ASTM C1508-2018 Standard Test Method for Determination of Bromine and Chlorine in UF6 and Uranyl Nitrate by X-Ray Fluorescence (XRF) Spectroscopy.pdf

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1、Designation: C1508 01 (Reapproved 2011)C1508 18Standard Test Method forDetermination of Bromine and Chlorine in UF6 and UranylNitrate by X-Ray Fluorescence (XRF) Spectroscopy1This standard is issued under the fixed designation C1508; the number immediately following the designation indicates the yea

2、r oforiginal adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This method covers the determination of bromine (Br) an

3、d chlorine (Cl) in uranium hexafluoride (UF6) and uranyl nitratesolution. The method as written covers the determination of bromine in UF6 over the concentration range of 0.2 to 8 g/g, uraniumbasis. The chlorine in UF6 can be determined over the range of 4 to 160 g/g, uranium basis. Higher concentra

4、tions may be coveredby appropriate dilutions. The detection limit for Br is 0.2 g/g uranium basis and for Cl is 4 g/g uranium basis.1.2 The values stated in SI units are to be regarded as the standard.1.3 This standard may involve hazardous materials, operations and equipment. This standard does not

5、 purport to address allof the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriatesafety safety, health, and healthenvironmental practices and determine the applicability of regulatory limitations prior to use.1.4 This inter

6、national standard was developed in accordance with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development of International Standards, Guides and Recommendations issuedby the World Trade Organization Technical Barriers to Trade (TBT) Comm

7、ittee.2. Referenced Documents2.1 ASTM Standards:2C761 Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of UraniumHexafluorideC787 Specification for Uranium Hexafluoride for EnrichmentC788 Specification for Nuclear-Grade Uranyl Nitrate Solution or Cr

8、ystalsC1118C859 Guide for Selecting Components for Wavelength-Dispersive X-Ray Fluorescence (XRF) SystemsTerminologyRelating to Nuclear Materials (Withdrawn 2011)D1193 Specification for Reagent Water3. Terminology3.1 Definitions:3.1.1 For definitions of terms relating to the nuclear fuel cycle, refe

9、r to Terminology C859.4. Summary of Test Method4.1 A sample of hydrolyzed UF6 (uranyl fluoride) or uranyl nitrate solution is treated with sodium nitrite to reduce oxidizedforms of bromine and chlorine (bromates and chlorates) to their respective halide ions. Addition of silver nitrate precipitates

10、thesilver halides. Spike recoveries can be improved by the addition of potassium iodide causing coprecipitation of the halides. Thehalides are collected on filter paper and are analyzed by X-ray fluorescence using two different crystal/detector systems.5. Significance and Use5.1 The method is design

11、ed to show whether or not the tested materials meet the specifications as given in Specifications C787and C788.1 This test method is under the jurisdiction of ASTM Committee C26 on Nuclear Fuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods of Test.Current edition approved

12、June 1, 2011June 1, 2018. Published June 2011June 2018. Originally approved in 2001. Last previous edition approved in 20062011 asC1508 01 (2011).(2006). DOI: 10.1520/C1508-01R1.10.1520/C1508-18.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at s

13、erviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous versio

14、n. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.Copyright ASTM International

15、, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States16. Interferences6.1 Plastic equipment must be used throughout the method for uranyl fluoride as the hydrofluoric acid in the uranyl fluorideleaches chloride from glassware causing a high bias.6.2 Low recoveries may

16、 occur as the precipitate can be difficult to transfer quantitatively to the filter paper. A surfactant can beadded (optional step) to minimize the adhesion of the precipitate to the walls of the beakers and the funnel.7. Apparatus7.1 X-Ray Spectrometer, see Guide appropriate C1118for the selection

17、of the X-ray Spectrometer.intended use.7.2 Plastic Vacuum Filtration Apparatus, for 47 mm diameter filter paper.7.3 Filter Paper, 0.45 micron, 47 mm diameter.37.4 Beakers, polypropylene, 250 mL.7.5 Stirring Rods, plastic or Teflon.7.6 X-ray Sample Support, Rings. Inner diameter approximately 40 mm.8

18、. Reagents8.1 Purity of ReagentsReagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that allreagents conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where suchspecifications are available.4 Other grade

19、s may be used, provided it is first ascertained that the reagent is of sufficiently high purityto permit its use without lessening the accuracy of the determination.8.2 Purity of WaterUnless otherwise indicated, references to water shall be understood to mean reagent water conforming toSpecification

20、 D1193, Type I.8.3 Ammonium Hydroxide, NH4OH, concentrated, specific gravity 0.90.8.4 Ammonium Hydroxide Solution, 1 + 3 (3.7 M). Dilute 1 part NH4OH with 3 parts water.8.5 Surfactant, bromine and chlorine free.5 (Optional).8.6 Surfactant Solution, 1 + 999. Add 1 mL of surfactant to approximately 1

21、litre of water. (Optional).8.7 Nitric Acid, HNO3, concentrated, specific gravity 1.42.8.8 Nitric Acid Solution, 1 + 999 (0.016 M). Add 1 mL of concentrated HNO3 to approximately 200 mL of water. Add 1 mLof the surfactant (7.68.6). (Optional). Dilute to 1 litre.8.9 Sodium Nitrite, NaNO2.8.10 Sodium N

22、itrite Solution, 2 g/L. Dissolve 1 g of sodium nitrite in water and dilute to 500 mL. Prepare fresh immediatelybefore use.8.11 Silver Nitrate, AgNO3.8.12 Silver Nitrate Solution, 2 g/L. Dissolve 2 g of silver nitrate in water and dilute to 1 litre. Keep away from light in an opaquebottle. The soluti

23、on should be made fresh weekly. Silver is an RCRAlisted hazardous waste. Make up only as much of this solutionas required to minimize excess waste.8.13 Potassium Bromide, KBr.8.14 Bromide Solution, 500 mg Br/L. Dissolve 0.1861 g of KBr (dried at 110C for 1 hour) in water and dilute to 250 mL ina vol

24、umetric flask.8.15 Sodium Chloride, NaCl.8.16 Sodium Chloride Solution, 1000 mg Cl/L. Dissolve 1.648 g NaCl (dried at 110 C for 1 hour ) in water and dilute to 1 litrein a volumetric flask.8.17 Spike Solution, 5 mg Br/L, 100 mg Cl/L. Transfer 10 mL of 500 mg Br /L Br/L solution into a 1 litre volume

25、tric flask bypipette. Transfer 100 mL of 1000 mg Cl /L Cl/L into the flask by pipette. Dilute to volume.3 The last approved version of this historical standard is referenced on www.astm.org.3 The filter must be Cl and Br free. Millipore membrane filter type HABP () has been successfully used. An alt

26、ernate is 15A from S.C.B, BP6, RN86,07130 Soyons France. Any other equivalent is acceptable.4 Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed bythe American Chemical Society, see Analar Stan

27、dards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and NationalFormulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.5 Triton X-100, Rohm and Haas, has been successfully used.C1508 1828.18 Potassium Iodide, KI. (Optional).8.19 Potassium I

28、odide Solution, (Optional), 1g I/L. Dissolve 0.131 g potassium iodide in water and dilute to 100 mL. Thesolution should be prepared weekly.9. Standard Preparation9.1 Pipette the following aliquots of spike solution (from 7.178.17) into polypropylene beakers. 0 mL, 1 mL, 2 mL, 5 mL, 10mL. The aliquot

29、s represent 0g Br, 5g Br, 10g Br, 25g Br, 50g Br and 0g Cl, 100g Cl, 200g Cl, 500g Cl, 1000g Cl.9.2 Add 70 mL water to each beaker.9.3 Follow steps 9.310.3 9.810.8 at the same time as the samples.10. Procedure10.1 Transfer a known aliquot of uranyl fluoride solution (prepared following Test Methods

30、C761) or uranyl nitrate that containsa known amount of uranium, approximately 5 g, with a plastic graduated cylinder into a polypropylene beaker containing 70 mLwater.NOTE 1Recommend cleaning all laboratory equipment with ammonium hydroxide solution (7.48.4) prior to use.10.2 Follow laboratory QA pr

31、actices and run the necessary duplicates, spikes and controls with the samples. Use the solutionprepared in 7.178.17 for the spikes.NOTE 22 mL and 4 mL spike aliquots were found to be reasonable volumes.10.3 Add 0.5 mL of potassium iodide solution to each sample and standard. (Optional step).10.4 Ad

32、d 4 mL of surfactant solution 7.68.6. (Optional step).10.5 Add 10 mL of sodium nitrite solution to each sample and standard. Stir each solution with a dedicated plastic stirring rodand allow to stand for a minimum of 2 minutes.10.6 Slowly and with stirring add 25 mL of the silver nitrate solution. R

33、emove the plastic stirring rods. Heat the solution in awater bath at approximately 80C 6 10C for 11.512 hours.10.7 Remove from the bath. Allow the halides to precipitate overnight. A2A two hour precipitation time has been found to besuccessful, but the user must establish precision and bias based on

34、 the shorter time. The precision and bias data in this standardwere generated using an overnight precipitation.10.8 Filter using 0.45 micron filter paper. Use a plastic vacuum filtration assembly. Use a plastic rod with a rubber policemanto aid the transfer of precipitate to the filter. Use 1 + 999

35、nitric acid solution to wash the precipitate. Dry the filters before countingin the X-ray.XRF system.10.9 Place the filters on X-ray sample support rings and tape or glue in place.10.10 Analyze using the X-ray.XRF system following manufacturers guidelines and laboratory specific procedures.11. Instr

36、ument Calibration11.1 Follow the manufacturers instructions for setting up the instrument to achieve an inert gas environment and to obtain thefollowing instrument parameters. (See Table 1).11.2 Run the standards and construct a calibration curve using the instruments software or by manually plottin

37、g the curve usinglinear chart paper.11.3 Run the samples. Determine the weight of Br and Cl present on the filter papers from the calibration curves. Calculate theconcentration of Br and Cl in the samples by following Section 1112.TABLE 1 Suggested X-Ray SettingsBromine ChlorineLine Ka KaLine Ka KaC

38、rystal LiF 200(Lithium fluoride)PE (Tetrakis(hydroxymethyl)-methane)Detector Scintillation FlowOrder 1 1X-ray tube Rhodium RhodiumTube voltage (kV) 45 45Tube Amperage(mA)45 75Counting Time (s) 40 40C1508 18312. Calculation12.1 Calculate the halide content as follows:Halide,g/guranium basis5A31000B3C

39、where:A 5 micrograms halide from the calibration curve,1000 5 conversion factor, litres to millilitres,B 5 sample aliquot from 9.1, in millitres, andC 5 uranium concentration of sample solution, in g/L.13. Precision and Bias13.1 Uranium Hexafluoride Data:13.1.1 Precision in UF6 SamplesThe single lab

40、oratory precision for the average of multiple determinations is given in Table2. The data for laboratory A were collected using a rhodium X-ray tube and a LiF200 crystal for bromine and a PE crystal forchlorine. Potassium iodide (optional 9.310.3) was added to the samples in laboratory A. The result

41、s were obtained over a 3 monthperiod by two technicians. The results for laboratory B was obtained by 1 technician over a 1 year period. Potassium iodide wasnot added to Laboratory B samples. The precision is given in Table 2.13.1.2 Bias in UF6 SamplesNo standard material certified for bromine and c

42、hlorine in UF6 is available. Therefore bias cannotbe determined. To determine lower bound bias indications uranyl fluoride solutions were spiked with NIST SRM. The uncertaintyof the NIST traceable standard is less than the uncertainty of the procedure. The data for Laboratory A were collected over a

43、 3month period by two technicians. Potassium iodide was added to laboratory A samples. The result data for Laboratory B wereobtained over a 1 year period by 1 technician. No potassium iodide was added to laboratory B samples. The mean minus theprepared values are an indication of the bias. The relat

44、ive differences are given in Table 3. The relative difference is(mean-known)/known 100 %.13.2 Uranyl Nitrate Data:13.2.1 Precision in Uranyl Nitrate SamplesThe result data were collected in 1 day by 1 technician. The precision is given inTable 4. No potassium iodide (optional 9.310.3) was added to t

45、he uranyl nitrate samples.13.2.2 Bias in Uranyl Nitrate SamplesThe bias should be equivalent to the bias in UF6 samples.13.3 The supporting data for Tables 2-4 are available from ASTM headquarters.14. Keywords14.1 bromine; chlorine; uranium hexafluoride; X-ray fluorescence; XRFTABLE 2 Within Laborat

46、ory Precision For UF6Laboratory Halide Concentration(g halide/g U)StandardDeviation(g halide/g U)Number ofDeterminationsA Bromine 0.44 0.06 10A Bromine 3.1 0.2 9B Bromine 5.1 0.7 109A Chlorine 2.4 2.1 9A Chlorine 66 6 8A Chlorine 185 19 9B Chlorine 48 5 107C1508 184ASTM International takes no positi

47、on respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility

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49、nternational Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained b