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Method for measuring content of phosphorus in sintered flux

A technology for sintering flux and measuring method, applied in material excitation analysis, thermal excitation analysis and other directions, can solve the problem of difficult phosphorus content, improve accuracy and precision, avoid working curve drift and low result system, solve The effect of long-term low accuracy

Inactive Publication Date: 2015-07-29
武汉钢铁有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In order to solve the difficult problem of determining the phosphorus content in the sintered flux, the present invention provides a method for determining the phosphorus content in the sintered flux, by adding reagents to the sintered flux and performing a certain treatment to prepare the sample solution to be tested at a constant volume , using state-of-the-art high-frequency inductively coupled plasma emission spectrometry to directly determine the phosphorus content in sintered flux

Method used

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  • Method for measuring content of phosphorus in sintered flux
  • Method for measuring content of phosphorus in sintered flux
  • Method for measuring content of phosphorus in sintered flux

Examples

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Effect test

Embodiment 1

[0028] 1) The sintered flux used by Baoji Yusheng Flux Factory was used as sample 1#.

[0029] 2) Weigh 0.5000g of sample 1#, place it in a 300mL polytetrafluoroethylene beaker, moisten it with a small amount of water, add nitric acid and hydrofluoric acid, heat at low temperature for 20 minutes, add hydrochloric acid, and continue heating for 30 minutes. The volume ratio of nitric acid, hydrofluoric acid, and hydrochloric acid is 1:1:4, add 5mL perchloric acid, heat at low temperature until perchloric acid fumes, and continue heating until the volume is about 2mL. Continue to add 5mL of perchloric acid, heat at low temperature and smoke perchloric acid until nearly dry. Cool slightly, add 10mL hydrochloric acid (1+9), rinse the wall of the cup with a small amount of water, heat for 5min to dissolve the salt, remove it, and cool to room temperature. Filter with slow filter paper with a small amount of pulp, rinse the beaker and precipitate with hot water for 5-6 times, and ke...

Embodiment 2

[0034]1) Use the sintered flux used by Luoyang Peony Flux Factory as sample 2#.

[0035] 2) Weigh 1.0000g of sample 2#, place it in a 300mL polytetrafluoroethylene beaker, moisten it with a small amount of water, add nitric acid and hydrofluoric acid, heat at low temperature for 20 minutes, add hydrochloric acid, and continue heating for 30 minutes. The volume ratio of nitric acid, hydrofluoric acid, and hydrochloric acid is 1:1:6, add 5mL perchloric acid, heat at low temperature until perchloric acid fumes, and continue heating until the volume is about 2mL. Continue to add 8mL of perchloric acid, heat at low temperature and smoke perchloric acid until nearly dry. Cool slightly, add 15mL hydrochloric acid (1+9), rinse the wall of the cup with a small amount of water, heat for 5min to dissolve the salt, remove it, and cool to room temperature. Filter with slow filter paper with a small amount of pulp, rinse the beaker and precipitate with hot water for 5-6 times, and keep the...

Embodiment 3

[0040] 1) The sintered flux used by Wuhan Iron Anchor is used as sample 3#.

[0041] 2) Weigh 0.8000g of sample 3#, place it in a 300mL polytetrafluoroethylene beaker, moisten it with a small amount of water, add nitric acid and hydrofluoric acid, heat at low temperature for 20 minutes, add hydrochloric acid, and continue heating for 30 minutes. The volume ratio of nitric acid, hydrofluoric acid, and hydrochloric acid is 1:1:5, add 8mL perchloric acid, heat at low temperature until perchloric acid fumes, and continue heating until the volume is about 2mL. Continue to add 3mL of perchloric acid, heat at low temperature and smoke perchloric acid until it is almost dry. Cool slightly, add 12mL of hydrochloric acid (1+9), rinse the wall of the cup with a small amount of water, heat for 5min to dissolve the salt, remove it, and cool to room temperature. Filter with slow filter paper with a small amount of pulp, rinse the beaker and precipitate with hot water for 5-6 times, and kee...

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Abstract

The invention discloses a method for measuring the content of phosphorus in sintered flux. The method comprises the following steps: (1) acid solution treatment of the sintered flux; (2) secondary perchloric acid smoking treatment; (3) alkali fusion recovery treatment of acid solution residues; (4) working curve creation and result measurement. According to the method, a reagent is added into the sintered flux, the sintered flux is treated to a certain extent, a to-be-tested sample solution with the constant volume is prepared, and the content of phosphorus in the sintered flux is directly measured with a high-frequency inductively coupled plasma emission spectrometry method in the prior art. The method is convenient, quick, easy to operate, high in accuracy for measuring the content of phosphorus and suitable for measuring the content of phosphorus in the sintered flux in production and scientific research. The method is accurate in system quantification, effectively solves a problem of relatively low accuracy of a sintered flux sample result in conventional production for a long term, effectively improves the accuracy and precision of an analytic result, and is environment-friendly.

Description

technical field [0001] The invention relates to the technical fields of chemistry and metallurgy, in particular to a method for determining phosphorus content in sintered flux. Background technique [0002] Sintered flux is widely used in the welding of steel structures such as bridges, boilers, and pipelines. Unlike smelting flux, sintered flux has not been roasted at a high temperature above 500°C. Through the practice of mass production and scientific research, it is found that the sintered flux contains relatively high content of calcium, fluorine and silicon, and also contains a certain amount of aluminum, so it is difficult to completely decompose the sample. At present, there is no standard sample of sintered flux in the metallurgical industry, and the accuracy of the results can only be tested by using sintered flux with similar properties as a substitute standard sample. However, sintered flux roasted at high temperature is easily decomposed, and the standard sample...

Claims

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Application Information

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IPC IPC(8): G01N21/71
Inventor 周郑闻向东张穗忠谭谦董蓓谢芬邵梅黄治军牟文广
Owner 武汉钢铁有限公司
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