Method for testing content of oxygen in villaumite

A test method and technology for oxygen content, which are applied in measurement devices, material analysis by optical means, instruments, etc., can solve the problems of low relative standard deviation, low detection limit, high measurement lower limit, etc., to prevent the influence of moisture and oxygen, The effect of low relative standard deviation and high test accuracy

Active Publication Date: 2014-10-08
上海联和日环能源科技有限公司
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  • Abstract
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AI Technical Summary

Problems solved by technology

[0011] The technical problem to be solved by the present invention is to overcome the existing test method of oxygen content in fluorine salts, which requires high sample volume, high measurement lower limit, poor measurement repeatability, long time required for a single measurement, easy water absorption of samples and instrument corrosion. Serious and other defects, but provides a test method for oxygen content in fluoride salts
The test method of the present invention is an absolute determination method of oxygen, which can measure the total amount of oxygen elements in all forms in the sample to be tested; the amount of test samples is small, the detection limit is low, the measurement range is wide, the test accuracy is high, and the relative standard deviation is low. , sample preparation is convenient, and can well prevent samples from being affected by moisture and oxygen in the air during sample preparation and testing, and can solve the problem of corrosion of instruments by halogen-containing volatiles generated during sample heating, simple operation and fast measurement

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  • Method for testing content of oxygen in villaumite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] 1.1 Instruments and materials

[0042] American LECO oxygen analyzer model RO600 or RO836, including halogen trap, gas system, sample injector, high temperature furnace, detection system, etc.; glove box; electronic balance; tin capsule; high-purity graphite crucible; standard sample (steel) ; LiF single crystal; NaF powder sample.

[0043] 1.2 Analytical conditions

[0044] The oxygen analyzer uses nitrogen as the power gas, and the pressure is 0.28MPa ~ 0.29MPa. High-purity argon with water and oxygen content below 1ppm is used as the carrier gas, and the pressure is 0.15MPa. The power of the high temperature furnace is set to 2900W, and the degassing cycle is 3 times.

[0045] 1.3 Operation steps

[0046] Sample preparation: Put the capsule-shaped tin capsule on the electronic balance in the glove box, fill it with about 0.15g of NaF powder sample after peeling, fold and seal the capsule-shaped tin capsule after weighing and recording;

[0047] Start-up and para...

Embodiment 2

[0056] 2.1 Instruments and materials

[0057] American LECO oxygen analyzer, including halogen trap, gas system, sample injector, high temperature furnace, detection system, etc.; glove box; electronic balance; tin bag; high-purity graphite crucible; standard sample (lithium fluoride single crystal) ; LiF-NaF-KF (46.5-11.5-42 mol%) eutectic salt.

[0058] 2.2 Analysis conditions

[0059] The oxygen analyzer uses high-purity argon and high-purity nitrogen with an oxygen content of less than 1ppm as the carrier gas, the pressure is 0.15MPa and 0.28-0.29MPa respectively, the high-temperature furnace analysis power is set to 2500W, and the degassing cycle is 3 times.

[0060] 2.3 Operation steps

[0061] Sample preparation: Put the tin bag on the electronic balance in the glove box, put about 0.15g of LiF-NaF-KF powder sample into it after peeling, fold and seal the tin bag after weighing and recording;

[0062] Start-up and parameter setting: According to the operation require...

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Abstract

The invention discloses a method for testing the content of oxygen in villaumite. The method comprises the following steps: carrying out halogen removal on a sample to be tested by adopting an inert gas fusion process, and detecting the oxygen in villaumite, wherein monocrystalline lithium fluoride is used as a standard sample, and the sample to be tested has no contact with air in the preparation and test process of the sample to be tested. The testing method is an absolute oxygen determination method, has the advantages of small amount of the tested sample, low detection limit, wide determination range, high testing precision and low deviation, can prevent the water absorption or oxygen in the sample preparation process of villaumite, and can solve a problem that halogen-containing volatile matters generated in the heating of the sample corrode apparatuses.

Description

technical field [0001] The invention relates to a method for testing oxygen content in fluoride salts. Background technique [0002] Inorganic salts and their melts can be widely used as heat transfer and chemical reaction media because of their advantages such as large heat capacity, fast heat transfer, good fluidity, wide temperature range, and high solubility for substances. It has special application prospects in chemical industry, electrolytic metal, rare and precious metal smelting, three wastes treatment, emerging energy such as solar energy, hydrogen energy and nuclear energy. [0003] However, inorganic salts with low purity are highly corrosive to structural materials, which is one of the main factors limiting their applications. Taking fluorine molten salt as an example, a few hundred ppm of oxygen impurities will significantly enhance its corrosiveness. The higher oxygen content especially limits the application of fluorine salts in nuclear energy and the prepa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/3504
Inventor 赵素芳李明广谢雷东汪洋苏兴治
Owner 上海联和日环能源科技有限公司
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