Worldwide Open Proficiency Test: Determination of ... - Nucleus - IAEA

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TABLE 3: TARGET VALUES, STANDARD UNCERTAINTIES AND ACCEPTANCE LIMITS FOR LAP (%) AND MAB (%) OF ANALYTES IN MOSS-SOIL (SAMPLE 01) USED IN THE EVALUATION Analytes Draft, page 10 Massic activity* (Bq/kg) The moss-soil reference material IAEA-447 Uncertainty (Bq/kg) MAB (%) LAP (%) K-40 550 20 20 20 Sr-90 5.0 0.3 20 20 Cs-137 425 10 20 20 Tl-208 13.0 0.5 20 20 Pb-210 420 20 20 20 Po-210 423 10 20 20 Pb-212 37.0 1.5 20 20 Pb-214 26.0 2.0 20 20 Bi-214 24.8 2.0 20 20 Ra-226 25.1 2.0 20 20 Ac-228 37.0 2.0 20 20 Th-234 25.5 3.0 20 25 U-234 21.8 0.8 20 30 U-238 22.2 0.8 20 30 Pu-238 0.15 0.015 20 35 Pu-239+240 5.3 0.16 20 20 Am-241 2.2 0.2 20 25 *Massic activities of daughter radionuclides are valid when secular equilibrium is maintained. The reference date for decay correction is 2009-November-15.
2.3.4.3. Determination of U-234, U-238, Pu-239+240, Pu-238, Am-241 and Sr-90 using the conventional sequential separation method Preparation of the samples The samples were ashed at 600 o C. Ten g weighed ash replicates were taken from the different bottles. Sample decomposition was carried out using the conventional wet digestion procedure, after addition of Sr carrier, Pu-242 and Am-243 tracers. Nine samples were spiked with U-232 tracer too, for the determination of U-238 and U-234. Radiochemical Separations For the separation of uranium, the supernatant obtained from Ca-oxalate precipitation was evaporated to dryness, the oxalate was decomposed by digestion and repeated evaporation with 65% HNO3. The residues were dissolved in 15-30 ml 3 M HNO3, and then loaded on UTEVA resin column (Bed volume; 1.4 ml, column length: 26 mm) pre-conditioned with 20 ml 3M HNO3. The column was washed with 30 ml 3 M HNO3, followed by 20 ml 6 M HCl. Uranium fraction was eluted with 6 ml of H2O eluted with 6 ml of H2O, and then evaporated with 2 ml 65% HNO3. After electro-deposition onto stainless steel discs, uranium was determined by alpha-spectrometry. 2.3.4.4. Determination of U-234, U-238, Pu-239+240, Pu-238, Am-241 using the rapid method Preparation of the samples The samples were ashed at 600 o C. Half g weighed ash replicates were taken from the different bottles. Sample decomposition was carried out by molten salt fusion with 2 g LiBO2, 0.2 g NaCO3 and 0.1 g KI after addition of Pu-242 and Am-243 and U-232 tracers. The melt was pured into 100 ml 1MHCl and then dissolved. Radiochemical Separations The actinides were preconcentrated after reduction with N2H4 by co-precipitation with calcium fluoride in acidic solution [3]. After dissolution of the precipitate the actinides were separated by selective extraction chromatography using a single column filled with TRU resin. Am, Pu and Th were stripped separately, while U and Np were stripped together. U fraction was purified by extraction chromatography using UTEVA resin. Alpha sources were prepared from the chromatographic strip solutions directly by micro-coprecipitation with neodymium fluoride. Activities were determined by isotope dilution alpha spectrometry. Figures 6, 7, 8 and 9 shows the alpha spectra obtained from the moss-soil sample. 2.3.4.5. Instrumentation Alpha-spectrometer system Canbrerra Alpha Analyst Alpha-spectrometer system: EG & G ORTEC OCTETE, with EG & G Ultra BU-020-450-AS PIPS detectors, Canberra AMX 884 multiplexer, RPI 554, ADC 8701,and AIM556 modules.The alpha spectra were collected and evaluated using Canberra Genie 2000 software. WALLAC QUANTULUS 1220 Liquide Scintillation Spectrometer. Liquid Scintillation Spectra were collected and evaluated using Wallac WINQ v. 1.1 and EASYview v.1.0.3.4. Claisse Fluxer and Milestone MLS-Ethos plus microwave. Final Darft, page 11
Page 1 and 2: IAEA Analytical Quality in Nuclear
Page 3 and 4: FOREWORD A reliable determination o
Page 5 and 6: 1. INTRODUCTION A reliable determin
Page 7 and 8: 2.1. Proficiency test objectives 2.
Page 9 and 10: To confirm the assigned target valu
Page 11: program achieving complete sample d
Page 15 and 16: AlphaCounts per channel 2000 1500 1
Page 17 and 18: 3. PERFORMANCE CRITERIA Several rat
Page 19 and 20: acceptable”, a further check is a
Page 21 and 22: TABLE 4. SUMMARY EVALUATION OF ALL
Page 23 and 24: Lab. code Number of reported Scored
Page 29 and 30: 4.2. General recommendations and le
Page 31 and 32: Difference S2-S4 (%) Difference S2-
Page 33 and 34: 4.4. Recommendations related to the
Page 35 and 36: [Bq/kg] 70 60 50 40 30 20 10 0 Ra-2
Page 37 and 38: Figure 22: Part of the Thorium radi
Page 39 and 40: 5. CONCLUSIONS The IAEA-CU-2009-03
Page 41 and 42: REFERENCES [1] DUEWER, D.L., A Robu
Page 43 and 44: APPENDIX I: PERFORMANCE EVALUATION
Page 45 and 46: Lab code Rep. Value Rep. Unc. Unc.
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Lab code Rep. Value Rep. Unc. Unc.
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[Bq/kg] 650 575 500 425 350 275 200
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[Bq/kg] 650 600 550 500 450 400 350
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[ B q /k g ] 70 60 50 40 30 20 10 L
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[Bq] 50 45 40 35 30 25 20 15 10 120
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[Bq/kg] 60 50 40 30 20 10 0 25 223
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[ B q /k g ] 60 50 40 30 20 10 0 72
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[Bq/kg] 15 13 11 9 7 5 3 1 74 131 2
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[Bq/kg] 45 41 37 33 29 25 21 17 13
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[Bq/kg ] 19 17 15 13 11 9 7 5 3 286
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[Bq/kg] 19 17 15 13 11 9 7 5 3 1 25
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[ B q /k g ] 5.5 5 4.5 4 3.5 3 2.5
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[ B q /k g ] 3.5 3.0 2.5 2.0 1.5 1.
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[Bq /kg ] 8.5 7.5 6.5 5.5 4.5 3.5 2
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[Bq/kg] 7.5 6.5 5.5 4.5 3.5 2.5 1.5
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[B q /k g ] 13 11 9 7 5 3 1 515 26
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[Bq /kg ] 11 9 7 5 3 1 219 250 233
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[Bq/kg] 13 11 9 7 5 3 1 273 5264 26
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APPENDIX II: LIST OF PARTICIPATING
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Dr. Victor Badulin Public Exposure
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Dr. David Lobb Department of Soil S
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Petr Rulik Monitoring Department Na
Page 233 and 234:
Mr. Benoit Daniel Eichrom Europe Ru
Page 235 and 236:
Prof. Dr. Constantin Papastefanou A
Page 237 and 238:
Mr. A.G. Hegde Health Physics Divis
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Mr. Mario Montalto Istituto Di Radi
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Mr. Samer J. Al-Kharouf Radiation P
Page 243 and 244:
Ms. Snezana Dimovska Radioecology R
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Dr. Andrzej Komosa Department of Ra
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Ms. Ana-Maria Apostu Dept. of Life
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Mr. Peter Jovanovic Department of P
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Dr. Catalina Gasco Leonarte Ed. 3a
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Dra. Montserrat Llaurado Departamen
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Mr. Abdullah Dirican Turkish Atomic
Page 257 and 258:
Dr. Paul Smedley Centre For Environ
Page 259 and 260:
Mr. Kevin T. Claver Environmental A
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