ASTM C1508-2001(2011) Standard Test Method for Determination of Bromine and Chlorine in UF6 and Uranyl Nitrate by X-Ray Fluorescence (XRF) Spectroscopy《用X射线荧光(XRF)光谱法测定UF6 和硝酸铀酰中溴和.pdf
《ASTM C1508-2001(2011) Standard Test Method for Determination of Bromine and Chlorine in UF6 and Uranyl Nitrate by X-Ray Fluorescence (XRF) Spectroscopy《用X射线荧光(XRF)光谱法测定UF6 和硝酸铀酰中溴和.pdf》由会员分享,可在线阅读,更多相关《ASTM C1508-2001(2011) Standard Test Method for Determination of Bromine and Chlorine in UF6 and Uranyl Nitrate by X-Ray Fluorescence (XRF) Spectroscopy《用X射线荧光(XRF)光谱法测定UF6 和硝酸铀酰中溴和.pdf(4页珍藏版)》请在麦多课文档分享上搜索。
1、Designation: C1508 01 (Reapproved 2011)Standard Test Method forDetermination of Bromine and Chlorine in UF6and UranylNitrate by X-Ray Fluorescence (XRF) Spectroscopy1This standard is issued under the fixed designation C1508; the number immediately following the designation indicates the year oforigi
2、nal 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)and chlorine
3、 (Cl) in uranium hexafluoride (UF6) and uranylnitrate solution. The method as written covers the determina-tion of bromine in UF6over the concentration range of 0.2 to8 g/g, uranium basis. The chlorine in UF6can be determinedover the range of 4 to 160 g/g, uranium basis. Higherconcentrations may be
4、covered by appropriate dilutions. Thedetection limit for Br is 0.2 g/g uranium basis and for Cl is 4g/g uranium basis.1.2 This standard may involve hazardous materials, opera-tions and equipment. This standard does not purport to addressall of the safety concerns, if any, associated with its use. It
5、 isthe responsibility of the user of this standard to establishappropriate safety and health practices and determine theapplicability of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2C761 Test Methods for Chemical, Mass Spectrometric,Spectrochemical, Nuclear, and Rad
6、iochemical Analysis ofUranium HexafluorideC787 Specification for Uranium Hexafluoride for Enrich-mentC788 Specification for Nuclear-Grade Uranyl Nitrate Solu-tion or CrystalsC1118 Guide for Selecting Components for Wavelength-Dispersive X-Ray Fluorescence (XRF) SystemsD1193 Specification for Reagent
7、 Water3. Summary of Test Method3.1 A sample of hydrolyzed UF6(uranyl fluoride) or uranylnitrate solution is treated with sodium nitrite to reduce oxidizedforms of bromine and chlorine (bromates and chlorates) to theirrespective halide ions.Addition of silver nitrate precipitates thesilver halides. S
8、pike recoveries can be improved by theaddition of potassium iodide causing coprecipitation of thehalides. The halides are collected on filter paper and areanalyzed by X-ray fluorescence using two different crystal/detector systems.4. Significance and Use4.1 The method is designed to show whether or
9、not thetested materials meet the specifications as given in Specifica-tions C787 and C788.5. Interferences5.1 Plastic equipment must be used throughout the methodfor uranyl fluoride as the hydrofluoric acid in the uranylfluoride leaches chloride from glassware causing a high bias.5.2 Low recoveries
10、may occur as the precipitate can bedifficult to transfer quantitatively to the filter paper. A surfac-tant can be added (optional step) to minimize the adhesion ofthe precipitate to the walls of the beakers and the funnel.6. Apparatus6.1 X-Ray Spectrometer, see Guide C1118 for the selectionof the X-
11、ray Spectrometer.6.2 Plastic Vacuum Filtration Apparatus, for 47 mm diam-eter filter paper.6.3 Filter Paper, 0.45 micron, 47 mm diameter.36.4 Beakers, polypropylene, 250 mL.6.5 Stirring Rods, plastic or Teflon.6.6 X-ray Sample Support, Rings. Inner diameter approxi-mately 40 mm.1This test method is
12、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 June 1, 2011. Published June 2011. Originallyapproved in 2001. Last previous edition approved in 2006 as C1508 01(2006).DOI: 10.1520/C1
13、508-01R1.2For 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 website.3The filter must be Cl and Br free. Millipore membra
14、ne filter type HABP() has been successfully used. An alternate is 15A from S.C.B,BP6, RN86, 07130 Soyons France. Any other equivalent is acceptable.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.7. Reagents7.1 Purity of ReagentsReag
15、ent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents conform to the specifications of the Committee onAnalytical Reagents of the American Chemical Society, wheresuch specifications are available.4Other grades may be used,provided it is first asce
16、rtained that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination.7.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean reagent water conformingto Specification D1193, Type I.7.3 Ammonium Hydroxide,NH4O
17、H, concentrated, specificgravity 0.90.7.4 Ammonium Hydroxide Solution, 1 + 3 (3.7 M). Dilute 1part NH4OH with 3 parts water.7.5 Surfactant, bromine and chlorine free.5(Optional).7.6 Surfactant Solution, 1 + 999. Add 1 mL of surfactant toapproximately 1 litre of water. (Optional).7.7 Nitric Acid, HNO
18、3, concentrated, specific gravity 1.42.7.8 Nitric Acid Solution, 1 + 999 (0.016 M). Add 1 mL ofconcentrated HNO3to approximately 200 mL of water. Add 1mL of the surfactant (7.6). (Optional). Dilute to 1 litre.7.9 Sodium Nitrite, NaNO2.7.10 Sodium Nitrite Solution, 2 g/L. Dissolve1gofsodiumnitrite in
19、 water and dilute to 500 mL. Prepare fresh immedi-ately before use.7.11 Silver Nitrate, AgNO3.7.12 Silver Nitrate Solution, 2 g/L. Dissolve2gofsilvernitrate in water and dilute to 1 litre. Keep away from light in anopaque bottle. The solution should be made fresh weekly.Silver is an RCRA listed haza
20、rdous waste. Make up only asmuch of this solution as required to minimize excess waste.7.13 Potassium Bromide, KBr.7.14 Bromide Solution, 500 mg Br/L. Dissolve 0.1861 g ofKBr (dried at 110C for 1 hour) in water and dilute to 250 mLin a volumetric flask.7.15 Sodium Chloride, NaCl.7.16 Sodium Chloride
21、 Solution, 1000 mg Cl/L. Dissolve1.648 g NaCl (dried at 110 C for 1 hour ) in water and diluteto 1 litre in a volumetric flask.7.17 Spike Solution, 5 mg Br/L, 100 mg Cl/L. Transfer 10mL of 500 mg Br /L solution into a 1 litre volumetric flask bypipette. Transfer 100 mL of 1000 mg Cl /L into the flas
22、k bypipette. Dilute to volume.7.18 Potassium Iodide, KI. (Optional).7.19 Potassium Iodide Solution, (Optional), 1g I/L. Dis-solve 0.131 g potassium iodide in water and dilute to 100 mL.The solution should be prepared weekly.8. Standard Preparation8.1 Pipette the following aliquots of spike solution
23、(from7.17) into polypropylene beakers. 0 mL, 1 mL, 2 mL, 5 mL, 10mL. The aliquots represent 0g Br, 5g Br, 10g Br, 25g Br,50g Br and 0g Cl, 100g Cl, 200g Cl, 500g Cl, 1000g Cl.8.2 Add 70 mL water to each beaker.8.3 Follow steps 9.3-9.8 at the same time as the samples.9. Procedure9.1 Transfer a known
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