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Method capable of determining major element(s) in ferrochrome alloy by using X-ray fluorescence melting piece method

A ferrochromium alloy and fusing technology, applied in the field of physical and chemical testing, can solve the problems of low test results, long melting time, material loss of alloy samples, etc., to eliminate the risk of corrosion, solve the effect of particle size effect, and improve the effect of oxidizing ability

Inactive Publication Date: 2020-01-03
HANDAN IRON & STEEL GROUP +1
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  • Summary
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  • Application Information

AI Technical Summary

Problems solved by technology

This technical scheme is aimed at ferrochromium alloy, and the reagent wrapped into balls is an oxidizing agent, and its formula is: 2 parts by weight of lithium tetraborate+1 part by weight of lithium carbonate+0.5 parts by weight of sodium nitrate, and the sample size is 0.1 parts by weight. Usually, each part by weight is 1 gram, and the patent solution has the following disadvantages: 1. During the burning process, due to the presence of lithium carbonate, the mixture of oxidant and ferrochrome powder will splash heavily in the graphite powder, and some alloy Graphite powder splashes into the graphite powder, and the amount of splashing is uncontrollable, resulting in material loss of the alloy sample and lower test results; The part of a sample splashed into graphite powder will pollute the current sample, so that the data obtained in the final test often cannot represent the sample; 3. The melting time is too long, and the residual amount of release agent is not enough to ensure the quality of release. Severe residual
[0005] At present, there are many reports on the analysis of ferroalloys by X-ray fluorescence pellet method, but because the pellet method is greatly affected by the sample size effect and matrix effect, the accuracy of the analysis data is poor; and the attempt to analyze ferroalloys by X-ray fluorescence pellet method is often due to inability Find a suitable oxidant but cannot completely oxidize the iron alloy sample, causing corrosion of the platinum crucible, or in order to protect the platinum crucible from corrosion, the oxidation effect of the oxidant can meet the requirements, but it is easy to cause splashing and loss of the alloy, resulting in unstable final test results, so The application of X-ray fluorescence fusion method in the test of ferroalloy is not widespread yet

Method used

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  • Method capable of determining major element(s) in ferrochrome alloy by using X-ray fluorescence melting piece method

Examples

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preparation example Construction

[0028] 2) Preparation and storage of composite oxidant: mix and prepare the required reagent lithium hydroxide monohydrate, boric acid and potassium nitrate solid reagent by mass (4-10): (1-2): 1;

[0029] 3), preparation of working curve standard sample: Weigh 0.1-0.2g standard sample in a porcelain crucible, add compound oxidant and 0.2-0.5g viscosity reducer relative to the quality of standard sample 10-20 times, stir evenly, in Weigh into the platinum crucible the flux lithium tetraborate 30 to 80 times the mass of the standard sample, stir evenly, and make the central area slightly depressed, completely pour the standard sample in the porcelain crucible into the depression, place it in the muffle furnace from room temperature to The speed of 15-20°C / min is raised from room temperature to 770-800°C to complete the pre-oxidation, then transfer the platinum crucible to the melting furnace to melt according to the set procedure, rotate and shake, add the release agent ammonium...

Embodiment 1-6

[0036] Embodiment 1-6, condition A

[0037] First, prepare the required reagents: lithium hydroxide monohydrate, boric acid, potassium nitrate, lithium tetraborate;

[0038] Lithium tetraborate, lithium metaborate, lithium fluoride is the mixed flux that mass ratio is 65:25:10 composition; Potassium bromide, ammonium bromide, stand-by;

[0039] Second, the selection of standard samples: select 10 ferrochrome standard samples, the content range should cover the analysis sample content, the composition content is shown in the following table 1, the standard sample particles are less than 200 mesh, the standard sample should be processed to 200 mesh and mixed , can pass through a 200-mesh sieve; accurately weigh 0.1500 g of the ground standard sample in a porcelain crucible, add 2.0000 g of composite oxidant lithium hydroxide monohydrate, 0.5000 g of boric acid, and 0.5000 g of potassium nitrate, and add viscosity reducer bromine Potassium chloride 0.2000 g, stir evenly; weigh 7...

Embodiment 7-8

[0059] Embodiment 7-8, condition B

[0060] Medicines and standard samples were prepared according to the conditions of Example 1.

[0061] First, prepare the required reagents: lithium hydroxide monohydrate, boric acid, potassium nitrate, lithium tetraborate;

[0062] Lithium tetraborate, lithium metaborate, lithium fluoride are the mixed flux of 65:25:10 composition by mass ratio, potassium bromide, ammonium bromide, stand-by;

[0063]Second, prepare the standard sample according to Table 1 of Example 1, the sample weight is determined to be 0.1000 grams, add 1.2000 grams of composite oxidant lithium hydroxide monohydrate, 0.2000 grams of boric acid, 0.2000 grams of potassium nitrate, and add 0.5000 grams of viscosity reducer potassium bromide gram, and stir evenly; weigh 8.0000g of lithium tetraborate flux into a platinum crucible, the center area is slightly lower and in a concave shape, pour the uniformly mixed standard sample into the center of the platinum crucible, an...

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Abstract

The present invention discloses a method capable of determining major element(s) in a ferrochrome alloy by using an X-ray fluorescence melting piece method. The method comprises the following steps: (1) selecting multiple standard samples with the grain size up to 200 meshes; (2) weighing the standard samples, adding a compound oxidant and a viscosity reducer, and stirring well; (3) weighing and adding a flux in a platinum crucible, pouring the well mixed standard samples into the platinum crucible and covering the flux, and placing the platinum crucible in a muffle furnace to complete alloy sample pre-oxidation; (4) putting the pre-oxidized platinum crucible in a sample melting furnace to perform sample melting, before demoulding, adding a demoulding agent, rotating, shaking, then performing cooling demoulding, and making glass piece(s) used for analysis; (5) testing main element strength value in the standard samples by using a X-ray fluorescence spectrometer, and building the measured strength value and a standard value into a primary working curve; and (6) grinding the to-be-tested sample(s) of the block ferrochrome alloy to the same grain size as the standard samples, meltinginto the glass piece(s) according to steps (2) to (5), and analyzing the component value of the glass piece(s) by using the X-ray fluorescence spectrometer. The method can extend the life of the platinum crucible and ensure accuracy and precision of the result(s).

Description

technical field [0001] The invention relates to a method for measuring major elements in ferrochrome alloys by an X-fluorescence fusion chip method, belonging to the technical field of physical and chemical detection. Background technique [0002] In order to meet the industrial requirements for steel properties, it is necessary to add ferrochromium and other alloying elements for microalloying treatment in the steelmaking process to improve the crystal structure of steel and improve the mechanical and physical properties of materials. On the one hand, or to guide the operation of the steelmaking process, it is necessary to carry out laboratory analysis on the chemical composition of ferrochrome alloy. Using traditional wet chemical analysis and the current national standard method to determine the content of chromium, silicon, phosphorus, manganese and other related elements in ferrochrome alloy, the operation is complicated and cumbersome, the steps are long, time-consumin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N23/207G01N23/2005
CPCG01N23/2005G01N23/2076
Inventor 顾强左丽峰张秀宏张建中冀丽英王敏徐静
Owner HANDAN IRON & STEEL GROUP
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