes — No
Satisfactory Yes — No
-------
00
K>
THIN WINDOW GAS-FLOW PROPORTIONAL COUNTER
Laboratory
Location
Date
E valuator.
Instrument number
Manufacturer
Counting gas
Model
Year
Window density (g/cm2 )
Calibration frequency1
D
W
M
Other
Sample changing
Manual
Automatic
Instrument
Alpha
Operating voltage
cpm
Capacity
background
Beta
Operating voltage
Service maintenance frequency2
Q
S
A
Other
cpm
Condition3
G
P
No
'Daily, weekly, monthly.
Quarterly, semiannually, annually.
Good, operating but needs repair, not operating.
Are manufacturer's operating manuals readily available to the operator? Yes No
Is there a calibration protocol available to the operator? Yes No
Are calibrations kept in a permanent control chart record? Yes No
Is a permanent service maintenance record kept on these instruments? Yes No
Satisfactory Yes — No
-------
ALPHA SCINTILLATION COUNTER
Laboratory.
Location.
Date
E valuator.
00
to
Instrument number
Manufacturer
Model
Year
Alpha phosphor location
Photo tube
Samples
Calibration frequency1
D
W
M
Other
Sample changing
Manual
Automatic
Capacity
Instrument background
Operating voltage
Service maintenance frequency2
Q
S
A
Other
cpm
Condition3
G
P No
Daily, weekly, monthly.
2Quarterly, semiannually, annually.
Good, operating but needs repair, not operating.
Are manufacturer's operating manuals readily available to the operator? Yes No
Is there a calibration protocol available to the operator? Yes No
Are calibrations kept in a permanent control chart record? Yes No
Is a permanent service maintenance record kept on these instruments? Yes No
Satisfactory Yes No
-------
GAMMA SPECTROMETER SYSTEMS
Laboratory,
Location
Date
Evaluator.
System number
Detector system
Type Make Model Year Size
Analyzer system
Make Model Year Channels
Calibration frequency1 Service maintenance frequency2 Condition3
D W M Other Q S A Other G P No
Daily, weekly, monthly.
2Quarterly, semiannually, annually.
3Good, operating but needs repair, not operating.
Are operating manuals readily available to the operator?
Are calibration protocols available to the operator?
Are calibrations kept in a permanent control chart record?
Yes
Yes
Yes
Are permanent service maintenance records kept on these systems? Yes —
Satisfactory
Yes No
No
No
No
No
No
-------
GENERAL LABORATORY PRACTICES
Laboratory
Location
Date.
Evaluator.
Item
Comments
(where applicable, cite system, quality control check, adequacy of procedures)
Glassware preparation
Water quality (distilled/deionized)
Chemicals/reagents
Radioactive standards and wastes
Standards and sample preparation
Other
85
-------
SAMPLE HANDLING, PRESERVATION, METHODOLOGY, AND MAJOR INSTRUMENTATION
Laboratory
Location
Date
E val uator_
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
86
-------
METHODOLOGY
Laboratory.
Location
Date
Evaluator.
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.
Name or description of method
Method used
(Cite page and year)
FR
ASTM
EPA
Other
Frequency
Daily
Weekly
Monthly
Satisfactory
Yes
No
-------
QUALITY CONTROL
Laboratory.
Location—
Date
E valuator.
Item
Minimum requirements:
Participation in intercomparison studies
Use of unknown performance sample
Verification of samples
Use of quality control charts or records
Operation manuals and calibration
protocols available to analyst
Quality control data (including
calibration and maintenance
records) available
Optional requirements:
Service contract on balances
Use of Class S weights
Dating and replacement of chemicals
Electronics technician available or
service contracts on instruments
Done
Yes
No
Frequency
Comments
Satisfactory
Yes
No
X
88
-------
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
DATA REPORTING
Laboratory
1 oration
Pate ,
Evaluator
Comments: system(s) used, frequency, etc.
89
-------
-------
GLOSSARY
Analyst: A chemist, microbiologist, physicist, or technician who actually performs a test. The
analyst may carry out the complete test or participate jointly with other analysts. The qualifications
an analyst needs depend greatly on functions being performed.
Interim Approval: An administrative recognition to temporarily certify laboratories until EPA
establishes its program of Interim Certification. Laboratories awarded Interim Approval must be
evaluated on-site by EPA as soon as possible after the Region has been certified. (See Water Supply
Guidance to the Regional Water Supply Representatives, No. 39.)
Interim Certification: Nonregulatory recognition given to any laboratory that it meets minimal
analytical performance standards.
Interim Certification (Provisional): Qualified recognition given to any laboratory, granting a
grace period of up to 1 year to correct deficiencies.
Local Laboratory: Any laboratory under a state or EPA certification program which performs
analyses for drinking water under the Safe Drinking Water Act. A local laboratory may be a labora-
tory of the Federal, State, or local government or a private laboratory located in or out of a particu-
lar State or Region.
Minimum Requirements: Criteria which are critical to the generation of valid data. These crite-
ria describe the lowest level of capability at which the analyses can be successfully performed.
Optional Requirements: Suggested criteria which would contribute to the goal of accurate and
precise data. Optional Requirements recognize that there are equivalent and alternate criteria
equally as good or better.
Primary Enforcement Responsibility: The primary responsibility for administration and en-
forcement of primary drinking water regulations and related requirements applicable to public
water systems within a State.
Principal Laboratory: A laboratory that has major analytical capability and/or enforcement
responsibility for water supplies with respect to analytical data under the Safe Drinking Water Act.
Any Federal, State, or local government or private laboratory located in or out of a particular State
or Region may be designated a Principal Laboratory by the agency with primary enforcement re-
sponsibility.
Quality Control Samples: Known value samples distributed on a continuing basis by the EMLS's
of EPA for use as secondary check on their within-laboratory quality control programs.
State: The agency of the State government which has jurisdiction over public water systems.
During any period when a State does not have primary enforcement responsibility under section
1413 of the Safe Drinking Water Act, the term "State" means the Regional Administration, U.S. En-
vironmental Protection Agency.
91
-------
Supervisor: The chemist, microbiologist, or physicist who is directly responsible for the techni-
cal performance of analysts for a given test(s) or test area or section. The supervisor may or may not
actually perform the test operations but should be cognizant of and preferably experienced in the
test operations being performed under his direction.
92
-------
TECHNICAL REPORT DATA
(Please read Instructions on the reverse before completing)
1. REPORT NO.
EPA 600/8-78-008
2.
3. RECIPIENT'S ACCESSIOC+NO.
4. TITLE AND SUBTITLE
Manual for the Interim Certification of
Laboratories Involved In Analyzing Public
Drinking Water Supplies-Criteria & Procedures
5. REPORT DATE
May 1978
6. PERFORMING ORGANIZATION CODE
7. AUTHOR(S)
8. PERFORMING ORGANIZATION REPORT NO.
Thomas W. Stanley, Chairman - Water Supply
Quality Assurance Work Group
9. PERFORMING ORGANIZATION NAME AND ADDRESS
Office of Monitoring S Technical Support
Office of Research and Development
U.S. Environmental Protection Agency
Washington, DC 20460
10. PROGRAM ELEMENT NO.
1HD621
11. CONTRACT/GRANT NO.
12. SPONSORING AGENCY NAME AND ADDRESS
13. TYPE OF REPORT AND PERIOD COVERED
Office of Monitoring £ Technical Support
Office of Research and Development
U.S. Environmental Protection Agency
Washington, DC 20460
14. SPONSORING AGENCY CODE
EPA/600/19
15. SUPPLEMENTARY NOTES
Interim guidance for the evaluation and approval at
Laboratories analyzing public drinking water under the Safe Drinking
Water Act.
16. ABSTRACT
Section 1401(1) of the Safe Drinking Water Act (SDWA), Public Law 93-523, defines "primary drinking water regulations"
to include "quality control and testing procedures" to ensure compliance with maximum contaminant levels. Pursuant to the
Act, the National Interim Primary Drinking Water Regulations (NIPDWR), 40 CFR 141 and 142 require that for compliance
purposes, "samples" will be considered only if they have been analyzed by a laboratory approved by the State except that
measurement for turbidity and free chlorine residual may be performed by any person acceptable to the State, and the States
must establish and maintain a program for certification of laboratories conducting measurements of drinking water contami-
nants. This manual describes evaluation procedures and minimum technical requirements recommended for certifying labora-
tories analyzing public drinking water supplies. In addition to identifying requirements that are critical to the generation of
valid data, optional certification requirements have been included as guidance.
In formulating an imp'ementation strategy, EPA fully recognizes that there are many excellent State laboratory certification
programs in operation. EPA is also aware that the capabilities of State and local laboratories vary greatly, and that a phased
implementation program may be necessary to permit moving toward our goal without creating artificial impediments to the
attainment of State primacy. This manual describes how EPA will carry out a program for interim approval and certification
of its 10 Regional laboratories and principal State laboratories, States without certification programs are encouraged to use
this program as a model; States with equivalent or better certification programs are encouraged to continue and improve.
EPA welcomes any comments or suggestions that will improve this manual.
17.
KEY WORDS AND DOCUMENT ANALYSIS
DESCRIPTORS
Pollution-Water pollution, Water
supply; Sanitary engineering, envirc
engineer.; quality control; chemisti
inorganic, chemistry-organic;
radiochemistry, microbiology
b.lDENTIFIERS/OPEN ENDED TERMS
c. COSATI Field/Group
Environmental Data
Environmental
Measurements
Environmental Labs
Laboratory Certi-
fication
05A
06F 07B
12A 07C
12B 07E
13B 14B
14D
18. DISTRIBUTION STATEMENT
Release to Public
19. SECURITY CLASS (ThisReport)
unclassified
21. NO. OF PAGES
100
20. SECURITY CLASS (Thispage)
unclassified
22. PRICE
EPA Form 2220-1 (9-73)
-------
-------
-------
United States
Environmental Protection
Agency
Environmental Research
Information Center (TIOS)
Cincinnati OH 45268
Postage and Fees Paid •
Envirnomental Protection Agency
EPA 335
Official Business
Penalty for Private Use $300
Third-Class
If your address islncorrect, please change on the above label;
tear off; and return to the above address.
If you do not desire to continue receiving this technical report
series, CHECK HERE D; tear off label, and return it to the
above address.
------- |