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Method for detecting 1,3-bis(1-isocyanate-1-methylethyl)benzene in adhesive through liquid chromatography

A technology of liquid chromatography and methyl ethyl, which is applied in the field of quality inspection, can solve the problems of rare reports on product residue detection, and achieve the effects of low detection limit, good precision, and small matrix interference

Active Publication Date: 2020-12-18
广电计量检测(无锡)有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Based on safety considerations, the International Aerospace Environment Organization has listed it as a banned substance. However, the current research on it is concentrated in the field of synthesis and application, and there are few reports on the detection of its residues in products.

Method used

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  • Method for detecting 1,3-bis(1-isocyanate-1-methylethyl)benzene in adhesive through liquid chromatography
  • Method for detecting 1,3-bis(1-isocyanate-1-methylethyl)benzene in adhesive through liquid chromatography
  • Method for detecting 1,3-bis(1-isocyanate-1-methylethyl)benzene in adhesive through liquid chromatography

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Embodiment 1

[0052] A method for detecting 1,3-bis(1-isocyanato-1-methylethyl)benzene in an adhesive by liquid chromatography may further comprise the steps:

[0053] (1) Sample pretreatment

[0054] Weigh 1.0g±0.1g (accurate to 0.1mg) of a representative adhesive sample, put it into a 20mL brown sample bottle, add 10mL of dichloromethane and 200μL of derivatization reagent to it, and sonicate at room temperature for 40min; after the reaction Concentrate to dryness with nitrogen blowing, then add 10mL of derivative solvent, ultrasonically dissolve and filter through a 0.22μm filter membrane for on-machine measurement;

[0055] (2) Liquid chromatography detection

[0056] The sample solution is detected by a liquid chromatograph, and the chromatographic conditions are as follows:

[0057] Chromatographic column: ZORBAX SB-Aq (4.6*250mm, 5μm);

[0058] Injection volume: 10μL;

[0059] Column temperature: 40°C;

[0060] Mobile phase: use 20mM ammonium acetate solution as mobile phase A, ...

Embodiment 2

[0064] A method for liquid chromatography detection of 1,3-bis(1-isocyanato-1-methylethyl)benzene in adhesive, said method comprising the following steps:

[0065] (1) Sample pretreatment

[0066] Weigh 1.0g±0.1g (accurate to 0.1mg) of a representative adhesive sample, put it into a 20mL brown sample bottle, add 5mL of dichloromethane and 100μL of derivatization reagent to it, and ultrasonicate for 30min at room temperature; after the reaction Concentrate to dryness with nitrogen blowing, then add 10mL of derivative solvent, ultrasonically dissolve and filter through a 0.22μm filter membrane for on-machine measurement;

[0067] (2) Liquid chromatography detection

[0068] The sample solution is detected by a liquid chromatograph, and the chromatographic conditions are as follows:

[0069] Chromatographic column: ZORBAX SB-Aq (4.6*250mm, 5μm);

[0070] Injection volume: 2μL;

[0071] Column temperature: 40°C;

[0072] Mobile phase: use 5mM ammonium acetate solution as mobi...

Embodiment 3

[0076] A method for liquid chromatography detection of 1,3-bis(1-isocyanato-1-methylethyl)benzene in adhesive, said method comprising the following steps:

[0077] (1) Sample pretreatment

[0078] Weigh 1.0g±0.1g (accurate to 0.1mg) of a representative adhesive sample, put it into a 20mL brown sample bottle, add 15mL of dichloromethane and 300μL of derivatization reagent to it, and ultrasonicate for 60min at room temperature; after the reaction Concentrate to dryness with nitrogen blowing, then add 15mL of derivative solvent, ultrasonically dissolve and filter through a 0.22μm filter membrane for on-machine measurement;

[0079] (2) Liquid chromatography detection

[0080] The sample solution is detected by a liquid chromatograph, and the chromatographic conditions are as follows:

[0081] Chromatographic column: ZORBAX SB-Aq (4.6*250mm, 5μm);

[0082] Injection volume: 15μL;

[0083] Column temperature: 40°C;

[0084] Mobile phase: use 20mM ammonium acetate solution as m...

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Abstract

The invention relates to an analytical test method for determining 1,3-bis(1-isocyanate-1-methylethyl)benzene in an adhesive product by a high performance liquid chromatography fluorescence method, and the 1,3-bis(1-isocyanate-1-methylethyl)benzene can form symmetrical chromatographic separation peaks within 15 minutes through the optimal setting of instrument analysis parameters. The analytical test method provided by the invention is low in detection limit, good in precision and high in sample adding standard recovery rate, and meets the test requirements of 1,3-bis(1-isocyanate-1-methylethyl)benzene in adhesive products, wherein the correlation coefficient of the derivative product reaches 0.9996 within the concentration range of 0.01-0.20 mg / L; the detection limit and the quantitativelimit are relatively low and are only 0.0014 mg / L and 0.0048 mg / L respectively; rSD%<4.5%; and the average adding standard recovery rate of the sample is 91.7%-100.3%.

Description

technical field [0001] The invention relates to a method for detecting 1,3-bis(1-isocyanato-1-methylethyl)benzene in an adhesive by liquid chromatography, and belongs to the technical field of quality detection. Background technique [0002] 1,3-bis(1-isocyanato-1-methylethyl)benzene (TMXDI), molecular formula C 14 h 16 N 2 o 2 . It is a colorless liquid at room temperature. As a new type of chemical raw material, it can improve the performance of coatings, adhesives, inks and other products, such as enhancing product strength, adhesion and flexibility, and has yellowing resistance and acid resistance. advantages of durability and durability. But it will also bring harm to people's health: studies have confirmed that it has a strong irritating effect on the eyes and respiratory tract. Inhalation of high-concentration vapor can cause bronchitis, bronchial pneumonia and pulmonary edema, and long-term exposure can cause chronic bronchitis and asthma. Wait. [0003] Based...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
CPCG01N30/88G01N2030/884
Inventor 钟琳李支薇张兰兰杨文宇严洪连林炼锋
Owner 广电计量检测(无锡)有限公司
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