1、9009276 DO28257 933 Designation:D 3315-86#Ib AMERICAN SOCIETY FOR TESTING AND MATERIALS 1916 Race S i.Philadelphia,Pa.19103 Reprinted from the Annual Book of ASTM Standards,Copyright ASTM If not listed in the current combined index,will appear in the next edition.Standard Test Method for RADIOACTIVE
2、 ZIRCONIUM IN WATER This standard is issued under the fixed designation D 33 15;the number immediately following the designation indicates the year of original adoption or,in the case of revision,the year of lasr revision.A number in parentheses indicates the year of last napproVal.A superscript eps
3、ilon(e)indicates an editorial change since the last revision or reapproval.1.scope i.1 This test method covers the determination of radioactive zirconium in water in concentra-tions greater than 100 pCi/L.Concentration of the sample can increase the sensitivity of the method.It is applicable to the
4、analysis of mix-tures of zirconium isotopes of atomic mass 95 and 97,if a high resolution semiconductor detec-tor is available,Otherwise it is limited to the analysis of zirconium-95.1.2 This test method may be used for absolute determinations by calibrating the nuclear detec-tor with a standard zir
5、conium-95 source.or for relative determinations by comparing measure-ments with each other.1.3 This test method does not meet the re-quirements of the current edition of Practice D2777.I.4 This standard may involve hazardous ma-lerials,operations,and equipment.This standard does not purport to addre
6、ss a l i of rhe sahty prob lems associated with its use.11 is lhe responsibii-ity of the user of rhis standard to establish appro-priate safety and health practices and determine the applicability o f regulatory limitations prior to use.A specific precautionary statement is given in Note 1.2.Referen
7、ced Documents 2.i ASTM Standards:D 1066 Practice for Sampling Steam2 D 1129 Definitions of Terms Relating to D i i92 Specification for Equipment for Sam-D 1193 Specification for Reagent Wate?D 2777 Practice for Determination of Preci-sion and Bias of Applicable Methods of Committee D-19 on Wate3 Wat
8、e3 pling Water and Steam D 3370 Practices for Sampling Wate?D3648 Practices for the Measurement of D 3649 Practice for High-Resolution Gamma-Radioacthit?Ray Spectrometry of Wate?3.Definitions 3.1 For definition of terms used in this test method,refer to Definitions D 1129.For terms not defined in De
9、finitions D 1 i 29,reference may be made to other published glossaries.4 4.Summary of Test Method 4.1 This test method is based on the extraction of zirconium from the sample with S-thenoyltn-fluoroacetone(TTA)in xylene A fluoride pretreatment converts hydrolytic and colloidai species of zirconium t
10、o an extractable form.Ra-dio-iodine,the only fission product significantly extracted with zirconium,is separated by strip-ping the zirconium from the organic phase with a dilute nitric-hydrofluoric acid mixture.The aqueous phase containing the zirconium is gamma counted.No yield determination is re-
11、quired,since the recovery is greater than 97%.5.Significance and Use 5.1 Zirconium-95 is formed by neutron irra-diation of nuclear reactor structural materials or fuel element cladding materials(Zircaioy).It is also a fission product.Zirconium-95 is of impor-This test method is under the jurisdictio
12、n of ASTM Com-mittee Dl9 on Water and is the direct responsibility of D 1 9.0 4 on Methods of Radiochemical Analysis.Current edition approved Oct.3 1.1986.Published December 1986.Onginally published as D3315-73 T.Last previous edition D 3315-77(1981)t.Anniral Book qf ASTM Slandards.Vol 1 1.O I.Annua
13、l Book of ASTM Standards.Vol I 1.02.ANSI Standard Glossary of Terms in Nuclear Science and The boldface numbers in parentheses refer to the list of Technology,N.l-1967.references at the end of this test method.NOTICE:This standard has either been superseded and replaced by a new version or discontin
14、ued.Contact ASTM International(www.astm.org)for the latest information.9009276 0028258 87T m D 3315 tance,therefore,in evaluating corrosion of reac-tor components and the potential radiological hazard of the cooling water.5.2 This test method is limited by analytical completion time to 64-day zircon
15、ium-95 and to 17-h zirconium-97.5.3 Radio-iodine,present in fresh fission product mixtures,is partially extracted.The io-dine is eliminated by the addition of iodine hold-back carrier and by stripping the zirconium from the organic phase prior to counting.Large amounts of fluoride and sulfate interf
16、ere with the TTA extraction method,requiring further treat-ment.Two fumings with perchloric acid elimi-nate fluoride interference,and reduce the inter-ference from sulfates.6.Interferences 6.1 Niobium-95,the daughter product of zir-conium-95,is found in the sample and also will grow-in to the separated zirconium-95 after completion of step 1 1.1 O in the procedure.Nio-bium-95 interferes in the final activity measure-ment when made with a sodium iodide detector which cannot resolve the gamma ray