ASTM C1307-2002(2008) Standard Test Method for Plutonium Assay by Plutonium (III) Diode Array Spectrophotometry《用(III)钚数组分光光度法鉴定钚的标准试验方法》.pdf
《ASTM C1307-2002(2008) Standard Test Method for Plutonium Assay by Plutonium (III) Diode Array Spectrophotometry《用(III)钚数组分光光度法鉴定钚的标准试验方法》.pdf》由会员分享,可在线阅读,更多相关《ASTM C1307-2002(2008) Standard Test Method for Plutonium Assay by Plutonium (III) Diode Array Spectrophotometry《用(III)钚数组分光光度法鉴定钚的标准试验方法》.pdf(6页珍藏版)》请在麦多课文档分享上搜索。
1、Designation: C 1307 02 (Reapproved 2008)Standard Test Method forPlutonium Assay by Plutonium (III) Diode ArraySpectrophotometry1This standard is issued under the fixed designation C 1307; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revis
2、ion, 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 test method describes the determination of totalplutonium as plutonium(III) in nitrate and chlor
3、ide solutions.The technique is applicable to solutions of plutonium dioxidepowders and pellets (Test Methods C 697), nuclear grademixed oxides (Test Methods C 698), plutonium metal (TestMethods C 758), and plutonium nitrate solutions (Test Meth-ods C 759). Solid samples are dissolved using the appro
4、priatedissolution techniques described in Practice C 1168. The use ofthis technique 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 Th
5、e values stated in SI units are to be regarded asstandard. 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-pria
6、te safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:3C 697 Test Methods for Chemical, Mass Spectrometric, andSpectrochemical Analysis of Nuclear-Grade PlutoniumDioxide Powders and PelletsC 698 Test Methods f
7、or Chemical, Mass Spectrometric, andSpectrochemicalAnalysis of Nuclear-Grade Mixed Oxides(U, Pu)O2)C 757 Specification for Nuclear-Grade Plutonium DioxidePowder, SinterableC 758 Test Methods for Chemical, Mass Spectrometric,Spectrochemical, Nuclear, and Radiochemical Analysis ofNuclear-Grade Plutoni
8、um MetalC 759 Test Methods for Chemical, Mass Spectrometric,Spectrochemical, Nuclear, and Radiochemical Analysis ofNuclear-Grade Plutonium Nitrate SolutionsC 833 Specification for Sintered (Uranium-Plutonium) Di-oxide PelletsC 1168 Practice for Preparation and Dissolution of Pluto-nium Materials for
9、 Analysis3. Summary of Method3.1 In a diode array spectrophotometric measurement, as ina conventional spectrophotometric measurement, the substancebeing determined absorbs light at frequencies characteristic ofthat substance. The amount of light absorbed at each wave-length is directly proportional
10、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 interest relative to a traceable standard when bothsolutions are measured under
11、 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).An entire absorption spectrum can be obtained in0.1 s; however, optimum
12、precision is obtained from multiplespectra collected over a 4-s period.3.2 Reduction to plutonium(III) is accomplished by theaddition of a measured quantity of reductant solution to thesample aliquant.3.2.1 For nitrate solutions, ferrous sulfamate is the recom-mended reductant. Aliquants (1 mL or le
13、ss) of the samplesolution are diluted with 10 mL of a ferrous reductant/matrixsolution to 1 g Pu/L, and measured.1This test method is 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 J
14、une 1, 2008. Published July 2008. Originally approvedin 1995. Last previous edition approved in 2002 as C 1307 02.2For 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
15、method has been applied 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
16、 website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.3.2.2 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 ofzirco
17、nium 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 solutions for measurement.3.3 Plutonium concentration is determined from light ab-sorption measurements taken on the sample solution in theblue-green region from
18、516 to 640 nm where a broad doubletband is observed. Spectral quantifying software capable offitting the sample spectrum with spectral information fromstandard solutions is used to calculate the plutonium concen-tration. Both commercially available (6) and custom-designed(7-12) spectral fitting soft
19、ware have been developed whichmay be used for plutonium measurements. The users of thisprocedure are responsible for selecting or customizing, or both,the spectral fitting (and instrument control) software that bestmeets their individual measurement methodology and needs.Software selection will dict
20、ate many of the procedural specificsnot included in this procedure. This procedure is intended toaddress key measurement requirements and to allow usersdiscretion in establishing appropriate procedural details andtechnique variations. The software package selected shouldinclude a feature that indica
21、tes the quality of spectral fit,thereby providing information on the measurement reliabilityand the presence of interferences that absorb light or otherwisealter the plutonium(III) spectrum without requiring supplemen-tal measurements.4. Significance and Use4.1 This test method is designed to determ
22、ine whether agiven material meets the purchasers specification for pluto-nium content.5. Interferences5.1 Materials meeting the applicable material specificationsof theASTM standard for which this procedure was developed,when dissolved and diluted without introduction of interferingcontaminants as d
23、escribed in Practice C 1168, will contain nointerfering elements or species.NOTE 1Fluoride, if present, would interfere if the zirconium, rou-tinely added to the sample solution aliquant for the chloride matrix, wereomitted from the procedure. Zirconium may be added to the nitrate matrix.Ferrous-Red
24、uctant Solution to handle fluorides if present. Zirconium,when used, should be added to all samples, blanks, and standards to obtaina consistent matrix. Refer to Specifications C 833 and C 757.5.2 Interferences are caused by: 1) materials that absorblight in the region of the plutonium absorption, 2
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