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a tir x and/or vr y The sample preparation method and detection method of the material

A material and sample technology, applied in the field of sample preparation and detection of materials containing TiRx and/or VRy, can solve problems such as easy water absorption and easy oxidation, and achieve the effect of solving water absorption or oxidation and reducing analysis errors

Inactive Publication Date: 2016-11-16
PANZHIHUA IRON & STEEL RES INST OF PANGANG GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a TiR-containing x and / or VR y The sample preparation method and detection method of the material

Method used

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  • a tir <sub>x</sub> and/or vr <sub>y</sub> The sample preparation method and detection method of the material

Examples

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Effect test

Embodiment 1

[0040] KCl-NaCl-TiCl 3 Electrolyte (the molar ratio of KCl to NaCl is 1:1, TiCl 3 content of 4.50wt%) 100g and acetone 200g are placed in the ball mill, the number of balls is 100, the particle diameters of the balls are 5mm, 10mm, 20mm and 40mm respectively, and the number ratio distribution is 12:5:2 : 1, after ball milling 2h, obtain the material that particle diameter is 45-95 μ m, the material after ball milling is carried out the reduction operation according to the reduction grade of 1 / 8 and obtains solid-liquid sample 50g, distills and removes acetone under argon protective atmosphere, uses Determination of TiCl by titration analysis 3 The content of is 4.45%, calculates error rate by formula (1) 1.1%.

Embodiment 2

[0042] KCl-NaCl-VCl 4 Electrolyte (among them, the molar ratio of KCl to NaCl is 1:1, VCl 4 content of 5.50wt%) 100g and butanone 400g are placed in the ball mill, the number of the balls is 200, and the particle diameters of the balls are respectively 2mm, 8mm, 16mm and 25mm, and the number ratio distribution is 9:7: 3:1, after ball milling for 1.5 hours, a material with a particle size of 75-100 μm was obtained, and the material after ball milling was subjected to a reduction operation according to a reduction grade of 1 / 8 to obtain 50 g of a solid-liquid sample. Ketones, determination of VCl by titration analysis 4 The content of is 5.39%, calculates error rate by formula (1) 2%.

Embodiment 3

[0044] KCl-NaCl-TiCl 2 Electrolyte (the molar ratio of KCl to NaCl is 1:1, TiCl 2 The content is 4.5wt%) 100g and acetone 800g are placed in the ball mill, the number of balls is 300, the ball diameters are respectively 2mm, 5mm, 10mm and 15mm, and the number ratio distribution is 9:8:2: 1. After ball milling for 2.5 hours, a material with a particle size of 48-70 μm was obtained. The material after ball milling was subjected to a reduction operation according to a reduction grade of 1 / 8 to obtain 112.5 g of a solid-liquid sample, and acetone was distilled off under an argon protective atmosphere. Determination of TiCl by Titration Analysis 2 The content of is 4.43wt%, calculates error rate by formula (1) 1.6%.

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Abstract

The invention discloses a TiR-containing x and / or VR y The sample preparation method of the material, wherein, R is a halogen atom, x is the integer of 2-3, y is the integer of 2-4, and the method comprises the following steps: (1) will contain TiR x and / or VR y The material and the ketone compound are subjected to wet ball milling, wherein the ketone compound is a compound shown in formula (I), R 1 COR 2 (I), in formula (I), R 1 with R 2 The same or different, each independently being an alkyl group with 1-20 carbon atoms, a cycloalkyl group with 3-20 carbon atoms and an aryl group with 6-20 carbon atoms; (2) the Step (1) shrinking the material obtained after wet ball milling in a shrinking device; (3) removing ketone compounds in the material obtained after step (2) shrinking. The method of the invention effectively solves the problem of water absorption or oxidation of materials containing low-valent titanium or vanadium in the process of sample preparation and detection, and greatly reduces the final analysis error.

Description

technical field [0001] The invention relates to a TiR-containing x and / or VR y The sample preparation method of the material and the TiR-containing x and / or VR y TiR in the material x and / or VR y content detection method. Background technique [0002] At present, compounds containing low-valent titanium or vanadium are widely used in chemical industry, metallurgy and other fields, such as titanium trichloride vanadium removal agent in aluminum powder removal of vanadium, electrolyte KCl-NaCl-TiCl selected for electrolysis of titanium molten salt x system, the use of low-valent titanium or vanadium to synthesize organic heterocyclic compounds, etc., all of which are due to the strong reducibility and ion conductivity of low-valent titanium or vanadium. [0003] However, due to the strong reducibility of low-priced titanium or vanadium, it is easy to absorb water or oxidize and deteriorate during the process of sample preparation and detection, which increases the final ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N1/28G01N31/16
Inventor 付晓林
Owner PANZHIHUA IRON & STEEL RES INST OF PANGANG GROUP