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ASTM C696-11

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

Automaticky preložený názov:

Štandardné skúšobné metódy pre chemický, hmotnostná spektrometria a spectrochemical analýza jadrových uránu uhličitého práškov a peliet

NORMA vydaná dňa 1.9.2011

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Informácie o norme:

Označenie normy: ASTM C696-11
Poznámka: NEPLATNÁ
Dátum vydania normy: 1.9.2011
Kód tovaru: NS-14644
Počet strán: 11
Približná hmotnosť: 33 g (0.07 libier)
Krajina: Americká technická norma
Kategória: Technické normy ASTM

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Anotácia textu normy ASTM C696-11 :

Keywords:
impurity content, isotopic composition, stoichiometry, uranium content, uranium dioxide: Carbon content--nuclear materials, Chemical analysis--nuclear materials, Atomic ratio--uranium dioxide (powders and pellets), Chlorine content--nuclear materials/applications, Fluoride content, Fluorine content, Gases--radioactive, Dichromate titration, Hydrogen content--nuclear materials, Ferrous sulfate reduction, Ignition--rubber/cellular materials, Ignition impurity correction method

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Significance and Use

Uranium dioxide is used as a nuclear-reactor fuel. In order to be suitable for this purpose, the material must meet certain criteria for uranium content, stoichiometry, isotopic composition, and impurity content. These test methods are designed to show whether or not a given material meets the specifications for these items as described in Specifications C753 and C776.

An assay is performed to determine whether the material has the minimum uranium content specified on a dry weight basis.

The stoichiometry of the oxide is useful for predicting its sintering behavior in the pellet production process.

Determination of the isotopic content of the uranium in the uranium dioxide powder is made to establish whether the effective fissile content is in compliance with the purchaser's specifications.

Impurity content is determined to ensure that the maximum concentration limit of certain impurity elements is not exceeded. Determination of impurities is also required for calculation of the equivalent boron content (EBC).

1. Scope

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.

2. Referenced Documents

C1408-16	Standard Test Method for Carbon (Total) in Uranium Oxide Powders and Pellets By Direct Combustion-Infrared Detection Method
C1413-18	Standard Test Method for Isotopic Analysis of Hydrolyzed Uranium Hexafluoride and Uranyl Nitrate Solutions by Thermal Ionization Mass Spectrometry
E402-02	Standard Test Method for Spectrographic Analysis of Uranium Oxide (U₃O₈)by Gallium Oxide-Carrier Technique (Withdrawn 2007)
E130-08	Standard Practice for Designation of Shapes and Sizes of Graphite Electrodes (Withdrawn 2013)
E115-97	Standard Practice for Photographic Processing in Optical Emission Spectrographic Analysis (Withdrawn 2002)
D1193-06(2018)	Standard Specification for Reagent Water
C1287-18	Standard Test Method for Determination of Impurities in Nuclear Grade Uranium Compounds by Inductively Coupled Plasma Mass Spectrometry
C753-16a(2021)	Standard Specification for Nuclear-Grade, Sinterable Uranium Dioxide Powder (Includes all amendments and changes 10/22/2021).
C1457-18	Standard Test Method for Determination of Total Hydrogen Content of Uranium Oxide Powders and Pellets by Carrier Gas Extraction
C1502-16	Standard Test Method for Determination of Total Chlorine and Fluorine in Uranium Dioxide and Gadolinium Oxide
C1347-08(2023)	Standard Practice for Preparation and Dissolution of Uranium Materials for Analysis
C776-17(2022)	Standard Specification for Sintered Uranium Dioxide Pellets for Light Water Reactors
C1453-19	Standard Test Method for the Determination of Uranium by Ignition and the Oxygen to Uranium (O/U) Atomic Ratio of Nuclear Grade Uranium Dioxide Powders and Pellets
C1267-17(2022)	Standard Test Method for Uranium by Iron (II) Reduction in Phosphoric Acid Followed by Chromium (VI) Titration in the Presence of Vanadium
C761-18	Standard Test Methods for Chemical, Mass Spectrometric, Spectrochemical, Nuclear, and Radiochemical Analysis of Uranium Hexafluoride

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