Regulatory Guide 5.16
| ML12191A018 | |
| Person / Time | |
|---|---|
| Issue date: | 05/31/1975 |
| From: | Office of Nuclear Regulatory Research |
| To: | |
| References | |
| RG-5.016, Rev. 1 | |
| Download: ML12191A018 (2) | |
Revision 1 U.S. NUCLEAR REGULATORY COMMISSION May 1975 REGULATORY GUIDE W/
OFFICE OF STANDARDS DEVELOPMENT
REGULATORY GUIDE 5.16 STANDARD METHODS FOR CHEMICAL, MASS SPECTROMETRIC,
SPECTROCHEMICAL, NUCLEAR, AND RADIOCHEMICAL ANALYSIS OF
NUCLEAR-GRADE PLUTONIUM NITRATE SOLUTIONS AND PLUTONIUM METAL
A. INTRODUCTION
of Nuclear-Grade Plutonium Metal,"2 and ANSI
N573-1974 (ASTM C759-73), "Chemical, Mass Paragraph (b) of Section 70.22, "Contents of Spectrometric, Spectrochemical, Nuclear and Applications," of 10 CFR Part 70, "Special Nuclear Radiochemical Analysis of Nuclear-Grade Plutonium Material," requires an applicant for a license to possess Nitrate Solutions."2 As used in these standards, certain quantities of special nuclear material in an nuclear-grade material means material that is to be used unsealed form to describe, among other things, his exclusively for the fabrication of nuclear fuel.
procedures for control of and accounting for special nuclear material. This guide identifies methods Plutonium Nitrate Solutions acceptable to the NRC staff for chemical, isotopic, and impurity analyses that an applicant may specify as part Included in this standard are two methods i'or the of his procedures for accounting for special nuclear determination of plutonium:
material.
1. Controlled-Potential Coulometry. The optimum quantities of plutonium to be determined are 2 to 6 mg
B. DISCUSSION
with a stated precision of 0.14 percent relative standard deviation (RSD).
Committee C-26 on Fuel, Control, and Moderator Materials for Nuclear Reactor Applications of the 2. Amperome.tric Titration with Iron (II). The American Society for Testing and Materials (ASTM) has optimum quantities of plutonium to be determined are developed standards containing methods for the 10 to 20 mg with a stated precision of 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 phltonium metal.. These standards are ASTM C759-73, "Standard Methods for This standard also includes a method for the Chemical, Mass Spectrometric, Spectrochemical, determination of the absolute isotopic composition of Nuclear, and Radiochemical Analysis of Nuclear-Grade plutonium nitrate solutions allowing for the use of Plutonium Nitrate Solutions," 1 and ASTM C758-73, reference standards to determine bia
s. The stated
"Standard Methods for Chemical, Mass Spectrometric, 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 Nuclear-Grade Plutonium Metal."' On June 20, 1974, 7.9% concentration level, 0.182% RSD; for Pu-241 at these standards were approved by the ANSI Board of the 0.63% concentration level, 0.978% RSD; and for Standards review and were designated ANSI N572-1974 Pu-242 at the 0.033% concentration level, 4.6% RSD.
(ASTM C758-73), "Chemical, Mass Spectrometric, Various impurities such as uranium, thorium, iron, Spectrochemical, Nuclear and Radiochemical Analyses chloride, fluoride, and sulfate can be determined using ICopies may be obtained from the American Society for Testing Materials, 1916 Race Street, Philadelphia, Pennsylvania 19103. 2 Copies may be obtained from the American National Standards
- Lines indicate substantive changes from previous issue. Institute, Inc., 1430 Broadway, New York, New York 10018.
USNRC REGULATORY GUIDES Comments should be sent to the Secretary of the Commission. U.S. Nuclear Regulatory Commission. Washington. D.C. 20555. Attention: Docketing and Regulatory Guides are issued to describe and make available to the public Service Section.
methods acceptable to the NRC staff of implementing specific parts of the Commission's regulations, to delineate techniques used by the staff in evalu- The guides are issued in the following ten broad divisions:
ating specific problems or postulated accidents, or to provide guidance to appli cants. Regulatory Guides are not substitutes tor regulations. and compliance 1. Power Reactors 6. Products with them is not required. Methods and solutions different from those set out in 2. Research and Test Reactors 7. Transportation the guides will be acceptable if they provide a basis for the findings requisite to 3. Fuels and Materials Facilities 8. Occupational Health the issuance or continuance of a permit or license by the Commission. 4. Environmental and Siting 9. Antitrust Review Comments and suggestions for improvements in these guides are encouraged 5. Materials and Plant Protection 10. General at all times, and guides will be revised, as appropriate, to accommodate comr ments and to reflect new information or experience. However. comments on Copies of published guides may be obtained by written request indicating the this guide, if received within about two months after its issuance, will be par- divisions desired to the U.S. Nuclear Regulatory Commission. Washington, D.C.
ticularly useful in evaluating the need for an early revision. 20555. Attention: Director. Office of Standards Development.
the methods that are included in this standard. Two Spectrochemical, Nuclear and Radiochemical Analysis of methods for the determination 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 2 , "Standard Methods for Chemical, Mass Plutonium Metal Spectrometric, Spectrochemical, Nuclear and Radiochemical Analysis of Nuclear-Grade Plutonium
-Metal," are acceptable to the NRC staff and provide Included in this standard are three methods for the an adequate basis for the assay, isotopic measurement, determination of plutonium: and impurity analysis of nuclear-grade plutonium nitrate solutions and plutonium metal, subject to the following:
1. Controlled-Potential Coulometry. The optimum quantities of plutonium to be determined are 2 to 6 mg with a stated precision of 0.14 percent relative-standard 1. Precision and Accuracy Statements. The listed deviation (RSD). statements provide guidance to the levels of performance which may be attained using the described methods. The
2. Ceric Sulfate Titration. The stated precision is actual precision and accuracy of a method applied
0.27 percent RSD. within a selected laboratory can only be determined through a well-planned measurement control program.
3. Amperometric Titration with Iron(II). The optimum quantities of plutonium to be determined are 2. Calibration and Standardizatio
n. The standards
10 to 20 mg with a stated precision 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 or less. and the calibration points should bracket the estimated range of the samples.
This standard also includes a method for the determination of the absolute isotopic composition of 3. Safety. Procedures involving the use of perchloric plutonium metal allowing for the use of reference acid in radiochemical hoods and glove boxes should be standards to determine bias. The stated precision of the performed with caution because of the potential method for Pu-239 at the 91% concentration level is explosion and fire hazard.
0.034% RSD; for Pu-240 at the 7.9% c6ncentration level, 0.182% RSD; for Pu-241 at the 0.63%
D. IMPLEMENTATION
concentration level, 0.978% RSD; and for Pu-242 at the
0.033% concentration level, 4.6% RSD. Various impurities such as uranium, thorium, iron, chloride, fluoride, nitrogen, carbon, sulfur, and americium-241 can be determined using the methods that are included The purpose of this section is to provide information to applicants and licensees regarding the NRC staff's plans for utilizing this regulatory guide.
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in this standard. This guide reflects current regulatory practice.
Therefore, except in those cases in which the applicant
C. REGULATORY POSITION
proposes an alternative method for complying with specified portions of the Commission's regulations, the The analytical methods for the measurement of method described herein will be used in the evaluation nuclear-grade plutonium nitrate solutions contained in of submittals in connection with special nuclear material ASTM C759-73' or ANSI N573-1974 2 , "Standard license or operating license applications docketed after Methods for Chemical, Mass Spectrometric, this guide is issued.
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