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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:

  • anion and cation analysis by ion chromatography (IC)
  • elemental analysis by graphite furnace atomic absorption (AA) spectrometry
  • elemental analysis by flow injection hydride AA spectrometry
  • mercury analysis by flow injection cold vapor AA spectrometry
  • 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

IC (Anions)

IC (Cations)

Hydrides (As, Sb and Se) and Hg, Flow Injection AA

Trace Elements (for ICP-ES & AA)

Air
Filter extraction with DI water and isopropanol
Filter extraction with DI water and isopropanol
 
Aqueous extract
Total dissolution
Drinking and Natural Waters
Syringe filtration with direct injection
 
 Syringe filtration with direct injection
Dissolved
Total recoverable
Soils
Aqueous extract
 
Total recoverable
 
Sediments
Aqueous extract
 
Total recoverable