Method for detecting the purity of n,n,n'-trimethylethylenediamine by gas chromatography

A technology of trimethylethylenediamine and gas chromatography, which is applied to the detection of the purity of N,N,N'-trimethylethylenediamine by gas chromatography, and the detection of unknown single impurities and total impurities, and can solve unknown Discovery and other problems, to achieve the effect of high repeatability, peak time and peak stability

Active Publication Date: 2020-07-07
ENANTIOTECH CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] At present, there is no relevant report on the purity detection method of N,N,N'-trimethylethylenediamine. In order to strengthen the quality control of N,N,N'-trimethylethylenediamine, it is necessary to establish a stable , reliable and accurate N,N,N'-trimethylethylenediamine purity gas chromatography detection method to quickly analyze the purity, unknown single impurities and total of N,N,N'-trimethylethylenediamine miscellaneous

Method used

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  • Method for detecting the purity of n,n,n'-trimethylethylenediamine by gas chromatography
  • Method for detecting the purity of n,n,n'-trimethylethylenediamine by gas chromatography
  • Method for detecting the purity of n,n,n'-trimethylethylenediamine by gas chromatography

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Embodiment 1

[0024] A method for detecting the purity of N, N, N'-trimethylethylenediamine by gas chromatography, comprising the following steps:

[0025] 1) Set the working conditions of the instrument: the temperature of the injection port is 200°C, the temperature of the detection port is 250°C, the carrier gas is high-purity nitrogen, the fuel gas is hydrogen, the auxiliary gas is compressed air, the column flow rate is 1.0ml / min, and split flow is used Injection, the split ratio of split injection is 50:1; among them, the chromatographic column used is DB-624 chromatographic column, the specification of chromatographic column is 30m*320μm*1.8μm, and the detector used is hydrogen flame ionization detector , the column temperature adopts a temperature program, the initial temperature is 48 ° C for 1 min, and then rises to 118 ° C at 18 ° C / min, then increases to 152 ° C at 3 ° C / min, maintains 3 min, and finally rises to 210 ° C at 3 ° C / min;

[0026] 2) Sampling detection: Precis...

Embodiment 2

[0029] A method for detecting the purity of N, N, N'-trimethylethylenediamine by gas chromatography, comprising the following steps:

[0030] 1) Set the working conditions of the instrument: the temperature of the injection port is 220°C, the temperature of the detection port is 280°C, the carrier gas is high-purity nitrogen, the fuel gas is hydrogen, the supporting gas is compressed air, the column flow rate is 1.0ml / min, and split flow is used Injection, the split ratio of split injection is 50:1; among them, the chromatographic column used is DB-624 chromatographic column, the specification of chromatographic column is 30m*320μm*1.8μm, and the detector used is hydrogen flame ionization detector , the column temperature adopts a temperature program, the initial temperature is 50°C for 2 minutes, and then rises to 120°C at 20°C / min, then rises to 160°C at 5°C / min, maintains it for 2 minutes, and finally rises to 220°C at 5°C / min;

[0031] 2) Sampling detection: Precisely meas...

Embodiment 3

[0034] A method for detecting the purity of N, N, N'-trimethylethylenediamine by gas chromatography, comprising the following steps:

[0035] 1) Set the working conditions of the instrument: the temperature of the injection port is 250°C, the temperature of the detection port is 300°C, the carrier gas is high-purity nitrogen, the fuel gas is hydrogen, the auxiliary gas is compressed air, the column flow rate is 1.0ml / min, and split flow is used. Injection, the split ratio of split injection is 50:1; among them, the chromatographic column used is DB-624 chromatographic column, the specification of chromatographic column is 30m*320μm*1.8μm, and the detector used is hydrogen flame ionization detector , the column temperature adopts a temperature program. The initial temperature is 52°C for 2 minutes, then rises to 125°C at 22°C / min, then rises to 162°C at 6°C / min, maintains it for 2 minutes, and finally rises to 225°C at 6°C / min;

[0036] 2) Sampling detection: Precisely measure ...

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Abstract

The invention discloses a method for detecting the purity of N,N,N'-trimethyl-ethanediamine with a gas chromatographic method. A DB-624 capillary chromatographic column is adopted for detection; the purity is calculated by adopting a peak area normalization method; the detection conditions are as follows: the temperature of a sample inlet is 200-250 DEG C, the temperature of a detection port is 250-300 DEG C, carrier gas is high-purity nitrogen, fuel gas is hydrogen, combustion-supporting gas is compressed air, the column flow is 1.0ml / min, split sampling is adopted, the split ratio is 50:1, adetector is a hydrogen flame ionization detector, the column temperature is risen by a program. The gas chromatographic detection method is stable, reliable, accurate, highly repeatable, and stable in appearance time and peak value of materials; through adoption of the detection method, the quality of the N,N,N'-trimethyl-ethanediamine can be well controlled.

Description

technical field [0001] The invention relates to the technical field of substance purity analysis, in particular to a method for detecting the purity of N,N,N'-trimethylethylenediamine, and more specifically to the detection of N,N,N'-trimethylethylenediamine by gas chromatography. The detection method of the purity of diamine, unknown single impurity and total impurity. Background technique [0002] N,N,N'-trimethylethylenediamine is the main component of more than a dozen products such as 4-chloro-2-methylbenzaldehyde and N-(2-dimethylaminoethyl)-N-methylformamide Production raw materials, when the impurity content of N,N,N'-trimethylethylenediamine is high, it will affect the quality of the produced product. Therefore, it is particularly important to establish a stable, reliable and accurate method for detecting the purity of N,N,N'-trimethylethylenediamine. [0003] Gas chromatography detection method has the advantages of high separation efficiency, fast analysis speed...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/54
CPCG01N30/02G01N30/54
Inventor 蒙发明曹欢燕徐亮
Owner ENANTIOTECH CORP
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