1、Designation:C130715Standard Test Method forPlutonium Assay by Plutonium(III)Diode ArraySpectrophotometry1This standard is issued under the fixed designation C1307;the number immediately following the designation indicates the year oforiginal adoption or,in the case of revision,the year of last revis
2、ion.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 test method describes the determination of totalplutonium as plutonium(III)in nitrate and chloride solutions.The technique is ap
3、plicable to solutions of plutonium dioxidepowders and pellets(Test Methods C697),nuclear grade mixedoxides(Test Methods C698),plutonium metal(Test MethodsC758),and plutonium nitrate solutions(Test Methods C759).Solid samples are dissolved using the appropriate dissolutiontechniques described in Prac
4、tice C1168.The use of thistechnique for other plutonium-bearing materials has beenreported(1-5),but final determination of applicability must bemade by the user.The applicable concentration range forplutonium sample solutions is 10200 g Pu/L.21.2 The values stated in SI units are to be regarded asst
5、andard.No other units of measurement are included in thisstandard.1.3 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 determine the applic
6、a-bility of regulatory limitations prior to use.2.Referenced Documents2.1 ASTM Standards:3C697 Test Methods for Chemical,Mass Spectrometric,andSpectrochemical Analysis of Nuclear-Grade PlutoniumDioxide Powders and PelletsC698 Test Methods for Chemical,Mass Spectrometric,andSpectrochemical Analysis o
7、f Nuclear-Grade Mixed Ox-ides(U,Pu)O2)C757 Specification for Nuclear-Grade Plutonium DioxidePowder,SinterableC758 Test Methods for Chemical,Mass Spectrometric,Spectrochemical,Nuclear,and Radiochemical Analysis ofNuclear-Grade Plutonium MetalC759 Test Methods for Chemical,Mass Spectrometric,Spectroch
8、emical,Nuclear,and Radiochemical Analysis ofNuclear-Grade Plutonium Nitrate SolutionsC833 Specification for Sintered(Uranium-Plutonium)Diox-ide PelletsC859 Terminology Relating to Nuclear MaterialsC1168 Practice for Preparation and Dissolution of PlutoniumMaterials for Analysis3.Terminology3.1 Defin
9、itions:3.1.1 For definitions of terms related to nuclear materials,refer to Terminology C859.4.Summary of Method4.1 In a diode array spectrophotometric measurement,as ina conventional spectrophotometric measurement,the substancebeing determined absorbs light at frequencies characteristic ofthat subs
10、tance.The amount of light absorbed at each wave-length is directly proportional to the concentration of thespecies of interest.The absorption is a function of the oxidationstate and the complexation obtained in the solution matrixselected for measurement.Beers Law permits quantifying thespecies of i
11、nterest relative to a traceable standard when bothsolutions are measured under the same conditions.The array ofphotosensitive diodes permits the(virtually)simultaneouscollection of spectral information over the entire range of theinstrument,for example,190820 nm(or any selected portionof the range).
12、An entire absorption spectrum can be obtained in0.1 s;however,optimum precision is obtained from multiplespectra collected over a 4-s period.4.2 Reduction to plutonium(III)is accomplished by theaddition of a measured quantity of reductant solution to thesample aliquant.4.2.1 For nitrate solutions,fe
13、rrous sulfamate is the recom-mended reductant.Aliquants(1 mL or less)of the sample1This test method is under the jurisdiction ofASTM Committee C26 on NuclearFuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods ofTest.Current edition approved Jan.1,2015.Published January 2015
14、.Originallyapproved in 1995.Last previous edition approved in 2014 as C1307 14.DOI:10.1520/C1307-15.2For solid samples,select the sample size and dissolved solution weight to yieldsample solutions in the 1030 g Pu/L range.With special preparation and spectralanalysis techniques,the method has been a
15、pplied to nitrate solutions in the 0.110g Pu/L range.3For 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.Copyright AST
16、M International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 solution are diluted with 10 mL of a ferrous reductant/matrixsolution to 1 g Pu/L,and measured.4.2.2 For chloride solutions,ascorbic acid is the recom-mended reductant.Aliquants of the sample solution,eachcontaining 50100 mg of plutonium,are diluted with 2 mL ofzirconium solution to complex fluoride ions,2 mL ascorbicacid reductant solution,and 1.0 M HCl to a total volume of 25mL,yielding 24 g Pu/L s
