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Sample pretreatment method for determining content of chloride ion and sulfate radical in limestone solid

A sample pretreatment and limestone technology, which is applied in the field of chemical analysis and testing, can solve the problems of complicated operation steps, expensive equipment, and inability to guarantee the complete release of ions to be detected, and achieves good reproducibility, easy operation, and simple sample pretreatment method. Effect

Active Publication Date: 2012-06-20
安徽科测检测有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the water / eluent extraction method cannot guarantee that the ions to be detected are completely released into the aqueous solution; the microwave digestion method has high test efficiency and ideal effect, but the equipment is expensive; the high-temperature hydrolysis method has cumbersome operation steps and time-consuming tests.

Method used

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  • Sample pretreatment method for determining content of chloride ion and sulfate radical in limestone solid
  • Sample pretreatment method for determining content of chloride ion and sulfate radical in limestone solid
  • Sample pretreatment method for determining content of chloride ion and sulfate radical in limestone solid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Embodiment 1: Accurately take by weighing 0.5g the crushed limestone sample, place in a 50ml small beaker, add 10ml of 0.5mol / L perchloric acid solution, cover a watch glass, and keep shaking well, after the sample dissolves, add Secondary deionized water, dilute to 50ml. Take 2 parts of 20ml solution, one part is not added with standard, one part is added with 2ml of 100mg / L chloride ion standard solution and 1ml of 1000mg / L sulfate root standard solution respectively, and 1ml of 1mol / L sodium hydroxide solution is added to both solutions, the pH value When it reaches 7, dilute to 100ml.

[0017] The solution passes through a 0.22μm disposable filter membrane to remove small solid particles, and then enters the ion chromatography for analysis, so as to measure the concentration of chloride ions and sulfate radicals in it, and calculate the content and recovery of chloride ions and sulfate radicals in the sample. The results are shown in Table 1.

[0018] Calculation ...

Embodiment 2

[0024] Embodiment 2: Accurately take by weighing 0.5g the crushed limestone sample, place in a 50ml small beaker, add 1.0mol / L perchloric acid solution 15ml, cover the watch glass, and keep shaking, after the sample dissolves, add Secondary deionized water, dilute to 50ml. Take 2 parts of 20ml solution, one part is not added with standard, one part is added with 2ml of 100mg / L chloride standard solution and 1ml of 1000mg / L sulfate radical standard solution respectively, and 2ml of 1mol / L sodium hydroxide solution is added to both solutions, the pH value When it reaches 8, dilute to 100ml.

[0025] The solution passes through a 0.22μm disposable filter membrane to remove small solid particles, and then enters the ion chromatography for analysis, so as to measure the concentration of chloride ions and sulfate radicals in it, and calculate the content and recovery of chloride ions and sulfate radicals in the sample. The results are shown in Table 2. The calculation of the conte...

Embodiment 3

[0026] Embodiment 3: Accurately take by weighing 0.5g the crushed limestone sample, place in a 50ml small beaker, add 20ml of 1.5mol / L perchloric acid solution, cover a watch glass, and keep shaking, after the sample dissolves, add Secondary deionized water, dilute to 50ml. Take 2 parts of 20ml solution, one part is not added with standard, one part is added with 2ml of 100mg / L chloride ion standard solution and 1ml of 1000mg / L sulfate root standard solution respectively, and 5ml of 1mol / L sodium hydroxide solution is added to both solutions, the pH value When it reaches 10, dilute to 100ml.

[0027] The solution passes through a 0.22μm disposable filter membrane to remove small solid particles, and then enters the ion chromatography for analysis, so as to measure the concentration of chloride ions and sulfate radicals in it, and calculate the content and recovery of chloride ions and sulfate radicals in the sample. The results are shown in Table 3. The calculation of the co...

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Abstract

The invention discloses a sample pretreatment method for determining the content of chloride ions and sulfate radicals in limestone solid, which comprises grinding a limestone sample, sieving with a 110 mesh sieve, and sealing in a sample flask; accurately weighing the limestone sample, adding a certain concentration of an acid solution for dissolving the sample to ensure the chloride ions and sulfate radicals to be fully released into the solution, and diluting to a constant volume; and neutralizing the sample solution with a certain concentration of alkali to regulate a pH value to a certain range, performing membrane filtration, and determining the content of chloride ions and sulfate radicals in the sample by ion chromatography. The method has simple process, easy operation, good repeatability, relative standard deviation smaller than 1.68%, and recovery of standard addition above 94.1%.

Description

technical field [0001] The design of the invention belongs to the technical field of chemical analysis and testing, and relates to the determination of the content of chloride ions and sulfate radicals in insoluble solid samples by ion chromatography, in particular to the determination of the content of chloride ions and sulfate radicals in limestone samples. Background technique [0002] The main component of limestone is calcium carbonate (CaCO 3 ). Lime and limestone are used in large quantities as building materials and as important raw materials for many industries. Cement is made by mixing limestone and clay and calcining at high temperature. Glass is made by mixing limestone, quartz sand, soda ash, etc., and melting at high temperature. Limestone is burnt and processed to produce relatively pure powdered calcium carbonate, which is used as a filling material for rubber, plastic, paper, toothpaste, cosmetics, etc. Because limestone is mainly used in building materi...

Claims

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Application Information

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IPC IPC(8): G01N1/28G01N1/38
Inventor 焦霞盖学武
Owner 安徽科测检测有限公司
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