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Test sample treatment method for simultaneously measuring content of silicon and phosphor in silicon-manganese alloy by ICP

A treatment method, silicon-manganese alloy technology, applied in the field of metallurgical material testing and analysis, can solve the problems of not being able to measure the silicon content of the sample at the same time, intense chemical reaction, low measurement results, etc., achieve good promotion and application prospects, and the treatment method is simple , to avoid the effect of volatilization loss

Inactive Publication Date: 2015-04-08
WUKUN STEEL
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  • Summary
  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

However, because this method adds nitric acid and hydrofluoric acid to decompose the sample during the sample dissolution process, the chemical reaction is more intense, and silicon tetrafluoride formed by silicon and hydrofluoric acid is easy to volatilize in the beaker, resulting in low measurement results, so it cannot be used. Simultaneously used to determine the silicon content in the sample

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0025] 1. Preparation of working curve calibration solution: Use the same kind of standard substance solution to draw the working curve, weigh several silicon-manganese alloy standard substances with similar composition to the sample to be tested, each element has more than 4 measurement points, and its content is as much as possible has a gradient distribution. Prepare the mother liquor from the weighed standard substance according to the operation procedure, and then standardize it on the machine, and prepare the corresponding standard curve. With the percentage content of the standard solution as the abscissa and the average value of the spectral intensity as the ordinate, the working curve of each element to be measured is drawn by the instrument data processing software.

[0026] 2. Measure the spectral intensity of each element to be measured in the target sample solution on the working curve obtained in the previous step, calculate the content value of each element to b...

Embodiment 1

[0028] Weigh 0.1000g silicon-manganese alloy sample with a particle size of 160 mesh, place it in filter paper pre-installed with a total of 2.5g of anhydrous sodium carbonate: boric acid = 2:1 mixed flux, mix well and put 25g of graphite at the bottom Put the iron crucible in a high-temperature box-type resistance furnace to melt at 800°C for 18 minutes, take it out and cool it for 3 minutes to obtain sample a. Put sample a into a 500ml tall beaker pre-filled with a total of 110ml of hydrochloric acid: water = 1:3 dilute hydrochloric acid solution, and wait for the frit to completely dissolve in the dilute hydrochloric acid solution at 60°C to obtain sample b. Filter sample b into a 250ml volumetric flask with rapid quantitative filter paper, wash the glass container and filter paper containing sample b with deionized water, collect the filtrate and lotion, cool to room temperature, dilute to the mark with deionized water, and shake well Obtain the target sample solution.

Embodiment 2

[0030] Weigh 0.1000g silicon-manganese alloy sample with a particle size of 180 mesh, place it in filter paper pre-installed with a total of 2.0g of anhydrous sodium carbonate: boric acid = 2:1 mixed flux, mix well and put 20g of graphite at the bottom Put the iron crucible in a high-temperature box-type resistance furnace to melt at 850°C for 15 minutes, take it out and cool it for 2 minutes to obtain sample a. Put sample a into a 500ml tall beaker pre-filled with a total of 100ml of hydrochloric acid: water = 1:3 dilute hydrochloric acid solution, and wait for the frit to completely dissolve in the dilute hydrochloric acid solution at 50°C to obtain sample b. Filter sample b into a 250ml volumetric flask with rapid quantitative filter paper, wash the glass container and filter paper containing sample b with deionized water, collect the filtrate and lotion, cool to room temperature, dilute to the mark with deionized water, and shake well Obtain the target sample solution.

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Abstract

The invention discloses a test sample treatment method for simultaneously measuring content of silicon and phosphor in a silicon-manganese alloy by ICP. The test sample treatment method comprises the following steps: weighing 0.1000g of a silicon-manganese alloy test sample with particle size of 160-200mesh, putting the silicon-manganese alloy test sample into filter paper which is pre-filled with 2.0-2.5g of a mixed solvent of anhydrous sodium carbonate and boric acid in a ratio of 2 to 1, uniformly mixing, packaging and putting into an iron crucible with a graphite layer bottom for fusing for 12-18 minutes at 800-900 DEG C, cooling for 2-3 minutes to obtain a sample, putting the sample into a container which is pre-filled with 90-110ml of a diluted hydrochloric acid solution consisting of hydrochloric acid and water in a ratio of 1 to 3, dissolving clinkers, filtering the obtained sample through rapid quantitative filter paper into a 250ml volumetric flask, cleaning the sample containing container and the filter paper with deionized water, and adding deionized water to the scale after cooling the filtrate and washing liquor. According to the test sample treatment method, the silicon-manganese alloy test sample is fused and decomposed through an alkaline fusion method, thereby avoiding volatilization loss of silicon when hydrofluoric acid is added to dissolve the test sample through an acid dissolving method; the test sample is completely decomposed without interference or dissipation, so that the analyzed results are accurate and stable; moreover, an ICP spectrograph is used for simultaneously measuring the content of silicon and phosphor in the silicon-manganese alloy.

Description

technical field [0001] The invention belongs to the technical field of metallurgical material testing and analysis, and in particular relates to a sample processing method for simultaneously measuring silicon and phosphorus contents in silicon-manganese alloys by using ICP. Background technique [0002] The chemical composition of silicon-manganese alloys at home and abroad is mainly detected by traditional chemical analysis methods. For example, the chemical analysis method for the determination of silicon is the two-way differential colorimetry method, and the phosphorus content is determined by the phosphorus-molybdenum blue photometry method. The chemical analysis method has a long operation process and is time-consuming. Many, for the determination of a large number of samples, neither the vessel nor the measurement speed can meet the needs of fast-paced production, and the analysis results vary greatly due to different operators. Now the phosphorus content in silicon-m...

Claims

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Application Information

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IPC IPC(8): G01N1/44
Inventor 陈彬彬朵勇苏莉段璇周字勇张炬
Owner WUKUN STEEL
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