ASTM_C_1502_-_16.pdf

Designation:C150216Standard Test Method forDetermination of Total Chlorine and Fluorine in UraniumDioxide and Gadolinium Oxide1This standard is issued under the fixed designation C1502;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 chlorineand fluorine in nuclear-grade uranium dioxide(UO2)powderand pellets,nuclear grade gadolinium oxide(Gd2O3)powderand gadolinium oxide-uranium oxide(Gd2O3-UO2)powderand pellets.1.2 With a 2 gram UO2sample size the detection limit of themethod is 4 g/g for chlorine and 2 g/g for fluorine.Themaximum concentration determined with a 2 gram sample is500 g/g for both chlorine and fluorine.The sample size usedin this test method can vary from 1 to 10 grams resulting in acorresponding change in the detection limits and range.1.3 The values stated in SI units are to 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 determine the applica-bility of regulatory limitations prior to use.2.Referenced Documents2.1 ASTM Standards:2C753 Specification for Nuclear-Grade,Sinterable UraniumDioxide PowderC776 Specification for Sintered Uranium Dioxide PelletsC859 Terminology Relating to Nuclear MaterialsC888 Specification for Nuclear-Grade Gadolinium Oxide(Gd2O3)PowderC922 Specification for Sintered Gadolinium Oxide-UraniumDioxide PelletsD1193 Specification for Reagent Water3.Terminology3.1 DefinitionsExcept as otherwise defined herein,defini-tions of terms are given in Terminology C859.3.2 Definitions of Terms Specific to This Standard:3.2.1 acceleratora chemical compound or a flux that willdecrease the reaction time or prohydrolysis time.4.Summary of Test Method4.1 The halogens are separated from the test materials bypyrohydrolysis in a quartz reaction tube with a stream of wetoxygen or air at a temperature of 900 to 1000C(1-4).Chlorideand fluoride are volatilized simultaneously as acids,absorbedin an absorption solution as chloride and fluoride and measuredwith ion selective electrodes(4-6).5.Significance and Use5.1 The method is designed to show whether or not thetested materials meet the specifications as given in eitherSpecification C753,C776,C888 or C922.6.Interferences6.1 The absorption solution controls the pH of the measuredsolution to avoid hydroxide ion interference or the formation ofhydrogen complexes with fluoride.6.2 Bromide,iodide,cyanide and sulfide,if present in thecondensate,interfere in the measurement of chloride withion-selective electrodes,but have very little effect upon themeasurement of fluoride with ion-selective electrodes.6.3 As the ionic activity of the chloride and fluoride ions istemperature dependent,the standard solutions and samplesolutions should be measured at the same temperature.7.Apparatus7.1 Pyrohydrolysis Equipment,the assembly of suitableequipment is shown in Fig.1.7.2 Gas Flow Regulator and Flowmeter.7.3 Hot Plate,used to warm the water saturating the spargegas to 50 to 80C.7.4 Combustion Tube Furnace,having a bore of about 32mm with a length of about 300 mm and the capability of1This 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.15,2016.Published February 2016.Originallyapproved in 2001.Last previous edition approved in 2009 as C1502 09.DOI:10.1520/C1502-16.2For 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.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 maintaining a temperature of 950 6 25C.Combustion tubefurnaces with different dimensions may be satisfactory.Tem-peratures between 900 and 1000C have been found to besatisfactory.7.5 Quartz Reaction Tube(Fig.2)The exit end should notextend more than 50 mm beyond the furnace with a groundjoint connecting to the delivery tube.The delivery tube extendsinto a polyethylene or Pyrex absorption vessel with a tipcapable of giving a stream of very fine bubbles.A secondabsorption vessel connected in series,may be necessary toensure complete collection of the fluorine and chlorine fromthe sample.7.6 Combustion Boat,a ceramic,platinum or quartz boatwith a 10 mL capacity(approx.90 to 100 mm long,13 mmwide,and 10 mm high).Boats with different dimensions maybe satisfactory.7.7 Absorption Vessel,a 50-ml po