Method for jointly determining silicon, aluminum, barium, manganese, phosphorus and iron in silicon-aluminum-barium by inductively coupled plasma

A plasma and inductive coupling technology, applied in the field of metallurgical chemical analysis and testing, can solve the problems of chemical reagents harmful to the human body and the environment, unable to meet production needs, low detection efficiency, etc. good precision

Pending Publication Date: 2021-04-09
YANGCHUN NEW STEEL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the determination method of silicon in silicon-aluminum-barium is dehydration by adding perchloric acid after alkali fusion, and then igniting and precipitating after filtration. The step of filtering and washing precipitation takes a long time; the determination of aluminum is dissolved by hydrofluoric acid, nitric acid and perchloric acid. After nearly dry, constant volume fractionation and titration, the process requires a variety of chemical reagents; the pretreatment of barium determination is similar to the pretreatment of aluminum, adding sodium chloride to form barium sulfate precipitation, filtering, washing and burning the precipitate also takes time; manganese The pre-treatment for the determination of phosphorus and phosphorus is acid dissolution, and the absorbance is measured by a spectrophotometer. At the same time, a working curve must be prepared to obtain the results on the working curve. There are many chemical reagents used, and the determination of iron requires heavy and toxic dichromic acid. Potassium reagent
[0003] The above six methods are all to analyze one of the elements, and the cycle is long, the steps are cumbersome, and many reagents are used. Many chemical reagents are harmful to the human body and the environment. For high-paced production, the detection efficiency is low. Low, unable to meet production needs

Method used

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  • Method for jointly determining silicon, aluminum, barium, manganese, phosphorus and iron in silicon-aluminum-barium by inductively coupled plasma
  • Method for jointly determining silicon, aluminum, barium, manganese, phosphorus and iron in silicon-aluminum-barium by inductively coupled plasma
  • Method for jointly determining silicon, aluminum, barium, manganese, phosphorus and iron in silicon-aluminum-barium by inductively coupled plasma

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Experimental program
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Effect test

Embodiment 1

[0036] The mensuration of embodiment 1 element content 1

[0037] S1 sample melting: adopt precision weighing equipment to take by weighing 0.1000g silicon aluminum barium sample that has been crushed through 120 mesh sieves, and the accuracy of weighing is accurate to 0.0001g; In a crucible with a 3:1 mixed flux, fully mix the sample with the mixed flux, then cover with 0.5g of sodium carbonate-boric acid mixed flux, cover the crucible lid, and melt in a high-temperature furnace at 950°C for 10 minutes until the sample melts into red When it is in a transparent melt state, take the sample out and cool to room temperature; take it out and cool to room temperature.

[0038] S2 sample acidification leaching: select a clean container without interference from impurities, clean it with tap water and deionized water in turn, transfer the crucible containing the sample and cooled to room temperature into the container, rinse the outer wall of the crucible with water, and rinse the c...

Embodiment 2

[0055] The mensuration of embodiment 2 element content 2

[0056] S1 sample melting: adopt precision weighing equipment to take by weighing 0.2000g silicon-aluminum-barium sample that has been crushed through a 120 mesh sieve, and the accuracy of weighing is accurate to 0.0001g; In a crucible with a 3:1 mixed flux, fully mix the sample and the mixed flux, then cover with 1g of sodium carbonate-boric acid mixed flux, cover the crucible lid, and melt in a high-temperature furnace at 950°C for 10 minutes, until the sample melts into red and transparent In the melt state, take the sample out and cool to room temperature; take it out and cool to room temperature.

[0057] S2 sample acidification leaching: select a clean container without interference from impurities, clean it with tap water and deionized water in turn, transfer the crucible containing the sample and cooled to room temperature into the container, rinse the outer wall of the crucible with water, and rinse the contain...

Embodiment 3

[0074] The mensuration of embodiment 3 element content 3

[0075] S1 sample melting: adopt precision weighing equipment to take by weighing 0.3000g silicon aluminum barium sample that has been crushed through a 120 mesh sieve, and the accuracy of weighing is accurate to 0.0001g; In a crucible with a 3:1 mixed flux, fully mix the sample with the mixed flux, then cover with 1.5g of sodium carbonate-boric acid mixed flux, cover the crucible lid, and melt in a high-temperature furnace at 950°C for 10 minutes until the sample melts into red When it is in a transparent melt state, take the sample out and cool to room temperature; take it out and cool to room temperature.

[0076] S2 sample acidification leaching: select a clean container without interference from impurities, clean it with tap water and deionized water in turn, transfer the crucible containing the sample and cooled to room temperature into the container, rinse the outer wall of the crucible with water, and rinse the ...

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Abstract

The invention discloses a method for jointly determining silicon, aluminum, barium, manganese, phosphorus and iron in silicon-aluminum-barium through inductively coupled plasma, and relates to the technical field of metallurgical chemical analysis tests. The method mainly comprises the following steps: melting a silicon-aluminum-barium sample with sodium carbonate and boric acid, adding hydrochloric acid for acidification, diluting to a certain volume, measuring the emitted light intensity of the silicon-aluminum-barium sample at the wavelength of a recommended analysis line on an inductively coupled plasma emission spectrometer, finding out the content of a to-be-measured element according to a working curve, and calculating the mass fraction of the to-be-measured element. Compared with existing traditional manual wet chemical analysis, the method adopting the above technical scheme has the advantages that the detection efficiency can be improved by 70%, meanwhile, the method is suitable for measuring the content of barium with the content being larger than 5% and the content of silicon, aluminum and iron with the content being 20% or above, silicon, aluminum, barium, manganese, phosphorus and iron main trace elements in silicon-aluminum-barium can be measured at the same time through the measuring method, and the method is simple and rapid. A large amount of chemical reagents and manpower are saved, and the labor productivity is greatly improved.

Description

technical field [0001] The invention relates to the technical field of metallurgical chemical analysis tests, in particular to a method for inductively coupled plasma joint determination of silicon, aluminum, barium, manganese, phosphorus and iron in silicon-aluminum-barium. Background technique [0002] Silicon-aluminum-barium alloy is a deoxidizer in the steelmaking process. There are various methods for determining the content of silicon, aluminum, barium, manganese, phosphorus, and iron in silicon-aluminum-barium, including perchloric acid dehydration gravimetric method, EDTA titration method, and barium sulfate gravimetric method. , Periodate Spectrophotometry, Molybdenum Blue Spectrophotometry, Potassium Dichromate Titration, the determination of the six components requires separate sample pretreatment and separate detection. Among them, the determination method of silicon in silicon-aluminum-barium is dehydration by adding perchloric acid after alkali fusion, and then...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/73
CPCG01N21/73
Inventor 伍绍双傅余东许家宝柳锐松覃双环
Owner YANGCHUN NEW STEEL CO LTD
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