United States       Office of          October 1 982
             Environmental Protection   Drmkinq Water (WH-550)    EPA-570/9-82-002
             Agency          Washington DC 20460
&EPA       Manual for the
             Certification of Laboratories
             Analyzing Drinking Water

             Criteria and Procedures
             Quality Assurance

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Disclaimer
This manual has been reviewed by the
Office of Drinking Water and the Office of
R- Ch and Development and approved
for publication. The mention of commercial
products does not constitute endorsement
by the U.S. Environmental Protection
Acknowledgments
This manual was prepared through the
efforts of many individuals. These included
representatives from USEPA program
offices and laboratories. Regional Offices.
States, and utility laboratories. The princi-
pal contributors are listed below.
Drinking Water Laboratory Certification
ImplementatIon Work Group (DWLCI)
P. Berger. Chairman. 00W
R. Bordner, EMSL-Ct
B. Carroll. Region IV
T. Covert. EMSL-Cl
R. Cothern, 00W
J. Downey, Alabama
C. Gesalman. OWEP (OW)
M. Gomez-Taylor. 00W
A. Greenberg, California
G. Hicks. Cincinnati Water Works
J. Longbottorn. EMSL-Cl
H. Nash. MERL(ORD)
J. Pfaff. EMSL-Cl
I. Pomerantz. ODW
T. Ray. Region VI
L Resi, 00W
T. Stanley. QAMS (ORD)
R. Thomas. ODW
E.Whittaker, EMSLLV
J. Winter. EMSL-C1
DWLCI Work Group. Chemistry
3. Longbottom. Chairman, EMSL-Cl
U. Gomez Taylor. 00W
G. Hicks, Cincinnati Water Works
3. Lichtenberg, EMSL-Cl
L Lobring, £MSL-Cl
G. Md(es. EMSL-O
3. Pfaff. EMSI-CI
I Pomerantz 00W
DWLCI Work Group. Radiochemi
Subcommfttee
E. Whittaker, Chairman. EMSL-LV
R. Cothern. 00W
D. Easterly. EMSL-LV
A. Jarvis. EMSL-LV
H. Krieger. EMSL-Cl
G. Uyesugi. California
Other Major Contributors
R. Booth, EMSL-Cl
J. Cotruvo, 00W
E. Geldreich. MERL
C. Hendricks. OEPER (ORD)
W. Lappenbusch. ODW
M. Owens, EMSL-CI
DWLCI Work Group. Microbiology
Subcommittee
H. Nash. Chairmen. MERL(ORD)
P. Berg.r. 00W
0. Bordner. EMSL-Cl
T. Covert. EMSL-Ct
3. Stan*idge, Wisconsin
3. Williams. Arizona
J. Winter, EMSL-Cl
I

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United States         Office of           October 1982
Environmental Protection    Drinking Water (WH-550)    EPA-570/9-82-002
Agency            Washington DC 20460
Manual for the
Certification of Laboratories
Analyzing Drinking Water
Criteria and Procedures
Quality Assurance
Prepared by
The Drinking Water Laboratory Certification Implementation
WorkGroup
Supersedes EPA 600/8-78-008. May 1978, entitled Manual for the Interim Certification
of Laboratories Involved in Analyzing Public Drinking Water Supplies

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Preface
This document is a revision of the Manual
for the Interim Certification of Labora-
tones Involved in Analyzmg Public Drink-
ing Water Supplies, EPA 600/8-78-008. It
was prepared by the Drinking Water Labo-
ratory Certification Implementation Work
Group in an effort to update and improve
technical criteria and implementation
strategy in light of newly approved method-
olo9y and over four years of experiencewith
the program. The technical criteria for
chemistry, microbiology, and radiochemistry
have been updated, clarified, and reorgan-
ized, but are similar in substance to the
earlier edition of the manual. Implementa-
tion policy is very similar to the earlier
edition, but “Interim Approval” status has
been eliminated and the term “Interim
Certification” has been changed to “Certifi-
cation.” In addition, the program now in-
cludes criteria and procedures for down-
grading a laboratory’s certification status.
Comments from the Regions and States
were solicited and considered in the prepa-
ration of this revised manual. These in-
cluded recommendations from a workshop
held in June 1981, in which all Regions and
States were invited to participate and share
their views with respect to both the techni-
cal criteria and implementation policy.
Almost all majority views at that workshop
were incorporated into this manual.
There is a U.S. EPA quality assurance
program which covers all activities relating
to data collection, processing, and report-
ing. This is managed by the Quality Assur-
ance Management Staff (QAMS), the Office
of Research and Development. The portion
of the QAMS program applicable to labora-
tories conducting drinking water analyses is
indicated in Chapter III (Quality Assurance
Plan.)
Like the previous edition, this program is
not regulatory in nature (except for method-
ology), but rather is guidance describing the
minimum procedures and criteria for assur-
ing data validity.
Contents
Chapter I: Introduction 1
Chapter II: Responsibilities 2
Office of Drinking Water 2
Office of Research and Development -. . 2
US EPA Regional Offices . : .. 7.7 7T -; 7 T
Drinking Water Laboratory Certification Implementation (DWLCI) Work Group 2
Chapter Ill: Implementation of Certification Program . . .
Certification of Regional Laboratories and Programs.. . ............
Certification of State Laboratories ... . ............ 3
Certification of Local Laboratories . . - 4
Other Considerations for Certification 4
Quality Assurance Plan
Chain-of-Custody Procedures
Requirements for Maintaining Certification Status. 4
Criteria and Procedures for Downgrading/Revoking Certification Status 5
Reciprocity ...... ...... .. ................
Training 5
Technical Services 5
Reference Samples
Early Warning System for Problems with Test Supplies and Equipment
Alternate Analytical Techniques 6
Chapter IV: Chemistry ............_ .. ..
Critical Elements for Certification 9
Recommended Practices 14
Chapter V: Microbiology.. ...... . .. ............ .. .
Critical Elements for Certification 27
Recommended Practices 3
Chapter VI: Radiochemistry . - - .--
Critical Elements for Certification . 39
Recommended Practices 41
Appendices
AppendixA: Chain-of-Custody 54
Appendix B: Recommended Protocol for Regions Conducting bn-site Laboratory Evaluations... 57
Appendix C: Abbreviations ..

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Chapter I
I ntroduction
P ublic water systems serving 25 persons
or more must conform with the provi-
sions of the Safe Drinking Water Act, as
amended (42 U.S.C. S 300f et seq.), and the
requirements of the National Interim Pri-
mary Drinking Water Regulations (NIPDWR)
(4OCFR 141 and 142). Section 1401 (1)(D)
of the Act defines a primary drinking water
regulation as consisting of “criteria and
procedures. . . including quality control
and testing procedures to insure compli-
ance
The Regulations at 40 CFR 141 .28 re-
quire that all testing for compliance pur-
poses, except for turbidity, free chlorine
residual, temperature, and pH, be per-
formed by laboratories approved by either
the U.S. EnviLonmental Protection Agency
(U.S. EPA) or Those States with primary en-
forcement responsibility (primacy). This
manual is intended to assist in the imple-
mentation of Section 141.28 by providing
a mechanism for the evaluation of these
laboratories in order to help assure the
validity of data generated.
The U.S. EPA program extends to its Re-
gional laboratories, principal State and
Territorial laboratories in primacy States,
laboratories on Federal Indian reservations,
and laboratories in States without primacy
which perform analyses under the Safe
Drinking Water Act.
Primacy States must have a certification
program for local laboratories if all analyses
are not performed in principal State labora-
tories (see Table 1-1), and should adopt
provisions at least as stringent as those in
this manual for certifying these laborato-
tories.
The certification program operates as
follows: U.S. EPA’s Environmental Monitor-
ing and Support Laboratory in Cincinnati,
Ohio (EMSL-Cl), is responsible for deter-
mining the certification status of U.S. EPA
Regional laboratories for microbiology and
for chemistry. The Environmental Monitor-
ing Systems Laboratory in Las Vegas
(EMSL-LV) has this responsibility for radio-
chemistry. Regional certification officers
determine the certification status of princi-
pal State laboratories in primacy States and
are also responsible for local laboratories in
non-primacy States. Evaluations of State
laboratories for radiochemistry are con-
ducted by EMSL-LV, except where the
Regions have this capability.
Primacy States with certification programs
are responsible for certifying local laborato-
ries. Regional laboratories and principal
State laboratories must successfully ana-
lyze a complete set of unknown perform-
ance evaluation (PE) samples annually from
EMSL-Cl (EMSL-LV, where applicable) and
pass an on-site evaluation every three
years. The criteria given herein will be used
at the on-site evaluation.
Chapter II describes the responsibilities of
each of the U.S. EPA organizations for this
certification program. Chapter Ill describes
how the program will be operated. Chapters
lv, V, and VI cover the technical criteria for
chemistry, microbiology, and radiochemis-
try, respectively, used during an on-site
evaluation of a laboratory. The technical
criteria for each of Chapters IV, V, and VI
are divided into two sections: Critical Ele-
ments for Certification and Recommended
Practices. The first section details items
which are essential for the certification of
laboratories performing drinking water
analyses under the Safe Drinking Water
Act. The second section contains items
which are highly recommended for good
laboratory operaiions. Only the first section
will be used to determine certification
status. Evaluation forms are also included
in Chapters IV, V. and VI.
The appendices include recommended
chain-of-custody procedures, a recom-
mended protocol and format for conducting
on-site laboratory evaluations, which may
be used by the evaluators, and abbrevia-
tions.
All specifications, whether critical or
recommended, are guidance, except for
those methods and procedures specified in
the NIPDWR (see 40 CFR, Part 141) as
mandatory. Laboratories wishing to use an
alternative method to those prescribed
must first obtain U.S. EPA approval in accord-
ance with the established procedure out-
lined in Chapter III. Alternate Analytical
Techniques. The U.S. EPA may approve alter-
nate test procedures on either a case-by-
case basis or on a nationwide basis.
Table I-i. Requirements of Primacy
To obtain and maintain primary enforcement
responsibility (primacy), a State must conform
to the following provisions of 4.0 CFR 142.10
(b):
(3) The establishment and maintenance of
a State program for the certification of labora-
tories conducting analytical measurements of
drinking water contaminants pursuant to the
requirements of the State primary drinking
water regulations including the designation
by the State of a laboratory officer, or officers.
certified by the Administrator, as the official(s)
responsible for the State’s certification pro-
gram. The requirements of this paragraph
may be waived by the Administrator for any
State where all analytical measurements
required by the State’s primary drinking water
regulations are conducted at laboratories
operated by the State and certified by the
Agency. Until such time as the Agency estab-
lishes 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 Admin-
istrator and capable of performing analytical
measurements of all contaminants specified
in the State primary drinking water regula-
tions.
1

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Chapter U
Responsibilities
T he success of the laboratory certification
program depends upon cooperation
among the organizations responsible for its
implementation. This is achieved primarily
through the Drinking Water Laboratory
Certification Implementation Work Group
(DWLCI). Within the Agency, primary re-
sponsibilities for laboratory certification are
shared by the Office of Drinking Water
(ODW). the Office of Research and Develop-
ment(ORD). and the U.S. EPA Regional Of-
ces.
Office of
Drinking Water
ODW is responsible for supervising the
national certification program for laborato-
ries analyzing drinking water samples and
for implementing the Safe Drinking Water
Act, including the preparation of regula-
tions and standards.
Office of Research and
Development
The EMSLs at Cincinnati and Las Vegas
share responsibility with ODW in develop-
ing and implementing the laboratory certif i-
cation program.
EMSL-Cl is the lead organization for oper-
ational control of the national ce,-tification
program for laboratories performing chemi-
cal and microbiological analyses. EMSL-Cl:
• Reviews Regional certification programs
and conducts on-site evaluations of all
Regional laboratories every three years;
• Prepares and distributes unknown PE
samples and known quality control (QC)
samples for all regulated chemical and
microbiological contaminants;
• Conducts water supply performance
evaluation studies at least annually for all
Regional and principal State laboratories,
and laboratories in non-primacy States
wishing certification. Other laboratories
may participate;
• Evaluates the resources and personnel
available in each U.S. EPA Region to carry
out the certification program;
• Participates in all DWLCI Work Group
activities;
• Develops and participates in training
courses to support the certification program
(if resources are available); and
• Provides technical assistance, as re-
quired.
EMSL-LV is the lead organization for
operational control of the certification pro-
gram for laboratories performing radio-
chemical analyses. Its duties correspond
with those described for EMSL-Cl. In addi-
tion, at the request of a Region, EMS L-LV is
responsible for conducting on-site inspec-
tions for radiochemistry capability of princi-
pal State laboratory systems and, if re-
sources are available, other laboratories not
covered by State certification programs. In
these cases, EMSL-LV will report the re-
sults of its inspection to the responsible
Regional Administrator, who will have final
authority to determine certification status.
U.S. EPA
Regional Offices
The ten Regions are responsible for over-
seeing progress of the certification program
in the States. The Regions:
• Monitor the adequacy of State programs
for certifying laboratories;
• Evaluate the certification status of princi-
pal State laboratories and laboratories in
non-primacy States. This includes an on-
site inspection at least once every three
years. The Regional Administrator is certify-
ing authority;
• Coordinate EMSL water supply perform-
ance evaluation studies with laboratories in
the Region;
• Participate in the annual review of certifi-
cation programs and performance evalua-
tion reports;
• Provide technical assistance to U.S. EPA-
certified drinking water laboratories, as
needed;
• Operate the certification program in non-
primacy States;
• Insure that the Regional laboratory con-
tinually maintains its capability of meeting
all certification criteria; and
• Maintain a current list of the certification
status of all laboratories in the Region certi-
fied by U.S. EPA or the States.
In non-primacy States, the Region, in
addition to its laboratory certification duties,
has administrative, enforcement, and local
laboratory certification responsibilities
normally performed by the State. Some of
these duties may be performed by the State,
but the Region must retain responsibility for
the on-site evaluation of the designated
principal State laboratory. Local laborato-
ries may be evaluated by the Region or
under a Region-approved program carried
out by a designated principal State labora-
tory. In either case, this manual shall pro-
vide the basis for the on-site evaluation.
Drinking Water Laboratory
Certification Implementation
Work Group
The DWLCI Work Group was established to
oversee the operation of the national certifi-
cation program for drinking water laborato-
ries. This group advises ODW and includes
representatives from ODW. ORD (EMSL-CI.
EMSL-LV. MERL and QAMS), Office of
Water Enforcement and Permits, Region&
Offices, and States. The DWLCI Work
Group:
• Mcnitors the certification program and
recommends technical and administrative
revisions to ODW as dictated by experience
or updated information;
• Develops guidance and responds to ques-
tions and comments from the States and
Regions;
• Develops technical and administrative
criteria to support additional certification
needs imposed by future regulations;
• Ascertains laboratory availability and
capability for future regulatory activities;
and
. Makes recommendations to ODW on
resources needed to implement the certif i-
cation program.

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Chapter III
Implementation of
Certification Program
Certification of Regional
Laboratories and Programs
E MSL-Cl is responsible for certifying the
Regional laboratory, if one exists, for
microbiological and chemical analyses, and
for approving the Regional program for
certifying other laboratories for these pa-
rameters. EMSL-LV has similar responsi-
bilities for a Region having radiochemistry
capability. The Regional certification pro-
gram must be approved before a Region can
exercise its authority to certify other labora-
tories.
Certification of Laboratories
Regional laboratories analyzing potable
water samples under the Safe Drinking
Water Act must meet the minimum criteria
specified in this manual, pass an on-site
inspection at least once every three years.
and satisfactorily analyze an annual set of
PE samples. For those Regions certified for
radiochemistry, satisfactory performance
on two cross check samples per year is also
necessary.
Individual(s) Responsible for Certification
Program
The U.S. EPA Region must designate an
individual(s) to coordinate drinking water
certification activities. This individual(s)
must be experienced in quality assurance;
hold an advanced degree or have equivalent
experience in microbiology, chemistry, or
radiochemistry; and have sufficient admin-
istrative and technical stature to be con-
sidered a peer of the director of the principal
State laboratory.
On-Site Evaluation Team
One or more teams must be established by
the Region to evaluate a laboratory in
microbiology and chemistry. Team mem-
bers must be experienced professionals.
holding at least a bachelor’s degree (or
equivalent education and experience) in the
specific discipline being evaluated. Team
members must participate in training activi-
ties as specified by EMSL-Cl.
Development of Regional Plans for
Certifying Local Laboratories in Non-
Primacy States
Regions are required to develop plans for
certifying local drinking water laboratories
in non-primacy States. Written plans
should include the following:
• Certification official;
• Types and numbers of laboratories;
• Analyses to be examined;
• Schedule for on-site evaluations; and
• Plans for providing technical assistance
to laboratories in need of upgrading.
Certification of
State Laboratories
The principal State laboratory system must
have the capability to analyze every param-
eter included in the drinking water regula-
tions(40 CFR 142.10(b) (4)); however, an
individual laboratory which is part of a
principal State laboratory system may be
certified for only one, several, or all the
cited analyses. If a principal State labora-
tory contracts with another laboratory,
including a laboratory outside the State, to
assume the lead role in analyzing a regu-
lated parameter (e.g., radiochemical con-
taminants), that contract laboratory will, for
the purposes of this manual, be considered
part of the principal State laboratory sys-
tem. In this case, the contract laboratory
must be certified either by U.S. EPA or by the
State in which the laboratory is located for
the contaminants of interest. In the latter
case, the State must have primacy.
The certification process for a principal
State laboratory or a local laboratory in a
non-primacy State will begin when the
laboratory director makes a formal request
to the Region. This application may result
from the following:
• A request for first-time certification for
microbiology, chemistry and/or radio-
chemistry;
• A request for certification to analyze
additional or newly regulated parameters;
• A request to renew a laboratory’s certifi-
cation status after three years; and
• A request to reapply for certification after
correction of deficiences which resulted in
the downgrading/revocation of certification
status.
The Region should respond to a formal
application for any of the requests within 30
days, and a mutually agreeable date and
time should be set for the on-site laboratory
evaluation. The recommended protocol for
conducting these evaluations is given in
Appendix B. For certification, a laboratory
must pass an on-site inspection and satis-
factorily analyze performance evaluation
samples for those parameters for which it
requests certification.
After the on-site visit and the review of
PE sample results, the Region can classify
the laboratory for each type of analysis
according to the following ranking scheme:
• Certified—a laboratory that meets the
minimum requirgments of this manual. The
certification shall be valid for up to three
years.
• provisionally Certified—a laboratory
which has deficiencies but can still produce
valid data.
• Not Certified—a laboratory possessing
major deficiencies and, in the opinion of the
Regional Administrator, cannot consistently
produce valid data.
In the case of laboratories classified as
Provisionally Certified, up to one year will
be permitted for correction of the deficien-
cies. A one-time extension of no more than
6 months may be considered by the Region
as long as the laboratory is making “good
faith” progress in the resolution of its de-
ficiencies and the continued provisional
status does not impact the generation of
valid data. A Provisionally Certified labora-
tory may analyze drinking water samples for
compliance purposes. In no case should
provisional certification be given if the
evaluation team believes that the laboratory
lacks the capability of performing the anal-
ysis within specified limits. Once deficien-
cies have been corrected to the Regional
Administrator’s satisfaction, the latter
should upgrade the laboratory to Certified
status.
3

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For laboratories requesting first-time
certification or certification to analyze addi-
tional or newly-regulatedparameters, the
Region, at its discretion, may administra-
tively grant a laboratory Provisionally Certi-
fied status, pending an on-site evaluation. It
is granted only when the Region judges that
the laboratory has both the appropriate
instrumentation and trained personnel to
perform the analyses, and the laboratory
has satisfactorily analyzed PE samples for
the contaminants in question.
For those Regions lacking the expertise
required to certify laboratories in radio-
chemistry, EMSL-LV will conduct on-site
inspections.
Certification of
Local Laboratories
For the purposes of this document, local
laboratories include any State, county,
municipal, utility, Federal, or commercial
laboratory, but excludes principal State
laboratories and U.S. EPA Regional labora-
tories. In non-primacy States, the Regions
will certify local laboratories, using the
criteria and policies in this manual.
Only primacy States where not all drink-
ing water analyses are conducted at State-
operated laboratorlesaje required toes-
tablish a certification program for !ocal
laboratories (see 44) CFR 142.10(b), Table
I-i .). All States, however, are encouraged to
develop such programs. Certification must
be based upon criteria contained in this
manual or State-developed equivalents at
least as stringent as those herein. Those
States required by regulation to develop a
certification program must appoint a labora-
tory certification officer(s), certified by the
Region, as the official(s) responsible for the
State program.
The principal State laboratory system
must have the technical capability to ana-
lyze for all regulated contaminants. If the
principal State laboratory has the resources
to perform 100% of the analyses for one
contaminant (e.g.. lead), but does not have
adequate resources to perform 100% of the
analyses for another contaminant (e.g.. can
only analyze 20% of all total coliform sam-
ples). then the State certification program
need only include certification criteria for
contaminants for which the State will not
be analyzing 100% of the samples.
Federal facilities must comply with all
Federal, State and local requirements with
respect to the Safe Drinking Water Act. For
the purpose of certification, Federal labora-
tories in which routine monitoring of public
drinking water supplies is conducted are to
be considered local laboratories. The agen-
cy with primary enforcement authority,
either the State or the Region, will be re-
sponsible for carrying ourtertification activ-
ities. If requested by the State, the Region
may conduct on-site evaluations of Federal
laboratories in that State. U.S. EPA will have
primary enforcement authority over any
facilities on Federal Indian lands.
Other Considerations for
Laboratory Certification
Quality Assurance Plan
It is essential that all laboratories analyzing
drinking water compliance samples adhere
to defined quality assurance procedures.
This is to insure that routinely generated
analytical data are scientifically valid and
defensible and are of known and acceptable
precision and accuracy. To accomplish
these goals, each laboratory should prepare
a written description of its quality assur-
ance activities (a GA Plan). The following
items should be addressed in each QA plan:
I Sampling procedures.
2 Sample handling procedures.
— specify procedures used to maintain
integrity of all samples, i.e., tracking sam-
ples from receipt by laboratory through
analysis to disposal.
— samples likely to be the basis for an
enforcement action may require special
safeguards (see Chain-of-Custody proce-
dures).
3 Instrument or equipment calibration
procedures and frequency of their use.
4 Analytical procedures.
5 Data reduction, validation and reporting.
— data reduction: conversion of raw data
to g/L picocuries/L coliforms/100 mL,
etc.
— validation: includes insuring accuracy of
data transcription and calculations.
— reporting: includes procedures and
format for reporting data to utilities, State
officials, and U.S. EPA.
6 Types of internal quality control (QC)
checks and frequency of their use.
— may include preparation of calibration
curves, instrument calibrations, replicate
analyses, use of EMSL-provided QC sam-
ples or calibration standards and use of QC
charts.
7 Preventive maintenance procedures and
schedules.
QC chart for chemistry is explained in Hand-
book for Analytical Quality Control in Water
and Wastswatsr Laboratories, EPA-600/4-79-
019, March 1979. OC chart for radiochemistry is
explained in Handbook for Analytical Quility
Control in Radio.nalytical Laboratories. EPA-
600/7-77-088. August 1977.
8 Specific routine procedures used to de-
termine data precision and accuracy for
each contaminant measured.
— precision is based on the results of repli-
cate analyses.
— accuracy is normally determined by
comparison of results with “known” con-
centrations in reagent water standards and
by analyses of water matrix samples before
and after adding a known contaminant
“spike”.
9 Corrective action contingencies.
— response to obtaining unacceptable
results from analysis of PE samples and
from internal QC checks.
The QA plan may consist of already avail-
able standard operating procedures (SOPs),
which are approved by the laboratory direc-
tor and which address the listed items, or
may be a separately prepared GA docu-
ment. Documentation for many of the listed
GA plan items can be by reference to appro-
priate sections of this manual, the labora-
tory’s SOPs or to other literature (e.g.,
Standard Methods for the Examination
of Water and Wastewater).
If a particular listed item is not relevant,
the GA plan should state this and provide a
brief explanation (e.g.. some laboratories
never collect samples and thus have no
need to describe sampling procedures). A
laboratory GA plan should be concise but
responsive to the above-listed items (a
maximum of five pages is suggested). Mini-
mizing paperwork while improving depend-
ability and quality of data are the intended
goals.
Chain-of-Custody Procedures
Certified laboratories which may be re-
quested to process a sample for possible
legal action against a supplier must have a
chain-of-custody procedure available. An
example of such a procedure is found in
Appendix A.
Requirements for Maintaining
Certification Status
Periodic Performance Evaluation (PE)
Samples
Certified drinking water laboratories must
satisfactorily analyze PE samples on an
annual basis for each chemical, radio-
chemical, or microbiological parameter
(when available) for which certification has
been granted. Results must be within the
acceptance limits established by U.S. EPA for
each analysis. To maintain certification in
radiochemistry, the laboratory must satis-
factorily analyze two cross check samples
per year in addition to the annual set of PE
samples.

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Methodology
Laboratories must use methodologies sanc-
tioned by the drinking water regulations (40
CFR 141.21 - 141 .25)or otherwise ap-
proved by U.S. EPA for compliance with the
Sate Drinking Water Act.
Notification of Certifying Authority (CA)
for Major Changes
Laboratories must notify the appropriate CA
(Region al Administrator or the appropriate
EMSL), in writing, within 30 days of major
changes in personnel, equipment, or labo-
ratory location which might impair analyti-
cal capability. A major change in personnel
is defined as the loss or replacement of the
laboratory supervisor or a situation in which
a trained and experienced analyst is no
longer available to analyze a particular
parameter for which certification has been
granted. The CA will discuss the situation
with the laboratory supervisor and establish
a schedule for the laboratory to rectify de-
ficiencies.
On-Site Evaluation
The CA must be satisfied that a laboratory is
maintaining the required standard of quali-
ty for certification. Normally, this will be
based upon recommendation of a U.S. EPA
on-site evaluation conducted at least every
three years.
Criteria and Procedures for
Downgrading! Revoking
Certification Status
I Criteria for Downgrading Certification
Status
A laboratory may be downgraded to a Pro-
visionally Certified status for a particular
contaminant analysis for any of the follow-
ing reasons:
1. Failure to analyze a PE sample (or an
EMSL-LV cross check sample) within the
acceptance limits established by U.S. EPA. If
more than one concentration of a particular
contaminant is provided, the laboratory
must satisfactorily analyze all concentra-
tions, except where otherwise stated. After
downgrading to a Provisionally Certified
status, a laboratory may request that U.S
EPA çrovide QC samples (standard solution
samples for radiochemical contaminants)
and technical assistance to help identify
and resolve the problem. Provisionally Cer-
tified status will continue until the labora-
tory’s analysis of a follow-up PE sample (or
EMSL-LV cross check sample) produces
data within the acceptance limits estab-
lished by U.S. EPA.
2. Failure of a certified laboratory to notify
the CA within 30 days of major changes in
personnel, equipment, or laboratory loca-
tion which might impair analytical capa-
bility.
3. Failure to satisfy the CA that the labora-
tory is maintaining the required standard of
quality, based upon an U.S. EPA on-site eval-
uation.
During the provisional status period, which
may last for up to one year with a possible
six month extension, the laboratory may
continue to analyze samples for compliance
purposes until it resolves its difficulties. It
must, however, notify its clients of its
downgraded status.
Criteria for Revoking Certification Status
A laboratory may be downgraded from
Certified or Provisionally Certified status to
a Not Certified classification for a particular
contaminant analysis for the following
reasons:
1. Failure to analyze an initial and follow-
up PE sample (or EMSL-LV cross check
sample) for a particular contaminant within
the acceptance limits established by U.S. EPA.
2. Failure to correct identified deviations
(including continued use of unapproved
methods and equipment) by the time speci-
fied by the CA.
3. Submission of a PE sample to another
laboratory for analysis and reporting data as
its own.
4. Falsification of data or other deceptive
practices.
Procedures for Revocation
The CA will notify the laboratory in writing
(registered or certified mail) of the intent to
revoke certification. If the laboratory wishes
to challenge this decision, a notice of appeal
must be submitted in writing to the CA
within 30 days of receipt of the notice of
intent to revoke certification. If no notice of
appeal is so filed, certification will be re-
voked.
The notice of appeal must be supported
with an explanation of the reasons for the
challenge and must be signed by a respon-
sible official from the laboratory such as the
president/owner for a commercial labora-
tory, or the laboratory supervisor in the case
of a municipal laboratory.
Within 60 days of receipt of the appeal,
the CA will make a decision and notify the
laboratory in writing. Denial of the appeal
results in immediate revocation of the
laboratory’s certification. The CA will re-
quest the laboratory to notify its clients of
its status in writing, and to submit verifica-
tion that this has been accomplished. Once
certification is revoked, a laboratory may
not analyze drinking water samples for
compliance purposes until its certification
has been reinstated.
If the appeal is determined to be valid, the
CA will take appropriate measures to re-
evaluate the facility and to issue to the
laboratory within 60 days a written decision
on its certification status.
Reinstatement of Certification
Certification will be reinstated when and if
the laboratory can demonstrate to the CA’s
satisfaction that the deficiencies which
produced Provisionally Certified status or
revocation have been corrected. This may
include an on-site evaluation, a successful
artalysis of samples on the next regularly
scheduled EMSL water supply performance
evaluation study, or any other measure the
CA deems appropriate.
Reciprocity
Reciprocity, which is defined as mutually
acceptable certification among Regions and
States, is endorsed by U.S. EPA as a highly
desirable element in the certification pro-
gram for drinking water laboratories. States
are encouraged to adopt provisions in their
laws and regulations to permit it. States
may request U.S. EPA to arbitrate disputes
involving reciprocity. Data from U.S. EPA-
certified laboratories will be acceptable
under the Safe Drinking Water Act in juris-
dictions where U.S. EPA has primary enforce-
ment responsibility.
Training
Training functions are no longer provided in
support of U.S. EPA’s laboratory certification
program. Training, however, is an integral
part of the laboratory certification process
for: a) personnel responsible for certifying
laboratories either on behalf of the Regional
Office or a primacy State; b) the laboratory
analysts responsible for microbiological,
chemical, and radiochemical measure-
ments. Mechanisms for providing adequate
training should be examined by primacy
agencies or other groups.
Technical Services
Reference Samples
There are four types of EMSL reference
samples: calibration standards, quality
control (QC), performance evaluation (PE),
and intercomparison cross check samples.
EMSL-Cl provides QC and PE samples for
all regulated chemical and microbiological
contaminants and residual chlorine, and in
addition, provides calibration standards for
trace organic chemicals. EMSL-LV provides
calibration standards, PE samples, and
intercomparison cross check samples for all
regulated radiochemical contaminants.

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QC samples and standards are provided
on request as part of a laboratory S own
quality assurance activities (see section on
Quality Assurance Plan). Contaminant
concentrations are furnished. They serve as
independent checks on reagents, instru-
ments, and analytical techniques; as an aid
for testing or training analysts; or for deter-
mining within laboratory precision and
accuracy. Although no certification or other
formal U.S. EPA evaluation functions result
from using these samples, their routine use
is considered fundamental to a proper
laboratory QA plan.
EMS L-Cl and EMS L-LV conduct periodic
water supply performance evaluation
studies using PE samples as a requirement
for certification. In contrast to QC samples
and calibration standards, contaminant
concentrations are not furnished before
analysis. Laboratories should request PE
samples through the appropriate Regional
Office for chemistry and microbiology, or
EMSL-LV for radiochemistry.’
At the conclusion of each study, the
EMSLs prepare individual reports for each
laboratory and provide them to the partici-
pants. The certifying authority reviews
unacceptable data with the laboratory to
identify and resolve problems. QC samples
and calibration standards are useful for this
purpose. Once problems are corrected, the
laboratory must analyze a second series of
PE samples for problem parameters during
a follow-up EMSL study.
In addition to the annual PE sample re-
quirement, EMSL-LV also requires satisfac-
tory performance in two intercomparison
cross check studies per year. lntercompari-
son cross check samples differ from PE
samples in that the former contain only one
or two radionucl ides (e.g.. radium-226 and
radium-228), while PE samples for radio-
chemistry are complex mixtures of alpha,
beta, and photon-emitting radionuclides. In
neither case are contaminant concentra-
tions furnished to the laboratory until after
completion of the study.
Early Warning System for Problems With
Test Supplies and Equipment
A voluntary national system has been es-
tablished to (1) identify potential problems
with chemical and microbiological test
materials and equipment (2) notify the
U.S. EPA. manufacturers, and users of these
problems; and (3) encourage improvements
and tighter quality control over the prod-
ucts. The problems are concerned with
performance, QA, specification, design, and
labeling of microbiological media and mem-
brane filters, chemical reagents, and other
supplies, equipment, and instrumentation
EMSL-LV ad&ess is U.S. EPA/EMSL P.O. Box
15027, Las Vegas, Nevada 89114
used in microbiological and chemical anal-
yses of drinking water. EMSL-Cl has the
responsibility for maintaining a QA program
on methodologies and test materials, and
serves as the focal point for identifying and
reporting significant problems with such
materials to the users and the manufac-
turers. The following protocol is used:
1. State and local drinking water laborato-
ries or Regional staff members should
report microbiological and chemical prob-
lems by phone or in writing to the Micro-
biology Section (513-684-7319) or the
Physical and Chemical Methods Branch
(513-684-7306), respectively, of EMSL-Cl,
USEPA, 26W. St. Clair St., Cincinnati, Ohio
45268. Forms for written reports are pro-
vided in Figures Ill-i and 111-2. A copy of the
report should be sent to the QA Officer in
the appropriate Region.
2. EMSL-Cl will record the details of the
problem, including name and location of the
reporting laboratory; product type, manu-
facturer, lot/catalog/model numbers and
date received; description of the problem;
specific observations; method of prepara-
tion, and length and conditions of storage
for media or reagents; and data document-
ing unacceptable test results.
3. EMSL-Cl will then describe the reported
problem to the manufacturer, obtain manu-
facturing and QA data, and discuss its sig-
nit icance. Corrections or changes by the
manufacturer will be encouraged.
4. Based on the results of discussions with
the reporter(s) of the problem and the man-
ufacturer, EMSL-Cl will alert the Regional
QA Officers of possible problems with the
product. The QA Officers will alert the
appropriate U.S. EPA and State personnel.
This system is not intended to label the
media, reagents, or other materials as
unacceptable, but rather to alert water
laboratories that a problem may exist and to
determine if similar problems have been
observed elsewhere.
5. If multiple reports of the same problem
are received, EMSL-CI will inform the man-
ufacturer of a potentially broad-scope prob-
lem and request samples from reporting
laboratories for testing.
6. If the product is unsatisfactory in these
tests, EMSL-Cl will notify the manufacturer
and the Regional QA Officers who, in turn,
will notify the Regional, State, and local
authorities.
Alternate Analytical
Techniques
Section 141.27 of the NIPDWR permits
approval of alternate analytical techniques.
Such a technique, also known as an alter-
nate test procedure (ATP), shall be accepted
only if it is substantially equivalent to
the prescribed test in both precision and
accuracy as it relates to the determination
of compliance with any maximum contami-
nant level.”
EMSL-Cl, through its Equivalency Staff,
is responsible for and provides coordination
of a program to determine the acceptability
of proposed techniques, and makes recom-
mendations for approval or denial to the
appropriate authority. Applications for
approval of an ATP may be made on a lim-
ited or a nationwide basis. Requests for
limited use approvals are submitted to the
appropriate Regional Administrator or
designee who, after receiving recommen-
dations from the Director of EMSL-Cl and
the Director of ODW. has the final authority
to approve requests. Requests for nation-
wide use approvals should be forwarded
directly to the Director of EMSL-Cl, who,
after review by the Equivalency Staff, will
provide recommendations to the Director of
ODW, with whom final authority for ap-
proval rests.
• Applicants who propose an ATP need to
provide a step-by-step procedure, applica-
ble literature citations or other references,
and any available comparability data be-
tween the proposed ATP and the US EPA-
approved test procedure for the same con-
taminant.
In the case of new techniques where
precision and accuracy data may not be
available to support an application, the
applicant for a limited use AlP will be asked
to provide comparability data from the anal-
ysis of samples collected from one to five
water supply systems most representative
of those routinely analyzed. From each of
these systems, three samples, in which the
concentrations range from the limit of de-
tection (LD) to the maximum contaminant
level (MCL), should be collected and each
sample analyzed eight times, four times
each, by the proposed technique and the
U.S. EPA-approved test procedure. Samples
can be spiked as necessary to cover the
concentration range between the LD and
MCL. Applicants for a nationwide ATP may
also be asked to provide comparability data.
For each of a minimum of five sources, six
samples should be collected and analyzed
eight times, four times by each technique.
The water supply sources selected must be
dispersed geographically throughout the
United States. Samples may also be spiked
as necessary to cover the concentration
range between the ID and the MCL.
The EMSL-Cl Equivalency Staff will apply
a series of proven statistical techniques to
the data submitted with all applications to
determine equivalency between the pro-
posed and the approved techniques, and
submit recommendations to approval au-
thorities.

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Figure Ill-i
Report of Problem With Microbiological Supplies or Equipment
Product*
Manufacturer
Date
Address
Date Received
Lot No. Cat. No.
Expiration Date
Model No.______________________
Description of Problem: **
Name
(Person Reporting) Phone No.
Laboratory! Facility
Address
Membrane Filters, Microbiological Media, Reagents. Portable Incubators, Waterbaths, etc.
**lnformation should include the length and condition of storage, and the method of preparation for
media and reagents. Specific observations, quality control checks, and data that document unaccept-
able results are useful in describing the problem.
Send to: Microbiology Section. EMSL-Cl, U.S. EPA, 26W. St. Clair St., cincinnati, OH 45268. or phone
(513) 684-7319.
7

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Figure 111-2
Report of Problem With Chemica
I Supplies or Equipment
Product*
Date
Manufacturer
Address
Date Received
Expiration Date
Lot No._________________________
Cat. No._________________________
Model No._____________________
Description of Problem: **
Name
Phone No._____________________
(Person Reporting)
Laboratory/Facility
Address
Chemicals. Prepared Reagents. Instruments. etc.
intormation should include the length and condition of storage, and the method of preparation for
reagents. Specific observations, quality control checks. and data that document unacceptable results
are useful in describing the problem.
Send to: Physical and Chemical Methods Branch. EMSL-Cl. U.S. EPA. 26W. St. Clair St.. Cincinnati,
OH 45268, or phone (513) 684-7306.

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chapter IV
Chemistry
Critical Elements
for Certification
he technical criteria in this chapter are
divided into two sections: Critical Ele-
ments for Certification and Recommended
Practices. Only the first section will be used
to determine certification status.
1. Personnel
Although there are no critical elements for
laboratory analysts, laboratory administra-
tors and evaluators should recognize train-
ing and experience as essential to the
acquisition of valid compliance monitoring
data. Recommended minimum standards
can be found in Recommended Practices.
2. Laboratory Facilities
There are no critical elements for certifica-
tion of laboratory facilities for chemistry.
Minimum standards are inherent to the
instrumentation required to perform the
tests. Additional recommendations may be
found in Recommended Practices.
3. Laboratory Equipment and
Supplies
Only those instruments needed to perform
the approved methodology for the contami-
nants for which the laboratory is being
certified are required. Those instruments,
‘however, must meet the following specifi-.
cations. Additional useful information is
available in the document “Guidelines for
the Selection of Laboratory Instruments,”
AWWA No. M 15, American Water Works
Association.
3.1 General
3.1 .1 Analytical balance: Sensitivity of at
least 0.1 mg. The balance must be
seated on a steady base to prevent
interference due to vibration and
should be protected from interfer-
ence due to air currents.
3.1 .2 Magnetic stirrer: Variable speed,
with stirring bar coated with inert
material.
3.1.3 pH meter: Accuracy, ± 0.05 units.
Scale readability, ± 0.1 units. Labora-
tories purchasing a new pH meter are
strongly advised to purchase one
capable of functioning with specific
ion electrodes. Unit may be line/
bench or battery/portable operated.
3.1.4 Conductivity meter: Suitable for
checking distilled water quality.
Should be readable in ohms or mhos,
have a range from 2 ohms to 2 meg-
ohms or equivalent micromhos ± 1
percent. Unit may be line/bench or
battery/portable operated.
3.1.5 Hot plate: Large or small unitswith
selectable temperature controls for
safe heating of laboratory reagents.
3.1.6 Refrigerator: A standard kitchen type
domestic, commercial, or laboratory
grade refrigerator for storage of
aqueous reagents and samples.
3.1.7 Drying oven: Gravity or mechanical
convection units with selectable
temperature control from room tem-
perature to 180°C (±2°) or higher.
3.1.8 Thermometer: Any good grade
mercury-filled centigrade thermome-
ter with 1°C or finer subdivisions
calibrated to 180°C or higher.
3.2 Inorganic contaminants
Spectrophotometer: Usable
wavelength range. 400 to
700 nm. Maximum spectral
bandwidth, no more than 20
nm. Wavelength accuracy, ±
2.5 nm. Photometer must be
capable of using several
sizes and shapes of absorp-
tion cells providing a sample
path length from approxi-
mately 1 to 5 cm.
3.2.1.2 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
or other isolation device at or
near the maximum absorp-
tion of the colorimetric meth-
ods. Photometer should be
capable of using several
sizes and shapes of absorp-
tion cells providing a sample
path length varying from
approximately 1 to 5 cm.
3.2.2 Specific ion meter: Readable and
accurate to ± 1 mV. Unit may be line!
bench or battery/portable operated.
3.2.3 Electrodes: pH electrodes, specific
ion electrodes and reference elec-
trodes as specified by the individual
method.
3.2.4 Stirred water bath: For operation up
to 100°C (with gable lid).
3.2.5 Automated analysis systems: Exact
equipment used is specified by the
individual method; includes:
3.2.5.1 Sampler
3.2.5.2 Proportioning pump
3.2.5.3 Manifold or analytical car-
tridge
3.2.5.4 Heating bath
3.2.5.5 Heating bath with distillation
head
3.2.5.6 Continuous filter
3.2.5.7 Colorimeter with filters
3.2.5.8 Ion selective electrode detec-
tor with electrodes
3.2.5.9 Recorder
3.2.6 Arsine generator and absorption
system: A Gutzeit generator or
equivalent used in conjunction with
an absorber tube or assembly.
3.2.7 Atomic absorption spectrophotome-
ter: Single-channel, single- or double-
beam instrument having a grating
monochromator, photomultiplier
detector, adjustable slits, a wave-
length range of at least 190 to 800
nm.
3.2.7.1 Readout system: An appro-
priate readout system that
has a response time capable
of measuring the atomic
absorption signal generated
is required. This includes the
capability to detect positive
interference on the signal
from intense non-specific
absorption. In furnace anal-
ysis a strip chart recorder
must be used for verification
3.2.1 Photometer:
3.2.1.1

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CRITICAL ELEMENTS FOR CERTIFICATION
of adequate background cor-
rection if a CRT video readout
or hard copy plotter is not
available. The recorder must
have a chart width of 10
inches or 25cm. full scale
response time of 0.5 sec. or
less, 10- or 1 00-mV input to
match the instrument and
variable chart speeds of 5 to
50 cm/mm. or equivalent.
3.2.7.2 Fuel and oxidant: Commer-
cial grade acetylene , ener-
ally acceptab’e. Air may be
supplied from a compressed
airline, a laboratory com-
pressor, or from a cylinder of
compressed air. Reagent
grade nitrous oxide is also
required for certain determi-
nations. Standard, commer-
cially available argon and/or
nitrogen are required for
furnace work, and hydrogen
is required for the flame
hydride systems. The sup-
plies of fuel and oxidant shall
be maintained at pressures
somewhat higher than the
controlled operating pres-
sure of the instrument by
suitable valves.
3.2.7.3 Burner:The burner recom-
mended by the particular
instrument manufacturer
and consistent with the
approved method should be
used. For certain elements
the nitrous oxide burner is
required.
3.2.7.4 Hollow cathode lamps: Sin-
gle element lamps are to be
preferred but multi-element
lamps may be used. Elec-
trodeless discharge lamps
may also be used.
3.2.7.5 Graphite furnace: Any fur-
nace device capable of
reaching the specified tem-
peratures is satisfactory.
3.27.6 Pipets: Microliter with dis-
posable tips. Sizes can range
from 5 to 100 microliters as
required. Pipet tips which are
white in color and do not
contain CCIS have been found
suitable.
3.2.7.7 Background corrector: A
background correction sys-
tem or provision for a subse-
quent analysis using a non-
absorbing line is required for
furnace analysis.
3.2.7.8 Separatory funnels: 250 mL
or larger, for extraction with
organic solvents.
3.2 7.9 Hydride generation system:
Any gaseous hydride system
used in conjt nction with an
atomic absorption spectro-
photometer equipped for
direct aspiration analysis.
3.2.8 Mercury cold vapor analyzer: Corn-
mercially available vapor mercury
analyzer can be substituted for the
equipment listed below.
3.2.8.1 Absorption cell: Standard 10
cm quartz cell with end win-
dows or 11.5 cm plexiglass
cell with an l.D. of 2.5 cm.
3.2.8.2 Air pump: Peristaltic pump
with an air flow of 1 L per
minute.
3.2.8.3 Flowmeter: Capable of
measuring an air flow of 1 L
per minute.
3.2.8.4 Spectrophotometer: Atomic
absorption spectrophotome-
ter equipped with a mercury
hollow cathode lamp.
3.2.8.5 Aeration tube: A straight
glass fit having a coarse
porosity.
3.2.8.6 Drying unit: A6 inch drying
tube containing 20 grams of
magnesium perchlorate or a
heating device is required to
prevent condensation of
moisture.
Gas chromatograph: A commercial or
custom-designed gas chromatograph
(GC) with a column oven capable of
isothermal temperature control
± 0.2°C to at least 220°C. Additional
accessories and specifications are
listed below by methodology.
3.3.1.1 Chlorinated hydrocarbons:
Equipped with a glass lined
injection port suitable for
chlorinated hydrocarbon
pesticides with a minimum
of decomposition, and
equipped with either an elec-
tron capture, microcoulomet-
nc titration, or electrolytic
conductivity detector.
3.3.1.2 Chlorophenoxys: Equipped
with a glass lined injection
port and either an electron
capture, microcoulometric
titration, or electrolytic con-
ductivity detector.
3.3.1.3 T HM by purge andtrap:
Temperature programmable
from 45° to 220° at about
8°C/mm and equipped with
either microcoulometricti-
tration or e lectrqlytic con-
ductivity detector.
3.3.1.4 TTHM by liquid/liquid ex-
traction: Equipped with a
linearized (frequency modu-
lated) electron capture detec-
3.3.1.5 lTffM by gas chromatogra-
phy/mass spectrometry: The
gas chromatograph, which
must be temperature pro-
grammable, should be inter-
faced to the mass spectrom-
eter with an all-glass
enrichment device and an
all-glass transfer line. Mass
spectral data are to be ob-
tained with electron-impact
ionization at a nominal elec-
tron energy of 70 eV. The
mass spectrometer needs to
produce a spectrum that
meets all criteria in Table
lV-1 when 50 ng or less of p-
bromofluorobenzene (BFB) is
introduced into the gas chro-
matograph. An interfaced
data system is necessary to
acquire, store, reduce and
output mass spectral data.
The data system needs to be
equipped with software to
acquire and manipulate data
for only a few ions that were
selected as characteristic of
trihalomethanes and the
internal standard (or surro-
gate compound).
3.3.2Recorder for gas chromatograph:
Strip chart recorder having a chart
width of 10 in or 25 cm, a full scale
response time of 1 sec. or less, 1 -mV
(-0.05 to 1.05) signal to match the
instrument, and a chart speed of 0.25
to 0.5 in/minor equivalent.
3.3.3 Purge sndtrap system: A commercial
or custom-designed system contain-
ing three separate elements. When
used with a compatible gas chromat-
ograph, the assembly should be able
to detect 0.5 zg/L of each of the indi-
vidual trihalomethanes and measure
them with a reproducibility not to
exceed 8% relative standard devia-
tion at 20 zg/L.
TABLE lV-1
p-Bromofluorobenzene Key Ions
and Ion Abundance Criteria
Mass Ion Abundance Criteria
50 15to40%ofmass95
75 30 to 60% of mass 95
95 base peak, 100% relative abun-
dance
96 5 to 9% of mass 95
173 less than 2% of mass 174
174 greater than 50% of mass 95
175 5to9%ofmassll4
176 96to100%ofmassl74
177 5to9%ofmass l76
3.3 Organic Contaminants
3.3.1
toT.

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CRITICAL ELEMENTS FOR CERTIFICATION
3.3.3.1 Purging device: Designed for
a 5 ml sample volume. Gas
inlet disperses finely divided
gas bubbles through the
sample.
3.3.3.2 Trapping device: Capable of
retaining purged trihalo-
methanes at room tempera-
tures.
3.3.3.3 Desorber assembly: Capable
of heating the trapping de-
vice to 180°C in one minute
with less than 40°C over-
shoot.
3.3.4 Kuderna-Danish glassware: Sets of
tapered glassware, each consisting of
a three ball Snyder column, evapora-
tive flask, and calibrated ampul.
3.3.5 Water bath: Electric or steam heated
capable of temperature control to
within 5°C to 100°C. Concentric ring
or other cover is required to support
Kuderna-Danish concentrators.
Table IV-2
4. General Laboratory
Practices
Although laboratory practices are not speci-
fied here for laboratory certification, it must
be recognized that the generation of valid
analytical data is dependent upon proper
laboratory practices (see Recommended
Practices).
5. Analytical Methodology
5.1 General: All prepackaged kit proce-
dures, other than the DPD Colorimetric
Test Kit, are considered alternative
analytical tec niques, and procedures
described under Section 141.27 of the
National Interim Primary Drinking
Water Regulations (NIPDWR) are to be
followed.
5.2 Inorganic contaminants: Table IV-2
shows the approved methodology and
references for inorganic chemical
contaminants as described in Secticn
141.23 of the NIPDWR. All other proce-
dures are considered alternataive ana-
lytical techniques.
5.3 Organic contaminants: Table lV-3
shows the approved methodology and
references for organic chemical
contaminants as described in Sections
141.24 and 141.30 of the NIPDWR. All
other procedures are considered
alternative analytical techniques.
6. Sample Collection,
Handling, and Preservation
When the laboratory has been delegated
responsibility for sample collection, han-
dling, and preservation, there needs to be
strict adherence to correct sampling proce-
dures, complete identification of the sam-
ple, and prompt transfer of the sample to
the laboratory.
6.1 General
6.1 .1 the collector should be trained in
sampling procedures and approved
by the State regulatory authority or
its delegated representative.
6.1.2 The sample needs to be representa-
tive of the potable water system. The
water tap must be sampled after
“Methods of Chemical Analysis of Water and Wastes.” EPA Environmental Monitoring and Support Laboratory. Cincinnati, Ohio. 45268 (EPA-600/4-79-020). March
1979. Available from ORD Publications. CERI. EPA. Cincinnati, Ohio. 45268. For approved analytical procedures for metals, the technique applicable to total metals must
be used.
2 Annual Book of ASTM Standards. Part 31 Water, American Society for Testing and Materials. 1916 Race Street. Philadelphia, Pennsylvania. 19103.
“Standard Methods for the Examination of Water and Wastewater.” 14th Edition. American Public Health Association, American Water Works Association. Water Pollu-
tior, Control Federation. 1975.
‘Techniques of Water Resources Investigation of the United States Geological Survey. Chapter A-i. “Methods for Determination of Inorganic Substances in Water and
Fluvial Sediments,” Book 5(1979. Stock #024-001-03177-9). Available from Superintendent of Documents, U.S. Government Printing Office. Washington. D.C. 20402.
“Fluoride in Water and Wastewater. Industrial Method #129-71 W.’. Technicon Industrial Systems. Tarrytown, New York, 10591, December 1972.
“Fluoride in Water and Wastewater,” Technicon Industrial Systems. Tarrytown. New York, February 1976.
“Methods Manual-93 Series Electrodes.” Form 93 MM/9790. pp.3-6.1979. Orion Research Incorporated. Cambridge, Mass.
Approved Methodology
for Inorganic Contaminants
Comsmln.nt
Reference (Method Number)
Methodology EPA 1 ASTM ’ SM’ Other
Arsenic
Atomic absorption; furnace technique
Atomic absorption; gaseous hydride
206.2
206.3
206.4
-
D2972-78B
D2972-78A
-
301 A-Vll
404A after B(4)
-
I-i 062-78k
-
Spectrophotometric, silver diethyldithiocarbamate
Barium
Atomic absorption; direct aspiration
Atomic absorption; furnace technique
208.1
208.2
-
301 A-lV
-
-
-
Cadmium
Atomic absorption; direct aspiration
Atomic absorption; furnace technique
213.1
213.2
D3557-78A or B
-
301 A-Il or Ill
-
-
-
Chromium
Atomic absorption; direct aspiration
Atomic absorption; furnace technique
218.1
218.2
Dl 687-770
-
301 A-lI or III
-
.
.
Fluoride
Lead
Colorimetric SPADNS; with distillation
Potentiometric ion selective electrode
Automated Alizarin fluoride blue; with distillation
Automated ion selective electrode
Zirconium eriochrome cyanine R; with distillation
Atomic absorption; direct aspiration
Atomic absorption; furnace technique
340.1
340.2
340.3
-
-
239.1
239.2
Dli 79-72A
Dii 79-72B
-
-
D3559-78A or B
-
414 A and C
41 4B
603
-
301 A-Il or Ill
-
.
.
129-71 W
380-75WE°
l-3325-78
-
-
Mercury
Manualcoldvaportechnique
Automated cold vapor technique
245.1
245.2
D3223-79
-
301A-Vl
-
-
Nitrate
Colorimetricbrucine
Spectrometric; cadmium reduction
Automated hydrazine reduction
Automated cadmium reduction
Ion selective electrode
352.1
353.3
353.1
353.2
-
D992-71
D3867-79B
-
D3867-79A
4190
41 9C
-
605
-
-
. -
-
93MM-79 ’
Selenium
Silver
Atomic absorption; furnace technique
Atomic absorption; gaseous hydride
Atomic absorption; direct aspiration
Atomic absorption; furnace technique
270.2
270.3
272.1
272.2
-
03859-79
-
-
-
301 A-VlI
301A-ll
-
I-i 667-78k
-
.
11

-------
CRITICAL ELEMENTS FOR CERTIFICATION
maintaining a steady flow of 2 or 3
minutes to clear service line. The tap
must be free of aerator, strainer, hose
attachment, or water purification
devices.
6.1.3 The sample report form should be
completed immediately after collec-
tion with location, date and time of
collection, collector’s name, and any
special remarks concerning the sam-
ple.
6.2 Inorganic contaminants
6.2.1 The type of sample container and the
required preservative for each in-
organic chemical contaminant are
listed in Table lV-4.
6.2.2 It is essential that all samples be
analyzed within the maximum hold-
ing times listed in Table IV-4. Where
maximum holding times cannot be
met, the sample is to be discarded
and resampling requested.
6.3 Organic Contaminants
6.3.1 The type of sample container and the
required preservative for the organic
chemical contaminants are listed in
Table IV-5.
6.3.2 When sampling chlorinated waters
for 1THM analysis, sodium thiosul-
fate or sodium sulfite should be
added to the empty sample bottles
prior to shipping to the sampling site.
6.3.3 The T1HM bottles need to be filled in
such a manner that no air bubbles
pass through the sample as the bottle
is filled. The bottle is to be sealed so
that no air bubbles are entrapped in
it. The hermetic seafon the sample
bottle needs to be maintained until
analysis.
6.3.4 It is essential that all samples be
analyzed within the maximum hold-
ing times listed in table lV-5. Where
maximum holding times cannot be
met, the sample is to be discarded
and resampling requested.
7. Quality Assurance
The critical elements for quality assurance
are described below. Additional specifica-
tions can be found in the Recommended
Practices section.
7.1 General
7.1.1 The laboratory should prepare and
follow a written QA plan (see Chapter
Ill, section on QA plans). All quality
assurance data should be available
for inspection.
7.1.2 It is essential that the laboratory
analyze an unknown performance
evaluation sample (when available)
once per year for all regulated con-
taminants measured. Results need to
be within the control limits estab-
lished by US EPA for each analysis for
which the laboratory wishes to be
certified.
7.1.3 A manual of analytical methods
should be available to the analysts.
7.1.4 pH meters are calibrated each use
period with fresh standard buffers at
pH 7.0 and at the pH appropriate for
the test being performed.
7.2 Inorganic contaminants
7.2.1 A standard reagent curve composed
of a minimum of a reagent blank and
three standards covering the concen-
tration range of the samples needs to
be prepared. At least one of the
standards should be at or below the
MCL.
7.2.2 For each day on which analyses are
performed, the standard curve needs
to be verified by use of at least a labo-
ratory method blank and one stand-
ard within the range of the standard
curve. Daily checks should be within
± 10 percent of the original curve.
7.2.3 If 20 or more samples per day are
analyzed, the working standard curve
needs to be verified by running an
additional standard within the range
of the standard curve every 20 sam-
ples. Each check should be within ±
10 percent of original curve.
7.3 Organic contaminants
7.3.1 For each day on which pesticide or
phenoxyacid analyses are initiated,
or trihalomethane reagent water is
prepared, it is essential that a labora-
tory method blank be analyzed with
the same procedures used to analyze
samples.
7.3.2 A minimum of three calibration
standards should be analyzed each
day to calibrate the analytical system.
If the laboratory can demonstrate that
the instrument response is linear
through the origin, this practice can
be reduced to one standard per day,
providing the response of the stand-
ard is within ± 15 percent of previous
calibrations.
Table IV-3
Approved Methodology
for Organic Contaminants
Methodology
Reference (Method Number or page numbers)
EPA’ ASTM 2 SM USGS 4
Total Trihalomethanes
(1THM)
(7)
‘“Methods for Organochlarine Pesticides and Chiorophenoxy Acid Herbicides in Drinking Water and Raw Source Water,” Available from ORD Publications. CERI. EPA.
Cincinnati, Ohio, 45268.
ZMnu& Bock of ASTM Standards, Part 31 Water, American Society for Testing and Materials, 1916 Race Street. Philadelphia. Pennsylvania 19103.
3 Standard Methods for the Examination of Water and Wastewater.” 14th Edition, American Public Health Association, American Water Works Association. Water Pollu-
tion Control Federation. 1975.
4 Techniques of Water-Resources Investigation of the United States Geological Survey, Chapter A-3. Methods for Analysis of Organic Substances in Water.” BookS,
1972. Available from Superintendent of Documents. U.S. Government Printing Office. Washington. D.C. 20402.
Analysis of Thhalømethanes in Finished Waters by the Purge and Trap Method.” Method 501.1. EMSL EPA. Cincinnati, Ohio 45268.
Th. Analysis of Thhalomethanes in Drinking Water by Liquid/Liquid Extraction.” Method 501.2. EMSL EPA, Cincinnati, Ohio 45268.
7 ”Measurement of Trihalomethanes in Drinking Water by Gas Chromatography/Mass Spectrometry and Selected Ion Monitoring,” Method 501.3, EMSL EPA. Cincin-
nati, Ohio 45268.
Chlorinated hydrocarbons:
endrin
lindane
methoxychior
toxaphene
Chlorophenoxys:
2,4-D
2,4,5-TP
Solvent extraction, gas chromatography
Solvent extraction, derivatization, gas
chromatography
Purge and trap, gas chromatography
Solvent extraction, gas chromatography
Gas chromatography/mass spectrometry
03086-79
D3478-79
pp. 1-19
pp. 20-35
(5)
(8)
509A
509B
pp. 24-39
pp. 24-39

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CRITICAL ELEMENTS FOR CERTIFICATION
7.3.3 Each quarter, it is essential that the
laboratory analyze certified quality
control check standards for each
contaminant. If the criteria estab-
lished by US EPA are not met, correc-
tive action needs to be taken and
documented.
7.3.4 It is essential that the laboratory
analyze a field blank for trihalometh-
anes with each sample set. If reporta-
ble levels of trihalomethanes are
demonstrated to have contaminated
the field blank, resampling is essen-
tial.
7.3.5 The laboratory is to analyze 10 per-
Cent of all samples for TTHM in dupli-
Table IV-4
Nitrate
Chlorinated supplies
Non-chlorinated supplies
Selenium
Silver
Table IV-5.
Refrigerate at 4°C as
soon as possible after
collection
Chlorophenoxys Refrigerate at4° as
soon as possible after
collection
1THM Sodium thiosulfate
or sodium sulfite
cate. A continuing record of results
and subsequent actions taken needs
to be maintained.
7.3.6 The laboratory needs to analyze a
known TTHM laboratory control
standard each day. If errors exceed
20 percent of the true value, all tn-
halomethane results since the previ-
oUs successful test are to be consid-
ered suspect.
7.3.7 Each time the TTHM analytical sys-
tem undergoes a major modification
or prolonged period of inactivity, the
precision of the system needs to be
demonstrated by the analysis of repli-
cate laboratory control standards.
Maximum
Holding
Container 3 urn. 4
Container
Glass with foil
or Teflon-lined
cap
Glass with foil
or Teflon-lined
cap
Glass with 28 days
Teflon-lined
septum 4
7.3.8 It is critical that laboratories that
analyze for TTHM by liquid-liquid
extraction demonstrate that raw
source waters do not contain inter-
ferences under the chromatographic
conditions selected.
7.3.9 If a mass spectrometer detector is
used for TTHM analysis, it is essential
that the mass spectrometer perform-
ance tests described under equip-
ment specifications using BFB be
conducted once during each 8-hour
work shift. Records of satisfactory
performance and corrective action
need to be maintained.
8. Recordsand Data
Reporting
8.1 Records of chemical analyses are to be
kept by the laboratory for not less than
3 years. This includes all raw data,
calculations, and quality control data.
8.2 Actual laboratory reports may be kept.
However, data, with the exception of
compliance check samples as detailed
in Section 141.33(b) of the NIPDWR.
may be transferred to tabular sum-
maries. The following information
should be included:
8.2.1 Date, place, and time of sam-
pling; name of person who col-
lected the sample.
8.2.2 Identification of sample as to
whether it is a routine distribu-
tion system sample, check sam-
ple, raw or process water sam-
ple, or other special purpose
sample.
8.2.3 Date of receipt of sample and
date of analysis.
8.2.4 Laboratory and persons respon-
sible for performing analysis.
8.2.5 Analytical technique/method
used.
8.2.6 Results of analysis. -
9. Action Response to
Laboratory Results
10. Maximum Total Trihalo-
methane Potential
10.1 Method: Gas chromatography.
“Method for the Determination of
Maximum Total Trihalomethane.
Potential — Method 510.1.” EMSL,
U.S. EPA, Cincinnati, Ohio 45268.
Contaminant
Sample Collecting, Handling, and Preservation for Inorganic Contaminants’
Arsenic
Barium
Cadmium
Chromium
Fluoride
Lead
Mercury
Conc HNO 3 to pH <2
Conc HNO 3 to pH <2
Conc HN O 3 to pH <2
ConcHNO 3 topH<2
None
Conc HNO 3 to pH <2
Conc HNO 3 to pH <2
Cool, 4°C
Conc H 2 S0 4 to pH <2
Conc HNO 3 to pH <2
Conc HNO 3 to pH <2
P or G
Por G
P or G
PorG
P or G
P or G
G
P
PorG
PorG
P or G
P or G
6 months
6 months
6 months
6 months
1 month
6 months
38 days
14 days
28 days
14 days
6 months
6 months
‘If 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.
ft HNO 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 conc HNO 3 to pH <2.
At time of analysis, sample container should be thoroughly rinsed with 1:1 HNO 3 ; washings should be added to
sample.
= Plastic, hard or soft G = Glass. hard or soft.
4 1n all cases, samples should be analyzed as soon after collection as possible.
Chlorinated
hydrocarbons
Sample Collection, Handling and Preservation for Organic Contaminants 1 When action response is a designated labo-
Maximum ratory responsibility, the proper authority
Holding must be promptly notified of non-compliance
Contaminant Preservative sample results and a request made for
resampling from the same sampling point.
14 days 3
7 days 3 Laboratories that are engaged in the deter-
mination of maximum total trihalomethane
potential (MTP) need to meet the following
requirements for that test.
‘If a laboratory has no control over these factors, it is critical that the laboratory director reject any samples not meet-
ing these criteria and so notify the authority requesting the analyses.
2 1n all cases, samples should be analyzed as soon after collection as possible.
3 Well-stoppered and refrigerated extracts can be held up to 30 days.
4 A11 samples are collected in duplicate.
13

-------
CRITICAL ELEMENTS FOR CERTIFICATION
10.2 Sampl.Container:Tl ’HM sample
bottle.
10.3 Supplemental equipment: Constant
temperature storage container, water
bath or incubator, 25°C or above.
10.4 The laboratory must be certified for
TIHM analysis.
11. Sodium and Corrosivity
Measurements for sodium and certain cor-
rosivity characteristics to meet special
monitoring regulations are to be performed
in an approved laboratory. The critical ele-
ments for these tests are described below.
11.1 Methodology-TabIeIV-6showsthe
approved methodology and refer-
ences for sodium and corrosivity
measurements as described in Sec-
tions 141.41 and 141.42 of the NIP-
DWR. All other procedures are con-
sidered alternative analytical tech-
niques.
11.2 AddItional Criteria
11.2.1 Sodium - Samples may be collected
in plastic or glass. Samples are pre-
served by the addition of conc.
HNO 3 to pH <2; analyses are per-
formed within 6 months. An atomic
absorption spectrophotometer or
flame photometer is necessary.
11.2.2 Alkalinity — Samples may be col-
lected in plastic or glass, and are
preserved by cooling to 4°C; analy-
sis are performed within 14 days.
11.2.3 Calcium — Samples may be collected
in plastic or glass, aFid are preserved
by the addition of conc. HNO 3 to pH
<2 and cooling to 4°C; analyses are
performed within 6 months.
11.2.4 Chloride - Samples may be collected
in plastic or glass. Samples are not
preserved; analyses are performed
within 7 days. An electronic volt-
meter with a glass and silver-silver
chloride electrode system is neces-
sary.
11.2.5 Sulfate — Samples may be collected
in plastic or glass, and are preserved
by cooling to 4°C; analyses are
performed within 7 days.
11.2.6 Total filterable residue — Samples
may be collected in plastic or glass.
and are preserved by cooling to 4°C;
analyses are performed within 7
days. Glass or plastic desiccator is
necessary.
Recommended
Practices
1. Personnel
1.1 Laboratory Director. The following
are recommended minimum standards
for the laboratory director.
1.1.1 Academictraining: Minimum of
bachelor of science degree or its
equivalent.
1.1.2 Experience: Minimum of 5 years
of experience.
1.2 Supervisor. This position may not be
necessary in smaller laboratories. The
following are recommended minimum
standards for the supervisor.
1.2.1 Academic training: Minimum
bachelor’s degree in chemistry
or its equivalent.
1.2.2 Experience: Minimum of 2 years
otexperience in measurements
being considered for certifica-
tion.
1.3 Analyst for Inorganic Contaminants.
The following are recommended mini-
mum standards for the analyst posi-
tion.
1.3.1 Academic training: Minimum of
high school diploma or its equiv-
a lent (State certification or li-
censing may be considered).
1.3.2 Experience: Minimum of 6
months of on-the-job training,
under direct supervision of qual-
ified analyst, in measurements
being considered for certifica-
tion.
1.3.3 After 6 months, the analyst
must demonstrate acceptable
Alkalinity
Calcium
Methyl orange titrimetric or potontiometric
EDTA titrimetric
Atomic absorption; direct aspiration
Potentiometric
Langelaer index
Aggressive index
Colorimetric or titrimetric DPD
Colorimetric syringaldazine
Potentiometric
Atomic absorption; direct aspiration
Atomic absorption; furnace technique
Flame photometric
Turbidimetric
Thermometric
Gravimetric
Nephelometric
150.1
273.1
273.2
375.4
16.1
180.1
403 -
306C -
301 A-lI -
408C -
203 -
- C400-77
4 O9EorF -
- 408G 5
D1293-78AorB 424 -
320A
427C
212
208B
21 4A
Table lV-6
Approved
Methodology
.
for Free
Residual Chlorine.
Turbidity, Sodium and
CorTosivity Measurements
R.fsrenca (Method Number)
Msssure.nsnt
M.thodoloi,y
EPA’
ASTM ’ SM’ Other
310.1
215.2
215.1
Dl 067-70B
Dl 126-67B
D2576-70
Free chlorine residual
pH
Sodium
Sulfate
Temperature
Total filterable residue
Turbidity
- D1428-64A
“MethodsotChemical An&ysisof Water and Wastes,” EPA Environmental Monitoring and Support Laboratory. Cincinnati, Ohio. 45268 (EPA-600/4-79-020). March
1979. Available from ORD Publications, CERI. EPA, Cincinnati. Ohio. 45268. For approved analytical procedures for metals, the technique applicable to total metals must
beused
‘Annual Bock of ASTM Standards. Part 31 Water, American Society for Testing and Materials, 1916 Race Street, Philadelphia. Pennsylvania, 19103.
“Standard Methods far the Examination at Water and Wasfewater.” 14th Edition, American Public Health Association, American Water Works Association, Water Pollu-
tion Control Federation, 1976.
“ ‘Aw.qA standard f Asbestos - ment Plpe. 4 in. through 24 in. for Water and Other Liquids.” AWINA C400-77, Revision of C400-75, AWWA, Denver. Colorado.
“‘Standard Methods for the Examination of Water and Wastewater,” 15th EditiOn. American Public Health Association, American Water Works Association. Water Pollu-
tion Control Fadsratiori. 1980.

-------
RECOMMENDED PRACTICES
skills through the successful
participation in the analysis of
applicable performance evalua-
tion samples.
1.4 Analyst for Organic Contaminants.
The following are recommended mini-
mum standards for the analyst posi-
tion.
1.4.1 Academic training: Minimum of
bachelor’s degree in chemistry
or its equivalent (State certifica-
tion or licensing may be con-
sidered).
1.4.2 Experience: Minimum of 6
months of experience in meas-
urements being considered for
certification and 2 years of ex-
perience in organic analysis.
Each year of college level train-
ing in related scientific fields or
demonstrated equivalency shall
be considered equal to 1 year of
work experience. Such a substi-
tution should not exceed one-
half of the required experience.
1.4.3 Supervision: Supervision by an
analyst (also eligible to analyze
for organic chemicals) who has:
1.4.3.1 Minimum of bachelor’s
degree or its equivalent.
with 1 year of course
work in organic chem-
istry.
1 .4.3.2 One year of experience
in measurement of or-
ganic chemicals by gas
chromatography.
1.5 GC/MS Operator. In addition to the
organic analyst requirements above.
the following are recommended mini-
mum standards for the GC/MS opera-
tor, if this technique is used.
1.5.1 Training: Satisfactory comple-
tion of a minimum one week
course in GC/MS offered by
equipment manufacturer, pro-
fessional organization, universi-
ty, or other qualified operator.
1.5.2 Experience: Minimum of 1 year
experience in the operation of a
GC/MS instrument.
2. Laboratory Facilities
The laboratory facilities should be clean, air
conditioned and with adequate lighting at
the bench top, It is recommended that 150
to 200 square feet/person be available. The
laboratory should contain at least 15 linear
feet of usable bench space per analyst.
The laboratory should have provisions for
the disposal of chemical wastes. While
safety is not an aspect of laboratory certifi-
cation, exhaust hoods are recommended for
the analysis of trace elements and organics.
This includes venting for preparation, ex-
traction and analysis.
3. Laboratory Equipment and
Supplies
The specifications for instruments that are
required for the measurement of chemistry
contaminants can be found under Critical
Elements for Certification for Chemistry. In
addition, it is recommended that,a laborato-
ry purchase equipment that meets the
specifications below.
3.1 Muffle furnace: Capable of heating
glassware to 400°C for cleaning.
3.2 Centrifuge: Capable of handling, as a
minimum, 15 mLcentrifugetubes.
3.3 Refrigerator: For storing organics and
flammable materials, an “explosion-
proof” type of refrigerator should be
used. When refrigeration is not re-
quired, an explosion-proof cabinet may
be used.
3.4 Glassware: Should be of borosilicate
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 Specifi-
cations and need not be calibrated
before use.
3.5 GC/MS interface: It is recommended
that the interface between the end of
the chromatographic column and the
ion source of the mass spectrometer
be constructed with deactivated glass
or glass-lined materials. However, the
GC/MS interface can use any separa-
tor, transfer line, or other interface
part, provided it is demonstrated that
the system meets the BFB perform-
ance specifications.
3.6 GC/MS data system: It is desirable,
but not required, that the GC/MS data
system have the following additional
features:
3.6.1 Ability to perform automatic
quantitative analysis using inte-
grated specific ion abundances
and either a single internal or
external standard.
3.6.2 Ability to perform automatic
quantitative analysis using inte-
grated specific ion abundances
and regression analysis with
multiple internal or external
standards.
4. General
Laboratory Practices
Chemicals/reagents: “Analyti-
cal reagent grade” (AR) chemi-
cals should be used for most
analyses required of water treat-
ment laboratories. Consult
“Standard Methods for the Ex-
amination of Water and Waste-
water,” 14th edition, part 102,
pages 5-8, or the latest edition
of this reference, for more de-
tailed information on reagent
grades. Individual analytical
procedures in “Standard Meth-
ods for the Examination of
Water and Wastewater,” and
the U.S. EPA’s “Methods for
Chemical Analysis of Water and
Wastes” may specify special
requirements for the reagents to
be used.
4.1.2 Laboratory safety: While safety
is not an aspect of laboratory
certification, evaluators should
point out, on an informal basis,
potential safety problems ob-
served during an on-site visit.
4.2 Inorganic contaminants
4.2.1 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 suffi-
cient 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 (suit-
ably prepared) for the nitrate,
mercury, and lead procedures
due to the potentiality for con-
tamination from the laboratory
environment.
4.2.2 Distilled/deionized water:
Water having resistivity values
of 0.5 megohms (2.0 micro-
mhos)/cm at 25°C is satisfacto-
ry. Megohms are related to
microjnhos in the following
manner:
= micromhos,
megohms
= megohms
micromhos
Excellent quality water has re-
sistivity values exceeding 1.0
megohms/cm(less than 1.0
micromhos/cm) at 25°C. High
quality water meeting such spe-
cifications may be purchased
from commercial suppliers; lab-
oratories should request a list of
quality specifications for any
water purchased. Quality ofdis-
tilled/deionized water is best
maintained by sealing from the
atmosphere. Quality checks
should be made at planned in-
tervals and documented.
4.1 General
4.1.1
15

-------
RECOMMENDED PRACTICES
4.3 Organic contaminants
4.3.1 Glassware preparation: All
glassware should be washed in
a warm detergent solution and
thoroughly rinsed first in tap
water and then in distilled water.
All glassware should have a
final rinse with nanograde ace-
tone or its equivalent and should
then be air dried in an area free
of organic contamination.
4.3.2 Reagent water: Reagent water
for organic analysis should be
free of interferences that coe-
lute from the gas chromato-
graph with the compound being
measured. It may be necessary
to treat distilled water with acti-
vated carbon to eliminate all
interferences.
5. Analytical Methodology
A list of the approved methodology for in-
organic contaminants can be found in Table
IV-2. The approved methodology for organic
contaminants is listed in Table IV-3.
6. Sample Collection,
Handling, and Preservation
The type of sample containers required.
preservation techniques, and maximum
holding times for all inorganic contami-
nants can be found in Table lV-4. Table lV-5
identifies these critical elements for the
organic contaminants.
7. Quality Assurance
The minimum requirements for quality con-
trol are described in Critical Elements for
Certification. Performance and documenta-
tion of the following quality control prac-
tices are strongly recommended.
7.1 Current service contract should be in
effect on all balances.
7.2 Class S weights should be available to
make periodic checks on balances.
7.3 Thermometer certified by the National
Bureau of Standards (or one of equiva-
lent accuracy) should be available to
check thermometers in ovens, etc.
7.4 Color standards or their equivalent
should be available to verify wave-
length settings on spectrophotome-
ters.
7.5 Chemicals should be dated upon re-
ceipt of shipment and replaced as
needed or before shelf life has been
exceeded.
7.6 Additional recommended practices
have been established for a laboratory
analyzing supply samples other than
its own:
7.6.1 Laboratory should analyze a
certified laboratory control
standard (U.S. EPA Quality Con-
trol Sample. or equivalent) once
per quarter 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.
7.6.2 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.
7.6.3 Standard deviations should be
calculated and documented for
all methods being conducted.
7.6.4 Quality control charts or a tabu-
lation of mean and standard
deviation or equivalent should
be used to document validity of
data on an as-run basis.
8. Records and Data
Reporting
9. Action Response to
Laboratory Results
10. Free Chlorine Residual,
Turbidity, pH and Temperature
Free chlorine residual, turbidity, pH and
temperature measurements do not need to
be done in approved laboratories, 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 criti-
cal measurements.
10.1 Methodology - Only approved meth-
odology may be used for free chlorine
residual, turbidity, pH and tempera-
ture. The approved methods are listed
in Table lV-6. All other procedures
are considered alternative analytical
techniques.
10.2 Sealed liquid turbidity standards
purchased from the instrument man-
ufacturer must be calibrated against
properly prepared and diluted forma-
zin or styrene di inylbenzene polymer
standards at least every 4 months in
order to monitor for any eventual
deterioration. These standards
should be replaced when any major
change from the original calibration
occurs. Solid turbidity standards
composed of plastic, glass, or other
materials are not reliable and should
not be used.
10.3 Calibration intervals for color wheels,
sealed ampules, and other visual
standards for free chlorine residuals:
Laboratories utilizing visual compari-
son devices should calibrate the
standards incorporated into such
devices at least every six months.
These calibrations should be docu-
mented. Directions for preparing
temporary and permanent type visual
standards can be found in Method
4.09F, “Standard Methods for the Ex-
amination of Water and Wastewater,”
14th edition, published in 1975 by
the American Public Health Associa-
tion. By comparing standards and
plotting such a comparison on graph
paper, a correction factor can be de-
rived and applied to all future results
obtained on the now calibrated appa-
ratus.
10.4 Additional criteria - The following
criteria are recommended for use by
the State for approval of persons for
performing free chlorine residual,
turbidity. pH and temperature meas-
urements.
10.4.1 Free chlorine residual -
Samples may be collected in
plastic or glass. Samples are
not preserved; analyses are
to be made as soon as practi-
cable, or within 1 hour. A
DPO Colorimetric Test Kit,
spectrophotometer, or pho-
tometer is required.
10.4.2 Turbidity - Samples may be
collected in plastic or glass.
Samples are not preserved;
analyses are to be made as
soon as practicable, or with-
in 1 hour. Nephelometer is
needed with light source for
illuminating the sample and
one or more photoelectric
detectors with a readout de-
vice to indicate the intensity
of light scattered at right
angles to the path of the inci-
dent light. Unit may be line!
bench or battery/portable
operated.
10.4.3 pH - Samples may be col-
lected in plastic or glass.
Samples are not preserved;
analyses are to be made as
soon as practicable, or with-
in 1 hour. A pH meter is
necessary.
10.4.4 Temperature - Samples are
to be analyzed immediately.
Requires any good grade
mercury-filled or dial type
centigrade thermometer, or
a thermistor.

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Sample Forms for
On-Site Evaluation of Laboratories Involved in Analysis of Public Water Supplies—Chemistry
Laboratory:
Street:
City: State: _________________________________________
Survey By:
Affiliation:
Date: _________________________________________ Telephone No.:

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I ,•
Personnel
Position/Titis
Laboratory Director
Evaluator
N ,ne
Academic Training
HS BA/as
Present
Specialty
Experience
(years and areas
Supervisor
Inorganic analysts
.
Organic analysts
.
GC/MS operators

-------
Laboratory Evaluator
Location Date —
General Laboratory Equipment and Instruments
No.of
Units
Manufacturer
Model
Satisfactory
Yes No
Analytical balance
Magnetic stirrer
pH meter
a
Conductivity meter
Hot plate
Refrigerator
Drying oven
Thermometer

-------
— __I_
Laboratory.
I . ti#srl
I.’—.—
Laboratory Equipment—Inorganic Contaminants
Units

Manufecturer
M

SatisfaCtory
Yss No N/A
Photometer
Spectrophotometer
Filter photometer
Specific ion meter
Electrodes
Stirred water bath
Automated analysis system
Sampler
.
Proportioning pump
Manifold or cartridge
Heating bath
Bath with distilling head
Continuous filter
Colorimetér
ISE detector
Recorder
Arsine generator
20

-------
C.,. I. atar
Laboratory
Locaflon
Laboratory Equipment—Inorganic Contaminants
Date
Item
No. of
Uflks
Manufacturer
Model
S.d$faCtory
V.. No rd,A
Atomic absorption spectrophotometer
Readout system
Fuel and oxidants
Burner
.
Hollow cathode lamps
Graphite furnace
Pipets
Background corrector
Separatory funnels
Hydride generation system
Mercury analyzer
Absorption cell
Air pump
Flow meter
Spectrophotometer
Aeration tubs
-
Drying unit

-------
Laboratory
I ,‘ t a rt
Laboratory Equipment—Organic Contaminants
Item
No. of
Units
Manufacturer
Model
Satisfactory
Yes No N/A
Gas chromatography
Chlorinated hydrocarbons
Chiorophenoxys
rrHMbypurgeandtrap
TTHM by solvent extraction
TlHM by GC/MS
Recorder
Purge and trap system
Purging device
Trapping device
Desorber assembly
Kuderna-Danish sets
Water bath
22

-------
c. _I.
Laboratory.
I sa fir fl
Date -
Methodology
Co lnsM
Name or Description of Method
Reference (Cite
Source and Method by
Number or Page and Year)
Sample
Load per
Month
Yes No
Inorganic
Arsenic
Barium
Cadmium
Chromium
Fluoride
Lead
-
Mercury
Nitrate
Selenium
Silver
Organic
Chlorinated hydrocarbons
Chlorophenoxys
UHM
M W
23

-------
ta Ii i tnr
La
Loca on -
Sample Handing and Preservation
Contaminant
Container Used (Material and Size)
eservatlv Used
Maximum
Holding
Tim.
Saa o
No
Inorganic
Arsenic
.
Barium
Cadmium
Chromium
Fluoride
Lead
Mercury
Nitrate
Selenium
Silver
Organic
Chlorinated hydrocarbons
Chiorophenoxys
1THM
MW
24

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Laboratory
Location
Sample Collection
r t
Item
Comments
Satisfactory
y, No
General
Trained sample collector
Representative sampling
Complete sample form
,
Inorganic
Appropriate sampling
and preservation
Overaged samples
discarded
Organic
Appropriate sampling
and preservation
TTHM stabilizer added
in laboratory
TTHM hermetic seal
Overaged samples
discarded
25

-------
I
.._g.
Location Date
Quality Assurance and Data Reporting
Organic
Daily method blank
Daily calibration
Quarterly QC samples
TIHM field blanks
IO%UHM in duplicate
TrHM control standards
.
TTHM startup test
.
501.2 Source water
blank check
.
BFB tuning check
Item
Comments
Satisfactory
Yes No
General
QA plan and data
.
Annual performance
samples analyzed
Methods manual
available
Records kept 3 years
.
pH meter calibration
Inorganic
Standard curve
Daily calibration check
.
Check after 20 samples
26

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Chapter V
M icrobiology
Critical Elements for Certification
T he technical criteria in this chapter are
divided into two sections: Critical Ele-
ments for Certification and Recommended
Practices. Critical Elements for Certification
are necessary for generation of valid data
and certification, and consequently will be
used to determine certification status. All
quality control items are designated as
‘QC. “QC” items in the Critical Elements
for Certification section necessitate written
records.
1. Personnel
Although there are no certification require-
ments for laboratory analysts, laboratory
administrators and evaluators should rec-
ognize the importance of relevant training
and experience to the acquisition of valid
compliance monitoring data. Recommended
minimum standards can be found under
Recommended Practices.
2. Laboratory Facilities
3. Laboratory Equipment
and Supplies
Laboratories must have available or have
working access to items listed below for
analyzing potable water samples for the
detection of coliform organisms.
A laboratory may request or contract an-
other laboratory to conduct specified quality
control testing, e.g., testing the quality of
laboratory pure water (4.3.2); calibration of
non-reference weights (3.2.2); and calibra-
tion of temperature monitoring devices
(3.3.2). The laboratory conducting the ac-
tual quality control test(s) must be certified
for the specific parameter and provide
copies of quality control data to the request-
ing laboratory. Therefore, the requesting.
laboratory is not required to have equip-
ment, supplies, and materials to conduct
specified quality control tests.
3.1 pH Meter
3.1.1 Accuracy and scale graduations
within ± 0.1 units.
3.1.2 Use pH buffer aliquot only once.
QC 3.1.3 Standardize pH meter each use
period with pH 7.0 standard
buffer.
3.2 Balance (top loader or pan)
3.2.1 Balance detects 100 mg at a 150
gram load.
QC 3.2.2 Calibrate balance monthly,
using Class S or S-i reference
weights or weights traceable to
Class S or S-i weights. If non-
reference weights are used,
calibrate annually with Class S
or S-i reference weights.
QC 3.2.3 Maintainservicecontractor
internal maintenance protocol
and maintenance records.
3.3 Temperature Monitoring Device
3.3.1 Glass/mercury or dial thermom-
eters used in incubator units
graduated in 0.5°C increments.
Mercury column for glass ther-
mometers is not separated.
Check calibration of glass/
mercury thermometers annually
and dial thermometers quarterly
against a reference NBS ther-
mometer or one which meets
the requirements of NBS mono-
graph 150.
3.4 Incubation Unit
3.4.1 The incubator unit has an inter-
nal temperature monitoring de-
vice and maintains a tempera-
ture of 35±0.5°C. For nonporta-
ble incubators, thermometers
are placed on the top and bottom
shelves of the use area, the
thermometer bulb immersed in
liquid. If an aluminum block is
used, culture dishes and tubes
fit snugly.
QC 3.4.2 Record temperature for days in
use at least twice per day with
each reading separated by at
least 4 hours.
3.5 Autoclave
3.5.1 The autoclave has a tempera-
ture gauge with a sensor on the
exhaust, and an operational
safety valve. Maintains steriliza-
tion temperature during the
sterilizing cycle and completes
an entire cycle within 45 min-
utes when a 12-15 minute steri-
lization period is used. Autoclave
depressurizes slowly to insure
media do not boil over and bub-
bles do not form in inverted
tubes.
3.5.2 Because of safety concerns and
difficulties with operational con-
trol, approval of pressure cook-
ers and vertical autoclaves
requiresQC data demonstrating
sterility and proper media reac-
tions.
QC 3.5.3 Record date and sterilization
time and temperature for each
cycle. Establish service contract
or internal maintenance proto-
col, and maintain records.
3.6 Conductivity Meter (needed only for
laboratories analyzing laboratory pure
water; optional for laboratories which
send water to another certified labora-
tory for analysis).
3.6.1 Conductivity meter graduated in
ohms or mhos with a sensitivity
of at least 0.33%. Has a range
from 2 ohms to 2 megohms or
equivalent micromhos ± 1%.
3.7 Refrigerator
3.7.1 Refrigerator maintains a tem-
perature of 1 °C to 5°C. Ther-
mometer graduated in at least
1 °C increments and the ther-
mometer bulb immersed in
liquid.
QC 3.7.2 Record temperatures for days in
use at least once per day.
. .8 Inoculating Equipment
3.8.1 Metal or plastic loops, or dry
heat-sterilized hardwood appli-
cator sticks.
3.9 Membrane Filtration Equipment
(needed if MF procedure is used).
3.9.1 MF units are stainless steel,
glass, or autoclavable plastic.
Not scratched, corroded, and do
not leak.
There are no critical elements for laboratory QC 3.3.2
facilities. Recommended guidelines can be
found under Recommended Practices.
27

-------
CRITICAL ELEMENTS FOR CERTIFICATION
3.9.2 10 to 1 5X magnification device
with fluorescent light source
used to count Sheen colonies.
3.9.3 Membrane filters approved by
the manufacturer for total coli-
form water analysis. Approval
based on data relating to toxici-
ty. recovery, retention, and ab-
sence of growth-promoting
substances. Filters are cellulose
ester, white, gridmarked, 47 mm
diameter, and 0.45 um pore size.
Alternate pore sizes may be
used if manufacturer provides
performance data equal to or
better than the 0.45 urn pore
size. Membrane filters are pre-
sterilized or autoclaved before
3.10 Culture Dishes (Loose airTight Lid)
3.10.1 Presterilized plastic or steri-
lizable glass culture dishes
are used. To maintain sterili-
ty of glass culture dishes.
use stainless steel or alumi-
num canisters, or wrap dish-
es in a heavy aluminum foil
or char-resistant paper.
3.10.2 Loose-lid dishes are incu-
bated in a tight-fitting con-
tainer. e.g., plastic vegetable
crisper, to prevent dehydra-
tion of membrane filter and
medium.
3.10.3 Opened packs of disposable
culture dishes resealed
between major uses.
To sterilize and maintain
sterility of glass pipets. use
stainless steel or aluminum
canisters, or wrap individual
pipets in char-resistant
paper.
3.11.2 Opened packs of disposable
sterile pipets are resealed
between major use periods.
3.12 Culture Tubes and Closures
3.12.1 Tubes are made of borositi-
cate glass or other corrosion-
resistant glass.
3.12.2 Culture tubes used for Pre-
sumptive Test in Fermenta-
tion Tube procedure (MPN)
are of a sufficient size to
contain medium plus sample
without being more than 3/4
full.
3.12.3 Tube closures are stainless
steel, plastic, aluminum, or
loosened screw caps with
non-toxic liners. Cotton
plugs are not acceptable.
3.13 Sample Containers
3.13.1 Sample bottles are wide-
mouth plastic or non-cor-
rosive glass with either
screw cap with non-toxic
liner or ground glass stopper,
which withstand repeated
sterilization, or other USEPA-
approved sample containers.
Capacity is at least 120 mL
(4 oz.).
3.13.2 Glass-stoppered bottle clo-
sures are covered with alu-
minum foil or char-resistant
paper for sterilization.
Glassware is made of boro-
silicate glass or other corro-
sion-resistant glass and free
of chips and cracks. Mark-
ings on graduated cylinders
and pipets are legible. Plastic
items are clear and non-
toxic.
3.14.2 Graduated cylinders for
measurement of sample vol-
umes have a tolerance of
2.5% or better.
3.14.3 Pipets delivering volumes of
10 mL or less are accurate
within a 2.5% tolerance.
4. General
Laboratory Practices
4.1 Autoclave Sterilization Procedures
4.1.1 The times for autoclaving mate-
rials at 121°C are listed. Except
for membrane filters and pads
and carbohydrate-containing
media, indicated times are mini-
mal times which may necessi-
tate adjustment depending upon
volumes, containers and loads.
Item
Tim.
(minutee)
Membrane filters& pads
10
Carbohydrate containing media
12-15
Contaminated test materials
30
Membrane filter assemblies
15
Sample collection bottles
15
Individual glassware
15
Dilution water blank
15.
Rinsewater
15
4.1.2 Autoclaved membrane filters
and pads and all media are re-
moved immediately after com-
pletion of cycle.
4.1.3 Metal filtration equipment
is autoclaved between filtra-
tion series. Glass and plastic
filtration equipment is steri-
lized between filtration series. A
filtration series ends when 30
minutes or longer elapse be-
tween sample filtrations.
4.2 Sample Containers
4.2.1 Sodium thiosulfate(100 mg/L)
should be added before steriliza-
tion to sample containers (0.1
mL of 10% sodium thiosulfate
solution per 120 mL container).
QC 4.2.2 Select at least one bottle at
random from each batch and
confirm sterility by adding ap-
proximately a 25-mL volume of a
sterile non-selective broth. Incu-
bate at 35° ± 0.5° C for 24 hours
and check for growth.
4.3 Laboratory Pure Water
4.3.1 Only satisfactorily-tested labo-
ratory pure water from stills or
deionization units is used to
prepare media, reagents, and
dilution/rinse water for per-
forming bacteriological anal-
yses.
Test the quality of the laboratory
pure water or have it tested by
another certified laboratory to
assure it meets the following
requirements:
Psr.mM.r
R.quirem.nts
Frequency
Conductivity
.
>0.5 meg-
ohms resist-
anceor< 2
micromhos/
cm at 25CC
Monthly
Total Chlorine
Non-
Monthly
Residual
detectable
Qualityof
Ratio0.8-3.0
Annually
Laboratory
Pure Water
•Test for bacteriological quality of distilled
water (Standard Methods, p. 888; also
Microbiological Methods for Monitoring
the Environment EPA-600/8-78-O1 7. p.
200).
4.4 Dilution/Rinse Water
4.4.1 Stock buffer solution is prepared
according to Standard Methods
p. 892, or Microbiological
Methods for Monitoring the
Environment, p. 57, using labo-
ratory pure water.
4.4.2 Stock buffer is autoclaved or
filter-sterilized, labeled and
dated. Insure stored stock buffer
is free of turbidity.
4.4.3 Dilution/rinse water is prepared
by adding 1.25 mL of stock buf-
fer solution and 5 mL of MgCl 2
solution (38g MgCl 2 /L) per liter
of laboratory pure water and
sterilize. Do not use MgSO 4
71120 because of possible pre-
cipitation problems. The pH of
References for Chapter V: Standard
Msthods for the Examination of Water
and Wa,tewster. 14th ed.; Microbiologi-
cal Method, for Monitoring the Environ-
ment EPA-600/8-78-017.
use.
3.14 Glassware and Plasticware
3.14.1
QC 4.3.2
3.11 Plpets
3.11.1

-------
CRITICAL ELEMENTS FOR CERTIFICATION
both the stock buffer solution
and the final dilution/rinse
water is 7.2 ± 0.2.
QC 4.4.4 Check each batch of rinse water
for sterility by adding 20 mL of
water to a 1 00-mL volume of a
non-selective broth. Incubate at
35°C ± 0.5°C for 24 hours and
check for growth.
4.5 Glassware Washing
4.5 1 Distilled or deionized water is
used for final rinse.
QC 4.5.2 Perform the Inhibitory Residue
Test (Standard Methods. p.
885. and Microbiological Meth-
ods for Monitoring the Envi-
ronment. p. 199) on initial use
of a washing compound and
whenever a different formula-
tion of washing compound is
used in order to insure that
glassware is free of toxic resi-
due.
4.6 Media—General Requirements
4.6.1 Dehydrated or pre-prepared
media manufactured commer-
cially is used. Store media in
cool, dry location and discard
caked or discolored dehydrated
media.
QC 4.6.2 For media prepared, record the
date of preparation, type of
medium, lot number, steriliza-
tion time and temperature, final
pH, technician’s initials.
4.7 Membrane Filter (MF) Media (needed
only if laboratory conducts MF proce-
dure)
4.7.1 m-Endo broth or agar in the
single step procedure, or m-Endo
agar LES in the enrichment
technique is used. Insure that
ethanol used in rehydration pro-
cedure is not denatured. To dis-
solve medium, use boiling water
bath (or direct heat if constantly
attended) to bring medium just
to boiling point. Do not boil
medium. Final pH 7.2 ± 0.2 C.
4.7.2 MF broth. MF agar medium, and
ampou led m-Endo broth are
refrigerated no longer than 96
hours, 2 weeks, and manufac-
turer’s expiration date, respec-
tively.
4.8 Most Probable Number (MPN) Media
4.8.1 Double strength lauryl tryptose
(lauryl sulfate) broth or lactose
broth is used for Presumptive
Test and single strength brilliant
green lactose bile broth for Con-
firmed Test. Dispense broth
medium volume of not less than
10 mL per tube and autoclave
media at 121°Cforl2-15 min-
utes. Final pH 6.8 ± 0.2(7.2 ±
0.2 for brilliant green broth).
4.8.2 If MPN media are refrigerated.
after sterilization, incubate
overnight at 35°C before use.
Discard tubes showing growth
and/or bubbles. Use MPN çnedia
prepared in tubes with loose-
fitting closures within oneweek.
Store broth media in screw cap
tubes no longer than 3 months,
provided media are stored in
dark. Discard media if evapora-
tion exceeds 10% of original
volume.
4.8.3 If Levine Eosin Methylene blue
(EM B) agar is used for Comple-
ted Test, dissolve by using boil-
ing water bath (or direct heat if
constantly attended) to bring
medium just to boiling point.
Autoclave medium at 121°C for
12-15 minutes. Final pH 7.1 ±
0.2. Use medium not autoclaved
on the day of preparation; DO
NOT STORE. Autoclaved agar
which is refrigerated is used
within two weeks.
4.9 Standard Plate Count Medium (SPC)
4.9.1 SPC agar is autoclaved at 121°C
for 15 minutes depending upon
volume. Final pH 7.0 ± 0.2.
Temper melted agar between
44°C to 46°C before pouring.
Hold melted agar no longer than
8 hours. Do not melt sterile
medium more than once.
5. Analytical
Methodology
5.1 Approved analytical methodology is
stated in the National Interim Primary
Drinking Water Regulations (NIPDWR),
as amended. Do not use tentative
methods, equipment, or procedures
unless they satisfy the requirements of
Section 141.27 of the NIPDWR.
Sample volumes analyzed by the
MF procedure must be 100 mL ±
2.5 mL.
5.2.2 Confluent growth is defined as
bacterial growth with or without
sheen covering the entire mem-
brane filter.
TNTC (too numerous to count)
is defined as greater than 200
total bacterial colonies on the
membrane filter.
5.2.3 Samples resulting in confluent
growth or TNTC with less than
five distinguishable sheen colo-
nies are invalid. Record as “con-
fluent growth” or “TNTC” and
request a new sample from the
same sampling Site.
5.2.4 Samples resulting in confluent
growth or TNTC with five or
more distinguishable sheen
colonies may be a MCL violation.
Report as “confluent growth” or
“TNTC” with the number of dis-
tinguishable sheen colonies.
Check samples must be ob-
tained from the same sampling
site.
9.2.5 Verify all sheen colonies regard-
less of the amount of sheen
when the number of the sheen
colonies is five to and including
10/100 mL. When the number
of sheen colonies exceeds 10/
100 mL, randomly pick and
verify at least 10 colonies repre-
sentative of all sheen types.
5.2.6 Adjust initial counts based only
upon verification data.
QC 5.2.7 Conduct MF sterility check (rinse
water, medium, and supplies) at
the end of each filtration series.
If controls indicate contamina-
tion, reject all data on samples
affected and request immediate
resampling of the samples in-
volved.
5.3 MPN Procedure
5.3.1 Conduct MPN Completed Test
on all unsatisfactory samples C>
three positive tubes). Gram-
staining is optional for potable
water samples.
5.3.2 For unsatisfactory samples,
adjust the number of positive
tubes on the basis of the Com-
pleted Test.
5.3.3 If the MPN test is used on water
supplies that have a history of
confluent growth or TNTC by the
MF procedure, all presumptive
tubes with heavy growth with-
out gas production are submit-
ted to the Confirmed Test to
check for coliform suppression.
QC 5.3.4 If no positive tubes result from
potable water samples, perform
the MPN procedure, including
the Completed Test, quarterly on
all positive confirmed tubes from
at least one coliform-positive
water sample.
6. Sample Collection,
Handling, and Preservation
(applicable to those laboratories delegated
responsibility for sample collection. All
laboratories are responsible for items 6.4
and 6.5).
6.1 Sampling frequency must conform to
that specified by the regulations. Col-
lector is trained in sampling proce-
dures and approved by the appropriate
regulatory authority or its designated
representative.
6.2 Samples must be representative of the
potable water distribution system.
5.2 MF Procedure
5.2.1
29

-------
Recommended
CRITICAL ELEMENTS FOR CERTIFICATION
Water taps used for sampling are free
of aerators, strainers, hose attach-
ments, mixing type faucets and purifi-
cation devices. A steady water flow
should be maintained for at least 2
minutes to clear the service line before
sampling. Collect at least a 100 mL
sample, allowing ample air space to
facilitate mixing of sampling by shak-
ing. Immediately after collection, enter
on the sample report form the sample
site location, sample type (e.g., routine,
check), date and time of collection, free
chlorine residual, collector’s initials,
and any remarks.
6.3 Applicable State re9ulations pertaining
to chain-of-custody are followed.
6.4 The report form includes the date and
time of sample arrival at the laboratory
and the date and time analysis begins.
Record additional information as re-
quired by the NIPDWR, Section
141.33.
6.5 Holding/transit time between sam-
pling and analysis does not exceed 30
hours. If the laboratory is required by
State regulation to examine samples
after 30 hours and up to 48 hours, the
laboratory is to indicate that the data
may be invalid because of excessive
delay before sample processing. Sam-
ples arriving after 48 hours shall be
refused without exception and a new
sample requested.
7. Quality Assurance
7.1 The laboratory prepares and follows a
written GA plan (see Chapter Ill, sec-
tion on GA plans).
7.2 All items under Critical Elements for
Certification which are designated as
quality control by the “QC” notation
relating to analytical quality control
and quality control checks on media,
equipment, and materials, necessitate
written records which are retained by
the laboratory for 5 years.
QC 7.3 A quality control sample is ana-
lyzed annually (when available).
QC 7.4 An unknown performance evalu-
ation sample is satisfactorily
analyzed annually (when avail-
able).
8. Records and.
Data Reporting
Records of microbiological analyses must
be kept by the laboratory or must be acces-
sible to the laboratory for at least 5 years.
Actual laboratory reports may be kept, or
data may be transferred to tabular sum-
maries, provided that the following informa-
tion is included:
8.1 Date, place, and time of sampling,
name of persons who collected the
sample.
8.2 Identification of sample as to whether
it is a routine distribution system sam-
ple, check sample, raw or process
water sample, or other special purpose
sample.
8.3 Date of receipt of sample and analysis.
8.4 Laboratory and persons responsible for
performing analysis.
8.5 Analytical technique/method used.
8.6 Results of analysis.
9. Action Response to
Laboratory Results
Promptly notify the proper authorities of
unsatisfactory sample results on the basis
of MPN Confirmed Test or unverified MF
coliform data, and check sampling from the
same sampling point must be initiated.
Practices
All laboratories should perform a minimum
of 20 coliform examinations monthly, pref-
erably five per week, by either the MPN or
MF procedures to qualify for certification
and to maintain certification status. This
will insure that the analyst maintains ex-
pertise in water bacteriological methodol-
ogy.
The minimum number of coliform exami-
nations (20) may be performed on a variety
of water sample types collected from differ-
ent stages of the water treatment process,
raw source water, surface or ground water,
as well as potable water samples collected
from a distribution system.
1. Personnel
1.1 Analyst
The analyst performs microbiological
tests with minimal supervision.
AcademicTraining: Minimum of high
school education.
Joblraining: Oneweekoftraining in
microbiological analysis of drinking
water acceptable to the State (or U.S.
EPA for non-primacy States), plus a
minimum of 30 days on-the-job train-
ing. Personnel should take advantage
of sources available from Federal and
State regulatory agencies.
1.2 Supervisor/Consultant
Supervision by a professional scientist
experienced in water microbiology. If a
supervisor is not available, a consult-
ant having the same qualifications may
be substituted. State laboratory per-
sonnel would be a primary source for
consultations.
Academic Training: Minimum of a
bachelor’s degree in microbiology,
biology, chemistry, or a closely related
field.
Job Training: Minimum of two weeks
training from a Federal agency, State
agency, or academic institution in
microbiological analysis of drinking
water.
Experience: At least one year of bench
experience in sanitary (water, milk, or
food) microbiology.
2. Laboratory Facilities
Laboratory space should be adequate (200
ft 2 and 6 linear ft of bench per analyst) to
accommodate peak workload. Work space
should include sufficient bench-top area for
processing samples; storage space for
media, glassware, and portable equipment;
floor space for stationary equipment (incu-
bators, waterbaths, refrigerators. etc.); and
associated area for cleaning glassware and
for sterilizing materials. In small water plant
laboratories, the space required for labora-
tory analyses and preparation may be con-
solidated into one room with the various
functions allocated to different parts of the
room. Facilities should be clean, air-condi-
30

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RECOMMENDED PRACTICES
tioned, and with adequate lighting at the
bench top(100 ft. candles).
Laboratory safety should involve a con-
scious effort to safeguard against electrical
shock, fire, accidental chemical spills, and
to minimize microbiological hazards, facility
deficiencies, and equipment failures. While
safety is not an aspect of laboratory certif i-
cation, the evaluator should informally
indicate potential safety problems observed
during an on-site Visit.
3. Laboratory Equipment
and Supplies
Electrodes are maintained ac-
cording to manufacturer recom-
mendations.
QC 3.1.2 Date commercial buffer solution
container upon receipt and dis-
card before expiration date.
QC 3.1.3 Checkforaccuracyquarterly,
using NBS standard reference
materials.
3.2 Temperature Monitoring Device
3.2.1 The calibration of any continu-
ous recording device used to
monitor incubator temperature
should be checked annually by
determining whether it is sensi-
tive to within 1 °C of a reference
NBS thermometer.
3.3 Incubator Unit
3.3.1 A continuous recording device
should be used to monitor gen-
eral operation of incubator unit.
3.4 Autoclave
3.4.1 In addition to temperature
gauge, autoclave should have
pressure gauge. Avoid over-
crowding in autoclave, and
monitor temperature throughout
sterilization cycle.
QC 3.4.2 Use heat sensitive tapes, spore
strips or ampoules, or maxi-
mum-temperature-registering
thermometer during autoclave
cycle.
QC 3.4.3 Check automatic timing mecha-
nism with stopwatch.
3.5 Hot Air Oven
3.5.1 The oven should maintain a
stable sterilization temperature
(170°C-180°C). Sterilize only
dried items, avoid overcrowding,
and use heat sensitive tape to
insure sterilization time is at-
tained. The oven thermometer
should be graduated in at least
10°C increments, with the bulb
placed in sand during use.
QC 3.5.2 Record date, sterilization time
and temperature of each cycle.
3.6 Colony Counter
3.6.1 A colony counter, dark field
model, should be used to count
standard plate count colonies.
3.6.2 A mechanical hand tally for
counting bacterial colonies
should be used.
3.7 Membrane Filters and Pads
QC 3.7.1 Record lot number and date
received.
QC 3.7.2 Test recovery and performance
of membranes compared to a
previously acceptable lot.
4. General
Laboratory Practices
4.1 Sterilization Procedures
4.1 .1 As an alternative to autoclaving,
dried glassware can be sterilized
in an oven(170°-180°C for a
minimum of 2 hours).
4.1 .2 The membrane filter assembly
should be exposed to UV light or
boiling water for at least 2 min-
utes to prevent bacterial carry-
over between filtrations.
4.2 Laboratory Pure Water
QC 4.2.1 Test the bacteriological quality
of the laboratory pure water
monthly by the Use Test (EPA
Microbiological Methods for
Monitoring the Environment,
p. 203).
QC 4.2.2 If laboratory pure water does not
meet quality requirements, per-
form the following supplemen-
tary to determine cause:
Parameter Limits
Pb, Cd, Cr, Cu, Ni, Zn Not greater than
0.5 mg/I
Total metals not Equal to or less
limited to those above than 1.0 mg/I
pH 5.5-7.5
Standard Plate Count <1,000/mI
4.3 Dilution Water
OC 4.3.1 Perform sterility check by adding
20 ml of water to 100 mL
volume of non-selective broth,
incubate at 35° ± 0.5°C for 24
hours, and check for growth.
Discard if contaminated.
Media should be ordered on a
12-month need basis. Purchase
1/4 lb. bottles, except for large
volume uses, and date bottles
upon receipt and also when ini-
tially opened. Determine recov-
ery and performance of new
media compared to previously
acceptable lots by using positive
and negative control cultures.
4.4.2 Dehydrated media should be
discarded 6 months after open-
ing; if stored in a desiccator,
storage may be extended to 12
months. Discard unopened de-
hydrated media after 2 years.
4.4.3 Sterile flasks should be used for
preparation of MF medium.
5. Analytical Methodology
5.1 The analyst has the option of
conducting either the MPN or MF
procedure; however, the MF pro-
cedure is preferred when applic-
able because it permits analysis of
a larger sample volume in reduced
analytical time.
QC 5.2 Laboratories which conduct the
MF procedure and have two or
more analysts should analyze one
known coliform-positive sample
monthly and each analyst should
count the sheen colonies on the
same membrane. The counts
should agree within 10%. This
insures that the analysts are
capable of distinguishing sheen
from non-sheen colonies.
QC 5.3 At least one non-sheen colony of
each morphological type should
be verified monthly.
6. Sample Collection,
Handling, and Preservation
6.1 Samples should be iced during transit,
and refrigerated at 1 °C-5°C during
storage in the laboratory.
6.2 Samples delivered by collectors to the
laboratory should be analyzed on the
day of collection. (This item may be-
come a Critical Element for Certifica-
tion).
7. Quality Assurance
8. Records and
Data Reporting
Proper authorities should be alerted to the
occurrence of high background levels of
noncoliform organisms by the MF pro-
cedure; or turbid tubes lacking gas, using
the MPN procedure; or heterotrophic bac-
terial densities exceeding 500 colonies/mI.
9. Action Response
to Laboratory Results
Although check sampling is to be initiated
on the basis of MPN Confirmed Test and
unverified MF coliform counts, data used to
determine monthly compliance maybe
adjusted by conducting the Completed Test
for the MPN procedure and/or verifying MF
counts.
3.1 pH meter
3.1.1
4.4 Media
4.4.1
31

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Sample Forms for On-Site Evelu ‘ ion of Laboratories Involved in Analysis of Public Water Supplies—Microbiology
I
Telephone Number.
Survey By
a £tZi:_a.
Stata
Codes for Marking On-Site Evaluation Forms S - Satisfactory X - Unsatisfactory U - Undetermined NA - Not Applicable
1. Personnel
Position/title
Name
Academic training
HS BA/BS MA/MS Ph.D.
Present
speci&ty
Experience (years/area)
Laboratory
director
Supervisor/
consultant
Professionals
(note discipline)
Technician!
analyst
32

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Laboratory Evaluator ______________
Location Date __________________
2. Laboratory Facilities is Omitted
3. Laboratory Equipment, Supplies, and Materials
3.1 pHMeter
Manufacturer Model
Accuracy. ±0.1 unit -
Scale graduation, 0.1 units -
Use pH buffer aliquot only once -
QC Standardize pH meter each use period with pH 7.0 standard buffer
3.2 Balance (Top Loader or Pan)
Manufacturer Model..
Detects 100 mg at a 150 gram load -
QC Calibrate balance performance using Class S or S-i reference weights. If non-reference
weights used, they are calibrated initially with Class S or S-i reference weights. -
QC Service contract or internal maintenance protocol and record maintained
3.3 Temperature Monitoring Device
Glass/mercury or dial thermometer used in incubator units graduated in 0.5°C increments
No separation in mercury column -
QC Check calibration of glass/mercury thermometer annually and dial thermometer quarterly
against a reference NBS thermometer or one meeting NBS monograph 150 requirements
3.4 Incubation Unit
Manufacturer. -
Maintains internal temperature of 35° ± 0.5°C
Thermometers placed on top and bottom shelves in use area of non-portable incubators -
Immerse thermometer bulb in liquid -
Culture dishes and tubes fit snugly in aluminum block incubator -
QC Record temperature morning and afternoon for days in use -
3.5 Autoclave
Pressure cooker/vertical aUtoclave -
Manufacturer
Temperature gauge with sensor on exhaust -
Operational safety valve -
Maintains sterilization temperature during cycle
Completes entire cycle within 45 minutes when a 12-15 minute sterilization period is used -
Depressurizes sufficiently slowly to insure media do not boil over and bubbles do not form in
fermentation tubes -
Approval of pressure cookers and vertical autoclaves requires quality control data demon-
strating sterility and proper media reactions -
QC Record date, sterilization time, and temperature for each cycle -
QC Establish service contract or internal maintenance protocol -
3.6 Conductivity Meter
Manufacturer Model
Graduated in ohms or mhos; range of 2 ohms to 2 megohms or equivalent micromhos ± 1
percent; sensitivity of 0.33 percent or better
33

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3.7 Refrigerator
Maintain temperature at 1°C to 5°C
Thermometer graduated in 1° increments
Immerse thermometer bulb in liquid
QC Record temperature for days in use
3.8 Inoculating Equipment
Metal or plastic loops, or dry heat sterilized applicator sticks
3.9 Membrane Filtration Equipment
vwnuwcturer Type
Stainless steel, glass or autoclavable plastic
Units non-leaking, unscratched, not corroded
10 to 1 5X magnification device with fluorescent light source
Forceps, tips without corrugations
3.10 Membrane Filters and Pads
uYIdnu1d turer Type
Made from cellulose ester material, white, gridmarked, 47 mm diameter, 0.45 urn pore size.
Alternate pore size used
Membranes recommended by manufacturer for total coliform water analysis
Membranes and pads are presterilized or autoclaved
3.11 Culture Dishes
Presterilized plastic or sterilized glass dishes used
Loose-lid dishes incubated in a tight-fitting container
Glass culture dishes are sterilized in stainless steel or aluminum canisters or in heavy
aluminum foil or char-resistant paper
Open packs of disposableculture dishes are resealed between uses
3.12 Pipets
Glass pipets sterilized in stainless steel or aluminum canisters or individual
pipets wrapped in char-resistant paper
Reseal packs of disposable sterile pipets between major use periods
Pipets not etched, mouthpiece and tip are not chipped, graduation markings legible
3.13 Culture Tubes and Closures
Tubes are borosilicate glass or other corrosion-resistant glass
Culture tubes are of sufficient size that medium plus sample does not exceed 3/4 full
Closures are stainless steel, plastic, aluminum, or loosened screw caps with non-toxic liner
3.14 Sample Containers
Capacity at least 120 mL (4 oz.)
Wide-mouth plastic or glass bottle with screw cap or non-corrosive glass bottle
with ground glass stopper
Non-toxic liner in screw caps
Glass-stoppered bottle top covered with aluminum foil or char-resistant paper before
sterilization
3.15 Glassware and Plasticware
Glass made of borosilicate or other corrosive-resistant glass
Free of chips and cracks
Graduation marks are legible
Plastic items are clear and non-toxic
Graduated cylinders used to measure sample volume have a 2.5% tolerance or better
Pipets used to measure sample volumes have a 2.5% tolerance or better
34

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Laboratory.
Location Date ___________
4. General Laboratory Practices
4.1 Autoclave Sterilization Procedures at 121°C
Item Time
Membrane filter and pads 10 mm
Carbohydrate media 12-15 mm
Contaminated test materials 30 mm
Membrane filter assemblies 15 mm
Sample collection bottles 15 mm
Individual glassware 15 mm
Dilution water blanks 15 mm
Rinsewater 15mm
Autoclaved MF filters and pads and all media are removed immediately
after sterilization cycle
Membrane filter assemblies are sterilized at start of each filtration series
4.2 Sample Containers
Sodium thiosulfate added to sample containers before sterilization
QC At least one bottle per batch checked for sterility
4.3 Laboratory Pure Water
Laboratory pure water is used to prepare media, reagents, and dilution/rinse water
QC Requirements for laboratory pure water:
Parameters Frequency
(a) conductivity of>0.5 megohms or <2 micromhos at 25°C Monthly
(b) total chlorine residual non-detectable Monthly
(c) test for bacteriological quality for laboratory pure water, ratio of 0.8-3.0 Annually
4.4 Dilution/Rinse Water
Stock buffer prepared according to Standard Methods and/or EPA Manual 600/8-78-017
Stock buffer autoclaved or filter sterilized, labeled, and dated, and stock buffer
free of turbidity
Dilution/rinse Iater is prepared by adding 1.25 mL of stock buffer solution
and 5mL of MgCI 2 solution per liter of laboratory pure water
QC pH of stock buffer solution is 7.2 ± 0.2
QC pH dilution/rinse water 7.2 ± 0.2, adjust pH if necessary
QC Rinse water checked for sterility
4.5 Glassware Washing
Distilled or deionized water used for final rinse
QC Inhibitory residue test performed on clean glassware
4.6 Media (General Needs)
Commercially prepared dehydrated media used
Dehydrated media stored in cool, dry location
Check media pH, adjust if necessary
QC Record for media prepared:
(a) date of preparation
(b) type of medium
(c) lot number
(d) sterilization time and temperature
(e) final pH
(f) technician’s initials
35

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4.7 Membrane Filter Media
m-Endo broth or agar; final pH 7.2 ±0.2
m-Endo agar LES; final pH 7.2 ± 0.2
Dissolution of m-Endo broth or agar and m-Endo agar LES:
(a) boiling water bath
(b) direct heat
Use only ethanol
Membrane filter broth refrigerated no longer than 96 hours
Membrane filter agar refrigerated no longer than 2 weeks
Ampouled m-Endo broth refrigerated in accord with manufacturer’s expiration date
4.8 MPN Media
Lauryl tryptose (lauryl sulfate) broth
Lactose broth
Broth medium dispensed in volumes not less than 10 mL/tube
MPN media in tubes with loose-fitting closures used within one week
MPN media in screw cap tubes stored no longer than three months;
discarded if evaporation exceeds 10% of original volume
Overnight incubation at 35°C of refrigerated sterilized MPN media
Lauryl tryptose (lauryl sulfate) broth
(a) autoclave at 121°C for 12-15 minutes
(b) double strength; final pH 6.7 ± 0.2
Lactose broth
(a) autoclave at 121°C for 12-15 minutes
(b) double strength; final pH 6 7 ± 0.2
Brilliant green lactose bile broth
(a) autoclave at 121 °C for 12-15 minutes
(b) final pH 7.2 ± 0.2
Levine Eosin Methylene Blue (EMB) agar
(a) autoclave at 121°C for 12-15 minutes or use boiling water bath or
direct heat for dissolution
(b) final pH 7.1 ±0.2
4.9 Standard Plate Count Agar
Temper melted agar (44° to 46°C ) before pouring
Melted agar held no longer than eight hours
Do not melt sterile medium more than once
Autoclave at 121°C for 15 minutes, time adjusted depending on volume
Final pH 7.0 ± 0.2
36

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Laboratory Evaluator
Location Date
5. Analytical Methodology
5.1 Use approved ènalytical methodorogy
5.2 Approval for tentative and alternate methods and other modifications received
from the Alternate Test Procedure Program
5.3 Sample volume examined by MF is 100 mL ± 2.5 mL _____________
5.4 Coliforms detected by MF procedure reported as coliform density per 100 mL _____________
Confluent growth — membrane covered with bacterial growth
TNTC — greater than 200 total bacterial colonies ______________
(a) if reported as confluent growth or TNTC with less than 5 coliforms,
another sample requested from same sampling site
(b) if reported as confluent growth or TNTC with 5 or more coliforms,
indicate an MCL violation and a check sample requested from same sampling site _____________
5.5 Verification procedure conducted on all unsatisfactory samples
5.6 Completed MPN Test conducted on all unsatisfactory samples
QC 5.7 MF sterility check conducted at end of each filtration series ______________
6. Sample Collection, Handling, and Preservation
6.1 Follow sample procedures described in Standard Methods and EPA Manual 600/8-78-017 ______________
6.2 Sample collectors receive training
6.3 Samples representative of distribution system
6.4 Water taps free of any attachments and mixing type faucets ______________
6.5 Water run to waste for at least two minutes
6.6 Sample volume is at least 100 mL with sufficient space for mixing sample
6.7 Sample report form completed by collector ______________
6.8 Compliance with state chain-of-custody regulations, if required
6.9 Date and time of sample arrival at laboratory are recorded, date and time analysis
begins are recorded
6.10 Transit time does not exceed 30 hours _____________
If laboratory required by state regulation to examine samples after 30 hours
and up to 48 hours, data are indicated as possibly invalid
All samples arriving in laboratory after 48 hours are rejected and new samples reouested
37

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Laboratory Evaluator
Location ____________________________________________________
7. Quality Assurance Program
7.1 Written QA plan implemented and available for review _____________
7.2 Quality control records maintained for five years
QC 7.3 One quality control sample analyzed per year (when available) for parameter(s) measured _____________
QC 7.4 Analyze one unknown performance sample satisfactorily per year (when availabl.
for parameter(s) measured _____________
8. Data Reporting
8.1 Data entered on the sample report form is checked and initialed _____________
8.2 Sample report forms are retained by laboratory or State program for five years
9. Action Response by Laboratory
9.1 The proper authorities notified of unsatisfactory results
9.2 Proper authorities notified of check sample results
38

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Chapter VI
Radiochemistry
Critical Elements for Certification
T he technical criteria in this chapter are
divided into two sections: Critical Ele-
ments for Certification and Recommended
Practices. Only the first section will be used
to determine certification status.
1. Personnel
Although there are no critical elements for
laboratory personnel, laboratory adminis-
trators and evaluators should recognize
training and experience as essential to the
acquisition of valid compliance monitoring
data. Recommended minimum standards
can be found in the Recommended Prac-
tices section.
Laboratory Facilities
The analysis of compliance monitoring
samples should be conducted in a
laboratory facility where security and
integrity of the drinking water samples
and analytical data are provided. In
addition, a work-place for wet chemis-
try operations and for equipment that
is critical to valid measurement of
radioactive contaminants is necessary.
2.2 The counting instrument(s) necessary
for measurementof those radionuclides
described in the NIPDWR must be lo-
cated in a room other than the one in
which samples and standards are being
prepared and in which othertypes of wet
chemical analyses are being performed.
All instruments should be properly
grounded, and a regulated power sup-
ply, either external or internal, should be
available to each instrument.
2.3 In areas where radioactive standards
are being prepared, care must be taken
to minimize contamination of surfacds,
other samples and personnel. Either
bench surfaces of an impervious mate-
rial covered with absorbent paper, or
trays (stainless steel, plastic, or fiber-
glass) lined with absorbent paper are
acceptable.
2.4 The following items are necessary in a
laboratory performing even the most
basic radiochemical measurements
(gross alpha and gross beta radio-
activities) for compliance monitoring of
drinking water supplies.
2.4.1 Sink with tap water and connec-
tion to the sanitary sewer
system.
2.4.2 Electrical outlets (120 VAC
grounded).
2.4.3 Souróe of distilled or deionized
water.
2.4.4 Exhaust hood.
2.4.5 For laboratories that are per-
forming wet chemistry separa-
tions that require filtration of a
precipitated fraction of the
sample, a vacuum source (pump
or aspirator) should also be
available.
3. Laboratory Equipment
and Supplies
The following equipment and supplies are
necessary for the analyses of regulated
radionuclides. If a laboratory is not to be
certified for a particular radionuclide pa-
rameter, instruments specified for analysis
of that parameter are not necessary.
3.1 General Instrumentation and
Equipment:
3.1.1 Analytical balance: Precision,
±0.05 mg. Minimum scale
readability, 0.1 mg.
3.1.2 pH meter or specific ion meter:
3.1.2.1 pH meter: Accuracy,
± 0.5 units. Scale read-
ability, ±0.1 units.
3.1.2.2 Specific ion meter: Ex-
panded scale millivolt
capability. Readable
and accurate to ± 0.1
mV.
3.1.3 Conductivity meter: Readable
in ohms or mhos, a rai ge of up
to 2 million ohms or down to
0.5 micromhos ± 1 percent,
and a sensitivity of 0.33 per-
cent of full scale or better.
3.1.4 Drying oven or lamp: Gravity
convection type, or infrared
drying lamp.
3.1.5 Desiccator: Glass or plastic
models, depending on particu-
lar application.
3.1.6 Hot Plate: Units with selectable
temperature control for safe
heating of laboratory reagents
and samples.
3.1.7 Glassware: Borosilicate type
glass. All volumetric glassware
should be marked Class A,
denoting that it meets Federal
specifications and need not be
calibrated before use.
3.1.8 Muffle furnace: Automatically
controlled with a chamber ca-
pacity of at least 2,200cc (10 x
9.5 x 23) and a maximum oper-
ating temperature of 1,000°C
continuous and 1,100°C inter-
mittent.
3.1.9 Centrifuge: General purpose
table-top model with a maxi-
mum speed of at least 3,000
rpm and a loading option of 4 x
50 ml.
3.1.10 Fluorometer: Capable of de-
tecting 0.0005 microgram of
uranium.
3.2 Radiation
Counting Instruments
The types of radiation counting systems
needed to comply with measurements
described in the NIPDWR, are set forth
below.
3.2.1 Liquid scintillation system: A liquid
scintillation system is essential if the
laboratory is to be certified for the
measurement of tritium in drinking
water samples. The system must be
such that the sensitivity will meet or
exceed the requirements of section
141.25 of the NIPDWR.
3.2.2 Gas-flow proportional counting sys-
tem: A gas-flow proportional count-
ing system may be used for the meas-
urement of gross alpha and gross
beta activities, radium-226, radium-
228, strontium-99, strontium-90,
cesium-i 34, and iodine-i 31 as de-
scribed in the reference cited in sec-
tion 141.25(a). The detector may be
either a “windowless” (internal pro-
portional counter) or a “thin window”
type. A combination of shielding and
a cosmic (guard) detector operated in
anticoincidence with the main detec-
tor must be used to achieve low back-
ground beta counting capability. The
alpha and beta background count of
the system must be such that the
sensitivity of the radioanalysis of
water samples will meet or exceed
the requirement of section 141.25 of
39

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CRITICAL ELEMENTS FOR CERTIFICATION
the NIPDWR with reasonable count-
ing time (not more than 1000 min-
utes)..
3.2.3 Alpha scintillation counting system:
For measurement of gross alpha
activities and radium-226, a scintilla-
tion system designed for alpha count-
ing 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 placec
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, preamplifier, ampli-
fier, timer and scaler).
3.2.4 Low background alpha and beta
counting systems other than a gas-
flow proportional counting system:
Such a system should have a cosmic
guard detector operated in anti-
coincidence with the signal from the
sample detector, and shielding, such
that the alpha background will not
exceed 0.2 cpm and the beta back-
ground will not exceed 2.0 cpm for a
2 inch diameter counting planchet
geometry.
3.2.5 Scintillation cell system: A scintilla-
tion system designed to accept scin-
tillation flasks (“Lucas cells”) should
be used for the specific measurement
of radium-226 by the radon emana-
tion method. The system consists of a
light-tight enclosure capable of ac-
cepting the scintillation flasks, a
detector (phototube), and the appro-
priate electronics (high voltage sup-
ply, amplifier, timers, and scalers).
The flasks (cells) needed for this
measurement may either be pur-
chased from commercial suppliers or
constructed by the laboratory.
3.2.6 Gamma spectrometer systems:
Either a sodium iodide, Nal(Tl), crys-
tal; a solid state lithium drifted ger-
manium detector; or a gamma-X
photon detector connected to a Multi-
channel analyzer is required if the
laboratory is to be certified for anal-
yses of man made photon emitters.
3.2.6.1 If a sodium iodide detector is
used, a cylindrical 7.5 cm x
7.5 cm Nal crystal is satisfac-
tory. However,al0cmx 10
cm crystal is recommended.
The detector should be
shielded with a minimum of
10cm 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 30cm. The multichan-
nel analyzer, in addition to
appropriate electronics,
should contain a memory of
not less than 200 channels
and at least one readout
device.
3.2.6.2 A system with a lithium
drifted germanium, or a high
purity germanium, or a
gamma-X photon detector
may be used for measure-
ment of manmade photon
emitters if the efficiency of
the detector is such that the
sensitivity of the system
meets the minimum detecta-
ble activity requirements
cited in section 141.25 of the
NIPDWR. These detectors
should be shielded with a
minimum of 10cm of iron or
equivalent. The multichannel
analyzer, in addition to ap-
propriate electronics, should
contain a memory of not less
than 2000 channels and at
least one readout device.
4. General
Laboratory Practices
Laboratory practices are specified in the
Recommended Practices section.
5. Analytical Methodology
The approved mqthods indicated in the
NIPDWR or U.S. EPA-approved alternate
methods, are to be used for drinking water
compliance monitoring.
6. Sample Collection,
Handling, and Preservation
Table Vl-1 gives critical elements for sam-
ple handing including Preservation, and
Applicable Counting Instrumentation.
7.1 Quality control data and records must
be available for inspection.
7.2 A laboratory must participate at least
twice each year in those U.S. EPA labo-
ratory intercomparison cross check
studies that include each of the anal-
yses for which the laboratory is, or
wants to be, certified. Analytical re-
sults must be within control limits
described in “Environmental Radio-
activity Laboratory Intercomparison
Studies Program-FY-1 981-1982”
(EPA-600/4-81 -004), or in subse-
quent revisions.
7.3 A laboratory must also participate once
each year in an appropriate water
supply performance evaluation (blind
sample) study administered by U.S. EPA.
Analytical results must be within con-
trol limits established by U.S. EPA for
each analysis for which the laboratory
is, or wants to be, certified.
7.4 Operating manuals and calibration
protocols for counting instruments
should be available to analysts and
technicians.
7.5 Calibration data and maintenance
records on all radiation instruments
and analytical balances should be
maintained in a permanently bound
record.
7.6 The following specifications are in-
cluded in minimum daily quality con-
trol:
7.6.1 A minimum of 10-percent dupli-
cate samples should be analyzed
to verify internal laboratory
precision for a specific analysis.
The difference between dupli-
cate measurements must be
less than two times the stand-
7. Quality Assuranàe
Table Vl-1
Parameter Prsssrvative’ Container 2 Instrumentation 3
Gross alpha Conc. HCI or HNO 3 to pH <2 P or G A, B or G
Grossbeta Conc.HCIorHNO 3 topH<2 PorG AorG
Strontium-89 Conc. HCI or HNO 3 to pH <2 P orG A orG
Strontium-90 Conc. HCI or HNO 3 to pH <2 P or G A or G
Radium-226 Conc. HCI orHNO 3 to pH <2 P or G A, B, D or G
Radium-228 Conc. HCI or HNO 3 to pH <2 P or G A orG
Cesium-i 34 Conc. HCI to pH <2 P or G A, C or G
lodine-131 None PorG AorG
Tritium None P or G E
Uranium Conc.HCI0HNO 3 topH<2 PorG F
Photon emitters Conc. HCI or HNO 3 to pH <2 P or G C
‘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 ori9inal container) 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.
= Low background proportional system; B = Alpha scintillation system; C = Gamma spectrometer (Nal(Tl) or
Ge(U); D = Scintillation cell (radon) system; E = Liquid scintillation system (section C.2.a); l = Fluorometer (section
C.1 .i) G = Low background alpha and beta counting system other than gas-flow proportional.
4 1f H is used to acidify samples which are to be analyzed for gross alpha or gross beta activities, the acid salts must
be converted to nitrate salts before transfer of the samples to planchets.
40

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ard deviation of the specific
analysis as described in EPA-
600/4-81 -004, Table 3. If differ-
ence exceeds two standard
deviations, prior measurements
are suspect, calculations and
procedures should be examined
and samples should be reana-
lyzed when necessary.
7.6.2 When 20 or more specific anal-
yses are performed each day, a
counting standard and a back-
ground sample should be meas-
ured with each 20 samples. If
less than 20 specific analyses
are performed in any 1 day, a
counting standard and a back-
ground sample should be meas-
ured along with the samples.
7.7 Quality control performance charts, or
performance records, should be main-
tained for each instrument.
7.8 The laboratory should prepare and
follow a written QA plan (see Chapter
Ill, section on QA plan).
8. Records and Data Reporting
8.1 Compliance monitoring activities
should be made legally defensible by
the records kept of such activities.
8.2 Recb!ds of radioanalyses for compli-
ance monitoring of drinking water
supplies must be kept by the laboratory
for not less than three years. This
includes raw data, calculations, quality
control data, and reports.
8.3 Actual laboratory reports may be kept,
or data may be transferred to tabular
summaries provided that the following
information is included:
8.3.1 Date, place, and time of sam-
pling; name of person who col-
lected the sample.
8.3.2 Identification of sample as to
whether it is a routine distribu-
tion system sample, check sam-
ple, raw or process water sam-
le, surface or ground water
sample, or other special pur-
pose sample.
8.3.3 Date of sample receipt and
analysis.
8.3.4 Laboratory and persons respon-
sible for performing analysis.
8.3.5 Analytical technique/method
used.
8.3.6 Results of analysis.
9. Action Response to
Laboratory Results
When action response is a designated labo-
ratory responsibility, the proper authority
must be promptly notified of non-compli-
ance sample results, and a request must be
made for resampling from the same sam-
pling point.
Recommended
Practices
The following items and procedures are
considered to be good laboratory practices
and are therefore recommended.
All laboratories are urged to maintain and
continually improve their personnel, facili-
ties, equipment, instrumentation, and
quality control procedures. To ensure con-
tinued production of scientifically and
legally defensible data, an ongoing training
program should be an integral part of a
laboratory’s program.
Analyst or technician responsible only
for the measurement of gross alpha
and gross beta radioactivities.
1.1.1 Academic training: Minimum of
a high school diploma or its
equivalent, plus at least 2 weeks
of specialized training in stand-
ards and sample preparation,
instrument calibration, calcula-
tions, and data handling.
1.1.2 Experience: Minimum of 6
months of on-the-job.
1.2 Analyst or technician responsible for
the measurement of specific radio-
nuclides described in the National
Interim Primary Drinking Water Regu-
lations.
1.2.1 Academic training: Minimum of
bachelor’s degree in chemistry,
radiochemistry, radioisotope
technology, or its equivalent.
1.2.2 Experience:’ Minimum of 1 year
of appropriate experience in
radiation measurements and
radiochemical procedures.
This analyst may be assisted in routine
sample preparation and radioanalytical
procedures by one or more technicians with
at least the minimum qualifications de-
scribed in item 1.1, provided that such work
is directly supervised by the analyst.
1.3 Laboratory Supervisor, Manager, or
Director.
1.3.1 Academic training: Minimum of
bachelor’s degree or its equiva-
lent.
1.3.2 Experience:’ Minimum of 5
years of experience.
2. Laboratory Facilities
2.1 Space
Laboratory space should be adequate
(150 to 200 ft 2 per analyst is recom-
mended). This space should contain no
less than 15 linear ft of bench space.
2.2 Lighting
2.2.1 Lighting should be provided to
‘Each year of college-level training in related
scientific fields of demonstrated equivalency
shall be considered equal to 1 year of work exper-
ience. Such a substitution should not exceed
one-half of the required experience.
wet-chemistry laboratory rooms
to the extent of 100-150 foot
candles.
2.2.2 70-100 footcandles is usually
sufficient lighting for counting
rooms. Controlled variable light-
ing is recommended for count-
ing rooms in which liquid scintil-
lation counting instruments are
located.
2.3 Ventilation
2.3.1 An exhaust hood with a face
velocity of 80-100 feet per min-
ute and a maximum limit of 70
percent supplied outside air to
the exhaust hood should effect
an adequate ventilation in wet-
chemistry laboratory rooms, if
volatile chemicals are restricted
to exhaust hood use.
2.3.2 For other rooms in the laborato-
ry, including the counting rooms,
where people are working rou-
tinely, a 20 percent or more air
change per hour is recom-
mended.
2.4 Temperature of this room should not
exceed 26.7°C (80°F). Temperature
variation under normal operating con-
ditions should not exceed 5°C (90 F) per
day.
3. Laboratory Equipment
and Supplies
3.1 Safety cans and safety storage cabi-
nets should be available and readily
accessible to taboratory analysts for
the safe use of volatile and flammable
solvents.
3.2 Eye wash equipment and showers
should also be readily accessible to
laboratory personnel.
3.3 Fire protection and explosion protec-
tion equipment should also be readily
available.
4. General
Laboratory Practices
The following general laboratory practices
are recommended:
4.1 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 clean-
ing procedure is sufficient for most
analytical needs. However, specific
analytical methods may dictate the
need for more elaborate procedures for
ensuring cleanliness of glasswa
such as hot acid wash followed by tap
water and distilled water rinses.
4.2 Water quality: All water used in prepa-
ration f reagents, standards, and
samples should have resistance values
1. Personnel
1.1
41

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RECOMMENDED PRACTICES
between 0.5 and 2.0 megohms (2.0
and 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 labora-
tory should request a list of quality
specifications for water purchased and
periodically check actual quality
against these specifications.
4.3 Chemicals and reagents: “Analytical
reagent grade’ (AR) chemicals should
be used for most analyses. For more
detailed information on reagent grades,
consult the 14th edition of Standard
Methods for the Examination of
Water and Wastewater. Individual
analytical procedures in Standard
Methods often specify special require-
ments for reagents to be used.
4.4 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.
4.5 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 radio-
active contamination. Provisions
should be made for safe storage and
disposal of radioactive wastes and for
monitoring of the work area.
4.6 High and Low Level Radioactive Mate-
rial: Environmental samples (such as
drinking water samples) that are to be
analyzed for radioactivity content
should be protected from other sam-
ples (and standard solutions) that con-
tain significantly higher levels of radio-
activity. Separate designated areas
(separate rooms if possible) should be
made available in the laboratory when
routine samples of significantly differ-
ent radioactivity levels are being
brought into the laboratory.
5. Analytical Methodology
6. Sample Collection,
Handling, and Preservation
7. Quality Assurance
The following practices are recommended:
7.1 A current service contract should be in
effect on all be lances.
7.2 Class S weights should be available to
make periodic checks on balances and
a record of such checks should be kept
in a bound logbook.
7.3 Chemicals should be dated upon re-
ceipt of shipment and replaced when
needed or before shelf life has been
exceeded.
7.4 An electronics technician should be
available or a service contract should
be in effect for all major instruments.
Sample Forms for On-Site Evaluation of Labo
ratories Involved in Analysis of Public Water
Supplies—Radiochemistry
Laboratory
Street
City
State
.
Survey By
Affiliation
DatA
Telephone No.
8. Records and
Data Reporting
9. Action Response
to Laboratory Results
42

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Laboratory
Location —
Personnel
flatA
Position/title
Nam.
Academic training
HS BA/BS MA/MS Ph.D.
Present

ExperIence (years and area)
Analyst(s)!
technician(s)
Supervisory
analyst
Laboratory
supervisor!
director
Support
(e.g.. electronic
technician)
43

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Laboratory.
Laboratory Facilities
Item
AV&IbIS
Y.s No
Cmnsots
Laboratory
Sink — with tap water
and sanitarysewer
connections
1—
Electrical outlets —
1 20V ac. grounded
Distilled or deionized
water
.
Exhaust hood
Vacuum source
Counting Room
Separate from wet chemis-
try, sample and standards
preparation area
Regulated power
supply
Adequate electrical ground
44

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Evaluator
Date ____
Laboratory
Location
General Laboratory Equipment and Instruments
.
No.ot
Units
Manufacturer
Model
Ageand Condition
Analytical balance
pH meter
Specific ion meter
conductivity meter
Drying oven
Infrared lamp
)esiccator
ot plate
.
Viuffle furnace
entrifuge
Fluorometer
45

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Laboratory
Date
Thin Window Gas-Flow Proportional Counter
ktsfrument number
Manufacturer
Model
Year Sample changing
Manual Automatic Capacity
Counting gas
Window density
(g/cm’)
Instrument
Op fJng voltage cpm
baCkground
Operating voltage Cpm
C a l enSta
Type:

Supplier:
Mpha
Beta
Calibration frequency’ Service Maint.nanc. frequency’ Condition’
D W M Otber 0 8 A Other G R N
‘Daily, weekly, monthly. Are operating manuals readily available to the operator? Yes ö No o
‘Quarterly, semiannually, annually. Are calibration protocols availabln to the operator? Yes No o
‘Good operating but needs repair, not operating. Are calibrations kept in a permanent control chart record? Yes o No o
Are permanent service maintenance records kept on these systems? Yes o No o
Windowless Gas-Flow Proportional Counter
Instrument number
Manufacturer
Model

Year
Sample changing
Manual Automatic Capacity
I I
Counting gs
Sample dish
diameter (In)
Alpha Instrument background Beta
Operating voltage cpm Operating voltage cpm
a n d erd
Type:

Supplisr:
Mpha
Beta
.
Calibration frequency’ Service Maintenance frequency’ Conditio n 3
D W M Other 0 S A Other G R N
‘Daily, weekly, monthly.
Are operating manuals readily available to the operator?
Yes o
No o
‘Quarterly, semiannually, annually.
Are calibration protocols available to the operator?
Yes o
No o
‘Good operating but needs repair, not operating.
Are calibrations kept in a permanent control chart record?
Are permanent service maintenance records kept on these systems?
Yes o
Yes o
No o
No
Location Evaluator
46

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Laboratory
Date
Location Evaluator —
Low Background Alpha and Beta Counter (other than gas-flow proportional)
Instrument number
Manufacturer Model
Year
Sample changing
Manual Automatic Capacity
I
Sample dish Instrument background
diameter (in.) Operating vol ge cpm Operating vot . cpm Operating cpm
Calibration Standard
Type:

Supplier:
Alpha
Beta
1
I
Calibration frequency’ Service Maintenance frequency 2 Condition 3
D W M Other Q S A Other 0 R N
‘Daily, weekly, monthly. Are operating manuals readily available to the operator? Yes ci No ci
2 Ouarterly, semiannually, annually. Are calibration protocols available to the operator? Yes ci No ci
3 Good operating but needs repair, not operating. Are calibrations kept in a permanent control chart record? Yes ci No ci
Are permanent service maintenance records kept on these systems? Yes ci No ci
Liquid Scintillation Counter
Instrument number
Manufacturer Model Year
Sample changing
Manual Automatic Capacity
I I
Discriminator channels
1 2 3
Data readout .
Channel pnntout
Visual 2 3
External standard
Yes No
Refrigeration
Yes No
Calibration Standard
Type:
Su her ’
pp.
Calibration frequency’
D W M Other
5e,vtce Maintenance frequency2
Q S A Other
Condftion3
G R N
I I
•
J___
‘Daily, ieekly, monthly.
Are operating manuals readily available to the operator?
Yes ci
No ci
2 Quarterly, semiannually, annually.
Are calibration protocols available to the operator?
Yes ci
No ci
3 Good operating but needs repair, not operating.
Are calibrations kept in a permanent control chart record?
Are permanent service maintenance records kept on these systems?
Yes ci
Yes ci
No ci
No ci
47

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Laboratory
Date
Alpha Scintillation Counter
Instrument number
Manufacturer
Model Veer
SatflPIS changing
Manuel Automatic Capacity
I
Alpha phosphor location
Photo tube Samples
Instrument backglound
Operating voltage cpm
C bm t i o n Standard
Type:

•
Calibration frequency’ Service Maintenance frequency 2 CondItion 3
D M Othsri Q S A iO H N IN
‘Delly, weekly, monthly. Are operating manuals readily available to the operator? Yes 0 No a
2 Quarterly, semiannually, annually. Are calibration protocols available to the operator? Yes 0 No a
3 Good operating but needs repair, not operating. Are calibrations kept in a permanent control chart record? Yes a No a
Are permanent service maintenance records kept on these systems? Yes a No a
Radon Gas-Counting System
System number
Counting
Make Model Year
Gas-counting ceus/system
Manufacturer of gas-counting cells
.
Calibration Standard
Type:
Supplier:
Calibration frequency 1
D W I d Other
Service Maint.nance frequency 2
0 S A Other
Condition 3
G N N
‘Daily,, weekly, monthly.
Are operating manuals readily available to the operator?
Yes
o No C)
2 Quarterly, semiannually, annually.
Are calibration protocols available to the operator?
Yes
.o
No ii
3 Good operating but needs repair, not operating.
Are calibrations kept in a permanent control chart record?
Are permanent service maintenance records kept on these systems?
Yes
Yes
a
a
No a
No a
Location
48

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Laboratory
Date
Location
Evaluator
Gamma
Spectrometer
Systems
DectorSystem
Type
Make
Make
Model
I
System number
Model Year
I
Analyzer System
Year
F
Size
Channels
Calibration Standard
Type:
Supplier:
Calibration frequency’
D W M Other
Q
Service Maintenance frequency 2
S A Other
G
Cond ition 3
R
N
‘Daily, weekly, monthly.
‘Quarterly, semiannually, annually.
Are operating manuals readily available to the operator?
Are calibration protocols available to the operator?
Yes El
Yes a
No 0
No a
‘Good operating but needs repair, not operating.
Are calibrations kept in a permanent control chart record?
Are permanent service maintenance records kept on these systems?
Yes o
Yes a
No a
No a
49

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Laboratory Date —
Location Evaluator
Sample Handling and Preservation
Paramstsr
Container
Used
preservative
Used
Comments
Satisfactory
Yes No
Gross alpha activity
Gross beta activity
Strontium-89
Strontium-90
Radium-226
Radium-228
Cesium-i 34
lodine-131
Tritium
Uranium
Photon emitters:
a.
b.
C.
d.
.
e.
50

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Laboratory
Met odoIogy
Parameter
Sampi. ‘ -
per Month
Method’ used. Cite Edition. Year. and 2 Approved Other
EPA APHA ASTM HASL-300 Alternate
Satisfactory
Yes No
Gross alpha
activity
Gross beta
activity
.
Strontium-89
:
Strontium-90
Radium-226
Radium-228
Cesium-i 34
lodir te - 131
Tritium
Uranium
Photon
emitters
(identify):
a.
b.
C.
d.
e.
‘Methods used, other then approved alternate methods, must be referenced n the Drinking Water Regulations (Federal Register)
aCite approval date.
Location
Date —
Evaluator
51

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Laboratory Date —
Location Evaluator
Quality Control
Item.
Cross Check Studies
(water) A 1 B 2
Performance (Bled)
Studies (Water) A 1 B 2
Participation in
intercomparison
(cross check) studies
and performance
(blind) studies
(studies conducted
by EMSL-LV)
Reporting Period:
Gross alpha
Gross alpha
Gross beta
Gross beta
Sr-89
Sr-89
Sr -90
Sr-90
Ra-226
Ra-226
Ra-228
Ra-228
Tritium
Uranium
Uranium
Cs-i 34
1-131
Cs-137
Cs-134
Co-60
Cs- 137
Ru-106
Co-60
Written QA plan implemented
and available for review
Ru-106
Verification of sample
results by duplicate
sample analysis
Yes
No
Frequency
Comments
Satisfactory
Yes No
Use of quality
control charts or
records
Calibration and
maintenance
records available ______ ______ ___________________________________ —
‘Scheduled frequency of participation by the L oetory. times per year.
2 Number of acceptable performsnces(resufts) in the past year, where an acceptable result isa normalized deviation from the known value of ( 3.0 sigma.
52

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Laboratory
Location —
Time of sampling
Date —
Evaluator
Person collecting sample
Date of receipt of sample
Date of analysis
Type of analysis
Laboratory and person
responsible
Method(s) used
Results
Data Reporting
Item
Comments: system(s) used, frequency. etc.
Records kept for 3 years
Actual laboratory reports
Tabular summary
Information included:
Date
Place of sampling
53

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Appendix A
Chain-of-Custody
A. Introduction
Written procedures for sample handling
should be available and followed whenever
samples are collected, transferred, stored,
analyzed or destroyed. For the purposes of
litigation, it is necessary to have an accu-
rate written record which can be used to
trace the possession and handling of sam-
ples from the moment of collection through
analysis. The procedures defined here
represent a means to satisfy this require-
ment.
A sample is in someone’s “custody’ it:
1. it is in one’s actual physical possession;
2. it is in one’s view, after being in one’s
physical possession;
3. it is in one’s physical possession and
then locked up so that no one can tamper
with it;
4. it is kept in a secured area, restricted to
authorized personnel only.
B. Sampling Collection,
Handling and Identification
1. It is important that a minimum number
of persons be involved in sample collection
and handliag. Guidelines established in
standard manuals for sample collection,
preservation and handling should be used.
(e.g., EPA NPDES Compliance Sampling
Inspection Manual, MCD 51; Standard
Methods for Examination of Water and
Wastewater). Field records should be com-
pleted at the time the sample is collected
and should be signed or initialed, including
the date and time, by the sample collec-
tor(s). Field records should contain the
following information:
(a) unique sample or log number;
(b) date and time;
(c) source of sample (including name, loca-
tion and sample type);
(d) preservative used;
(e) analyses required;
(f) name of collector(s);
(9) pertinent field data (pH, 00, Cl residual,
etc.);
(h) serial number on seals and transporta-
tion cases.
2. Each sample is identified by afflxing a
pressure sensitive gummed label or stand-
ardized tag on the container(s). This label
should contain the sample number, source
of sample, preservative used, and the collec-
tor(s’) initials. Analysis required should be
identified. Where a label is not available,
the same information should be written on
the sample container with an indelible
marking pen. An example of a sample iden-
tification tag is illustrated in Figure A-i.
3. The sample container should then be
placed in a transportation case along with
the chain-of-custody record form, pertinent
field records, and analysis request form.
The transportation case should then be
sealed and labeled. All records should be
filled out legibly in pen. The use of locked or
sealed chests will eliminate the need for
close control of individual sample contain-
ers. However, there will undoubtedly be
occasions when the use of a chest will be
inconvenient. On these occasions, the
sampler should place a seal around the cap
of the individual sample container which
would indicate tampering if removed.
C. Transfer of Custody and
Shipment
1. When transferring the possession of the
samples, the transferee must sign and
record the date and time on the chain-of-
custody record. Custody transfers, if made
to a sample custodian in the field, should
account for each individual sample, al-
though samples may be transferred as a
group. Every person who takes custody
must fill in the appropriate section of the
chain-of-custody record.
2. The field custodian (or field sampler if a
custodian has not been assigned) is re-
sponsible for properly packaging and dis-
patching samples to the appropriate labora-
tory for analysis. This responsibility includes
filling out, dating, and signing the appropri-
ate portion of the chain-of-custody record.
A recommended chain-of-custody format is
illustrated in Figure A-2.
3. All packages sent to the laboratory
should be accompanied by the chain-of-
custody record and other pertinent forms. A
copy of these forms should be retained by
the field custodian (either carbon or photo-.
copy).
4. Mailed packages can be registered with
return receipt requested. If packages are
sent by common carrier, receipts should be
retained as part of the permanent chain-of-
custody documentation.
5. Samples to be transported must be
packed to prevent breakage. If samples are
shipped by mail or by other common carrier.
the shipper must comply with any applica-
ble Department of Transportation regula-
tions. (Most water samples are exempt
unless quantities of preservatives used are
greater than certain levels.) The package
must be sealed or locked to prevent tamper-
ing. Any evidence of tampering should be
readily detected if adequate sealing devices
are used.
6. If the field sampler delivers samples to
the laboratory, custody may be relinquished
to laboratory personnel. If appropriate per-
sonnel are not present to receive the sam-
ples. they should be locked in a designated
area of the laboratory to prevent tampering.
The person delivering the samples should
make a log entry stating where and how the
samples were delivered and secured. Labo-
ratory personnel may then receive custody
by noting in a logbook the absence of evi-
dence of tampering, unlocking the secured
area, and signing the custody sheet.
D. Laboratory Sample
Control Procedures
Sample control procedures are necessary in
the laboratory from the time of sample
recelpt to the time the sample is discarded.
The following procedures are recommend-
ed for the laboratory:
1. A specific person must be designated
custodian and an alternate designated to
act as custodian in the custodian’s absence.
All incoming samples must be received by
the custodian, who must indicate receipt by
signing the accompanying custody/control
forms and who must retain the signed
forms as permanent records.
2. The custodian must maintain a perma-
nent logbook to record, for each sample,
the person delivering the sample, the per-
son receiving the sample, date and time
received, source of sample, date the sample
was taken, sample identification or log
number, how transmitted to the laboratory,
and condition received (sealed, unsealed,
broken container, or other pertinent re-
marks). This log should also show the
movement of each sample within the labo-
ratory; i.e., who removed the sample from
the custody area, when it was removed,
when it was returned, and when it was
destroyed. A standardized format should be
established for logbook entries.
3. A clean, dry, isolated room, building,
and/or refrigerated space that can be se-
curely locked from the outside must be
designated as a “custody room.”
4. The custodian must ensure that heat-
sensitive samples, light-sensitiv’ samples,
radioactive samples, or other sample mate-
rials having unusual physical characteris-
tics, or requiring special handling, are
properly stored and maintained prior to
analysis.
5. Distribution of samples to the analyst
performing the analysis must be made by
the custodian.
6. The laboratory area must be maintained
as a secured area, restricted to authorized
personnel only.
54

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7. Laboratory personnel are responsible for
the care and custody of the sample once it is
received by them and must be prepared to
testify that the sample was in their posses-
sion and view or secured in the laboratory
at all times from the moment it was re-
ceived from the custodian until the time
that the analyses are completed.
8. Once the sample analyses are com-
pleted. the unused portion of the sample.
together with all identifying labels, must be
returned to the custodian. The returned
tagged sample must be retained in the
custod ? room until permission to destroy
the sample is received by the custodian.
9. Samples will be destroyed only upon the
order of the responsible laboratory official
when it is certain that the information is no
longer required or the samples have deteri-
orated. (For example, standard procedures
should include discarding microbiological
samples after the maximum holding time
has elapsed.) The same procedure is true
for sample tags. The logbook should show
when each sample was discarded or if any
sample tag was destroyed.
10. Procedures must be established for
audits of sample control information. Rec-
ords should be examined to determine
traceability, completeness, and accuracy.
Figure A-I Sample Identification Tag Examples
Official Sample No.
IL l
U
D
0
U)
Date and Time
Office
Date and Time
Sampler’s Si nature Office
GENERAL CHEMISTRY
______________________________ PH Acid
2 Cond Alk
O TS SO 4
D I
4
SS F
• ___________________________ BOD 2 Cr.+6
Turb BOD 5
Sampler’s signature Color
Other Parameters:
MICROBIOLOGY
Official Sample No. Tot. Colif.
U Fecal Colif.
0
_________________________________ Fecal Strep.
I L ’
__________________________________ Salmonella
PESTICIDES. ORGANICS
Pesticides
0
O PCB’s:
w
4 Organics:
0 .
w
D
Official Sample No.
w
U
D
0
U)
Date and Time
Sampler’s Signature Office
EPA
Station No. Date Time Sequence No.
Station Location ________________Grab
Comp.
Remarks/Preservative:
BOD
_________Solids
______COD
_________Nutrients
_______Metals
_______Oil and Grease
______DO.
_______Bact.
_______Other
Samplers:
55

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Figure A-2 Chain-of-Custody Record
Survey Samplers: Signature
Station
Number
Station Location
Date
Time
Sample Type
Water Air
Comp. Grab
Seq. No.
No. of
Containers
Analysis
Required
Orig.—Acoompany Shipment
1 Copy—Survey Coordinator Field Files
by:
Signature
Received by: Signature
Date/Time
by:
Signature
Received by: Signature
Date/Time
by:
Signature
Received by: Signature
Date/Time
by:
Signature
Received by Mobile Laboratory for Field analysis:
Signature
Date/Time
by: Signature
Date/Time Received for Laboratory by:
Date/Time
Metnod of Shipment:
Dlstributiàn:
56

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Appendix B
Recommended
Protocol for Regions
Conducting On-Site
Laboratory
Evaluations
Before conducting the on-site evaluation,
the Region shall:
• Hold a pre-evaluation conference with
appropriate laboratory and field activity
representatives to establish a schedule that
would have a minimum impact on the labo-
ratory activities.
• Request that a variety of tests be sched-
uled during the on-site evaluation.
• Arrange for the laboratory staff to be
available during the on-site visit.
During the on-site visit, the team will:
• Evaluate the procedures and equipment
used for those specific analyses for which
the laboratory has requested certification,
using the criteria in this manual.
• Review the records and written standard
operating procedures for compliance with
the required sampling frequency, sample
collection, sample holding times, and if
appropriate, resample notification.
• Insure that the laboratory has a QA plan
in effect by:
— Determining if the laboratory has writ-
ten procedures (QA plan or equivalent) for
conducting its quality assurance program.
— Examining the quality assurance data to
determine if the quality assurance program
is being implemented.
• Complete the on-site checklists and other
evaluation forms during the visit (see Chap.
ters IV, V. and VI).
• Review the results of the evaluation with
the director of the laboratory, the director of
State water supply activities, and appro-
priate staff members. The review should:
— Discuss any deviations in the observed
procedures and records.
— Recommend changes in equipment and
supply needs, staffing requirements, and
facility improvements, if necessary.
— Discuss possible assistance the Region
can provide the laboratory.
Evaluation Report for Principal
State Laboratories and
Laboratories in Non-Primacy
States
After an on-site inspection, the evaluation
team should prepare a narrative report and
action memorandum. This report should
contain all information pertinent to the
evaluation and also recommend the certif i-
cation status for all analyses evaluated. The
report should then be forwarded for evalua-
tion to the Regional Director of the Environ-
mental Services Division and the Regional
Director of the Water Division. After consid-
ering the report, they should transmit it to
the Regional Administrator for action.
The Regional Administrator should de-
cide the certification status of the laboratory
within 30 days and notify the State. The
State should be sent the complete report. If
the report indicates that the laboratory not
be given Certified status for an analysis, the
Regional Administrator shall give the spe-
cific reasons.
The narrative report should be attached to
each copy of the completed evaluation form.
It should include the general headings and
information listed below:
Title Page
The title page should contain the following:
Report of an on-site evaluation of the
(name of laboratory)
at (city, State, and zip code)
on (date)
by
(name, title, organization,
and address
of the certification team)
Certification Status
List either Certified, Provisionally Certified,
or Not Certified for each contaminant
evaluated.
List of Deviations
List each deviation by item number used on
the evaluation checklists. Describe the
exact deviation and recommend changes.
Remarks
Recommend improvements which, while
not affecting certification status, would
improve laboratory operation. Other re-
marks might include reasons for failing the
on-site evaluation, special recognition for
outstanding performance, and description
of unusual tests.
List of Personnel
List name and title of personnel along with
the individual tests that ea’*i normally per-
forms. Also identify the critical laboratory
personnel.
Signature
Team members should sign the report.
Distribution
Copies of this report should be distributed to
the State requesting the evaluation and
EMSL-Cl. For local laboratories in non-
primacy States, reports should be distribu-
ted to appropriate Regional personnel.
Annually, each Region should submit to
ODW a brief listing of laboratories in the
Region having U.S. EPA or State certification
status. The listing shouldinclude the names
and location of each laboratory, and its
certification status for all regulated con-
taminants. In addition, Regions should
notify ODW of all changes in status soon
after they occur so that ODW can maintain
an updated list of certification status.
57

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Appendix C
Abbreviations
ATP—Alternate analytical procedures (or
techniques).
CA—Certifying authority. Regional Admin-
istrator for principal State laboratories and
laboratories in non-primacy States; EMSL-
a and EMSL-LV for Regional laboratories.
DWLCI—Drinking Water Laboratory Certi-
fication Implementation Work Group.
EMSL-Cl—Environrnental Monitoring and
Support Laboratory in Cincinnati. Ohio.
EMSL-LV—Environmental Monitoring Sys-
tems Laboratory in Las Vegas. Nevada.
MCL—Maximum Contaminant Level.
MEAL—Municipal Environmental Re-
search Laboratory in Cincinnati. Ohio.
NIPDWR—National Interim Primary
Drinking Water Regulations.
ODW—Off ice of Drinking Water.
ORD—Off ice of Research and Develop-
ment.
PE—Performance evaluation.
QA—Quality assurance.
QAMS—Quality Assurance Management
Staff.
QC—Qua lity control.
58 *U.S. Government Printing Office : 1983 —381-082/413

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