ML19221B366

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Reg Guide 5.16,Revision L, Std Methods for Chemical Mass Spectrometric,Spectrochemical,Nuclear & Radiochemical Analysis of Nuclear-Grade Pu Nitrate Solutions & Pu Metal
ML19221B366
Person / Time
Issue date: 05/31/1975
From:
NRC OFFICE OF STANDARDS DEVELOPMENT
To:
References
REGGD-05.016, REGGD-5.016, NUDOCS 7907200166
Download: ML19221B366 (2)


Text

Revision 1 U.S. NUCLEAR REGULATORY COMMISSION May 1975 9

REGE LE'ORV GEDDE OFFICE OF STANDARDS DEVELOPMENT REGULATORY GUIDE 5.16 STANDARD METHODS FOR CHEMICAL, MASS SPECTROMETRIC, SPECT ROCHEMICAL, NUCLEAR, AND RADIOCHEMICAL ANALYSIS OF NUCLEAR-GRADE PLUTONIUM NITRATE SOLUTIONS AND PLUTONIUM METAL A. INTRODUCTION of Nuclear-Grade Plutonium Me tal,"2 and ANSI N573-1974 (ASTM C759 73), "Chemica Mau Paragraph (b) of Section 70.22, " Con ten ts of Spectrometrie, Spectrochenucal.

Nuclear and Apphcations," of 10 CFR Part 70, "Special Nuclear Radiochemical Anaiysis of Nuclear-Grade Plutonium Material," requires an apphcant for a hcense to possess Nitrate Solutions."2 As used in these standards, certam quanuues of special nuclear matenal in an nudcar. grade ma'erial means material that is to be used unsealed form to describe, among other things, his exclusnely fer the fabncation of nuclear fuel.

procedures for control of and accounung for special ruclear material. This guide identifies methods Plutonium Nitrate Solutions ceceptable to the NRC staff for chemical, isotopic, and impurity analyses that an applicant may specify as part included in this standard are two methods for the of his procedures for accounting for special nuclear determination of plutonium:

ma tenal.

1. Centrolled Potental Coulometry. The optimum quanuties of plutonium to be determmed are 2 to 6 mg B. DISCUSSION with a stated urecision of 0.14 percent relative standard deviation (RSD).

Committee C 26 on Fuel, Control, and Moderator Matenals for Nuclear Reactor Applications o; the

2. Amperometnc Titration with Iron (11). The American Society for Tesung and Materials (ASTM)has optimum quantities of plutonium to be determined are developed standards contairung methods for the 10 to 20 mg with a stated precision (f 0.03 to 0.06 chemical analysis of (1) nuclear-grade plutonium nitrate percent RSD and a bias of 0.02 percent or less.

solutions and (2) nuclear-grade plutonium metal. These standards are ASTM C759 73, " Standard Methods for This standard also includes a method for the

Chemical, Mass Spectrometric, Spactrochemical, determination of the absolute isotopic composition of Nuclar, and Radiochemical Analysis of Nuclear-Grade plutonium nitrate solutions allowing for the use of Plutonium Nitrate Solutions,"' and ASTM C758 73, reference standards to determme bias. The stated

" Standard Methods for Chemical, Mass Spectrometnc, precision of the method for Pu 239 at the 91%

Spectrochemical. Nuclear, and Radiochemical Analysis concentration level is 0.034% RSD, for Pu 240 at the of Nulear-Grade Plutonium Metal."' On June 20,1974, 7.97c concentration level, 0.la2ye RSD, fer Pu-241 at these standards were approved by the ANSI Board of the 0.63% concentrauon level, 0.978% RSD, and for Standards review and were designated ANSI N572-974 Pu-242 at the 0.0339 concentration level, 4.6% RSD.

(ASTM C758-73). " Chemical, Mass Spectrometric, Vanous impunties such as uramum, thonum, iron, Spectrochemical, Nuclear and Radiochemical Analpes chloride, fluoride, and sulfate can be determined using 1

' Copies may be obtained from de Amencan Society for Tesung 2

,1 Materuls.1916 Race Street, Philadelphia. Pennsylvania 19103.

Copies rnay b e obtained from the American National Standards

' Lines indicate subsunuve changes from prenous issue.

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tne methods that are included in this standard. Two Spectrochemical, Nuclear and Radiochemical Analysis of methods for the determ. nation of the free acid content Nuclear-Grade Plutonium Nitrate Solutions," and the of the plutonium nitrate solutions are also included in analytical methods for the measurement of nuclear-grade this standard plutonium metal contained in ASTM C758-73' or ANSI N572-1974, " Standard Methods for Chemical, Mass 2

P!utordum Metaj Spectrometnc, SpectroJtemical, Nuclear and Radiochemical Analysis of Nuclear Grade Plutonium Metal," are acceptabie to the NRC staff and provide included in this standa d are three methods for the an adequate basu for the assay,isotopc measurement, determination of plutoniun :

and impurity ana ysis of nuclear-grade plutonium nitrate i

solutions and plutoruum metal, subject to the fol!cwing:

1. Controlled. Potential Co 'lometry. The optimum quantities of plutonium to be o>termined are 2 to 6 mg w.th a stated precision of 0.14 p trcent relative s'.sndard
1. Precision and Accuracy Statements. The hsted deviation (RSD).

statements provide guidance to the le eels of performance which may be attained usi.. ine described methods. The

2. Ceric Sulfate Titration. The stated precision is actual precision ar.a accuracy of a raethod applied 0.27 percent RSD.

within a selected laboratory can only be aetermined through a well-planned measurement control program.

3. Amperometne Titration with iron (ll). The optimum quanutics of plutonium to be determined are
2. Calibration and Standardization. The standards 10 to 20 mg with a stated precisicn of 0.03 to 0.06 should be prepared in the same matrix as the samples, percent RSD and a bias of 0.02 percent oc less.

and the cabbracon pomts should bracket the estimated range of the samples.

This standard also includes a method for 'he deternunation of the absolute isotopic composition of

3. Safety. Pn. edures involvmg the use of perchioric plutcnium metal allowmg for the use of reference acsd in radiochemical hoods and glove boxes should be standards to determine bi's. The stated precision of the performed with caution because of the potential method for Pc-239 at the 91% concentration level is explosion and fire hazard.

0.034% RSD; for Pu-240 at the 7.9% concentratior' level, 0182% RSD; for Pu-241 at the 0.63 %

D. IMPLEMENTATION ccmcentrat2on level,0.978% R3D; and for Pu 242 at the 0.033 % concentration Irvel, 4.6% RSD. Various The r urpose of this section is to provide mformation impunties such as uranium, snorium, iron, chloride, to apphcants and licensees regarding the NRC staff's fluonde, nitrogen, carbon, suaur, and americium-241 plans for utilincg this regulatory guide.

on be deternuned using the methods that are included ir. this standard.

'Ihis guide reflects cur rent regulatory practice.

Therefore, except in those cases in which the applicant C. REG'JLATORY POSITION proposes an alternative method for complymg with specified portions of the Comm asion's regulations, the The analyucal methods for the measurement of method desenbed herein will be used in the evaluation nuclear-grade plutonium nitrate soluticos contained in of submittals in connection with special nuclear material ASTM C759 73' or ANSI N5731974, "Staadard license or operating license applications docketed after 2

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