ASTM C696-11

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

ASTM International , 09/01/2011

Publisher: ASTM

File Format: PDF

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Description

Standard By:ASTM International , 09/01/2011

Published:09/01/2011

Pages:11

File Size:1 file , 150 KB

Language:English

Note:This product is unavailable in Russia, Ukraine, Belarus

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

1.2 The analytical procedures appear in the following order:

	Sections

Uranium by Ferrous Sulfate Reduction in Phosphoric Acid and Dichromate Titration Method
C1267 Test Method for Uranium By Iron (II) Reduction In Phosphoric Acid Followed By Chromium (VI) Titration In The Presence of Vanadium
Uranium and Oxygen Uranium Atomic Ratio by the Ignition (Gravimetric) Impurity Correction Method
C1453 Standard Test Method for the Determination of Uranium by Ignition and Oxygen to Uranium Ratio (O/U) Atomic Ratio of Nuclear Grade Uranium Dioxide Powders and Pellets
Carbon (Total) by Direct Combustion-Thermal Conductivity Method
C1408 Test Method for Carbon (Total) in Uranium Oxide Powders and Pellets By Direct Combustion-Infrared Detection Method
Total Chlorine and Fluorine by Pyrohydrolysis Ion-Selective Electrode Method
C1502 Standard Test Method for the Determination of Total Chlorine and Fluorine in Uranium Dioxide and Gadolinium Oxide
Moisture by the Coulometric, Electrolytic Moisture Analyzer Method	7-14
Nitrogen by the Kjeldahl Method	15-22
Isotopic Uranium Composition by Multiple-Filament Surface Ionization Mass Spectrometric Method
Spectrochemical Determination of Trace Elements in High-Purity Uranium Dioxide	23-30
Silver, Spectrochemical Determination of, by Gallium OxideCarrier D-C Arc Technique	31 and 32
Rare Earths by Copper Spark-Spectrochemical Method
Impurity Elements by a Spark-Source Mass Spectrographic Method
C761 Test Method for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Uranium Hexafluoride
C1287 Test Method for Determination of Impurities In Uranium Dioxide By Inductively Coupled Plasma Mass Spectrometry
Surface Area by Nitrogen Absorption Method	33-39
Total Gas in Reactor-Grade Uranium Dioxide Pellets
Thorium and Rare Earth Elements by Spectroscopy
Hydrogen by Inert Gas Fusion
C1457 Standard Test Method for Determination of Total Hydrogen Content of Uranium Oxide Powders and Pellets by Carrier Gas Extraction
Uranium Isotopic Analysis by Mass Spectrometry
C1413 Test Method for Isotopic Analysis of Hydrolysed Uranium Hexafluoride and Uranyl Nitrate Solutions By Thermal Ionization Mass Spectrometry

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

15.1 This test method covers the determination of nitride nitrogen in uranium dioxide in the range from 10 to 250 μg.

23.1 This test method covers the spectrographic analysis of nuclear-grade UO₂ for the 26 elements in the ranges indicated in Table 1.

23.2 For simultaneous determination of trace elements by plasma emission spectroscopy refer to Test Method C761.

TABLE 1 Recommended Analytical Spectral Lines and Concentration Range of Trace Elements

Element	Analytical Line, °A^A	Concentration range, μg/g of U
Ag^B	3280.68	0.1 to 50
Al	2367.06	10 to 200
As	2349.84	5 to 50
B	2497.73	0.10 to 5
Ba	4554.04	10 to 300
Be	2348.61	0.1 to 3
Bi	3067.72	5 to 50
Ca	4226.73	1 to 50
Cd	2288.02	0.15 to 5
Co	3453.51	5 to 50
Cr	2843.25	10 to 100
Cu	3247.54	1 to 10
Fe	2462.64	10 to 300
In	3256.09	5 to 50
Mg	2779.83	10 to 100
Mn	2605.69	5 to 50
Mo	3132.59	0.5 to 10
Na	3302.32	80 to 400
Ni	3050.82	5 to 100
P	2553.28	50 to 500
Pb	2833.07	5 to 50
Sb	2598.05	1 to 50
Si	2435.16	10 to 200
Sn	3175.02	5 to 50
Ti	3361.26	1 to 100
V	3183.41	1 to 100
Zn	3345.02	20 to 300
Zr	3438.23	25 to 300

^A All of the above lines are photographed in the second order, except barium and calcium which are first order lines.

^B A gallium oxide carrier must be used for silver. See Test Method E402.

31.1 This test method covers the spectrochemical determination of silver in nuclear-grade uranium dioxide. The relative standard deviation is 15 % for the concentration range of 0.1 to 50 μg/g.

33.1 This procedure is designed for a rapid determination of surface area of nuclear-grade uranium dioxide (UO₂) powders. The determination of surface area by this procedure is automatic, simple, and fast enough to be used in quality control work. The range of analysis is from 1 to 1500 m²/g.