ASTM_C_1771_-_13.pdf

Designation:C177113Standard Test Method forDetermination of Boron,Silicon,and Technetium inHydrolyzed Uranium Hexafluoride by Inductively CoupledPlasmaMass Spectrometer After Removal of Uranium bySolid Phase Extraction1This standard is issued under the fixed designation C1771;the number immediately following the designation indicates the year oforiginal 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 test method covers the determination of boron,silicon and technetium in hydrolyzed uranium hexafluoride(UF6)by Inductively Coupled Plasma Mass Spectrometry(ICP-MS)after separation of the uranium by solid phaseextraction.1.2 The 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-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.Some specifichazards statements are given in Section 7 on Hazards.2.Referenced Documents2.1 ASTM Standards:2C787 Specification for Uranium Hexafluoride for Enrich-mentC859 Terminology Relating to Nuclear MaterialsC996 Specification for Uranium Hexafluoride Enriched toLess Than 5%235UC1346 Practice for Dissolution of UF6from P-10 TubesC1689 Practice for Subsampling of Uranium HexafluorideD1193 Specification for Reagent Water3.Terminology3.1 DefinitionsFor definitions of other standard terms inthis test method,refer to Terminology C859.3.2 Definitions:3.2.1 internal reference solution,na solution containingnon-analyte elements,the signal from which is used to correctfor variation in the performance of a measuring instrumentthrough the course of analyzing a batch of samples,therebyimproving precision.3.2.2 method blank,na solution which in so far as ispractical duplicates the sample to be analyzed and passesthrough the same measurement process but does not initiallycontain significant quantities of any of the analytes to bemeasured.3.2.2.1 DiscussionThe method blank does not initiallycontain significant quantities of analyte,hence the value of anyanalyte measured may be assumed to be due to interference,matrix effects or contamination introduced as a consequence ofsample processing,The contribution of such factors to thevalue measured on the genuine sample may therefore beeliminated by subtracting the measured value for the methodblank,typically providing a better estimate for the true value ofthe quantity of analyte in the sample.3.2.3 recovery correction,na factor applied to the mea-sured value of the analyte in the sample to account for lossesof analyte during sample processing.3.2.3.1 DiscussionSome of the analyte originally presentin a sample is likely to be lost during the process of preparingthe sample for instrumental measurement,so that the measuredvalue will typically be subject to negative bias.The proportionof analyte lost may be estimated by repeated measurement ofa sample containing a known quantity of the analyte and acorrection factor introduced to account for losses.Recoverycorrection is only required when analyte losses are significantwhen compared with overall measurement uncertainty.3.2.4 spike,na known quantity of analyte added to asample.4.Summary of Test Method4.1 A4%by weight solution of UF6is initially prepared byreacting a quantity of UF6with water.Sub-sampling of UF6may be carried out as described in Practice C1689.Preparation1This 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.1,2013.Published February 2013.DOI:10.1520/C1771-132For 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 ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 of the hydrolyzed solution may be carried out as described inPractice C1346.The laboratory may choose to adopt a simpli-fied version of the standard practices,or to adopt otherpractices,provided that any additional error thereby introducedis incorporated within precision statements for the method.4.2 Concentrated nitric acid is added to the uranium solutionto give a nitric acid concentration of approximately 1.5 M.Thesolution is then passed through a diamyl amylphosphonate(DAAP)resin column which retains the uranium.Boron,silicon and technetium are eluted from the column with 2 Mnitric acid and the solution made up to volume with reagentwater.The boron,silicon and technetium concentrations arethen meas