1、Designation: C1022 05 (Reapproved 2010)1Standard 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 case of rev
2、ision, 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.1NOTESections 1.4 and 7.2 were editorially corrected in August 2010.1. Scope1.1 These test methods cover proced
3、ures for the chemicaland atomic absorption analysis of uranium-ore concentrates todetermine compliance with the requirements prescribed inSpecification C967.1.2 The analytical procedures appear in the following order:SectionsUranium by Ferrous Sulfate ReductionPotassium DichromateTitrimetry 9Nitric
4、Acid-Insoluble Uranium 10 to 18Extractable Organic Material 19 to 26Determination of Arsenic 27Carbonate by CO2Gravimetry 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 to 66Determ
5、ination of Silicon 67Determination of Thorium 68Calcium, Iron, Magnesium, Molybdenum, Titanium, and Vana-dium by Atomic Absorption Spectrophotometry 69 to 78Potassium and Sodium by Atomic AbsorptionSpectrophotometry 79 to 88Boron by Spectrophotometry 89 to 981.3 The values stated in SI units are to
6、be regarded asstandard. No other units of measurement are included in thisstandard.1.4 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-priate safety and health practices and
7、determine the applica-bility of regulatory limitations prior to use. A specific precau-tionary statement is given in Section 7.2. Referenced Documents2.1 ASTM Standards:2C761 Test Methods for Chemical, Mass Spectrometric,Spectrochemical, Nuclear, and Radiochemical Analysis ofUranium HexafluorideC859
8、 Terminology Relating to Nuclear MaterialsC967 Specification for Uranium Ore ConcentrateC1110 Practice for Sample Preparation for X-Ray EmissionSpectrometric Analysis of Uranium in Ores Using theGlass Fusion or Pressed Powder MethodC1219 Test Methods for Arsenic in Uranium HexafluorideC1254 Test Met
9、hod for Determination of Uranium in Min-eral Acids by X-Ray FluorescenceC1267 Test Method for Uranium by Iron (II) Reduction inPhosphoric Acid Followed by Chromium (VI) Titration inthe Presence of VanadiumC1287 Test Method for Determination of Impurities inNuclear Grade Uranium Compounds by Inductiv
10、elyCoupled Plasma Mass SpectrometryC1347 Practice for Preparation and Dissolution of UraniumMaterials for AnalysisD1193 Specification for Reagent WaterE60 Practice for Analysis of Metals, Ores, and RelatedMaterials by Molecular Absorption Spectrometry3. Terminology3.1 DefinitionsFor definitions of t
11、erms used in these testmethods, refer to Terminology C859.4. Significance and Use4.1 The test methods in this standard are designed to showwhether a given material meets the specifications prescribed inSpecification C967.4.2 Because of the variability of matrices of uranium-oreconcentrate and the la
12、ck of suitable reference or calibration1These test methods are under the jurisdiction of ASTM Committee C26 onNuclear Fuel Cycle and are the direct responsibility of Subcommittee C26.05 onMethods of Test.Current edition approved June 1, 2010. Published June 2010. Originallyapproved in 1984. Last pre
13、vious edition approved in 2005 as C1022 05. DOI:10.1520/C1022-05R10E1.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM
14、 website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.materials, the precision and bias of these test methods shouldbe established by each individual laboratory that will use them.The precision and bias statements given for each t
15、est methodare those reported by various laboratories and can be used as aguideline.4.3 Instrumental test methods such as X-ray fluorescenceand emission spectroscopy can be used for the determination ofsome impurities where such equipment is available.5. Interferences5.1 Interferences are identified
16、in the individual test meth-ods.5.2 Ore concentrates are of a very variable nature; therefore,all interferences are very difficult to predict. The individualuser should verify the applicability of each procedure forspecific ore concentrates.6. Reagents6.1 Purity of ReagentsReagent grade chemicals sh
17、all beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.3Other grades may beused, provided it is first ascertained that t
18、he reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.6.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean reagent water conformingto Specification D1193.7. Precautions7.1 Proper precautions should be ta
19、ken to prevent inhalationor ingestion of uranium during sample preparation and anysubsequent sample analysis.7.2 Hydrofluoric acid is a highly corrosive acid that canseverely burn skin, eyes, and mucous membranes. Hydrofluo-ric acid is similar to other acids in that the initial extent of aburn depen
20、ds on the concentration, the temperature, and theduration of contact with the acid. Hydrofluoric acid differsfrom other acids because the fluoride ion readily penetrates theskin, causing destruction of deep tissue layers. Unlike otheracids that are rapidly neutralized, hydrofluoric acid reactionswit
21、h tissue may continue for days if left untreated. Due toserious consequences of hydrofluoric acid burns, prevention ofexposure or injury of personnel is the primary goal. Utilizationof appropriate laboratory controls (hoods) and wearing ad-equate personal protective equipment to protect from skin an
22、deye contact is essential.8. Sampling8.1 Collect samples in accordance with Specification C967.8.2 Special requirements for subsampling are given in theindividual test methods.URANIUM BY FERROUS SULFATEREDUCTIONPOTASSIUM DICHROMATETITRIMETRY9. Scope9.1 This test method covers the determination of ur
23、anium inuranium-ore concentrates. This test method was discontinuedin January 2002 and replaced with Test Method C1267.9.2 The uranium content of the sample may also be deter-mined using Test Method C1254. The users laboratory mustestablish and document method performance.NOTE 1Dissolution of UOC sa
24、mples may be achieved using thetechniques or combination of techniques described in C1347 The labora-tory must validate the performance of C1347 using characterized UOCsamples. If C1347 methods are not suitable for UOC sample dissolution,the user may establish and document applicable dissolution met
25、hods.NITRIC ACID-INSOLUBLE URANIUM10. Scope10.1 This test method covers the determination of thatquantity of uranium in uranium-ore concentrate that is notsoluble in nitric acid.11. Summary of Test Method11.1 A sample of ore concentrate is digested in 10 M nitricacid at 95 to 100C for 1 h. The slurr
26、y is filtered and the residuewashed with 1 M nitric acid until the filtrate gives a negativetest for uranium. The washed residue is then dried and ignitedat 1000 6 25C for 1 h. The uranium content is determined onthe ignited residue by spectrophotometry.12. Interference12.1 At the specification limi
27、t for nitric acid insolubleuranium usually established for uranium-ore concentrates,interference effects are insignificant.13. Apparatus13.1 Digestion Flask, 500-mL, with side entry tube andattached reservoir.13.2 Stirring Apparatus, with sleeve-type stirrer.13.3 Heating Mantle, 250-W, controlled by
28、 a variable trans-former.13.4 Bchner Funnel.13.5 Porcelain Crucibles, 40-mL.13.6 Muffle Furnace.13.7 Filter Paper,4of medium porosity.13.8 Spectrophotometer, with 1-cm cells that are in accor-dance with Practice E60.14. Reagents14.1 Nitric Acid (10 M)Dilute 62.5 mL of HNO3(sp gr1.42) to 100 mL with
29、distilled water.3Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United S
30、tates Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.4Whatman brand No. 40 or its equivalent has been found suitable.C1022 05 (2010)1214.2 Nitric Acid (1 M)Dilute 62.5 mL of HNO3(sp gr1.42) to 1 L with distilled water.14.3 Sodium Hydroxide (100 g/L)Disso
31、lve 10 g of NaOHin 100 mL of 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 diluteto 1 L with water.15. Procedure15.1 Wei
32、gh a 50.0 6 0.1-g sample directly into the diges-tion flask.15.2 Place the flask in the heating mantle and adjust thesupport ring so that the joints of the flask and sleeve stirrer areengaged, and the stirrer blades turn freely but just clear thebottom of the flask.15.3 Transfer 95 mL of 10 M nitric
33、 acid to a 250-mL beakerand heat between 95 to 100C.15.4 Slowly transfer the heated nitric acid solution to thedigestion flask through the entry side tube with the stirrerturning.NOTE 2The stirrer is started before the acid is added to preventmaterial from sticking to the flask.15.5 Align a thermome
34、ter in such a manner that the mercurychamber of the thermometer is immersed in the stirring slurry,but adequately clears the turning stirrer blades.15.6 Quickly bring the sample to 97C and digest between95 to 100C for 1 h while stirring. (Measure the 1-h digestiontime after the temperature of the sl
35、urry has reached 97C.)15.7 Turn off the variable transformer, but allow the stirrerto continue turning.15.8 Remove the thermometer and carefully rinse withwater all slurry that adheres to it.15.9 Wipe the immersed portion of the thermometer withone fourth of a circle of filter paper and transfer the
36、 paper to aprepared Bchner funnel fitted with a filter paper.15.10 Add 10 mL of paper pulp to the slurry and continuestirring 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 stirrershaft and blades into the flask with wa
37、ter.15.13 Wipe the shaft and blades with one fourth of a circleof filter paper and transfer the filter paper to the Bchnerfunnel.15.14 Filter the slurry through the Bchner funnel and washcontents of the flask into the funnel.15.15 Wash the residue with 1 M nitric acid until a 10-mLportion of the fil
38、trate shows no detectable yellow color whenmade basic with sodium hydroxide and after a few drops ofH2O2(30 %) have been added as a color developer.15.16 Wash the residue several times with water after anegative test is obtained.15.17 Draw air through the filter until the residue and filterpad are d
39、ry.15.18 Scrape the residue and paper into a preignited(1000C) tared 40-mL crucible, place on a hot plate and slowlychar off the organic material.15.19 Ignite the residue for1hat1000C in a mufflefurnace.15.20 Cool the crucible in a desiccator and weigh.15.21 Calculate the percentage of solids in acc
40、ordance with17.1.NOTE 3If the percentage of solids (insoluble residue) is greater than0.1 %, grind and mix the residue and determine the total milligrams ofuranium in the residue by the photometric procedure in 16.1-16.10.16. Photometric Procedure for Uranium16.1 Transfer the ground, blended residue
41、 from 15.20 to a100-mL beaker.16.2 Add 10 mL of water and 10 mL of HCl (sp gr 1.19),cover, and boil for 10 min.16.3 Add 5 mL of HNO3(sp gr 1.42) and boil until fumingof NO2ceases. Remove cover glass.16.4 Add 5 mL of 9M H2SO4and 2 mL of HF (48 %), thenheat to dryness on the hotplate. Bake to fume off
42、 remainingH2SO4and cool.16.5 Wash down sides of beaker with water and add 5 mLof HNO3.16.6 Cover with a watchglass and digest for approximately10 min near the boiling point.16.7 Quantitatively transfer the solution to a 250-mL volu-metric flask. Add 25 mL of NaOH solution and a few drops ofH2O2. Mak
43、e up to mark with water and mix.NOTE 4The solution must be basic for yellow sodium peruranatecolor to develop.16.8 Measure the absorbance of the solution in a spectro-photometer at 425 nm in a 1-cm cell using a blank as reference.The blank is prepared by diluting 25 mL of NaOH, plus a fewdrops of H2
44、O2, to 250 mL with water.16.9 Prepare a calibration curve covering the range from 0to 50 mg of uranium from aliquots of a standard uraniumsolution. Proceed as in 16.5-16.8. Plot the milligrams ofuranium against absorbance readings.16.10 Determine the total milligrams of uranium in thesample solution
45、 from the calibration curve.NOTE 5If the sample solution falls outside the calibration range,dilute a portion with the reference-blank solution and read again.17. Calculation17.1 Calculate the percentage of insoluble residue, R,present as follows:R 5Rw3 100Sw(1)where:Rw= weight of residue (see 15.20
46、), g, andSw= weight of samples, g.17.2 If the insoluble residue exceeds 0.1 %, calculate thepercentage of nitric acid-insoluble uranium, UN, and present asfollows:UN5USw3 10(2)C1022 05 (2010)13where:U = uranium content calculated in 16.10, mg, andSw= weight of sample, g.17.3 Calculate the percentage
47、 of nitric acid-insoluble ura-nium, Uu, on a uranium basis as follows:Uu5UN3 100Us(3)where:UN= nitric acid-insoluble residue present (see 17.2), %,andUs= uranium in sample, %.18. Precision and Bias18.1 PrecisionA relative standard deviation for this testmethod has been reported as 10 % at the 0.2 %
48、HNO3insolubleuranium level (see 4.2).18.2 BiasFor information on the bias of this test methodsee 4.2.EXTRACTABLE ORGANIC MATERIAL19. Scope19.1 This test method is used to determine the extractableorganic material in uranium-ore concentrates. It is recognizedthat certain water-soluble organic materia
49、ls, such as flocculat-ing agents, are not measured by this test method.20. Summary of Test Method20.1 This test method consists of a dual extraction usingn-hexane on the solid uranium-ore concentrate sample andchloroform on a subsequent nitric acid solution of the sample.Each of the extractants is evaporated to measure the amount oforganic material extracted.21. Interferences21.1 At the specification limit for extractable organic mate-rial established for uranium-ore concentrations, and within thescope of this test method, interferences are insig
