1、Designation: C1022 05 (Reapproved 2010)1C1022 17Standard Test Methods forChemical and Atomic Absorption Analysis of Uranium-OreConcentrate1This standard is issued under the fixed designation C1022; the number immediately following the designation indicates the year oforiginal adoption or, in the cas
2、e 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 NOTESections 1.4 and 7.2 were editorially corrected in August 2010.1. Scope1.1 These test methods cov
3、er procedures for the chemical and atomic absorption analysis of uranium-ore concentrates todetermine compliance with the requirements prescribed in Specification C967.1.2 The analytical procedures appear in the following order:SectionsUranium by Ferrous Sulfate ReductionPotassium DichromateTitrimet
4、ry 9Nitric Acid-Insoluble Uranium 10 to 18Extractable Organic Material 19 to 26Determination of Arsenic 27Carbonate by CO2 Gravimetry 28 to 34Fluoride by Ion-Selective Electrode 35 to 42Halides by Volhard Titration 43 to 50Moisture by Loss of Weight at 110C 51 to 57Phosphorus by Spectrophotometry 58
5、 to 66Phosphorus by Spectrophotometry 52 to 60Determination of Silicon 67Determination of Silicon 61Determination of Thorium 68Determination of Thorium 62Calcium, Iron, Magnesium, Molybdenum, Titanium, and Vana-dium by Atomic Absorption Spectrophotometry 69 to 78Calcium, Iron, Magnesium, Molybdenum,
6、 Titanium, and Vana-dium by Atomic Absorption Spectrophotometry 63 to 72Potassium and Sodium by Atomic AbsorptionSpectrophotometry 79 to 88Potassium and Sodium by Atomic AbsorptionSpectrophotometry 73 to 82Boron by Spectrophotometry 89 to 98Boron by Spectrophotometry 83 to 921.3 The values stated in
7、 SI units are to be regarded as standard. No other units of measurement are included in this standard.Thevalues given in parentheses are for information only.1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user
8、 of this standard to establish appropriate safety safety, health, and healthenvironmental practices and determine theapplicability of regulatory limitations prior to use. A specific precautionary statement is given in Section 7.1.5 This international standard was developed in accordance with interna
9、tionally 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) Committee.1 These test methods are under the jurisdiction of A
10、STM Committee C26 on Nuclear Fuel Cycle and are the direct responsibility of Subcommittee C26.05 on Methodsof Test.Current edition approved June 1, 2010Nov. 1, 2017. Published June 2010November 2017. Originally approved in 1984. Last previous edition approved in 20052010 asC1022 05.C1022 05 (2010)1.
11、 DOI: 10.1520/C1022-05R10E1.10.1520/C1022-17.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 version. Becauseit may not be technically possible to adequately depict all changes accurately,
12、 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. United States12.
13、Referenced Documents2.1 ASTM Standards:2C761 Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of UraniumHexafluorideC859 Terminology Relating to Nuclear MaterialsC967 Specification for Uranium Ore ConcentrateC1110 Test Method for Determining Element
14、s in Waste Streams by Inductively Coupled Plasma-Atomic Emission Spectroscopy(Withdrawn 2014)3C1219 Test Methods for Arsenic in Uranium Hexafluoride (Withdrawn 2015)3C1254 Test Method for Determination of Uranium in Mineral Acids by X-Ray FluorescenceC1267 Test Method for Uranium by Iron (II) Reduct
15、ion in Phosphoric Acid Followed by Chromium (VI) Titration in thePresence of VanadiumC1287 Test Method for Determination of Impurities in Nuclear Grade Uranium Compounds by Inductively Coupled PlasmaMass SpectrometryC1347 Practice for Preparation and Dissolution of Uranium Materials for AnalysisC184
16、3 Test Method for Determining Moisture Content in Uranium-Ore ConcentrateD1193 Specification for Reagent WaterE60 Practice for Analysis of Metals, Ores, and Related Materials by Spectrophotometry3. Terminology3.1 DefinitionsFor definitions of terms used in these test methods, refer to Terminology C8
17、59.4. Significance and Use4.1 The test methods in this standard are designed to show whether a given material meets the specifications prescribed inSpecification C967.4.2 Because of the variability of matrices of uranium-ore concentrate and the lack limited availability of suitable reference orcalib
18、ration materials, the precision and bias of these test methods should be established by each individual laboratory that will usethem. The precision and bias statements given for each test method are those reported by various laboratories and can be used asa guideline.4.3 Instrumental test methods su
19、ch as X-ray fluorescence and emission spectroscopy can be used for the determination of someimpurities where such equipment is available.5. Interferences5.1 Interferences are identified in the individual test methods.5.2 Ore concentrates are of a very variable nature; therefore, all interferences ar
20、e very difficult to predict. The individual usershould verify the applicability of each procedure for specific ore concentrates.6. Reagents6.1 Purity of ReagentsReagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that allreagents shall conform to the specif
21、ications of the Committee on Analytical Reagents of the American Chemical Society, wheresuch specifications are available.4 Other grades may be used, provided it is first ascertained that the reagent is of sufficiently highpurity to permit its use without lessening the accuracy of the determination.
22、6.2 Purity of WaterUnless otherwise indicated, references to water shall be understood to mean reagent water conforming totype I water in Specification D1193.7. Precautions7.1 Proper precautions should be taken to prevent inhalation or ingestion of uranium during sample preparation and anysubsequent
23、 sample analysis.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.3 The last approved version of this historic
24、al standard is referenced on www.astm.org.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 Standards for Laboratory Chemicals, BDH Ltd., Poole, D
25、orset, U.K., and the United States Pharmacopeia and NationalFormulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.C1022 1727.2 Hydrofluoric acid is a highly corrosive acid that can severely burn skin, eyes, and mucous membranes. Hydrofluoric acidis similar to other acids in that the i
26、nitial extent of a burn depends on the concentration, the temperature, and the duration of contactwith the acid. Hydrofluoric acid differs from other acids because the fluoride ion readily penetrates the skin, causing destructionof deep tissue layers. Unlike other acids that are rapidly neutralized,
27、 hydrofluoric acid reactions with tissue may continue for daysif left untreated. Due to serious consequences of hydrofluoric acid burns, prevention of exposure or injury of personnel is theprimary goal. Utilization of appropriate laboratory controls (hoods) and wearing adequate personal protective e
28、quipment to protectfrom skin and eye contact Familiarization and compliance with the Safety Data Sheet is essential.7.3 Chloroform is a dangerous chemical causing acute toxicity with repeated inhalation, dermal, or oral exposure. Many healthhazards are associated with exposure to chloroform includin
29、g its potential to cause cancer. Familiarization and compliance withthe Safety Data Sheet is essential.8. Sampling8.1 Collect samples in accordance with Specification C967.8.2 Special requirements for subsampling are given in the individual test methods.URANIUM BY FERROUS SULFATEREDUCTIONPOTASSIUM D
30、ICHROMATE TITRIMETRY9. Scope9.1 This test method covers the determination of uranium in uranium-ore concentrates. This test method was discontinued inJanuary 2002 and replaced with Test Method C1267.9.2 The uranium content of the sample may also be determined using Test Method C1254. The users labor
31、atory must establishand document method performance.NOTE 1Dissolution of UOC samples may be achieved using the techniques or combination of techniques described in C1347 The laboratory mustvalidate the performance of C1347 using characterized UOC samples. If C1347 methods are not suitable for UOC sa
32、mple dissolution, the user mayestablish and document applicable dissolution methods.9. Scope9.1 This test method covers the determination of uranium in uranium-ore concentrates. This test method was discontinued inJanuary 2002 and replaced with Test Method C1267.9.2 The uranium content of the sample
33、 may also be determined using Test Method C1254. The users laboratory must establishand document method performance.NOTE 1Dissolution of UOC samples may be achieved using the techniques or combination of techniques described in Practice C1347. The laboratorymust validate the performance of Practice
34、C1347 using characterized UOC samples. If Practice C1347 methods are not suitable for UOC sampledissolution, the user may establish and document applicable dissolution methods.NITRIC ACID-INSOLUBLE URANIUM10. Scope10.1 This test method covers the determination of that quantity of uranium in uranium-
35、ore concentrate that is not soluble innitric acid.10. Scope10.1 This test method covers the determination of that quantity of uranium in uranium-ore concentrate that is not soluble innitric acid.11. Summary of Test Method11.1 A sample of ore concentrate is digested in 10 M nitric acid at 95 to 100C
36、for 1 h. The slurry is filtered and the residuewashed with 1 M nitric acid until the filtrate gives a negative test for uranium. The washed residue is then dried and ignited at 10006 25C for 1 h. The uranium content is determined on the ignited residue by spectrophotometry.12. Interference12.1 At th
37、e specification limit for nitric acid insoluble uranium usually established for uranium-ore concentrates, interferenceeffects are insignificant.13. Apparatus13.1 Digestion Flask, 500-mL, with side entry tube and attached reservoir.13.2 Stirring Apparatus, with sleeve-type stirrer.C1022 17313.3 Heati
38、ng Mantle, 250-W, controlled by a variable transformer.13.4 Bchner Funnel.13.5 Porcelain Crucibles, 40-mL.13.6 Muffle Furnace.13.7 Filter Paper, ashless of medium porosity.porosity, and a medium flow rate with a particle retention of 8 m has been foundto be suitable.13.8 Spectrophotometer, with 1-cm
39、 cells that are in accordance with Practice E60.14. Reagents14.1 Nitric Acid (10 M)Dilute 62.5 mL of HNO3 (sp gr 1.42) to 100 mL with distilled water.14.2 Nitric Acid (1 M)Dilute 62.5 mL of HNO3 (sp gr 1.42) to 1 L with distilled water.14.3 Sodium Hydroxide (100 g/L)Dissolve 10 g of NaOH in 100 mL o
40、f water.14.4 Hydrogen Peroxide (H2O2, 30 %).14.5 Hydrochloric Acid (HCl, sp gr 1.19).14.6 Hydrofluoric Acid (HF, 48 %).14.7 Sulfuric Acid (9 M)Add 500 mL H2SO4 (sp gr 1.84) to 500 mL of iced water with constant stirring. Cool and dilute to1 L with water.15. Procedure15.1 Weigh a 50.0 6 0.1-g sample
41、directly into the digestion flask.15.2 Place the flask in the heating mantle and adjust the support ring so that the joints of the flask and sleeve stirrer are engaged,and the stirrer blades turn freely but just clear the bottom of the flask.15.3 Transfer 95 mL of 10 M nitric acid to a 250-mL beaker
42、 and heat between 95 to 100C.15.4 Slowly transfer the heated nitric acid solution to the digestion flask through the entry side tube with the stirrer turning.NOTE 2The stirrer is started before the acid is added to prevent material from sticking to the flask.15.5 Align a thermometer in such a manner
43、 that the mercury chamber Adjust the thermometer so that the bulb of thethermometer is immersed in the stirring slurry, but adequately clears the turning stirrer blades.15.6 Quickly bring the sample to 97C and digest between 95 to 100C for 1 h while stirring. (Measure the 1-h digestion timeafter the
44、 temperature of the slurry has reached 97C.)15.7 Turn off the variable transformer, but allow the stirrer to continue turning.15.8 Remove the thermometer and carefully rinse with water all slurry that adheres to it.15.9 Wipe the immersed portion of the thermometer with one fourth of a circle of filt
45、er paper and transfer the paper to a preparedBchner funnel fitted with a filter paper.15.10 Add 10 mL of paper pulp to the slurry and continue stirring for about 5 min.15.11 Turn off the stirrer, then lower the flask and mantle.15.12 Carefully wash the slurry that adheres to the stirrer shaft and bl
46、ades into the flask with water.15.13 Wipe the shaft and blades with one fourth of a circle of filter paper and transfer the filter paper to the Bchner funnel.15.14 Filter the slurry through the Bchner funnel and wash contents of the flask into the funnel.15.15 Wash the residue with 1 M nitric acid u
47、ntil a 10-mL portion of the filtrate shows no detectable yellow color when madebasic with sodium hydroxide and after a few drops of H2O2 (30 %) have been added as a color developer.15.16 Wash the residue several times with water after a negative test is obtained.15.17 Draw air through the filter unt
48、il the residue and filter pad are dry.15.18 Scrape the residue and paper into a preignited (1000C) tared 40-mL crucible, place on a hot plate and slowly char offthe organic material.15.19 Ignite the residue for 1 h at 1000C in a muffle furnace.15.20 Cool the crucible in a desiccator and weigh.C1022
49、17415.21 Calculate the percentage of solids in accordance with 17.1. If the percentage of solids (insoluble residue) is greater than0.1 %, grind and mix the residue and determine the total milligrams of uranium in the residue by the photometric procedure in 16.1 16.10.NOTE 3If the percentage of solids (insoluble residue) is greater than 0.1 %, grind and mix the residue and determine the total milligrams of uraniumin the residue by the photometric procedure in 16.1 16.10.16. Photometric Procedure for Uranium16.1 Transfer the ground, blended
