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Method for detecting residual amount of triphosgene in industrial waste liquid

A technology of industrial waste liquid and triphosgene, applied in the field of chemical analysis, achieves good stability, good linearity and good specificity

Active Publication Date: 2022-02-08
CHANGZHOU HEQUAN PHARMA CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, no effective test method for triphosgene residues in industrial waste liquids has been found in this field. Therefore, to establish a method with simple operation, accurate results and high sensitivity, which can be used for the analysis of triphosgene residues in industrial waste liquids is Technical problems to be solved in this field

Method used

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  • Method for detecting residual amount of triphosgene in industrial waste liquid
  • Method for detecting residual amount of triphosgene in industrial waste liquid
  • Method for detecting residual amount of triphosgene in industrial waste liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0059] The content of triphosgene in embodiment 1 industrial waste liquid

[0060] 1) Preparation of standard reference solution: Weigh 50 mg of triphosgene into a 50 mL volumetric flask, add 25 mL of acetonitrile solvent to dissolve, add 300 mg of benzylamine after dissolving, and ultrasonicate for 30 min at 35±5°C (ultrasonic power 50W), after the reaction is complete Then add 25mL of the mixed solution of acetonitrile and dimethyl sulfoxide (the volume ratio of the two is 1:1), to obtain a standard reference substance stock solution with a concentration of 1 mg / mL; take the standard reference substance stock solution, and diluent (water and two The mixed solution of methyl sulfoxide, the volume ratio of the two is 1:1; unless otherwise specified, the diluents in this application are all this solution) to dilute and prepare the standard reference solution with the following concentration: 2.0ng / mL, 5.0 ng / mL, 8.0ng / mL, 10.0ng / mL, 12.0ng / mL and 20.0ng / mL.

[0061] 2) Prepara...

Embodiment 2

[0064] Embodiment two methodological verification

[0065] 1) Specificity experiment

[0066] Preparation of the test sample spiked solution: Take 50mg of industrial waste liquid in a 50mL volumetric flask, add 25mL of acetonitrile solvent to dissolve, add 300mg of benzylamine after dissolution, and ultrasonicate for 30min at 35±5°C (ultrasonic power 50W), after the reaction is complete Then add the mixed solution of 25mL acetonitrile and dimethyl sulfoxide (the volume ratio of the two is 1:1), to obtain the stock solution of the test substance whose concentration is 1mg / mL; take the standard control of 1mL of the stock solution of the test substance and 100ng / mL Put 1mL of the test solution in a 10mL volumetric flask, shake it to a constant volume with a diluent, and obtain the test solution with a concentration of 0.1mg / mL.

[0067] Get the blank solution prepared in embodiment 1, concentration is the standard reference substance solution of 10ng / mL, concentration is the ne...

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Abstract

The invention discloses a method for detecting the residual amount of triphosgene in industrial waste liquid. The method comprises the following steps: preparing a standard reference solution, preparing a test sample solution, detecting a triphosgene derivative by adopting a high performance liquid chromatography-mass spectrometry method, and then calculating the residual amount of the triphosgene by adopting an external standard method. According to the triphosgene detection method provided by the invention, the amount of triphosgene is obtained by detecting the amount of a derivative by utilizing the specificity that triphosgene and a derivatization reagent are completely reacted; methodology verifies that the content of the triphosgene in the industrial waste liquid can be detected to be at least lower than 2ng, and the requirement of the industrial waste liquid on the triphosgene emission standard is met; the method is high in precision, and the retention time RSD% is 0.02%; the method is good in specificity, and the triphosgene derivative chromatogram is not interfered by other peaks; according to the method, the linearity of the triphosgene derivative is good in a range of 2ng / mL to 20ng / mL; the triphosgene derivative is stable in a recovery solution for at least 12 hours, the stability is good, and the recovery rate is high.

Description

technical field [0001] The invention relates to the technical field of chemical analysis, in particular to a method for detecting residual triphosgene in industrial waste liquid. Background technique [0002] Triphosgene, also known as solid phosgene, has a chemical name of bis(trichloromethyl)carbonate, or BTC for short, and is a white crystalline compound with an odor similar to phosgene, and its molecular formula is CO(OCCl 3 ) 2 . The reactivity of triphosgene is similar to that of phosgene. It can react with various compounds such as alcohols, aldehydes, amines, amides, carboxylic acids, phenols, and hydroxylamines. It can also be cyclized and condensed to prepare heterocyclic compounds. The main reactions that can be carried out are carbonylation reaction, cyclocondensation, and some polymerization reactions, etc., can be applied to the production of all chemical products using phosgene and diphosgene. Because triphosgene is a stable solid compound, it can be sealed...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/72
CPCG01N30/02G01N30/06G01N30/72G01N2030/067G01N2030/027
Inventor 胡研黄勤琴陈伊杰叶立文
Owner CHANGZHOU HEQUAN PHARMA CO LTD
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