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Method for measuring concentration of chloroacetic acid in air by gas chromatography and application thereof

A technology of gas chromatography and determination method, which is applied in the field of gas chromatography to measure the concentration of chloroacetic acid in the air, which can solve the problems such as cumbersome steps, achieve the effects of reducing polarity, good linear relationship, and solving inaccurate quantification

Pending Publication Date: 2020-12-25
ZHEJIANG CENT FOR DISEASE CONTROL & PREVENTION
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Problems solved by technology

[0004] In order to reduce the polarity of chloroacetic acid, concentrated sulfuric acid-ethanol solution is used in the prior art to derivatize chloroacetic acid into ethyl chloroacetate and then measure it by gas chromatography, but the method steps are cumbersome, and concentrated sulfuric acid has certain dangers

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  • Method for measuring concentration of chloroacetic acid in air by gas chromatography and application thereof
  • Method for measuring concentration of chloroacetic acid in air by gas chromatography and application thereof
  • Method for measuring concentration of chloroacetic acid in air by gas chromatography and application thereof

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Embodiment

[0040] Scope: the present invention is suitable for gas chromatography to measure the concentration of chloroacetic acid in the air.

[0041] Principle: Use silica gel tubes to collect chloroacetic acid in the air, dry the sampled silica gel tubes in an oven, add acetonitrile:N,O-bis(trimethylsilane)trifluoroacetamide mixed solution, desorb and react at room temperature, The silanized product was analyzed by gas chromatography and quantified by an external standard method.

[0042] Instruments and equipment: Samples were collected using a Gilair plus explosion-proof personal air sampler (0-2L / min) (Gilian Company, USA).

[0043] Preparation of standard stock solution: add a small amount of acetonitrile to a 10mL volumetric flask, accurately weigh 108.40mg of chloroacetic acid and add it to the volumetric flask, and dilute to the mark with acetonitrile to obtain a standard stock solution with a concentration of 10.840mg / mL.

[0044] Preparation of standard series solutions: Ad...

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Abstract

The invention belongs to the technical field of chemical component detection and analysis, and discloses a method for measuring the concentration of chloroacetic acid in air by gas chromatography andapplication thereof. According to the measuring method, under the detection means of gas chromatography, N, O-bis (trimethylsilane) trifluoroacetamide is used for silanizing chloroacetic acid under acertain condition, so that the polarity of chloroacetic acid is greatly reduced, the problem of inaccurate quantification caused by strong polarity trailing of chloroacetic acid is solved, and the detection sensitivity of chloroacetic acid is greatly improved. The detection method has a good linear relationship in the concentration range of 0-162.6 micrograms / mL, the correlation coefficient is 0.9997, the detection limit is 0.8 micrograms / mL, the minimum detection concentration is 0.05mg / m< 3 > (by collecting 15L of air), the Relative Standard Deviation (RSD) of five times of parallel determination is 0.5-1.3%, and the blank adding standard recovery rate is 98.6-101.2%. The method is sensitive, simple and accurate, and can be used for measuring chloroacetic acid in air in a workplace.

Description

technical field [0001] The invention belongs to the technical field of chemical component detection and analysis, and in particular relates to a method for measuring the concentration of chloroacetic acid in air by gas chromatography and an application thereof. Background technique [0002] Chloroacetic acid is an intermediate in industries such as dyestuffs, pharmaceuticals, and pesticides, and has broad application prospects. At room temperature, chloroacetic acid is a colorless or white crystal with a pungent odor and strong corrosiveness. It can be absorbed through the respiratory tract, digestive tract and skin, causing damage to multiple organs in the human body. The maximum allowable concentration (MAC) of chloroacetic acid in the air of daily workplaces is 2mg / m 3 . [0003] Among the methods provided in the current national standard, chloroacetic acid in the workplace air is routinely collected by silica gel tube, desorbed by water, and determined by packed column...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/86
CPCG01N30/02G01N30/06G01N30/8675G01N2030/047
Inventor 王鹏曹艺耀任鸿张东霞张美辨楼晓明徐秋凉周振胡勇
Owner ZHEJIANG CENT FOR DISEASE CONTROL & PREVENTION
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