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Analysis of trichloromethane stationary phase by gas chromatography method, and preparation method and applications of stationary phase

A gas chromatography and chloroform technology, applied in the field of preparation of the stationary phase, can solve the problems of high use cost of capillary column, low use temperature of packed column, etc., and achieve short analysis period, long service life and low use cost. Effect

Active Publication Date: 2013-10-09
安徽翔基科学仪器有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] In view of the shortcomings of the low operating temperature of the packed column in the GB / T4118-1993 standard and the high cost of the capillary column in the GB / T21541-2008 standard, there is an urgent need for an analytical instrument with low cost, high operating temperature, corrosion resistance, high sensitivity, and low baseline noise. Chloromethane packed chromatographic column, and stationary liquid is not easy to lose

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  • Analysis of trichloromethane stationary phase by gas chromatography method, and preparation method and applications of stationary phase
  • Analysis of trichloromethane stationary phase by gas chromatography method, and preparation method and applications of stationary phase

Examples

Experimental program
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Effect test

Embodiment 1

[0026] The preparation of high-temperature packed chromatographic column for chloroform analysis comprises the following steps:

[0027] 1. Preparation of stationary phase

[0028] In this example, the packed column uses modified polyethylene glycol (TM-FFAP), methyl silicone rubber SE30, and 6201 support with a particle size of 60 mesh as the stationary phase at a mass ratio of 9.5:10.5:100. The specific preparation method is as follows:

[0029] A. Accurately weigh the amount of modified polyethylene glycol (TM-FFAP) and 6201 support, then add the modified polyethylene glycol (TM-FFAP) into a 250mL Erlenmeyer flask and add acetone equivalent to the volume of 6201 support , install a condenser tube and reflux at a temperature of 60°C for 1.5 hours to completely dissolve (TM-FFAP), then add the formulated amount of 6201 support to the Erlenmeyer flask, continue heating and reflux for 1.5 hours, and shake 3 times during the reflux process. Avoid sticking to the carrier on the ...

Embodiment 2

[0035] 1. Preparation of stationary phase

[0036]In this example, the packed column uses modified polyethylene glycol TM-FFAP, methyl silicone rubber SE30, and 6201 support with a particle size of 70 mesh as the stationary phase at a mass ratio of 9:11:100. The specific preparation method is as follows:

[0037] A. Accurately weigh the modified polyethylene glycol TM-FFAP and the 6201 carrier of the formula, then add the modified polyethylene glycol TM-FFAP to a 250mL Erlenmeyer flask and add acetone equivalent to 1.05 times the volume of the 6201 carrier. The upper condenser was refluxed for 1 hour at a temperature of 62 ° C to completely dissolve TM-FFAP, then add the formulated amount of 6201 support into the Erlenmeyer flask, continue heating and reflux for 3 hours, and shake 3 times during the reflux process to avoid contamination of the bottle wall. Attached carrier, after the reflux is completed, remove the condenser tube, let the acetone evaporate to dryness, and obta...

Embodiment 3

[0042] 1. Preparation of stationary phase

[0043] In this example, the packed column uses modified polyethylene glycol TM-FFAP, methyl silicone rubber SE30, and 6201 support with a particle size of 80 mesh at a mass ratio of 10:10:100 as the stationary phase. The specific preparation method is as follows:

[0044] A. Accurately weigh the modified polyethylene glycol TM-FFAP and 6201 support in the formula, then add the modified polyethylene glycol TM-FFAP into a 250mL Erlenmeyer flask and add acetone equivalent to 1.1 times the volume of the 6201 support. The upper condenser tube was refluxed for 2 hours at a temperature of 62°C to completely dissolve TM-FFAP, then add the formulated amount of 6201 support into the Erlenmeyer flask, continue heating and reflux for 2 hours, and shake twice during the reflux process to avoid contamination of the bottle wall. Attached carrier, after the reflux is completed, remove the condenser tube, let the acetone evaporate to dryness, and obt...

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Abstract

The invention discloses analysis of trichloromethane stationary phase by a gas chromatography method, and a preparation method and applications of the stationary phase. The stationary phase consists of modification polyethylene glycol, methyl silicone rubber SE30 and a 6201 supporter with a mass ratio of 9-10:10-11:100. The preparation method of the stationary phase is simple, and free in special equipment; and the prepared stationary phase is used to prepare a gas chromatography column. The gas chromatography column is low in cost, economical and practical; the analysis period is short and can be finished in 15 minutes; the peak time of carbon tetrachloride is ahead of the main peak trichloromethane; and thereby the detection accuracy is improved, and a new detection chromatography column is provided for the analysis of trichloromethane.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and in particular relates to a stationary phase for analyzing chloroform by gas chromatography and a chromatographic column containing the stationary phase, as well as a preparation method and application of the stationary phase. Background technique [0002] In the original GB / T4118-1993 product standard, the stationary phase of the packed chromatographic column for the analysis of chloroform is based on the mass ratio of DBP: PEG-2000: 6201, and the support is 15: 5: 100. The use temperature of the liquid is low (the maximum use temperature is 100 degrees), and the stationary liquid is easy to lose, the service life is short, and the basic current is large, so the hydrogen flame detector (FID) cannot be used to measure the concentration of chloroform under high sensitivity. Impurity content. The new version of the GB / T4118-2008 product standard refers to the GB / T21541-2008 method standard, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/281B01J20/30G01N30/02
Inventor 左祥东江朝学
Owner 安徽翔基科学仪器有限公司
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