1、Designation:C 1317 95Standard Practice forDissolution of Silicate or Acid-Resistant Matrix Samples1This standard is issued under the fixed designation C 1317;the number immediately following the designation indicates the year oforiginal adoption or,in the case of revision,the year of last revision.A
2、 number in parentheses indicates the year of last reapproval.Asuperscript epsilon(e)indicates an editorial change since the last revision or reapproval.1.Scope1.1 This practice covers alkaline fusion of silicate matrixsamples(or other matrices difficult to dissolve in acids)usingan electric Bunsen b
3、urner mounted on an orbital shaker.Thispractice has been used successfully to dissolve borosilicateglass,dried glass melter feeds,various simulated nuclear wasteforms,and dried soil samples.1.2 This fusion apparatus and the alkaline fluxes describedare suitable for use in shielded radiation containm
4、ent facilitiessuch as hot cells and shielded hoods.1.3 When samples dissolved using this practice are radio-active,the user must follow radiation protection guidelines inplace for such materials.1.4 This standard does not purport to address all of thesafety concerns,if any,associated with its use.It
5、 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.Specific precau-tionary statements are given in Section 8.2.Referenced Documents2.1 ASTM Standards:C 169 Test Methods for C
6、hemical Analysis of Soda-Limeand Borosilicate Glass2C 1109 Test Method for Analysis of Aqueous Leachatesfrom Nuclear Waste Materials Using Inductively CoupledPlasma-Atomic Emission Spectrometry3C 1111 Test Method for Determining Elements in WasteStreams by Inductively Coupled Plasma-Atomic EmissionS
7、pectroscopy2C 1220 Test Method for Static Leaching of MonolithicWaste Forms for Disposal of Radioactive Waste2C 1285 Test Methods for Determining Chemical Durabilityof Nuclear Waste Glasses:The Product Consistency Test(PCT)2D 1193 Specification for Reagent Water43.Summary of Practice3.1 An aliquot o
8、f the dried and ignited sample is weighedinto a tared nickel or zirconium metal crucible and an appro-priate amount of alkaline flux(potassium hydroxide or sodiumperoxide)is added.The crucible is placed on a preheatedelectric Bunsen burner(1000C capability)mounted on anorbital shaker.The speed of th
9、e shaker is adjusted so that theliquefied alkali metal flux and the sample are completely fusedat the bottom of the crucible.When the fusion is complete(about 5 min),the crucible is removed from the heater andcooled to room temperature.The fused mixture is dissolved inwater,acidified with hydrochlor
10、ic acid,and diluted to anappropriate volume for subsequent analysis.3.2 With appropriate sample preparation,the solution result-ing from this procedure can be analyzed for trace metals byinductively coupled plasma-atomic emission spectroscopy(ICP-AES),inductively coupled plasma-mass spectrometry(ICP
11、-MS),and atomic absorption spectroscopy,and for radio-nuclides using applicable radiochemical methods.4.Significance and Use4.1 This practice describes a method to fuse and dissolvesilicate and refractory matrix samples for subsequent analysisfor trace metals and radionuclides.These samples may cont
12、ainhigh-level radioactive nuclear waste.Nuclear waste glassvitrification plant feeds and product can be characterized usingthis dissolution method followed by the appropriate analysis ofthe resulting solutions.Other matrices such as soil and sedi-ment samples and geological samples may be totally di
13、ssolvedusing this practice.The ICP-AES methods in Test MethodsC 1109 and C 1111 can be used to analyze the dissolved samplewith additional sample preparation as necessary and withmatrix effect considerations.Additional information as to otheranalytical methods can be found in Test Method C 169.4.2 T
14、his practice has been used to analyze round-robinsimulated nuclear waste glass samples.4.3 This practice can be used for bulk analysis of glasssamples for the product consistency test(PCT)as described inTest Methods C 1285 and for the analysis of monolithicradioactive waste glass used in the static
15、leach test as describedin Test Method C 1220.4.4 This practice can be used to dissolve the glass referenceand testing materials described in Refs(1)and(2).55.Interferences5.1 Elements that form volatile species under these alkaline1This practice is under the jurisdiction of ASTM Committee C-26 on Nu
16、clearFuel Cycle and is the direct responsibility of Subcommittee C26.05 on Methods ofTest.Current edition approved Nov.10,1995.Published March 1996.2Annual Book of ASTM Standards,Vol 15.02.3Annual Book of ASTM Standards,Vol 12.01.4Annual Book of ASTM Standards,Vol 11.01.5The boldface numbers in parentheses refer to the list of references at the end ofthis practice.1AMERICAN SOCIETY FOR TESTING AND MATERIALS100 Barr Harbor Dr.,West Conshohocken,PA 19428Reprinted from the Annual Book of ASTM Stand