Norm

ASTM C697 - 10 en

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

  • Deze norm is ingetrokken sinds 01-06-2016

73,70 89,18 Incl BTW

Over deze norm

Status Ingetrokken
Aantal pagina's 28
Gepubliceerd op 01-06-2010
Taal Engels

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 Array   Spectrophotometry
Nitrogen by Distillation Spectrophotometry Using Nessler
Reagent
11 to 18
Carbon (Total) by Direct CombustionThermal 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 CarrierDistillation Spectroscopy 56 to 63
Impurities by ICP-AES
Impurity Elements by Spark-Source Mass Spectrography64 to 70
Moisture by the Coulometric Electrolytic Moisture Analyzer71 to 78
Total Gas in Reactor-Grade Plutonium Dioxide Pellets79 to 86
Plutonium-238 Isotopic Abundance by Alpha Spectrometry
Americium-241 in Plutonium by Gamma-Ray Spectrometry
Rare Earths By Copper Spark-Spectroscopy87 to 96
Plutonium Isotopic Analysis by Mass Spectrometry97 to 105
Oxygen-To-Metal Atom Ratio by Gravimetry106 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

ElementWavelength, ÅConcentration
Range, ppm
Al2567.99A10500
Al3082.68A
Ag3280.681250
As2349.8410250
Au2427.952.550
B2497.73150
Ba4554.032.5100
(first order)
Be2348.610.525
Bi3067.722.5100
Ca3933.67101000
Cd2288.021100
Co2407.25101000
Co3044.00
Cu3247.541250
Cr2835.63A5500
Fe2983.57A101000
Ga2450.07A1500
Ga2943.64
In3039.362.5100
K7664.9131000
(first order)
Mg2802.7011000
Mn2798.275250
MoB3132.595250
Ni3002.49A101000
P2553.281001000
Pb2614.185100
Pd3242.702.5100
Sb2598.052.5100
Si2514.32A10300
Sn2863.332.5100
Sr4607.335100
(first order)
Ti3223.525100
VB3183.98A5100
WB2724.35A20200
Zn3345.0210250
Zr3438.235100

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.

Details

ICS-code 27.120.30
Engelse titel Standard Test Methods for Chemical, Mass Spectrometric, and Spectrochemical Analysis of Nuclear-Grade Plutonium Dioxide Powders and Pellets
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