1、Designation: C 1287 03Standard Test Method forDetermination of Impurities in Nuclear Grade UraniumCompounds by Inductively Coupled Plasma MassSpectrometry1This standard is issued under the fixed designation C 1287; the number immediately following the designation indicates the year oforiginal adopti
2、on or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the determination of 67 ele-ments in uranium diox
3、ide samples and nuclear grade uraniumcompounds and solutions without matrix separation by induc-tively coupled plasma mass spectrometry (ICP-MS). Theelements are listed in Table 1. These elements can also bedetermined in uranyl nitrate hexahydrate (UNH), uraniumhexafluoride (UF6), triuranium octoxid
4、e (U3O8) and uraniumtrioxide (UO3) if these compounds are treated and converted tothe same uranium concentration solution.1.2 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-
5、priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. For a specificwarning statement, see Note 1.NOTE 1Warning: The ICP-MS is a source of intense ultra-violetradiation from the radio frequency induced plasma. Protection from radiofrequency radia
6、tion and UV radiation is provided by the instrument undernormal operation.1.3 The elements boron, sodium, silicon, phosphorus, po-tassium, calcium and iron can be determined using differenttechniques. The analysts instrumentation will determinewhich procedure is chosen for the analysis.1.4 The test
7、method for technetium-99 is given in AnnexA1.2. Referenced Documents2.1 ASTM Standards:C 753 Specification for Nuclear-Grade, Sinterable UraniumDioxide Powder2C 776 Specification for Sintered Uranium Dioxide Pellets2C 787 Specification for Uranium Hexafluoride for Enrich-ment2C 788 Specification for
8、 Nuclear-Grade Uranyl Nitrate So-lution2C 967 Specification for Uranium Ore Concentrate2C 996 Specification for Uranium Hexafluoride Enriched toLess Than 5 %235U2C 1346 Practice for Dissolution of UF6 from P-10 Tubes2D 1193 Specification for Reagent Water33. Summary of Test Method3.1 The sample is d
9、issolved in acid if it is not already asolution. A fixed quantity of internal standard is added tomonitor and correct for signal instability. The level of impuri-ties in the solution is measured by ICP-MS. Customizedsoftware calculates the concentration of each element.3.2 Uranium-concentration-matc
10、hed standard solutions areused to calibrate the ICP-MS instrument. The calibration islinear up to at least 0.2 g/ml (100 g/g U) for each analyte.4,54. Significance and Use4.1 This test method is capable of measuring the elementslisted in Table 1, some of which are required by SpecificationsC 753, C
11、776, C 787, C 788, C 967 and C 996.5. Apparatus5.1 ICP-MS, controlled by computer and fitted with theassociated software and peripherals. May be fitted with coldplasma option.5.2 Autosampler, with tube racks and disposable plasticsample tubes compatible with 5.1 (optional).5.3 Variable Micropipettes
12、:5.3.1 10 L to 100 L capacity.5.3.2 100 L to 1000 L capacity.1This test method is under the jurisdiction of ASTM Committee C26 on NuclearFuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods ofTest.Current edition approved July 10, 2003. Published August 2003. Originallyappro
13、ved in 1994. Last previous edition approved in 2001 as C 1287 95 (2001).2Annual Book of ASTM Standards, Vol 12.01.3Annual Book of ASTM Standards, Vol 11.01.4“ICP-MS Versus Conventional Methods for the Analysis of Trace Impurities inNuclear Fuel,” by Allenby, P., Clarkson, A. S., Makinson, P. R., pre
14、sented at 2ndSurrey Conference on Plasma Source Mass Spectrometry, Guildford, UK, July1987.5“Trace Metals in NBL Uranium Standard CRM 124 Using ICP-MS,” byAldridge, A. J., Clarkson, A. S., Makinson, P. R., Dawson, K. W., presented at 1stDurham International Conference on Plasma Source Mass Spectrome
15、try, Durham,UK, September 1988.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5.3.3 1000 L to 10.00 mL capacity.5.4 Volumetric Flasks:5.4.1 50 mL capacitypolypropylene.5.4.2 100 mL capacitypolypropylene.5.4.3 1 L capacityglass.5.5 P
16、latinum Dish100 mL capacity.5.6 Silica Beaker250 mL capacity.5.7 Watch Glasses75 mm diameter.5.8 Polypropylene Tubes50 mL, with graduation marksand with caps.6. Reagents6.1 The sensitivity of the ICP-MS technique requires the useof ultra high purity reagents in order to be able to obtain thelow leve
17、ls of detection. All the reagents below are ultra highpurity grade unless otherwise stated:6.1.1 Element stock standards at 1000 g/mL for all theelements in Table 1.6.1.2 Hydrofluoric acid (HF), (40 g/100 g), 23 molar.6.1.3 Nitric acidConcentrated nitric acid (HNO3), 15molar.6.1.4 Rhodium Stock Solu
18、tion (1000 g/mL Rh)Commercially available solution (see Note 2).NOTE 2Rhodium stock solution is commercially available suppliedwith a certificate of analysis for the element and a full range of traceimpurities. The solutions are prepared by the manufacturer using a varietyof media designed to keep e
19、ach element in solution for a minimum of oneyear.6.1.5 Sulfuric acid Concentrated sulfuric acid (H2SO4),18 molar.6.1.6 Uranium Standard Base SolutionUranyl nitrate so-lution to Specification C 788, of known uranium (100 g/L) andaluminum content (# 2 g/g U). The total metallic impurity(TMI) content m
20、ust not exceed 50 g/g U and no individualanalyte must exceed 10 g/g U.6.1.7 Purity of WaterUnless otherwise indicated, refer-ences to water shall be understood to mean reagent waterconforming to Specification D 1193, Type I.TABLE 1 Reporting Limits of Impurity ElementsNOTE 1The impurity elements wer
21、e determined in 0.2 % uraniumsolutions, prepared following Section 8.NOTE 2Acquisition time = 10 s/isotope using peak jump mode.NOTE 3103 Rh was used as an internal standard. For the elementswhere the technique is identified as Perkin Elmer Elan 5000A P-E Elan5000A scandium was used as internal stan
22、dard.NOTE 4The LRL is based on the within run standard deviation (Sb)of20 uranium-matched blank determinations for each analyte. This limitequals 4 3 Sb, rounded up to a preferred value in the series 1, 1.5, 2, 3, 4,6, multiplied or divided by the appropriate integer power of ten.NOTE 5The upper rep
23、orting limit can be increased by extending thecalibration to 10 g/mL (5000 g/g U) if the ICP-MS used has an extendeddynamic range (EDR) accessory.NOTE 6For the elements where the technique is listed as P-E Elan5000A, the instrumentation may be specific to those elements. Alterna-tively cold plasma t
24、echnique may be used and it is up to the analyst toperform testwork using spikes and reference materials and to determinethe lower reporting levels.NOTE 7Some of the elements are not included in the materialspecifications and have been included only as a research record for thereaders interest.Analy
25、teMassUsedAnalyteGroupLowerReportingLimit (LRL),g/g UUpperReportingLimit (URL),g/g UTechniqueLithium 7 A 0.01 100 normal plasmaBeryllium 9 A 0.04 100 normal plasmaBoron 11 E 0.3 100 P-E Elan5000ASodium 23 E 0.3 100 P-E Elan5000AMagnesium 24 A 4 100 normal plasmaAluminum 27 D 2 1000 normal plasmaSili
26、con 28 E 1.5 100 P-E Elan5000APhosphorus 31 E 1.5 100 P-E Elan5000APotassium 39 E 2 100 P-E Elan5000ACalcium 44 E 6 100 P-E Elan5000AScandium 45 A 4 100 normal plasmaTitanium 48 B 0.2 100 normal plasmaVanadium 51 B 0.04 100 normal plasmaChromium 52 B 0.1 100 normal plasmaManganese 55 A 0.1 100 norma
27、l plasmaIron 56 A 15 100 normal plasmaCobalt 59 A 0.02 100 normal plasmaNickel 60 A 0.4 100 normal plasmaCopper 65 A 0.2 100 normal plasmaZinc 66 A 0.3 100 normal plasmaGallium 69 A 0.04 100 normal plasmaGermanium 74 A 0.2 100 normal plasmaArsenic 75 A 0.2 100 normal plasmaSelenium 82 A 3 100 normal
28、 plasmaRubidium 85 A 0.06 100 normal plasmaStrontium 88 A 0.06 100 normal plasmaYttrium 89 A 0.04 100 normal plasmaZirconium 90 B 0.02 100 normal plasmaNiobium 93 B 0.01 100 normal plasmaMolybdenum 95 B 0.04 100 normal plasmaRuthenium 102 B 0.02 100 normal plasmaPalladium 106 B 0.2 100 normal plasma
29、Silver 107 A 0.1 100 normal plasmaCadmium 111 A 0.03 100 normal plasmaIndium 115 A 0.04 100 normal plasmaTin 116 B 0.04 100 normal plasmaAntimony 121 B 0.02 100 normal plasmaTellurium 130 B 0.4 100 normal plasmaCaesium 133 A 0.06 100 normal plasmaBarium 138 A 0.02 100 normal plasmaLanthanum 139 C 0.
30、1 100 normal plasmaCerium 140 C 0.01 100 normal plasmaPraseodymium 141 C 0.01 100 normal plasmaNeodymium 146 C 0.01 100 normal plasmaSamarium 149 C 0.01 100 normal plasmaEuropium 151 C 0.01 100 normal plasmaGadolinium 158 C 0.01 100 normal plasmaAnalyteMassUsedAnalyteGroupLowerReportingLimit (LRL),g
31、/g UUpperReportingLimit (URL),g/g UTechniqueTerbium 159 C 0.01 100 normal plasmaDysprosium 163 C 0.01 100 normal plasmaHolmium 165 C 0.01 100 normal plasmaErbium 166 C 0.01 100 normal plasmaThulium 169 C 0.01 100 normal plasmaYtterbium 174 C 0.01 100 normal plasmaLutetium 175 C 0.01 100 normal plasm
32、aHafnium 178 B 0.01 100 normal plasmaTantalum 181 B 0.01 100 normal plasmaTungsten 184 B 0.01 100 normal plasmaRhenium 187 A 0.02 100 normal plasmaOsmium 190 B 0.2 100 normal plasmaIridium 193 B 0.2 100 normal plasmaPlatinum 195 B 0.2 100 normal plasmaGold 197 B 0.06 100 normal plasmaMercury 202 A 0
33、.4 100 normal plasmaThallium 205 A 0.02 100 normal plasmaLead 208 A 0.02 100 normal plasmaBismuth 209 A 0.03 100 normal plasmaThorium 232 B 0.01 100 normal plasmaC12870327. Standards7.1 Four separate mixed standard solutions (A, B, C, and E)are prepared to prevent the precipitation of some elements
34、(asinsoluble chlorides, fluorides etc; see Table 1 for details of theanalyte groups). Analyte group A contains element stocksolutions prepared in HNO3or HNO3/HF, analyte group Bcontains element stock solutions prepared in HCl or HCl/HF,analyte group C contains the rare earth element stock solutions,
35、and analyte group E contains boron sodium silicon, phospho-rus, potassium and calcium. The mixed standard solutionsshould be prepared to contain only the analytes of interest.Other combinations of mixed standard solutions may beprepared to minimize the precipitation of the analytes.7.1.1 Mixed stand
36、ard solution A is prepared from stocksolutions of each element from analyte group A. Transfer 1000L of the stock solution (1000 g/mL) of each element into a50 mL polypropylene volumetric flask and add 500 L ofconcentrated nitric acid. Dilute to 50 mL with water and mix.This multi-element standard co
37、ntains 20 g/mL of each analytein 1 % nitric acid. This solution must be used on the day ofpreparation.7.1.2 Mixed standard solution B is prepared from stocksolutions of each element from analyte group B. Transfer 1000L of the stock solution (1000 g/mL) of each element into a50 mL polypropylene volum
38、etric flask and add 500 L ofconcentrated nitric acid. Dilute to 50 mL with water and mix.This multi-element standard contains 20 g/mL of each analytein 1 % nitric acid. This solution must be used within one weekof preparation.7.1.3 Mixed standard solution C is prepared from stocksolutions of each el
39、ement from analyte group C. Transfer 1000L of the stock solution (1000 g/mL) of each element into a50 mL polypropylene volumetric flask and add 500 L ofconcentrated nitric acid. Dilute to 50 mL with water and mix.This multi-element standard contains 20 g/mL of each analytein 1 % nitric acid. This so
40、lution must be used within one weekof preparation.7.2 Standard solution D is prepared from the stock solutionof aluminum from analyte group D. Transfer 1000 L of thestock solution (1000 g/mL Al) into a 50 mL polypropylenevolumetric flask and add 500 L of concentrated nitric acid.Dilute to 50 L with
41、water and mix. This standard contains 20TABLE 2 Precision Data Derived from PCS and CRM SamplesNOTE 1Acquisition time = 10 s/isotope using peak jump mode. Ac-quisition time is2s/isotope for B, Na, Si, P, K, Ca ( mass 44).NOTE 2Table 2 is a list of “between-run” standard deviations for asingle determ
42、ination based on the analysis of in-house primary controlsamples (PCS series), NBL Certified Reference Material CRM 124-2 andCRM 98-2.NOTE 3103 rhodium was used as the internal standard for allelements except 45 scandium was used as the internal standard for B, Na,Si, P, K and Ca (mass 44).NOTE 4Som
43、e of the elements are not included in the materialspecifications and have been included only as a research record for thereaders interest.Analyte IsotopeConcentration,g/g UStandardDeviation,g/g UNumber ofDeterminationsLithium 7AA.Beryllium 9 10 1.5 10BoronB11 2.9 0.3 8SodiumB23 206 10 8MagnesiumB24
44、52 3.7 5Aluminum 27 21.5 2.5 50SiliconB28 115 19 8PhosphorusC31 204 19 9PotassiumC39 288 20 9CalciumB44 104 8 8Scandium 45AA.Titanium 48 2.0 0.21 29Vanadium 51 2.0 0.19 27Chromium 52 5.0 0.51 27Manganese 55 5.0 0.80 10Iron 56AA.CobaltB59 12.7 0.49 5Nickel 60 22 3.2 7Copper 65 25 4.6 6ZincB66 101 3.5
45、 5Gallium 69AA.Germanium 74 .Arsenic 75 1.0 0.14 10Selenium 82AA.Rubidium 85 .Strontium 88 N/AD. .Yttrium 89AA.Zirconium 90 1.00 0.090 27Niobium 93 1.00 0.095 15Molybdenum 95 2.00 0.091 20Ruthenium 102 2.00 0.141 17Palladium 106AA.Silver 107 N/A . .Cadmium 111 5.0 0.29 10Indium 115 5.0 0.21 10Tin 11
46、6 5.0 0.16 9Antimony 121 1.0 0.10 27Tellurium 130AA.Caesium 133 .Barium 138 10 1.5 10Lanthanum 139AA.Cerium 140 .Praseodymium 141AA.Neodymium 146 .Samarium 149 N/A . .Europium 151 N/A . .Gadolinium 158 N/A . .Terbium 159AA.Dysprosium 163 N/A . .Holmium 165AA.Erbium 166 .Thulium 169AA.Ytterbium 174 .
47、Lutetium 175AA.Hafnium 178 1.00 0.093 35Tantalum 181 1.00 0.100 27Tungsten 184 1.00 0.060 27Rhenium 187AA.Analyte IsotopeConcentration,g/g UStandardDeviation,g/g UNumber ofDeterminationsOsmium 190AA.Iridium 193 .Platinum 195AA.Gold 197 .Mercury 202AA.Thallium 205 5.0 0.16 10Lead 208 5.0 0.25 10Bismu
48、th 209 5.0 0.60 10Thorium 232 5.00 0.020 22AThe elements are not determined on a routine basis. Insufficient precision dataare available but are expected to be similar to those of the analytes where data areavailable.BData obtained from CRM 124-2 analytes.CData obtained from CRM 98-2 analytes.DN/A =
49、 Data not available; still being obtained.C1287033g/mL of aluminum in 1 % nitric acid. This solution must beused within one week of preparation.7.3 Mixed standard solution E is prepared from stocksolutions of each element from analyte group E. Transfer 1000L of the stock solution (1000 g/mL) of each element into a50 mL polypropylene volumetric flask and add 500 L ofconcentrated nitric acid. Dilute to 50 mL with water and mix.This multi-element standard contains 20 g/mL of each analytein 1 % nitric acid. This solutio
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