&EPA
United States
Environmental Protection
Agency
Environmental Monitoring and Support EPA-600/7-78-137
Laboratory July 1978
Cincinnati OH 45268
Research and Development
Evaluation of the
U.S. Geological
Survey Laboratory
Atlanta, Georgia
Interagency
Energy/Environment
R&D Program
Report
-------
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.
-------
EPA-600/7-78-137
July 1978
EVALUATION OF THE
U.S. GEOLOGICAL SURVEY LABORATORY
ATLANTA, GEORGIA
by
Robert L. Booth
Environmental Monitoring and Support Laboratory
Cincinnati, Ohio 45268
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
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, 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.
-------
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
solid 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 capabilities
of the U.S. Geological Survey Laboratory, Atlanta, Georgia, 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
-------
ABSTRACT
An onsite evaluation was made of the capabilities of the U.S. Geological
Survey Laboratory at Atlanta, Georgia. 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
eastern United States.
Overall, water analyses for parameters related to the broad areas of
chemistry, organics and pesticides, and aquatic biology 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.
-------
CONTENTS
Foreword . . . iii
Abstract iv
1. Executive Summary 1
2. Background 2
3. Hater Chemistry 3
4. Aquatic Biology 8
5. Performance Evaluation 11
-------
SECTION 1
EXECUTIVE SUMMARY
An onsite evaluation was made of the capabilities of the U.S.
Geological Survey Laboratory at Atlanta, Georgia. Particular emphasis was
placed on determining their ability to meet the monitoring requirements con-
nected with their contractual efforts with the U.S. Environmental Protection
Agency (USEPA). This monitoring is a major part of EPA's quality assur-
ance program in support of energy-related activities in the eastern United
States.
Team members consisted of Dwight G. Ballinger, Director; Robert L. Booth,
Deputy Director; and Cornelius I. Weber, Aquatic Biology Section Chief, of
the Environmental Monitoring and Support Laboratory - Cincinnati, Office of
Monitoring and Technical Support, Office of Research and Development.
Overall, water analyses for parameters related to the broad areas of
chemistry, organics and pesticides, and aquatic biology 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, to recognize the overall responsibilities of the
Section Chiefs and reclassify their positions to at least one higher GS level.
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.
-------
SECTION 2
BACKGROUND
An evaluation was made of the U.S. Geological Survey (USGS) Laboratory
at Atlanta, Georgia. The evaluation consisted of preliminary questionnaires
and an onsite visit January 16 - 20, 1978. The visits Included an initial
briefing session attended by the USGS senior staff and chaired by
Donald Leifeste, Laboratory Director; a general laboratory tour; three days
of detailed discussions with their staff (ranging from the respective
section chiefs to the personnel working at the bench and responsible for
processing the collected samples); and a debriefing attended by Director's
Office 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 Suppprt Laboratory - Cincinnati,
to document their ability to generate valid data in the areas of trace
organics, minerals, nutrients, demand, and trace metal analyses.
-------
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 Atlanta Facility for processing and analyses.
Approximately 95% of the samples are surface waters, and 5% are other.
At present, no samples are being analyzed for either the Safe Drinking
Water Act (SDWA) or the National Pollutant Discharge Elimination 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.
2. For inorganics, use polyethylene containers direct from manufacturer
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. Temperature settings should be
verified on storage refrigerators; consideration should be given to a
recording-type thermometer.
Recommended holding times are not being observed at all times.
Primarily, the problem appears to be in delayed and extended shipment times.
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).
Analytical 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. Exceptions to 304(cj) test procedures are 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 con-
sideration.
Personnel
The Atlanta facility has 40 permanent, 12 permanent part-time, and 12
temporary positions. The ratio of technicians to professionals is approxi-
mately two to one. Overall, the staff is composed of well-qualified, con-
scientious scientists and technicians. There are at least two areas, how-
ever, that need additional manpower.
RECOMMENDATION: 1. Provide additional senior staff to conduct project
studies.
2. Provide additional professional staff to the
Quality Assurance Section to document quality
control programs and institute a daily quality
control practice.
Space and Services
The Atlanta facility is exceptionally well equipped and capable of per-
forming 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 Atlanta facility is currently expanding its computer handling of 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 utilize results of performance
on replicates (precision) and spiked (accuracy) samples. Thus for measure-
ments that do not have unknown standard reference materials (SRM), 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.
It will be coordinated by David Erdmann, Deputy Laboratory Director and
Bernard Malo of USGS. Key elements of the present system are:
1. Use of standard water reference samples (SRMs) furnished by
flarv Fishman at least 1 to 3 times per day for major cations/ions
and trace metals.
2. SRMs are also submitted as unknowns to analysts on a scheduled
basis.
3. Next-morning computer evaluation: Any values that exceed
1.5 x SD* is flagged and reviewed by section responsible for
analysis.
4. Also submit samples to District Offices, who in turn ship into
Denver on a 1-per-week basis using dummy stations. The following
morning results are reviewed. The computer simply states, for
example, "chloride missed."
5. Use of EPA nutrients standard only (used only as a check on
standard curve).
6. Rejection rate of approximately 20%.
7. Performance of approximately 100 checks, including cation/ion
balance checks, that are done automatically by the computer (ditto
for total versus dissolved, etc.).
The Organics Section has its own written quality assurance program
that operates independently of the above general practice. Key elements of
its present system are:
1. Standard checks must fall within +_ 5". If not, standing current
is adjusted.
2. Spiked samples/blanks must be >_70%. If not, checks are made on
system.
3. Do sample splitting with Denver USGS Lab.
4. Do not use EPA quality assurance check samples or participate
in round robin studies.
*SD from Skougstad's/Fishman's RR studies.
5
-------
Summary of Recommendations by Sections
A. Logistics Support (I)
1. Verify temperature settings on storage refrigerator. Con-
sideration should be given to a recording-type thermometer.
2. Stop using color wheel for color measurements; instead, use
approved platinum-cobalt spectrophotometric procedure.
3. Turbidity samples with values greater than 40 NTUs should be
diluted and re-run.
B. Automated Wet Methods (II)
1. Use stirrer mechanism (similar to that used for automated
mercury) when doing "total" ammonia, nitrate/nitrite, and
nitrite. As it is, at best, a decanted sample is being used.
2. In addition to making corrections for color interference,
corrections should be made for turbidity interference when
necessary.
C. Trace Metals (III)
1. Hhen doing total metals, standards should be carried through the
complete digestion step with each sample set (blanks already
are).
2. Verify that metal samples have been acidified before beginning
any analyses. A simple check with pH paper will suffice.
3. Use the Environmental Protection Agency's Quality Assurance Check
Sample, at least on a quarterly basis, as an independent check
on the entire system.
4. Check out deionized water, especially before making up primary/
working standards.
5. Be more systematic in use of SRMs and in recording of checks
made.
D. Manual Methods (IV)
1. When ordered National Bureau of Standards thermometer arrives,
institute routine, documented checks on two ovens set at 105°
and 180°C.
2. Process metal standards through digestion step (see item C.I)
-------
E., Pesticides (V)
1. Make use of the Environmental Protection Agency's Quality Assurance
Check Samples as an independent check on the entire system.
F. Automatic Data Processing
1. Verify data being transferred to computer disc (this 1s not
being done by anybody).
5. Quality Assurance
1. Review computer checks to determine 1f all parameters possible are
being covered.
2.* Broaden use of blind SRMs. Add series for detergents, pesticides,
and total organic carbon.
3.* Include ammonia, orthophosphate, and TKN in nutrient series
blind SRMs.
4.* Document actions taken on SRMs that are "rejections" and subse-
quent steps taken to correct potential problems.
H. Management
1. Routine checks need to be made on the deionized water and out-
lets at sinks need to be policed.
2. Safety Hints:
a. Hot all of the staff use safety glasses.
b. Box for safety glasses for visitors was empty.
c. Eye wash facilities are not that noticeable or prevalent in
most of the working areas.
3. Staff should be "brought on board" as soon as possible to explain
how lab automation system will work, what it will do for them, and
how is can be used on a real-time basis to document quality of data.
4. Written quality assurance plan should be prepared as soon as
possible that can act as a minimal, base-line program that all
Sections must follow (Pesticides was the only section that had a
written plan).
5. Better communication is needed between Quality Assurance and the
Sections.
*A third person may be needed to do this.
-------
SECTION 4
AQUATIC BIOLOGY
(Reported by Cornelius I. Weber, EMSL-CI)
General Comments
Staff members within the Biology Section are very concerned about the
quality of their data, and carry out many basic quality assurance practices.
A quality assurance plan was recently prepared, but it has not been imple-
mented. As a result, quality assurance practices are limited largely to
instrument calibration.
It is recommended that management assume a more aggressive role in
supporting the Biological Quality Assurance Program, and authorize the
staff to dedicate a significant part of their time to quality assurance
activities. In this regard, it would be advisable to formally designate one
of the senior staff as Quality Assurance Officer 1n the Section, and give
them the authority to develop and implement a comprehensive Biological
Quality Assurance Program.
Deficiences in the Biological Quality Assurance Program were especially
noticable in the following areas: sample replication; the use of blind and
split samples; use of available biological reference materials; proofing and
verification of data on bench sheets by a second party; use of log books to
record instrument calibration, performance checks and service.
Phytoplankton Analysis (Counts and Identification)
Current phytoplankton analyses are limited to counts and identifications
to the genus level. Most of the phytoplankton analysis staff are relatively
inexperienced. At the time of the onsite evaluation, there was a large
backlog of plankton samples. The staff was under considerable pressure to
process the samples as rapidly as possible and did not feel free to
allocate time for quality assurance. However, adequate quality assurance
in the analyses is especially important because of the relative inexperience
of most of the bench personnel. It is recommended, therefore, that blind and
split samples be incorporated into the sample stream as soon as possible
at a level of approximately 10% of the total number of samples processed.
It is recommended that identifications be carried to the species level.
Data at the genus level are of very limited use because species within a
genus often differ greatly in their response to environmental conditions.
Identifications could be carried out to the species level with very little
8
-------
additional effort and would be much more useful in supporting the mission of
the laboratory. It is also recommended that diatom species proportional
counts be added to the phytoplankton analyses. Diatom identifications can
be taken to the species level with a greater degree of certainty than with
other groups, and the data are more useful because of the large literature
that has already been published on diatom ecology.
The sampling schedule should be modified to include spring and fall
bloom periods. Clump counts should be used instead of cell counts, except
for the diatoms because of the preponderance of historical data, and the
greater sensibility of the counting unit in data interpretation. The
calculations on the completed bench sheets should be routinely verified by
a second person to detect arithmetical errors before the data are machined.
Periphyton
Samples are collected primarily for biomass and chlorophyll a. measure-
ments, but a qualitative taxonomic analysis, consisting of identifications
and determination of relative abundance, is also carried out. Standard
practices are employed in the biomass analysis. However, sample collection
methods (substrate depth and exposure time) do not conform to generally
accepted practices and should be standardized. It is recommended that the
substrates be exposed only at (near) the surface of the water for a standard
exposure period within the range of 2-4 weeks (preferably 2 weeks), which
should be held constant at all stations within a drainage basin. At least
three replicate samples should be collected for biomass and chlorophyll a_
measurements. Bound log books should be used to record data on the perform-
ance of the balances, which should be checked with standard weights before,
during, and after each group of samples are weighed.
Periphyton samples are analyzed for chlorophyll using high-pressure
liquid chromatography. The analysis is limited to chlorophyll a^ and Ib. The
method is new and was recently submitted to the Journal of Chromatography
for publication. It is recommended that the method be checked with standard
reference materials available from the Environmental Monitoring and Support
Laboratory.
Some carelessness was noted in the handling of incoming samples which
must remain frozen to ensure sample integrity. Receiving personnel and the
laboratory staff should exercise greater care in sample handling and must
discard samples which are not frozen when they arrive from the field.
Macroi nvertebrates
Samples are collected with hardboard multiplate samplers and are analyzed
to determine numbers, identification and biomass of the organisms. This
program is in a pilot phase and samples are collected at only a few stations.
It is suggested that the substrates be exposed at a standard depth (within the
interval of 1-2 meters) at all stations for a fixed period of time, preferably
4-6 weeks. At least three replicates samples should be taken at each station.
-------
Organisms should be identified to the species level whenever possible for
the same reasons discussed under the phytoplankton section.
Adenosine Triphosphate (ATP)
Kits are supplied to field personnel for the extraction of ATP from
seston in grab water samples, and the extract is returned to the laboratory
for analysis. The instrument calibration is thorough. However, the sample
preparation instructions in the field kit are inadequate and should be
modified to prevent the loss of ATP (the details of this problem were
discussed with Dr. Shoaf). Arrangements should also be made with field
personnel to collect replicate samples and to provide blind and split
samples. Laboratory personnel should take advantage of round robin samples
available from the American Society for Testing and Materials (ASTM) (a
second round robin will be carried out in 1978). Reference samples will be
available from the Quality Assurance Branch, Environmental Monitoring and
Support Laboratory - Cincinnati, in 1979.
Algal Growth Potential (AGP)
The method employed for the AGP analysis is essentially the one
developed by the EPA with some modifications. If only one AGP value is to
be obtained, it is recommended that the "total" AGP be measured. In this
case, samples should be autoclaved before filtering to release the
nutrients in the particulate fraction. These nutrients are generally re-
cycled within the plankton community and would be available for algal growth.
If the AGP of the "residual" nutrients (dissolved nutrients only) is desired
as a second value, aliquots of the sample could be filtered (without auto-
claving) and analyzed along with autoclaved-filtered aliquots.
The calibration of the Coulter Counter appeared to be adequate, but it
is suggested that the instrument be checked regularly with the "simulated
plankton" reference sample available from the Quality Assurance Branch,
Environmental Monitoring and Support Laboratory - Cincinnati. Three
replicate inoculations of standard culture medium should be incubated
with each group of field samples as a quality assurance check on culture
conditions, and the factor employed to convert cell volume to dry weight
("yield") should be validated. It is also recommended that temperature
recorders be installed on the exterior of all environmental chambers.
10
-------
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, Environmental Monitoring and Support Laboratory
- Cincinnati, 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, inter!aboratory data.
Overall, the laboratory staff performed very well. A low level result
on one of the arsenic samples was reported, but subsequent analyses of
additional check and performance samples were acceptable. Likewise, unac-
ceptable results on fluoride were corrected in a subsequent set of samples;
apparently, the initial error was due to mislabeling and not to a laboratory
analysis problem. Data were not reported for selenium and dieldrin in the
first set of samples, but subsequent checks were acceptable. Thus, the
laboratory ultimately showed satisfactory performance for all the parameters
cited in the following major groups:
Trace Metals Minerals Organics
Aluminum Calcium Aldrin
Arsenic Chloride Chlordane
Beryllium Fluoride Dieldrin
Cadmium Magnesium ODD
Cobalt pH DDE
Chromium Potassium DDT
Copper Sodium Heptachlor
Iron Specific Conductane PCB (1016)
Mercury Sulfate PCB (1254)
Manganese TDS PCB (1016 and 1254)
Nickel Total Alkalinity
Lead Nutrients
Selenium Demands
Zinc Ammonia-N
COD Kjeldahl-N
TOC Nitrate-N
Orthophosphate
Total Phosphorus
11
-------
TECHNICAL REPORT DATA
(Please read Instructions on the reverse before completing)
1. REPORT NO.
EPA-600/7-78-137
3. RECIPIENT'S ACCESSION NO.
4. TITLE AND SUBTITLE
EVALUATION OF THE UNITED STATES GEOLOGICAL SURVEY
LABORATORY, ATLANTA, GEORGIA
5. REPORT DATE
July 1978 issuing date
6. PERFORMING ORGANIZATION CODE
7. AUTHOR(S)
Robert L. Booth
8. PERFORMING ORGANIZATION REPORT NO.
9. PERFORMING ORGANIZATION NAME AND ADDRESS
10. PROGRAM ELEMENT NO.
1NE 625
SANE AS BELOW
11. CONTRACT/GRANT NO.
12. SPONSORING AGENCY NAME AND ADDRESS
Environmental Monitoring and Support Lab.
Office of Research and Development
U.S. Environmental Protection Agency
r.inn'nnat.i. Ohio 4B?68
- Cinn, OH
13. TYPE OF REPORT AND PERIOD COVERED
In-House
14. SPONSORING AGENCY CODE
EPA/600/06
15. SUPPLEMENTARY NOTES
16. ABSTRACT
An on-site evaluation was made of the capabilities of the U.S. Geological Survey
Laboratory at Atlanta, Georgia. 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 eastern United States.
Overall, water analyses for parameters related to the broad areas of chemistry,
organics and pesticides, and aquatic biology are being conducted by approved
sampling/preservation techniques and laboratory methods. Specific recommendations
for areas of improvement are given.
17.
KEY WORDS AND DOCUMENT ANALYSIS
DESCRIPTORS
b.IDENTIFIERS/OPEN ENDED TERMS
c. COSATI Field/Group
Evaluation
Water Analysis
Quality Assurance
Valid Data
Monitoring, Ambient
14-B
18. DISTRIBUTION STATEMENT
Release to public
19. SECURITY CLASS (ThisReport)
Unclassified
21. NO. OF PAGES
17
20. SECURITY CLASS (TMspage)
Unclassified
22. PRICE
EPA Farm 2220-1 (9-73)
12
»U.S. OOVDIKMEOTPSIimKISOmCt 197E—757- HO/14
-------
U.S. ENVIRONMENTAL PROTECTION AGENCY
Office of Research and Development
Environmental Research Information Center
Cincinnati, Ohio 45268
OFFICIAL BUSINESS
PENALTY FOR PRIVATE USE, S3OO
AN EQUAL OPPORTUNITY EMPLOYER
POSTAGE AND FEES PAID
U S ENVIRONMENTAL PROTECTION AGENCY
EPA-335
THIRD CLASS
If your address is incorrect, please change on the above label
tear off; and return to the above address.
If you do not desire to continue receiving these technical
reports. CHECK HERE d tear off label, and return it to the
above address.
EPA-600/7-78-137
------- |