ASTM C799-2012 Standard Test Methods for Chemical Mass Spectrometric Spectrochemical Nuclear and Radiochemical Analysis of Nuclear-Grade Uranyl Nitrate Solutions 《核纯级硝酸铀酰溶液的化学 质谱 光.pdf

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1、Designation:C79999(Reapproved2005) Designation: C799 12Standard Test Methods forChemical, Mass Spectrometric, Spectrochemical, Nuclear,and Radiochemical Analysis of Nuclear-Grade Uranyl NitrateSolutions1This standard is issued under the fixed designation C799; the number immediately following the de

2、signation indicates the year 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 These test methods cover pro

3、cedures for the chemical, mass spectrometric, spectrochemical, nuclear, and radiochemicalanalysis of nuclear-grade uranyl nitrate solution to determine compliance with specifications.1.2 The analytical procedures appear in the following order:SectionsDetermination of Uranium 7Specific Gravity by Pyc

4、nometry 15-20Free Acid by Oxalate Complexation 21-27Determination of Thorium 28Determination of Chromium 29Determination of Molybdenum 30Halogens Separation by Steam Distillation 31-35Fluoride by Specific Ion Electrode 36-42Halogen Distillate Analysis: Chloride, Bromide, and Iodide byAmperometric Mi

5、crotitrimetry43Determination of Chloride and Bromide 44Determination of Sulfur by X-Ray Fluorescence 45Sulfate Sulfur by (Photometric) Turbidimetry 46Phosphorus by the Molybdenum Blue (Photometric) Method 54-61Silicon by the Molybdenum Blue (Photometric) Method 62-69Carbon by Persulfate Oxidation-Ac

6、id Titrimetry 70Conversion to U3O871-74Boron by Emission Spectrography 75-81Impurity Elements by Spark Source Mass Spectrography 82Isotopic Composition by Thermal Ionization Mass Spectrometry 83Uranium-232 by Alpha Spectrometry 84-90Total Alpha Activity by Direct Alpha Counting 91-97Fission Product

7、Activity by Beta Counting 98-104Entrained Organic Matter by Infrared Spectrophotometry 105Fission Product Activity by Gamma Counting 106Determination of Arsenic 107Determination of Impurities for the EBC Calculation 108Determination of Technetium 99 109Determination of Plutonium and Neptunium 1101.3

8、 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use. Specific precaution

9、ary statements are given in Section 5.2. Referenced Documents2.1 ASTM Standards:2C696 Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Uranium DioxidePowders and Pellets1These test methods are under the jurisdiction of ASTM Committee C26 on Nuclear Fuel Cy

10、cle and are the direct responsibility of Subcommittee C26.05 on Methodsof Test.Current edition approved June 1, 2005. Published October 2005. Originally approved in 1975. Last previous edition approved in 1999 as C79999e1. DOI:10.1520/C0799-99R05.Current edition approved Jan. 1, 2012. Published Febr

11、uary 2012. Originally approved in 1975. Last previous edition approved in 2005 as C799 99(2005). DOI:10.1520/C0799-12.2For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to

12、the standards Document Summary page on the ASTM website.1This 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 version. Becauseit may not be technically possible to adequately depict all changes

13、 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, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, Unite

14、d States.C761 Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of UraniumHexafluorideC788 Specification for Nuclear-Grade Uranyl Nitrate Solution or CrystalsC1219 Test Methods for Arsenic in Uranium HexafluorideC1233 Practice for Determining Equival

15、ent Boron Contents of Nuclear MaterialsC1254 Test Method for Determination of Uranium in Mineral Acids by X-Ray FluorescenceC1267 Test Method for Uranium by Iron (II) Reduction in Phosphoric Acid Followed by Chromium (VI) Titration in thePresence of VanadiumC1287 Test Method for Determination of Imp

16、urities in Nuclear Grade Uranium Compounds by Inductively Coupled PlasmaMass SpectrometryC1295 Test Method for Gamma Energy Emission from Fission Products in Uranium Hexafluoride and Uranyl Nitrate SolutionC1296 Test Method for Determination of Sulfur in Uranium Oxides and Uranyl Nitrate Solutions b

17、y X-Ray Fluorescence(XRF)C1380 Test Method for the Determination of Uranium Content and Isotopic Composition by Isotope Dilution MassSpectrometryC1413 Test Method for Isotopic Analysis of Hydrolyzed Uranium Hexafluoride and Uranyl Nitrate Solutions by ThermalIonization Mass SpectrometryC1561 Guide f

18、or Determination of Plutonium and Neptunium in Uranium Hexafluoride and U-Rich Matrix by AlphaSpectrometryD1193 Specification for Reagent WaterE12 Terminology Relating to Density and Specific Gravity of Solids, Liquids, and GasesE60 Practice for Analysis of Metals, Ores, and Related Materials by Spe

19、ctrophotometry2.2 American Chemical Society Specification:Reagent Chemicals32.3 Other Documents:ISO 7097 Determination of Uranium in Uranium Product Solutions and Solids with Cerium IV Oxidation Titrimetric Method43. Significance and Use3.1 Uranyl nitrate solution is used as a feed material for conv

20、ersion to the hexafluoride as well as for direct conversion to theoxide. In order to be suitable for this purpose, the material must meet certain criteria for uranium content, isotopic composition,acidity, radioactivity, and impurity content. These methods are designed to show whether a given materi

21、al meets the specificationsfor these items described in Specification C788.3.1.1 An assay is performed to determine whether the material has the specified uranium content.3.1.2 Determination of the isotopic content of the uranium is made to establish whether the effective fissile content is inaccord

22、ance with the purchasers specifications.3.1.3 Acidity, organic content, and alpha, beta, and gamma activity are measured to establish that they do not exceed theirmaximum limits.3.1.4 Impurity content is determined to ensure that the maximum concentration limit of certain impurity elements is notexc

23、eeded. Impurity concentrations are also required for calculation of the equivalent boron content (EBC), and the total equivalentboron content (TEBC).4. Reagents4.1 Purity of ReagentsReagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that allreagents shall

24、conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, wheresuch specifications are available.3Other grades may be used, provided it is first ascertained that the reagent is of sufficiently highpurity to permit its use without lessening the accuracy o

25、f the determination.4.2 Purity of WaterUnless otherwise indicated, references to water shall be understood to mean reagent water conforming toSpecification D1193.5. Safety Precautions5.1 Use of this standard does not relieve the user of the obligation to be aware of and to conform to all health and

26、safetyrequirements.5.2 The user should also be cognizant of and adhere to all federal, state, and local regulations for processing, shipping, or inany way using uranyl nitrate solutions.3Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For sugge

27、stions on the testing of reagents not listed bythe American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and NationalFormulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.4Available from American Nat

28、ional Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036, http:/www.ansi.org.C799 1226. Sampling6.1 Criteria for sampling this material are given in Specification C788.DETERMINATION OF URANIUM7. Scope7.1 Uranium can be determined using iron (II) reduction and dichromate titrat

29、ion. Test Method C1267 can be used.7.2 Uranium can also be determined using cerium (IV) oxidation titrimetry. ISO 7097 Test Method can be used.7.3 Uranium can also be determined by X-Ray Fluorescence using Test Method C1254.7.4 Previous sections have been deleted.URANIUM BY IGNITION GRAVIMETRY8. Sco

30、pe8.1 This test method covers the determination of uranium in nuclear-grade uranyl nitrate solution. Appropriate size samplealiquots are chosen to obtain 5 to 10 g of U3O8.9. Summary of Test Method9.1 The uranyl nitrate solution is evaporated to dryness, ignited to U3O8, and weighed. Corrections are

31、 made for any impuritiespresent (1, 2).10. Interferences10.1 The weight of U3O8is corrected for the nonvolatile impurities present as determined by spectrographic analysis.10.2 Volatile anions that are difficult to decompose require an extended ignition period.11. Apparatus11.1 Heat Lamp, infrared.1

32、1.2 Hot Plate.11.3 Muffle Furnace.12. Procedure12.1 Transfer a weighed portion of uranyl nitrate solution containing 5 to 10 g of uranium into a preweighed platinum dish andadd 2 drops of HF (48 %).12.2 Position the dish under the heat lamp and evaporate the solution to dryness.12.3 Place the dish o

33、n a hot plate with a surface temperature of about 300C and heat until most of the nitrate has decomposed.12.4 Transfer the dish to a muffle furnace and ignite for2hat900C.12.5 Remove the dish to a desiccator and allow to cool to room temperature.12.6 Weigh the dish; then repeat 12.4-12.6 until a con

34、stant weight is obtained.13. Calculation13.1 Calculate the uranium content as follows:Uranium, g/g 5 B 2 C!/A! D (1)where:A = sample, g,B =U3O8obtained, g,C = impurity-element oxides, g, andD = gravimetric factor, grams of uranium/grams of U3O8(varies according to uranium enrichment).14. Precision14

35、.1 The limit of error at the 95 % confidence level for a single determination is 60.03 %.SPECIFIC GRAVITY BY PYCNOMETRY15. Scope15.1 This test method covers the determination of the specific gravity of a solution of uranyl nitrate to 60.0004.16. Summary of Test Method16.1 A known volume of the solut

36、ion adjusted at a controlled temperature is weighed and compared to the weight of watermeasured in the same container (Terminology E12).C799 12317. Apparatus17.1 Volumetric Flasks, 50-mL, Class A.17.2 Water Bath, temperature controlled to 60.1C at a temperature slightly above normal room temperature

37、, and provided withclips for holding volumetric flasks.18. Procedure18.1 Weigh the clean, dry volumetric flask and its stopper to the nearest 0.1 mg.18.2 Fill the volumetric flask with the uranyl nitrate solution to a point close to the volume mark, using a thinstemmed funneland a glass dropper.18.3

38、 Place the stoppered volumetric flask in the water bath for 30 min.18.4 Use a finely drawn glass dropper to adjust the liquid volume to the mark.18.5 Leave the flask in the water bath an additional 10 min to make sure that the bath temperature has been reached.18.6 Dry and weigh the flask to the nea

39、rest 0.1 mg.18.7 Repeat 18.2-18.6 using boiled and cooled distilled water instead of the uranyl nitrate solution.19. Calculation19.1 Very accurate determinations of specific gravity require that vacuo corrections be made, but if a median correction figurein terms of grams per grams of sample is appl

40、ied to the solution weights in all cases the resulting error will not exceed 0.05 %.Sp gr 5B 2 A 1 0.0007 B 2 A!C 2 A 1 0.0010 C 2 A!(2)where:B = sample plus flask in air, g,A = flask in air, g,C = water plus flask in air, g,0.0007 g/g = correction factor applicable for densities of 1.3 to 1.5, and0

41、.0010 g/g = correction factor for water.20. Precision20.1 The limit of error at the 95 % level for a single determination is 60.03 %.FREE ACID BY OXALATE COMPLEXATION21. Scope21.1 This test method covers the determination of the free acid content of uranyl nitrate solutions that may contain a ratio

42、ofup to 5 moles of acid to 1 mole of uranium.22. Summary of Test Method22.1 To a diluted solution of uranyl nitrate, solid, pulverized potassium oxalate is added until a pH of about 4.7 is reached. Thesolution is then titrated with standard NaOH solution by the delta pH method to obtain the inflecti

43、on point (3).23. Apparatus23.1 pH Meter, with glass and calomel electrodes.23.2 Buret, Class A, 50-mL.24. Reagents24.1 Nitric Acid (2.0 N)Dilute 130 mL of HNO3(sp gr 1.42) to 1 L with water. Standardize with sodium hydroxide solution(see 24.3).24.2 Potassium Oxalate (K2C2O4H2O), crystals.24.3 Sodium

44、 Hydroxide Solution (0.3 N)Dissolve 12.0 g of NaOH in 1 Lof water. Standardize with acid potassium phthalate.525. Procedure25.1 Transfer a 5-mL sample aliquot into a 250-mL beaker.25.2 Add 100 mL of distilled water or such volume that the uranium concentration will be between 7 and 50 g/L.25.3 Add a

45、 spike of sufficient 2.0 N standard HNO3to make the sample definitely acid if the sample is neutral or acid deficient.25.4 Add pulverized K2C2O4H2O slowly and with constant stirring until a pH of 4.7 to 4.9 is reached.5NBS SRM 84h.C799 12425.5 Immerse the titration beaker in an ice bath. (Titrations

46、 made at room temperature are possible but are less sharp.)25.6 Titrate with 0.3 N NaOH using 0.20-mL increments and determine the inflection point by the delta pH or “analytical”method.NOTE 1This test method of locating the end point depends on the fact that the second derivative D2pH/Dvol2is zero

47、at the point where the slopeDpH/Dvol is a maximum.26. Calculation26.1 Calculate the free acid normality, N, as follows:N 5 A 3 NB2 C 3 NA!/5 (3)where:A = NaOH solution used in the titration, mLNB= normality of the NaOH solution,C = HNO3solution used in the spike, mL, andNA= normality of HNO3solution

48、.NOTE 2Negative values of free acid indicate an acid deficiency.27. Precision27.1 The limit of error at the 95 % confidence level for a single determination is 63%.DETERMINATION OF THORIUM28. Scope28.1 The determination of thorium by the arsenazo (III) (photometric) method has been discontinued, (se

49、e C799-93).28.2 As an alternative, thorium can be determined using Inductively Coupled Plasma Mass Spectrometry (ICP-MS). See TestMethod C1287.28.3 Previous sections have been deleted.DETERMINATION OF CHROMIUM29. Scope29.1 The determination of chromium by the diphenyl carbazide method has been discontinued, (see C799-93).29.2 As an alternative, chromium can be determined using inductively coupled plasma atomic emission spectrometry(ICP-AES). Test Method C761 can be used providing a transformation to U3O8so described hereafter in sections 117120.Adirectconve