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Gas chromatographic column pretreatment method for high-viscosity alcohol or/and amines

A gas chromatographic column and amine compound technology, which is applied in the field of high-viscosity alcohol or/and amine compound gas chromatographic column pretreatment, and can solve the problems of large sample volume, derivatization reagents, and cumbersome post-processing steps

Inactive Publication Date: 2012-10-10
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, this method requires a large amount of sample and derivatization reagents, and the post-processing steps are cumbersome

Method used

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  • Gas chromatographic column pretreatment method for high-viscosity alcohol or/and amines
  • Gas chromatographic column pretreatment method for high-viscosity alcohol or/and amines
  • Gas chromatographic column pretreatment method for high-viscosity alcohol or/and amines

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1 3

[0022] Embodiment 1 Trifluoroacetic anhydride blank experiment

[0023] Put 1mL of trifluoroacetic anhydride in a 5mL volumetric flask, shake at 0°C for 1min, keep at 50°C for 20min, and cool to 25°C to obtain a blank test sample of trifluoroacetic anhydride for gas chromatography detection.

Embodiment 2

[0024] Example 2 3-amino-1,2-propanediol derivatization method

[0025] 1. Derivatization treatment method

[0026] Put 1mL of trifluoroacetic anhydride in a 5mL volumetric flask, add 40.0mg of 3-amino-1,2-propanediol at 0°C, shake for 1min, react at 50°C for 20min, and cool to 25°C to obtain 3, which is used for gas chromatography detection. -Amino-1,2-propanediol sample.

[0027] After sample injection, the content of 3-amino-1,2-propanediol calculated by the area normalization method was 99.52%, which was consistent with the content ≥ 99.5% marked on the purchased 3-amino-1,2-propanediol sample.

[0028] 2. Linear analysis

[0029] Accurately weigh 3-amino-1,2-propanediol, process it according to the above method and detect it by gas chromatography, the data are shown in Table 1. Its linear equation is: y=12896x-5326, r 2 =0.998, this method has good linearity in the range of 10-50 mg.

[0030] Table 1 Linear equation experimental data

[0031] mass (mg)

...

Embodiment 3

[0041] Embodiment 3 glycerol derivatization treatment method

[0042] Put 0.8mL trifluoroacetic anhydride in a 5mL volumetric flask, add 20.0mg glycerol at 0°C, shake for 0.5min, react at 60°C for 10min, and cool to 20°C to obtain a glycerol sample for gas chromatography detection.

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Abstract

The invention discloses a gas chromatographic column pretreatment method for high-viscosity alcohol or / and amines. The pretreatment method comprises the following steps of: placing 0.5-1mL of derivatization reagent trifluoroacetic anhydride in a volumetric flask with the volume of 5mL; adding 10-50mg of high-viscosity alcohol or / and amines in the volumetric flask at the temperature of 0-5 DEG C; oscillating the mixture for 0.5-1 minute; reacting for 10-30 minutes at the temperature of 30-60 DEG C; and cooling to the temperature of 20-25 DEG C to obtain a sample for gas chromatography detection. The pretreatment method is mainly used for quickly analyzing high-viscosity alcohol or / and amines.

Description

technical field [0001] The invention relates to a gas chromatography detection column pretreatment method, in particular to a high viscosity alcohol or / and amine compound gas chromatography column pretreatment method. Background technique [0002] High-viscosity alcohols or / and amine compounds, such as glycerol and its derivatives, are an important class of chemical raw materials and are widely used in the field of fine chemicals: glycerin is widely used in pharmaceuticals, food processing, cosmetics preparation and organic synthesis; 2- Amino-1,3-propanediol, 3-amino-1,2-propanediol and 3-methylamino-1,2-propanediol are the key to the synthesis of non-ionic contrast agents iopamidol, iohexol and iopromide respectively Raw material, 2-amino-1,3-propanediol can also be used for the synthesis of antidiabetic drug voglibose (voglibose); 3-dimethylamino-1,2-propanediol can be used to produce cationic waterborne polyurethane, Degraded fabric softeners, anion exchange resins and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06
Inventor 梅苏宁吕剑杨建明赵锋伟王伟薛云娜余秦伟王为强
Owner XIAN MODERN CHEM RES INST
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