United States
Environmental Protection
Agency
Environmental Monitoring
and Support Laboratory
Cincinnati OH 45268
EPA-600/4 78-017
March 1978
Research and Development
c/EPA
Procedure for
the Evaluation of
Environmental Monitoring
Laboratories
Environmental Monitoring Series
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RESEARCH REPORTING SERIES
Research reports of the Office of Research and Development, U.S. Environmental
Protection Agency, have been grouped into nine series. These nine broad cate-
gories were established to facilitate further development and application of en-
vironmental technology. Elimination of traditional grouping was consciously
planned to foster technology transfer and a maximum interface in related fields.
The nine series are:
1. Environmental Health Effects Research
2. Environmental Protection Technology
3. Ecological Research
4. Environmental Monitoring
5. Socioeconomic Environmental Studies
6. Scientific and Technical Assessment Reports (STAR)
7. Interagency Energy-Environment Research and Development
8. "Special" Reports
9. Miscellaneous Reports
This report has been assigned to the ENVIRONMENTAL MONITORING series.
This series describes research conducted to develop new or improved methods
and instrumentation for the identification and quantification of environmental
pollutants at the lowest conceivably significant concentrations. It also includes
studies to determine the ambient concentrations of pollutants in the environment
and/or the variance of pollutants as a function of time or meteorological factors.
This document is available to the public through the National Technical Informa-
tion Service, Springfield, Virginia 22161.
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EPA-600/4-78-017
March 19"/8
PROCEDURE FOR THE EVALUATION OF
ENVIRONMENTAL MONITORING LABORATORIES
by
Charles Sicking, Steven Olin and Peter King
I
Tracer Jitco, Inc.
Rockville,. Maryland 20852
Contract No. 68-03-2171
Project Officer
Edward L. Berg
Quality Assurance Branch
Environmental Monitoring and Support Laboratory
Cincinnati, Ohio 45268
ENVIRONMENTAL MONITORING AND SUPPORT LABORATOTRY
OFFICE OF RESEARCH-AND DEVELOPMENT
U.S. ENVIRONMENTAL PROTECTION AGENCY
CINCINNATI, OHIO 45268
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DISCLAIMER
This report has been reviewed by the Environmental Monitoring and
Support Laboratory-Cincinnati, U.S. Environmental Protection Agency, and
approved for publication. Approval does not signify that the contents
necessarily reflect the views and policies of the U.S. Environmental
Protection Agency, nor does mention of trade names or commercial products
constitute endorsement or recommendation for use.
ii
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FOREWORD
Environmental measurements are required to determine the quality of
ambient waters and the character of waste effluents. The Environmental
Monitoring and Support Laboratory-Cincinnati conducts research to:
* Develop and evaluate techniques to measure the presence and
concentration of physical, chemical and radiological pollutants
in water, wastewater, bottom sediments and solid waste.
* Investigate methods for the concentration, recovery and identi"
fication of viruses, bacteria and other microbiological organisms
in water. Conduct studies to determine the responses of aquatic
organisms to water quality.
* Conduct an Agency-wide quality assurance program to assure
standardization and quality control of systems for monitoring
water and wastewater.
The latest quality assurance report on procedures for evaluation of
environmental monitoring laboratories was prepared by Tracer Jitco, Inc.
The report, in detail, contains registration and preliminary questionnaire
forms, on-site visit checklist, evaluator's guide, and a scoring system
for assessment of the laboratory's management, personnel, facilities,
analytical methodology and instruments, and its quality control procedures.
This research report is not an official EPA Manual. Rather, it is a
report which is but one of a series being used as input to develop EPA
Manuals and Guidelines for Certification Programs.
Dwight G. Ballinger
Director, EMSL-Cincinnati
11
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ABSTRACT
Tracer Jitco, Inc., examined in depth existing evaluation procedures
of EPA, Federal and State Agencies with the aim of incorporating their
best features in a procedure for general use in evaluating laboratories
engaged in measuring environmental pollution.
\ The procedures developed are suitable for the media of air, water,
radiation, and pesticides. They are intended for use by EPA Regions in
evaluating state laboratories and by the states in evaluating local or
private laboratories. They are useful as a management tool to control or
upgrade laboratory performance or they could be used as part of a labora-
tory accreditation or certification system.\ The inclusion of a scoring
plan makes it possible, with suitable training of evaluators in uniform
application of the procedures, to make comparisons with standards of
performance.
The laboratories are required to provide information on physical
plant, equipment, personnel, quality control and other general aspects of
laboratory performance on check-off types of forms provided. This is
followed by an on-site inspection during which information on less quanti-
fiable aspects are obtained. This phase of the evaluation is oriented to
the specific methodology for which the laboratory is to be qualified.
The scoring system includes inherent weighing of criteria. The
procedure is designed to be compatible with programs of proficiency
testing and taken as a part of a total quality assurance program will
contribute to the objectivity of the determination of laboratory capability.
This research report is not an official EPA manual. Rather, it is a
report which is but one of a series being used as input to develop EPA
Manuals and Guidelines for Certification Programs.
iv
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CONTENTS
Foreword ill
Abstract iv
Acknowledgements viii
1. Introduction 1
2. Conclusions 3
3. Background and Scope 4
Purpose of Evaluation 5
Intended Applications of Procedure 5
Use of Procedure 7
A. Registration and Preliminary Evaluation 9
Registration Form 11
Preliminary ques tionnaire 12
General Information about the Laboratory 13
Personnel 15
Laboratory Space and Facilities 17
Technical Service Offered 20
Instructions 20
Chart C: Table of Analytical Methods 23
Alternate Analytical Method 40
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Analytical Instruments and Special Apparatus 40
Index of Analytical Instruments and Special
Apparatus 42
Chart D: Analytical Instruments and Special
Apparatus 44
Internal and External Controls 66
Instructions 66
Chart E 67
5. Evaluator's Guide 69
General Information about the Laboratory 69
Personnel 72
Laboratory Space and Facilities 74
Analytical Methods 78
Forms for On-Site Evaluation 80
Medium-Water Chemistry 81
Medium-Water Bacteriology 87
Medium-Water Biology 97
Medium-Air Ill
Medium-Pesticides 115
Medium-Radiation 118
6. Instructions and Rating System 125
General Instructions 125
Specific Instructions and Rating System 127
Management and Organization Area 127
Technical Service Area 139
Internal and External Controls 145
Follow-up on Deficiencies 174
vi
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7. Calculation of Score 175
Acceptability of a Laboratory 175
Score Sheets 177
General Information about the Laboratory 177
Personnel 178
Laboratory Space and Facilities 179
Analytical Methods 180
Instruments 181
Internal and External Controls 182
Summary of Laboratory Evaluation 183
Bibliography 184
Appendix 189
vii
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ACKNOWLEDGMENTS
Thanks are due to the Project Officer, Mr. Edward Berg, and to the
staff of the Environmental Monitoring and Support Laboratory, Cincinnati,
for their support of this project. The many EPA Research Laboratories
and Regional Laboratories visited at various stages of development of
the procedure were all most generous in providing information and in
giving advise. We also found very helpful the review of the draft of
the procedure by the Wisconsin Department of Natural Resources and the
Illinois Environmental Protection Agency. We encountered many points
of view and have done our best to reconcile differences and to come up
with a procedure that is standardized, widely useful, and fair in its
application.
viii
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SECTION 1
INTRODUCTION
An evaluation procedure has been developed based on EPA experience in
evaluating its Regional Laboratories, the experience of other govern-
mental and private evaluating agencies, and the combined experience of
the contractor's senior staff.
Nevertheless, the result has been arrived at independently, specifi-
cally without reference to EPA's conclusions about its own evaluation efforts.
This was done consciously so that the result of the contractor's efforts
will stand on its own merits. Moreover, it has the advantage that a
completely disinterested point of view has been brought to bear on the
problem.
Two objectives of the project have had a strong bearing on the nature
of the procedure that has been developed:
1. A major objective was to produce combined forms containing
sections with general application and sections with applications
to specific media, in recognition of the fact that the areas of
uniformity in an evaluation protocol outweigh the differences
required by the media covered, namely air, water, radiation,
and pesticides.
2. A plan of scoring was required, using rating criteria based
on standards of acceptability in operation in EPA and else-
where and based on the contractor's own experienced judgment.
The resulting procedure has several unique aspects.
It collects information about areas of management, personnel,
facilities, methodology, instrumentation, and quality control
oriented toward the requirements of environmental monitoring
laboratories.
It presents criteria against which the individual laboratory
may be judged in each area.
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It contains an Evaluator's Guide which explains the intent
of inspection in each area and suggests specific questions
to be asked to enable the evaluator to arrive at the necessary
judgments.
It is sectionalized as to methodology and equipment so that
only the parts applicable to even a small laboratory or to
a laboratory devoted to a single medium need be used, thus
avoiding unnecessary burden on the laboratory.
The scoring system is adjustable to the size and scope of the
laboratory yet provides a final score which is comparable under
any circumstances of use of the procedure.
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SECTION 2
CONCLUSIONS
The procedure which has been presented in this manual is directly
applicable to the evaluation of laboratories of all sizes. In its
entirety it will apply to large laboratories. In this application it
is lengthy, but its length is justified by the necessity for a thorough
inspection of all aspects of laboratory personnel, facilities, equipment,
and operations. To do less would be to slight some important aspect and
make difficult a balanced, meaningful scoring system.
For smaller laboratories or specialized laboratories, only the appli-
cable portions of the procedure need to be used. The Registration Form
is intended to provide information that will make it necessary to send
out only the pertinent parts of the Preliminary Questionnaire. The
information provided by the Preliminary Questionnaire, assimilated by
the evaluator, or evaluation team, before the onsite visit should limit
the first hand inspection to the aspects of the laboratory's operations
that appear to deviate from standard.
When used conscientiously by evaluators with pertinent scientific back-
ground the procedure and its scoring system should result in the ability
to discern those laboratories that are acceptable participants in the
environmental monitoring programs.
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SECTION 3
BACKGROUND AND SCOPE
The pollution of the atmosphere, the contamination of the waters,
and the littering of the land have become problems international in
scope. The continued violence done by man to the total environment
must be checked if this planet is to remain a fit place in which to
live. One of the first steps that can be taken is the qualitative and
quantitative monitoring of the environment.
Successful monitoring of the environment requires the identifica-
tion of the contaminants, an accurate measurement of the amounts present,
and pin-pointing of the sources of the pollution. Because of the in-
crease in number of contaminating substances, many of which require
sophisticated analysis, and because of the reduction in levels of pol-
lution that can be tolerated, the involvement of an increasingly large
number of people and of laboratories is required.
In the United States, the U.S. Environmental Protection Agency
has the responsibility for enforcement of national laws and regulations
designed to restore and protect the environment. Its work is assisted
and supplemented by environmental programs carried out by the states.
The private sector is also depended upon to carry a part of the labora-
tory analytical workload. The wide diffusion of monitoring and analysis
leads to a need for standards of performance. Extensive laboratory
inspection and evaluation must be done to ascertain the capabilities of
the participating laboratories. In order to avoid arbitrary inspections
and to protect both the evaluating agency and the laboratories from
capricious judgements, this procedure which standardizes requirements
has been prepared.
The procedure provides a basis for inspection and evaluation of
environmental monitoring laboratories at national, state, and private
levels. It is applicable to laboratories concerned with the various
media, particularly air, water, pesticides, and radiation. The ex-
perience of EPA and of other standardizing institutions has been used
as a basis for this procedure. It is thorough, yet as concise as the
intended wide range of applicability permits.
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This procedure employs standards which will make evaluation as
objective as it can be made. It includes a scoring system for assess-
ment of the laboratory's management, personnel, facilities, analytical
methodology and instruments, and its quality control procedures. An
acceptable score will signify that there are no serious deficiencies
in the organization, physical plant, or technical operations of the
laboratory.
PURPOSE OF EVALUATION
Enhancement of the performance of environmental monitoring
laboratories is the primary goal of the laboratory evaluation. Its
purpose is to ascertain that the laboratory follows sound scientific
procedures in its analytical work; that it operates under the auspices
of good management and professional supervisors; that it utilizes proper
equipment; and that it maintains and uses accurate records. The evalua-
tion procedure provides the laboratory an opportunity for improvement by
identifying weaknesses in its organization or performance and to obtain
information and assistance for overall improvement. In this sense, the
evaluation may serve not only to assure laboratory competence; but also
to promote professionalism in the laboratory by facilitating the estab-
lishment of standards of excellence.
Any system designed for the evaluation of laboratories will in-
evitably identify certain laboratories which fail to meet the established
standards. This procedure for evaluation of laboratories does not
necessitate a definitive rejection of unqualified laboratories. It
provides an opportunity for the laboratory to correct existing deficien-
cies. If the laboratory complies with recommended modifications, it may
receive an acceptable rating.
The uniform scoring system employed in the procedure considers a
large number of characteristics which are given preassigned weights.
This contributes to the objectiveness and comparability of the evaluation
which are among its principal purposes.
INTENDED APPLICATIONS OF THE PROCEDURE
The procedure for laboratory evaluation is a versatile instrument.
The preliminary questionnaire coupled with the onsite checklists is
suitable to a number of situations. It may serve as a self-evaluation
for Environmental Protection Agency laboratories. It may be used by
EPA for the evaluation of state laboratories. It could be used by state
laboratory personnel to evaluate commercial laboratories. The procedure
was not designed for use in a formal certification program, however, it
could readily be adapted for that purpose.
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Although it is recognized that the different media of air, water,
pesticides, and radiation have some unique methodologies, the areas of
uniformity in all laboratories outweigh the differences and a generally
applicable procedure has been developed. Sections with application to
specific media can be used for inspection to the extent necessary.
The procedure does not purport to be a panacea. For example, al-
though recognition is given to the necessity for participation in inter-
laboratory proficiency testing programs,'the scores obtained in such
programs do not enter directly into the scoring recommended in this
procedure. The procedure simply provides a methodology necessary for
environmentally concerned scientists to ensure that a laboratory has
the capability for valid analyses. The combination of the score from
applying this procedure with scores from inter-laboratory testing pro-
grams should be the object of further consideration.
The extremely large number of data points collected may have to be
collated by computer. Although this is not one of the requirements of
this procedure, most of the data will have been recorded in such a way
that it can readily be computerized. Most of the answers to the ques-
tionnaire require only a checkmark and not involved descriptions of the
laboratory.
The media covered include the broad application of environmental
monitoring to air, water, pesticides, and radiation. This involves
chemical methodology appropriate to potable water, wastewater, ambient
water, ambient air, stack emissions and other source emissions into the
atmosphere, sediments, pesticides and other organic chemicals, both
natural and industrial. It involves biology, including aquatic biology
and virology. It also includes bacteriology as applied to potable water,
waste water and ambient water. Finally, it includes radiation measurement.
The analytical methodology required is in a state of flux. Some
methods are EPA approved, some are used as interim methods and others
are in various states of development and are in more or less wide use.
Although this procedure lends itself to the evaluation of performance
of all methodology required in the various areas, the material actually
presented on methodology is limited to those methods referenced in the
Federal Register. These are the presently EPA approved methods. For
water and radiation test methods, see Federal Register, Vol. 35, No. 199,
October 16, 1973. Interim methods for algicides, chlorinated organic
compounds, and pesticides can be obtained from the Environmental Monitor-
ing and Support Laboratory, USEPA, 1014 Broadway, Cincinnati, Ohio 45268.
Air test methods are referenced in Federal Register, Vol. 36, No. 228,
November 25, 1971 and Vol. 38, No. 110, June 8, 1973.
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Methods for measurement of emissions from stationary sources differ
in important aspects from methods for measurement in ambient air. These
source methods are to be found in Federal Register, Vol. 36, No. 247,
Part II, December 1971; Vol. 38, No. Ill, June 11, 1973; Vol. 39, No. 47,
March 8, 1974; Vol. 40, No. 152, August 6, 1975; and Vol. 40, No. 194,
October 6, 1975.
Biology is an important area not covered by referenced methods. How-
ever, see Bibliography items 6-7-8-9 for methods in use that may be
consulted for methodological requirements of satisfactory laboratory per-
formance in this area.
Modified or alternate methods ("equivalent" methods) may be used if
specifically approved under published regulations. A laboratory under
evaluation is required to provide information on any such methods in
use. The evaluator must refer to this information in order to judge
whether the laboratory's use of the methods produces satisfactory
results.
Although some state environmental monitoring laboratories are a
part of, or are closely associated with, Health Laboratories, this pro-
cedure is not intended for use in any health oriented analyses. Pro-
cedures exist for evaluation of health laboratories where this is required
for certification or licensing.
Although the word "laboratory" is used, it is emphasized that the
field aspects as well as the laboratory aspects of environmental monitor-
ing must be a part of any complete evaluation. The procedure developed
herein is compatible with the "total system" concept. The evaluator
should go into the field to look at monitoring equipment including flow
measurement instrumentation and automatic sample compositing equipment.
USE OF PROCEDURE
Experts, such as those found in the larger environmental protection
agencies, who are experienced in all of the media may not always be
available for inspection and evaluation duties. It may be necessary
to employ evaluators who have not had long years of experience in all
the details of methodology of environmental monitoring. Therefore, this
procedure has been designed for use by individuals who are skilled in
science, but who will find guidelines useful for the evaluation of
specialized laboratories. An elaborate "Guide for Evaluators" is an
essential part of the Manual.
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As a part of this "Guide" there is included, where available, very
detailed background material in some of the specialized methodologies.
For example, the EPA Check List for Bacteriological Examination of
Water is to be found in Part 4. Also, recommended laboratory performance
standards are included, such as "A Schedule of Suggested Instrument
Calibrations" and a "Table of Recommendations for Sampling and Sample
Preservation" from the EPA Manual of Methods for Chemical Analysis of
Water and Wastes. Other such helps could be added, if so desired, as
they became available.
The ideal evaluator should possess a broad understanding of scien-
tific methods and an appreciation of the complexity of analytic pro-
cedures. A strong background in an applied science, preferably chemistry,
coupled with some experience in laboratory management should equip the
inspector with the insight required to thoroughly assess a laboratory's
operation.
The qualifications required for the position of evaluator should
be strictly observed. Failure to do so would be a disservice to both
the EPA and the laboratory undergoing evaluation. For even the most
detailed and efficient guidelines cannot guarantee a quality evaluation
if administered by an unqualified individual.
The evaluation procedure, though not extremely complex, is lengthy
and time-consuming. It will run most smoothly if the evaluators have
had soma training in its use. The introductory material, the various
instruction sheets, and particularly the "Evaluator's Guide" may be
used as a text in training sessions for evaluators. If such training
sessions are not arranged, at least the evaluator should study the en-
tire procedure thoroughly before embarking on an evaluation.
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SECTION 4
REGISTRATION AND PRELIMINARY EVALUATION
The U.S. Environmental Protection Agency is engaged in the monumental
task of pollution abatement and control on a national scale. Tne work-
load grows with the increase of substances which require sophisticated
analyses, with the growing technical complexity of analytical proce-
dures and with the reduction of tolerated contamination levels. The
cooperation of many laboratories, state and commercial, must be en-
listed to further EPA's efforts to maintain the integrity of the
environment.
Laboratories which participate in environmental monitoring must meet
rigid standards of excellence. The data gleaned from their analyses
must be defendable for it may serve as evidence in a court of law. To
ensure the analytic capabilities of collaboratoring laboratories, EPA
has instituted a systematic evaluation procedure.
The evaluation procedure is a standardized instrument designed to pro-
duce an objective appraisal of a laboratory's performance. It strives
to utilize the insights of a qualified evaluator without falling prey
to the caprices of a subjective appraisal. It employs a numerical
scoring system to organize the myriad details and to produce a manage-
able result. The scoring framework supplies a strong influence to-
ward uniformity in the application of criteria from laboratory to
laboratory.
A laboratory evaluation is a time consuming endeavor. To minimize this
time factor, the EPA procedure consists of a three step process: Regis-
tration, Completion of a Preliminary Questionnaire by the laboratory,
and an Onsite survey by personnel of the evaluating agency.
A laboratory interested in participating in an evaluation may identify
itself by completion of a brief registration form. This form will in-
dicate to the evaluating agency the extent of the evaluation required,
i.e., whether it is to cover all media or a few tests for one medium.
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Parts 1, 2, 3, and 6 will go to all laboratories. Those parts of Part 4
(Chart C - Analytical' Methodology) and of Part 5 (Chart D - Analytical
Instruments) applicable to the media with which the laboratory is in-
volved will be selected and sent to the laboratory for completion.
Return of the completed questionnaire triggers the final phase of the
evaluation.
The evaluator carefully studies the information provided by the labora-
tory and notes any items which require special attention. The onsite
visit is then scheduled.
During the onsite visit, the evaluator implements the numerical scoring
system to assess the laboratory operation. Any deficiencies which re-
quire improvement prior to scoring are identified and discussed with
the laboratory.
When the evaluation has been completed, a written report of deficiencies
and recommendations will be sent to the laboratory director. Upon re-
turn of satisfactory evidence that all reported deficiencies have been
taken care of, a final score will be issued.
An acceptable score will signify that the laboratory is fully qualified
to participate in the vital work of preserving a safe, liveable environment.
10
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REGISTRATION FORM
The evaluation of Environmental Monitoring.Laboratories is designed to assist the participating
laboratories to upgrade their overall performance in order to safeguard the scientific and legal
validity of their data. Submission of this registration form is the first step in the evaluation process.
A preliminary questionnaire which requests background information about the laboratory's staff,
facilities, and operating procedures is the second step. Upon completion of the preliminary
questionnaire, an onsite visit to assess the performance capability of the laboratory will be scheduled
at the convenience of the laboratory.
I. Name of Laboratory
2. Address
3. Telephone Number
4. Name of Laboratory Director
5. If Private, Name of Owner
6: Type of Laboratory
D Commercial (privately owned, works on fee or contract basis)
LJ Noncommercial (publicly controlled; usually does not work on a fee basis)
7. Provide a brief functional description of the activities of the laboratory
8. Media to be covered in evaluation
D Water
O Chemistry
D Bacteriology
D Biology
D Air
D Pesticides
LJ Radiation
D Other (specify)
9. If evaluation is not desired for complete analysis of any one of the media, list the specific
tests for which you wish to be evaluated. An index of tests for which EPA approved methods
are availiable is given on overleaf.* (Do not list for any medium for which you desire complete
evaluation.)
10. Total Number of employees Technical Administrative.
* EPA approved water and radiation test methods are referenced In Federal Register, Vol. 35, No. 199, October 16, 1973
Interim methods for alglcldes, chlorinated organic compounds, and pesticides can be obtained from Environmental
Monitoring and Support Laboratory, U. S. Environmental Protection Agency, 1014 Broadway, Cincinnati, Ohio 45268.
EPA approved air test methods are referenced in Federal Register, Vol. 36, No. 228, November 25, 1971, and Vol. 38,
No. 110, JuneS, 1973.
Signature of Director Date
EML-01-9/75 II
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PRELIMINARY QUESTIONNAIRE
This questionnaire is designed to elicit all the information required
prior to an onsite survey. Please make a concerted effort to furnish
the information as accurately and concisely as possible.
For convenience, the questionnaire has been divided into six parts:
1) General Laboratory Information
2) Personnel
3) Laboratory Space and Facilities
4) Technical Services
5) Analytical Instruments and Special Apparatus
6) Quality Control
In each section, the questions are styled for the ease of the labora-
tory's response. In many cases only a check (vO is required. Other ques-
tions call for a short answer; clarity and brevity should hallmark your re-
sponse. If you need more space, please continue on blank sheets and
attach them to the questionnaire.
Each section is independent, so that the different sections may be
distributed to the most knowledgeable persons in the laboratory who
can complete their parts independently. Finally, management can assemble
and check all responses before returning the completed forms.
Upon return of the completed questionnaire, the onsite visit will be
scheduled at your convenience. The time involved in the onsite evalua-
tion can be minimized by a thorough presentation of the information
sought in the preliminary questionnaire. Therefore, it is advantageous
to both your laboratory and the evaluating agency if these questions
are answered precisely and completely.
Thank you for your cooperation.
12
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PART 1. GENERAL INFORMATION ABOUT THE LABORATORY
1. Name of Laboratory
2. Address
3. Telephone Number
4. Name of Laboratory Director
5. Provide an organization chart of the laboratory, including any field operations or other internal
affiliations to show how the laboratory fits into the general organizational structure. If attached,
please check.
6. List names and addresses of external organizations used for significant supporting technical services.
7. List names of principal users of services of the laboratory.
8. Has the laboratory been evaluated previously? Yes D No D If yes, when
by whom
9. Do you perform monitoring activities? Yes D No D If yes, please check nature of
monitoring activity:
D Water Quality D Air-Ambient D Radiation
D Estuaries D Air-Source D Other (specify)
D Oceans D Pesticides
D NPDES
13
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Lab Name
10. Do you participate in enforcement actions, emergency episodes, or special studies? Please
specify.
11. Provide a copy of the latest annual report of the laboratory.
D Attached D Not Available
Completed by Date
NAME TITLE
14
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Lab Name
PART 2. PERSONNEL
1. Laboratory staff. Complete Chart A for all technical personnel, including the
laboratory director.
2. Provide brief summary job description for each supervisory, professional, and technical position.
If attached, please check. Q|
3. What is the total number of laboratory employees? Has this number
increased over the past five years? Check if yes Q
4. What portion of your staff participated in a formal training program related to improving work
performance during the past year? Number %
5. What was your turnover rate during the last 12 months?
a) Administrative Staff Number
b) Technical Staff Number %
6. What portion of your staff was formally evaluated for performance during the past year?
Number %
7. What portion of your staff received merit increases in grade or salary during the past year?
Number %
8. What portion of your staff received service increases in grade or salary during the past year?
Number %
Completed by Date
NAME TITLE
15
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Lab Name
CHART A
Complete Chart A for all technicalpersonnel, including the laboratory director.Use a separate block
for each employee and arrange the presentation to reflect the lines of organizational responsibility.
Date
No.
of
pages.
Name
Training
Degree
(Circle One)
Ph.D.
MS
BS
Assoc.
HS
Ph. D.
MS
BS
Assoc.
HS
Ph. D.
MS
BS
Assoc.
HS
Major
Position
Years of Experience
Present J ob
Previous Jobs
Identify Analyses Performed by
Numbers From Attached Index
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Lab Name
PART 3. LABORATORY SPACE AND FACILITIES
CHART B
Complete Chart B. Please indicate both the availability and the adequacy of laboratory equipment
and facilities.
Adequate
Item
Buildings in Use Total m2 (Sq. Ft.)
Office Space Total m2 (Sq. Ft.)
r\
Lab Space Total m^ (Sq. Ft.)
Bench-top Space Total rrr (Sq. Ft.)
Bench Hoods No Capacity
(m/sec.) (lin. ft./min.)
Description
Yes
No
Information
/
Storage Space Chemicals
Sample Storage - General
Secured Space
Refrigerated Space
Hazardous Samples
Controlled Space - Temperature
Humidity
Noise Insulation
Shielded
Clean Rooms
Heat
Air-Conditioning
Electrical Services
Gas
Compressed Air
Available
Yes
No
Adequate
Yes
. No
Additional
Information
17
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Item
Vacuum
Safety Equipment - Fire Alarm
Fire Extinguishing Equipment
Emergency Showers
Eye Fountains
Personal Equipment: glasses, gloves
Hazardous Area Escape
Flammable Material Storage
Safety Cans
Ventilation
Smoking Areas
Handling Equipment for Acids,
Caustic
OSHASigns
Water Supply - Distilled
Deionized
Ammonia - free
CC«2 free
Bacteriologically Suitable
Glassware Supply
Glassware Washing Equipment
Disposal Equipment - Broken Glass
Contaminated Material, Solvents
Library
Conference Room
Employee Lounge
Employee Lockers
Drinking Fountains
Lunch Room
Data Processing Equipment
Available
Yes
No
Adequate
Yes
No
Additional
Information
18
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Logistic Services - Telephone
Intercom
Emergency Line
Motor Vehicle
Facilities as a Whole
Available
Yes
No
Adequate
Yes
No
Additional
Information
Completed by
Date
NAME
TITLE
19
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PART 4. TECHNICAL SERVICES OFFERED
Instructions
In Chart C, Table of Analytical Methods, you are asked to indicate the
tests which are performed by this laboratory and the specific method(s)
which you use for each test. This may be done simply by circling the
appropriate references under Method Used in This Laboratory. In cases
where you follow an EPA method which refers to ASTM or Standard Methods
for the detailed procedure, you may circle the EPA reference only.
The Standard Methods, ASTM, and EPA references are given for your con-
venience. Standard Methods refers to Standard Methods for the Examina-
tion of Water and Wastewater, 13th Edition, 1971, published jointly by
the American Public Health Association, the American Water Works Associa-
tion, and the Water Pollution Control Federation. ASTM refers to the
Annual Book of ASTM Standards, Part 31, Water, 1974, published by the
American Society for Testing and Materials. EPA refers to Methods for
Chemical Analysis of Water and Wastes, 1974, published by the Environ-
mental Monitoring and Support Laboratory (National Environmental Research
Center, Cincinnati, Ohio) and the Office of Technology Transfer, U.S.
Environmental Protection Agency or to the Federal Register (for air tests),
References in Standard Methods and ASTM are to method numbers, whereas
references in the EPA Manual are to page numbers in the 1974 edition.
If this laboratory uses an alternate method or a modification of a
referenced method, write "Other" under "Method Used in This Laboratory"
and provide the requested information for each such case on a copy of
the form "Alternate Analytical Method", page 40.
Under "Sample Frequency," please enter, in the ///Month column, the average
number of samples per month tested by the specified method over the last
12 months. In the Peak Load column, give the maximum number of samples
analyzed in a one-month period during the last 12 months. Your best
estimates of these numbers will be satisfactory.
The tests listed in Chart C are limited to those referenced in the Federal
Register. Referenced in the Federal Register but not included in Chart C
are the variations in air methods suitable for measurement of emissions
from stationary sources. Refer to Federal Register Vol. 36, No. 247,
Part II, December 23, 1971; Vol. 38, No. Ill, June 11, 1973; Vol. 39, No.
47, March 8, 1974; Vol. 40, No. 152, August 6, 1975; and Vol. 80, No. 194,
October 6, 1975. There are, however, important areas not yet covered by
such references. Biology is one such area. The bibliography appended
to this procedure lists some of the sources of information on missing
tests. Method 406, Standard Plate Count, is found in Standard Methods
(Ref. 4). Refer also to the so-called "Equivalency Document," Federal
Register, February 18, 1975.
20
-------
At the end of Chart C a blank chart is included, page 20, on which infor-
mation may be supplied on important tests performed by the laboratory
which are not included in the check list.
21
-------
Lab Name
1. Complete Chart C indicating analytical methodology which the laboratory wishes to have
evaluated.
2. Provide a brief description of any special or unusual technical capability provided by the
laboratory.
3. Provide a brief description of methods that you use for pretreatment of samples before
analysis for trace metals, Tests No. 16-43
Completed by Date
NAME TITLE
22
-------
CHART C. TABLE OF ANALYTICAL METHODS
Lab Name:
Test and Unit
General Analytical Tests:
1 . Alkalinity as CaCC>3
(mg CaCOs/liter)
2. Biochemical Oxygen
Demand (B.O.D.) 5-day
20° C (mg/liter)
3. Chemical Oxygen Demand
(C.O.D.) (mg/liter)
4. Total Solids (Total
Residue) (mg/liter)
5. Total Dissolved Solids
(Total Filterable Residue)
(mg/liter)
Method
(a) Electrometric Titration, Manual
(b) Electrometric Titration, Automated
(c) Automated, Methyl Orange
(a) Modified Winkler with Full-Bottle
(b) Probe Method
(a) Dichromate Reflux (organic C > 15
mg/liter)
(b) Low Level Modification
(c) Saline Water Modification (C1 > 2000
mg/liter)
(a) Gravimetric, Dried at 103-105° C
(a) Glass Fiber Filtration, Dried at
180°C
Method Used in This Lab
Circle Appropriate Reference1
Check next col. if copies available in lab.
Standard
Method
201
201
219
220
224A
224E
ASTM
D1067-70B
D1 252-67
EPA
p. 3
p. 3
p. 5
p.11,51
p.11,56
p. 20
p. 21
p. 25
p. 270
p. 266
Copy
Avail-
able
Sample
Frequency
#/
Month
Peak
Load
ho
Ul
-------
N)
Test and Unit
6. Total Suspended Solids
(Total Nonfilterable
Residue) (mg/liter)
7. Total Volatile Solids
(Volatile Residue)
(mg/liter)
8. Ammonia (as N) (mg/liter)
9. Total Kjeldahl Nitrogen
(as N) (mg/liter)
10. Nitrate (as N) (mg/liter)
Method
(a) Glass Fiber Filtration, Dried at
103-105° C
(a) Gravimetric, Dried at 550° C
(a) Distillation and Titratipn
(b) Distillation and Nesslerization
(c) Distillation and Ammonia Electrode
(d) Automated Colorimetric Phenate
Method
(a) Digestion, Distillation & Titration
(b) Digestion, Distillation &
Nesslerization
(c) Digestion, Distillation & Ammonia
Electrode
(d) Automated Phenate Method
(a) Cadmium Reduction Method (Nitrate-
Nitrite)
Method Used in This Lab
Grcle Appropriate Reference 1
Check next col. if copies available in lab.
Standard
Method
224C
224B
216
213B
ASTM
D992-71
EPA
p. 268
p. 272
p. 159
p. 159
p. 159,165
p. 168
p. 175-181
p. 175-181
p. 165, 175-
181
p. 182
p. 201
Copy
able
Sample
Frequency
#/
Month
Peak
Load
-------
Test and Unit
10. Nitrate (as N) (mg/liter) (Cont.)
1 1 . Total Phosphorus (as P)
(mg/liter)
1 2. Acidity (mg CaCC>3/liter)
13. Total Organic Carbon
(T.O.C.) (mg/liter)
Method
(b) Automated Cadmium Reduction
Method (Nitrate-Nitrite)
(c) Brucine Method
(d) Automated Hydrazine Reduction
Method
(a) Single Reagent (Ascorbic Acid
Reduction Method)
(b) Automated Colorimetric Ascorbic
Acid Reduction Method
(c) Automated SnCI2 Method
(a) Hydrogen Peroxide Digestion &
Electrometric Titration
(b) Hydrogen Peroxide Digestion &
Phenolphthalein End-Point Titration
(a) Combustion and Infrared Method
CO2
(b) Combustion & Flame lonization
Method (CH4)
Method Used in This Lab
Circle Appropriate Reference 1
Check next col. if copies available in lab.
Standard
Method
223CIM
223F
223E
138A
ASTM
D1067-70E
D1067-70E
D2579-74
EPA
p. 207
p. 197
p. 1852
p. 249
p. 256
P- 1
p. 236
p. 236
Copy
Avail-
able
Sample
Frequency
#/
Month
Peak
Load
-------
Test and Unit
14. Total Hardness
(mg CaCC>3/liter)
15. Nitrite (as N) (mg/liter)
Method
(a) EDTA Titration
(b) Automated Colorimetric
(c) Atomic Absorption (Ca + Mg)
(a) Manual Colorimetric Diazotization
(b) Automated Colorimetric
Diazotizatipn
Method Used in This Lab
Grcle Appropriate Reference!
Check next col. if copies available in lab.
Standard
Method
122
ASTM
D1126-67B
EPA
p. 68
p. 70
p. 78-91,
103, 114
p. 215
p. 207*
Copy
Avail
able
Sample
Frequency
#/
Month
Peak
Load
-------
CHART C. TABLE OF ANALYTICAL METHODS
Lab Name:
Test and Unit
Tests for Trace Metals:
16. Aluminum (mg/liter)
17. Antimony (mg/liter)
18. Arsenic (mg/liter)
19. Barium (mg/liter)
20. Beryllium (mg/liter)
21. Boron (mg/liter)
22. Cadmium (mg/liter)
23. Calcium (mg/liter)
Method
(a) Atomic Absorption
(a) Atomic Absorption
(a) Atomic Absorption (Gaseous Hydride
Method)
(b) Gaseous Hydride - Silver Diethyl-
dithiocarbamate Colorimetric
(a) Atomic Absorption
(a) Atomic Absorption
(b) Aluminon Method
(a) Curcumin Method
(a) Atomic Absorption
(b) Dithizone Colorimetric Method
(a) Atomic Absorption
(b) EDTA Titration
Method Used in This Lab
Circle Appropriate Reference!
Check next col. if copies available in lab.
Standard
Method
103A
104A
129A
129A
106B
107 A
129 A
211(II)B
HOC
ASTM
D2576-70
D2576-70
EPA
p. 92*
p. 94*
p. 95*
p. 9
p. 97*
p. 99*
p. 13
p. 101 *
p. 103*
p. 19
Copy
Avail-
able
Sample
Frequency
#/
Month
Peak
Load
-------
CO
Test and Unit
24. Chromium VI (mg/liter)
25. Chromium, Total (mg/liter)
26. Cobalt (mg/liter)
27. Copper (mg/liter)
28. Iron (mg/liter)
29. Lead (mg/liter)
30. Magnesium (mg/liter)
31. Manganese (mg/liter)
Method
(a) Extraction and Atomic Absorption
(b) Diphenylcarbazide Colorimetric
(a) Atomic Absorption
(b) Oxidation & Diphenylcarbazide
Colorimetric
(a) Atomic Absorption
(a) Atomic Absorption
(b) Neocuproine Colorimetric
(a) Atomic Absorption
(b) O-Phenanthroline Colorimetric
(a) Atomic Absorption
(b) Dithizone Colorimetric
(a) Atomic Absorption
(b) Gravimetric
(a) Atomic Absorption
Method Used in This Lab
Circle Appropriate Reference1
Check next col. if copies available in lab.
Standard
Method
211(II)D
129A
211(II)C
129 A
211(II)E
129A
211(II)F
129A
211(II)G
129A
127A
129A
ASTM
D2576-70
D1 687-67
D2576-70
D2576-70
D1 688-68
D2576-70F
D1068-68A
D2576-70G
D2567-70
D511-52
D2567-70
EPA
p. 78-91,
105 *
p. 78-91,
105*
p. 105
p. 107*
p. 108*
p.110*
p. 112*
p. 114*
p. 116*
Copy
Avail-
able
Sample
Frequency
#/
Month
Peak
Load
-------
N3
VO
Test and Unit
32. Mercury (mg/liter)
33. Molybdenum (mg/liter)
34. Nickel (mg/liter)
35. Potassium (mg/liter)
36. Selenium (mg/liter)
37. Silver (mg/liter)
Method
(a) Flameless Atomic Absorption: Man-
ual Cold Vapor Technique (Hg in
Water)
(b) Flameless Atomic Absorption: Auto-
mated Cold Vapor Technique (Hg in
Water) (not approved generally)
(c) Flameless Atomic Absorption: Man-
ual Cold Vapor Technique (Hg in
Sediment)
(a) Atomic Absorption
(a) Atomic Absorption
(b) Heptoxime Colorimetric
(a) Atomic Absorption
(b) Colorimetric
(c) Flame Photometric
(a) Atomic Absorption (Gaseous Hydride
Method)
(a) Atomic Absorption
Method Used in This Lab
Circle Appropriate Reference 1
Check next col. if copies available in lab.
Standard
Method
211(11)1
147B
147 A
129A
ASTM
D3223-73
D3223-73
D2576-70
D1 428-64
EPA
p. 118*
p. 127*
p. 134*
p. 139*
p. 141 *
p. 143*
p. 145*
p. 146*
Copy
Avail-
able
Sample
Frequency
#/
Month
Peak
Load
-------
Test and Unit
38. Sodium (mg/liter)
39. Thallium (mg/liter)
40. Tin (mg/liter)
41. Titanium (mg/liter)
42. Vanadium (mg/liter)
43. Zinc (mg/liter)
Method
(a) Atomic Absorption
(b) Flame Photometric
(a) Atomic Absorption
(a) Atomic Absorption
(a) Atomic Absorption
(a) Atomic Absorption
(b) Colorimetric (Catalysis of Gallic
Acid Oxidation)
(a) Atomic Absorption
(b) Dithizone Colorimetric Method
Method Used in This Lab
Circle Appropriate Reference!
Check next col. if copies available in lab.
Standard
Method
153A
164A
129A
165B
ASTM
D 1428-64
D1691-67
EPA
p. 147 *
p. 149*
p. 150*
p. 151 *
p. 153*
p. 155*
Copy
Avail-
able
Sample
Frequency
#/
Month
Peak
Load
-------
U)
THARTr TARI FOF ANAI YTirAI MFTHOnS 1 ah Name:
Test and Unit
Tests for Nutrients, Anions, and Organics
44. Organic Nitrogen (as N)
(mg/liter)
45. Orthophosphate (as P)
(mg/liter)
46. Sulphate (as $04)
(mg/liter)
47. Sulfide (as S) (mg/liter)
48. Sulfite (as 803) (mg/liter)
49. Bromide (mg/liter)
50. Chloride (mg/liter)
Method
(a) Kjeldahl Nitrogen minus Ammonia
Nitrogen
(a) Single Reagent Ascorbic Acid
Reduction Method
(b) Automated Colorimetric Ascorbic
Acid Reduction Method
(a) Gravimetric
(b) Turbidimetric
(c) Automated Colorimetric Barium
Chloranilate
(a) Titrimetric Iodine
(a) Titrimetric lodide-lodate
(a) Titrimetric lodide-lodate
(a) Silver Nitrate
(b) Mercuric Nitrate
(c) Automated Colorimetric Ferricyanide
Method Used in This Lab
Circle Appropriate Reference 1
Check next col. if copies available in lab.
Standard
Method
215
223F
156A
156C
228A
158
112A
112B
ASTM
D5 15-72 A
D5 16-68 A
D5 16-688
D1339-72C
D1246-68C
D512-67B
D5 12-67 A
EPA
See (8) and
(9) above
p. 249
p. 256
p. 283
p. 277
p. 279
p. 284
p. 285
p. 14
p. 29
p. 31
Copy
Avail-
able
Sample
Frequency
#/
Month
Peak
Load
-------
U)
S3
Test and Unit
51. Cyanide, Total (mg/liter)
52. Fluoride (mg/liter)
53. Chlorine, Total
Residual (mg/liter)
54. Oil and Grease
(mg/liter)
55. Phenols (mg/liter)
Method
(a) Distillation & Silver Nitrate
Titration
(b) Distillation & Pyridine-Pyrazolone
(or Pyridine - Barbituric Acid)
Colorimetric
(a) Distillation-SPADNS
(b) Automated Complexone Method
(c) Fluoride Electrode
(a) Starch-Iodide Titration
(b) Amperometric Titration
(a) Gravimetric (Separatory Funnel
Extraction)
(b) Infrared (Separatory Funnel
Extraction)
(a) Colorimetric (4-AAP Method with
Distillation)
Method Used in This Lab
Circle Appropriate Reference!
Check next col. if copies available in lab.
Standard
Method
207A,
207B
207A,
207C
121A,
121C
204A
204A
137
222E
ASTM
D2036-74A
D2036-74A
D1179-72A
D1427-68A
D1427-68B
D1 783-70
EPA
p. 40
p. 40
p. 59
p. 61
p. 65
p. 35 '
p. 35
p. 229
p. 232
p. 241
Copy
Avail-
able
Sample
Frequency
#/
Month
Peak
Load
-------
u>
u>
Test and Unit
56. Surfactants (mg/liter)
57. Algicides (mg/liter)
58. Benzidine (mg/liter)
59. Chlorinated Organic Compounds
(Except Pesticides) (mg/liter)
60. Pesticides (mg/liter)
Method
(a) Methylene Blue Colorimetric
(a) Gas Chromatography
(a) Diazotization & Colorimetric
(a) Gas Chromatography
(a) Gas Chromatography
(b) Thin Layer Chromatography
Method Used in This Lab
Circle Appropriate Reference 1
Check next col. if copies available in lab.
Standard
Method
159A
ASTM
D2330-68
EPA
p. 157
§
t
§
§
§
Copy
Avail-
able
Sample
Frequency
#/
Month
Peak
Load
-------
CHART C. TABLE OF ANALYTICAL METHODS
Lab Name:
Test and Unit
Physical and Biological Tests
61. Color
62. Specific Conductance
(mho/cm @ 25° C)
63. Turbidity (Jackson Units)
64. Streptococci Bacteria,
Fecal (number/1 00 ml)
65. Coliform Bacteria,
Fecal (number/100 ml)
66. Coliform Bacteria,
Total (number/100 ml)
Method
(a) Platinum-cobalt Colorimetric
(b) Spectrophotometric (Dominant wave-
length, hue, luminance, purity)
(a) Wheatstone Bridge
(a) Turbidimeter Method
(a) MPN
(b) Membrane Filter
(c) Plate Count
(a) MPN
(b) Membrane Filter
(a) MPN
(b) Membrane Filter
Method Used in This Lab
Circle Appropriate Reference 1
Check next col. if copies available in lab.
Standard
Method
118
206A
154
163 A
409A
409 B
409C
407C
408 B
407A
408A
ASTM
D1 125-64
D1 889-71
(Sect. 1 0-
16)
EPA
p. 36
p. 39
p. 275
p. 295
Copy
Avail-
able
Sample
Frequency
#/
Month
Peak
Load
u>
-------
CHART C. TABLE OF ANALYTICAL METHODS
Lab Name:
Test and Unit
Radiological Tests
67. Alpha, Total (pCi/liter)
68. Alpha, Counting Error
(pCi/liter)
69. Beta, Total (pCi/liter)
70. Beta Counting Error
(pCi/liter)
71. Radium, Total (pCi/liter)
Method
(a) Proportional Counter
(b) Scintillation Counter
(a) Proportional Counter
(b) Scintillation Counter
(a) Proportional Counter
(a) Proportional Counter
(a) Proportional Counter
(b) Scintillation Counter
Method Used in This Lab
/
Circle Appropriate Reference 1
Check next col. if copies available in lab.
Standard
Method
302
302
302
302
304
304,305
ASTM
D1 943-66
D1 943-66
D3085-72T
D3085-72T
D1 890-66
D3085-72T
D2460-70
D2460-70
EPA
Copy
Avail-
able
Sample
Frequency
#/
Month
Peak
Load
10
Ui
-------
CHART C TARI F OF ANALYTICAL METHODS Lab Name:
Test and Unit
Tests for Other Characteristics
72. Temperature
73. pH
Method
(a) Thermometer or Thermistor
(a) Electrometric
Method Used in This Lab
Circle Appropriate Reference ^
Check next col. if copies available in lab.
Standard
Method
162
144A
ASTM
Dl 293-65
EPA
p. 286
p. 239
Copy
Avail-
able
Sample
Frequency
#/
Month
Peak
Load
-------
CHART C. TABLE OF ANALYTICAL METHODS
Lab Name:
Test and Unit
Tests for Air Characteristics
74. Sulphur Dioxide
75. Suspended Particulates
76. Carbon Monoxide
77. Photochemical Oxidants
(Ozone)
78. Hydrocarbons (minus Methane)
79. Nitrogen Dioxide
Method
(a) Pararosaniline Method /Manual
v ' \ Automated
(a) High Volume Method
(a) Nondispersive Infrared
Spectrometry
(a) Chemluminescence, Continuous
(a) GC-FID
(a) Arsenite 24-Hr Sampling Method
Manual Automated
(b) Chemluminescence, Continuous
Method Used in This Lab
Circle Appropriate Reference
Check next col. if copies available in lab.
Standard
Method
ASTM
EPA
b.22385-7 0
b. 22388-900
b.22391 0
b.22392 0
b. 223940
b. 15175V
22396 0
b.|15177\7
Copy
Avail-
able
Sample
Frequency
#/
Month
Peak
Load
to
vj
-------
Chart C. Table of Analytical Methods
Lab Name:
Test and Unit
Non-referenced Tests in Use
Method
Method Used in This Lab
Give Method Number or Page
Check next col. if copies available in lab.
Standard
Method
ASTM
EPA
Copy
Avail-
able
Sample
Frequency
#/
Month
Peak
Load
co
-------
REFERENCE MARKS IN CHART C
1 - Federal Register. Vol. 38. No. 199. October 16. 1973.
2 - EPA Method! Manual, 1971.
v An introduction to atomic absorption ipectrophotometry and a general procedure for trace metal analyili by atomic absorption Is given In EPA Manual, pp. 78-91.
§ Interim procedures for alglcldes, chlorinated organic compounds, and pesticides obtained from the Environmental Monitoring and Support Laboratory, USEPA, Cincinnati, Ohio 45268.
t - Estimated by the method of M.A. EI-Dlb, "Colorlmetrlc Determination of Aniline Derivatives In Natural Waters," Journal of the Association of Official Analytical Chemists.Vol. 54. No. 6,
November, 1971, pp. 1363-1387.
^7 Federal Register. Vol. 38. No. 110. June 8. 1973.
0 - Federal Register. Vol. 36, No. 228, November 25, 1971.
- Without Cd reduction.
U>
VO
-------
ALTERNATE ANALYTICAL METHOD
Name of Laboratory
(a) # Test:
(b) If this is a modification of a referenced method,
(1) Which referenced method (give manual name and pages)?.
(2) Purpose of modification:
(3) Brief description of modification:
(4) Literature reference,
-------
Lab Name
PART 5. ANALYTICAL INSTRUMENTS AND SPECIAL APPARATUS
(1) Complete Chart D indicating analytical instruments and special apparatus available in the
laboratory. See complete list of equipment, by analytical method, in the Appendix.
Completed bv Date
NAME TITLE
41
-------
INDEX OF ANALYTICAL INSTRUMENTS AND SPECIAL APPARATUS
Chart D
Page
1. Technicon Auto Analyzer 44
2. Colorimeters/Filter Photometers 46
3. Spectrophotometers (UV-visible) 46
4. Atomic Absorption Spectrophometers 48
5. Mercury Analyzers 49
6. Flame Photometers 49
7. Infrared Spectrophometers 49
8. Conductivity Meters 50
9. Electrometric Apparatus 50
10. Automatic Titrimeters 51
11. Amperometric Titration Apparatus 51
12. Analytical Balances 51
13. Carbon Analyzer 51
14. Nephelometers/Turbidimeters 52
15. Blenders 52
16. Vacuum Pumps 52
17. Magnetic Stirrers 52
18. Drying Ovens 52
19. Muffle Furnace 53
20. Hotplate/Autoclave 53
21. Water Baths 53
22. B.O.D. Incubation Bottles 53
23. Gravimetric Evaporating/Weighing Dishes 53
24. Dessicators 54
25. Kjeldahl Distillation Apparatus 54
26. Arsine Generator/Absorption Apparatus 54
27. Cyanide Distillation Apparatus 54
28. Soxhlet Extraction Apparatus 54
29. Phenol Distillation Setups 54
30. Messier Tubes 55
31. Refrigerators 55
32. Special Thermometers 55
33. Thin-layer Chromatography Apparatus 55
34. Column Chromatography Apparatus eg
35. Gas Chromatographs gg
36. Other Special Instrumentation 57
Special Microbiological Equipment
37. Incubation Oven 58
38. Water Baths 58
39. Autoclave 58
40. Light Microscope "
41. Misc. Microbiological Containers 59
42. Membrane Filters 59
43. Colony Counters 59
44. Other Microbiological Instruments 60
42
-------
Special Radiological Equipment
45. Alpha/Beta Particle Counters 61
46. Spectrometer Systems 61
47. Other Radiological Instruments and Apparatus 62
Special Air Equipment
48. Sulfur Dioxide Monitoring 63
49. High Volume Sampler (Particulates) 63
50. Carbon Monoxide Monitor 63
51. Total Hydrocarbons Monitor 64
52. Photochemical Oxidants Monitor 64
53. Nitrogen Dioxide Monitor 64
54. Other Air Monitoring Equipment
Including Calibration Equipment 65
43
-------
Lab Name
CHART D. ANALYTICAL INSTRUMENTS AND SPECIAL APPARATUS
Identify the instruments and apparatus in use and in good working condition in your laboratory.
Instrument
1. Technicon Autoanalyzer
AAI Unite
AAII Unit-;
Samplers
# of
Units
Manufacturer
Model
Year
Purchased
Operating Manual
Avail, in Lab.
Manifolds for:
Alkalinity
Ammonia Nitrogen (Colorimetric Phenate)
Kjeldahl-Nitrogen (Colorimetric Phenate)
Kjeldahl Nitrogen (Selenium Method)
Nitrate-Nitrite (Cd Reduction)
Total Phosphorus or Orthophosphate
Total Hardness
Analytical Cartridges for:
Ammonia Nitrogen (Colorimetric Phenate)
Total Phosphorus or Orthophosphate
Mercury (Cold Vapor Technique)
Sulphur (Chloranilate)
Chloride (Ferricyanide)
Fluoride (Complexone)
Phenols (4-AAP)
Others (Specify):
Nitrate-Nitrite (Cd Reduction)
Others (Specify):
44
-------
Accessory
Tnlnrimptpr*
# of
Units
Manufacturer
Model
Year
Purchased
Operating Manual
Avail, in Lab.
Cells, tubular flow (Give number of each type.
15 mm
Filters:
Wavelength of
Max. Transmittance
Range Expansion
50 mm
Wavelength of
Max. Transmittance
Accessory
Recorders
# of
Units
Manufacturer
Model
Year
Purchased
Operating Manual
Avail, in Lab.
Digital Printer
Associated Apparatus:
Continuous Filter
Proportioning Pump
Planetary Pump
Vapor-liquid Separator (for Hg Cold Vapor)
Continuous Digester
Others (Specify):
Heating Bath
45° - 80° C Range
With Distillation Coil & Head
With Double Delay Coil
High Temperature with 2
Distillation Coils
45
-------
Instrument
2. Colorimeters/Filter
Photometers
Ranee:
Range:
# of
Units
Manufacturer
Model
Year
Purchased
Operating Manual
Avail, in Lab.
Filters:
Wavelength of
Max. Transmittance
Bandwidth
Wavelength of
Max. Transmittance
Bandwidth
Special Associated Apparatus (Specify):
Instrument
3. Spectrophotometers
(UV- visible)
Recording (Range: )
Manual (Range: )
# of
Units
Manufacturer
Model
Year
Purchased
Operating Manual
Avail, in Lab.
Soecial Attachments (Soecifvk
46
-------
Metal
Magnesium
Manganese
Mercury
(Cold Vapor)
Molybdenum
Nickel
Potassium
Selenium
(Gaseous
Hydride)
Silver
Sodium
Thallium
Tin
Titanium
Vanadium
Zinc
Lamps
Hollow
Cathode
Electric
Discharge
Other (Specify)
Fuels
Acetylene
Air
Nitrous
Oxide
Argon
Hydrogen
-
Associated Equipment:
Spectrophotometric gas cells, 10 cm, quartz
windows (for Hg Cold Vapor)
Others (Specify):
Mercury Cold Vapor Setup
-------
Instrument
4. Atomic Absorption
Spectrophotometers
# of
Units
Manufacturer
Model
Year
Purchased
Operating Manual
Avail, in Lab.
Recorders (Specify):
Indicate lamps and fuels used for each metal:
Metal
Aluminum
Antimony
Arsenic
(Gaseous
Hydride)
Barium
Beryllium
Cadmium
Calcium
Chromium VI
Chromium,
Total
Cobalt
Copper
Iron
Lead
Lamps
Hollow
Cathode
Electric
Discharge
Other (Specify)
Fuels
Acetylene
Air
Nitrous
Oxide
Argon
Hydrogen
48
-------
Instrument
# of
Units
Manufacturer
Model
Year
Purchased
Operating Manual
Avail, in Lab.
5. Mercury Analyzers
Technique:
Range:
Sensitivity:
Instrument
6. Flame Photometers
Dirert Reading:
Internal Standard:
# of
Units
Manufacturer
Model
Year
Purchased
Operating Manual
Avail, in Lab.
Special Apparatus:
Setup for Na in low-solids water
(Air blower & filter, Oxy-hydrogen
flame, polyethylene, or Teflon apparatus)
Others (Specify):
Instrument
7. Infrared
Spectrophotometers
Single Beam (Range: )
Double Beam (Range: ) ..
# of
Units
Manufacturer
Model
Year
Purchased
Operating Manual
Avail, in Lab.
Special Features:
IR Cells (Specify):
49
-------
Instrument
8. Conductivity Meters
Field (Cell Type: )
Laboratory (Cell Type: )
# of
Units
Manufacturer
Model
Year
Purchased
Operating Manual
Avail, in Lab.
Associated Apparatus (Specify):
Instrument
9. Electrometric Apparatus
Electrometers:
Field - ASTM Type 1
ASTMTypell
1 ahnratory - ASTM 1 . ,.
ASTM II
# of
Units
Manufacturer
Model
Year
Purchased
Operating Manual
Avail, in Lab.
Electrodes:
pH
Dissolved Oxygen
Ammonia
Fluoride
Cyanide
Other (Specify):
Manufacturer
Type
50
-------
Instrument
10. Automatic Titrimeters
# of
Units
Manufacturer
Model
Year
Purchased
Operating Manual
Avail, in Lab.
RernrHers (Specify)-
Frequently Used Electrodes ,
(Specify):
Instrument
1 1 . Amperometric Titration
Apparatus
# of
Units
Manufacturer
Model
Year
Purchased
Operating Manual
Avail, in Lab.
Instrument
12. Analytic Balan
Capacity
ces
Sensitivity
# of
Units
Manufacturer
Model
Year
Purchased
Operating Manual
Avail, in Lab.
Certified Weights H Certification
Instrument
13. Carbon Analyzers
Infrared (as CO->)
Flame lonization
(«ChM
# of
Units
Manufacturer
Model
Year
Purchased
Operating Manual
Avail, in Lab.
51
-------
Instrument
14. Nephelometers/
Turbidimeters
Range: _ . . .
#
Units
Manufacturer
Model
Year
Purchased
Operating Manual
Avail, in Lab.
Sensitivitv Below 1 NTU:
Instrument
IS. Blenders
# of
Units
Manufacturer
Model
Year
Purchased
Operating Manual
Avail, in Lab.
Instruments
16. Vacuum Pumps
Type:
Type: ... ..._._.
# of
Units
Manufacturer
Model
Year
Purchased
Operating Manual
Avail, in Lab.
Apparatus
17. Magnetic Stirrers
With Heater
With Timer
# of
Units
Manufacturer
Model
Year
Purchased
Operating Manual
Avail, in Lab.
18. Drying Ovens
98° C
103°-105°C
180°C
52
-------
19. Muffle Furnance
550° C
20. Hot Plate (persulphate digestion)
Autoclave (persulphate digestion)
21. Water Baths/Incubators
10°-15°C
100° C, well stirred, with Neoprene
coated wire rack for 40-50 ml sample
tubes (for Brucine Nitrate Method)
25° C with rack (for conductance
measurements)
20° C incubator (for B.O.D.)
with circulator
22. B.O.D. Incubation Bottles
Number
23. Gravimetric Evaporating/Weighing Dishes
Porcelain
Vycor
Platinum
Number
53
-------
Apparatus
24.
Dessicators
Typp-
Type:
Number
Apparatus
25.
Kjeldahl Distillation Apparatus
Marro
Mirrn
Number
Apparatus
26.
Arsine Generator A Absorption Apparatus . , .,
Number
Apparatus
27.
Cyanide Distillation Apparatus
Number
Apparatus
28.
Soxhlet Extraction Apparatus
Thimble Size:
Number
Apparatus
29.
Phennl Distillation Setups
Number
-------
Apparatus
30.
Nessler Tubes, matched sets, APHA standard
SO ml, tall
100 ml, tall
Apparatus
31.
Refrigerators
Number
Model
Temperature Cubic Feet
Apparatus
32.
Special Thermometers
Certification Range
Apparatus
33.
Thin-Layer Chromatography Apparatus (Describe chambers; plates, commercial or homemade;
spray reagents and apparatus; spotting apparatus; special equipment)
55
-------
34. Column Chromatography Apparatus (Describe columns; adsorbents - type, source, grade,
special handling; solvent evaporation apparatus; special equipment)
35. Gas Chromatographs (Describe for each instrument: make and model; column type-
capillary, 1/8 in., 1/4 in., etc., temperature programming; detector type and model; re-
corder; most commonly used columns; special equipment)
56
-------
instrument
36. Other Special Instruments (Mass
Spec., NMR, Flowmeters,
Electrom Microscope, etc.)
'# of
Units
Manufacturer
Model
Year
Purchased
Operating Manual
Avail, in Lab.
57
-------
CHART D. ANALYTICAL INSTRUMENTS AND SPECIAL APPARATUS
Lab Name:
Special Microbiological Equipment
37. Incubation Oven 35 ± 0.5° C
Humidity controlled? (Specify relative humidity)
38. Water Baths
35 ± 0.5° C
44.5 ± 0.2° C
39. Autoclave (to121°C)
40. Light Microscope
Type:
Type:
#of
Units
Manufacturer
Magnification
Light
Source
58
-------
41 . Miscellaneous Microbiological Containers
Sample Bottles
Inoculation Tubes
Dilution Bottles
Containers for Media
Petri Dishes
Other (Specify)
Plastic
Glass
Other (Specify)
42. Membrane Filters
Manufacturer
Type
Instrument
43. Colony Counters
# of
Units
Manufacturer
Model
Year
Purchased
Operating Manual
Avail, in Lab.
59
-------
Instrument
44. Other Microbiological/Biological
Instrumentation
# of
Units
Manufacturer
Model
Year
Purchased
Operating Manual
Avail, in Lab.
60
-------
CHART D. ANALYTICAL INSTRUMENTS AND SPECIAL APPARATUS
Lab Name:
Special Radiological Equipment
Instrument
45. Alpha & Beta Particle
Counters
Windowless Gas-Flow
Proportional Counter
Thin Window Gas-Flow
Proportional Counter
Alpha Scintillation
Counter
Beta Scintillation
T.ni inter
Liquid Scintillation
Counter
# of
Units
Manufacturer
Model
Year
Purchased
Operating Manual
Avail, in Lab.
Instrument
46. Spectrometer Systems
Alpha Spectrometer
(Surface Barrier Tvoe)
Detector
Analyzer
# of
Units
Manufacturer
Model
Year
Purchased
Operating Manual
Avail, in Lab.
Other Pertinent Information
61
-------
Instrument
46. Spectrometer Systems (Con't.)
Hamma Spertrnmetpr
Detector
Analyzer
# of
Units
Manufacturer
Model
Year
Purchased
Operating Manual
Avail, in Lab.
Other Pertinent Information
Instrument
47. Other Radiological
Instrumentation
(Radon Gas Counters,
Survey Instrument^ err )
# of
Units
Manufacturer
Model
Year
Purchased
Operating Manual
Avail, in Lab.
62
-------
CHART D. ANALYTICAL INSTRUMENTS AND SPECIAL APPARATUS
Lab Name:
Special Air Monitoring Equipment
Instrument
# of
Units
Manufacturer
Model
Year
Purchased
Operating Manual
Avail, in Lab.
48. Sulphur Dioxide Monitor
(Field Sampling/Lab Analysis)
Field Sampler
Lab Analytical Method:
(Field Sampling/Field
Analysis)
Field Sampler/Analyzer
Analytical Method:
Instrument
49. Suspended Particulates
(High Volume Sampler)
Filter Type ,
# of
Units
Manufacturer
Model
Year
Purchased
Operating Manual
Avail, in Lab.
Instrument
50. Carbon Monoxide Monitor
#of
Units
Manufacturer
Model
Year
Purchased
Operating Manual
Avail, in Lab.
63
-------
Instrument
51. Total Hydrocarbons
(corrected for CH^)
Monitor
# of
Units
Manufacturer
Model
Year
Purchased
Operating Manual
Avail, in Lab.
Instrument
52. Photochemical Oxidants
(03) Monitor
# of
Units
Manufacturer
Model
Year
Purchased
Operating Manual
Avail, in Lab.
Instrument
#of
Units
Manufacturer
Model
Year
Purchased
Operating Manual
Avail, in Lab.
53. Nitrogen Dioxide Monitor
(Field Sampling/
Lab Analysis)
Field Sampler
Lab Analytical Method:
(Field Sampling/
Field Analysis)
Field Sampler/Analyzer
Analytical Method:
64
-------
Instrument
54. Other Air Monitoring
Equipment Including
Calibration Equipment
Permeation Tubes
Standard Cylinders
Gas Phase Titration-Commercial
-Home Made
Air Dilution Systems
Variable Temperature Bath:
25°C±0.1°C
#of
Units
Manufacturer
Model
Year
Purchased
/
Operating Manual
Avail, in Lab.
65
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INTERNAL AND EXTERNAL CONTROLS
The first three sections of this chart contain lists on which the
availability of written operating procedures is to be checked. These
parts cover instrument maintenance and calibration, all aspects of
sampling, and the quality control program of the laboratory. You may
be asked to show these documents to the evaluator during the onsite
inspection and to discuss them with him.
This check list should not be looked upon as a demand for written pro-
cedures (for example, a Quality Control Program) in a particular stan-
dard format. The important thing is that the principal laboratory con-
trols should be documented in a permanent way. Some procedures may be
brief or may not include all of the items to be checked. In the list
please check those items which you believe to be adequately documented.
The onsite visit will provide an opportunity to discuss the complete-
ness of the documentation with the evaluator.
Part 4 of this chart asks for information on participation in inter-
laboratory proficiency testing programs. Information is required on
the test methods covered in any plan in which you have participated,
the organization conducting the program and the date of the last check
sample reported upon.
You will be rated on the extent of your participation in such programs.
However, as of the present, the actual standing you have achieved in
proficiency tests is not a part of the scoring system for this evaluation.
66
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Lab Name
PART 6. INTERNAL AND EXTERNAL CONTROLS
CHART E
1. Control of Analytical Methods and Instruments
(1) Written Instrument Maintenance and
Calibration Procedures and Log Books
(2) Written Bench Operating Procedures
2. Control of Sampling and Sample Preservation
(1) Written Sampling Procedures Covering:
Sampling Plans and Sampling Equipment
Sample Collection and Preservation
Identification and Storage of Samples
Laboratory Handling of Samples
(Request for analysis, sample
preparation, timely performance, etc.)
(2) Written Description of the Chain of Custody
of Samples
(3) Written Procedures for Field Measurement
(Flow, critical tests: D.O., Residual C1,
etc.)
(4) Written Procedures for Monitoring
(Water supply, effluents, ambient air,
stacks, mobile vehicles, pesticides,
radiation, etc. )
3. Quality Control
(1) Written Quality Control Program Covering:
Quality Policy
Assignment of Responsibility
Training in Quality Control Methods
Control of Purchased Chemicals/Reagents
Internal Field and Laboratory Checks:
Precision/Accuracy
Routine Duplicates, Spiked, and
Standard Samples
Statistical Methods, Including
Control Charts and/or Computer Methods
(2) Written Description of Lab Record System
(Data handling/calculations, data review, validation
and audit)
(3) Written Description of Lab Report Systems
(4) If you have a Quality Control Manual,
please provide a copy. Attached D
Available
Yes
No
67
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4. Inter-laboratory Proficiency Testing Programs
Test Method
Participated in Program of:
EPA
CDC
State
USGS Other (Specify)
Date of
Last Check
Sample
Within
Acceptable
Limits
Completed by:
Date
NAME
TITLE
68
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SECTION 5
EVALUATOR'S GUIDE
PART 1. GENERAL INFORMATION ABOUT THE LABORATORY
Appropriateness of Organization
Intent. To determine appropriateness of the organization to render the
services offered by the laboratory. This protocol is primarily concerned
with the laboratory's monitoring activities: analyses performed to
determine compliance with laws and regulations. The organization should
be suited to the media that the evaluation covers: air, water, pesti-
cides, or radiation.
Request a short discussion of the organization as seen from management's
viewpoint.
Is the organization chart supplied with the preliminary
information up-to-date? Does it agree with the actual
organization?
Do functions performed in the laboratory follow the organiza-
tion chart exactly?
Are problems handled strictly through chain of command or do
sections of the laboratory interact to get timely solutions?
Does the laboratory experience difficulty in meeting perform-
ance requirements?
Impairment of Functions
Intent. To determine whether management perceives problems that might
lead to impairment of laboratory functions.
Request a brief oral description of any problems encountered in opera-
ting the laboratory. Ask specifically about the following:
Does the laboratory have difficulties in obtaining a suffi-
cient number of well qualified staff in all disciplines?
69
-------
Are the facilities, equipment and services adequate to perform
the services offered in the media covered by the laboratory?
Water? Air? Pesticides? Radiation?
Does the laboratory have difficulties in getting adequate ser-
vices from outside supporting organizations? Specifically,
is it satisfied with the validity of sampling, performed for
it by others? With testing? With calibration? Are reports
from outside signed?
Does the laboratory have any problems in budgeting for next
year? Does it have separate budgets for routine operations
and for equipment and apparatus? Who is responsible for
preparing the different parts of the budget? Is there input
from all levels of the organization?
Does the laboratory have any problems in satisfying those who
use its services?
Strength of Management
Intent. To discover something about the strength of management.
Request discussion on the following items.
' Does the laboratory experience difficulties in maintaining
cooperation between different laboratory groups? Between
supervisors and analysts?
Does the laboratory have specific plans and procedures for
rapid to-the-point internal communications?
Does the laboratory prepare an annual plan for operation of
the laboratory? A long-range plan? What is management's
experience with performance according to plan?
Does the laboratory have a policy manual? Does sufficient
informal control exist to ensure that things that need to
be done quickly get done, for example cross over lines of
authority in the lab or change-orders for sample analyses?
Refer to Preliminary Questionnaire, Part 1, Items 9 and 10,
dealing with involvement in activities outside the laboratory.
Is the level of involvement in these activities consistent
with the expectations the user should have of the laboratory?
Objectivity of the Laboratory
Intent. To determine whether there are reasons for questioning or dis-
counting the objectivity of the laboratory.
70
-------
Request a brief discussion of the relationship of the laboratory with
its own organization and with its customers. If laboratory is pri-
vately owned the enquiry should be deeper than for publicly controlled
laboratories.
Inquire more about:
Ownership
Managerial structure and individuals in sensitive and
controlling positions
Any other affiliations of principal officers and directors
and those in supervisory positions in laboratory
Any chance of conflict of interest of individuals in manage-
ment - in laboratory work
Basis for funding other than fees for direct services performed.
Cooperation Obtained
Intent. To determine the degree of cooperation of the entire laboratory
in the total evaluation procedure. If such cooperation is not evident,
capability of management is questionable.
Request a brief oral description of how the preliminary questionnaire
was handled. How were various sections distributed for completion?
Who decided who would answer the different sections? How were person-
nel advised of the importance of cooperation in the evaluation? Try to
discover:
Reasons for not providing complete information
Any plans for using results of evaluation for benefit of
the laboratory.
71
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PART 2. PERSONNEL
Before visit is made some scores can be assigned from data already
received on Chart A, Preliminary Questionnaire, Section 4.
Supervisor Training
All personnel in supervisory positions should have a university
degree. Under unusual circumstances experience in specific methodology
used in environmental monitoring laboratories and experience in such a
laboratory may be substituted; however, a non-degree person should have
had 5-10 years of experience.
Supervisor Experience
Determine from questioning of each supervisor the pertinence of
his experience to environmental monitoring problems, e.g.
Laboratory and field experience
Involvement in investigation of emergency episodes and
enforcement actions
Leadership in special studies
Length of experience in operation of laboratory functions
now engaged in.
Job Descriptions
Study job descriptions carefully to determine if indeed the jobs
are carried out according to the description. Make notes about jobs
beside each name on Chart A, Section 4, so that you can ascertain
through conversation whether what he actually does compares closely
with the position as described.
Training Program
Check information received on training programs. If no formal
training program exists, more time will be required on the visit to
determine what is done for training. Question individuals to determine
if they have received any training since joining the laboratory. Ask
how much time is devoted to training on starting employment at the
laboratory and how it is continued.
Turnover Rate
The rate of turnover may serve as an unobtrusive measure of
effective personnel management. A consistently high turnover rate may
indicate operating problems which the management is not successfully
72
-------
handling. However, this is not the whole story because turnover rate
may be due to causes beyond the laboratory management's control.
Discreet questions may be asked about employment problems both of
supervision and of analysts. Do personnel ceilings or funding problems
interfere with administration of a sound salary policy? Are sound
hiring procedures used for obtaining new personnel? Is hiring
according to the crony system? Do Civil Service regulations apply?
Is there a functioning affirmative action program?
General Morale
This question is related to the general morale and well being .
of the people employed at the laboratory. Determine by questions if
any positive stpes are taken by the laboratory management to indicate
some concern for individuals.
Does management urge that training programs are taken either
on site or at a nearby school?
Is there a definite program for advancement?
Are careful records kept on advancement?
What is done regarding health programs?
The morale question is wider than whether policies exist and records
are kept. Are employee organizations or unions in existence? What
percentage of employees belong to unions? Ask analysts as well as
supervisors about the state of relations between workers and management.
Is there an opportunity for input by laboratory personnel into technical
and management concerns of the laboratory?
73
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PART 3. LABORATORY SPACE AND FACILITIES
Refer to Chart B, Preliminary Questionnaire, Section 4.
General Characteristics
The location of the laboratory, proximity to public transportation,
its outside appearance, and a walk through of the building should help
the evaluator to determine whether it is generally acceptable as an
environmental monitoring laboratory.
Although many general features of the laboratory may have been
checked in Chart B of the Preliminary Questionnaire, some discreet
questions of laboratory personnel may be helpful.
» Is the location such that housing is available to the staff
without excessive travel?
Are there public eating facilities nearby, available for
the entire staff?
Is the neighborhood one that would cause no worry to any
staff member who worked late?
Consider whether general support facilities are 'appropriate to the
size and nature of the laboratory, i.e., secretarial'and technician
support, duplication facilities, photographic facilities, machine
shop, electrical/electronics shop, glass blowing, etc.
Observe the adequacy of the visitor reception area, conference
room, employee lounge or lunch room, locker space, drinking fountains,
heating and air conditioning, service for electricity (Voltage stable?),
gas, compressed air, and vacuum, etc. (filters installed?) Use Chart B
as a guide, if desired.
Office Space
How does the square foot of office space per person compare to the
adopted standard of 16.7 m2 (180 sq. ft)?
Laboratory Space
How does the square foot of laboratory space per person compare
to the adopted standard of 18.5 m2 (200 sq. ft)?
Bench Top Space
How does the length of bench top per person compare to the adopted
standard of 1.2m (4 ft)?
74
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Hood Space and Operation
Examine hoods to make certain they operate properly. Ask, if in
the opinion of the lab staff they are sufficient both in space and
exhaust capability. Are records kept showing hood monitoring with
velometer, last cleaning of ducts, general condition of glass, services,
etc.? Filters last changed? Adopted standard 0.5 m/s (100 ft./min.).
Storage Space for Chemicals, Reagents, Glassware, and Supplies
The laboratory should have separate storage spaces for general
chemicals, volatile chemicals and solvents, reagents, glassware and
general supplies.
Closed cabinets should be used to keep bottles, glassware etc.,
free of dust and contamination from fumes.
Storage of volatile chemicals should meet OSHA standards:
closed metal cabinet, under negative pressure, and away from flame/
heat or sparks. (This may be storage under hood if under constant
negative pressure).
No more than one liter each of volatile chemicals and solvents
should be stored in the laboratory area. Larger amounts should be
held in a. separate storage facility away from the laboratory.
Use of carcinogenic/mutagenic chemicals should be kept to a
minimum. If used these should be stored, handled and weighed in a glove
box under constant negative pressure. Wherever possible, substitute
chemicals or procedures should be used.
There should be sufficient in-lab storage available to permit
the clearing of bench tops between test series. This is important for
assurance of good control over procedures and for safety of the worker.
Storage areas should be inspected and corrected for overcrowding,
breakage, outdated chemicals and general condition as a part of the
routine lab clean-up.
Sample Storage
It is necessary not only that there be sufficient, accessible,
well arranged storage space for general samples but also that provisions
be made for special requirements of some samples, such as secured areas,
refrigerated areas, and facilities for isolated storage of contaminated
samples.
Controlled Space
The need for temperature and humidity control, for noise or
electrical shielding and for clean rooms will depend on the media
75
-------
handled by the laboratory. Using answers given In preliminary
questionnaire, Chart B, question staff about requirement if space
is not available.
Safety Equipment/Procedures
An opportunity was given in the preliminary questionnaire
to check availability of specific items of equipment. Check the
condition of this equipment.
In addition, observe, or ask questions about safety related matters.
Examples:
Eye protections, respiratory protection, floors not slippery,
trash cans adequate and emptied regularly, first aid kit
available?
Does lighting in the laboratory meet standard of 100 ft.
candles at bench top? If possible, carry a light meter to
place on benches and desks to actually measure amount of
light.
Are fire prevention regulations posted? Smoking rules?
Is area use clearly marked?
Is the fire alarm clearly audible?
Are exits marked and illuminated?
Are fire extinguishers conspicuously located and in working
order? Inspected last?
Are emergency telephone numbers posted?
Fire Medical
. Are regular fire drills conducted? When? Has local fire
department ever visited laboratory? When?
Does the laboratory give the appearance of having a constant
awareness of the importance of safety?
Distilled Water/Deionized Water
Determine who is responsible for the stills, which supply distilled
water. Is there a central supply of deionized water? Are checking
procedures written and a record maintained?
76
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Glassware Supply and Washing
Is a sufficient supply of all the necessary types of glassware
available? Is the glassware washing area convenient to work areas
served? Is sufficient space provided for washing and drying? Are
water supply, drains, drying ovens (165°C) and racks adequate? Are
there written procedures for handling special glassware? Are
contaminated containers sterilized or disinfected prior to washing?
Are water spots present on recently washed ware? Are items tested
for detergent removal (by appropriate indicator)? Is rinse water
supply adequate? Are chipped or scratched items discarded? Are
pipettes stored in aluminum or stainless steel (not copper) cans?
Housekeeping
Are passageways kept clear? Are broken glass and contaminated
materials properly collected and disposed of? Are floors clean and
well maintained? Are rooms and benches clean and uncluttered?
Data Processing Equipment and Logistic Services
Does laboratory have its own data processing facilities or access
to a shared system? Is telephone service adequate? Is there an intercom
system? Is there an emergency outside line? Is there a motor vehicle
pool of any sort?
77
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PART. A. ANALYTICAL METHODS
Refer to Chart C, Preliminary Questionnaire, Section 4.
Intent. The intent of the part is to determine actual laboratory
practices in the conduct of tests. Discuss each test for which the
laboratory is being evaluated with individual "bench analysts", or
their immediate supervisors.
Are copies of the correct methods readily available to
analysts?
Do the analysts follow the methods exactly?
Does the laboratory require adherence to a specific control
program for each sampling procedure and analytical test?
(Note: specific questions about sampling, calibration, and
laboratory quality control procedures are asked in Part 6,
Section 6.)
Reference Methods or Approved Alternates
All methods must be Federal Register referenced methods or
specific EPA approval must have been obtained for modifications or
alternates.
Reagent and Media Preparation
Intent. To assess the care taken in preparation, use, and storage of
reagents and microbiological culture media.
Suggested Approach
The evaluator should inspect reagent bottles and media containers
for clear and complete labelling, including date of preparation (or
reference to a log containing dates of preparation). Containers should
be appropriate for the particular reagent or medium and should be stored
under appropriate conditions (temperature, light, etc.). Questions
might include:
, Is there a written schedule for preparation of fresh reagents
and media? (Some must be prepared on the day of the analysis,
while others may be kept for extended periods under proper
conditions.)
Are new reagent batches always checked immediately against
reference standards?
Is a record kept of reagent batches and dates used?
78
-------
Is responsibility clearly assigned for preparing and
maintaining fresh supplies of reagents and media?
Are reagents rechecked at intervals against standards for
possible contamination or degradation?
79
-------
PART 5. FORMS FOR ONSITE EVALUATION
The following pages contain questions that may be asked about
performance of specific tests, arranged by media.
In putting this material together, we have drawn on many sources, some
of which, such as the EPA form for the bacteriological survey for water
laboratories, have been used successfully in practice for some time.
Other parts are drawn from recent USEPA or State EPA experience wherever
the material appears to have been assembled in form most closely fitting
the purpose of this procedure. Although, in the following outline of
this material, we have indicated the primary source from which we ob-
tained the material, we realize that many people may have been involved
and we acknowledge our debt to the many individuals and groups with
whom we have held discussions during the course of this task.
Part A. Medium- Water (Chemistry). Illinois EPA, Springfield
Laboratory.
Part B. Medium- Water (Bacteriology). USEPA, Water Quality Office,
Water Hygiene Division, Cincinnati.
Part C. Medium- Water (Biology). USEPA Environmental Monitoring
Laboratory, Cincinnati.
Part D. Medium- Air. USEPA Environmental Monitoring Laboratory,
Research Triangle Park.
Part E. Medium- Pesticides. USEPA Environmental Monitoring
Laboratory, Research Triangle Park
Part F. Medium- Radiation. USEPA Environmental Monitoring
Laboratory, Las Vegas.
Some of the material available to us was in rough draft form and,
as updated versions become available, it may be desirable to include
them in this Evaluator's Guide.
80
-------
PART A. MEDIUM - WATER
(CHEMISTRY)
Type of samples
Surface or ground water
Industrial waste
Domestic mixed sewage
Marine or estuary water
Sediment, sludge, or semi-solid
Equipment-Analytical balance-
Annual service, documented
Certified weights available
Monthly check with certi-
fied weights, documented
Autoclave
Checked yearly by manufacturer
with maximum registering thermo-
meter
Safety valve works
Operating instructions posted or
available
Deionizer
Million ohm water checked daily and
documented
KMnO. 60 min. color retention check-
ed daily and documented
Still
Checked daily and quality documented
Operating instructions posted or available
81
-------
Distilled water
Checked for copper, ammonia,
and chlorine documented
Conductivity bridge
Checked daily, documented
Double deionized water
Available for trace anal-
ysis
pH meter
Standardized for each use with buffer,
documented
Checked daily against second buffer
for linearity, documented
Flouride electrode
standardized with each use,
documented
Colorimeter
Calibration curves checked with at
least one standard each time used
Drying ovens
Temperature checked daily and re-
corded
record indicates satisfactory oper-
ation and temperature controller
functioning correctly
Muffle furnace pyrometer
Pan balances
Clean and in servicable condition
82
-------
Checked each month with two anal-
ytical balance weights
Automated analyzers
Standard and blanks run
each time
Test frequency allows instru-
ment to return to baseline
between tests
Record maintained of readings
of standards for each test
each time instrument is oper-
ated
Maintenance schedule followed
for pump tube replacement,
colorimeter cell cleaning,
etc.
Incubator BOD
Thermometer calibrated, Documented
Daily record
Uniformity of temperature check,
documented
Certified thermometer
Certification on file
Record of thermometer
checks
Pipette containers-
Alumimum or stainless steel,
no copper
83
-------
Dry heat sterilizer
Temperature documented with
recorder, charts filed
accuracy of recorder checked
Microscope
Binocular wide field
Fluorescent light source
84
-------
CHEMISTRY METHODS
BOD
Dilution water checked for residual chlorine, NHL and Cu
Dilution water depletion on 5 days not more than 0.2 mg/l
If D.O. probe is used, calibration documented
If D.O. probe is used, correlation with Winkler method documented
Water seals on bottles protected
Dilutions for calculation are in the range which shows depletion of
at least 2 mg/l and residual D.O. of I mg/l
Supersaturated samples deaerated before setting up
Chlorinated effluents checked for residual chlorine
Incubator temperature 20 ± 1 C documented
Method checked periodically by running glucose-glutamic acid standard
Seeding used when required On chlorinated effluents
On other sterile samples
Sodium thiosulfate stock preserved, standardized, refrigerated, and documented
o
Samples refrigerated at 4 C immediately at point of collection and
delivered to lab within 12 hours
Analyst does not pipet samples by mouth
Samples pipetted by
COD - dichromate reflux method
Samples preserved by .acidification, refrigeration, or both
Silver sulfate catalyst used
Mercuric sulfate used to depress chloride interference
Standardization of dichromate documented
Use boiling chips for smooth boiling
85
-------
Daily standardization of ferrous ammonium sulfate documented
Sample, reagents, and sulfuric acid mixed thoroughly before heat is applied
Analyst uses safety glasses or eye protection
Analyst does not pipet sample or reagents by mouth
Wastes properly disposed of
pH - electrometric method
Instrument manufacturer's instructions available and followed
Instrument checked for linearity with two buffers, documented
Instrument standardized daily, documented
Calomel electrode - liquid junction functioning
Calomel electrode - contains at least a crystal of KC1 but not solid
with KC1
Electrodes rinsed between samples with distilled water and/or
sample to be measured
Measurements made on successive portions of sample until
two successive portions give equal readings
Sample temperature compensation applied
Solution pressure inside the calomel liquid junction in excess
of that outside the junction
Immersible tips of electrodes stored in reagent water between
periods of use
Sample agitated while making measurement
86
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PART B. MEDIUM - WATER
(Bacteriological Examination)
ENVIRONMENTAL PROTECTION AGENCY
Water Quality Office
Water Hygiene Division
Bacteriological Survey for
Water Laboratories
Indicating conformity with the 13th
edition of "Standard Methods for the
Examination of Water and Waste-
water," 1971.
Survey By
X = Deviation
U = Undetermined
O = Not Used
Laboratory
Location
Date
Sampling and Monitoring Response
1. Location and Frequency
Representative points on system .
Frequency of sampling adequate .......
2. Collection Procedure
Faucets with aerators should not.be used
Flush tap 1 min. prior to sampling
Pump well 1 min. to waste prior to sampling
River, stream, lake, or reservior sampled at least
6 inches below surface and toward current
Minimum sample not less than 100 m! . .
Ample air space in bottle for mixing
Promptly identify sample legibly and indelibly
3. Sample Bottles
Wide mouth, glass or plastic bottles of capacity . .
Sample bottles capable of sterilization and rinse
Closure:
a. Glass stoppered bottles protected with metal foil,
rubberized cloth or kraft type paper
b. Metal or plastic screw cap with leakproof liner . .
Sodium thiosulfate added for dechlorination
Concentration of 100 mg/l added before sterilization . .
Chelation agent for stream samples (optional) ,
Concentration 372 mg/l added before sterilization ...
4. Transportation and Storage
Complete and accurate data accompanies sample ....
Transit time for potable water samples should not exceed
48 hrs, preferably within 30 hrs
Transit time for source waters, reservoirs, and natural
bathing waters should not exceed 6 hrs
All samples examined within 2 hrs of arrival
Sample refrigeration mandatory on stream samples,
optional on potable water samples
5. Record of Laboratory Examination
Results assembled and available for inspection
Number of tests per year
87
-------
Laboratory Location Date
5. Record of Laboratory Examination (Continued)
MPN Test - Type of sample
Confirmed (+) (-) (Total).
Completed (+) (-) (Total).
MF Test - Type of sample
Direct Count (+) (-) (Total).
Verified Count (+) (-) (Total).
Data processed rapidly through laboratory and engineering sections
Unsatisfactory sample defined as 3 or more positive tubes per
MPN test or 5 or more colonies per 100 ml in MF test . . . .
High priority placed on alerting operator to unsatisfactory
potable water results
Prompt resampling for unsatisfactory samples
6. Laboratory Evaluation Service
State program to evaluate all laboratories which examine
potable water supplies
Frequency of surveys on a year basis
State survey officer (namp) . .
Status of laboratory evaluation services
Total labs known to examine water
approved laboratories
provisional laboratories
Laboratory Apparatus
7. Incubator
Manufacturer Model
Sufficient size for daily work load . . .
Maintain uniform temperature in all parts (± 0.5° C) . . . .
Accurate thermometer with bulb immersed in liquid on
top and bottom shelves
Daily record of temperature or use of recording thermometer
sensitive to 0.5° C change
Incubator not subject to excessive room temperature variations
beyond a range of 50 - 80° F
8. Incubator Room (Optional) Manufacturer
Well insulated, equipped with properly distributed heating
and humidifying units for optimum enviornmental control .
Shelf areas used for incubation must conform to 35° C ± 0.5°
temperature requirement
Accurate thermometers with bulb immersed in liquid ....
Daily record of temperature at selected areas or use
recording thermometer sensitive to 0.5° C changes ....
9. Water Bath
Manufacturer Model
Sufficient size for fecal coliform tests
Maintain uniform temperature 44.5° C ± 0.2° C.
Accurate thermometer immersed in water bath
Daily record of temperature or use of recording
thermometer sensitive to 0.2° C changes
88
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Laboratory
Location Date
10. Hot Air Sterilizing Oven
Manufacturer Model
Size sufficient to prevent crowding of interior. .
Constructed to insure a stable sterilizing temperature ....
Equipped with accurate thermometer in range of 160 -180° C
.. .or .with.recording thermometer
11. Autoclave
Manufacturer Model
Size sufficient to prevent crowding of interior.
Constructed to provide uniform temperature up to and
including 121° C
Equipped with accurate thermometer with bulb properly located
. to .register minimal temperature within chamber
Pressure gage and operational safety valve
Steam source from saturated steam line, or from gas or
. electrically heated steam generator
Reach.sterilization temperature in 30 min
Pressure cooker may be used only if provided with a pressure
gage and thermometer with bulb 1 inch above water level . .
12. Thermometers
Accuracy checked with thermometer certified by National
Bureau of Standards or one of equivalent accuracy
Liquid column free of discontinuous sections and graduation
marks legible
13. pH Meter
Manufactuer : Model
Electronic pH meter accurate to 0.1 pH units
14. Balance
Balance with 2 g sensitivity at 150 g load used for general
media preparations, Type
Analytical balance with 1 mg sensitivity at 10 g load used
for weighing quantities less than 2 g, Type
Appropriate weights of good quality for each balance . . .
15. Microscope and Lamp
Preferably binocular wide field, 10 to 15 diameters magnifi-
cation for MF colony counts, Type.
Fluorescent light source for sheen discernment
16. Colony Count
Quebec colony counter, dark-field model preferred for
standard plate counts
17. Inoculating Equipment
Wire loop of 22 or 24 gauge chromel, nichrome, or platinum
iridium, sterilized by flame
Single-service transfer loops of aluminum or stainless steel, pre-
sterilized by dry heat or steam
Disposable single service hardwood applicators, pre-
sterilized by dry heat only
18. Membrane Filtration Units
Manufacturer Type
Leakproof during filtration .
Metal plating not worn to expose base metal
89
-------
Laboratory Location Date
19. Membrane Filters
Manufacturer Type
Full bacterial retention, satisfactory filtration speed
Stable in use, glycerin free
Grid marked with non-toxic ink
Presterilized or autoclaved 121 ° C for 10 min. . .
20. Absorbent Pads
Manufacturer Type
Filter paper free from growth inhibitory substances . . . :
Thickness uniform to permit 1.8 - 2.2 ml medium absorption
Presterilized or autoclaved with membrane filters
21. Forceps
Preferably round tip without corrugations
Forceps are alcohol flamed for use in MF procedure . . . .
Glassware, Metal Utensils and Plastic Items
22. Media Preparation Utensils
Borosilicate glass
Stainless steel
Utensils clean and free from foreign residues or
dried medium
23. Pipettes
Brand Type
Calibration error not exceeding 2.5%
Tips unbroken, graduation distinctly marked . .
Deliver accurately and quickly
Mouth end plugged with cotton (optional) . . .
24. Pipette Containers
Box, aluminum or stainless steel
Paper wrapping of good quality sulfite paper (optional)
25. Petri Dishes
Brand Type
Use 100 mm x 15 mm dishes for pour plates . . . .
Use 60 mm x 15 mm dishes for MF cultures . . . .
Clear, flat bottom, free from bubbles and scratches
Plastic dishes may be reused if sterilized in 70% ethanol for
30 min. or by ultraviolet radiation
26. Petri Dish Containers
Aluminum or stainless steel cans with covers, coarsely woven
wire baskets, char-resistant paper sacks or wrappings . . .
27. Culture Tubes
Size sufficient for total volume of medium and sample portions
Borosilicate glass or other corrosive resistant glass
28. Dilution Bottles or Tubes
Borosilicate or other corrosive resistant glass
Screw cap with leakproof liner free from toxic substances
on sterilization
Graduation level indelibly marked on side of bottle or tube
90
-------
Laboratory Location Date
Materials and Media Preparation
29. Cleaning Glassware
Dishwasher manufacturer Model
Thoroughly washed in detergent at 160° F, cycle time
Rinse in clean water at 180° F, cycle time .
Final rinse in distilled water, cycle time . .
Detergent brand
Washing procedure leaves no toxic residue
Glassware free from acidity or alkalinity
30. Sterilization of Materials
Dry heat sterilization (1 hrat170°C)
Glassware not in metal containers
Dry heat sterilization (2 hrs at 170° C)
Glassware in metal containers
Glass sample bottles
Autoclaving at 121° C for 15 min
Plastic sample bottles
Dilution water blanks
31. Laboratory Water Quality
Still manufacturer Construction material _
Demineralizer with recharge frequency
Protected storage tank
Supply adequate for all laboratory needs
Free from traces of dissolved metals or chlorine
Free from bactericidal compounds as measured
by bacteriological suitability test
Bacteriological quality of water measured once each year
by suitability test or sooner if necessary
32. Buffered Dilution Water
Stock phosphate buffer solution pH 7.2
Prepare fresh stock buffer when turbidity appears
Stock buffer autoclaved and stored at 5 -10° C
1.25 ml stock buffer per 1 liter distilled water
Dispense to give 99 ± 2 ml or 9 ± 0.2 ml after autoclaving . . . .
33. pH Measurements
Calibrate pH meter against appropriate standard buffer prior to use
Standard buffer brand pH
Check the pH of each sterile medium batch or at least one batch
from each new medium lot number
Maintain a pH record of each sterile medium batch,
the date and lot number
34. Sterilization of Media
Carbohydrate medium sterilized 121° C for 12 min
All other media autoclaved 121° C for 15 min
Tubes packed loosely in baskets for uniform heating and cooling
Timing starts when autoclave reaches 121° C
Total exposure of carbohydrate media to heat not over 45 min. .
Media removed and cooled as soon as possible after sterilization .
91
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Laboratory
Location Date
35. Storage
Dehydrated media bottles kept tightly closed and stored
at less than 30° C
Dehydrated media not used if discolored or caked . . . .
Sterile culture media stored in clean area free from
contamination and excessive evaporation
Sterile batches used in less than 1 week
All media protected from sunlight
If media is stored at low temperatures, it must be incubated
overnight and any tubes with air bubbles discarded . . .
Culture Media - Specifications
36. Lactose Broth
Manufacturer Lot No.
Single strength composition 13 g per liter distilled water. .
Single strength pH 6.9 ± 0.1, double strength pH 6.7 ± 0.1 .
Not less than 10 ml medium per tube
Composition of medium after 10 ml sample is added must
contain 0.013 g per ml dry ingredients
37. Lauryl Tryptose Broth
Manufacturer Lot No.
Single strength composition 35.6 g per liter distilled water .
Single strength pH 6.8 ± 0.1, double strength pH 6.7 ± 0.1 .
Not less than 10 ml medium per tube
Composition of medium after 10 ml sample is added must
contain 0.0356 g per ml of dry ingredients
38. Brilliant Green Lactose Bile Broth
Manufacturer Lot No.
Correct composition, sterility and pH 7.2
Not less than 10 ml medium per tube
39. Eosin Methylene Blue Agar
Manufacturer Lot No.
Medium contains no sucrose, Cat. No.
Correct composition, sterility and pH 7.1 . . . .
40. Plate Count Agar (Tryptose Glucose Yeast Agar)
Manufacturer Lot No.
Correct composition, sterility and pH 7.0 ±0.1 . .
Free from precipitate
Sterile medium not remelted a second time after sterilization
41. EC Medium
Manufacturer ' Lot No.
Correct composition, sterility and pH 6.9
Not less than 10 ml medium per tube
42. M-Endo Medium
Manufacturer Lot No.
Correct composition and pH 7.1 - 7.3
Reconstituted in distilled water containing 2% ethanol
Heat to boiling point, promptly remove and cool . .
Store in dark at 2-10° C
Unused medium discarded after 96 hrs
92
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Laboratory Locati°P Date
43. M-FC Broth
Manufacturer Lot No.
Correct composition and pH 7.4
Reconstituted in 100 ml distilled water containing 1 ml of
a 1% rosolic acid reagent
Stock solution of rosolic acid discarded after 2 weeks or
when red color changes to muddy brown
Heat to boiling point, promptly remove and cool ...
Store in dark at 2-10° C
Unused medium discarded after 96 hrs
44. Broth
Manufacturer Lot. No.
Correct composition and pH
45. Agar
Manufacturer Lot No.
Correct composition and pH
Multiple Tube Coliform Test
46. Presumptive Procedure
Lactose broth lauryl tryptose broth ,
Shake sample vigorously
Potable water: 5 standard portions, either 10 or 100 ml . . .
Stream monitoring: multiple dilutions
Incubate tubes at 35° ±0.5° C for 24 ±2 hrs
Examine for gas any gas bubble positive
Return negative tubes to incubator
Examine for gas at 48 ± 3 hr from original incubation
47. Confirmed Test
Promptly submit all presumptive tubes showing gas production
before or at 24 hr and 48 hr periods to confirmed test . . .
a. Brilliant green lactose broth
Gently shake presumptive tube or mix by rotating
Transfer one loopful of positive broth or one dip of applicator .
from presumptive tube to brilliant green lactose broth . . .
Incubate at 35° ± 0.5° C and check at 24 hrs for gas production
Reincubate negative tubes for additional 24 hrs
and check for gas production
Calculate MPN or report positive tube results
b. Endo or eosin methylene blue agar plates adequate streaking
to obtain discrete colonies separated by 0.5 cm
Incubate at 35° ± 0.5° C for 24 ±2 hrs
Typical nucleated colonies with or without sheen are coliforms .
If atypical unnucleated pink colonies develop, result is
doubtful and completed test must be applied
If no colonies or only colorless colonies appear, the
confirmed test is negative
48. Completed Test
Applied to all potable water samples or a proportion each three
months to establish the validity of the confirmed test in
determining their sanitary quality
93
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Laboratory
Location Date
48. Completed Test (Continued)
Applied to positive confirmed tubes or to doubtful colonies
on differential medium
Streak positive confirmed tubes on Endo or EMB plates for
colony isolation
Choice of selected isolated colony for verification should be one
typical or two atypical to lactose or lauryl tryptose broth and
to agar slant for gram stain
lncubateat35°C±0.5°Cfor24hrsor48hrs
Gram negative rods without spores and gas in lactose tube
with 48 hrs in positive completed test
Membrane Filter Coliform Test
49. Application as Standard Test
Use as a standard test for determining potability of water after
demonstration by parallel testing that it yields information
equal to that from the multiple-tube fermentation procedure . . .
50. MF Procedure
Filter funnel and receptacle sterile at start of series
Rapid funnel resterilization by UV, flowing steam or boiling water
acceptable
Membrane filter cultures and technician eyes should not be
subject to UV radiation leaks
Filtration volume not less than 50 ml for potables water; multiple
dilutions for stream pollution
Rinse funnel by flushing several 20 - 30 ml portions of sterile buffered
water through MF
Remove filter with sterile forceps
Roll filter over M-Endo medium pad or agar so air bubbles
will not form
51. Incubation
In high humidity or in tight fitting culture dishes
At 35° C ± 0.5° C for 22 - 24 hrs
52. Counting
All colonies with a metalljc yellowish green surface sheen
If coliforms are found in potable samples, verify by transfers
to lactose broth, then to BGB broth for evidence of gas
production at 35° C within 48 hr limit
Calculate direct count in cofiform density per 100 ml
53. Standard MR Test with Enrichment
Incubate MF after filtration on pad saturated with lauryl tryptose
broth for 1 1/2 - 2 hrs at 35° C ± 0.5° C .
Transfer MF culture to M-Endo medium for a final
20 - 22 hr incubation at 35° C ± 0.5° C
Count sheen colonies, verify if necessary, and calculate
direct count in coliform density per 100 ml
Supplementary Bacteriological Methods
54. Standard Plate Count
Plate not more than 1 or less than 0.1 ml (sample or dilution)
Add 10 ml or more liquified agar medium at a temperature
between 43 - 45° C
94
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Laboratory
Location Date
54. Standard Plate Count (Continued)
Melted medium stored for no more than 3 hrs at 43 - 45° C . . .
Liquid agar and sample portion thoroughly mixed by gently
rotating to spread mixture evenly
Count only plates with between 30 and 300 colonies, exception
being 1 ml sample with less than 30 colonies
Record only two significant figures and calculate as "standard
plate count at 35° C per 1 ml of sample"
55. Fecal Coliform Test
a. Multiple Tube Procedure
Applied as an EC broth confirmation of all positive
presumptive tubes
Place EC tubes in water bath within 30 min. of transfers. .
lncubateat44.5°C±0.2°Cfor24hrs
Gas production is positive test for fecal coliforms ....
Calculate MPN based on combination of positive EC tubes .
b. Membrane Filter Procedure
Following filtration place MF over pad saturated with
M-FC broth
Place MF cultures in waterproof plastic bag and submerge
in water bath within 30 min
lncubateat44.5°C±0.2°Cfor24hrs
All blue colonies ar fecal coliforms
Calculate direct count in density per 100 ml
56. Delayed-lcubation Coliform Test
After filtration, place MF over pad of M-Endo containing 3.2 ml
of a 12% sodium benzoate solution per 100 ml of medium . .
Addition of 50 mg cycloheximide per 100 ml of preservative
medium for fungus suppression is optional
Transport culture by mail service to laboratory within 72 hrs . . .
Transfer MF cultures to standard M-Endo medium
at laboratory
lncubateat35°C±0.5°Cfor20-22hrs
If at time of transfer growth is visible, hold in refrigerator
till end of work day then incubate at 35° C overnight
(16-18 hr period)
Count sheen colonies, verify if necessary, and calculate ,
direct count in coliform density per 100 ml
57. Additional Test Capabilities
Fecal streptococci Method
Pseudomonas aeruginosa Method
Staphylococcus Method
Salmonellae Method
Biochemical tests Purpose
Serological tests __ Purpose
Other Purpose
95
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Laboratory
Location Date
Laboratory Staff and Facilities
58. Personnel
Adequately trained or supervised for bacteriological
examination of water
Laboratory staff (Total) Prep room staff (Total)
59. Reference Material
Copy of the current edition of Standard Methods available
in the laboratory
State or federal manuals on bacteriological procedures for
water available for staff use
60. Physical Facilities
Bench-top area adequate for periods of peak work in
processing samples
Sufficient cabinet space for media and chemical storage
Office space and equipment available for processing water
examination reports and mailing sample bottles
Facilities clean, with adequate lighting, ventilation and
reasonably free from dust and drafts
61. Laboratory Safety
Proper receptacles for contaminated glassware and pipettes ....
Adequately functioning autoclaves with periodic inspection
and maintenance
Accessible facilities for hand washing
Proper maintenance of electrical equipment to prevent fire
and electrical shock
Convenient gas and electric outlets
First aid supplies available and not out-dated
62. Remarks
96
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PART C. MEDIUM-WATER BIOLOGY
BIOLOGICAL FIELD EQUIPMENT
A. Mobile Labs
1. Number available ( )
(Check) 2. Equipped for:
___ a. Static bioassay
b. Flow-through bioassay
c. Fish bioassay
d. Macroinvertebrate bioassays
e. Algal assay
B. Boat and Motors
C.
D.
Type
1.
2.
3.
4.
S.
Age
Condition.
Hull
Length
Beam
HP
Floatation
Integral
Other
Scuba Gear
General description of available gear.
Sampling Equipment
1. Plankton
a. Water Bottles
(1) Kemmerer
a
L&J
c)
(2) Van Dorn
a)
b)
(c)
Metallic
Plastic
Volume
(liters)
b.
c.
d.
Pump sampler
Integrated (Tubular) sampler
Plankton Net
Wisconsin type (net mesh size
Clark-Bumbus type (net mesh size.
-------
BIOLOGICAL FIELD EQUIPMENT
D. Sampling Equipment (Continued)
2. Periphyton
a. Substrate type
(1) Glass
(2) Plexiglass
(3) Other (specify)
vo
oo
b.
c.
d.
Substrate dimensions
cmX
cm
Substrate exposure depth,
Substrate Orientation
(1) Vertical
(2) Horizontal
cm
3. Macrophyton:
Specify:
4. Macroinvertebrates:
a. Grabs
Type
Ponar
Petersen
Ekman
Tall Ekman
Other (specify)
Area of bite (m^)
.0232
.0523
.0929
Other
b. Corers
Specify:
-------
BIOLOGICAL FIELD EQUIPMENT
D. Sampling Equipment (Continued)
4. Macroinvertebrates (Continued)
c. Artificial Substrates
(1) Multiplate
(2) Masonite
(3) Other (Specify)
vo
VO
d.
e.
f.
g.
Basket
(1) Limestone
(2) Other (Specify)
Surber sampler
Other samplers
Sieves
(1) #30 Standard
(2) #40 Standard
(3)
.(Other)
5. Fish
a. Shocker
(1) AC
(2) DC
(3) Operating voltage
(4) Manufacturer
b. Gill nets
(1)
(2)
(3)
(4)
Mesh size (cm)
Length (m)
-------
BIOLOGICAL FIELD EQUIPMENT
c. Trammel nets
o
o
d.
e.
0)
(2)
(3)
(4)
Mesh size (cm)
Length (m)
Seines
(D
(2)
(3)
(4)
Mesh size (cm)
Length (m)
Trawls
(1 ) Specify
E. Miscellaneous
Instrument
1. Submarine Photometer
2. Current meter
3. Secchi measurement
4. Benthic respirometer
5. Secchi disk
Manufacturer
Type/Model
Age
Condition
r
:.
-------
A.
Counting and Identification
1. Microscopes
a. Compound, monocular
(D
(2)
(3)
b. Compound, binocular
(D
(2)
(3)
c. Portable field microscope
d. Stereo (dissection) microscope
(1) Rotating nosepiece
(a)
(b)
(c)
(2) Zoom
(a)
(b)
(c)
Age/
Cond.
Manuf.
Ocular(s)
Magnif.(X)
Objectives
X
X
X
X
Magnifica-
tion range
1
1!
11
m
HI
Nomarski
I
i:i:i:i:i:i:
^P
^
M
^ kj
h_
~o o
o. E
.9- Q
§ °
u
Q.
0.
-------
BIOLOGICAL LABORATORY EQUIPMENT
B. Biomass Determination
o
NJ
1. Balance
a.
b.
c.
2. Drying oven
3. Vacuum oven
4. Muffle furnace
Temp cnntrnl (7)
5. Desiccators
6. ATP measuring instruments
a.
b.
7. Centrifuge
Refrigerateri (?)
8. Freeze drier
No.
Avail.
Make
Type/Model
Size, etc.
Age
Condition
-------
BIOLOGICAL LABORATORY EQUIPMENT
C. Chlorophyll Measurements
Instrument
1 . Spectrophotometer c
a.
b.
c.
2. Fluorometer
a.
b.
c.
(List excitation and emission
filters for fluorometers)
3. Tissue grinder
4. Sonifier
No.
Avail.
Make
Type/Model
Size, etc.
s
Age
Condition
D. Culturing and Rearing Equipment
1. Algal culture chamber
2. Macroinvertebrate
3. Fish
-------
BIOLOGICAL LABORATORY EQUIPMENT
E. Bioassay Facilities
1. Algal Assay - (Describe briefly)
2. Macroinvertebrate bioassay - (Describe briefly)
o
IS
3. .Fish bioassay
a. Static bioassay - (Briefly describe size and number of dilution water supply chambers, number
of replicates, number of tests that can be run simultaneously, temperature
control, and other supporting equipment.)
b. Flow-through -
(Briefly describe size and number of chambers, dilution water supply, temperature
control, diluters, etc. )
-------
BIOLOGICAL (SAMPLE ANALYSIS
i
(Work load and methodology)
Type of Analysis
A. Plankton
1. Phytoplankton count & identification
2. Diatom species proportional count
3. Zooplankton count and identification
4. Ash-free weight
5. Chlorophyll determination
6. ATP determination
7. Primary productivity, oxygen method
8. Primary productivity, carbon-14 method
9. Algal assay
B. Periphyton
1. Cell counts and identification
2. Diatom species proportional counts
3. Ash-free weight
4. Chlorophyll determinations
5. ATP determination
No.,
Samples/
y.
Methodology
EPA
Stand.
Methods
Other
Comments
-------
Type of Analysis
C. Macrophyton
1. Identification
2. Ash-free weight
3. Chlorophyll
D. Macroinvertebrates
1. Counts and Identification
2. Ash-free weight
3. Flesh tainting
4. Tissue analysis
5. Bioassay, static
6. : Bioassay, flow-through
E. Fish
1. Counts/I D/wgt/lgth
2. Flesh tainting
3. Tissue analysis
4. Bioassay, static
5. Bioassay, flow-through
No.
Samples/
y.
Metholology
EPA
Stand.
Methods
Other
Comments
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LIST OF BIOLOGICAL PROCEDURES
A. Phytoplankton
(Check) 1. Sample Volume (liters)
2. Preservative
a. Formalin
b. Merthiolate
c. Other (specify).
3. Counting Techniques used
a. Sedgwick-Rafter Cell
b. Palmer-Maloney Cell
c. Membrane Filter Counts
d. Inverted Microscope Method
e. Other (specify)
4. Counting units used
a. Natural Unit (clump count)
b. Areal Unit
c. Cell count
d. Cell volume
5. Identification Level
a. Total phytoplankton count
(1) Identify to genus
(2) Identify to species
(3) Identify to major groups only
b. Diatom species proportional count
6. Biomass measurements
a. Dry weight
b. Ash-free weight
c. ATP
d. DMA
e. Chlorophyll
(1) Solvent used
(2) Fluorometric, in vivo method
(3) Fluorometric, in vitro method
(4) Fluorometric, in pheophytin correction
(5) Spectrophotometric, Trichromatic, Strickland/Parsons
(6) Spectrophotometric, Trichromatic, SCQR/UNESCO
(7) Spectrophotometric, pheophytin correction
7. Metabolic Rates
a. Productivity, oxygen method
b. Productivity, Carbon-14 method
c. Nitrogen fixation, acetylene reduction
8. Algal Assay
a. Trophic level (biostimulation test)
b. Limiting nutrient test
c. Toxicity test
d. Bottle method
e. Flow-through method
107
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LIST OF BIOLOGICAL PROCEDURES (2)
B. Periphyton
(Check) 1. Sample area.
2. Preservative
a. Formalin
b. Merthiolate
c. Other (specify).
3. Counting Techniques used
a. Sedgwick-Rafter Cell
b. Palmer-Maloney Cell
c. Membrane Filter Counts
d. Inverted Microscope Method
e. Other (specify)
4. Counting units used
a. Natural Unit (clump count)
b. Areal Unjt
c. Cell count
d. Cell volume
5. Identification Level
a. Total phytoplankton count
(1) Identify to genus
(2) Identify to species
(3) Identify to major groups only
b. Diatom species proportional count
6. Biomass measurements
a. Dry weight
b. Ash-free weight
c. ATP
d. DNA
e. Chlorophyll
(1) Solvent used
(2) Fluorometric, in vivo method
(3) Fluorometric, in vitro method
(4) Fluorometric, pheophytin correction
(5) Spectrophotometric, Trichromatic, Strickland/Parsons
(6) Spectrophotometric, Trichromatic, SCQR/UNESCO
(7) Spectrophotometric, pheophytin correction
7. Metabolic Rates
a. Productivity, oxygen method
b. Productivity, Carbon-14 method
c. Nitrogen fixation, acetylene reduction
8. Bioassay
a. Trophic level (biostimulation test)
b. Limiting nutrient test
c. Toxicity test
d. Bottle method
e. Flow-through method
108
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LIST OF BIOLOGICAL PROCEDURES (3)
C. Macroinvertebrates
(Check) 1. Sample preservation
a. Formalin %
b. Ethanol %
c. Other (specify)
2. Sieve employed
a. Standard #30
b. Standard #40
c. Other (specify)
3. Sorting techniques
a. Stain with Rose bengal
b. Fluorescent stain
c. Other stain (specify)
d.~ Sugar floatation
e. Other separation method (specify).
4. Identification
(Check)
5.
6.
7.
8.
9.
Group
a. Diptera (excl. midges)
b. Midges
c. Trichoptera
d. Plecoptera
e. Ephemeroptera
f. Odonata
g. Neuroptera
h. Hemiptera
i. Crustacea
j. Hirudinea
k. Nematoda
1. Bivalvia
m. Gastropoda
Level of Identification
Order
Family
Genus
Species
Maintain reference collection of organ isms for identification
Use "outside" consultants for difficult identifications
Rear larvae to adult stage to aid in identifications
Tissue analysis for toxic substances
Bioassay
a. Static
b. Flow-through
109
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LIST OF BIOLOGICAL PROCEDURES (4)
D. Fish
(Check) 1. Preservative
a. Formalin
b. Other (specify).
2. Age determinations
a. Scales
b. Other (specify)
3. Condition factor (length-weight relationship)
4. Flesh tainting
5. Histopathological studies (describe):
6. Bioassays
a. Laboratory
(1) Static tests (describe):
(2) Flow-through tests (describe):
b. In-situ tests (describe):
110
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PART D. MEDIUM AIR
MANUAL - SO2 or N02
Sampling
Volume (No. of Samples)
Method of Delivery
(Field to Lab)
Sampler Used _
Frits-lmpingers
Time Between Sampling and Analysis
Storage Method
Analysis
Method
Copy Available
Calculations
Equipment
(Automated-Manual)
Preventive Maintenance
Chemical Purity of Reagents
Reagent Makeup Procedure
Reagent Standardization Procedure
Calibration
Procedure (Samplers)
Procedure (Analysis)
Copies Available
Frequency
Curves Available
Calibration History
Items
Reagents or
Schedule
Gases
111
-------
MANUAL - SO2 or NO2 (Continued)
Data Processing
Mode Utilized
(Strip Chart, Mag. Tape)
Discrepancies
S A ROAD Format _
Reduction Procedure
Reporting of Data
112
-------
Continuous SO2, NO2, C0>, or 03
Type of Analyzers
No. of Analyzers
No. of Field Stations
Containing Analyzers
Frequency of Sampling
Manpower (Attended-Unattended)
Frequency of Calibration
Method of Calibration
Traceability of Calibration
Curves Available
Documentation
Frequency of Zero and Span
Corrective Action Plan
If Out of Specs
Maintenance Log
Data Collection Device
(Strip Chart, Mag. Tape)
Data Reduction
Reports
113
-------
MANUAL-HI VOL
Type
No. of Analyzers
No. of Sites
Frequency
Type of Filter
Pre-exposure Checks and
Procedures
Collection Procedures
Calibrating Procedures
Weighing Procedures
Frequency
Data Handling
114
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PART E. MEDIUM - PESTICIDES
The following questions may be asked in toto if the personnel do not seem to know much about gas
chromatography. If personnel seem versed in GLC, it may be necessary only to pick out some
questions in each subsection.
I. GLC Calibration & Maintenance
A. Detector (EC)
1. Frequency of preparation of linearity curves for pesticides of interest - weekly D monthly D
never D
2. Frequency of determination of standing current profile - weekly D monthly D never D
other D (describe)
3. Frequency of construction of voltage/response curve - weekly D monthly D never D
other D (describe)
4. Comments on method of selection of optimum polarizing voltage.
B. Detector (FPD)
1. Date unit purchased .
2. Manufacturer of power supply unit
3. Voltage applied to photomultiplier tube volt. Awareness of operator
4. Has a determination been made of the signal to noise ratio as a criterion for optimal selection?
Yes D No D Comments:
5. Have heat shields and filters been checked on a spectrophotometer for light transmission at
specified wavelengths? Yes D No D If yes.at what wavelengths?
P (526 mu) Actual %T
S (394 mu) Actual %T
6. Have velocity of gases been adjusted to give optimum signal to noise ratio? Yes D No D
If yes, provide gas flows in ml/min. H2 , C>2 , Air
7. Date detector last cleaned? O-rings changed?
8. Sensitivity in terms of % F.S.D. for 2.5 ng of ethylparathion.
9. Baseline noise % F.S.D.
10. Is flame extinguished overnight? Yes D No D
11. Does instrument have vent valve? Yes D No D If no, how is flame-out avoided?
C. Alkaline Flame Detector
1. Which salt is used?
2. Is flame extinguished overnight? Yes D No D
3. Give frequency of cleaning of loop collector to detector
4. If electrical current to collector loop is supplied by batteries, give frequency of battery changing
or recharging
5. Give operating baseline current amps.
6. Baseline noise % F.S.D.
7. Give sensitivity in terms of % F.S.D. from 2.5 ng ethylparathion.
115
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D. Flame lonization Detector
1. Give frequency of cleaning of collector loop
2. If electrical current to collector loop is supplied by batteries, give frequency of battery changing
or recharging
3. Give operating baseline current amps.
E. Coulson Electrolytic Conductivity Detector
1. Date of purchase
2. Mode of operation
3. Sensitivity in terms of % F.S.D. resulting from 1 ng of aldrin
4. Normal baseline noise % F.S.D.
5. Pyrolysis furnace temperature °C.
6. Block temperature °C.
7. Flow rates in m1/min. of purge and carrier gas
8. Flow rates in m1/min. of Q2 or H2
9. Pretreatment of water used in cell
10. Flow velocity of water through pressure control tube ml/min.
11. Flow velocity of water through syphon arm of cell ml/min.
12. Identity of GLC column(s) used
F. Electrometers
1. Frequency of zeroing daily D weekly D monthly D never D other D (describe)
2. Frequency of determination of attenuator linearity daily D weekly D monthly D
never D other D (describe)
3. Frequency of repair
G. Strip Chart Recorders
1. Frequency of zeroing baseline daily D weekly D monthly D never D other D
(describe)
2. Describe method of determining optimum gain control setting
3. Frequency of cleaning of slide wire
H. GLC Columns
1. Is column efficiency determined before routine use? Yes D No D If yes, describe method
2. Are response characteristics determined before use? Yes D No D If yes, describe method
3. Frequency of changing demister tube, if used
4. Frequency of changing glass wool plug at column inlet
5. Is any determination made of compound degradation characteristics of column-endrin, p.p'-DDT?
6. If column used for FPD. are response characteristics determined prior to use? Yes D No D If
answer is yes, describe method.
7. In using the column for tentative identification of peaks, are RRT^ or EP data utilized?
Yes D No D If answer is no, describe the alternative used.
116
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I. GLC Operation - General
1. Is any method used to monitor accuracy of instrument pyrometer? Yes D No D If answer
is yes, describe.
2. Is carrier flow velocity monitored by bubble meter? Yes D No D If answer is no, request
operator to set what he thinks is 70 ml/min. and make actual check with bubble meter.
3. Assessment of flow system plumbing - molecular sieve filter, neatness of layout, knowledge of
operator pertinent to checking for leaks, etc.
4. Is a log maintained for each instrument showing chronological data such as change of detector,
etc.
5. General assessment of GLC operation capability for pesticide work:
6. Is any check made in the early A.M. with a working standard solution to relate response char-
acteristics to those of the pervious day's operation? Yes D No D Comment
117
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PARTF. RADIATION
Counting Room Facilities and Equipment
A. Counting Room Facilities
1. Are counting instruments located and operated in a separate
counting room facility?
Yes D No D
2. Number and size of counting rooms : Number Size
3. Are instruments operated from regulated power?
Yes D No D
4. Is there an adequate ground available to all counting
instruments?
Yes D No D
5. Can the light in the counting room that houses the liquid
scintillation systems be readily controlled (for sample loading,
etc. )?
Yes D No D
6. Are counting room facilities adequately protected (by location
or shielding) from higher radiation areas and sources? ;'/
Yes D NolD
7. Is there adequate temperature control in the counting room(s)?
Yes D No D
118
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B. - Special Questions
1. What beta emitter is used for gross beta calibration?
2. What alpha emitter is used for gross alpha calibration?
3. Are individual analyses logged in permanent type laboratory
notebooks and initialed and dated by the analyst?
' ' "' Yes D NoD
Comments :
4. Are working copies of all methods used readily available to
the laboratory analyst?
Yes D ' NoD
Comments :
5. Are standard solutions prepared and stored in an area separate
from areas where analysis of samples and blanks is being performed?
YesD NoD
Comments:
6. How often are standards preparation areas and sample working
areas being swiped and checked for radioactivity contamination?
Comments:
119
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Equipment
Refer to Chart D, Section on Special Radiological Equipment,
in the Preliminary Questionnaire.
For Alpha and Beta-particle Counters
Sample Changing
Manual
Automatic
Capacity
Instrument Background Alpha Beta
Operating voltage
cpm
Background Counts
Frequency
Log kept
For all Instruments
Frequency of calibration
Frequency of service maintenance
Alpha and Beta Particle Counters
Windowless Gas-flow Proportional Counter
Counting gas
Sample dish diameter
Thin Window Gas-flow Proportional Counter
Counting gas
f\
Window density (g/cm )
Alpha Scintillation Counter
Alpha Phosphor location
Photo tube
Samples
Beta Scintillation Counter
Beta Phosphor
Type
Thickness
Diameter
120
-------
Liquid Scintillation Counter
Discrimination channels -|
2
3
Data readout
Visual
Printout, Channel 1
2
3
Spectrometer Systems
Alpha Spectrometer (Surface Barrier Type)
Detector
Active diameter
Detectors/chamber
Analyzer
Channels
Gamma Spectrometer
Detector- size
Analyzer-Channels
Radon Gas Counter
Gas counting cells/system
Manufacturer of gas counting cells
121
-------
METHODS USED IN THE CALCULATION OF RADIATION DATA
NJ
Analysis
"Hand" or
Computer
Matrix or
Least Squares
"Spectrum
Stripping"
"Compton
Subtraction"
Precision/Accuracy
Reported
Opportunity for
Final Recheck
-------
CALIBRATED RADIOACTIVE SOURCES
Radionuctide
Supplier
Where Stored
Comments
123
-------
SAMPLING GUIDELINES
Radionuclide
Media
Site
Site Selection Criteria
Sampling Procedures
Grab
-
Continuous
Other
Custody
-------
SECTION 6
INSTRUCTIONS AND RATING SYSTEM
GENERAL INSTRUCTIONS
This section of the procedure provides instructions for the evaluators
who will conduct the onsite survey. The laboratory visit is the most
important part of the evaluation procedure. Thorough preparation is the
key to its success. Unless ample time is devoted to prior preparation,
an accurate laboratory evaluation will be impossible. "Ample" cannot
be rigidly defined, for the time involved will vary according to: the
talents and experience of individual evaluators; the information pro-
vided in the preliminary questionnaire; the number and variety of anal-
yses that a laboratory performs; and the number of inspectors performing
the site evaluation. A minimum of several hours preparation should be
allotted for even the most straightforward situation.
Initially, the evaluators must completely familiarize themselves with
the format and questions of the onsite checklist. This familiarity will
facilitate the flow of the interviews. It will help the evaluators to
anticipate laboratory reactions and to know when further probing of a
response is necessary. When an evaluator is required to exercise judg-
ment in rating a laboratory, close adherence to the procedural guidelines
will enhance the objectivity of the judgement.
Upon receipt of the preliminary questionnaire, the evaluator must care-
fully study all the information provided. Although responsibility for
different aspects of the laboratory evaluation may be divided among
several members of an evaluation team, each evaluator should be familiar
with the information contained in the entire report. A broad understand-
ing of the background information provides a valuable resource for the
evaluator who must assess a particular function such as quality control
or analytical procedures.
For convenience, the onsite survey has been divided into three areas:
(1) Management and Organization, (2) Tecnnical Services, and
(3) Internal/External Controls. Detailed instructions, suggested
questions and scoring procedures are provided for each of these areas.
125
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Prior to the onsite visit, some scores may be calculated from the data
recorded in the answers to the preliminary questionnaire. Careful study
of the detailed instructions will indicate those items which can be pre-
graded. In addition to the preliminary assignment of scores much can be
done in preparation for the visit. For example, in the technical serv-
ices section-, the apparatus list can be compared with the requirements
for each analysis allegedly performed to determine that the necessary
equipment is on hand. If a laboratory states that it performs atomic
absorption to determine cadmium but lists no cadmium hollow cathode, the
analysis could not be done. Awareness of such discrepancies before the
visit can highlight areas in need of the evaluator's scrutiny.
All questions suggested in the Evaluator's Guide will not require nu-
merical scores. Some demand only the evaluator's positive or negative
judgement in support of the overall laboratory score. However, there
are a sufficient number to be rated on the score sheets to allow an
objective laboratory evaluation which can be used for comparative
purposes.
Numerical scores should not be computed onsite. The evaluator should
gather information and check appropriate entries for possible scoring
levels. At the end of the laboratory visit, the data should be re-
viewed, all confusion dispelled, and discrepancies resolved. The score
can then be tabulated and the laboratory informed in writing of the out-
come of the evaluation process. Items which require correction or im-
provement prior to final scoring should also be highlighted to afford
the laboratory the opportunity to make the adjustments necessary for
subsequent acceptance.
Some items are more crucial to laboratory operation and security than
others. The onsite check list specifies certain conditions which must
be present and satisfactory for a laboratory to be deemed qualified.
These items are marked with an asterisk. For example, regardless of
the excellence of facilities and analytical competency of an establish-
ment, if it lacks adequate sample custody and control, it cannot be
found acceptable. If an item in any part of the check list is marked
with an asterisk, the problem must be resolved before the final score
is calculated.
Suggested Sequence of Onsite Interviews
Interview //I - Lab Director and Supervisors, (perhaps continued with
supervisors collectively or individually). Parts of
Onsite Questionnaire to be covered:
Part 1. General Information about the Laboratory
Part 2. Personnel (in part)
Part 3. Laboratory Space and Facilities (in part)
Interview //2 (or Series of Interviews) - Supervisors with their
laboratory personnel in the laboratories. (If number
of supervised personnel is large, subdivide the group
for convenience.)
126
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Part to be covered:
Part 2. Personnel (in part)
Part 3. Laboratory Space and Facilities (in part)
Part 4. Technical Service
Part 5. Equipment List
Part 6. Quality Control (in part)
Interview //3 Internal and External Controls - This may involve a designated
quality control officer, a section with responsibility for
review of operations, or an individual or individuals with part-
time responsibility for quality control in the lab.
SPECIFIC INSTRUCTIONS AND RATING SYSTEM
Management and Organization Area - Parts 1, 2 and 3
This area does not readily lend itself to an objective evaluation.
The questions frequently cannot be designed to elicit a "yes" or "no"
response. Therefore, the judgements made by the evaluator are of great
importance.
Guides are provided to help standardize the scores of the individual
evaluators. The scoring system is designed so that the values assigned
to any individual characteristic of the lab will affect the total score
by only a small increment. Thus, although many laboratories with many
different evaluators may be involved, scores should be comparable.
The experience gleaned from the onsite visit, from.witnessing the at-
titude and manner of responses by laboratory personnel to questions, from
watching the interplay between individuals when more than one is present
during the onsite evaluation is essential to the assignment of scores to
answers. The evaluator is responsible for the integration of all these
factors to arrive at the decision to score each question with 5, 3, or 1.
The rationale for particular questions and the approach to their
formulation may not always be apparent. Therefore, a statement of intent
for each series of questions is provided in the "Evaluator1s Guide",
Section 5. This will help the evaluator to ask suggested questions and
to develop a personal line of questioning.
If the laboratory is privately owned some determination of its
financial stability should be made. Some information can be gained from
the annual operating budget, fees charged for services and the number of
analyses performed per year. Also the age and condition of the real
estate and laboratory apparatus could indicate, in general terms, the
health of the organization. Laboratory apparatus is expensive and a
large investment is required to start an analytical laboratory. Much can
be learned without demanding an audit or inspection of the books. A study
of the annual report requested in the preliminary questionnaire should
provide a good deal of information about the financial condition of the
organization. If no fiscal information is contained in the annual report,
some inquiries concerning the financial condition of the laboratory should
be made.
127
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Name of Lab.
PART 1. GENERAL INFORMATION ABOUT THE LABORATORY
(1) Appropriateness of Organization
Best Description of Laboratory Score
D Responses to questions indicate the organization
is as reported, and that its functioning is not so
rigid as to interfere with operational requirements. 5
D Some doubt that organization as described is
really followed. Chain-of-command is followed
without deviation to the detriment of good
performance. 3
D Serious doubts concerning organization and
control of people. 1 *
(2) Impairment of Functions
Best Description of Laboratory Score
D Responses generally satisfactory, no real
problems in any of these areas. Certainly
nothing said that would indicate impairment
of laboratory functions. 5
D Some problems evident in one or two places.
These may. make it difficult to operate
effectively. 3
D Management problems are obvious in several areas,
hard to get help, customers complain, etc., and
performance is likely to suffer. 1 *
(3) Strength of Management
Best Description of Laboratory Score
D Firm stand taken concerning internal
communications and cooperation between groups.
Both annual and long-range plans are made and
followed. Firm authority demonstrated without
the feeling of an "absolute monarch." Impression
given of "wide awake" management. 5
D Some weaknesses indicated in a few of the items. 3
D It appears that management is weak - no plans
made for future - little cooperation or internal
communications. 1*
128
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(4) Objectivity of the Laboratory
Best Description of Laboratory Score
D Responses open and direct - no reason
to doubt objectivity. 5
n Some aspects of relationships unclear.
Objectivity not seriously questioned but some
doubts. 3
D A conflict of interest exists, is clearly
apparent in any part of the organization. 1*
(5) Cooperation Obtained
Best Description of Laboratory Score
D All information provided promptly.
Cooperative attitude displayed by all
personnel. Preliminary questionnaire
distributed to proper persons for completion. 5
D Most information supplied readily.
Satisfactory candid responses. 3
D Important information not provided and difficult
to draw out answers. Cooperation of all not
evident. Evaluation presented and no plans to
make constructive use of the results. 1 *
Note: A score of 1, when marked with an asterisk (1 *) in any
part of the check list must be resolved to the satisfaction of the
evaluator before a final score is calculated.
129
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Evaluator's Notes
130
-------
PART 2. PERSONNEL
(1) Supervisor Training
Best Description of Laboratory Score
D Supervisors have degrees. Sufficient
experience in place of degree. 5
D No degree and less than 5 years experience. 3
D No degree and insufficient experience. 1
(2) Supervisor Experience
Best Description of Laboratory Score
D The supervisors as individuals and
as a group are highly trained and experienced. 5
D The supervisors meet general requirements but
are weak in environmental monitoring work. 3
D Some of the group appear deficient in training
and experience. 1 *
(3) Job Descriptions
Best Description of Laboratory Score
D There is good agreement between
description and what is done. 5
D There is some agreement between
description and what is done but
considerable deviation. 3
D General agreement only. 1
(4) Training Program
Best Description of Laboratory Score
D Formal training program exists and is
followed. 5
D No formal training program but obviously some
training is continued. 3
D Little evidence that training is done. 1
(5) Turnover Rate
Best Description of Laboratory Score
D Rate is less than 25%. 5
D Rate is 25-50%. 3
D Rate is greater than 50%. 1 *
131
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(6) General Morale
Best Description of Laboratory Score
D Management exhibits real concern for individuals,
evidenced by central records kept for each
individual showing advancement dates,
promotions, training programs taken,
participation in health programs. General morale
of personnel is high. 5
D No formal central records are maintained
but some effort made to encourage people.
No evidence of serious morale problems. 3
D Little concern demonstrated for individuals.
Morale problems are evident. 1
132
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Evaluator's Notes
133
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PART 3. LABORATORY SPACE AND FACILITIES
(1) General Characteristics
Best Description of Laboratory Score
D General characteristics of laboratory
satisfactory. 5
D Impression of laboratory is only average. 3
D General features of the laboratory are poor. 1
(2) Office Space
Best Description of Laboratory Score
D 16.7m2 (180 sq. ft.) or greater/person. 5
D 12.5-16.7m2 (135-180 sq.ft.)/person. 3
D Less than 12.5m2 (135 sq. ft.)/person. 1
(3) Laboratory Space
Best Description of Laboratory Score
D 18.6m2 (200 sq. ft.) or greater/person. 5
D 13.9-18.6m2 (150-200 sq. ft.)/person. 3
D Less than 13.9m2(150 sq. ft.)/person. 1 *
(4) Bench-top Space
Best Description of Laboratory Score
D 1.2m (4 lin. ft.) or greater/person. 5
D 0.9-1.2m (3-4 lih. ft.)/person. 3
D Less than 0.9m (3 lin. ft.)/person. 1
(5) Hood Space and Operation
Best Description of Laboratory Score
D Hoods sufficient in number and capability. 5
D Some additional hoods and/or capacity needed. 3
D Hoods inadequate for purpose intended. 1
134
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(6) Storage Space Chemicals, Reagents, Glassware, Supplies t
Best Description of Laboratory Score
D Storage space adequate, accessible, and
kept orderly. 5
D Storage space available but overtaxed. 3
D Storage space insufficient. 1
t NOTE
Further questions about inventory policy and
materials identification are asked in Part 6.
(7) Sample Storage t
Best Description of Laboratory Score
D Sample storage space is adequate and
necessary provisions are made for samples
requiring special attention. ' 5
D Sample storage satisfactory in general but
some special requirements are not fully met. 3
D Sample storage space is inadequate and
inefficiently arranged. 1*
Further questions about control of samples
appear in Part 6.
(8) Controlled Space
Best Description of Laboratory Score
D Controlled space necessary for performance
of services offered by the laboratory is available.
Responsibility for operation of these rooms
is assigned and continuous check of conditions
is maintained. 5
D Necessary rooms are available but control is
slack and checks are made only daily. 3
D There are unsatisfied needs for controlled
space and/or responsibility is not well
defined and checking is less frequent than
daily. 1*
135
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(9) Library
Best Description of Library Score
D A library is available; it is easily
accessible, orderly, and well looked after. 5
D There is a library but it is disorganized
and difficult to use. 3
D No organized library exists and each section
or staff member keeps own references,
periodicals, etc. 1
(10) Safety Equipment and Procedures
Best Description of Laboratory Score
D Safety equipment is available, regulations
are posted, and regular drills are held. 5
D Safety equipment is good but improvements
in the lab safety program are needed. 3
D Safety equipment is not complete and an
effective program does not exist. 1 *
(11) Distilled Water/Deionized Water
Best Description of Laboratory Score
D Apparatus and water checked every day
and kept in proper condition by one
designated individual who keeps a record. 5
D Greater interval than one day between checks
by designated individual. 3
D No one person responsible and no written
procedure or records maintained. 1 *
(12) Glassware Supply and Washing
Best Description of Laboratory Score
D Glassware supply and washing are
satisfactory in all respects. 5
D More attention needs to be given to
washing equipment or procedures. 3
D Careless job done of glassware washing. 1 *
136
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(13) Housekeeping
Best Description of Laboratory Score
D Laboratory has clean, neat appearance;
movement and work are not impeded by
clutter. 5
D Laboratory is clean but not as neat
as should be expected. 3
D Poor housekeeping evident by dirt or clutter. 1
(14) Data Processing Equipment and Logistic Services
Best Description of Laboratory Score
CD Communication facilities within and
outside the laboratory good. Computing
capability present. 5
D Communications within and outside laboratory
are limited. Data processing facilities
inconvenient to use. 3
D Laboratory and sections thereof are
isolated and computing capability
sufficient for timely results not
available. 1
137
-------
Evaluator's Notes
138
-------
Technical Service Area - Parts 4 and 5
The technical services area encompasses analytical methods and
instrumentation. The questions are straight-forward. They seek to
determine the nature of analytical methods employed in the laboratory
and the adequacy of the instruments used in these procedures.
All analytical methods must be Federal Register referenced or
alternates which have been specifically approved by the Environmental
Protection Agency. EPA approved water and radiation test methods are
referenced in the Federal Register, Vol. 35, No. 199, October 16, 1973.
Air test methods with EGA approval are referenced in the Federal Register
Vol. 36, No. 228, November 25, 1971 and Vol. 38, No. 110, June 8, 1973.
Air methods for stationary sources are referenced in Federal Register,
Vol. 36, No. 247, Part II, December 23, 1971; Vol. 38, No. Ill, June 11,
1973; Vol. 39, No. 47, March 8, 1974; Vol. 40, No. 152, August 6, 1975;
and Vol. 40, No. 194, October 6, 1975. The interim methods for algicides,
chlorinated organic compounds and pesticides were issued by EPA's
Environmental Monitoring and Support Laboratory. For non-referenced
Biological Tests see Bibliography entries No. 6, 7, 8, and 9. See
Ref. 4, Standard Methods, for Test No. 406, Standard Plate Count.
Prior to the onsite visit, the evaluator should compare the apparatus
list in the preliminary questionnaire with the requirements for each
analysis that the laboratory performs. The absence of essential equipment
should be thoroughly investigated. If all necessary apparatus is avail-
able, the evaluator should carefully assess the condition of the instru-
ments. To function properly, the analytical equipment should be inspected
and serviced regularly.
In laboratories concerned with more than one medium, it may be
desirable to score the different sections of the laboratory individually
for Part 4 Analytical Methods and Part 5 Instruments. The separation of
Charts C and D in the Preliminary Questionnaire, Section 4, by media will
facilitate this.
The evaluator must complete a set of score sheets for Parts 4 and 5
for each section of the laboratory, if separate scores are desired.
Depending on the circumstance, the evaluators report might contain
one over-all score for the laboratory or two or more scores, one for each
media with which the laboratory is concerned.
A list of major equipment requirements for each analytical method
is given in the Appendix. Prior to the onsite visit this list should be
checked against the Analytical Methods circled in Chart C and the
Instruments checked in Chart D of the Preliminary Questionnaire, Section 4,
to verify that equipment is on hand to perform all the tests for which
evaluation is being made. Ask questions about any observed discrepancies.
Check the condition of the equipment and ascertain its capabilities in
every instance for:
139
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Required Instruments
Function Tests and Standardization of Instruments - It is
Important that calibration curves be available for all major
instruments and that they have been checked recently and
updated if necessary.
Calibration Equipment - The availability of suitable calibration
equipment is important. Standard weights and special thermometers
should be traceable back to a standardizing agency such as' the
National Bureau of Standards. In air monitoring, especially,
the calibration equipment available should be checked carefully.
Is equipment available for basic calibration of flow measure-
ment devices? Is the laboratory able to produce satisfactory
standard atmospheres? Note mention of required calibration
equipment in the Appendix, Major Equipment Requirements for
Each Analytical Method.
140
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PART 4. ANALYTICAL METHODS
(1) Reference Methods or Approved Alternates
Best Description of Laboratory Score
D All methods used are Federal Register
referenced methods or specific EPA
approval has been obtained. 5
D Some easily correctable minor deviations
from referenced methods exist and steps
are being taken to conform to standards. 3
L-I Some nonstandard methods which do not
have specific EPA approval are in use. 1 *
(2) Reagent and Media Preparation
Best Description of Laboratory Score
CD Laboratory personnel are clearly
aware of the importance of proper
preparation, use, and storage of
reagents and media, and laboratory
procedures and practices arc
adequate to ensure same. 5
D Although personnel awareness and
laboratory procedures regarding
preparation, use, and storage of
reagents and media are generally
satisfactory, one or two examples
of improper preparation, careless
use, improper storage (time,
temperature, container, etc.),
inadequate records, or other
unacceptable procedures or atti-
tudes were noted. 3
D Personnel attitudes and/or labor-
atory procedures for ensuring proper
preparation, use, and storage of
reagents and media are not adequate. 1
(3) Performance According to Standard
Best Description of Laboratory Score
D Performance of analysts is closely
supervised and all testing conforms
to standards. 5
D The laboratory does not have a specific
control program for each sampling
procedure and analytical test and perform-
ance is uneven. 3
D Supervision of the analysts is lax and
confusion exists about specific details of
some control procedures. 1
141
-------
Evaluator's Notes
142
-------
PART 5. ANALYTICAL INSTRUMENTS
(1) Required Instrumentation
Best Description of Laboratory Score
D All required instrumentation is in
good working condition. 5
D Some instrumentation is of doubtful
quality or is in some degree of
disrepair. 3
D Needed items of equipment are missing,
are not adequate for satisfactory
work, or are improperly maintained. 1 *
(2) Function Tests and Standardization of
Instruments
Best Description of Laboratory Score
D Instruments are maintained operative,
accurate, and precise by regular
functioning checks and by use of
standard before unknown samples.
Standard curves are available where-
ever indicated. 5
D Instruments are periodically checked
against zero point or other reference
and examined for evidence of physical
wear or inadequate maintenance. 3
D Instruments are checked only when they
stop working or when excessive
difficulties are experienced. 1
(3) Calibration Equipment
Best Description of Laboratory Score
D Necessary calibration equipment is
available and in good working condition. 5
D Calibration equipment is of doubtful
quality or is in some degree of
disrepair. 3
D Needed items for calibration are
missing, are not adequate for precise
work, or are improperly maintained. 1
143
-------
Evaluator's Notes
144
-------
Internal and External Controls - Part 6
Quality control is an indispensable aspect of laboratory performance.
Initiated by management's interest and concern and embodied in distinct
operating procedures, commitment to quality performance should pervade
all levels of the laboratory.
Concern for quality has many manifestations:
Responsibility for quality control is clearly assigned.
Analytical apparatus is adequately maintained and calibrations
are performed frequently.
Samples are carefully collected and identified, and promptly
processed.
Tests for precision and accuracy are employed to ascertain the
validity of data.
Laboratory uses quality control check (reference) samples on a
scheduled basis.
Laboratory records are assiduously kept and reports are completed
regularly.
The laboratory participates periodically in inter-laboratory
proficiency tests.
A training program exists for new employees; trainees' per-
formance is monitored and evaluated.
Corrective action procedures are available and can be quickly
implemented when necessary
With the guidance of Internal and External Controls Part 6, the
evaluator should explore the laboratory's provisions for quality control.
In addition to the operational components of a quality control plan, the
evaluator must assess a number of intangibles. An atmosphere conducive
to quality performance requires interest and enthusiasm, a cooperative
working relationship between supervisor, analyst and technician, dedica-
tion, and a free flow of communication. Through insight .and discussion,
the evaluator must determine whether or not a sincere concern for quality
control exists. The following guidance should assist the evaluator to
make this judgment.
145
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Control of Analytical Methods and Instruments
An effective environmental monitoring program must include a
quality assurance plan to protect the validity of its data. Quality
assurance has many components: calibration standards, standard reference
material, careful maintenance of records, sample taking, sample processing
and control, interlaboratory comparison studies and data validation.
Maintenance and calibration of analytical apparatus are critical to the
generation of good data. The evaluator must determine whether instruments
and apparatus are maintained and how well, whether calibrations are performed
in an appropriate manner and with sufficient frequency, and whether
records and documentation of maintenance and calibration are adequate. If
maintenance is done on an outside contract, determine for what instruments
such contracts exist. The following items should be considered to assess
the laboratory's quality assurance measurements.
Assignment of Responsibility - The evaluator1s first task will
be to determine who has the responsibility to see that each
of the instruments in Chart D in the preliminary forms is
properly maintained and calibrated on schedule. This may or
may not be the same person who"actually does the maintenance
and calibration. Here the intent is to evaluate whether the
responsibility is clearly assigned or not. It may be useful
to question several people, bench analysts and supervisors
alike, on this point to see if the assignment of responsibilities
is clearly and uniformly understood by all.
Maintenance and Calibration Logs - For legal and scientific
reasons, it is important to keep careful records of maintenance
and calibration of instruments and apparatus. Generally, these
records should be kept in permanent (bound) notebooks in ink
with each entry signed and dated. A separate log (or a separate
section of a log) should be assigned to each instrument or
piece of apparatus that requires any sort of periodic calibration
or maintenance, whether that activity is performed by laboratory
personnel or by an outside agency under contract. It is con-
venient to include all calibration, maintenance, and repair
actions on an instrument in the .log, as a complete and accessible
record of the conditions of that instrument. This includes
evidence of traceability of standards to the National Bureau of
Standards or other recognized source.
Each entry must specify clearly what action was taken when
and by whom. For example, if a new calibration curve was
established which will be the basis for future analyses, either
the curve or a reference to a notebook containing the curve should
be included, along with an explanation of how the curve was
established (identification of reference standards, methodology)
and when the analyst began using the curve in "real sample"
analysis.
146
-------
Adequacy of Calibration and Maintenance Practices - The
evaluator now must assess the laboratory's actual procedures
and practices for calibrating and maintaining its instruments
and apparatus. The critical factors for purposes of this
evaluation are the procedure itself. What maintenance checks
are routinely performed? How is calibration done and the
frequency and regularity with which it is carried out? This.
information should appear in the instrument calibration and
maintenance logs and the laboratory quality control manual. If
not, it will have to be obtained directly in conversations with
the analysts and their supervisors. In either case, it will
be important to discuss laboratory calibration and maintenance
practices in the onsite visit and how to ascertain insofar as
possible what is actually done and how frequently for each
instrument. The evaluator should look for calibration tags
on major pieces of instrumentation.
Ideally, the evaluation would involve simply comparing
this laboratory's practices to generally accepted standards,
summarized in some Table or reference test. Unfortunately,
there is no such Table or text that covers all instruments
and apparatus employed in environmental monitoring.
However, calibration recommendations for some of the
major instruments are included in Table I. These "recommendations"
are not to be considered rigid rules but rather guidelines for
the evaluator in estimating laboratory performance. It is
recognized that optimum procedures may vary somewhat as a
function of instrument manufacturer and model. Additional
materials that could be useful to the evaluator are operation
and maintenance manuals for the various instruments and
references in the Bibliography.
147
-------
TABLE 1. INSTRUMENT CALIBRATIONS*
Instrument
1) Analytical Balances
2) pH Meters
3) Conductivity Meters
4) Nephelometer/
Turbidimeters
5) Colorimeters/Filter
Photometers
6) UV/Visible
Spectrophotometers
*Continued
Procedure
(a) Zero
(b) Standard weights
(c) Full calibration and
adjustment
At pH 4,7, and 10
(a) Obtain cell constant
with potassium chloride
reference solutions
(b) Construct temperature
curve if measurements
are to be made other
than at 25 + 0.5°C
(a) Check instrument scales
or develop calibration
curve with formazin
stds. (<40NTU)
(b) If manufacturer's stds.
are not formazine, check
against formazine stds.
(£ 40NTU)
Curves determined with 5-6
laboratory-prepared std.
solutions for each param-
eter in cone, range of
samples
(a) Wavelength calibration
with holimum oxide glass
or solution, low-pressure
mercury arc, benzene vapor
(UV), or hydrogen arc
(visible)
(b) Absorbance vs. concentra-
tion curves with 5-6 std.
Solutions for each param-
eter at analytical wave-
length in cone, range of
samples
(c) Full servicing and adjust-
ment
Frequency
Before each use
Monthly
Annually
Daily
Daily
Monthly
Monthly
Annually
Daily
Quarterly
Daily
Annually
148
-------
TABLE 1. (Continued)*
Instrument
7) Infrared Spectro-
photometers
8) Atomic Absorption
Spectrophotometers
9) Carbon Analyzers
10) DO Meters
11) Other Selective
Ion Electrodes and
Electrometers
12) Thermometers
13) Technicon Auto
Analyzers
Procedure
(a) Wavelength calibration with
polystyrene or indene
(b) Absorbance vs. concentration
curves with 5-6 std. solu-
tions for each parameter
at analytical wavelength in
cone, range of samples
(c) Full servicing and adjust-
ment
(a) Response vs. concentration
curves with 6-8 std. solu-
tions for each metal (std.
mixtures are acceptable,
but with same acid as
samples to be run) in cone.
range of samples
(b) Full servicing and adjust-
ment
Curves determined with 5-6 std.
solutions in cone, range of
samples
Calibrated against modified
Winkler method on aerated
distilled or tap water
Curves determined with 5-6 std.
solutions in cone, range of
samples
Calibrate in constant temper-
ature baths at two temper-
atures against precision
thermometers certified by
NBS.
(a) Curves determined with
std. solutions for each
parameter.
(b) Full service and adjust-
ment (esp. colorimeter)
Frequency
Daily
Daily
Semi-annually
Daily
Annually
Daily
Daily
Daily
Quarterly
Each set of
samples
Annually
*Continued
149
-------
Instrument
14) Gas Chromatographs
TABLE 1. (Continued)*
Procedure Frequency
(a) Retention times and detector Daily
response checked with std.
solutions
(b) Response curves for each Monthly
parameter determined with
std. solutions'
(See Standard Methods, Sect. 300)
(a) Calibrate flowmeters and
hypodermic needle against
a wet test meter
(b) Spectrophotometric calibra-
tion curve with 5-6 std.
sulfite-TCM solutions at
controlled temperature
(± 1°C)
(c) Sampling calibration curve Monthly
with 5-6 std. atomospheres
from permeation tubes or
cylinders
(d) Calibrate associated thennom- Quarterly
eters, barometers, and
spectrophotometer (wave-
length)
17) Suspended Particulates (a) Calibrate sampler (curve of Monthly
15) Radiological
Equipment
16) Sulfur Dioxide in
Air Sampler/Analyzers
(Pararosaniline
Method)
Quarterly (Nee-
dles before and
after each run)
Monthly
(High-volume Sampler
Method)
true airflow rate vs. rota-
meter or recorder reading)
with orifice calibration
unit and differential manom-
eter at 6 air flow rates.
(b) Calibrate orifice calibra-
tion unit with positive
displacement primary
standard and differential
manometers
(c) Calibrate relative humidity
indicator in the condition-
ing environment against wet-
bulb/dry-bulb psychrometer
(d) Check elapsed time indicator
(e) Calibrate associated analy-
tical balances, thermom-
eters, barometers
Annually
Semi-annually
Semi-annually
As needed
*Continued
150
-------
TABLE 1. (Continued)*
Instrument
18) Carbon monoxide
(Non-dispersive IR)
19) Photochemical
Oxidants (Ozone)
20) Hydrocarbons
(corrected for
Methane)
Procedure
(a) Determine linearity of
detector response (cali-
bration curve) with cali-
bration gases (0, 10, 20,
40, and 80% of full scale,
certified to +2% and
checked against auditing
gases certified to
+1%)
(b) .Perform zero and span cali-
brations
(c) Calibrate rotameter and
. sample cell pressure gauge
(a) Calibrate standard KI/I2
solutipns in terms of
calculated 03 equivalents
at 352 nm
(b) Calibrate instrument response
with 6-8 test atmospheres
from ozone generator, span-
ning expected ranges of
sample concentrations
(usually 0.05-0.5 ppm 03)
(c) Calibrate flowmeters, barom-
eter, thermometer
(d) Calibrate and service spec-
trophotometer
(e) Calibrate ozone generator
Frequency
Monthly
Daily or every
three days
Semi-annually
At same time as
ozone generator
Monthly
Semi-annually
As specified
Monthly
(a) Determine linearity of detec- Monthly
tor response (calibration
curve) with calibration gases
(0, 10, 20, 40, and 80% of full
scale, certified to +2% and
checked against auditing
gages certified to +1%)
(b) Perform zero and span cali-
brations
(c) Calibrate flowmeters and
other associated
apparatus
Before and after
each sampling
period
Semi-annually
^Continued
151
-------
TABLE 1. (Continued)
Instrument Procedure Frequency
21) Nitrogen Dioxide (a) Calibrate flowmeter with wet Monthly
(Arsenite 24 hr. test meter
Sampling Method) (b) Calibrate Hypodermic needle Each new needle and
(flow restrictor) with before and after
flowmeter each run
(c) Obtain colorimetric calibra- Weekly
tion curves with 5-6 std.
nitrite solutions
22) Nitrogen Dioxide (a) Determine linearity of Monthly
(Chemiluminescence, detector response (cali-
Continuous) bration curve) with cali-
bration gases (-0, 10, 20,
40, and 80% of full scale,
certified to +2% and
checked against auditing
gases certified to +1%)
(b) Perform zero and span cali- Daily or every
brations three days
(c) Calibrate rotameter and Semi-annually
sample cell pressure gauge
23) Autoclaves and (a) Sterilization effectiveness Daily
Sterilizers checked (e.g., B. stearo-
thermophilus, color-indi-
cator tape for ethylene
oxide)
(b) Temperature-recording Semi-annually
device calibrated
152
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Control of Sampling
Sampling Plans and Sampling Equipment - The intent of this
item is to determine whether adequate attention has been
given to planning for sampling, whether appropriate sampling
instruments are available, and whether they are used properly.
Sampling is the operation of removing a part which is
of convenient size for testing from a much larger whole
substance in such a way that the measure of the characteristic
of interest (such as pH or chemical analysis) in the sample
is identical, within measureable limits of error, to that
characteristic's presence in the whole substance. It is
necessary that sampling be planned carefully in order to
measure and control sampling errors and minimize the
cost of sampling and testing.
If the substance to be sampled consists of discrete,
constant, identifiable units (as do agricultural commodities
tested for pesticide residues) standard sampling tables may
be used to determine sample size. However, in environmental
sampling the media are of a bulk nature (air, water, etc.)
and the sampling units must be created by means of a sampling
device, such as a bottle or sampling tube. The quantity and
often the form of the sample units depends on the particular
device, how it was used, and on the location and condition of
the substance being sampled.
Sampling may be instantaneous at a given station (grab
sampling) or continuous and automatic. Validity of sampling
depends on randomness of selection of the samples. Where
stratification exists, random samples must be taken from
each stratum in proportion to its size. When the statistical
criteria have been met, the required sample size may be
calculated.
The design of sampling is seen to require some special
skills and the person responsible for it must have consider-
able sophistication in handling the statistical aspects.
Generally, sampling instruments and their use are
described in the analytical methods and questions related to
sampling should be asked for each test or group of test
methods.
Sample Collection and Preservation -' The evaluator will want
to determine sample taking and preservation practices for at
least some of the tests performed by the laboratory. For
evaluation purposes, these practices can be compared with
the recommendations incorporated in Table 2 of the EPA Manual -
Methods for the Chemical Analysis of Water and Wastest
153
-------
for most water parameters; the Federal Register for air
parameters (Sect. 4, Precision, Accuracy and Stability,
for each method); Standard Methods: Sections 405
(microbiological), 200 and 300A (radiological); and
the specified references in the Analytical Methods
Table C, Section 4, for the remaining parameters (57-60).
The holding time given in Table 2 of the EPA Manual
is interpreted as the recommended maximum period between
sampling and analysis. Preservatives, where specified, are
required to ensure stability for the holding time. Look
at records, at sample bottles, etc., to assure yourself
that good procedures are actually followed. If holding
times are exceeded, a notation of that fact should be made
on data sheets before they are transmitted.
For some tests, to exceed the maximum holding time would
very seriously compromise the accuracy of the measurement.
If the laboratory is exceeding the maximum holding time
for these tests, the laboratory must be given a score of
1* and the problem must be resolved before a final score
is calculated. The parameters to which this applies
include the following:
Biochemical Oxygen Demand (Dissolved Oxygen)
Cyanide, Total
Chlorine, Total Residual
Phenols
Turbidity
Streptococci
Coliform Bacteria
Temperature
PH
Identification and Storage of Samples - All samples should be
clearly marked with a code number at the time of sampling.
Labels should be securely attached to the sample container.
In the field, information about the sample should be entered
immediately in a field notebook. In handling and storing
the samples precautions should be taken against mix-up
in identification.
154
-------
Storage space should permit storage of samples in a
separate area, refrigerated if necessary for preservation,
and secured against tampering.
Laboratory Handling of Sampling - The flow of samples through
the laboratory should be organized. Forms should be available
for requests for analysis and for reporting of results. Sample
handling procedures should be formalized so that samples
arriving at the lab are accepted, prepared and analyzed
promptly. Holding times given in Table 2 should be adhered
to. For air, requirements given in the referenced methods
should be followed.
Chain of Custody - Assignment of responsibility for custody
of samples should be clear and the importance of a tight system
of control should be understood by all. The procedures to be
followed should be written. Samples should be logged in and
their progress through the labs should be recorded and the
samples themselves should be in a secure location when not
signed out to an analyst.
Control of Field Sampling/Measurements - The requirements of
sampling in the field are as demanding as those of sampling
in the laboratory. Most sample taking is a field operation.
Sometimes measurement also must be done in the field. Certain
special analytical methods or modifications of standard methods
apply. Also, other measurements, such as flow rates, not made
in the laboratory must be done in the field.
Questions should be directed toward an understanding of
how well the field aspects of sampling and testing are attended
to when done by laboratory personnel or when done by a
service agency.
Control of Monitoring - The important thing to be checked for
in this item is whether written procedures cover all monitoring
activities in which the laboratory is engaged and whether they
are being followed exactly.
155
-------
TABLE 2. RECOMMENDATION FOR SAMPLING AND PRESERVATION
OF SAMPLES ACCORDING TO MEASUREMENT (1)*
Measurement
Acidity
Alkalinity
Arsenic
BOD
Bromide
COD
Chloride
Chlorine Req.
Color
Cyanides
Dissolved Oxygen
Probe
Winkler
Fluoride
Hardness
Iodide
MBAS
Metals
Dissolved
Suspended
Total
*Continued
Vol.
Req.
(ml)
100
100
100
1000
100
50
50
50
50
500
300
300
300
100
100
250
200
100
Container
P,
P,
P,
P,
P,
P,
P,
P,
P,
P,
G
G
P,
P,
P,
P,
P,
G<2>
G
G
G
G
G
G
G
G
G
only
only
G
G
G
G
G
Preservative
Cool, 4°C
Cool, 4°C
HN03 to pH < 2
Cool, 4°C
Cool, 4°C
H2S04 to pH < 2
None Req.
Cool, 4°C
Cool, 4°C
Cool, 4°C
NaOH to pH 12
Det. on site
Fix on site
Cool, 4°C
Cool, 4°C
Cool, 4°C
Cool, 4°C
Filter on site
HN03 to pH < 2
Filter on site
HN03 to pH < 2
Holding
Time(6)
24 Hrs.
24 Hrs.
6 Mos.
6Hrs.<3>
24 Hrs.
7 Days
7 Days
24 Hrs.
24 Hrs.
24 Hrs.
No Holding
No Holding
7 Days
7 Days
24 Hrs.
24 Hrs.
6 Mos.
6 Mos.
6 Mos.
156
-------
TABLE 2. (Continued)*.
Measurement
Mercury
Dissolved
Total
Nitrogen
Ammonia
Kjeldahl
Nitrate
Nitrite
NTA
Oil & Grease
Vol.
Req.
(ml) Container Preservative
100 P, G . Filter
HNO to pH < 2
. ,
100 P, G HN03 to pH< 2
f
400 P, G Cool, 4°C
H2S04 to pH < 2
500 P, G Cool, 4°C
H2S04 to pH < 2
100 P, G Cool, 4°C
H2S04 to pH < 2
50 P, G Cool, 4°C
50 P, G Cpol, 4°C
1000 G only Cool, 4°C
H2S04 to pH < 2
' Holding
Time(6)
38 Days
(Glass)
13 Days
(Hard
Plastic)
38 Days
(Glass)
13 Days
(Hard
Plastic)
24 Hrs.(A)
24Hrs.(4)
24 Hrs.(4)
24Hrs.(4)
24 Hrs.
24 Hrs.
Organic Carbon1
25
P, G
cool,
4°C
to pH < 2
24 Hrs.
*Continued
157
-------
TABLE 2. (Continued)*
,. Vol.
Req.
Measurement (ml) Container
pH 25 P, G
Phenol ics 500 G only
Phosphorus
Ortho-
phosphate 50 P, G
Dissolved
Hydrolyzable 50 P, G
Total 50 P, G
Total,
Dissolved 50 P, G
Residue
Filterable 100 P, G
Non-
Filterable 100 P, G
Total 100 P, G
Volatile 100 P, G
Settleable Matter 1000 P, G
Selenium 50 P, G
Silica 50 P only
Preservative
Cool, 4°C
Det. on site
Cool, 4°C
H-Po, to pH < 4
1.0 g CuS04/l
Filter on site
Cool, 4°C
Cool, 4°C
H2S04 to pH < 2
Cool, 4°C
Filter on site
Cool, 4°C
Cool, 4°C
Cool, 4°C
Cool, 4°C
Cool, 4°C
None Req.
HNO_ to pH < 2
Cool, 4°C
Holding
Time (6)
6Hrs.(3)
24 Hrs.
24 Hrs.(4)
24 Hrs.(4)
24 Hrs.(4)
24 Hrs.(4)
7 Days
7 Days
7 Days
7 Days
24 Hrs.
6 Mos.
7 Days
Specific
Conductance
*Continued
100
P, G
Cool, 4 C
24 Hrs.
(5)
158
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TABLE 2. (Continued)
Measurement
Sulfate
Sulfide
Sulfite
Temperature
Threshold
Odor
Turbidity
Vol.
Req.
(ml) Container Preservative
50 P, G Cool, 4°C
50 P, G 2 ml zinc
acetate
50 P, G Cool, 4°C
1000 P, G Det. on site
200 G only Cool, 4°C
100 P, G Cool, 4°C
Holding
Time (6)
7 Days
24 Hrs.
24 Hrs.
No Holding
24 Hrs.
7 Days
1. More specific instructions for preservation and sampling are found with
each procedure as detailed in this manual. A general discussion on
sampling water and industrial wastewater may be found in ASTM, Part 23,
p. 72-91 (1973).
2. Plastic or Glass
3. If samples cannot be returned to the laboratory in less than 6 hours
and holding time exceeds this limit, the final reported data should
indicate the actual holding time.
4. Mercuric chloride may be used as an alternate preservative at a con-
centration of 40 mg/1, especially if a longer holding time is required.
However, the use of mercuric chloride is discouraged whenever possible.
5. If the sample is stabilized by cooling, it should be warmed to 25°C for
reading, or temperature correction made and results reported at 25°C.
6. It has been shown that samples properly preserved may be held for
extended periods beyond the recommended holding time.
159
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Quality Control
Quality Policy - To ascertain that quality control is a pervasive
concern; one that merits attention not only at critical points,
but daily in the routine performance of analyses. There should
be a clear statement of policy by management.
Quality Program Manual - To identify the means by which quality
control procedures are disseminated in the laboratory.
Responsibility for Quality - To determine which person or
group of people assumes responsibility for quality control.
Training in Quality Control - To determine what measures are used
to prepare employees to meet quality control standards.
Control of Chemicals and Reagents - To assess the laboratory's
methods for monitoring the flow of chemicals and reagents.
Procurement control includes equipment and other materials
as well as chemicals and reagents.
Intra-Laboratory Checks; Precision and Accuracy - An analytical
laboratory must have a well-organized and clearly defined program
to check the validity of the data it produces. Validity is
usually expressed in terms of precision and accuracy. According
to the EPA Handbook for Analytical Quality Control in Water and
Wastewater Laboratories, "precision refers to the reproducibility
among replicate observations", and "accuracy refers to a degree
of difference between observed and known, or actual values".
An analyst initially may establish the precision of a
particular method by 5-10 replicate determinations on a single
"real sample". Generally, it will be necessary to repeat this
procedure on each of the various types of samples that will be
analyzed by this method (e.g., surface water, industrial
effluent, sea water, etc) and preferably on several samples
of each type from a variety of sources. Comparison of the pre-
cision obtained with reference standards and that obtained with
actual samples will reveal any interferences from contaminants
in the complex samples.
The accuracy of a method may be determined initially by
5-10 replicate analyses of samples to which known amounts of
reference standards have been added (spiked samples). The EPA
AQC Handbook mentioned above suggests reporting the results as
"percent recovery at the final concentration of the spiked
sample". The spiking of actual samples for these determinations
allows for a more realistic measurement of accuracy than the
exclusive use of pure reference standards, although again
comparison of the accuracy obtained with spiked samples and
that obtained with reference standards may be of interest in
160
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identifying the source of errors. Analysis of blanks also
will be important for many parameters where the apparent
background level may be non-zero and where a blank
correction may be necessary.
Routine Checks of Testing Performance - After the precision
and accuracy of the method are established, the analyst will
need to incorporate replicates, spikes, standards, and blanks,
as appropriate, into the sequence of routine analyses to
ensure that valid data is being generated. The frequency and
procedures required for adequate monitoring of the quality
of the data will depend on the method itself. The evaluator
will find some guidance as to what is adequate in the
references in the Bibliography, particularly in the EPA
AQC Handbook mentioned above, the 'EPA Guide lines for the
Development'of a Quality Assurance Program (for various air
parameters), and the Methods Manuals (EPA, ASTM, Standard
Methods). The experience of conscientious analysts and
statisticians in the field of environmental monitoring is
an invaluable source in this matter. For example, one
group of water chemists experienced oh the Technicon Auto
Analyzer usually runs a duplicate, a spiked sample, and a
reference standard every 8 samples in a large series of
similar samples, or once in each set of samples, whichever
is more frequent. A chemist experienced in the analysis of
Phenols and Cyanide suggests verifying the standard curves
each day that these parameters are analyzed with a low and a
high reference standard and a blank and running a duplicate
and a spike with each small set of samples. Gas chromatography
often requires multiple injections of the sample with and
without an internal standard, in addition to spiked samples
and a blank, for each sample analyzed. These examples are
given only to demonstrate how quality control protocols will
vary considerably with the method and the experience of the
analyst. The nature of the samples (simple or complex
mixtures), the condition of the instrument, the importance
of the sample (e.g., for enforcement action), the breadth
of the precision and accuracy control limits, and many
other factors may also affect the quality control requirements.
Because there are no universal guidelines for the
frequency and procedures required in the use of quality
control samples, it is very important that each laboratory
develop its own internal guidelines based on sound statistical
methods and experience. These should be in the form of
written, explicit protocols for each test or group of tests.
Statistical methods for the development of such protocols are
discussed in the quality control references in the Bibliography
and in standard quality control texts.
161
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For purposes of this evaluation it will be of primary
importance to determine if the analyst and the laboratory
have a proper appreciation of the importance of replicates,
spikes, standards, and blanks in assuring the validity
of their analytical data. Since the evaluator is not
expected to be an expert with long experience in the
performance of every method, this evaluation does not
place heavy emphasis on the content of the detailed protocols
for replicates, spikes, standards, and blanks used by the
laboratory. Rather, emphasis is laid on an assessment of
the concern for and awareness of quality control evidenced
and practiced by the analyst and the laboratory as a whole,
as discussed below. The evaluator is asked to make a
judgment as to whether quality control samples are run
with sufficient frequency, but it is recognized that the
evaluator may have little experience in many methods and may
wish to place proportionately little weight on this judgment.
The evaluator, nonetheless, should carefully record and
document laboratory practices, so that patterns of quality
control procedures can be developed.
The evaluator will want to discuss in the onsite visit
the actual laboratory protocol for the use of replicates,
spiked samples, reference standards, and blanks for each
test. Some tests, of course, can be considered in groups
with similar requirements (e.g., metals determined by
atomic absorption or many of the tests determined on the
Technicon Auto Analyzer). Questions to be asked by the
evaluator for each parameter (method) include the following:
'is there a formal protocol in this lab for the control
of analytical performance of this method, including
specifications of the frequency of and procedures for
replicate sample, spiked sample, reference standard, and
blank analyses, where applicable?
Are the analysts familiar with the protocol? Does the
protocol appear to vary from analyst to analyst?
Have the precision and accuracy of the method been
determined in this laboratory? By each analyst using
the method? How frequently?
Are replicates, spiked samples, reference standards, and
blanks, if applicable, run with sufficient frequency
to assure that precision and accuracy are remaining
within the control limits?
Is there a well-defined and clearly understood procedure
for evaluating the data and for handling "out-of-control"
data?
162
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Have you developed acceptance criteria for data
(could be three-sigma limits)? Is corrective action taken
on lack of control? One of the basic procedures of
statistical quality control is to associate troubles
with specific causes. Does the laboratory try to do this?
The answers to these and other questions the evaluator
may develop should offer a clear impression of the effort
devoted by laboratory and analyst to assuring that valid
data is produced for each parameter.
The score given is to be based on the laboratory's
quality control procedures, particularly as they relate to
replicates, spiked samples, reference standards, and blanks,
if applicable, and the analyst's familiarity and understanding
of the procedures.
Statistical Methods - A popular method of monitoring daily
performance is the use of Quality Control Charts. Basically,
these charts, constructed separately for each test, display
control limits for precision and accuracy. The precision and
accuracy measured from day to day are plotted on these charts
which provide a continuous visual picture of the control
of data quality. Details will be found in textbooks on
Quality Control and in the two EPA publications, Handbook for
Analytical Quality Control in Water and Wastewater Analysis
and Quality Control Practices in Processing Air Pollution
Samples. The control chart method is particularly helpful
is assisting in identifying causes of trouble in the
measurement process: both special causes within the power
of the analyst to correct and general causes, such as
fluctuations in the laboratory environment, which are the
duty of management to correct.
Inter-Laboratory Proficiency Tests - Refer to Chart E of
the Preliminary Questionnaire. Question the lab about results
of participation in formal programs. Ask questions about
cooperation with peer laboratories in the exchange of split
samples, as another sort of inter-laboratory control.
Laboratory Records - Accurate records provide a means for
the laboratory to monitor its workload, locate errors, and
evaluate its own progress. All three functions contribute to
quality control and, therefore, should be assessed from this
perspective. How does management decide whether data are
satisfactory? Can data be rejected in this laboratory?
(i.e., Are new samples collected and analyzed if results
are suspect?) Are results recorded in an acceptable manner
(in a notebook, on bench cards, or on NCR data forms)?
163
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Laboratory Reports - Regularly scheduled laboratory reports
may function as a catalyst to continuous awareness of the
importance of quality control. They are evidence both of
managements' demand and analysts' effort to achieve excellence
in quality control.
164
-------
Evaluator's Notes
165
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PART 6. INTERNAL AND EXTERNAL CONTROLS
1. Control of Analytical Methods and Instruments
(1) Assignment of Responsibility for Maintenance
and Calibration
Best Description of Laboratory Score
D Responsibility is clearly assigned in
this laboratory and understood by all
personnel. 5
D Responsibility is assigned but not
clearly recognized or understood by
assignee(s) or other personnel. 3
D Responsibility is not clearly assigned
or recognized in this laboratory. 1
(2) Maintenance and Calibration Logs
Best Description of Laboratory Score
D The instrument logs are properly
executed, complete, and up-to-date. 5
G An instrument log exists but is faulty. 3
D An instrument log does not exist. 1
(3) Adequacy of Calibration and Maintenance Practices
Best Description of Laboratory Score
D Calibration and maintenance of
instruments is adequate. 5
D Marginal. 3
G Inadequate. 1
166
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2. Control of Sampling
(4) Sampling Plans and Sampling Equipment
Best Description of Laboratory Score
D Samples are carefully designed, suitable
sampling equipment is on hand and is
used properly. 5
D Sampling is taken for granted and no
particular efforts are made to assure
validity of samples. 3
D Sampling is not organized, equipment is
poor, or insufficient care is taken in
obtaining the samples. 1
(5) Sample Collection and Preservation
Best Description of Laboratory Score
D Samples are kept in proper containers using
the recommended preservative for no longer
than the recommended maximum holding time. 5
D When possible, the recommended procedures
for collection and preservation are followed,
although circumstances (laboratory manpower,
lack of control over sample taking,
variability of workload, etc.) do not always
allow strict adherence. 3
D The laboratory often does not follow EPA
recommendations for maximum holding time,
preservation technique, and/or container
type. 1
167
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(6) ldent''ication and Storage of Samples
Best Description of Laboratory Score
D Samples are carefully and clearly identified
by code number and stored so as to protect
their identity and security. 5
D Sample identification system and storage
of samples not well organized. 3
D There are serious defects in sample
identification and storage practices
that could lead to serious mix-ups. 1 *
(7) Laboratory Handling of Samples
Best Description of Laboratory Score
D Activities of the laboratory are well
organized so that samples are given the
attention required and work proceeds
smoothly from sample receipt to report
of results. 5
D Procedures for assuring smooth flow of
samples through the laboratory are not
complete. 3
D The system and load are not well matched
so that there is a backlog of work and
time requirements are sometimes missed. 1
(8) Chain of Custody
Best Description of Laboratory Score
D A chain of custody procedure is followed
precisely, with clearly assigned
responsibility, complete recording of
activities, and careful security of
samples. 5
D A chain of custody procedure exists but
it is lax and not strictly followed. 3
D Chain of custody is not formally
organized. 1 *
168
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(9) Control of Field Sampling/Measurements '
Best Description of Laboratory Score
D Written procedures for field sampling/
measurements are complete and are
followed meticulously under surveillance
by the laboratory. 5
D Field sampling/measurement are subject
to standard methods but surveillance
by the laboratory is lax. 3
D Field sampling/measurement is not
treated as a major concern of the
laboratory. 1
t NOTE
If the laboratory does not participate in this
activity, do not score it and subtract 5 from
the denominator of the fraction in the formula
for calculating its score for internal and external
controls.
(10) Control of Monitoring t
Best Description of Laboratory Score
D Written procedures which are followed
exactly are available for all monitoring
activities in which this laboratory is
engaged. 5
D Written procedures exist but they are
incomplete and not followed exactly. 3
D No written procedures exist. 1
t NOTE
If the laboratory does not participate in this
activity, do not score it and subtract 5 from
the denominator of the fraction in the formula
for calculating its score for internal and external
controls.
169
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3. Quality Control
(11) Quality Policy
Best Description of Laboratory Score
D A clear statement of quality objectives
by the top executive exists with continuing
visible evidence of its sincerity to all
levels of the organization. 5
D Periodic meetings among the section heads
of service, research and development, and
quality assurance are held to discuss
quality objectives and progress toward their
achievement. 3
D There was a "one-shot" statement of the
desire for product quality by the top
executive after which the quality control
staff is on its own. 1
(12) Quality Program Manual
Best Description of Laboratory Score
D Formalized and documented by a set of
procedures which clearly describe the
activities necessary and sufficient to
achieve desired quality objectives.
This may be in the form of a Quality
Control Manual. S
D The Quality Program is contained in
methods procedures or is implicit in
those procedures. Experience with the
materials, product and equipment is needed
for continuity of control. 3
D The Quality Program is undefined in any
procedures and is left to the current
managers or supervisors to determine as
the situation dictates. 1*
170
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(13) Responsibility for Quality
Best Description of Laboratory Score
D Responsibility for quality is a full-time
assignment of a quality control department
with well-defined authority or in smaller
laboratories is clearly defined for all
sections and section chiefs. 5
D Responsibility for quality is assigned
to a part-time quality control coordinator
who must use whatever means possible to
achieve quality goals. 3
D Responsibility for quality is not defined. 1*
(14) Training for Quality Control
Best Description of Laboratory Score
D The people who have an impact on quality
(bench chemists, supervisors, etc.) are
trained in the reasons for and the benefits
of standards of quality and the methods by
which high quality can be achieved. 5
D Personnel are told about quality only when
their work falls below acceptable levels. 3
D Personnel are reprimanded when quality
deficiencies are directly traceable to
the chemists' analytical work. 1
(15) Control of Chemicals and Reagents
Best Description of Laboratory Score
D Reagents and chemicals are inspected upon
receipt and accepted only if they conform
to all specifications. In inventory they
are identified as to type and age and
issued on a first in/first out plan. 5
D Reagents and chemicals are only spot
checked for quantity and shipping damage;
in storage they are identified as to material
only and are issued randomly. 3
D Reagents and chemicals are not checked
on receipt, are not clearly identified,
and are issued on a last in/first out
basis. 1
171
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(16) Intralaboratory Checks - Precision and Accuracy
Best Description of Laboratory Score
D Laboratory has a well-organized program to
check the validity of data it produces. 5
G Incomplete information is available on
precision and accuracy of the tests in use. 3
D Laboratory has no plan to check on validity
of its data. ' 1
(17) Routine Checks of Testing Performance
Best Description of Laboratory Score
D Procedures are excellent and should provide
adequate assurance that the data is valid. 5
D Procedures are fair and should provide some
indication of the validity of the data. 3
D Procedures are poor or poorly defined and do not
provide adequate assurance that the data is valid. 1 *
(18) Statistical Methods
Best Description of Laboratory Score
D Use is made of statistical methods,
such as control charts to insure
continuing validity of tests. 5
D Some statistical checks of measure-
ments are made but level of assurance
of quality is uncertain 3
D No efforts are made to use statistical
methods of quality control. 1
172
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(19) Intel-laboratory Proficiency Tests
Best Description of Laboratory Score
D The laboratory has a good record of
participation in formal proficiency
tseting and has a good record of performance. 5
D Laboratory participates only sporadically
and not recently. Performance in programs
not outstanding. 3
D Laboratory does not participate in
proficiency testing programs. 1 *
(20) Laboratory Records
Best Description of Laboratory Score
D Analytical results are entered in a lab notebook
or in a card system which is signed and witnessed.
Results are summarized and entered in appropriate
data system promptly. 5
D Analytical results are complete but
they are not routinely signed and
witnessed. Data processing is not
always prompt. 3
D Data keeping is not organized, i.e.,
results kept on loose sheets of paper
and incompletely reviewed and analyzed. 1
(21) Laboratory Reports
Best Description of Laboratory Score
D Lab activities are reported regularly and
periodic quality reports are made to feed
forward to management and to feed back to
bench analysts quality of the work reported. 5
D Laboratory reports are sporadic and quality
reports do not result in bringing necessary
information for action on quality to all
levels of the organization. 3
D Reports are very irregular and no system
for quality reporting exists. 1
173
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FOLLOW-UP ON DEFICIENCIES
The goal of laboratory evaluation is the improvement of laboratory per-
formance. Identification of deficiencies is not intended to bar a labora-
tory from participation in environmental monitoring. Rather, it indicates
that improvements are necessary to enable the laboratory to fulfill its
role optimally.
Certain aspects of laboratory activity are more crucial to successful
environmental monitoring than are others. It is the evaluator's respon-
sibility to insist that rigid standards are met in these critical areas
before the laboratory receives a final score. In the Onsite Check List,
problems which must be resolved to the evaluator's satisfaction prior to
approval are marked by an asterisk next to the lowest possible score (1*).
Unacceptable deficiencies may be indicated in each area of laboratory
evaluation: Consistently high turnover rates, customer complaints, lack
of cooperation among laboratory employees, and obstacles to internal com-
munication are symptoms of poor organization and management which could
seriously impair laboratory operation. Supervisors who have neither
degrees nor sufficient experience may jeopardize the laboratory's analy-
tical capabilities. Inadequate space, whether it be laboratory space,
storage space or controlled space, impedes orderly laboratory function-
ing. Incomplete safety equipment may endanger both successful analyses
and laboratory personnel. The use of nonstandard methods, the absence
of essential instruments, or the malfunction of instruments as a result
of improper maintenance, may compromise all analytical results. Failure
to employ rigid quality control procedures may also ra,ise serious doubts
concerning the validity of laboratory data. If the quality assurance
plan is not clearly defined, and responsibility for its execution is not
assigned; if a chain of custody of samples is not established and fol-
lowed; if sample storage exceeds the recommended maximum holding time;
or if calibration is inadequate; the reliability of the laboratory's
work may be impugned.
To protect the scientific and legal defensibility of the data, the
evaluator must ensure that environmental monitoring laboratories are free of
these deficiencies. Any inadequacies discovered by the evaluator should
be brought to the attention of the laboratory management immediately,
before completion of the onsite visit. The evaluator may offer recom-
mendations for remedial action or stipulate essential adjustments which
must be made before the laboratory may be scored.
After discussion with laboratory management, the evaluator should make
note of the exchange and then compute a tentative score for the labora-
tory. The final score cannot be computed, nor approval given, until the
laboratory has submitted evidence that all deficiencies have been corrected.
174
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SECTION 7
CALCULATION OF SCORE
ACCEPTABILITY OF A LABORATORY
The Procedure for the Evaluation of Environmental Monitoring Laborator-
ies strives to construct a standardized system for the objective appraisal
of laboratory management, personnel, equipment, analytical capabilities
and quality control procedures. The numerical scoring system plays an
integral role in achieving this end. It provides a means to organize
the multiplicity of data and to produce a manageable result. The values
assigned to individual characteristics of the laboratory affect the total
score by very small increments. This affords a measure of -uniformity to
laboratory assessment which is essential for the comparison of results
compiled by a variety of evaluators in diverse situations.
The numberical scoring system is based upon 100 points. Each item may
be rated with 5 points, 3 points, or 1 point. While onsite, the evaluator
should check on the score sheets the scoring level for each item. If the
level checked is scored one followed by an asterisk (1*) the laboratory
fails to meet required specifications. The laboratory must resolve the
deficiency before a final score can be computed.
After the onsite survey has been completedj the evaluator should use
the summary sheets to calculate the numerical scores. On these forms, each
item's score is weighted according to its importance for successful lab-
oratory operation. After summing the weighted scores, performing the
calculation at the bottom of the page produces the final score for each
section.
Addition of the scores for each section provides the laboratory's final
evaluation score. The highest possible score is 100 points. The mini-
mum acceptable score is 60 points. Laboratories which score below this
minimum require major improvements to be capable of participation in
environmental monitoring programs.
175
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If separate scores are desired for each section of a laboratory
which deals with different media, the evaluator must have completed during
the onsite visit a set of score sheets for Part 4 Analytical Methods and
Part 5 Instruments for each section. In the event that this has been
done, a total score is obtained for each section of the laboratory by
adding to the separate scores on Parts 4 and 5, the general scores given
the Laboratory on Management and Organization (Parts 1, 2, 3) plus
Part 6, Internal and External Controls. Thus, a laboratory may obtain
an overall score or two or more scores covering individual media with
which it is concerned.
When the evaluator has computed the score for a laboratory, this
score coupled with the evaluator's recommendations and comments should
be sent to the participating lab. Laboratories which fail to meet
required standards may later submit proof of adjustments made in
compliance with the evaluator1s recommendations to receive an upward
revision.
In special circumstances, such as in evaluating very small
laboratories, it may be desirable to drop one or more questions from
the onsite score sheets. This should be done only after due deliberation
by the evaluating agency. In no instance should the evaluation team
arbitrarily eliminate or "forget" any question. If, for valid reasons,
a question is dropped from a Part, the prorating of the score on the
Scoring Forms may be accomplished as follows:
Multiply by five (5) the assigned weight in Column (2) of the
question dropped and subtract the product from the denominator in the
calculation of score for that part. Make such an adjustment for each
question dropped. For example, if Question 4, Bench-Top Space, is
dropped from Part 3, Laboratory Space and Facilities, the weight
(Col. 2) is 1, the denominator 100 is reduced by 5x1 to 95 and
calculation of score proceeds as indicated.
A report to the laboratory management might contain the following
sections:
1. Recommendations to improve overall performance
2. Amplification of recommendations for any equipment or
instrument purchases.
176
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PART 1. SCORE FOR GENERAL INFORMATION
ABOUT THE LABORATORY
Name of Laboratory
Question 1 .
Question 2.
Question 3.
Question 4.
Question 5.
Appropriateness of Organization*
Impairment of Functions*
Strength of Management* -
Objectivity of Laboratory*
Cooperation Obtained*
(D X (2)
Score Weight
2
2 .
4
1
1
(3)
Extension
TOTAL
Calculation:
Total Col (3)
50
X
Enter this figure in box below and carry it forward to Summary Evaluation.
Score carried forward to Summary Evaluation. DD
Any score of 1 in positions in Col (1) marked with an asterisk must be resolved before the final score is calculated.
Date
Visit Conducted by
177
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PART 2. SCORE FOR PERSONNEL
Name of Laboratory
'
Question 1 .
Question 2.
Question 3.
Question 4.
Question 5.
Question 6.
Supervisor Training
Supervisor Experience*
Job Descriptions
Training Program
Turnover Rate*
General Morale
(1) X (2)
Score Weight
1
2
1
2
2
2
(3)
Extension
TOTAL
Calculation:
Total Col (3)
50
X 20
Enter this figure in box below and carry it forward to Summary Evaluation.
Score carried forward to Summary Evaluation. DD
"Any score of 1 in positions in Col (1) marked with an asterisk must be resolved before the final score is calculated.
Date
.Visit Conducted by
178
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PART 3. SCORE FOR LABORATORY SPACE AND FACILITIES
Name of Laboratory
Question 1.
Question 2.
Question 3.
Question 4.
Question 5.
Question 6.
Question 7.
Question 8.
Question 9.
Question 10.
Question 11.
Question 12.
Question 13.
Question 14.
General Characteristics of
Space and Facilities
Office Space
Laboratory Space*
Bench-top Space
Hood Space and Operation
Storage Space - Chemicals
Sample Storage Space*
Controlled Space*
Library
Safety Equipment/Procedures*
Distilled/Deionized Water*
Glassware Supply and Washing*
Housekeeping
Data Processing Equipment
and Logistic Services
(D X (2)
Score Weight
1
1
2
1
1
1
2
2
1
2
2
2
1
(3)
Extension
TOTAL
Calculation:
Total Col (3)
K)0
X 10
Enter this figure in box below and carry it forward to Summary Evaluation.
Score carried forward to Summary Evaluation. DD
"Any score of 1 in positions in Col (1) marked with an asterisk must be resolved before the final score is calculated.
Date
Visit Conducted by
179
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PART 4. SCORE FOR ANALYTICAL METHODS
Name of Laboratory
Question 1. Reference Methods or
Approved Alternates*
Question 2. Reagent and Media
Preparation
Questions. Performance According
to Standard
(D X (2)
Score Weight
1
1
2
(3)
Extension
TOTAL
Calculation:
Total Col (3)
20
X 10
Score carried forward to Summary Evaluation. DD
'Any score of 1 in positions in Col (1) marked with an asterisk must be resolved before the final score is calculated.
Date
.VisitConducted by
180
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PART 5. SCORE FOR INSTRUMENTS
Name of Laboratory
Question 1. Required Instrumentation*
Question 2. Function Tests and
Standardization of
Instruments
Question 3. Calibration Equipment
(1) X (2)
Score Weight
1
2
1
TOTAL
Calculation:
Total Col (3)
20
X 10
Score carried forward to Summary Evaluation. DD
(3)
Extension
"Any score of 1 in positions in Col'(1) marked with an asterisk must be resolved before the final score is calculated.
Date
Visit Conducted by
181
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PART 6. SCORE FOR INTERNAL AND EXTERNAL CONTROLS
Name of Laboratory : ..-'--
(1) X (2) = (3)
Score Weight Extension
Question 1. Responsibility for ....-"
Calibration 1 ;.
Question 2. Adequacy of Calibration ...
Logs 1
Questions. Adequacy of Calibration and Maintenance .,.,."-
Practices* 2
Question 4. Sampling Plans and Sampling
Equipment 1
Questions. Sample Collection and Preservation:. - , 2 ,, :
Question 6. Identification and Storage
of Samples* 1 -;<
Question 7. Laboratory Handling of
Samples 1
Questions. Chain of Custody* 2
Question 9. Field Control of Sampling 1
Question 10. Control of Monitoring
Activities 1
Question 11. Clarity of QC Policy 1
Question 12. Written Program/Manual* 1
Question 13. Responsibility for Quality* 1
Question 14. Training in QC 1
Question 15. Control of Chemicals and Reagents 1
Question 16. Internal Checks: Precision and
Accuracy 1
Question 17. Internal Checks: Routine
Duplicates, Blanks, Spikes* 2
Question 18. Statistical Methods 1
Question 19. Inter-lab Proficiency Tests* 1
Question 20. Record System 1
Question 21. Report System 1
TOTAL
Calculation:
Total Col (3)
125X 3°
Enter this figure in the box below and carry it forward to Summary Evaluation.
Score carried forward to Summary Evaluation. DD
"Any score of 1 in positions in Col (1) marked with an asterisk must be resolved before the final score is calculated.
Date Visit Conducted by
182
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SUMMARY OF LABORATORY EVALUATION
Name of Laboratory.
Score
Parti. General Information
Part 2. Personnel
Part 3. Lab Space and Facilities
Part 4. Technical Services (Analytical Methods)
Part 5. Lab Equipment
Part 6. Internal and External Controls
TOTAL
Inadequacies marked by * in the score sheets have not been resolved and above is a tentative score.
Final Score
Date ____^____________^_^^_____ Evaluation Completed by
183
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BIBLIOGRAPHY
SAMPLING AND MEASUREMENT OF ENVIRONMENTAL CONTAMINANTS
Water - Chemical
Book of ASTM Standards, 1974 Edition, Part 31, Water.
Manual of Methods for Chemical Analysis of Water and Wastewater,
EPA, 1974, 298pp.
Recommended Methods for Water Data Acquisition, Federal
Interagency Work Group, 1972.
Standard Methods for the Examination of Water and Wastewater,
13th Edition, 1971, 874pp.
Water Measurement Manual, 2nd Revised Edition, U.S. Dept. of
the Interior, Bureau of Reclamation, Denver, (1967) 1974.
Water - Biological
Algal Assay Procedure Bottle Test, August 1971, EPA
Biological Field and Laboratory Methods, EPA, Cincinnati,
#670/4-73-001.
Marine Algal Assay Procedure Bottle Test, December 1974.
ORD Publications Staff, EPA, Washington, DC.
Methods for Collection and Analysis of Aquatic Biological and
Microbiological Samples, U.S. Geological Survay, 1973.
Development of Guidelines for Sampling and Sample Preservation
of Water and Wastewater, Envirex, Inc., EPA Proj. 68-03-2075,
1975 (Two parts).
Air
Collaborative Testing Methods for Measurement of N0£ in Ambient Air,
Vol 1, Midwest Research Institute, Kansas City, MO.
184
-------
Field Operations Guide for Automatic Air Monitoring Equipment,.
EPA, RTF, 1972, 154pp.
Guidelines for Determining Performance Characteristics of Automated
Methods for Measuring Nitrogen Dioxide and Hydrocarbons Corrected
for Methane, in Ambient Air, EPA RTP, #650/4-74-018, November 1974,
41pp.
Workshop on Ozone Measurement by the Potasium Iodide Method.
EPA 650/4-75-007
Pesticides
Analytical Reference Standards and Supplemental Data for
Pesticides, EPA, RTP, 1973.
Manual of Analytical Methods - Pesticide Residues in Human and
Environmental Samples, EPA, RTP, 1972.
Pesticide Residue Analysis in Water - Training Manual, EPA, Cincinnati
//430/1-74-012, September 1974, p. 1-1:36-13.
Pesticides Test Methods, National Pollutant Discharge Elimination
System, Appendix A, Federal Register, Vol. 38, #75, Part 2, 1973.
Solid Waste
Methods of Solid Waste Testing (Physical, Chemical, and Microbiological),
EPA, Cincinnati, #6700-73-01, 1973.
Environmental Monitoring
Handbook for Monitoring Industrial Wastewater, EPA, Washington, DC
1973.
Handbook of Statistical Tests for Evaluating Employee Exposure to Air
Contaminants, NIOSH 75-147, 208pp. & overlays.
Compliance Monitoring Procedures, NFIC - Denver, EPA
330/1-74-002, July 1974, 37 pp.
Quality Control Procedures
Calibration System Specifications, NCSL, 1971.
185
-------
Evaluation of a Contractor's Quality Program, Quality and Reliability
Assurance Handbook, (H50), ASD, Washington, DC, 1965, 35pp.
Guidelines for the Development of a Quality Assurance Program,
Reference Method for Continuous Measurement of Carbon Monoxide
in Air, EPA, Washington, D.C., #R4-75-028a, 1973, 110pp.
Guidelines for Development of a Quality Assurance Program, Reference
Method for the Determination of Suspended Particulates in the
Atmosphere (High Volume Method), EPA Washington, DC,
#R4-73-028b, 1973, 115pp.
Guidelines for Development of a Quality Assurance Program,
Reference Method for Measurement of Photochemical Oxidents,
EPA, Washington, DC //R4-73-028c, 1973, 98pp.
Guidelines for Development of a Quality Assurance Program,
Reference Method for the Determination of Sulphur Dioxide in
the Atmosphere, EPA, Washington, DC #R4-73-028d, 1973, 116pp.
Guidelines for Development of a Quality Assurance Program,
Determination of Stack Gas Velocity and Volumetric Flow Rate,
(Vol. 1).
Guidelines for Development of a Quality Assurance Program, Gas
Analysis for Carbon Dioxide, Excess Air and Dry Molecular
Weight, (Vol. 2). RTP,' NC
Guidelines for Development of a Quality Assurance Program,
Determination of Moisture in Stack Gases, (Vol. 3)
Guidelines for Development of a Quality Assurance Program,
Determination of Phosphorus in Gasoline, (Vol. 12).
Guidelines for Development of a Quality Assurance Program,
Test for Lead in Gasoline by Atomic Absorption Spectrometry,
(Vol. 13).
Handbook for Analytical Quality Control in Water and Wastewater
Laboratories, June 1972, EPA, Cincinnati. v
Quality Control Manual - Air, EPA, Region II.
Quality Control Manual - Chemistry, EPA, Region II.
Quality Control Manual - Microbiology, EPA, Region II.
Quality Control Manual, Kerr, R.S., Water Research Center, Ada,
Oklahoma.
186
-------
Quality Control Manual for Industrial Hygiene Service Laboratories,
HEW (PHS, CDC, & NIOSH) //TR78, 101 pp., 1974.
Quality Control Practices in Processing Air Pollution Samples,
EPA, RTP //APTD-1132, 1973.
Quality Control System for Independent Laboratories, American
Council of Independent Laboratories, 22pp., October 1971.
Quality Control Manual - Pesticides, EPA, Region II.
Quality Control Manual - Surveillance, EPA, Region II,
Rochester Field Office.
Quality Assurance Program - California State Water Resources Control
Board, Shimmin, K.G., Sacramento, Unpublished, July 1974.
p. 13, 5 attachments.
Spectrophotometer Calibration and Performance, AST,, Std.
E225-67.
Laboratory Evaluation Accreditation
Accreditation of Industrial Hygiene Laboratories: Application
(General Information), Site Visit Questionnaire, Site Visit
Summary Report, AIHA.
Accreditation of Testing Laboratories, Hearing Transcript, OSHA,
January 9, 1974.
Evaluation of Water Laboratories, HEW, PHS, 1966, 54pp.
Evaluation Manual - Pesticides, Bruce Mann, RTP, 1975
Feasibility of an EPA Certification Program, Speaker, D.M.,
Fensterstock, J.C. and Maker, A.M., Teknekson, Inc.,
Contract #68-03-2012, EPA, Washington, D.C., February 1975.
Standard Recommended Practice for Generic Criteria for Use in
the Evaluation of Testing and/or Inspection Agencies, ASTM
E 36.
Standards for the Accreditation of Medical Laboratories, College
of American Pathologists, Chicago, 20pp.
187
-------
Inter-Laboratory Testing
Clinical Laboratory Performance Analysis Using Proficiency Test
Statistics, HEW, Washington, DC, 1973, 53pp.
Environmental Radioactivity Laboratory Intercomparison Studies
Program, 1973-74, EPA #680/4-73-0016, February 1974, 23pp.
Inter-Laboratory Precision Test (Laboratory Evaluation of Algal
Assay Bottle Test) October, 1974.
Proficiency Test Assessment of Clinical Laboratory Capability in
the United States, HEW, Washington, DC, 1973, 101pp.
Radioactivity Standards Distribution Program, 1973-74, EPA
0680/4-73-0012, February 1974, 16pp.
Radioactivity Standards Distribution Program, EPA 680/4-75-002a,
April 1974, p.10.
Environmental Radioactivity Laboratory Intercomparison Studies
Program, EPA 680/4-75-002b, May 1975, 19pp.
188
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APPENDIX
MAJOR EQUIPMENT REQUIREMENTS FOR EACH ANALYTICAL METHOD
General Analytical Methods
1. Alkalinity as CaCO., (mg CaCO^/liter)
(a) Electrometric Titration, Manual
pH meter, Type I or II as defined in ASTM D1293
(b) Electrometric Titration, Automated
An automatic titrimeter meeting the pH meter specifications
in (a).
(c) Automated, Methyl Orange
Technicon AutoAnalyzer with
(1) Sampler I
(2) Continuous filter
(3) Manifold
(4) Proportioning pump
(5) Colorimeter with 15 mm tubular flow cell and 550 nm
filters
(6) Recorder with range expander
2. Biochemical Oxygen Demand (B.O.D.) 5-day, 20°C (mg.liter)
(a) Modified Wrinkler with Full-Bottle
B.O.D. incubation bottles
(b) Probe Method
No specific probe is recommended as superior in the 1974
EPA Methods Manual, but ones evaluated and found reliable
were Weston and Stack DO Analyzer Model 30, Yellow Springs
Instrument (YSI) Model 54, and the Beckman Fieldlab
Oxygen Analyzer.
189
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3. Chemical Oxygen Demand (C.O.D.) (mg/liter)
(a) No special equipment, other than standard laboratory glassware.
4. Total Solids (Total Residue) (mg/liter)
(a) Gravimetric, dried at 103-105°C
Blender (if samples contain oil or grease)
Porcelain, vycor, or platinum evaporating dishes
. Muffle furnace, 550°C
Steam bath or 98°C oven
Drying oven, 103-105°C
Dessicators
Analytical balance-, 200 g capacity, weighing to 0.1 mg
5. Total Dissolved Solids (Total Filterable Residue) (mg/liter)
(a) Glass fiber filtration, dried at 180°C
, Glass fiber filter discs: Reeve Angel 934A, 984-H, Gelman
type A, or equivalent
Filter holder, membrane filter funnel, or Gooch crucibles
and adapter
Suction flask
Porcelain, vycor, or platinum evaporating dishes
Muffle furnace, 550°C
Steam bath
. Drying oven, 180°C
Dessicators
Analytical balance, 200 g capacity, weighing to 0.1 mg
6. Total Suspended Solids (Total Non-Filterable Residue) (mg/liter)
(a) Glass fiber filtration, dried at 103-105°C
Same as (5), except drying oven is at 103-105°C and steam
bath, muffle furnace, and evaporating dishes are not required.
190
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7. Total Volatile Solids (Volatile Residue) (tag/liter)
(a) Gravimetric, dried at 550°C
Same as (5)
8. Ammonia (as N) (ing/liter)
(a) Distillation and titration
All glass distillation apparatus (Kjeldahl)
Standard titration apparatus
(b) Distillation and nesslerization
All-glass distillation apparatus (Kjeldahl)
Nessler tubes, 50 ml, matched set, APHA standard
Spectrophotometer or filter photometer for use at 425 run
with light path >_ 1 cm.
(c) Distillation and ammonia electrode
All-glass distillation apparatus (Kjeldahl)
Electrometer (pH meter) with expanded mV scale or specific
ion meter
t Ammonia selective electrode, such as Orion Model 95-10 or
EIL Model 8002-2
i
Magnetic stirrer, thermally-insulated, and Teflon-coated
stirring bar
(d) Automated colorimetric phenate method
Technicon AutoAnalyzer (AAI or AAII) with
(1) Sampler
(2) Manifold (AAI) or Analytical Cartridge (AAII)
(3) Proportioning pump
(4) Heating bath with double delay.coil (AAI)
(5) Colorimeter with 15 mm tubular flow cell and
630-660 nm filters
(6) Recorder
(7) Digital printer for AAII (optional)
191
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9. Total Kjeldahl Nitrogen (as N) (mg/liter)
(a) Digestion, distillation, and titration
Same as 8 (a) with suction takeoff to remove SO-j fumes
during digestion
(b) Digestion, distillation, and nesslerization
Same as 8(b) with suction takeoff to remove 503 fumes
during digestion
(c) Digestion, distillation, and ammonia electrode
Same as 8(c) with suction takeoff to remove SO-j fumes
during digestion
(d) Automated phenate method
Technicon AutoAnalyzer with
(1) Sampler II with continuous mixer
(2) Two proportioning pumps
(3) Manifolds I and II
(4) Continuous digester
(5) Planetary pump
(6) Five-gal. Carboy fume trap
(7) Heating bath, 80°C
(8) Colorimeter equipped with 50 mm tubular flow cell and
630 nm filters
(9) Recorder with range expander
(10) Vacuum pump
(e) Automated selenium method
Technicon AutoAnalyzer with
(1) Sampler
(2) Two manifolds (as in EPA Manual)
(3) Two proportioning pumps
(A) Continuous digester
(5) Two 5-gal. Carboys
(6) Colorimeter with 15 or 50 mm flow cell and 630 or 650 nm
filter
(7) Recorder
(8) Vacuum pump
192
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10. Nitrate (as N) (mg/liter)
(a) Cadmium Reduction Method (Nitrate - Nitrate)
Glass fiber or membrane filters and associated apparatus
Copper/cadmium reduction column
Spectrophotometer or filter photometer for use at 540 nm
with light path ^ 1 cm.
(b) Automated Cadmium Reduction Method (Nitrate - Nitrate)
Glass fiber or membrane filters and associated apparatus
Copper/cadmium reduction column
Technicon AutoAnalyzer (AAI or AAII) with
(1) Sampler
(2) Manifold (AAI) or Analytical Cartridge (AAII)
(3) Colorimeter with 15 or 50 mm tubular flow cell and
540 nm filters
(4) Recorder
(5) Digital printer for AAII (optional)
(c) Brucine Method
Spectrophotometer or filter photometer for use at 410 nm
Water bath at 100°C (Temperature control is critical: all
sample tubes must be held at the same temperature, and
temperature must not drop significantly -when tubes are
immersed in bath.)
. Water bath at 10-15°C
Neoprene-coated wire rack for holding sample tubes in baths
Glass sample tubes (40-50 ml)
11. Total Phosphorus (as P) (mg/liter)
(a) Single Reagent (Ascorbic Acid Reduction Method)
Spectrophotometer or filter photometer for use at 650 nm
(less sensitive) or 880 nm
Acid-washed, detergent-free glassware
Hotplate or autoclave (for persulfate digestion)
193
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(b) Automated Colorimetric Ascorbic Acid Reduction Method
Acid-washed, detergent-free glassware
Hotplate or autoclave (for persulfate digestion)
Technicon AutoAnalyzer with
(1) Sampler
(2) Manifold (AAI) or Analytical Cartridge (AAII)
(3) Proportioning pump
(4) Heating bath, 50°C
(5) Colorimeter with 15 or 50 mm tubular flow cell and
650-660 or 880 nm filter
(6) Recorder
(7) Digital printer for AAII (optional)
12. Acidity (mg CaCCyiiter)
(a) Hydrogen peroxide digestion and electrometric titration
pH meter, Type I or II as defined in ASTM D1293
(b) Hydrogen peroxide digestion and phenolphthalein end-point
titration
No special equipment, other than standard laboratory
glassware
13. Total Organic Carbon (T.O.C.) (mg/liter)
(a) Combustion and infrared method (C0£) or flame ionization
method
Waring or other blender
Apparatus for total and dissolved organic carbon (No
specific model is recommended, but several have been
found reliable: Dow-Beckman Carbonaceous Analyzer Model
#915 (infrared), Dohrmann Envirotech DC-50 Carbon
Analyzer (flame ionization) , Oceanographic International
Total Carbon Analyzer).
14. Total Hardness (mg CaC03/liter)
(a) EDTA titration
No special equipment, other than standard laboratory
glassware
194
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(b) Automated colorimetric
Technicon AutoAnalyzer with
(1) Sampler I
(2) Continuous filter
(3) Manifold
(4) Proportioning pump
(5) Colorimeter equipped with 15 mm tubular flow cell
and 520 nm filters
(6) Recorder with range expander
(c) Atomic absorption (Ca + Mg)
(See atomic absorption section below)
15. Nitrate (as N) (mg/liter)
(a) Manual colorimetric diazotization
Spectrophotometer for use at 540 nm with cells >_ 1 cm.
Nessler tubes or volumetric flasks, 50 ml
(b) Automated colorimetric diazotization
Glass fiber or membrane filters and associated apparatus
Technicon AutoAnalyzer (AAI or AAII) with
(1) Sampler
(2) Manifold (AAI) or Analytical Cartridge (AAII)
(3) Colorimeter with 15 or 50 mm tubular flow cell and
540 nm filters
(4) Recorder
(5) Digital printer for AAII (optional)
Analytical Methods for Trace Metals: Atomic Absorption Methods
For each parameter listed, EPA specifies atomic absorption as at least
one of the reference methods. The required equipment in each case will
include (1) an atomic absorption Spectrophotometer, (2) the hollow cathode
(or electric discharge) lamp for each metal, and (3) the fuels and other
apparatus specified below. Design features of some common atomic absorption
spectrophotometers (as of June, 1972) are discussed in the EPA Handbook
for Analytical Quality Control in Water and Wastewater Laboratories. If
extraction procedures are to be used, special reagents are required but
no special equipment other than standard laboratory glassware. Results
are reported in mg/liter.
195
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Fuels
Parameter | Acetylene
Aluminum
Antimony
Arsenic (Gaseous
Hydride)
Barium
Beryllium
Cadmium
Calcium
Chromium VI
Chromium, total
Cobalt
Copper
Iron
Lead
Magnesium
Manganese
Mercury (Cold Vapor)
Molybdenum
Nickel
X
X
X
X
X
X
X
X
X
X
X
X
X
X
9
X
X
Air Nitrous oxide Other
X X
X
X
X
X
X or X
X or X
X or X
X
X
X
X
X
X
X
X
Argon-hydrogen flame
Nitrous oxide more
sensitive
Nitrous oxide more
sensitive; extraction
with APDC required for
separation of Cr VI
from Cr III
Nitrous oxide more
sensitive
Flameless atomic
absorption: details
below
196
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Continued
Parameter
Fuels
{ Acetylene Air Nitrous oxide
Other
Potassium
Selenium (Gaseous
Hydride)
X
Osram potassium vapor
discharge lamp also may
be used.
Argon-hydrogen lamp
Silver
Sodium
Thallium
Tin
Titanium
Vanadium
Zinc
Other Reference
X
X
X
X
X
X
X
Methods for
X
X
X
X
X
Metals
X
X
16. Aluminum (mg/liter)
(a) Eriochrome cyanine R colorimetric method
Spectrophotometer for use at 535 nm, or
Filter photometer with 525-535 nm filters (green, p_r
Nessler tubes, 50 ml
17. Arsenic (mg/liter)
(a) Gaseous Hydride - Silver Diethyldithiocarbamate Colorimetric
Method
Arsine generator and absorption tube
Spectrophotometer for use at 535 nm, or
Filter photometer with 530-SAO nm filter (green)
197
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18. Beryllium (mg/liter)
(a) Aluminon method
Spectrophotometer or filter photometer for use at 515 nm
with 5 cm cells
19. Boron (mg/liter)
(a) Curcumin method
Spectrophotometer or filter photometer for use at 540 nm
with cells ^ 1 cm.
Vycor or platinum evaporating dishes, 100-150 ml
Water bath, 55 + 2°C
Ion exchange column, 50 cm x 1.3 cm (diameter)
20. Cadmiun (mg/liter)
(a) Dithizone Colorimetric Method
Spectrophotometer or filter photometer for use at 515 nm
21. Calcium (mg/liter)
(a) EDTA Titration
No special equipment
22. Chromium VI (mg/liter)
(a) Diphenylcarbazide colorimetric
Membrane or sintered glass filter
Spectrophotometer or filter photometer for use at 540 nm
with cells ^ 1 cm.
23. Chromium, total (mg/liter)
(a) Oxidation and diphenylcarbazide colorimetric
Membrane or sintered glass filter.
Spectrophotometer or filter photometer for use at 540 nm
with cells > 1 cm.
198
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24. Copper (ing/liter)
(a) Neocuproine colorlmetric
Spectrophotometer for use at 457 nm with cells ^_ 1 cm, or
Filter photometer with narrow-band violet filter (max.
transmittance at 450-460 nm) and cells >^ 1 cm, or
Nessler tubes, 50 ml.
25. Iron (mg/liter)
(a) o-Phenanthroline colorimetric
Spectrophotometer or filter photometer for use at 510 nm
with cells _£_ 1 cm, or
Nessler tubes, 100 ml
26. Lead (mg/liter)
(a) Dithizone colorimetric
Spectrophotometer or filter photometer for use at
520 nm with cells _>_ 1 cm
pH meter
27. Magnesium (mg/liter)
(a) Gravimetric
* No special equipment
28. Mercury (mg/liter)
(a) Manual Cold Vapor Technique (Water or Sediment)
. Commercially available mercury analyzer employing this
technique, or
Atomic absorption Spectrophotometer with open sample presen-
tation area for mounting 10 cm absorption cell ,
Mercury hollow cathode lamp: Westinghouse WL-22847, argon-
filled, or equivalent
Recorder: multi-range, variable speed, compatible with UV
detection system
199
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Absorption cell, 10 cm, quartz end windows, vapor inlet
and outlet ports
Air pump, peristaltic, 1 liter/min.
Flowmeter
Aeration tubing and drying tube (or incandescent lamp
to warm cell)
Autoclave (optional, for digestion procedure)
(b) Automated Cold Vapor Technique
Technicon AutoAnalyzer with
(1) Sampler II with provision for sample mixing
(2) Manifold
(3) Proportioning Pump II or III
(4) High temperature heating bath with two distillation
coils in series
Vapor-liquid separator
Absorption cell, 10 cm, quartz end windows
Atomic absorption spectrophotometer with open sample
presentation area for mounting 10 cm cell (or commercially
available analyzer employing this technique)
Mercury hollow cathode lamp: Westinghouse WL-22847, argon-
filled, or equivalent
Recorder: multi-range, variable speed, compatible with
UV detection system
Cooling water for mixing coil and connector and heat lamp
for absorption cell
29. Nickel (mg/liter)
(a) Heptoxime colorimetric method
Spectrophotometer or filter photometer for use at 445 nm with
cells ^ 1 cm.
30. Potassium (mg/liter)
(a) Colorimetric
Spectrophotometer for use at 425 nm with cells >_ 1 cm, or
200
-------
Filter photometer with violet.filter (max. transmittance
near 425 nm) and >_ 1 cm cells, or_
Nessler tubes, 100 ml
Centrifuge and 25 ml. centrifuge tubes
(b) Flame photometric
, Flame photometer, direct-reading or internal-standard,
and associated equipment for measurement at 768 nm
31. Sodium (mg/liter) . .
(a) Flame photometric
. Flame photometer, direct-reading or .internal-standard,
and associated equipment for measurement at 589 nm
For low-solids water, air filter and blower for burner
housing, oxyhydrogen flame, and polyethylene or Teflon
cups, bottles, etc.
32. Vanadium (mg/liter)
(a) Colorimetric (Catalysis of gallic acid oxidation)
Spectrophotometer or filter photometer for use at 415 nm
with 1-5 cm cells
. Water bath, 25 + 0.5°C
33. Zinc (mg/liter)
(a) Dithizone colorimetric method
Spectrophotometer or filter photometer for use at 535 or
620 nm with 2 cm cells, or_
, Nessler tubes, matched
pH meter
Analytical Methods for Nutrients, Anions. and Organics
34. Organic Nitrogen (as N) (mg/liter)
(a) KJeldahl Nitrogen minus Ammonia Nitrogen
. See (8) and (9) above.
201
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35. Orthophosphate (as P) (mg/liter)
See (11) above
36. Sulfate (as 804) (mg/liter)
(a) Gravimetric
Analytical balance, weighing to 0.1 mg
Steam bath
Drying oven, 180°C
Muffle furnace, 800°C
Appropriate filters or crucibles
(b) Trubidimetric
Nephelometer or
Spectrophotometer or filer photometer for use at 420 nm
with 4-5 cm cells
Magnetic stirrer with timer or stopwatch
(c) Automated colorimetric barium chloroanilate
Technicon AutoAnalyzer with
(1) Sampler I
(2) Continuous filter
(3) Manifold
(4) Proportioning pump
(5) Colorimeter with 15 mm tubular flow cell and 520 nm
filters
(6) Recorder
(7) Heating bath, 45°C
Magnetic stirrer
37. Sulfide (as S) (mg/liter)
(a) Titrimetric iodine
No special equipment, other than standard laboratory
glassware.
202
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38. Sulfite (as SO-j) (mg/liter)
(a) Titrimetric iodide-iodate
, No special equipment, other than standard laboratory
glassware
39. Bromide (mg/liter)
(a) Titrimetric iodide-iodate
No special equipment, other than standard laboratory
glassware
40. Chloride (mg/liter)
(a) Silver nitrate
. No special equipment, other than standard laboratory
glassware
(b) Mercuric nitrate
No special equipment, other than standard laboratory
glassware
(c) Automated colorimetric ferricyanide
Technicon AutoAnalyzer with
(1) Sampler I
(2) Continuous filter
(3) Manifold
(4) Proportioning pump
(5) Colorimeter with 15 mm tubular flow cell and 480 run
filters
(6) Recorder
41. Cyanide, total (mg/liter)
(a) Distillation and silver nitrate titration
Cyanide distillation apparatus
Koch microburet, 5 ml.
(b) Distillation and pyridine-pyrazolone (or pyridine-barbituric
acid) colorimetric
Cyanide distillation apparatus
203
-------
Spectrophotometer or filter photometer for use at
578 or 620 nm with >_ 1 cm cells.
42. Fluoride (rag/liter)
(a) Distillation - SPADNS
Simple Bellack distillation apparatus
* Spectrophotometer for use at 570 nm with ^ 1 cm cells, or_
Filter photometer with green-yellow filter (max.
transmittance 550-580 nm) and >_ 1 cm cells
(b) Automated complexone method
Technicon AutoAnalyzer with
(1) Sampler I
(2) Manifold
(3) Proportioning pump
(4) Continuous filter
(5) Colorimeter with 15 mm tubular flow cell and
650 nm filters
(6) Recorder with range expander
(c) Fluoride electrode
^ Electrometer
Fluoride ion activity electrode
Reference electrode, single junction, sleeve-type
Magnetic mixer
43. Chlorine, total residual (mg/liter)
(a) Starch-iodide titration
No special equipment, other than standard laboratory
glassware
(b) Amperometric titration
Amperometric end-point detection apparatus, consisting of
noble metal electrode, salt bridge, and silver - silver
chloride reference electrode cell unit connected to
microammeter with appropriate electrical accessories.
Agitator
204
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44. Oil and Grease (rag/liter)
(a) Gravimetric
Separatory funnels or soxhlet apparatus
Vaccuum
(b) Infrared
Spearatory funnels
Infrared spectrophotometer, double beam, with 1, 5, and 10
cm cells
45. Phenols (mg/liter)
(a) Colorimetric (4-AAP method with distillation)
Phenols distillation apparatus
Spectrophotometer or filter photometer for use at 460 nm
(following chloroform extraction) or 510 nm and 1-10 cm
cells
pH meter
(b) Automated 4-AAP method
Technicon AutoAnalyzer (I. or II) with
(1) Sampler
(2) Manifold
(3) Proportioning pump IJ or III
(4) Heating bath with distillation coil
(5) Distillation head
(6) Colorimeter with 50 mm flow cell and 505 or 520 nm
filter
(7) Recorder
46. Surfactants (mg/liter)
(a) Methylene blue colorimetric
Spectrophotometer or filter photometer for use at 625 nm
with ^ 1 cm cells
47. Algicides (mg/liter)
(a) Gas chromatography
205
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There is no reference procedure for algicides as a class,
and, therefore, detailed equipment requirements cannot be
specified. For general discussion of gas chromatography
and its application in environmental monitoring, see the
EPA Training Manual for Pesticide Residue Analysis in
Water and the EPA Methods Manual for Analysis of Pesticide
Residues in Human and Environmental Samples.
48. Benzidine (mg/liter)
(a) Diazotization and colorimetric
Spectrophotometer, scanning, 510-370 nm
Cells, 1-5 cm pathlength, 20 ml max. volume
49. Chlorinated organic compounds (except pesticides) (mg/liter)
(a) Gas chromatography
There is no reference procedure for chlorinated organic com
compounds as a class, and, therefore, detailed equipment
requirements cannot be specified. Gas chromatography
with electron capture, microcoulometry, or electrolytic
conductivity detection may be appropriate for individual
compounds or groups of compounds. For general discussions
of gas chromatography and its application in environmental
monitoring, see the EPA Training Manual for Pesticide
Residue Analysis in Water and the EPA Methods Manual for
Analysis of Pesticide Residues in Human and Environmental
Samples.
50. Pesticides (yg/liter)
There is no single reference procedure for pesticides as
a class. However, specific reference procedures for
several sub-classes are available from EMSL, USEPA,
Cincinnati, Ohio. To be qualified in this parameter, the
laboratory should be equipped to analyze for all specified
sub-classes. The analysis of pesticides at the levels
normally found in wastewater and other environmental sources
requires special expertise and experience, in addition to
up-to-date, well-maintained, calibrated instrumentation and
apparatus. The equipment lists below are based on the
EMSL methods; for further information on the equipment and
methodology of pesticide analysis, see the EPA Training
Manual for Pesticide Residue Analyses in Water and the
EPA Methods Manual for Analysis of Pesticide Residues in
Human and Environmental Samples.
206
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(a) Organochlorine pesticides
Gas chromatograph with
(1) Glass-lined injection port
(2) One or more of the following detectors:
Electron capture, radioactive (H^ or
Microcoulometric titration
Electrolytic conductivity
(3) Recorder, potentiometric, 10" strip chart
(4) Appropriate Pyrex gas chromatographic columns
Snyder columns, 3-ball (macro) and 2-ball (micro), and
other K-D glassware
Appropriate columns for liquid-solid partition chromatography
Blender
Special materials, such as PR Grade Florisil and pesticide
standards
(b) Organophosphorus pesticides
Gas chromatograph with
(1) Glass-lined injection port
(2) One or more of the following detectors:
Flame photometric, 526 nm phosphorus filter
1 Electron capture, radioactive (R3 or Ni*>3)
(3) Recorder, potentiometric, 10" strip chart
(4) Appropriate Pyrex gas chromatographic columns
Snyder columns, 3-ball (macro) and 2-ball (micro), and
other K-D glassware
Appropriate columns for liquid-solid partition
chromatography
Blender
: Special materials, such as PR Grand Florisil, Woelm
neutral alumina, and pesticide standards
(c) Polychlorinated biphenyls (PCB's)
Gas chromatograph with
(1) Glass-lined injection part
(2) One or more of the following detectors:
207
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Electron capture, radioactive (H^ or Ni63)
Microcoulometric titration
Electrolytic conductivity
(3) Recorder, potentiometric, 10" strip chart
(4) Appropriate Pyrex gas chromatographic columns
Snyder column, 3-ball (macro)
Appropriate columns for liquid-solid partition chromatography
Low-pressure regulator (0-5 psig) with low-flow needle
valve
Blender
« Special materials, such as PR Grade Florisil, high-quality
silica gel, and Aroclor (PCB) standards
(d) Triazine pesticides
Gas chromatograph with
(1) Glass-lined injection part
(2) Electrolytic conductivity detector
(3) Recorder, potentiometric, 10" strip chart
(4) Appropriate Pyrex gas chromatographic column
Snyder columns, 3-ball (macro) and 2-ball (micro), and
other K-D glassware
Appropriate columns for liquid-solid partition
chromatography
Blender
Special materials, such as PR Grade Florisil and
pesticide standards
(e) 0-Aryl carbamate pesticides
Thin layer chromatography plates, 200 x 200 mm, coated
with Silica Gel G, 0.25 mm
, Associated TLC apparatus, including spotting template,
developing chamber, and sprayer (20 ml)
208
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51. Specific Conductance (mho/cm @ 25°C)
(a) Wheatstone bridge
Commercial conductivity meter, or
Apparatus consisting of
(1) Wheatstone bridge (reading to. 1% accuracy or better)
(2) Appropriate source of electrical current
(3) Specific conductance cell
(4) Water bath, 25°C, with racks
52. Turbidity (Jackson units)
(a) Turbidimeter method
Nephelometric turbidimeter, such as Hach Model 2100 or
2100A or equivalent
53. Streptococci bacteria, fecal (number/100 ml)
(a) MPN
Autoclave (to 121°C)
Inoculation tubes
Incubator, 35 + 0.5°C
(b) Membrane filter
Autoclave (to 121°C)
Filter membranes
Petri culture dishes
Incubator, 35 + 0.5°C, ca. 90% relative humidity
Low-power (10-15X), binocular,-wide-field, dissecting
microscope and light source
(c) Plate count
Autoclave (to 121°C)
Petti culture dishes
Incubator, 35 + 0.5°C
209
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Microscope, and light source, or
Colony counter
54. Specific Conductance (mho/cm @ 25°C)
(a) Wheatstone bridge
Commercial conductivity meter, or_
Apparatus consisting of
(1) Wheatstone bridge (reading to 1% accuracy or better)
(2) Appropriate source of electrical current
(3) Specific conductance cell
(4) Water bath, 25°C, with racks
55. Turbidity (Jackson units)
(a) Turbidimeter method
Nephelometric turbidimeter, such as Hach Model 2100 or
2100A or equivalent
56. Streptococci bacteria, fecal (number/100 ml)
(a) MPN
Autoclave (to 121°C)
Inoculation tubes
Incubator, 35 + 0.5°C
(b) Membrane filter
Autoclave (to 121°C)
Filter membranes
Petri culture dishes
Incubator, 35 + 0.5°C, ca. 90% relative humidity
Low-power (10-15X), binocular, wide-field, dissecting
microscope and light source
(c) Plate count
0 Autoclave (to 121°C)
210
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Petri culture dishes
Incubator, 35 + 0.5°e
Microscope and light source, 01:
Colony counter
57. Coliform bacteria, fecal (number/100 ml)
(a) MPN
Autoclave (to 121°C)
Inoculation tubes
Incubator, 35 + 0.5°C
Water bath, 44.5 + 0.2°C
(b) Membrane filter
. Autoclave (to 121°C)
Filter membranes
Petri culture dishes
. Water bath, 44.5 + 0.2°C
Low-power (10-15X), binocular, wide-field, dissecting
microscope and light source
58. Coliform bacteria, total (number/100 ml)
(a) MPN
Same as 56 (a)
(b) Membrane filter
Same as 56 (b)
Radiological Parameters;
The analysis of radiological parameters requires special expertise
and experience, in addition to up-to-date, well-maintained, calibrated
instrumentation and apparatus.
211
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59. Alpha, total (pCi/liter)
Windowless Gas-Flow Proportional Counter and associated
equipment, or
Thin Window Gas-Flow Proportional Counter and associated
Equipment, or
V
Alpha Scintillation Counter and associated equipment, or_
Alpha Spectrometer (Surface Barrier Type) System and
associated equipment
60. Alpha counting error (pCl/liter)
Same as 59.
61. Beta, total (pCi/liter)
Windowless Gas-Flow Proportional Counter and associated
equipment, or_ ^
*.
Thin Window Gaff-Flow Proportional Counter and
associated equipment, or
Beta Scintillation Counter and associated equipment, or
Liquid Scintillation Counter and associated equipment
62. Beta counting error (pCi/liter)
Same as 61.
63. Radium, total (pCi/literX
Windowless Gas-Flow Proportional Counter and associated
equipment, or "
* Thin Window Gas-Flow Proportional Counter and associated
equipment, or
Alpha Scintillation Counter and associated equipment, or
Alpha Spectrometer (Surface Barrier Type) System and
associated equipment, or
Radon Gas Counting System and associated equipment
212
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Other Parameters
64. Temperature
Good quality mercury-filled or dial type centigrade
thermometer, or a thermistor
65. pH
pH meter (electrometer using either glass electrode
and reference, such as saturated calomel, or a combination
glass and reference electrode)
Air Parameters
66. Sulfur Dioxide (yg/m3 or ppm)
(a) Pararosamiline Method
Absorber
Pump
Air flowmeter or critical orifice
Spec tropho tome ter for use at 548 nm, band width
< 15 nm, with 1 cm cells
67. Suspended Particulates
(a) High- Volume Method
High-volume Sampler
Shelter for Sampler
Flow measurement equipment, including:
(1) Ro tame ter
(2) Orifice Calibration Unit
(3) Differential manometer
(4) Positive Displacement Meter
Barometer
Environment for conditioning filters
Analytical balance: chamber to hold unfolded 8" x 10"
filters, sensitivity - 0.1 mg
213
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Glass fiber filters
Acceptable alternative equipment for flow measurement
(3-6): Exhaust orifice meter, interfaced with a circular
chart recorder.
68. Carbon monoxide (yg/nr* or ppm)
(a) Non-dispersive Infrared Spectrometry
1 . . ; t.
Carbon monoxide analyzer (for example; Intech NDIR-CO
Analyzer) .-...,-
' Pump, flow control value, and flowmeter
In-line filter for particles (2-10 ym)
Moisture control (refrigeration unit, or drying tube)
. , \ .
69. Photochemical Oxidant (Oo) (yg/nr* or ppm)
J m
(a) Chemiluminescence, continuous
Commercial photochemical oxidant (0^) analyzer, or
Apparatus consisting of:
(1) Detector cell
(2) Flowmeters (air and ethylene)
(3) Air Inlet Filter (Teflon, 5 m)
(4) Photomultiplier tube
(5) High Voltage Power Supply
(6) Direct Current Amplifier
(7) Recorder
(8) Ozone Source (low pressure Hg lamp/quartz tube)
and Dilution System
Apparatus for Calibration (KI > 1% spectrophotometric
method)
70. Total Hydrocarbons (corrected for methane) GC - FID
(a) Method
Commercially Available THC, CH^, and CO Analyzer
Pump, flow control valves, automatic switching valves,
and flowmeter
. In-line filter (3-5 ym)
214
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Stripper or Precolumn
,' , Oven (for column and catalytic converter)
71. Nitrogen Dioxide (yg/m^ or ppm)
(a) Arsenite 24-Hour Sampling Method
Sampling train (Bubbler, trap, membrane filter,
27-gauge hypodermic needle, air pump, calibration
equipment)
Standard glassware (volumetrlcs, pipets, graduated
cylinders, etc.)
Spectrophotometer or colorimeter for use at 540 ran.
(b) Continuous Chemiluminescent Method
Commercial Chemiluminescent Analyzer: generally including
particulate filter, thermal converter (N02 -" NO),
ozone generator, reaction chamber, optical filter,
photomultiplier tube, and vacuum pump.
Calibration apparatus (gas-phase titration method):
generally including air flow controller, air flowmeters,
pressure regulator for NO cylinder, NO flowmeters,
capillary restriction, ozone generator, reaction
i chamber and mixing bulb, sample manifold, NO detector,
iodometrlc calibration apparatus.
(c) Griess-Saltzman Colorlmetric, Continuous
*. Sampling train
Colorimeter for use at 550 run
215
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TECHNICAL REPORT DATA
(Please read Instructions on the reverse before completing}
1. REPORT NO.
EPA-600/4-78- 017
3. RECIPIENT'S ACCESSION-NO.
4. TITLE AND SUBTITLE
PROCEDURE FOR THE EVALUATION OF ENVIRONMENTAL
MONITORING LABORATORIES
5. REPORT DATE
March 1978 issuing date
6. PERFORMING.ORGANIZATION CODE
7. AUTHOR(S)
Charles A. Bicking, Steven Olin and Peter King
8. PERFORMING ORGANIZATION REPORT NO.
9. PERFORMING ORGANIZATION NAME AND ADDRESS
Tracer Jitco, Inc.
1776 E. Jefferson Street
Rockvllle, MD 20852
10. PROGRAM ELEMENT NO.
1 HD 621
11. CONTRACT/GRANT NO.
Contract No. 68-03-2171
12. SPONSORING AGENCY NAME AND ADDRESS
Environmental Monitoring and Support Laboratory-Gin.,OH
Office of Research and Development
U.S. Environmental Protection Agency
Cincinnati. OH 45268
13. TYPE OF REPORT AND PERIOD COVERED
Contract lin75 fn 11076
14. SPONSORING AGENCY CODE
EPA/600/06
15. SUPPLEMENTARY NOTES
16. ABSTRACT
A procedure was developed for the on-site evaluation of environmental
laboratories in such media as air, water, radiation and pesticides. The
procedure includes registration and preliminary questionnaire forms, on-site
visits checklist, evaluator's guide and a scoring system for assessment of
the laboratory's management, personnel, facilities, analytical methodology
and instruments and its quality control procedures.
This research report is not an official EPA manual. Rather, it is a
report which is but one of a series being used as input to develop EPA
Manuals and Guidelines for Certification Programs.
17.
KEY WORDS AND DOCUMENT ANALYSIS
DESCRIPTORS
b.lDENTIFIERS/OPEN ENDED TERMS
c. COSATI I'iclcl/Croup
Laboratories*, Evaluation*,
Acceptability*, Assessments*,
Inspection*.
Testing Laboratories,
Scoring System, On-Site
Checklist, Preliminary
Forms, Evaluator's
Guide, Grading.
43F
680
91A
18. DISTRIBUTION STATEMENT
Release to Public
19. SECURITY CLASS (This Report I
Unclassified
21. NO OF PAGES
216
20. SECURITY CLASS (Thispage)
22. PRICE
EPA Form 2220-1 (9-73)
216
6 U.S. GOVERNMENT PRINTING OFFICE: 1978- 260-880.44
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