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Quality Assurance
The CEMRC is subject to the policies,
procedures and guidelines adopted by NMSU, as well as state and federal
laws and regulations that govern the operation of the university. The CEMRC
has adopted a general quality assurance policy (Appendix
J) that includes development and implementation of appropriate standards,
performance assessment and quality improvement, provision of infrastructure,
professional staff development, personal accountability and commitment
to compliance.
The CEMRC's quality assurance policy
and implementation plans recognize that there are distinctions between
standard analytical activities and experimental research settings. For
experimental research settings, there are frequently few if any recognized
analytical standards or procedures for the analyses of interest, and part
of the work that is conducted is to develop such procedures, or to modify
the application of standard procedures for novel media. Likewise, research
sampling designs are typically unique to the underlying scientific hypotheses,
and therefore may not follow any standardized external formats. Therefore,
the quality control measures applied to research contrast with those applied
in programs driven by regulatory requirements, where the sampling frequency
and methodologies and the analytical procedures are spelled out by various
compliance guidelines.
In the WIPP Environmental Monitoring
project, the CEMRC's strategy is to develop a set of independent data for
a variety of parameters of interest, frequently using sampling and analyses
that are different from those dictated by the regulatory requirements that
govern the WIPP's certification and operation. In many cases, these data
will target a larger suite of parameters or lower detection limits than
are of concern from a regulatory perspective. Although this approach may
include some sampling and analyses similar to those conducted by other
groups associated with the WIPP, other activities are unique to the CEMRC's
projects.
Personnel
Program managers provide training to
laboratory and field workers in methodologies, general laboratory protocol
and maintenance routines, and good safety practices. CEMRC laboratory and
technical support staff receive specialized training for operation of specific
equipment or systems, generally offered through equipment vendors. To support
continued professional development, staff members are also provided opportunities
for membership and participation in professional organizations, including
attendance at conferences and workshops. Access to current scientific literature
is provided through a current publications bulletin and a variety of journal
subscriptions and inter-library loans.
Regulatory
Compliance
To promote good health and safety practices
in the laboratories, the CEMRC maintains a Chemical Hygiene Plan and associated
training of personnel, in compliance with the requirements of 29 CFR 1910.1450,
"Occupational Exposure to Chemical Hazardous Chemicals in Laboratories."
A Hazard Communication Plan and associated training are maintained for
employees who do not meet the definition of laboratory workers, in compliance
with requirements of 29 CFR 1910.200. A Chemical Hygiene Officer is responsible
for management of the chemical and laboratory safety program, including
maintenance of a chemical inventory, periodic laboratory safety audits,
and management of any hazardous wastes generated by laboratory activities.
The CEMRC is a conditionally-exempt
small quantity generator of hazardous wastes, as defined and regulated
under the Resource Conservation and Recovery Act. Hazardous waste thus
generated is disposed of through licensed treatment, storage and disposal
facilities. Based on current chemical inventories, the CEMRC is exempt
from the reporting requirements in Section 313 of the Emergency Planning
and Community Right-to-Know Act. The CEMRC has had no spills of hazardous
substances that exceeded the reportable quantity limits under the Comprehensive
Environmental Response, Compensation and Liability Act. The CEMRC currently
has no air contaminant emissions subject to regulation under the Clean
Air Act, and no wastewater discharges subject to regulation under the Clean
Water Act beyond normal sanitary sewer discharges.
Use of radioactive materials is governed
by the CEMRC's Radioactive Materials License, issued by the New Mexico
Environment Department. A Radiation Control Manual and Implementation Plan
and associated training are provided for staff who deal with radioactive
materials. A Radiation Safety Officer is responsible for management of
the radiation safety program, including maintenance of a radioactive materials
inventory, periodic radiation contamination surveys, radiation safety audits,
and management of any radioactive waste generated by laboratory activities.
The CEMRC generates a small amount (<100 lb) of solid, low-level radioactive
waste annually, which is disposed of through a licensed commercial disposal
facility.
Field Sampling
Program Quality Assurance
For collection of most WIPP EM samples,
no external standard procedures are considered appropriate for the objectives
of the studies. In these cases, a customized preliminary plan was developed
and documented. After the activity was completed, the plan was revised
to reflect any departures from the original plan, and documented to file.
For most environmental media, the sampling plans combine selected standard
procedures with specific adaptations to address scientific objectives of
interest. For example, procedures for collection and preservation of samples
for compliance with Safe Drinking Water Act requirements are applied to
the collection of drinking water and surface water samples, but the locations
of sample collection are selected on the basis of other criteria. Likewise,
high-volume air samplers were operated to meet an EPA standard of 1.13
m3min-1, but the frequency of filter replacement
is based on optimal loading for radioanalysis.
Sampling procedures used for collection
and preparation of environmental samples for the WIPP EM project are described
in the individual data summaries that follow. Logbooks are maintained by
technical staff in field operations to record locations and other specifics
of sample collection, and data on instrument identification, performance,
calibration and maintenance. Data generated from field sampling equipment
are error-checked by using routine cross checks, control charts, and graphical
summaries. Original logbooks and field data forms are kept on file in the
program manager’s office. Most data collected in written form are also
entered in electronic files, and electronic copies are cross-checked against
the original data forms. All electronic files are backed up daily.
Calibration and maintenance of equipment
and analytical instruments are carried out on a predetermined schedule
coinciding with manufacturer's specifications or modified to adapt to special
project needs. Calibrations are either carried out by equipment vendors,
or by CEMRC personnel using certified calibration standards. Records of
calibration and maintenance are maintained in instrument-specific files
in the program manager's office.
Radiochemistry
Program Quality Assurance
During 1998, the CEMRC radiochemistry
program participated in one analytical round of the DOE Office of Environmental
Management (EML) Quality Assessment Program (QAP), but did not report results
for the analyses. The radiochemistry program also participated in one round
of testing in the NIST Radiochemistry Intercomparison Program (RIP) on
natural-soil matrix (NRIP98-SO). CEMRC reported 239,240Pu analyses
within 8% of NIST values, 232Th within 1% of NIST values, and
238U
within 16% of NIST values.
Through past intercomparison program
participation (reported in CEMRC
1997 Report), CEMRC has demonstrated basic capabilities to perform
standard radioanalytical procedures for various environmental media. However,
various aspects of the procedures were found to be unsatisfactory for meeting
many of the specific data quality objectives of the WIPP EM, and CEMRC
has undertaken an extensive method development and verification project
that began in May 1998 and will extend through 1999. Thus, virtually no
radioanalytical data were generated by the CEMRC radiochemistry program
for this report. The completion of this developmental phase will include
adoption of a formal quality assurance plan and implementing procedures
for radioanalyses in the WIPP EM project.
Environmental
Chemistry Program Quality Assurance
The analytical methods employed in
the environmental chemistry program at CEMRC are based, when applicable,
on various standard procedures (EPA, 1983, Methods for Chemical Analysis
of Water and Wastes, EPA/600/4-79-020; EPA, 1997, Test Methods for
Evaluating Solid Waste, Physical/Chemical Methods; EPA/SW-846; American
Public Health Association, 1981, Standard Methods for the Examination
of Water and Wastewater, 15th Edition). For some matrix/analyte
combinations, appropriate external standard procedures do not exist, and
CEMRC has developed specialized standard procedures to meet the needs of
the WIPP EM. The following types of analyses are performed at CEMRC:
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anion and cation analysis by ion chromatography (IC)
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elemental analysis by graphite furnace atomic absorption
(AA) spectrometry
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elemental analysis by flow injection hydride AA spectrometry
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mercury analysis by flow injection cold vapor AA spectrometry
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elemental analysis by inductively-coupled plasma atomic emission
(ICP-ES) spectrometry
For the WIPP EM, the IC was used to determine
the concentrations of a suite of major ions in water samples and aqueous
extracts of all media sampled except vegetation (Table
3). The AA and ICP-ES were used to analyze aqueous or acid extracts
of samples (excluding vegetation), depending on the particular question
or issue being addressed.
A set of standard operating procedures
and a formal quality assurance plan have been developed and implemented
for the inorganic analyses performed at CEMRC. A summary of the quality
assurance/quality control procedures applied by the environmental chemistry
program for WIPP EM studies is presented in Appendix
K.
In Vivo
Radiobioassay Quality Assurance
In vivo radiobioassays are performed
in accordance with a formal quality assurance plan and related documentation
that were developed to meet the requirements of the Department of Energy
Laboratory Accreditation Program (DOELAP) for Radiobioassay. The in
vivo radiobioassay program is in the final stages of the DOELAP accreditation
process and anticipates successful completion during 1999.
During 1998, the CEMRC in vivo
radiobioassay program participated in the Intercomparison Studies In
Vivo Program administered by Oak Ridge National Laboratory (ORNL).
This program provides quarterly testing for 137Cs, 60Co,
57Co,
88Y
and 133Ba deposited in whole body. For the three quarters completed
prior to December 1998, CEMRC reported values that were within -0.3 to
3.3% of the ORNL known value for all radionuclides.
External
Laboratory Services
Some analyses presented herein were
carried out by other laboratories through subcontract or fee service arrangements.
These include analyses of radiological and non-radiological constituents
in soils, sediments, surface water and drinking water samples, and analyses
of inorganic constituents in aerosol samples by X-ray fluorescence (XRF)
spectrometry.
Analyses of non-radiological constituents
of water samples were provided by the Soil, Water, and Air Testing Laboratory
(SWAT) at NMSU. SWAT is accredited by the American Association for Laboratory
Accreditation for all of the analyte/test methods applied to drinking water
and surface water samples as noted in summaries for these media. The SWAT
quality assurance/quality control program is documented in a Quality Assurance
Program Plan (QA-QAPP-1).
Radioanalyses of alpha-emitting radionuclides
in soils and sediments reported herein were conducted by Duke Engineering
& Services (DES) in Bolton, Massachusetts. DES maintains a quality
assurance program as documented in the DES Environmental Laboratory Quality
Assurance Plan (Manual 100). DES has achieved acceptable performance for
analyses of environmental samples in the DOE EML QAP, and maintains traceability
to NIST through the NEI/NIST Measurement Assurance Program.
A segment of the non-radiological analyses
of soils and sediments reported herein were conducted by A&L Plains
Laboratory in Lubbock, Texas. A&L soils analyses employ standard methods
as defined by EPA, the American Society of Agronomy, and the American Society
of Soil Chemists. A&L is approved by the Texas Agricultural Extension
Service for analysis of soils, and maintains a quality assurance/quality
control program as documented in the A&L Inter-Laboratory QA/QC Program.
XRF analyses of trace elements in aerosol
samples were conducted by the Desert Research Institute
(DRI), a division of the University and Community College System of
Nevada, in Reno, Nevada. Details of the XRF analytical procedure and the
quality assurance/quality controls (QA/QC) used for the analyses were presented
in the CEMRC
1997 Report.
Table 3. Inorganic Analyses
Conducted at CEMRC
Type of Sample
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IC (Anions)
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IC (Cations)
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Hydrides (As, Sb and Se) and Hg, Flow Injection AA
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Trace Elements (for ICP-ES & AA)
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Air
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Filter extraction with DI water and isopropanol
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Filter extraction with DI water and isopropanol
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Aqueous extract
Total dissolution
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Drinking and Natural Waters
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Syringe filtration with direct injection
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Syringe filtration with direct injection
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Dissolved
Total recoverable
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Soils
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Aqueous extract
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Total recoverable
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Sediments
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Aqueous extract
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Total recoverable
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