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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, 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 a major task is to develop such procedures, or to modify the application of standard procedures for new 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 typically 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, 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 also maintained for all employees, in compliance with requirements of 29 CFR 1910.200. A Chemical Hygiene Officer and Hazard Communications Coordinator are responsible for management of the chemical and laboratory safety programs, including maintenance of chemical inventories, periodic 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 the collection of most WIPP EM samples, no external standard procedures are considered completely appropriate for the objectives of the studies. In these cases, customized preliminary plans were 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 predetermined schedules 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.
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, 20th Edition).
For the WIPP EM, an ion chromatograph (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 atomic absorption spectrometer (AAS) and inductively coupled plasma-mass spectrometer (ICP-MS) were used to analyze aqueous or acid extracts of samples (excluding vegetation), depending on the particular question or issue being addressed.
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. 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. During November 1999, the environmental chemistry program began analyses for performance testing under the National Voluntary Laboratory Accreditation Program, but test results had not been received by the end of the year.
Radiochemistry Program Quality Assurance
During 1999, the CEMRC radioanalytical program participated in two rounds of the NIST Radiochemistry Intercomparison Program (NRIP) and achieved traceability for all analytes reported. The radioanalytical program also participated in the DOE Environmental Measurement Laboratory Quality Assurance Program (EML QAP), resulting in "acceptable" ratings for 45 results from glass fiber filters, soil, vegetation and water samples.
CEMRC has undertaken an extensive method development and validation project that began in May 1998 and will extend through 2000. New standard procedures have been developed and adopted for WIPP EM analyses for soil samples, water samples and aerosol filters. Method development will continue for sediment and biota during 2000. 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. A summary of general quality assurance/quality control procedures used by the radioanalytical program is presented in Appendix L.
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. During 1999, CEMRC received performance-testing results from DOELAP for 241Am and 235U in lungs and 134Cs and 137Cs in whole body. CEMRC passed all performance criteria with relative biases for 241Am, 235U, 134Cs and 137Cs of -0.14, 3.77, 2.00 and 6.25%, respectively. The DOELAP onsite assessment of CEMRC was performed during the summer of 1999. Through this assessment, CEMRC's radiobioassay quality assurance, quality control and operational practices are scrutinized by national experts in radiobioassay. No deficiencies were determined in the CEMRC program and final accreditation was awarded in late 1999.
During 1999, 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. From the 1998 annual report issued in the Spring of 1999 (four quarters in total), CEMRC reported values that were within -0.62 to 3.25% 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 constituents in sediments, surface water and drinking water samples and analyses of soil texture.
The Soil, Water, and Air Testing Laboratory (SWAT) at NMSU provided analyses of soil texture. The SWAT quality assurance/quality control program is documented in a Quality Assurance Program Plan (QA-QAPP-1).
Duke Engineering & Services (DES) (Bolton, Massachusetts) conducted Radioanalyses of alpha-emitting radionuclides in sediments reported herein. 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.
Los Alamos National Laboratory, Chemical Science and Technology Division conducted analyses of 239Pu in surface water and drinking water samples. These analyses employed distillation, separation, purification and electrodeposition, followed by thermal ionization mass spectrometry, as described by Perrin et. al., (1985, Int. J. Mass Spectrometry and Ion Physics, 64, 17). Use of this technique was recently successful in documenting long-distance migration of Pu in ground water at the Nevada Test Site (Kersting, A.J., et. al. 1999, Nature, 397, 56).
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-MS & 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 |
Total recoverable |
|
Sediments |
Aqueous
extract |
|
Total recoverable |
Total recoverable |
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