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Disclaimer The views expressed on this poster are those of the author and do not necessarily reflect the view of the CTBTO SnT2015 Poster No. T2.1-P12 Performances and lessons learned with a transportable radionuclide laboratory deployed during the IFE14 X. Blanchard 1 , A. Rizzo 2 , J. Kastlander 3 , P. Scivier 4 , R. Britton 5 , A. Gheddou 6 1 Preparatory Commission for the Comprehensive Nuclear-Test-Ban Treaty Organization, Austria, CTBTO / OSI, [email protected] 2 Italian National Agency for New Technologies, Energy and Sustainable Economic Development (ENEA), Italy, [email protected] 3 Swedish Defense Research Agency (FOI), [email protected] 4 United Kingdom's Atomic Weapons Establishment (AWE), Aldermaston, United Kingdom of Great Britain and Northern Ireland, [email protected] 5 United Kingdom's Atomic Weapons Establishment (AWE), Aldermaston, United Kingdom of Great Britain and Northern Ireland, [email protected] 6 Preparatory Commission for the Comprehensive Nuclear-Test-Ban Treaty Organization, CTBTO / IDC, [email protected] Analysis in a field Laboratory of radioactivity contained in environmental samples –solids, liquids or gases taken at, below or above the surface- constitutes a fundamental activity during on-site inspections. Goals and context are defined in the Protocol to the Treaty, Part.II, paragraph 69 c) and d) for on-site inspection (OSI) activities and techniques. The Inspected state party (ISP) has a right to observe such activity, and be provided with a copy of its products. For the IFE14, high resolution gamma-ray spectroscopy capabilities were developed to allow for high throughput and accurate measurement and analysis, and provide expected reporting to the joint area and working area for inspection team (IT) assessment [1] . INTRODUCTION The OSI specific constraints that should be taken into account include: • Transportable system on short notice, in order to reach the point of entry within 6 days; a short setup time with minimal labour required; robust equipment and operations • Sufficient space to accommodate IT analysts, an ISP representative, and an observer • Capability to cope with various environmental and logistical conditions including low ISP support, autonomy for stable and reliable power supply, air-conditioning, no dependence on liquid nitrogen (LN2) deliveries • Prevent the occurrence and monitor for absence of cross-contamination, maintain the chain of custody (CoC) and security of samples and data • Capability to process samples (e.g. splitting, compaction) • Capability to analyse high resolution in-situ spectra collected in the field • Capability to measure, analyse and interactively review a high number of samples, in various geometries, including with potentially elevated radioactivity content. Traceable sensitivity, accuracy and precision with documented calibrations accounting for field geometries [2] . GENERAL LAYOUT DURING THE IFE14 The RN Laboratory & Sample receipt area (SRA) in Maridia (Jordan) • Within the radionuclide (RN) Laboratory, sample processing, acquisition of gamma spectra and data reduction steps are intermediate activities carried out by a Laboratory analyst. The ISP has the right to access and observe this inspection activity. • The reviewed analysed concentrations of detected nuclides, with minimum detectable concentrations (MDC) constitute the products of the RN Laboratory. They are transferred to the Joint Area [1] through the IIMS, then made also available to the IT in the Field Information Management System (FIMS). • For convenience during the IFE14 and as planned, RN results were organised by categories of nuclides (Naturals, OSI relevant, other Fission or Activation nuclides, calibration nuclides); No information barrier was played during the IFE14 (methods for applying information barriers have yet to be agreed upon) References: [1] On-site inspection data flow, information handling and management during IFE14, P. Labak et al., Poster No. T2.1-P10 at SnT2015 [2] Expected capabilities for an OSI Laboratory, Chushiro Yonezawa, Presentation at the OSI Workshop 19 [3] Standard Operational Procedure (SOP) and Work Instructions (WIN) for the Field Laboratory analysis during an on-site inspection, CTBTO/OSI, May 2014 [4] Selection criteria for High-purity Germanium detectors, http://www.canberra.com/products/detectors/pdf/Germanium-Det-SS-C39606.pdf [5] High Purity Germanium (HPGe) detectors, Selection criteria, http://www.ortec-online.com/Products-Solutions/RadiationDetectors/Type.aspx [6] Lynx Digital Signal Analyzer, http://www.canberra.com/products/radiochemistry_lab/pdf/Lynx-SS-C38658.pdf [7] APEX-Gamma Lab Productivity Suite, http://www.canberra.com/products/radiochemistry_lab/apex-gamma.asp [8] User Manual for Open Spectra, interactive review tool from NDC-in-a-Box, CTBTO/IDC Documentation, [9] Formats and Protocols, CTBTO/IDC documentation [10] Model S574 LabSOCS Calibration Software, http://www.canberra.com/products/radiochemistry_lab/pdf/LabSOCS-SS-C40167.pdf [11] Technical Advantages of ISOCS / LabSOCS, Application Note, http://www.canberra.com/literature/isocs/application_notes/ISOCS-LabSOCS-App-Note-C39530.pdf [12] A Multiple Sample Holder for Ganging Samples During IFE14, A. Rizzo et al., Poster No. T2.1-P1 at SnT2015 [13] Comparing In situ γ-spectroscopy and sampling/lab assay, lessons that apply to their application in OSI, S. Kreek et al., Poster No. T2.1-P5 at SnT2015 CONFIGURATION OF HIGH-PURITY GERMANIUM DETECTORS AT IFE14 Early on planned for four germanium detectors (Q1 2013), the RN Laboratory hosted seven high purity germanium (HPGe) detectors [4,5] prepared for use during the IFE14. The main characteristics and preferred sample geometry types for these seven HPGes are: - All with electro-mechanical cooling, 2x Canberra CP5, 4x Ortec X-Cooler III (2 spare X-Coolers, and a compact LN2 production unit capable of cooling 2 HPGes were available – not used ) - Portable Falcon 5000, 18% relative efficiency, p-type BEGe BE2830, calibrated at 4 distances (1 to 4m) for high activity samples. Network cable to allow for measurement outside the RN Laboratory itself. - p-type BEGe BE5030 with thin carbon-epoxy window. Mostly used for gas cell measurements of Xe. - p-type GC7020, 70% rel. efficiency, 1.9 keV FWHM at 1332 keV, multi purpose incl. Marinelli 0,5L - Four p-type PopTop configurations, high relative efficiencies from 110% to 130%, Electronics: Digital 32k MCAs (six Canberra Lynx [6] units) operated through a Local Area Network (LAN) with Apex-Gamma Software modules: - Laboratory management of spectral acquisition and QA/QC functionalities: Canberra APEX-Gamma [7] ( one server with a mirrored spare and daily backup ; 2 Laptop clients) - Gamma-ray emission analysis : PTS / IDC developed NDC-in-a-Box [8,9] , customized for IFE14 needs ( isotope library; scripts for importing sample meta-data, specific reporting to IIMS & FIMS ) - PTS developed GUI for the Chain of custody of samples and data, Timelines during BOO setup and conduct of the IFE14: - Day 1 at BOO: download container, setup awning (0,5d) ; install detectors, 2 cooled down in evening - Day 2: first 2 detectors calibrated, Background measurements started. Install sample receipt area. - Day 3: first samples being counted on return of first field missions. E-cal. & background for other HPGes - End -4 days: Backgrounds, then all but 2 HPGes decommissioned . - End -3 days: started counting last samples from last field missions. -2 days: last analysis incl. In-situ - Last but 1 day: start packing. Last reporting incl. QA/QC. - Last day: catch-up with packing. Acknowledgements: The authors whish to thank all contributors that allowed the development , preparation, and deployment of this Mobile Field RN Laboratory during the IFE14. Several States Parties contributed with equipment (Mobile Lab container and awning, HPGe detectors, in-situ detectors, others), documentation of method and numerical studies (SOP, WIN, Monte Carlo simulations for f.e.p. Efficiency calibrations of specific geometries including in-situ) and hours of work. Special thanks also go to all RN surrogate inspectors that participated during Field Tests and Training activities to the timely development and validation of the IFE14 configuration. A new configuration for the Mobile RN Field Laboratory was successfully deployed and operated during the IFE14. The IFE14 constituted a real challenge, but offered a unique framework for testing equipment capability and operations in an realistic OSI environment. All 161 environmental samples and high resolution in-situ spectra taken during the field missions were analyzed, and results reported to the Joint Area. The RN Laboratory setup included seven high-purity germanium for high resolution gamma-ray spectroscopy, all electrically cooled, and a new Laboratory Information Management System (LIMS) to operate the network of HPGe detectors with QA/QC functionalities. All spikes prepared by the Control Team (5 samples with 1 Bq of OSI relevant radionuclide, and 5 samples at the 10 Bq level) were detected (no Type-II error). A few type-I errors were identified, which is statistically consistent with the number of analyses carried out; the false detections were cleared either through longer measurements or more sampling at the location of interest. The RN Laboratory raw data have been made available to State Parties, and careful analysis of its performances will benefit to refining deployment strategies (CONOPS) for RN field measurement and sampling techniques. Important lessons were learned and are being collected and analyzed. They will help shape future development and provide inputs to the next OSI Action Plan. CONCLUSIONS Conversion table: provided to the Lab analyst for mapping actual radionuclides detected to OSI relevant radionuclides, since no fresh fission products were actually used in the IFE14 1,2ton lead cave: equipped with three electromechanically cooled detectors –two internal lead separations. A second similar lead cave can be seen to the right. In the right corner: one in-situ 15% HPGe used for hot samples (not played during the IFE14), calibrated at 1-2-3-4meters. Can be moved 40m away from Lab using a network cable. On the top shelf: router and 6 MCAs to Apex-Gamma server Validation of HPGe f.e.p. efficiency calibrations obtained by LabSOCS [10,11] NPL Certificate Experimental Experimental PTS/OSI, 05 / 2014 Geant4 simulation AWE, 09/2013 LabSOCS calculation characterised crystal Bq @ Acq time unc. (abs) Energy (keV) Net Area (counts) Efficiency unc. ( abs) Efficiency unc. ( abs) Efficiency unc. ( abs) Diff (%) LabSoc/Exp -1 531 29 59.54 364 0.0315 0.0024 0.0312 0.0031 0.0338 0.0034 7.4 407.2 8 661.65 1120 0.0539 0.0019 0.0536 0.0032 0.0574 0.0023 6.6 141 2 1173.22 257 0.0360 0.0046 0.03641 0.0015 0.03840 0.00094 6.7 141 2 1332.49 246 0.0347 0.0043 0.03352 0.0010 0.03510 0.00083 1.3 Detector CAN01: is LabSOCS characterized. Results to the left show: 1 % to 4 % difference to the AWE Geant4 simulation ; 7,4% to 1,3% difference to the LabSOCS simulation for this specific crystal that is LabSOCS characterised. NPL Certificate Experimental Experimental 05 / 2014 Geant4 simulation AWE, 09/2013 LabSocs calculation similar crystal Bq @ Acq time unc. (abs) Energy (keV) Net Area (counts) Efficiency unc. ( abs) Efficiency unc. ( abs) Efficiency unc. ( abs) Diff (%) LabSoc/Exp -1 (%) AWE/Exp -1 531 29 59.54 333 0.0288 0.0070 0.0312 0.0031 0.0338 0.0034 17 8.2 407.2 8 661.65 1460 0.0702 0.0046 0.0536 0.0032 0.0574 0.0023 -18 -24 141 2 1173.22 329 0.0461 0.0044 0.0364 0.0015 0.03840 0.00094 -17 -21 141 2 1332.49 339 0.0478 0.0023 0.0335 0.0010 0.03510 0.00083 -27 -30 Detector ORT02: is NOT LabSOCS characterized. However a “close” LabSOCS characterization input file has been provided by Canberra for approaching detector characteristics. Results show: +8% to -30% difference to the AW E Geant4 simulation ; +17% to -27% difference to the LabSOCS simulation for this crystal that is NOT LabSOCS characterised. Method: Monte Carlo efficiency simulations are compared with experimental measurements of a standard from NPL, UK. (compressed IMS filter of 5 cm diameter x 7mm height). Screening capability : Efficiency for combined samples Prepared for IFE14: A set of up to 7 samples is measured on top of detector. The whole set is cleared or enters Newtonian search. A second screening geometry is available for 13 samples on 2 layers including around crystal. The 2 pre-defined geometries (7 and 13 samples) are LabSOCS characterized for each detector. QA/QC during IFE14 under APEX-GAMMA [ 6] 1 • Procedures were predefined and implemented for – Initial Energy calibrations using NORM QC sources – System Backgrounds: on inspection start / end – Periodic Background Checks, e.g. every 3 weeks – Daily QC calibration checks => cf Control chart example ca 115 QC measurements acquired / reviewed during IFE14 115 QC measurements acquired / reviewed during IFE14 115 QC measurements acquired / reviewed during IFE14 115 QC measurements acquired / reviewed during IFE14 • Defined levels of Warning and Action Limits • ca 18 predefined sample geometries ( LabSOCS) 18 predefined geometries for IFE14 and Detector efficiencies Control chart: preventative corrective action (Energy recalibration) after a 0,7 keV drift was detected. Recalibration using QC check source ( Zircon sand with high thorium content ) SAMPLE CHAIN OF CUSTODY (CoC) 1 CTBTO developed GUI application to manage mission planning and related field mission data: Information tracked for RN activities includes equipment allocated to missions, sample bar codes issued, sample meta-data, log of CoC of samples (tracking who did what, when and where with samples), and Laboratory analysis products. Sample relevant meta-data from the field is downloaded from the IIMS before Laboratory analysis, and reports are uploaded to the IIMS. RN TRANSPORTABLE LABORATORY : THE WAY FORWARD • Sea shipment is required for the current 20 feet container configuration: this implies transport delays that are inconsistent with OSI timelines. A multi-year project will be launched with the objective to design and implement the required functionalities within Modular and Rapid Deployment flight pods. • Analysis of lessons learned from IFE14 should lead to agreement on a configuration for HPGe detectors to be operated in an OSI field RN Laboratory. Synergies for HPGe detectors might be gained from IMS compatible systems. Options include 60 to 70% relative efficiency crystals rather than 110-130%. • Up to three independent sets would be required to allow for two concomitant inspections, as currently decided by the Preparatory Commission. • A multi-year funding capability would allow progressive implementation to be established, including recapitalization in the long term for aging detectors. • A critical requirement to ensure the availability of an operational system when required on short notice is the development of a technology Laboratory that can host 24/7 operations over several weeks, in order to allow for scheduled periodic preventative maintenance, calibration checks, documentation and certification of equipment and performances. OBJECTIVES Loss of 50% in efficiency, but gain of x7 or x13 in mass – quantity of samples. Low background sample holders for ganging samples were made available for the IFE14 [12] Discussion : 1) Both AWE Monte Carlo GEANT4 simulations and PTS/OSI efficiency calculations with LabSOCS are compatible 2) Experimental calibration conducted by PTS shows a bias of +20 to -30% over the energy range of interest for uncharacterized detector. The current available LabSOCS file would correspond to a smaller crystal with less attenuation at low energies. 3) It is recommended that all HPGe Laboratory detectors undergo a LabSOCS characterization to allow for accurate efficiency calculations. Field Activity IFE14: 130 samples in various geometries (excl. noble gas samples) IFE14: 31 in-situ spectra from 13 Field Missions Setup: during Mission RN013 RN Laboratory analyses: In-situ Cs-137: 97.3 ±8.6 Bq/m 2 MDC Cs-137 : 28 Bq/m 2 Total Cs-137 : 30.6 ±2.7 kBq Soil sample taken at the same location: Sample Cs-137 : 0.460 ±0.085 Bq or 184 ±34 Bq/m 2 MDA Cs-137 : 0.35 Bq MDC Cs-137 : 140 Bq/m 2 Sampled area: 25 cm 2 , volume ca 25 cm 3 At BoO / Sample Receiving Area: samples and In-situ spectra are handed-over to Laboratory custodian ACQUISITION AND ANALYSIS AT IFE14 HPGe full-energy peak efficiency calibrations: Monte Carlo simulations and validations before the conduct of the IFE14 Shoe covers and Lab coats before entering measurement area Sample storages under joint custody Interface to IIMS (air gap) Lab analyst, ISP and Control Team representatives at Separate sample preparation area, with contamination prevention procedures and equipment + - All 130 environmental samples collected were counted, analyzed including through interactive review, and final products delivered to the Joint Area at the BOO. - 31 high-resolution in-situ spectra were similarly analyzed and reported - Results above represent together 10 times more reported results than during the previous Integrated field exercise conducted in 2008. - 115 quality control (QC) measurements (for system backgrounds, Energy calibrations, and daily QC checks) were acquired and reviewed - Systematic approach for LabSOCS efficiency calibrations. - Detailed comparative analysis of MDCs obtained by Laboratory analysis versus high resolution in-situ will inform on respective advantages [13] of the methods to further develop the CONOPS for RN field measurements and sampling strategies. Not or little exercised : - “hot” sample collection, handling and analysis - Work in (potentially) contaminated environment - Sample processing (e.g. splitting, compacting) in the dedicated area - Data authentication - Information barriers Identified areas for substantial improvements: - Design study to adapt the RN Laboratory to flight pods for air instead of sea shipment - Improve or re-design various software modules (e.g. IIMS interface) for robustness and user-friendliness - Elaborate Working instructions (WIN) on several topics, including hot sample management, troubleshooting, planning and logging activities, reporting key findings, management of inspector rotations. - More dedicated training is needed under fully operational conditions MAIN ACHIEVEMENTS – GAPS – IMPROVEMENTS NEEDED
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