Method for measuring content of tellurium in antimony and antimonous oxide

A technology for the determination of antimony trioxide and its determination method, which is applied in the preparation of test samples and the measurement of color/spectral characteristics, and can solve the problems of no tellurium determination method for antimony and antimony trioxide, and achieve fast determination speed and analysis efficiency High and accurate effect

Active Publication Date: 2014-09-10
锡矿山闪星锑业有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, in the entire antimony industry, there is no method for the determination o...

Method used

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  • Method for measuring content of tellurium in antimony and antimonous oxide
  • Method for measuring content of tellurium in antimony and antimonous oxide
  • Method for measuring content of tellurium in antimony and antimonous oxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] In this embodiment, it is determined by an inductively coupled plasma emission spectrometer.

[0047] (1) Sample handling

[0048] a. Antimony sample

[0049]Weigh 0.5005g of antimony sample and place it in a 100mL beaker, dissolve it with 5mL of aqua regia, add 2mL of sulfuric acid, 5mL of hydrobromic acid and heat it on a low-temperature electric furnace. Below 80°C; Add 1mL of hydrochloric acid and 5mL of hydrobromic acid, heat to 200°C-340°C until white smoke comes out, then cool to below 80°C. Repeatedly add 1mL of hydrochloric acid and 5mL of hydrobromic acid, heat to 200°C-340°C, emit white smoke (only residue remains at this time), and cool to room temperature. Add 2mL of hydrochloric acid to dissolve the residue at 95°C-100°C, transfer the solution into a 10mL volumetric flask, dilute with water to the mark, and mix well.

[0050] b. Antimony trioxide sample

[0051] Weigh 0.5010g of antimony trioxide sample into a 100mL beaker, dissolve it with 5mL of hydr...

Embodiment 2

[0074] The present embodiment is determined by flame atomic absorption spectrometer.

[0075] (1) Sample handling

[0076] a. Antimony sample

[0077] Weigh 1.0008g of antimony sample and place it in a 100mL beaker, dissolve it with 5mL of aqua regia, add 2mL of sulfuric acid, 5mL of hydrobromic acid and heat it on a low-temperature electric furnace. Below 80°C; add 1mL hydrochloric acid, 5mL hydrobromic acid, heat to 200°C-340°C, until white smoke comes out, cool to below 80°C; add 1mL hydrochloric acid, 5mL hydrobromic acid repeatedly, heat to 200°C-340°C, Exhaust white smoke (only the residue remains at this time), cool to room temperature; add 2mL hydrochloric acid to dissolve the residue at 95°C-100°C, transfer the solution into a 10mL volumetric flask, dilute to the mark with water, and mix well.

[0078] b. Antimony trioxide sample

[0079] Weigh 1.0010g of antimony trioxide sample into a 100mL beaker, dissolve it with 5mL of hydrochloric acid, add 2mL of sulfuric ac...

Embodiment 3

[0102] In this embodiment, it is measured by an inductively coupled plasma emission spectrometer.

[0103] (1) Sample handling

[0104] a. Antimony sample

[0105] Weigh 1.0011g of antimony sample and place it in a 100mL beaker, dissolve it with 5mL of aqua regia, add 2mL of sulfuric acid, 5mL of hydrobromic acid and heat it on a low-temperature electric furnace. Below 80°C. Add 1mL of hydrochloric acid and 5mL of hydrobromic acid, heat to 200°C to 340°C until white smoke comes out, and cool to 80°C. Repeatedly add 1mL of hydrochloric acid and 5mL of hydrobromic acid, heat to 200°C-340°C, emit white smoke (only residue remains at this time), and cool to room temperature. Add 2mL of hydrochloric acid to dissolve the residue at 95°C-100°C, transfer the solution into a 10mL volumetric flask, dilute with water to the mark, and mix well.

[0106] b. Antimony trioxide sample

[0107]Weigh 1.0015g of antimony trioxide sample into a 100mL beaker, dissolve it with 5mL of hydrochlo...

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Abstract

The invention relates to a method for measuring the content of tellurium in antimony and antimonous oxide. The method comprises the steps of dissolving antimony through chloroazotic acid or dissolving antimonous oxide through hydrochloric acid, then adding sulfuric acid and hydrobromic acid for volatilizing antimony under the temperature of 200-340 DEG C, repeatedly adding hydrochloric acid and bromic acid, heating under low temperature to volatilize and remove antimony, adding hydrochloric acid to dissolve residues, and performing dilution to make up to the volume; measuring a standard tellurium solution through an electric inductance coupling plasma emission spectrometer or a flame atom absorption spectrometer and drawing a working curve, then measuring the emission spectrum intensity or the absorbancy of an impurity, namely tellurium in a test sample, and constructing methods for analyzing tellurium in antimony and antimonous oxide in sequence according to a linear relation between concentration of tellurium and the emission spectrum intensity or the absorbancy in a certain concentration range; and calculating the concentration of tellurium in test liquid according to the working curve of the measured standard tellurium solution, and further calculating the mass percentage of tellurium. The method disclosed by the invention has the advantages of high sensitivity, high precision, high accuracy, wide linear range, high analysis efficiency and the like.

Description

technical field [0001] The invention relates to a method for measuring tellurium content, in particular to a method for measuring tellurium content in antimony and antimony trioxide. Background technique [0002] Antimony trioxide is widely used in industry, and is often used as a flame retardant synergist for polyethylene, polypropylene, polystyrene, polyvinyl chloride, nylon, engineering plastics (ABS), rubber, paint, coating, synthetic resin , paper and other materials; as a defoamer for melting glass, removing air bubbles, and as a catalyst in polyester fibers; as a passivator for heavy oil, residual oil, catalytic cracking, and catalytic reforming in petroleum; as a passivator A white pigment, which can be used in paint and other industries, and can prepare various antimonides. For the application fields with color requirements, whiteness is an important quality index of antimony trioxide products. Antimony is used as a raw material for the production of antimony trio...

Claims

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Application Information

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IPC IPC(8): G01N21/25G01N21/31G01N1/28
Inventor 宗屹宋应球毛晓红
Owner 锡矿山闪星锑业有限责任公司
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