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Method for determining content of calcium fluoride in fluorite

A technology for medium calcium fluoride and fluorine content, which can be used in chemical analysis by titration, material analysis by observing the influence of chemical indicators, and analysis by making materials undergo chemical reactions, etc., which can solve the problem of low precision. , Introduce problems such as large errors and low calcium fluoride results to achieve the effect of improving accuracy and precision, good reduction and masking, and clear discoloration

Active Publication Date: 2015-12-09
武汉钢铁有限公司
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  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There is also a method that uses calcium oxalate precipitation and potassium permanganate titration to determine the total calcium content. Both methods need to subtract the calcium carbonate content, and the determination of calcium carbonate is necessary. The process is cumbersome and introduces large errors.
In the test methods introduced in this unit and some literatures, the calcium carbonate is removed with acetic acid before the determination of total calcium, and then the titration of calcium is carried out. However, because acetic acid can also dissolve a small amount of calcium fluoride, and improper operation, Such as dissolving, washing, etc. may cause part of calcium fluoride to dissolve together with calcium carbonate, making the determination result of calcium fluoride low and the precision is not high
Moreover, in these methods, the total calcium of calcium fluoride and calcium carbonate is obtained by acid-dissolving sample titration or calcium fluoride is obtained by acid-soluble titration after leaching to remove calcium carbonate. For fluorite whose main component is calcium fluoride, it is necessary to Put the sample in an agate mortar and crush it and pass through the 0.063mm sieve size, so that the calcium fluoride in the sample can be completely dissolved with acid, otherwise the determination of calcium fluoride will be low
However, the samples prepared in our daily production analysis are basically 0.080mm ~ 0.105mm in particle size, and it is impossible to prepare a particle size of 0.063mm. It takes a long time and poor feasibility to perform a sample crushing operation before analysis for daily production analysis.

Method used

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  • Method for determining content of calcium fluoride in fluorite
  • Method for determining content of calcium fluoride in fluorite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] For a fluorite standard sample BH0121-17W (CaF 2 standard value 98.59%) to measure:

[0022] (1) Weigh 0.2000g sample and place it in a 250mL beaker, add 5mL of calcium-containing acetic acid solution, the concentration of calcium-containing acetic acid solution is 2.0mg calcium per milliliter, cover with a watch glass, shake the beaker to distribute the sample evenly, heat Slightly boil for 2 minutes, keep warm for 2 minutes, then immediately filter into a 250mL beaker with slow filter paper, wash the beaker and the precipitate with hot (60-70°C) fluorine-containing washing solution with a concentration of 10μg / mL for 4 times;

[0023] (2) Put the slow-speed filter paper and the precipitate in a platinum crucible, ash and burn in a muffle furnace, take it out, cool it, add 3.2g of sodium carbonate and boric acid in a mass ratio of 2:1 mixed flux, mix well , placed in a high-temperature furnace at a temperature of 500°C, heated to 950°C and melted for 20 minutes, taken...

Embodiment 2

[0026] For a fluorite standard sample YSB14785-02 (CaF 2 standard value 93.28%) to measure:

[0027] (1) Weigh 0.5000g sample and place it in a 250mL beaker, add 10mL of calcium-containing acetic acid solution, the concentration of calcium-containing acetic acid solution is 0.8mg calcium per milliliter, cover with a watch glass, shake the beaker to make the sample evenly distributed, room temperature Stand for 30 minutes, stir once every 5 minutes, then immediately filter into a 250mL beaker with slow filter paper, wash the beaker and the precipitate with hot (60-70°C) fluorine-containing washing solution with a concentration of 20μg / mL for 5 times;

[0028] (2) Put the slow filter paper together with the precipitate in a platinum crucible, incinerate and burn in a muffle furnace, take it out, cool it down, add 5g of sodium carbonate and boric acid in a mass ratio of 2:1 to obtain a mixed flux, mix well, and place In a high-temperature furnace with a temperature of 500°C, hea...

Embodiment 3

[0031] For CaF in a fluorite sample 2 The content is measured:

[0032] (1) Weigh 0.4000g sample and place it in a 250mL beaker, add 10mL calcium-containing acetic acid solution, the concentration of calcium-containing acetic acid solution is 1.2mg calcium per milliliter, cover with a watch glass, shake the beaker to distribute the sample evenly, heat Slightly boil for 5 minutes, keep warm for 2 minutes, then immediately filter into a 250mL beaker with slow filter paper, wash the beaker and the precipitate with hot (60-70°C) fluorine-containing washing solution with a concentration of 15μg / mL for 6 times;

[0033] (2) Place the slow filter paper together with the precipitate in a platinum crucible, incinerate and burn in a muffle furnace, take it out, cool it down, add 4.5g of sodium carbonate and boric acid in a mass ratio of 2:1 to obtain a mixed flux, mix well, Place in a high-temperature furnace at 500°C, heat up to 950°C and melt for 15 minutes, take it out, cool, then p...

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Abstract

The invention relates to a method for determining the content of calcium fluoride in fluorite. The method comprises the steps that 1, a calcium-containing acetic acid solution with the calcium content ranging from 0.8 mg / mL to 2.0 mg / mL is prepared; 2, a fluorine-containing washing solution with the fluorine content ranging from 10 micrograms per milliliter to 20 micrograms per milliliter; 3, a fluorit sample is soaked with the calcium-containing acetic acid solution, then filtering is performed with low-speed filter paper, a beaker and precipitate are washed with the fluorine-containing washing solution, the low-speed filter paper and the precipitate are placed in a muffle furnace to be incinerated and burnt, a mixed solution of sodium carbonate and boric acid is added after the low-speed filter paper and the precipitate are cooled, the mixture is put in a high-temperature furnace to be fused and then put in a hydrochloric acid solution, a saturated boric acid solution is added for leaching, and the liquid is diluted with water to obtain a test solution after being cooled; 4, a magnesium sulfate solution, water, a triethanolamine solution, a mixed solution of sodium sulfide and hydroxylamine hydrochloride and a potassium hydroxide solution are added in the test solution, the mixture is shaken evenly, a calcein-thyme mixed phenolphthalein indicator is added, the mixed solution is titrated with an EDTA standard titration solution until the mixed solution turns into prunosus, and then the content of the calcium fluoride is calculated according to the volume number of the standard titration solution.

Description

technical field [0001] The invention relates to an analysis and test method, in particular to a method for determining the content of calcium fluoride in fluorite. Background technique [0002] In the iron and steel industry, fluorspar (also known as fluorspar) is used as a flux and is mainly used for slagging in converter or electric furnace steelmaking. In the chemical and building materials industry, it is also the basic raw material for the manufacture of hydrofluoric acid or other various fluorides, and it is also one of the raw materials for the manufacture of sound insulation and optical glass and welding flux in the glass manufacturing industry. Fluorite is mainly composed of calcium fluoride (CaF 2 ), the rest are carbonates, sulfates, silica. The content of calcium fluoride in fluorite determines the quality grade of fluorite, and it is an important item in the detection of fluorite components. The standard method for the determination of calcium fluoride in flu...

Claims

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Application Information

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IPC IPC(8): G01N31/16G01N21/79
Inventor 闻向东周郑夏念平谢芬宋育来杨艳潘菁李江文文斌赵希文
Owner 武汉钢铁有限公司
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