ASTM-C697 2010

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C697-10 Standard Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Plutonium Dioxide Powders and Pellets

Published By	Publication Date	Number of Pages
ASTM	2010	28

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Categories: 27.120.30 - Fissile materials and nuclear fuel technology, ASTM

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Description

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:

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 ? g/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 ? g of residual carbon in nuclear-grade plutonium dioxide.

31.1 This test method covers the determination of 5 to 100 ? g/g of chlorine and 1 to 100 ? g/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 ? g/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 (PuO ₂ ) in concentrations of 0.1 to 10 ? g/g of PuO ₂ .

FIG. 5 Schematic Diagram of Atmosphere Chamber

56.1 This test method covers the determination of 36 impurity elements in nuclear-grade plutonium dioxide (PuO ₂ ). 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

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

^B These elements are analyzed by using a AgCl carrier and PdCl ₂ as an internal standard. Mix 20 mg of PdCl ₂ with 10.0 g of AgCl. Add 80 mg of this mixture to 120 mg of PuO ₂ 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 ? g.

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 cm ³ 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 ? g/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.

PDF Catalog

PDF Pages	PDF Title
1	Scope Referenced Documents
2	Significance and Use Committee C26 Safeguards Statement Reagents Safety Precautions
3	Sampling and Dissolution Scope Summary of Test Method Sample Handling Conditions Scope Summary of Test Method Apparatus Reagents
4	Precautions Procedure FIG. 1
5	Calculation Precision Scope Summary of Test Method Interferences Apparatus Reagents and Materials Safety Precautions
6	Sampling Preparation of Apparatus Calibration Procedure Calculation Precision Scope Summary of Test Method Interferences (see and )
7	Reagents FIG. 2 FIG. 3
8	Pyrohydrolysis Procedure Measurement of Chloride and Fluoride
9	Precision Scope Summary of Test Method Interference Apparatus Reagents
10	Calibration Procedure FIG. 4
11	Calculations Precision Scope Summary of Test Method Interferences Apparatus FIG. 5
12	Reagents Procedure FIG. 6
13	Calculation Precision Scope Summary of Test Method Apparatus TABLE 1
14	Reagents and Materials Calibration Procedure Calculation Precision and Bias Scope Summary of Test Methods
15	Apparatus Reagents Procedure Calculation
16	Precision and Bias Scope Summary of Test Method TABLE 2
17	Apparatus Reagents Operation Standardization Calculation Precision Scope Summary of Test Method Interferences Apparatus
18	Reagents Procedure FIG. 7 FIG. 8
19	Calculation FIG. 9
20	Precision and Bias Scope Summary of Test Method Apparatus Reagents and Materials
21	Procedure Photo Processing Photometry Calibration Calculation Precision and Bias Scope Summary of Test Method TABLE 3 TABLE 4
22	Interferences Apparatus Reagents Calibration of the Mass Spectrometer
23	Procedure
24	Calculation
25	Precision and Bias Scope Summary of Test Method Interferences Apparatus Reagents Safety Precautions Procedure
26	FIG. 10
27	Calculation Precision and Bias Keywords REFERENCES

Additional information

Be	2348.61
P	2553.28
As	2349.84
Plutonium Isotopic Analysis by Mass Spectrometry	97 to 105
Au	2427.95
Zn	3345.02
Zr	3438.23
Ni	3002.49 A
Plutonium by Diode Array Spectrophotometry
Plutonium by Controlled-Potential Coulometry
Ba	4554.03
Oxygen-To-Metal Atom Ratio by Gravimetry	106 to 114
Al	3082.68 A
K	7664.91
Bi	3067.72
Impurities by ICP-AES
Sb	2598.05
Rare Earth Elements by Spectroscopy	48 to 55
Si	2514.32 A
V B	3183.98 A
Ga	2943.64
Sn	2863.33
Ca	3933.67
Plutonium-238 Isotopic Abundance by Alpha Spectrometry
Sr	4607.33
Total Chlorine and Fluorine by Pyrohydrolysis	31 to 38
Moisture by the Coulometric Electrolytic Moisture Analyzer	71 to 78
Fe	2983.57 A
Nitrogen by Distillation Spectrophotometry Using Nessler Reagent	11 to 18
Ti	3223.52
Cd	2288.02
Plutonium Sample Handling	8 to 10
Carbon (Total) by Direct Combustion Thermal Conductivity	19 to 30
Co	3044.00
Cr	2835.63 A
Total Gas in Reactor-Grade Plutonium Dioxide Pellets	79 to 86
Cu	3247.54
Pb	2614.18
Sulfur by Distillation Spectrophotometry	39 to 47
Pd	3242.70
Rare Earths By Copper Spark-Spectroscopy	87 to 96
Plutonium by Ceric Sulfate Titration
W B	2724.35 A
Americium-241 in Plutonium by Gamma-Ray Spectrometry
Mg	2802.70
Plutonium by Amperometric Titration with Iron(II)
Trace Elements by Carrier Distillation Spectroscopy	56 to 63
Mo B	3132.59
Mn	2798.27
B	2497.73
In	3039.36
Ag	3280.68
Impurity Elements by Spark-Source Mass Spectrography	64 to 70
ICS Codes	27.120.30 - Fissile materials and nuclear fuel technology
	(first order)

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