A Basic Course in the Fundamentals of Analytical Radiochemistry ...

A Basic Course in the Fundamentals of Analytical RadiochemistryState and Local government environmental radiological laboratories often must hire personnelwho are inexperienced in the area of radiochemistry and radiological sciences. As a result, mosttraining is done on-the-job usually with little or no formalized classroom training of relevantscientific principles. Often, no radiochemist is available who brings with them a strongbackground in the area of radiochemistry. In other cases, an experienced radiochemist may beavailable but may not have the time needed to develop and implement a formal training program.This document presents an outline for a formalized course designed to provide radiochemistrylaboratory personnel with a fundamental understanding of concepts and methodologies pertinentto radiochemical testing in general, with an additional focus on water handling and analysispertinent to routine drinking water and effluent water programs. The final day of the course willfocus on operational laboratory concerns including laboratory safety, radiological protection,radioanalytical contamination control, and while considering the potential impact on laboperations from an Incident of National Significance (INS) such as a terrorist radiological ornuclear attack.The course will be held at the U.S. EPA Office of Radiation and Indoor Air (ORIA) National AirRadiation Environmental Laboratory (NAREL) in Montgomery, Alabama. Although studentswill not likely be able to perform hands-on analytical duties at the host laboratory, being in alarge, working radiochemistry laboratory such as NAREL, will provide prospectiveradiochemists with:• Adequate facility space and instrumentation for training• Opportunities to observe laboratory operations including:o Radiological laboratory support operations;o Radiochemical preparations and separations;o Operations involving the major radioanalytical instrumentation types routinelyencountered in the environmental radiochemistry laboratory;o Observe operations from preparation through the radioanalytical process.After a basic introduction to radioactivity and principles critical to radiochemical separationstechniques on the first day, each day will focus on a different detection type beginning with themost basic technique, Liquid Scintillation Counting (LSC) and will culminate with spectroscopictechniques. This approach allows students to reinforce general principles while being introducedto more specific principles in the context of applied techniques. Students will be asked to do asmall amount of independent work in the evenings to further reinforce applied concepts and tohelp identify areas that need further clarification.The final day of the course will focus on applied operational issues of the radiochemistrylaboratory. Using an Incident of National Significance (INS) such as a radiological or nuclearterrorist attack as an example, fundamental concepts vital to everyday lab operations, as well asthe potential impact of an INS on a radiochemistry laboratory, will be presented and explored.Topics addressed will include: sample receipt, screening, handling and prioritization; radioactivematerial and waste management; measures for radiological safety and worker protection;radioanalytical contamination controls; method applicability, selection and validation; andappropriate quality assurance/quality control (QA/QC) measures in the radiochemistrylaboratory.December 2010 Page 1 of 7

About the Instructors:A Basic Course in the Fundamentals of Analytical RadiochemistryAnna Berne, Ph.D. is a nationally recognized expert in radiochemistry and radioanalytical methods,particularly in the field of radiochemical analysis of low-level environmental materials, with additionalinterest in generating data of known and appropriate quality. During her 16 years at the EnvironmentalMeasurements Laboratory, she gained expertise on an international scale in the field of radiochemicalanalysis of low-level environmental materials, with additional interest in generating data of known andappropriate quality. She has been responsible for radiochemical analysis of the Quality AssessmentProgram (QAP) Performance Evaluation (PE) samples, as well as analysis of samples for other nationaland international programs, such as the Radiological Traceability Program (RTP, sponsored by theDepartment of Energy and the National Institute for Standards and Technology) and the InternationalAtomic Energy Agency intercomparison programs. She has also been involved in developing new radioanalyticalmethods at EML and presented the results of her work at national and international meetingsand conferences, such the annual Conference on Bioassay, Analytical, and EnvironmentalRadiochemistry (BAER, currently called RRMC), the International Conference on Methods andApplications of Radioanalytical Chemistry (MARC) and The International Conference on RadionuclideMetrology and its Applications (ICRM). Dr. Berne is an active member in the ASTM Committee D19.Robert Litman, Ph.D. has been a researcher and practitioner of nuclear and radiochemical analysis forthe past 34 years. He is well respected in the nuclear power industry as a specialist in radiochemistry andradiochemical instrumentation and plant systems corrosion. He authored the section of the EPRI PWRPrimary Water Chemistry Guidelines on Radionuclides and has been a significant contributor to EPRIPrimary-to-Secondary Leak Detection Guidelines. For the past four years, he has been the radiochemicalspecialist at the decommissioning of the Yankee Rowe Nuclear Power Station for water and soilanalytical sampling and analysis. He has co-authored two chapters of MARLAP, and is currently one of ateam of specialists presenting MARLAP training. His areas of technical expertise are gammaspectroscopy and radiochemical separations. Dr. Litman has been teaching courses in Radiochemistryand related special areas for the past 18 years.Robert Shannon is recognized as a national expert in environmental radiochemistry and radiobioassay,radioanalytical laboratory management and QA/QC, and method, laboratory and information systemsdevelopment. His intimate familiarity with the methods, techniques and protocols of environmentalradiochemistry stems from years of applied laboratory experience. He has served as technical directorand radiochemistry manager with several commercial laboratories, as deputy manager of the on-sitelaboratories, and Radiochemistry and Radiobioassay Subject Matter Expert at the Rocky FlatsEnvironmental Technology Site, CO and is a radiochemistry auditor with the Department of EnergyConsolidated Audit Program (DOECAP). Mr. Shannon contributes extensively to methods, standards andQA system development activities with ASTM Committees D19 and C26, Standard Methods for theExamination of Water and Wastewater and is a member of the Health Physics Society and the AmericanChemical Society. In 2003, he received the RRM/BAER (Radiobioassay & Radiochemical Measurements/Bioassay,Analytical, and Environmental Radiochemistry Conference) Conference FoundersAward.December 2010 Page 2 of 7

A Basic Course in the Fundamentals of Analytical RadiochemistryPROJECTED COURSE OUTLINEWelcome and Introductions1. Introduction to Radioactivitya. Forms of radioactive decayb. Types of particles emitted in radioactive decayc. Interactions of radioactivity with matterd. Basic radioactive decay law and calculation of simple decaye. Units of radioactivity and radioactivity concentrationf. Natural chain decay relationships impacting presence and measurement ofcommonly-encountered, regulated natural and anthropogenic radionuclidesg. Examples of decay chains and radioactive equilibrium2. Liquid Scintillation Counting – Theory of Analysisa. Typical uses – strengths and limitationsb. Instrument theory and operationc. Detection efficiency (response)d. Background activitye. Basic equations for determining radioactivity from count data3. Tritium Analysis by Liquid Scintillation Counting (EPA Method 906.0)a. Natural and anthropogenic sources of tritiumb. Regulatory background (Safe Drinking Water Act-SDWA)c. Scope and application -typical used. EPA Method 906.0 summarye. Sample preparationf. Radioanalysisg. Typical LSC problems and method interferences; Quenchh. Example calculations4. Principles of Radiochemical Separationsa. Radiometric Measurements and Interferencesb. Solubility and precipitationc. Oxidation and reductiond. Complexatione. Solvent extraction and ion exchangef. Carriers and tracers5. Gas-Filled Detectors and Gas Flow Proportional Counting (GPC)a. Typical use – strengths and limitationsDecember 2010 Page 3 of 7

A Basic Course in the Fundamentals of Analytical Radiochemistryb. Instrument theory and operationc. Instrument set-upd. Background quantification and correctionse. Detector calibrationsf. Common problems and interferences6. Measurement of Gross Alpha and Beta Radioactivity (EPA Method 900.0)a. Natural and anthropogenic sources of alpha and beta emittersb. Regulatory background (SDWA)c. Scope and application - typical used. EPA Method 900.0 summarye. Sample preparationf. Radioanalysisg. Typical GPC problems and interferencesh. Calculation of example result7. Radium-228 Analysis (EPA Method 904.0)a. Natural and anthropogenic sources of Ra-228b. Regulatory background (SDWA)c. Scope and application - typical used. EPA Method 904.0 summarye. Sample preparationf. Radioanalysisg. Example calculations8. Alpha Spectrometrya. Instrument theory and operationb. Typical uses – strengths and limitationsc. Detector Calibrationd. Alpha Spectral Featurese. Background activityf. Basic equations for determining radioactivity from count data9. Isotopic Uranium by Alpha Spectrometry (ASTM Method D3972)a. Natural and anthropogenic sources of alpha emittersb. Regulatory background (SDWA)c. Scope and application - typical used. Overview EPA Method 908.0e. Review ASTM Method D3972f. Sample preparationDecember 2010 Page 4 of 7

A Basic Course in the Fundamentals of Analytical Radiochemistryg. Radioanalysish. Common problems and interferencesi. Calculations10. Sample Preservation and Sample Pretreatment and Preparationa. Types of samples expected by a laboratoryb. Purpose of sample preservationc. Preservation techniquesd. Maintaining sample integrity during sample preparatione. Techniques and strategies for sample dissolution11. Statistics Unique to Radiochemical Applicationsa. Estimation and reporting of uncertainty in radiochemical analysis,b. Counting uncertaintyc. Counting uncertainty vs. combined standard uncertaintyd. SDWA ‘Detection Limit’e. Critical level concentrationf. Minimum detectable activity and concentrationg. SDWA ‘Detection Limit’12. Radium-226 by Alpha Scintillation (EPA Method 903.1)a. Typical uses – strengths and limitationsb. Instrument theory and operationc. Detection efficiency (response)d. Background activitye. Natural and anthropogenic sources of Ra-226f. Regulatory background (SDWA)g. Scope and application - typical useh. Review EPA Method 903.1i. Sample preparationj. Radioanalysisk. Calculations13. Gamma Spectrometrya. Typical uses – strengths and limitationsb. Instrument theory and operationc. Spectral featuresd. Detection efficiency (response)e. Background activityf. Basic equations for determining radioactivity from count dataDecember 2010 Page 5 of 7

A Basic Course in the Fundamentals of Analytical Radiochemistry14. Gamma Spectrometry (EPA 901.0)a. Natural and anthropogenic sources of gamma emittersb. Regulatory background (SDWA)c. Scope and application - typical used. Libraries and spectral analysise. Review EPA Method 901.0f. Common problems and interferences15. Quality Assurance (QA) in Radiochemical Analysis Overview of Requirements forthe Laboratorya. Laboratory QA plan / manualb. Laboratory documents and recordsc. Method validationd. Training and demonstration of analyst capabilitiese. Maintaining chain of custodyf. Auditsg. Preventive maintenanceh. Corrective actionsi. Data reduction and reportingj. Data review16. Quality Assurance for Standards and Equipment (Non-Counting) in RadiochemicalAnalysisa. Labeling, sample flow and sample tracking practicesb. Sample preservation and preparationc. Statistical process controld. Batch conceptse. Batch QC sample evaluationf. Performance testing programsg. Sample specific quality indicating parametersh. Batch QC sample evaluation17. Concepts and Recommendations for a Radiation Incident of National Significancea. Radioanalytical Needs Following a Radiation Incidentb. Directed Exercise: Introduction of Drinking Water Contamination Scenario(Sample Control)c. The Data Quality Objectives / Measurement Quality Objectives (DQO/MQO)Processd. Methods for Incident Response ApplicationsDecember 2010 Page 6 of 7

A Basic Course in the Fundamentals of Analytical Radiochemistrye. Directed Exercise: Continuation of Drinking Water Contamination Scenario(Sample Screening and Handling)f. Radiation Protection and Contamination Control in a Radiochemistry Laboratoryg. Maintaining Quality Control During Incident Response Operationsh. Managing Operational Resources during Incident Responsei. Incident Response Laboratory Analysis: Protocol Paradigm Shift?j. Directed Exercise: Prioritization of Samples through Scenario IDecember 2010 Page 7 of 7