Method for rapidly and accurately determining sulphur element content in fluorite

An accurate determination of sulfur element technology, applied in the field of analytical chemistry, can solve problems such as spectral background interference, spectral line interference, and incomplete sample decomposition, and achieve the effects of shortening analysis time, high sensitivity, and reducing detection costs

Inactive Publication Date: 2010-02-03
武钢集团有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It uses an inductively coupled plasma emission spectrometer, which mainly solves the problems of incomplete sample decomposition, spectral background interference, and spectral line interference during measurement, and determines the appropriate operating parameters and steps to achieve efficient, fast and accurate measurement of sulfur in fluorite.

Method used

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  • Method for rapidly and accurately determining sulphur element content in fluorite
  • Method for rapidly and accurately determining sulphur element content in fluorite
  • Method for rapidly and accurately determining sulphur element content in fluorite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Dry the fluorite sample at 105-110°C for 3-5 hours in advance, put it in a desiccator and cool it to room temperature; weigh 2.0000g of fluorite sample 1# into a 200mL polytetrafluoroethylene beaker, add 30mL deionized water After wetting, add 5mL of 47% hydrofluoric acid, 10mL of 69% nitric acid, 20mL of 38% hydrochloric acid, and 8mL of 72% perchloric acid, heat and dissolve at 300°C, blow perchloric acid fumes until the volume of the solution is 1mL, and make fluorite The sample is completely converted into easily soluble salts; add 50mL of deionized water, then add 10mL of 38% hydrochloric acid, heat to dissolve the salts, after cooling, transfer to a 100mL volumetric flask, dilute to the scale of 100mL with deionized water, and mix well (above The concentration of each acid is the volume percent concentration, the same below). Other steps are the same as in Example 1.

[0052]Treat the blank sample in the same way, add the same concentration of calcium matrix as i...

Embodiment 2

[0057] Weigh 0.2000g of fluorite sample 2# into a 200mL polytetrafluoroethylene beaker, moisten it with a small amount of water, add 2mL of 47% hydrofluoric acid, 5mL of 69% nitric acid, 10mL of 37% hydrochloric acid, and 5mL of 70% perchloric acid. Heat to dissolve at ℃, smoke perchloric acid until the volume of the solution is 0.5mL, so that the fluorite sample is completely converted into easily soluble salts; add 50mL of deionized water, then add 5mL of 37% hydrochloric acid, heat to dissolve the salts, cool Afterwards, transfer to a 100mL volumetric flask and dilute to 100mL with deionized water.

[0058] Treat the blank sample in the same way, add the same concentration of calcium matrix as in the sample, add sulfur standard solutions of different concentrations, add water to make up to 100mL, measure the spectral intensity of sulfur on the ICP emission spectrometer, and draw the working curve. Then measure the spectral intensity of sulfur in the solution to be tested, o...

Embodiment 3

[0063] Weigh 1.0000g of fluorite sample 3# into a 200mL polytetrafluoroethylene beaker, add 20mL deionized water, then add 3mL of 47% hydrofluoric acid, 7mL of 69% nitric acid, 15mL of 38% hydrochloric acid, and 7mL of 72% perchloric acid , heat to dissolve at 250°C, smoke perchloric acid until the volume of the solution is 0.7mL, so that the fluorite sample is completely converted into easily soluble salts; add 50mL of deionized water, then add 7mL of 37% hydrochloric acid, and heat to dissolve the salt Classes, after cooling, transferred to a 100mL volumetric flask, diluted with deionized water to the scale of 100mL.

[0064] Treat the blank sample in the same way, add the same concentration of calcium matrix as in the sample, add sulfur standard solutions of different concentrations, add water to make up to 100mL, measure the spectral intensity of sulfur on the ICP emission spectrometer, and draw the working curve. Then measure the spectral intensity of sulfur in the soluti...

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Abstract

A method for rapidly and accurately determining sulphur element content in fluorite mainly comprises the following steps: weighing a fluorite sample, adding deionized water, and then adding mixed acidto cause the fluorite sample to be fully converted into diffluent salt; adding deionized water and heating till the salt is completely dissolved; metering volume till 100mL; adopting reagent withoutthe sample for blanking, adding calcium standard solution equivalent to the fluorite sample, and then adding standard solution of sulphur element of different volumes; using sulphur element concentration as a horizontal ordinate and the intensity of a light spectrum as a vertical coordinate to draw a working curve; and then automatically determining the concentration of the sulphur element in thesample solution by a computer according to the working curve. The method uses an inductance coupling plasma body emission light spectrum, mainly solves the problems in the existing method of incompletely decomposed sample, the background interference of the light spectrum during measurement, spectral line interference and the like, determines appropriate operational parameters and steps and rapidly determines the sulphur elements in the fluorite in high effect.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, more specifically it is a method for quickly and accurately measuring the content of sulfur in fluorite. Background technique [0002] Fluorspar, also known as fluorspar, is mainly composed of CaF 2 , in iron and steel production, it is mainly used for slagging in converter or electric furnace steelmaking, and can improve the fluidity of slag and enhance the interfacial reaction ability between slag and steel. It is one of the important auxiliary raw materials for steelmaking, so the accurate determination of The chemical composition is very important, especially the analysis of the harmful element sulfur content in fluorite. Sulfur in steel can cause hot brittleness of steel, reduce the mechanical properties of steel, and adversely affect the corrosion resistance and weldability of steel. Its content is an important indicator for controlling the quality of steel. At present, the analysis of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/73
Inventor 李洁张穗忠李杰陈士华谢芬陆珂刘秀莹
Owner 武钢集团有限公司
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