Sample treatment method in measurement of calcium content of industrial silicon

A technology for sample processing and industrial silicon, which is used in the preparation of test samples and the measurement of color/spectral characteristics. It can solve the problems of inaccurate data, unstable calcium color rendering, large deviation, etc. Stable, small deviation effect

Inactive Publication Date: 2012-07-04
登封电厂集团铝合金有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method uses sulfuric acid fuming to remove silicon and fluorine, which takes a long time, and in this method, when calcium and chlorophosphine azo I form a colored complex, the pH value is controlled to be 10-10.5, but when the pH is 10-10.5 Within the range, the calcium color development is unstable, the deviation between parallel experiments is large, and the data is inaccurate

Method used

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  • Sample treatment method in measurement of calcium content of industrial silicon
  • Sample treatment method in measurement of calcium content of industrial silicon
  • Sample treatment method in measurement of calcium content of industrial silicon

Examples

Experimental program
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Effect test

Embodiment 1

[0011] According to the following method, in different laboratories, let different analysts determine the calcium content of the standard sample with a calcium content of 0.315% by mass:

[0012] 1. Weigh 0.1g of industrial silicon sample, add 5ml of hydrofluoric acid to the sample, then slowly add 3ml of nitric acid dropwise, heat until the industrial silicon sample dissolves, keep the heating state at 80-90°C and add 2ml of nitric acid again, Stop heating after the nitric acid fumes are exhausted, then add 10ml of hydrochloric acid aqueous solution and heat to dissolve the salts to obtain mixture 1. After the mixture 1 is cooled, make up the mixture 1 to 100ml with water, so that the final concentration of the industrial silicon sample is 1mg / ml. Obtain sample liquid 1, the volume percent of hydrochloric acid in hydrochloric acid aqueous solution is 25%;

[0013] 2. Take 5ml of sample solution 1, add 5ml of triethanolamine aqueous solution, the volume percentage of triethano...

Embodiment 2

[0019] According to the following method, in different laboratories, let different analysts determine the calcium content of the standard sample with a calcium content of 0.315% by mass:

[0020] 1. Weigh 0.5g of industrial silicon sample, add 5ml of hydrofluoric acid to the sample, then slowly add 5ml of nitric acid dropwise, heat until the industrial silicon sample dissolves, then add 2ml of nitric acid again while heating, and wait for the nitric acid to smoke. After that, stop heating, then add 10ml of hydrochloric acid aqueous solution and heat to dissolve the salts to obtain a mixture 1. After the mixture 1 is cooled, make up the mixture 1 to 100ml with water, so that the final concentration of the industrial silicon sample is 5mg / ml, and the sample solution 1 is obtained. , the volume percent of hydrochloric acid in the hydrochloric acid aqueous solution is 27%;

[0021] 2. Take 5ml of sample solution 1, add 5ml of triethanolamine aqueous solution, the volume percentage...

Embodiment 3

[0026] The contrast of embodiment 3 different sample processing methods

[0027] Using GB / T14849.3-2007 "Chlorophosphine Azo I Spectrophotometric Determination of Calcium Content" 16.4.1-16.4.6 as a contrast method, compared with the sample processing method during the determination of calcium content in industrial silicon of the present invention, the work The drawing of curve and data processing are the same as steps 3 and 4 in embodiment 1, and the standard sample of calcium content 0.315% by mass is analyzed and compared, and the results are as follows:

[0028]

[0029] As can be seen from the above table: the calcium content mass percentage measured by the control method is unstable, the standard deviation is 0.056%, and the deviation with the actual calcium content is also large, the average calcium content of the 6 groups of data is different from the actual The absolute deviation of the calcium content is 0.05%; adopt the sample processing method during the determi...

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Abstract

The invention relates to a sample treatment method in measurement of calcium content of industrial silicon, which is rapid, stable and accurate. The method comprises the following steps of: (1) weighing a industrial silicon sample, adding hydrofluoric acid to the sample and then adding dropwise nitric acid, heating until the industrial silicon sample is dissolved, keeping heating and adding nitric acid again, stopping heating until smoke disappears, adding an aqueous solution of hydrochloric acid, heating to dissolve salts to obtain a mixture 1, cooling the mixture 1, and diluting with water to obtain a liquid sample 1; and (2) adding an aqueous solution of triethanolamine into the liquid sample 1, then adding an aqueous solution of malachite green, adjusting pH with an aqueous solution of sodium hydroxide until green color disappears, adjusting pH to 12.8-13.2, adding an aqueous solution of arsenazo I to obtain a mixture 2, diluting the mixture 2 with water until the final concentration of the industrial silicon sample is 0.1-0.5 mg / mL, and standing at room temperature for 15-20 min.

Description

technical field [0001] The invention relates to a chemical sample processing method, in particular to a sample processing method for measuring calcium content in industrial silicon. Background technique [0002] At present, when measuring the calcium content in industrial silicon in GB / T14849.3-2007 "Chlorophosphine Azo I Spectrophotometric Determination of Calcium Content", the principle used is: industrial silicon samples use HF and HNO 3 Dissolve, remove silicon and fluorine by fuming sulfuric acid, dissolve the residue with hydrochloric acid, mask interfering elements with triethanolamine, 1,10-phenanthrene, and acetylacetone, and form a colored complex with calcium and chlorophosphine azo at pH 10-10.5 matter, with the EGTA-Pb faded solution as a reference, the absorbance was measured with a spectrophotometer. This method uses sulfuric acid fuming to remove silicon and fluorine, which takes a long time, and in this method, when calcium and chlorophosphine azo I form a ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/31G01N1/38G01N1/44
Inventor 刘勇王锋仝选歌梁克源李凌云何平华杨军锋胡爱娟崔春霞
Owner 登封电厂集团铝合金有限公司
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