DOE PORTSMOUTH PADUCAH PROJECT OFFICE QUALITY SYSTEM FOR NONDESTRUCTIVE ASSAY CHARACTERIZATION

1. DOE PORTSMOUTH PADUCAH PROJECT OFFICE QUALITY SYSTEM FOR NONDESTRUCTIVE ASSAY CHARACTERIZATION ASP 2011 Workshop September 20, 2011 By Don Dihel and Tom Hines Portsmouth/Paducah Project Office and Greg Becker Restoration Services, Inc.

2. Introduction • DOE Portsmouth/Paducah Project Office (PPPO) currently in process of preparing for Deactivation and Decontamination (D&D) of the Portsmouth Gaseous Diffusion Plant. • Nondestructive (NDA) characterization of D&D generated materials must be known, compliant with applicable quality requirements, technically defensible and documented. • NDA program requirements at GDP facilities are primarily oriented to support Nuclear Material Control and Accountability and Nuclear Criticality Safety. • During D&D activities additional end users of NDA characterization data include: equipment decontamination and removal programs, packaging, transportation, storage facilities, disposal facilities, recycling, etc. • In general GDP NDA quality assurance is inadequate to support the needs of D&D end users.

3. Introduction • Lessons learned as a result of Oak Ridge K-25 D&D NDA characterization activities were reviewed by the PPPO in addition to the recommendations of the Defense Nuclear Facility Safety Board 2007-1. • The PPPO review revealed the lack of an NDA quality assurance program was a primary cause for inadequate measurement methods, increased costs and schedule delays during the K-25 D&D effort. • PPPO collaborated with DOECAP to develop a NDA quality program in 2008 (QSAS Appendix E). • PPPO continued to develop other areas of the NDA quality program. • Development of traceable enriched uranium NDA standards to support method development and instrument calibration through modeling. • A uranium based PE program for D&D waste characterization of the PGDP including drums, boxes, process equipment, etc. • Expanded QA system to include in-situ measurements. • Included requirements for development of DQOs. • Included requirements for verification and validation of data.

4. PPPO Quality System for Nondestructive Assay (QSNDA) Basis • PPPO NDA quality program requirements are delineated in the DOE PPPO Quality System for Nondestructive Assay, Rev 0, DOE/PPPO/03-0235&D0, May 2011. • A business entity intending to supply NDA services to the PPPO for D&D must comply with the requirements of the PPPO QSNDA. • Document has been added to contract requirements. • QSNDA based on: • DOE Order O 414.1D, Quality Assurance • National TRU Program, Transuranic Waste Acceptance Criteria for the Waste Isolation Pilot Plant, DOE/WIPP-02-3122, Rev 7.2 • DOE Quality Systems for Analytical Services, Rev 2.6

5. PPPO Quality System for Nondestructive Assay (QSNDA) Basis • QSNDA Comprised of two major sections: • Management requirements • Technical requirements • Management section primarily derived from DOE QSAS and DOE Order 414.1D • Technical section primarily derived from requirements of the National TRU Program WAC • Health and Safety Practices not addressed in PPPO QSNDA since it covered by other DOE contractual requirements. It is the responsibility of the NDA service provider to identify and comply with applicable H&S requirements • NDA Service provider may propose alternate methods of compliance with QSNDA provided PPPO concurrence obtained.

6. QSNDA Technical Provisions • All measurement item attributes affecting the NDA system response must be considered, appropriately addressed and documented. Factors affecting NDA measurement accuracy and uncertainty range from the measurement item configuration and radioactive material distribution to the competency of NDA personnel. • Personnel • Data Quality Objectives • NDA Methods • NDA System Calibration, Confirmation and Verification • NDA Method Detection Limit • NDA System and Support Equipment Maintenance and Records • NDA System Software • NDA Measurement Traceability

7. QSNDA Technical Provisions • NDA Quality Control • NDA Total Measurement Uncertainty (TMU) • NDA Performance Demonstration • NDA Measurement Data Reporting • NDA Data Verification and Validation • Data Management and Control

8. Data Quality Objectives • The NDA service provider shall understand contract DQOs as per end-user requirement and need statements. Concurrence between the NDA service provider, client, and/or end-user and other affected parties shall be documented.

9. NDA Performance Demonstration • The NDA service provider shall demonstrate successful participation in applicable performance demonstration programs (PDP) as part of any PPPO NDA characterization contract. • The NDA service provider shall demonstrate continued PDP acceptance throughout the term of the contracted work. The PDP testing will be single-blind and representative of the waste matrix types and configurations, and analytes to be characterized per the contract. • Unacceptable NDA results for PDP test item(s), as determined per program criteria, will require the NDA service provider to implement corrective action procedures and submit a corrective action plan to the PPPO. •  Until the corrective action is implemented and the results approved by the PPPO, the NDA service provider may not submit characterization reports for the measurement item matrix/radionuclide configurations related to the failed test item configuration.

10. NDA Data Verification and Validation • All NDA measurement data must be verified (reviewed and approved) by qualified personnel prior to being reported. At a minimum, the data and analysis must be reviewed by an independent technical reviewer. This reviewer shall be an individual other than the data generator (analyst) who is qualified to have performed the initial work. • A data validation program shall be in place to ensure provision of evidence that specified requirements has been met to ensure that the required data quality characteristics have been obtained.

11. Uranium NDA Standards (Working Reference Materials) • Radioactive working reference materials (WRMs) must be traceable to a nationally recognized reference base are essential in nondestructive assay (NDA) calibration processes, measurement traceability, and the assurance of data quality to support D&D activities. • WRM Standards (more than a few grams) for NDA are not commericially available at enriched levels using uranium as a basis. • WRM Standards have been developed by PPPO that can be used for: • Calibrations • Calibration Confirmation\Verifications • Performance Evaluations • Benchmarking computer models

12. Working Reference Materials from Sampled Waste • The PPPO has produced three WRMs derived from sampling of actual waste for use in their NDA technical and quality programs. • A subset of three WRM drums from a set of ten WRM drums were produced by Paducah Remediation Services, LLC, (PRS) while contracted by the DOE for disposition of legacy waste in inventory at the PGDP. • These drums were selected such that they span the fundamental characteristics of the waste population, e.g., drum type (geometry), matrix weight, uranium mass, fill height, etc. • Two of the drums are 55-gallon steel drums containing alumina subsequently overpacked in 85-gallon steel drums. The third drum is a 55-gallon steel drum containing alumina subsequently overpacked in an 85 gallon polyethylene overpack. • A QA program was used to ensure all generated data was reviewed and approved.

13. 55-gallon steel drums containing alumina 55-gallon steel drum containing alumina subsequently enclosed in an 85 gallon polyethylene overpack

14. Working Reference Materials from Highly Characterized Material • PPPO fabricated a set of WRMs from highly characterized material consisting of UO2F2 powder encapsulated in 1.0-inch diameter by 9.0-inch high aluminum cylinders. • The specification called for production of approximately three hundred grams of dried and size-reduced uranyl fluoride (UO2F2) at a nominal enrichment of 5%. • The specification included requirements to determine the isotopic composition, purity, radionuclide content, elemental impurities and hydration state of the UO2F2. • The UO2F2 material was required to be dried and size-reduced to a powder form. • The final powder form was then to be loaded into aluminum encapsulation cylinders each with a unique indelible identification. • Completion of the WRM project necessitated documentation of all physical and chemical processes, UO2F2 attribute measurements, measurement traceability, statistical analysis of WRM uncertainties, and preparation of a Certificate of Content and Traceability for each WRM. • A QA program was required to be in place to ensure all generated data was reviewed and approved. This QA program required production of a Level IV data package document. • Special thanks to Andrew Szilagyi and Alexander Williams for their support (Office of Deactivation & Decommissioning and Facility Engineering (EM-44)).

15. UO2F2 powder UF6 gas WRM Tube

16. Continued Development of Working Reference Materials from Highly Characterized Material • Developing thin layer, large surface area uranium WRMs using flexible metal cloth impregnated with UO2F2. • Can be used for to simulate deposit inside piping or GDP process components. • Flexible accommodating many differing thin layer UO2F2 configurations • Non-interfering to gammas and neutrons • Developing standard to represent converter core.

17. Development of Performance Demonstration Program • Through the PPPO QSNDA the NDA service provider is required to participate in a periodic PPPO specified NDA Performance Demonstration Program • the program is designed to yield objective data on NDA system capability and performance relative to uranium bearing wastes and large process components generated as a byproduct GDP D&D activities • The PPPO NDA PDP program is patterned after National Transuranic Program PDP, managed through the DOE Carlsbad Area Office having been successfully implemented for approximately 20 years. • The NDA PDP utilizes test samples comprised of matrix container/traceable radioactive configurations representative of actual waste forms • NDA PDP test samples provide an independent means to assess NDA measurement system performance and compliance per criteria delineated in the NDA PDP Plan.

18. Performance Demonstration Program • The primary isotopes evaluated under the PPPO NDA PDP Plan for uranium contaminated wastes are: • 234U, 235U and 238U • Participating NDA service provider are required to analyze NDA PDP test samples using the same procedures approved and implemented for routine operational waste characterization activities. • A PDP test sample consists of a waste matrix container or large process component representative of a particular waste type or configuration and radioactive material standards of known radionuclide and isotopic composition typical of a D&D waste type. • D&D matrix containers/materials currently in the design phase include: • Individual process components i.e., GDP piping, GDP convertors, compressors • Typical GDP wastes contained in drums and boxes, e.g., metals, combustibles, etc. • Non-containerized materials including; size reduced cell instrument tubing on pallets

19. Conclusion • Lessons learned as a result of Oak Ridge K-25 D&D NDA characterization activities and the recommendations of the Defense Nuclear Facility Safety Board 2007-1 have been incorporated into PPPO plans for D&D of the Portsmouth Gaseous Diffusion Plant. • The PPPO QSNDA provides quality assurance criteria to generate acceptable waste characterization data, decrease analytical costs, and prevent schedule delays due to poor data quality. • PPPO will continue to collaborate with DOECAP to further develop the NDA portion of the QSAS (Appendix E). • PPPO continues to develop other areas of the NDA quality program. • Development of additional traceable enriched uranium NDA standards to support method development and instrument calibration. • Implement a uranium based PE program for D&D waste characterization of the PGDP including drums, boxes, process equipment, etc. • Expand DOECAP Appendix E to include in-situ measurements. • Coordinate with state regulators with respect to the implementation of NDA measurements for waste characterization. • Support DOE resolution of Defense Nuclear Facility Safety Board recommendation 2007-1.

20. Questions?

21. Supplemental Slides

22. Personnel • Evaluation and establishment of personnel qualification requirements for identified project positions or job functions as necessary to execute specified NDA characterization work. • Establishment and documentation of training and proficiency of staff members responsible for technique development, data reduction methods, calibration regimens, performance of NDA measurements, acquired data analysis, QC check performance and monitoring, QA assessment and oversight, record management, etc.

23. NDA Methods • NDA measurement methods employed shall be commensurate with the NDA characterization task at hand, project DQOs, and applicable end user requirements. • The NDA service provider shall have and maintain in-house method manual(s) or equivalent document(s) for each NDA measurement method used to generate data for the end user. • The NDA service provider shall develop and maintain NDA measurement method implementing SOPs governing NDA characterization activities.

24. NDA System Calibration, Confirmation and Verification • A traceable NDA system “initial calibration” shall be performed to ensure the system response provides valid data of known quality relative to the attributes of the measurement items of interest. • The NDA method capability related to each initial calibration must be defined and documented. As applicable, this capability is in terms of waste matrix types, process equipment types, geometries, configurations, radioactive material types, matrix density range, hydrogenous material range, radioactive material mass range, radioactive material compound, etc. • Measurement uncertainties associated with the “initial calibration” shall be established and documented using a sound and technically defensible technique. • The “initial calibration” process shall be clearly documented including the calibration measurement configurations, data acquisition parameters, acquired data, data reduction methods, resultant calibration factors or expressions and statistical analysis.

25. NDA System Calibration, Confirmation and Verification • A “confirmation” of the “initial calibration” shall be performed, assessed, and determined to be correct and true by the collection of objective evidence. • Bias and precision limits are to be used to determine the acceptability of “calibration confirmation” measurements. Recommended acceptance limits are provided in the QSNDA. • Periodic “calibration verifications” are to be performed in a blind manner to ensure the continuing validity of the “initial calibration”. The “calibration verification” shall be performed at least once every five operational days for each measurement system and calibration.

26. NDA Method Detection Limit • A methodology shall be in place to determine NDA measurement system detection limit for those radionuclides specified in the DQOs or other end user requirements.

27. NDA System and Support Equipment Maintenance and Records • The NDA service provider shall maintain records of each major item of NDA instrumentation and support equipment and its software as applicable. These records must include a current list of available major equipment, date of purchase, repair history, calibration history and current status.

28. NDA System Software • Software quality assurance requirements must be implemented by NDA service providers utilizing software as part of NDA characterizations, developed in-house or acquired. • For software acquired from a commercial vendor or other third party, evidence of software QA, functionality, verification and validation (V&V), etc. shall be acquired and maintained by the NDA service provider. • For software developed or modified by the NDA service provider, software development planning and QA controls shall be identified in documented plans. • Computer software developed by the NDA service provider shall be documented as per applicable software development quality standards. • Software change procedures that include instructions for requesting, authorizing, software change requirements, testing, QA, approving, and implementing changes. Software version control methods shall be in place to document the software version currently used.

29. NDA Measurement Traceability • The calibration of NDA instrumentation and support measurement devices, e.g., weight scale, used for NDA characterization shall have traceable calibrations established and documented before being put into service. • The NDA service provider shall have a procedure(s) for the specification, procurement and acceptance of traceable working reference materials (WRMs). The WRM certifications shall be acquired and maintained, and traceable to a nationally recognized reference base, e.g., NIST, NBL. •  The NDA service provider shall retain records for all WRMs including the manufacturer/vendor, the manufacturer’s Certificate of Traceability, the date of receipt, and a certificate expiration date. •  Traceable standards shall be verified at a minimum every five years. Standards with an expiration date less than five years shall be verified at a period equal to the expiration time interval.

30. NDA Quality Control • A measurement quality control program (QC) shall be implemented to ensure that the NDA measurement process provides data of sufficient quality, i.e., the measurement system is in control per defined criteria. •  The NDA service provider shall have procedures implementing applicable QCs for monitoring the validity of NDA measurements and the analytical results. The NDA QC program shall specify qualitative and quantitative acceptance criteria for the QC checks. •  QC measurements are to be performed in conjunction with and related to a batch of NDA measurement items. A batch is a grouping of similar measurement items to which a set of QC criteria is applied to demonstrate acceptability of the results. • Statistical techniques shall be applied to the evaluation of acquired QC data and action levels specified. Procedures shall also be in place to implement corrective actions when QC criteria are not satisfied.

31. • NDA QC Requirements • Background measurements must be performed and recorded for fixed facility neutron and gamma systems for each system in use at least once per day and twice for each batch. •  Instrument performance measurement checks must be acquired for each NDA measurement system in use at least once per day and twice for each batch, one prior to and one after the batch measurements are complete. Performance checks include detection efficiency checks, matrix correction checks and, for spectrometric instruments, energy calibration and energy resolution checks. •  A replicate measurement on an actual measurement item is to be performed once per batch. The replicate item randomly selecting from a batch and is measured again. This measurement item is then to be re-measured using the same NDA system, software, and acquisition/reduction parameters. Data analysis is to be performed independently for the two measurements.

32. NDA Total Measurement Uncertainty (TMU) • The NDA service provider shall have a method to determine TMU for each NDA system employed. •  The NDA service provider shall develop a method for addressing the determination of TMU, definition of all significant uncertainty components, and a method for acquiring data/information on components of variance and processing acquired data and information to arrive at technically defensible TMU for the measurement item population of interest. •  The TMU determination method must be clearly documented for audit purposes and initially reviewed by the PPPO Technical Advisory Board. •  NDA service providers that utilize commercial off-the-shelf data analysis and uncertainty software are accountable to produce clear documentation of the TMU approach, components of variance and the technique for arriving at the TMU value. Proprietary claims by the vendor will not be permitted, although confidentiality agreements to prevent unnecessary spread of this information are acceptable.

33. NDA Measurement Data Reporting • The NDA service provider is to document individual NDA measurement item results in a standard report format agreeable to and approved by the end user(s). For each NDA measurement item there shall be a separate report. The NDA measurement item reports shall contain or reference the location of information sufficient to fully describe all input data, NDA configuration information, acquisition parameters, analysis technique, software version, QC data, etc. to allow reconstruction of the reported results.

34. Data Management and Control • Records including batch reports, raw data, calibrations, QA/QC data, etc. shall be maintained at the NDA service provider facility or shall be forwarded to a PPPO approved repository. • The NDA service provider shall have an information management system for control and maintenance of documents.

35. Working Reference Materials from Highly Characterized Material • The specification called for production of approximately three hundred grams of dried and size-reduced uranyl fluoride (UO2F2) at a nominal enrichment of 5%. Data quality objectives for the project are summarized below: • Load each WRM aluminum encapsulation cylinder with the same 235U mass to the extent practicable. • The maximum allowable 235U and 238U mass total uncertainty per WRM is ± 0.60% at a 95% confidence level. • The maximum allowable 234U mass total uncertainty per WRM is ± 1.0% at a 95% confidence level. • The maximum allowable 232U and 236U mass total uncertainty per WRM is ± 4.0% at a 95% confidence level when above the lower limit of quantification (LLQ). The LLQ must be less than or equal to 0.05 nanograms232U/ g U and less than or equal to 10 micrograms 236U/g U with all values stated at the 95% confidence level. • Each WRM must be traceable to a certified reference material (CRM) or equally valid documentation maintained or issued by a nationally recognized certifying body such as the New Brunswick Laboratory (NBL) or the National Institute of Standards and Technology (NIST).