significance And Use:

scope:

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 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

^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.