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

-------
                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.

-------
                                             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

-------
                                 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

-------
                                  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

-------
                                  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

-------
                                 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

-------
          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

-------
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

-------
                            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

-------
                             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.

-------
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.

-------
                              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.

-------
                              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.

-------
     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.

-------
     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.

-------
     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.

-------
     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.

-------
                             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.

-------
     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

-------
                                     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

-------
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

-------
             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

-------
                                             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

-------
                                              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

-------
                                                                                                     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
















-------
                                          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

-------
     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

-------
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

-------
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

-------
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

-------
                                             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

-------
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

-------
                             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

-------
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

-------
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

-------
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

-------
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

-------
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

-------
                               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

-------
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

-------
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

-------
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

-------
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

-------
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

-------
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

-------
                                 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















-------
                           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

-------
                   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

-------
             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

-------
                           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

-------
                               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

-------
                           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

-------
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

-------
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

-------
                         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

-------
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

-------
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

-------
     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

-------
          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

-------
                                                       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

-------
(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

-------
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

-------
(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

-------
Evaluator's Notes
        133

-------
                    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

-------
(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

-------
(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

-------
(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

-------
•  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

-------
                            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

-------
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

-------
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

-------
                         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

-------
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

-------
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

-------
     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

-------
     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

-------
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

-------
                   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

-------
                                    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

-------
(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

-------
(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

-------
                                      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

-------
(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

-------
(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

-------
(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

-------
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

-------
                              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

-------
     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

-------
             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

-------
                      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

-------
      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

-------
              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

-------
                   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

-------
    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

-------
               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

-------
                             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

-------
                               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

-------
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

-------
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

-------
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

-------
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

-------
     (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

-------
      (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

-------
         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

-------
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

-------
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

-------
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

-------
            •  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

-------
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

-------
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

-------
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

-------
            •  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

-------
(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

-------
                   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

-------
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

-------
            •  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

-------
            •  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

-------
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

-------
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

-------
            •  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

-------
            •  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

-------
                                   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

-------