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Gas chromatographic analysis method of 3-chloropropionyl chloride

A gas chromatographic analysis and chloropropionyl chloride technology, which is applied in the field of gas chromatographic analysis and gas chromatographic analysis of 3-chloropropionyl chloride, can solve the problems of complicated operation, long analysis period, poor parallelism, etc., and achieves accurate results and fast detection speed. , the effect of prolonging the service life

Inactive Publication Date: 2021-06-25
NANTONG TENDENCI CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Because 3-chloropropionyl chloride reacts with water, the liquid chromatography analysis method currently used for the determination of the purity of 3-chloropropionyl chloride has the disadvantages of long analysis period, cumbersome operation, and poor parallelism. Advanced detection and analysis methods to effectively detect and improve the purity of 3-chloropropionyl chloride products

Method used

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  • Gas chromatographic analysis method of 3-chloropropionyl chloride
  • Gas chromatographic analysis method of 3-chloropropionyl chloride
  • Gas chromatographic analysis method of 3-chloropropionyl chloride

Examples

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Embodiment 1

[0028] 1) Instruments: GC-2014 gas chromatograph, FID detector, split / splitless injector;

[0029] 2) Gas chromatography conditions: 30m×0.32mm×0.33um HT-FFAP capillary column; carrier gas pressure: 70kPa; hydrogen pressure: 50kPa; air pressure: 50kPa; detector temperature: 280°C; vaporization chamber temperature: 280°C; Temperature: 120°C; Split ratio: 10:1; Injection volume: 0.2uL.

[0030] 3) Determination steps:

[0031] A. Preparation of sample derivatives: Take about 5ml of 3-chloropropionyl chloride sample in a 25ml stoppered Erlenmeyer flask, add methanol for esterification, and shake well;

[0032] B. Injection analysis: take 0.2uL sample and inject it. When the instrument is stable and the error of two consecutive injections is less than 1%, take the average value to calculate the content of 3-chloropropionyl chloride;

[0033] C. Result calculation: figure 1 It is the gas chromatogram of sample detection, in which A is solvent, B is 3-chloropropionyl chloride, an...

Embodiment 2

[0035] 1) Instruments: GC-2014 gas chromatograph, FID detector, split / splitless injector;

[0036] 2) Gas chromatography conditions: 30m×0.32mm×0.33um HT-FFAP capillary column; carrier gas pressure: 70kPa; hydrogen pressure: 50kPa; air pressure: 50kPa; detector temperature: 280°C; vaporization chamber temperature: 280°C; Temperature: 120°C; Split ratio: 10:1; Injection volume: 0.1uL.

[0037] 3) Determination steps:

[0038] A. Preparation of sample derivatives: Take about 5ml of 3-chloropropionyl chloride sample in a 25ml stoppered Erlenmeyer flask, add methanol for esterification, and shake well;

[0039] B. Sampling analysis: Take 0.1uL sample and inject it. When the instrument is stable and the error of two consecutive injections is less than 1%, take the average value to calculate the content of 3-chloropropionyl chloride;

[0040] C. Result calculation: figure 2 It is the gas chromatogram of sample detection, in which A is solvent, B is 3-chloropropionyl chloride, an...

Embodiment 3

[0042] 1) Instruments: GC-2014 gas chromatograph, FID detector, split / splitless injector;

[0043] 2) Gas chromatography conditions: 30m×0.32mm×0.33um HT-FFAP capillary column; carrier gas pressure: 70kPa; hydrogen pressure: 50kPa; air pressure: 50kPa; detector temperature: 280°C; vaporization chamber temperature: 280°C; Temperature: 120°C; Split ratio: 10:1; Injection volume: 0.3uL.

[0044] 3) Determination steps:

[0045] A. Preparation of sample derivatives: Take about 5ml of 3-chloropropionyl chloride sample in a 25ml stoppered Erlenmeyer flask, add methanol for esterification, and shake well;

[0046] B. Sampling analysis: Take 0.3uL sample and inject it. When the instrument is stable and the error of two consecutive injections is less than 1%, take the average value to calculate the content of 3-chloropropionyl chloride;

[0047] C. Result calculation: image 3 It is the gas chromatogram of sample detection, in which A is solvent, B is 3-chloropropionyl chloride, and...

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Abstract

The invention provides a gas chromatographic analysis method of 3-chloropropionyl chloride. The method comprises the following steps of: taking a 3-chloropropionyl chloride sample in a container; adding methanol to realize esterification, and shaking up the container; introducing a sample after derivatization; separating and detecting the introduced sample through a gas chromatograph to obtain a gas chromatogram; and calculating the content percentage of the 3-chloropropionyl chloride through an area normalization method. According to the method of the present invention, an FFAP capillary chromatographic column is adopted, a result obtained through the detection of an FID detector is analyzed through the area normalization method, and therefore, the detection speed is fast, the result is accurate, the method is simple and practical; the 3-chloropropionic acid content and the 3-chloropropionyl chloride content in a prepared 3-chloropropionyl chloride product can be accurately detected; and the service life of the chromatographic column can be effectively prolonged.

Description

technical field [0001] The invention relates to a gas chromatography analysis method, in particular to a gas chromatography analysis method of 3-chloropropionyl chloride, which belongs to the technical field of analytical chemistry. Background technique [0002] 3-Chloropropionyl chloride, also known as β-chloropropionyl chloride, is one of the important downstream products of acrylic acid, and its molecular formula is C 3 h 4 Cl 2 O, the molecular structure formula is: [0003] [0004] The relative molecular mass is 126.97, the boiling point is 143-145°C, and the relative density is 1.33. It will react violently with water and is easily soluble in organic solvents such as alcohol, ether and chloroform. In the organic synthesis industry, 3-chloropropionyl chloride is a widely used fine chemical intermediate, mainly used in the fields of pesticides, medicine and organic synthesis. 3-Chloropropionyl chloride is mainly used in the synthesis of drugs for the treatment of...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/86G01N30/68G01N30/60G01N30/88
CPCG01N30/02G01N30/06G01N30/8634G01N30/68G01N30/60G01N30/6052G01N30/88G01N2030/067G01N2030/8845
Inventor 张岑卉
Owner NANTONG TENDENCI CHEM
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