&EPA
United States      Environmental Monitoring and Support FPA-tiOO '7-78-083
Environmental Protection   Laboratory         May 1978
Agency        Cincinnati OH 45268
Research and Development
Evaluation  of the
U.S.  Geological
Survey  Laboratory
Denver, Colorado

Interagency
Energy/Environment
R&D Program
Report

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                 RESEARCH  REPORTING SERIES

 Research reports of the Office of Research and Development, U.S. Environmental
 Protection Agency, have been grouped into nine series. These nine broad cate-
 gories were established to facilitate further development and application of en-
 vironmental technology. Elimination  of  traditional grouping was  consciously
 planned to foster technology transfer and a maximum interface in related fields.
 The nine series are:

      1.   Environmental Health Effects Research
      2.   Environmental Protection Technology
      3.   Ecological Research
      4.   Environmental Monitoring
      5.   Socioeconomic  Environmental  Studies
      6.   Scientific and Technical Assessment Reports (STAR)
      7.   Interagency Energy-Environment Research and Development
      8.   "Special" Reports
      9.   Miscellaneous Reports

 This report has been assigned to  the INTERAGENCY ENERGY-ENVIRONMENT
 RESEARCH AND DEVELOPMENT series. Reports in this series result from the
 effort funded under the 17-agency Federal Energy/Environment Research and
 Development Program. These studies relate to EPA's mission to protect the public
 health and welfare from  adverse effects of pollutants associated with energy sys-
 tems. The goal of the Program is to assure the rapid development of domestic
 energy supplies in an environmentally-compatible manner by providing the nec-
 essary environmental data and control technology. Investigations include analy-
 ses of the transport of energy-related  pollutants and their health and ecological
 effects; assessments of, and development of, control technologies for energy
 systems;  and integrated assessments of a wide range of energy-related environ-
 mental issues.
This document is available to the public through the National Technical Informa-
tion Service, Springfield, Virginia 22161.

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                                          EPA-600/7-78^083
                                          May 1978
               EVALUATION OF THE
       U.S. GEOLOGICAL  SURVEY LABORATORY
               DENVER,  COLORADO
                      by

                Robert L. Booth
            Office of  the Director
Environmental  Monitoring and Support Laboratory
            Cincinnati, Ohio 45268
                  US EPA
     Headquarters and Chemical Libraries
          EPA West Bldg Room 3340
               Mailcode 3404T
          1301 Constitution Ave NW
            Washington DC 20004
               202-566-0556
ENVIRONMENTAL MONITORING AND SUPPORT  LABORATORY
      OFFICE OF RESEARCH AND DEVELOPMENT
     U.S.  ENVIRONMENTAL PROTECTION  AGENCY
           CINCINNATI, OHIO 45268

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                               DISCLAIMER
     This report has been reviewed by the Environmental  Monitoring and
Support Laboratory, U.S.  Environmental  Protection Agency, and approved for
publication.  Mention of trade names or  commercial products does not con-
stitute endorsement or recommendation for use.

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                                FOREWORD
     Environmental  measurements are required to determine the quality of
ambient waters and the character of waste effluents.   The Environmental
Monitoring and Support Laboratory-Cincinnati conducts research to:

     o Develop and evaluate techniques to measure the presence and
       concentration of physical, chemical, and radiological
       pollutants in water, wastewater, bottom sediments, and
       sol id waste.

     o Investigate methods for the concentration, recovery,  and
       identification of viruses, bacteria, and other microbio-
       logical organisms in water.  Conduct studies to determine
       the responses of aquatic organisms to water quality.

     o Conduct an agency-wide quality assurance program to assure
       standardization and quality control of systems for monitor-
       ing water and wastewater.

     This report summarizes the results of an evaluation of the capabil-
ities of the U.S. Geological Survey Laboratory, Denver, Colorado, to
provide valid data for the analyses of water and waste samples on a
variety of contaminants and parameters commonly requested by the U.S.
Environmental Protection Agency.
                                 Dwight G.  Ballinger
                                 Director
                                 Environmental  Monitoring  and  Support
                                   Laboratory - Cincinnati

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                                ABSTRACT


     An onsite evaluation was made of the capabilities of the U.S.
Geological Survey Laboratory at Denver, Colorado.   Particular emphasis
was placed on determining their ability to meet the monitoring requirements
connected with their contractual efforts with the  U.S. Environmental
Protection Agency.  This monitoring is a major part of the Environmental
Protection Agency's quality assurance program in support of energy-related
activities in the western United States.

     Overall, water analyses for parameters related to the broad areas
of chemistry, organics and pesticides, and radiochemistry are being
conducted by approved sampling/preservation techniques and laboratory
methods.  Results on unknown performance samples and cross-check samples
were well within acceptable ranges, thus documenting their ability  to
generate valid data.  Specific recommendations for areas of improvement are
given.
                                   IV

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                                CONTENTS
Foreword	ni.n
Abstract	    lv

  1.    Executive Summary 	     1
  2.    Background	     2
  3.    Water Chemistry 	     3
  4.    Radiochemistry  	     °
  5.    Performance Evaluation	    10

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                                SECTION 1

                            EXECUTIVE SUMMARY

     An onsite evaluation was made of the capabilities of the U.S.
Geological Survey Laboratory at Denver, Colorado.  Particular emphasis was
placed on determining their ability to meet the monitoring requirements
connected with their contractual efforts with the U.S. Environmental
Protection Agency (U.S.EPA). This monitoring is a major part of EPA's
quality assurance program in support of energy-related activities in  the
western United States.

     Team members consisted of Dwight G. Ballinger, Director, and
Robert L. Booth, Deputy Director of the Environmental  Monitoring and
Support Laboratory - Cincinnati, Office of Monitoring and Technical
Support, Office of Research and Development.  A separate visit was  made
by David G.  Easterly of the Environmental  Monitoring and Support Labora-
tory - Las Vegas to determine their radiochemistry capabilities.

     Overall, water analyses for parameters related to the broad areas of
chemistry, organics and pesticides, and radiochemistry are being conducted
by approved sampling/preservation techniques and laboratory methods.
Results on unknown performance samples and cross-check samples were well
within acceptable ranges, thus documenting their ability to generate  valid
data.  The laboratory has ample space, services, and equipment.  The
present staff is composed of well-qualified, conscientious scientists and
technicians.  There is a need, however, for more senior professional  staff
to conduct project studies concurrently with the technicians responsible
for laboratory analyses.  Additional manpower is also  needed in the
organics program to establish the precision and accuracy of their method-
ology and to institute a daily program of quality control  techniques.

     Although approved sampling/preservation techniques are followed,
holding times are often exceeded even before arrival  at the laboratory.
This problem must be corrected.  In addition, a thorough review at  the
management level concerning more effective use of standard reference
materials, duplicates, and spikes is strongly recommended.

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                               SECTION 2

                               BACKGROUND

     An evaluation was made of the U.S.  Geological  Survey (USGS) Lab-
oratory at Denver, Colorado.  The evaluation consisted of preliminary ques-
tionnaires and onsite visits.   Radiochemistry was reviewed January 10-12,
1977, and water chemistry, January 31 through February 2, 1977.   The visits
included an initial briefing session attended by the USGS senior staff and
chaired by Russell McAvoy, Laboratory Director; a general laboratory tour;
two days of detailed discussions with their staff (ranging from the respec-
tive section chiefs to the personnel working at the bench and responsible
for processing the collected samples); and a debriefing attended by senior
staff and members of the evaluation team to discuss the preliminary
findings.  Subsequently, unknown performance samples were provided by the
Quality Assurance Branch, Environmental  Monitoring  and Support Laboratory  -
Cincinnati to document their ability to  generate valid data in the areas of
trace organics, minerals, nutrients, demand, and trace metal  analyses.

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                               SECTION 3

                             WATER CHEMISTRY

     (Reported by Dwight G. Ballinger and Robert L. Booth, EMSL-CI)

Sampling, Preservation, and Holding Times

     Most samples are collected by personnel from the USGS District
Offices/Laboratories and shipped to the Denver Facility for processing
and analyses.  Approximately 80,000 samples are received, and 20 to 30
tests per sample are made, generating 3 to 4 million pieces of data.
Minnesota and all states west of the Mississippi are serviced.  Approx-
imately 75% of the samples are surface waters, 20% are groundwater, and
5% are other.  At present, no samples are being analyzed for either the
Safe Drinking Water Act (SDWA) or the National Pollutant Discharge Elimi-
nation System (NPDES).

     The Sample Receiving Department is responsible for providing proper
containers for sample collection in the field:

     1.   For trace metals, use polyethylene that has been acid-rinsed; it
          may be reused.

     2.   For inorganics, use polyethylene containers direct from the man-
          ufacturer once only.

     3.   For TOC and organics, use glass.  Filtration and preservation are
          done in the field per approved techniques.   All  samples are
          processed as soon as possible and are held  at least 14 days after
          data are stored in the terminal.

     Recommended holding times are not being observed.   There was ample
evidence of samples with holding times that were exceeded even before
arrival at the laboratory.   Internal  lab tour also surfaced TOC samples
that were 2 to 3 weeks old, boron samples over 6 months old,  and pesticide
samples approximately 3 months old.

     RECOMMENDATION:   Institute an immediate program  to rectify problems
                      in (1) sample shipment (adhere  to recommended
                      holding times),  (2) sample receiving (process
                      samples in shortest turn-around time possible), and
                      (3)  the laboratory (guarantee timely analyses of
                      received samples).

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Anajjftj_ca 1  Methodology

     The laboratory has Its own methods that do not necessarily check
completely with USGS Techniques of Water Resources Investigations series.
For the most part, however, methodology appeared to be by approved methods
manuals.  Potential exceptions to 304(g) test procedures are boron,
antimony, molybdenum (need to do extraction techniques), arsenic, COD,
cyanide, color, and turbidity.


     RECOMMENDATION:  Document the methodology used in more formal fashion,
                      determine where variances are present, and submit
                      as proposed alternative test procedures for EPA
                      consideration.

Personnel
     The Denver facility has 47 permanent and 35 temporary positions.
The ratio of technicians to professionals is approximately 2:1.  They
are mandated to contract 0.5 million in FY 77 and 1.5 million in FY 78
for analytical services that will require strict quality control.  Over-
all, the staff is composed of well-qualified, conscientious scientists
and technicians.  There are at least two areas, however, that need
additional manpower.

     RECOMMENDATION:  1. Provide additional  senior staff to conduct
                         project studies.

                      2. Provide additional  professional staff to the
                         Organics Section to prevent backlog of samples,
                         document quality control programs, and institute
                         a daily quality control practice.

Space and Services

     The Denver facility is a comparatively new one-floor structure.   The
space has been utilized in a most efficient manner, and services are ex-
cellent.  Except for some minor first aid items that were verbally noted
in the debriefing, no problem areas were noted.

Equipment

     The Denver facility is exceptionally well  equipped and capable of
performing all the routine analyses in water and waste monitoring.  The
facility has the latest equipment, particularly, in atomic absorption
spectroscopy instrumentation, Technicon equipment, and gas chromatography
instrumentation.

Data Handling and Review

     The Denver facility is currently expanding its computer handling of

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all data by going to an online lab automation system via contract with
Lawrence Livermore Laboratories that will  be similar to EPA's system
operational at EMSL-CI and Region V's Central Laboratory.   Their Quality
Assurance Section has the responsibility for reviewing all  data before it
is reported and checking back with the respective Section  Chiefs on any
problem areas.  Results of performance on  standard reference materials
(USGS water samples used as Water Quality  checks) and computer logic
checks are the two basic mechanisms used for determining the validity of
the reported data.  The Quality Assurance  Section does not routinely uti-
lize results of performance on replicates  (precision) and  spiked (accuracy)
samples.  Thus for measurements that do not have unknown Standard Reference
Materials (SRMs), there are no quality control  checks other than what the
analyst does in preparation of calibration curves.

     RECOMMENDATION:  A thorough review should be made at the management
                      level to determine the most effective ways of
                      utilizing quality control data generated from SRMs,
                      duplicates, and spikes.

Quality Control

     The older version of their quality control program was available for
review, but a newly documented plan should be available in the near future.
We understand it will be coordinated by Bernard Malo of USGS.  Key elements
of the present system are:

     1.   Use of standard water reference samples furnished by Marv Fishman
          at least 1 to 3 times per day for major cations/ions.

     2.   Use of these samples at least twice per week for metals.

     3.   Submission of samples as unknowns to analysts.

     4.   Next-morning computer evaluation: Any value that exceeds 1.5 x SD*
          is flagged and reviewed by the section responsible for analysis.

     5.   A new Quality Assurance Section that submits samples to District
          Offices, who in turn ship into Denver on a 1-per-week basis.  Use
          of dummy stations again, the following morning results are re-
          viewed.  The computer simply states, for example, "chloride
          missed."

     6.   Use of standard water reference samples as known values by
          section chiefs.

     7.   Use of nutrients standard only (used only as a check on standard
          curve).

     8.   Rejection rate of approximately 12%.

*SD from Skougstad1s/Fishman1s RR studies.

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     9.    Use of demand  Analyses  Sets  not  as  quarterly  samples  but  only
          as  checks  on  standard  curve.

    10.    Request for pesticides/organics  quality  control  samples through
          Harold Clements,  EMSL-CI.   (Note:   These have since been  made
          available).

     11.   Performance of approximately 100 checks, including  ion/caton
          balance checks, that are done automatically by the  computer;
          (ditto for total  versus dissolved,  etc.).

     The  Organics Section has a  quality assurance  program that  operates
independently of the above general practice.   Key  elements of its present
system are:

1.    Quality  assurace practice

     a.    Dosed samples  (spiked)

          (1)  Once/month

               (a)  Use  levels from lower  (0.5 to  1.0 ppt) detection on
                    up to 0.5 to 1.0 ml acetone.

               (b)  Spike into distilled water only;  want to  expand to
                    natural  waters.

     b.    Check samples.  Use Applied Science and  their own;  will want
                          to use EMSL's.

     c.    Blind samples.  Hope eventually  to  have  SRM samples  (still
                          some question as to how  real  values will  be
                          determined).

     d.    Duplicates.  Don't use on water; some in sediments.

          (1)  Have done limited sample splitting  with Atlanta  facility.

     e.    Multi-lab studies. ASTM roundrobins.

2.    Performance eevaluation

     a.    No  established criteria for rejection of results (Need SRM's
          or  equivalent).

     b.    Unestablished precision of methods  (strive for ± 10%  in
          standards).

     c.    No  bias data.

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d.   No formal program for repeatability (again, strive for ± 10%).

RECOMMENDATION:  1. National  Bureau of Standards (NBS) thermometer
                    is needed to verify readings on ovens.

                 2. Formal use of class S weights is needed to check
                         out balances.

                 3. Methodology needs to be documented by establishing
                    the precision and accuracy of methods.

                 4. More frequent use needs to be made of duplicate
                    and spiked samples rather than almost total
                    dependence on SRMs.

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                                 SECTION 4

                (Reported by David G. Easterly, EMSL-LV)


     On the afternoon of January 10, 1977, I met with Russell L. McAvoy,
Vic Janzer, and Bernard Malo of the USGS.  Doug Skie of EPA also
attended the meeting.  A general discussion on the purpose and mode of
operation of the visit was held with the above personnel followed by a
tour of the USGS laboratory.

     On January 11, a more detailed discussion as well as an onsite in-
spection of the USGS facilities was conducted.  Topics of discussion in-
cluded staffing, facilities, equipment, quality assurance program responsi-
bilities, and general laboratory operations.

     The present staffing appears very knowledgeable in the field of radio-
chemistry, and all are very well experienced in this field.  For the present
workload at the USGS laboratory, and particularly for any expansion,
additional professional personnel should be considered.  Even though all
personnel are well experienced, it is felt that additional  periodic
training would be advantageous.  The laboratory facilities and equipment
are excellent, and the general laboratory operation appears excellent.

     All of the USGS personnel I talked with seemed aware of the importance
of good quality control practices and indicated a sincere desire to produce
data that are scientifically defensible.   These observations are also
supported by the good results obtained on samples they have analyzed from
the EMSL-LV cross-check program.  The following suggestions are offered for
consideration, however:

     1.   A written quality control plan should be developed.  Each
          branch and, in some cases, each project should have such a plan.

     2.   A routine performance check should be conducted on all balances,
          including documentation in log books.

     3.   Although background tables are kept on a continuing basis
          quality control charts should be employed in the laboratory
          operation.

     4.   A planned service maintenance program should be considered
          for all  counting equipment.

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     On the morning of January 12,  a debriefing was  held with  Russell
McAvoy, Vic Janzer, and Bernard Malo, and the above  topics  were  discussed.

     Again, it is felt that the personnel at the USGS laboratory are  doing
a good job and are aware of the importance of good quality  control
practices.

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                                SECTION 5

                         PERFORMANCE EVALUATION

                 (Conducted by John A. Winter, EMSL-CI)


     Performance evaluation samples were analyzed by the laboratory staff
for the following groups:  trace metals, minerals, nutrients, demands, and
trace organics.  Results of these analyses were reported directly to the
Quality Assurance Branch, EMSL-CI, and processed by means of a computer
program that compared reported values to actual values in relation to
results from previous EPA method studies or from similar interlaboratory
data.

     Overall, the laboratory staff had an outstanding performance.  With
the exception of values for low-level specific conductance, low-level
sulfate, and high-level methoxychlor, all reported values were well within
the warning limits (95% confidence level).  The values for conductance and
sulfate were still  well within the acceptance limits (99% confidence level),
and the potential problem with methoxychlor was resolved in subsequent
analyses of additional check and performance samples.  Thus the laboratory
ultimately showed satisfactory performance for all of the parameters cited
in the following major groupings:

Trace Metals                                 Nutrients

Aluminum                                     Ammonia-N
Arsenic                                      Nitrate-N
Beryl 1i urn                                    Orthophosphate
Cadmium                                      Kjeldahl-N
Cobalt                                       Total Phosphorus
Chromium
Copper                                       Demands
Iron
Mercury                                      COD
Manganese                                    TOC
Nickel
Lead                                         Organics
Selenium
Vanadium                                     Endrin
Zinc                                         Lindane
                                    10

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M1 n e r a l_s                                     Cr g a n 1 c s (Co n 11 n u e d)

pH                                           Mcthoxychlor
Specific Conductane                          Toxaphene
IDS                                          PCB (1254)
Total Hardness                               PCB (1016)
Calcium                                      PCB (1016 and 1254)
Magnesium
Sodium
Potassium
Total Alkalinity
Chloride
Fluoride
Sulfate
                                    11

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                                    TECHNICAL REPORT DATA
                            (Please read Instructions on the reverse be/ore completing}
  REPORT NO.
  EPA-600/7-78-083
                                                             3. RECIPIENT'S ACCESSIOt*NO.
4. TITLE AND SUBTITLE
             5. REPORT DATE

               May  1978  issuing date
  EVALUATION OF THE  U.S.  GEOLOGICAL SURVEY  LABORATORY,
  DENVER, COLORADO
                                                             6. PERFORMING ORGANIZATION CODE
7. AUTHORIS)

  Robert L. Booth
                                                             8. PERFORMING ORGANIZATION REPORT NO.
3. PERFORMING ORG\NIZATION NAME AND ADDRESS
  Environmental Monitoring  and  Support Lab- Cinn.,  OH
  Office of Research and  Development
  U.S.  Environmental Protection Agency
  rinn'nnat.i, Ohio 457KR	
              10. PROGRAM ELEMENT NO.
                IHD621
              11. CONTRACT/GRANT NO.
                In House
12. SPONSORING AGENCY .NAME AND ADDRESS
  Same  as above
                                                             13. TYPE OF REPORT AND PERIOD COVERED
                                                                In  House
              14. SPONSORING AGENCY CODE

                EPA/600/06
15. SUPPLEMENTARY NOTES
16. ABSTRACT
       An onsite evaluation was made of the  capabilities of the U.S.  Geological Survey
  Laboratory at Denver,  Colorado.  Particular  emphasis was placed on  determining
  their ability to meet  the monitoring requirements connected with  their contractual
  efforts with the U.S.  Environmental Protection Agency.  This monitoring is a major
  part of the Environmental Protection Agency's  quality assurance program in support
  of energy-related  activities in the western  United States.

       Overall, water  analyses for parameters  related to the broad  areas of chemistry,
  organics and pesticides,  and radiochemistry  are being conducted by  approved sampling/
  preservation techniques  and laboratory methods.   Results on unknown performance samples
  and cross-check samples  were well within acceptable ranges, thus  documenting their
  ability to generate  valid data.  Specific  recommendations for areas of improvement are
  given.
 7.
                                 KEY WORDS AND DOCUMENT ANALYSIS
                  DESCRIPTORS
                                               b.lDENTIFIERS/OPEN ENDED TERMS
                            c. COSATI Field/Group
  Evaluation
  Water Analysis
  Quality Assurance
 Valid  Data
 Monitoring, Ambient
   14B
18. DISTRIBUTION STATEMEN1


  RELEASE TO PUBLIC
19. SECURITY CLASS /Thit Report)
  UNCLASSIFIED
21. NO. OF PAGES

   18	
20. SECURITY CLASS (This page)

  UNCLASSIFIED
22. PRICE
KPA Form 2220-1 (9-73)
                                                               ir U S GOVERNMENT PRINTING OFFICE 1978 -767 14O/1388
                                              12

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