Name: ASTM C 697 : 2010
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Standard Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Plutonium Dioxide Powders and Pellets

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11-11-2014

Superseded by

ASTM C 697 : 2016

Language(s)

English

Published date

01-06-2010

Publisher

American Society for Testing and Materials

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Committee	C 26
DocumentType	Test Method
Pages	28
PublisherName	American Society for Testing and Materials
Status	Superseded
SupersededBy	ASTM C 697 : 2016
Supersedes	ASTM C 697 : 2004

1.1 These test methods cover procedures for the chemical, mass spectrometric, and spectrochemical analysis of nuclear-grade plutonium dioxide powders and pellets to determine compliance with specifications.

1.2 The analytical procedures appear in the following order:

	Sections
Plutonium Sample Handling	8 to 10
Plutonium by Controlled-Potential Coulometry
Plutonium by Ceric Sulfate Titration
Plutonium by Amperometric Titration with Iron(II)
Plutonium by Diode ArraySpectrophotometry
Nitrogen by Distillation Spectrophotometry Using Nessler Reagent	11 to 18
Carbon (Total) by Direct Combustion–Thermal Conductivity	19 to 30
Total Chlorine and Fluorine by Pyrohydrolysis	31 to 38
Sulfur by Distillation Spectrophotometry	39 to 47
Plutonium Isotopic Analysis by Mass Spectrometry
Rare Earth Elements by Spectroscopy	48 to 55
Trace Elements by Carrier–Distillation Spectroscopy	56 to 63
Impurities by ICP-AES
Impurity Elements by Spark-Source Mass Spectrography	64 to 70
Moisture by the Coulometric Electrolytic Moisture Analyzer	71 to 78
Total Gas in Reactor-Grade Plutonium Dioxide Pellets	79 to 86
Plutonium-238 Isotopic Abundance by Alpha Spectrometry
Americium-241 in Plutonium by Gamma-Ray Spectrometry
Rare Earths By Copper Spark-Spectroscopy	87 to 96
Plutonium Isotopic Analysis by Mass Spectrometry	97 to 105
Oxygen-To-Metal Atom Ratio by Gravimetry	106 to 114

1.3 The values stated in SI units are to be regarded as standard. The values given in parentheses are for information only.

1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For specific precautionary statements, see Sections 6, 15, 24, 111, and 52.9 and 101.5.1 .

8.1 This test method covers the conditions necessary to preserve the integrity of plutonium dioxide samples. Conditions listed here are directed toward the analytical chemist. However, they are just as applicable to any group handling the material.

11.1 This test method covers the determination of 5 to 100 μg/g of nitride nitrogen in 1-g samples of nuclear-grade plutonium dioxide.

19.1 This test method covers the determination of 10 to 200 μg of residual carbon in nuclear-grade plutonium dioxide.

31.1 This test method covers the determination of 5 to 100 μg/g of chlorine and 1 to 100 μg/g of fluorine in 1-g samples of nuclear-grade plutonium dioxide.

39.1 This test method coves the determination of sulfur in the concentration range from 10 to 600 μg/g for samples of nuclear-grade plutonium dioxide powders or pellets.

48.1 This test method covers the determination of dysprosium, europium, gadolinium, and samarium in plutonium dioxide (PuO₂) in concentrations of 0.1 to 10 μg/g of PuO₂.

FIG. 5 Schematic Diagram of Atmosphere Chamber

56.1 This test method covers the determination of 36 impurity elements in nuclear-grade plutonium dioxide (PuO₂). The concentration ranges covered by the method and the analytical lines used for each element are listed in Table 1.

TABLE 1 Impurity Elements, Lines, and Concentration Limits

Element	Wavelength, Å	Concentration Range, ppm
Al	2567.99^A	10–500
Al	3082.68^A
Ag	3280.68	1–250
As	2349.84	10–250
Au	2427.95	2.5–50
B	2497.73	1–50
Ba	4554.03	2.5–100
	(first order)
Be	2348.61	0.5–25
Bi	3067.72	2.5–100
Ca	3933.67	10–1000
Cd	2288.02	1–100
Co	2407.25	10–1000
Co	3044.00
Cu	3247.54	1–250
Cr	2835.63^A	5–500
Fe	2983.57^A	10–1000
Ga	2450.07^A	1–500
Ga	2943.64
In	3039.36	2.5–100
K	7664.91	3–1000
	(first order)
Mg	2802.70	1–1000
Mn	2798.27	5–250
Mo^B	3132.59	5–250
Ni	3002.49^A	10–1000
P	2553.28	100–1000
Pb	2614.18	5–100
Pd	3242.70	2.5–100
Sb	2598.05	2.5–100
Si	2514.32^A	10–300
Sn	2863.33	2.5–100
Sr	4607.33	5–100
	(first order)
Ti	3223.52	5–100
V^B	3183.98^A	5–100
W^B	2724.35^A	20–200
Zn	3345.02	10–250
Zr	3438.23	5–100

^A These elements are determined with the aid of a microphotometer.

^B These elements are analyzed by using a AgCl carrier and PdCl₂ as an internal standard. Mix 20 mg of PdCl₂ with 10.0 g of AgCl. Add 80 mg of this mixture to 120 mg of PuO₂ sample-blend before loading 50-mg charges in a graphite electrode ASTM-Type-S-4 (follow 96.2.2).

71.1 This test method covers the determination of moisture in plutonium dioxide samples. Detection limits are as low as 10 μg.

79.1 This test method covers the measurement of volatiles other than water in reactor-grade plutonium dioxide pellets (16). The lower limit of the test method using the described equipment and a sample of approximately 1 g is 0.01 cm³ per gram of sample at STP conditions.

87.1 This test method covers the determination of rare earths in plutonium dioxide over the range from 10 to 200 μg/g.

97.1 This test method covers the determination of the isotopic composition of plutonium in nuclear-grade plutonium dioxide powders and pellets.

106.1 This test method is applicable to the determination of the oxygen-to-metal atom ratio (O/M) in plutonium dioxide pellets and powders.

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ASTM C 697 : 2010

Standard Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Plutonium Dioxide Powders and Pellets

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