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Method for detecting monochloroacetic acid, dichloroacetic acid, trichloroacetic acid and sulfate radical in chloroacetic acid by ion chromatography

A technology of dichloroacetic acid and trichloroacetic acid, applied in the field of chemical analysis, can solve the problems of poor reproducibility, great influence on people and the environment, time-consuming and labor-intensive, etc., and achieves high reliability of results, saving labor time, environmental protection and the like. friendly effect

Active Publication Date: 2018-05-08
湖北省兴发磷化工研究院有限公司
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Problems solved by technology

[0003] At present, the commonly used detection methods for the content of chloroacetic acid are HG / T3271-2000 silver nitrate indirect titration and gas chromatography. These methods are complicated in pretreatment and require other chemical reagents in the process. The process is time-consuming and laborious, and has a great impact on people and the environment. poor reproducibility

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  • Method for detecting monochloroacetic acid, dichloroacetic acid, trichloroacetic acid and sulfate radical in chloroacetic acid by ion chromatography
  • Method for detecting monochloroacetic acid, dichloroacetic acid, trichloroacetic acid and sulfate radical in chloroacetic acid by ion chromatography
  • Method for detecting monochloroacetic acid, dichloroacetic acid, trichloroacetic acid and sulfate radical in chloroacetic acid by ion chromatography

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Embodiment Construction

[0015] The following examples are provided to further illustrate the present invention, but not to limit the scope of the present invention.

[0016] The required devices are DIONEX ICS-2000 ion chromatograph, anion suppressor, conductivity detector, analytical column AS19-HC anion exchange column (4×250mm), guard column AG19 (4×50mm).

[0017] Required reagents: ultrapure water with a resistivity of 18.2MΩ.cm (25°C), monochloroacetic acid (AR), dichloroacetic acid (AR), trichloroacetic acid (AR), anhydrous sodium sulfate (AR), hydrogen Potassium oxide eluent (Thermo).

[0018] 1. Configuration of standard solution: Configuration of chloroacetic acid mixed standard solution: Accurately weigh monochloroacetic acid, dichloroacetic acid, trichloroacetic acid, and sodium sulfate standard, and prepare them with ultrapure water to have concentrations of 10000ug / L and 1000ug / L respectively. L, 1000ug / L, stock solution of 1000ug / L. Store away from light at 4°C.

[0019] 2. Determin...

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Abstract

The invention discloses a method for detecting monochloroacetic acid, dichloroacetic acid, trichloroacetic acid and sulfate radical in chloroacetic acid by ion chromatography, which comprises the following steps: preparing a mixed standard solution of four anions including monochloroacetic acid, dichloroacetic acid, trichloroacetic acid and sulfate radical, feeding the mixed standard solution intoan ion chromatography detection system to perform gradient leaching by using an AS19-HC analytical column and KOH leacheate, thus obtaining a linear equation of concentration and peak area, and calculating the contents of all components in chloroacetic acid through the linear equation. The invention has the advantages that the whole analysis process is simple and convenient, the pollution and loss is smaller, the blank and marked sample recovery rate is 96 to 99.75 percent and the method is suitable for content detection of monochloroacetic acid, dichloroacetic acid, trichloroacetic acid andsulfate radical in chloroacetic acid.

Description

technical field [0001] The invention relates to the detection of monochloroacetic acid, dichloroacetic acid, trichloroacetic acid and sulfate, and belongs to the field of chemical analysis. Background technique [0002] Chloroacetic acid is an important intermediate in the industrial production of glycine. In the process of preparing glycine with chloroacetic acid method, in the process of industrial production, due to the change of conditions, dichloroacetic acid and trichloroacetic acid will be produced in the process of preparing chloroacetic acid. , sulfate and other by-products, and the purity of chloroacetic acid directly affects the quality of glycine, so in the process of producing chloroacetic acid, it is extremely important to detect the concentration of monochloroacetic acid, dichloroacetic acid, trichloroacetic acid and sulfate in chloroacetic acid. important. [0003] At present, the commonly used detection methods for the content of chloroacetic acid are HG / T3...

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/96
CPCG01N30/96
Inventor 肖清燕杜建侠荣沙沙徐柯杰李永刚郝晓斌袁木平郑群珍
Owner 湖北省兴发磷化工研究院有限公司
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