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Fast and accurate detection method for silicon dioxide content in limestone, kalk and dolomite

A silicon dioxide and detection method technology, applied in the direction of color/spectral characteristic measurement, etc., can solve the problems of incomplete sample decomposition, long analysis time, analysis error, etc., achieve good promotion and application prospects, high analysis efficiency, and reduce the number of experiments effect of error

Active Publication Date: 2014-04-16
WUKUN STEEL
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the traditional determination method of silica content, the upper limit of silica content measured by molybdenum blue photometry is 4%, which is not suitable for the determination of samples with silica content > 4%; although perchloric acid dehydration gravimetric method is applicable It is suitable for the determination of samples with silica content > 2%, but this method does not completely decompose some samples, which is easy to cause analysis errors, and the analysis time is long and the cost is high

Method used

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  • Fast and accurate detection method for silicon dioxide content in limestone, kalk and dolomite
  • Fast and accurate detection method for silicon dioxide content in limestone, kalk and dolomite
  • Fast and accurate detection method for silicon dioxide content in limestone, kalk and dolomite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] ——Determination of silica content in lime sample

[0048] Reagents for detection:

[0049] Sodium carbonate-boric acid mixed flux: It is made by mixing sodium carbonate and boric acid with a mass ratio of 2:1 and grinding them finely.

[0050] Hydrochloric acid solution: It is made by mixing 37% hydrochloric acid and water at a volume ratio of 1:1.

[0051] Ammonium molybdate solution: the concentration is 12.5g / L.

[0052] Mixed acid of oxalic acid-sulfuric acid: It is formed by mixing oxalic acid solution and sulfuric acid solution with a volume ratio of 3:1. become.

[0053] Mixed solution of ascorbic acid-ammonium ferrous sulfate: mixed with ascorbic acid solution and ammonium ferrous sulfate solution with a volume ratio of 1:1, the concentration of ascorbic acid solution is 2.0g / L, and the concentration of ferrous ammonium sulfate solution is 2.0g / L L.

[0054] Silica standard sample: the purity is 99.99%.

[0055] Sample testing:

[0056] A. Sample pretreat...

Embodiment 2

[0071] ——Determination of silica content in limestone samples

[0072] Detection reagent: same as embodiment 1

[0073] Sample testing:

[0074] A. Sample pretreatment: crush the limestone sample to a particle size of ≤0.125mm, dry at 108°C for 2 hours, seal the sample in a desiccator immediately after drying, and cool to 20~25°C.

[0075] B, C, D, E, F steps are the same as embodiment 1.

[0076] G. Calculation of content: the calculation of silica content in limestone sample is as follows:

[0077] m 1 ——Based on the limestone sample absorbance value of 0.472, the quality of silica obtained from the working curve is 198.84ug;

[0078] m - the mass of the sample in step B is 0.1000g;

[0079] V 1 - The volume of the test solution pipetted in step C is 5.00ml;

[0080] V—the total volume of the test solution in step B is 250ml.

[0081]

[0082] =

[0083] = 9.94 (%)

Embodiment 3

[0085] ——Determination of silica content in dolomite samples

[0086] Detection reagent: same as embodiment 1

[0087] Sample testing:

[0088] A. Sample pretreatment: crush the dolomite sample to a particle size of ≤0.125mm, dry at 108°C for 2 hours, seal the sample in a desiccator immediately after drying, and cool to 20~25°C.

[0089] B, C, D, E, F steps are the same as embodiment 1.

[0090] G. Calculation of content: the calculation of silica content in the sample is as follows:

[0091] m 1 ——Based on the absorbance value of the dolomite sample 0.336, the quality of silica obtained from the working curve is 125.39ug;

[0092] m - the mass of the sample in step B is 0.1000g;

[0093] V 1 - The volume of the test solution pipetted in step C is 5.00ml;

[0094] V—the total volume of the test solution in step B is 250ml.

[0095]

[0096] =

[0097] = 6.27 (%)

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Abstract

The invention discloses a fast and accurate detection method for silicon dioxide content in limestone, kalk and dolomite. The detection method comprises the following steps: crushing samples, and drying for 1.5-2.5 h under thea temperature of 105-110 DEG C; mixing 0.1000 g samples and 3.0-4.0 g mixed fluxing agent of sodium carbonate and boric acid evenly, liquating for 18-20 min under athe temperature of 890-910 DEG C, dissolving frits by a 45-55 ml hydrochloric acid and 25-35 ml water, and placing the test solution in a 250-ml volumetric flask; taking and adding 5.00 ml test solution in a 100-ml volumetric flask, adding 18-22 ml ammonium molybdate and still standing for 18-22 min, and adding 45-55 ml mixed acid of oxalic acid and sulfuric acid, 4.80-5.20 ml ascorbic acid-ammonium ferrous sulfate mixed solution; measuring the absorbency of a color development solution at the wavelength of 680 nm through a spectrophotometer, and using blank as a reference; preparing a silicon dioxide standard sample with the concentration of 40 ug / ml, moving and taking 0.00 ml, 2.00 ml, 4.00ml, 6.00 ml, 8.00 ml and 10.00 ml silicon dioxide standard samples, and placing the standard samples in 100-ml volumetric flasks respectively, adding 5.00 ml blank test solution in the volumetric flasks respectively, after color-developing, measuring the absorbency at the same conditions, and then drawing a working curve. The silicon dioxide content in the samples is calculated according to the following formula (shown in the specification). The detection method is fast and efficient, excellent in accuracy, reproducibility and stability, and particularly suitable for detection of samples with silicon dioxide content equal to or higher than 4 %.

Description

technical field [0001] The invention belongs to the technical field of metallurgical material testing and analysis, in particular to a fast and accurate detection method for silica content in limestone, lime and dolomite. Background technique [0002] In iron and steel smelting production, limestone is mainly used for slag making in iron smelting, lime is mainly used for slagging and desulfurization in steel making, and as a flux for sinter and pellet ore, and dolomite is mainly used for sintering metallurgical furnace bottom after calcination repair furnace lining. The main component of limestone, lime and dolomite—the content of silicon dioxide has an important impact on the performance of the product, so the accurate determination of its content has very important practical significance for smelting production. In the traditional silica content determination method, the molybdenum blue photometric method measures the upper limit of silica content to 4%, which is not suit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/31
Inventor 郑玲王磊李文生许涯平高丽萍
Owner WUKUN STEEL
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