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Method for measuring content of aluminum in silicon-calcium alloy

A silicon-calcium alloy and aluminum content technology, applied in the field of element detection, can solve the problems of measurement interference, complex processing methods, and large amount of chemical reagents, so as to reduce instrument detection interference, improve efficiency and accuracy, and reduce types and dosages. Effect

Pending Publication Date: 2021-11-23
PANZHIHUA IRON & STEEL RES INST OF PANGANG GROUP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, digestion under acidic conditions is not suitable for the pretreatment of impurity element aluminum in silicon-calcium alloys
The common sample pretreatment method is relatively complicated. Generally, it is acid-dissolved first, and a large amount of hydrofluoric acid, hydrochloric acid, nitric acid, perchloric acid, etc. are usually added. , and then acid-dissolve the alkali fusion residue, and then combine the main analysis solution and the alkali fusion solution. Acid white smoke cannot be absorbed by ordinary acid mist treatment systems, causing environmental pollution

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  • Method for measuring content of aluminum in silicon-calcium alloy
  • Method for measuring content of aluminum in silicon-calcium alloy
  • Method for measuring content of aluminum in silicon-calcium alloy

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preparation example Construction

[0047] In the present invention, the preparation method of the flux preferably includes: grinding and mixing carbonate and boric acid.

[0048] In the present invention, the amount of the flux is preferably 0.4-0.6 g, more preferably 0.5 g, which can be determined according to the difficulty of sample digestion.

[0049] In the present invention, the mass ratio of the sample to be tested and the flux is preferably (0.1~0.2):(0.4~0.6), more preferably (0.12~0.18):(0.45~0.55), most preferably (0.14~ 0.16): 0.5.

[0050] The amount of flux used in the invention is small, which significantly reduces the interference caused by the mixed reagent matrix effect on the detection accuracy.

[0051]In the present invention, the melting is preferably high-temperature alkali fusion; the melting temperature is preferably 900-100°C, more preferably 920-980°C, more preferably 940-960°C, most preferably 950°C; The melting time is preferably 15-25 minutes, more preferably 18-22 minutes, most ...

Embodiment 1

[0071] Weigh 0.10g silicon-calcium alloy sample to be tested, add 2ml hydrofluoric acid dropwise, after the reaction stops, heat it on the electric heating plate until it evaporates to dryness, add 0.4g anhydrous potassium carbonate and boric acid to grind and mix in a mass ratio of 1:1 Melt in a muffle furnace at 880°C for 20 minutes, add 12 ml of 1:1 hydrochloric acid solution (the volume ratio of hydrochloric acid and water is 1:1), and add an appropriate amount of ultrapure water during the dissolution process. Dilute it into a 100ml volumetric flask with ultrapure water, and finally measure the aluminum content with an inductively coupled plasma atomic emission spectrometer.

Embodiment 2

[0073] Weigh 0.15g of calcium-silicon alloy sample to be tested, add 2.5ml of hydrofluoric acid dropwise, after the reaction stops, heat it on the electric heating plate until it evaporates to dryness, add 0.45g of anhydrous potassium carbonate and boric acid to grind at a mass ratio of 1:1 Melt the mixed flux at 860°C for 22 minutes in a muffle furnace, add 15 ml of 1:1 hydrochloric acid solution (the volume ratio of hydrochloric acid and water is 1:1), add an appropriate amount of ultrapure water during the dissolution process, and completely dissolve Afterwards, the volume was fixed in a 100ml volumetric flask with ultrapure water, and finally the aluminum content was measured by an inductively coupled plasma atomic emission spectrometer.

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Abstract

The invention provides a method for measuring the content of aluminum in a silicon-calcium alloy, the method comprises the following steps: only dropwise adding hydrofluoric acid into a sample to be measured for reaction, after the reaction is stopped, heating and evaporating on an electric hot plate, firing at high temperature, then directly adding a flux formed by grinding and mixing anhydrous potassium carbonate and boric acid, melting in a high-temperature furnace, leaching with hydrochloric acid, and fixing the volume, and finally, measuring the content of aluminum by adopting instrument analysis methods such as inductively coupled plasma atomic emission spectrometry and the like. Only hydrofluoric acid is added in the sample pretreatment process so that the use of a large amount of acid is avoided; by utilizing the characteristic that hydrofluoric acid can react with silicon under high-temperature heating to generate a volatile substance silicon tetrafluoride (SiF4), a large amount of interference element silicon in the sample is removed; residues are burned at high temperature, and part of detection interference impurities are removed; residues are directly dissolved with hydrochloric acid after being subjected to high-temperature alkali fusion, and are directly detected after constant volume so that the tedious operation caused by combining a main solution obtained after acid dissolution with a diluent obtained after alkali fusion in the past is avoided.

Description

technical field [0001] The invention belongs to the technical field of element detection, in particular to a method for measuring aluminum content in silicon-calcium alloys. Background technique [0002] Silicon-calcium alloys are mostly used in composite deoxidation, desulfurization, denaturation of non-metallic inclusions, addition of alloying elements, and cast iron production in iron and steel smelting. Other impurity elements in silicon-calcium alloy except aluminum can generally be digested and dissolved under acidic conditions, and the pre-treatment is relatively simple. However, digestion under acidic conditions is not suitable for the pretreatment of impurity element aluminum in silicon-calcium alloys. The common sample pretreatment method is relatively complicated. Generally, it is acid-dissolved first, and a large amount of hydrofluoric acid, hydrochloric acid, nitric acid, perchloric acid, etc. are usually added. , and then acid-dissolve the alkali fusion resid...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/28G01N21/73
CPCG01N1/28G01N21/73
Inventor 刘力维成勇袁金红何其平
Owner PANZHIHUA IRON & STEEL RES INST OF PANGANG GROUP
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