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Preparation method of gdx porous polymer series hollow capillary gas chromatography column

A technology of capillary chromatographic columns and porous polymers, which is applied in the field of preparation of GDX porous polymer series hollow capillary gas chromatographic columns, which can solve the problems of unsatisfactory use of GDX packed columns, unsatisfactory separation of polar compounds, tailing of chromatographic peaks, etc. problems, to achieve the effect of good elasticity, low column loss, and expand the scope of application

Active Publication Date: 2015-11-11
兰州东立龙信息技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, there are three types of porous polymer capillary chromatographic columns available commercially: Q, S, and U. The composition of the stationary phases of these limited types of porous polymer capillary chromatographic columns is not exactly the same as that of the GDX series of stationary phases, and because of Its variety is limited and cannot meet the needs of GDX packed columns
And there are also some disadvantages that the separation of some polar compounds is not ideal, and the chromatographic peaks are seriously tailed
[0006] To sum up, in the field of gas chromatography column preparation, there is no report on the GDX series porous polymer microsphere stationary phase quartz capillary PLOT column. This type of stationary phase is generally made into glass or stainless steel packed columns.

Method used

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  • Preparation method of gdx porous polymer series hollow capillary gas chromatography column
  • Preparation method of gdx porous polymer series hollow capillary gas chromatography column
  • Preparation method of gdx porous polymer series hollow capillary gas chromatography column

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Example 1The preparation method of the GDX porous polymer series hollow capillary gas chromatography column comprises the following steps:

[0036] (1) First rinse the inner wall of the elastic quartz capillary column with 1mol / LHF, then rinse the inner wall of the elastic quartz capillary column with clear water for 3 times, and finally install the rinsed elastic quartz capillary column on the chromatographic instrument, and purge with nitrogen gas, And heated to 200 ° C, kept for 6h, that is, the pretreated elastic quartz capillary column.

[0037] Wherein: the inner diameter of the elastic quartz capillary is 0.32 mm, and the length is 15 meters.

[0038] (2) Preparation of polymer microsphere seed suspension: disperse GDX polymer nanospheres in the dispersant, and ultrasonically stir and disperse for 60 minutes at a temperature of 20°C and a power of 100W to obtain a polymer with a mass concentration of 1.0%. Microsphere seed suspension.

[0039] in:

[0040] G...

Embodiment 2

[0050] Example 2 The preparation method of the GDX porous polymer series hollow capillary gas chromatography column comprises the following steps:

[0051] (1) First rinse the inner wall of the elastic quartz capillary column with 3mol / LHF, then rinse the inner wall of the elastic quartz capillary column with clear water 4 times, and finally install the rinsed elastic quartz capillary column on the chromatographic instrument, and purge with nitrogen, And heated to 300 ° C, keep 4h, that is, the pretreated elastic quartz capillary column.

[0052] Wherein: the inner diameter of the elastic quartz capillary is 0.53 mm, and the length is 60 meters.

[0053] (2) Preparation of polymer microsphere seed suspension: disperse GDX polymer nanospheres in the dispersant, and ultrasonically stir and disperse for 30 minutes at a temperature of 25°C and a power of 150W to obtain a polymer with a mass concentration of 5%. Microsphere seed suspension.

[0054] in:

[0055] GDX polymer na...

Embodiment 3

[0065] Example 3 The preparation method of the GDX porous polymer series hollow capillary gas chromatography column comprises the following steps:

[0066] (1) First rinse the inner wall of the elastic quartz capillary column with 2mol / LHF, then rinse the inner wall of the elastic quartz capillary column with clear water for 3 times, and finally install the rinsed elastic quartz capillary column on the chromatographic instrument, and purge with nitrogen, And heated to 250 ℃, keep 5h, namely the pretreated elastic quartz capillary column.

[0067] Wherein: the inner diameter of the elastic quartz capillary is 0.40 mm, and the length is 35 meters.

[0068] (2) Preparation of polymer microsphere seed suspension: disperse GDX polymer nanospheres in the dispersant, and ultrasonically stir and disperse for 45 minutes at a temperature of 22°C and a power of 125W to obtain a polymer with a mass concentration of 3%. Microsphere seed suspension.

[0069] in:

[0070] GDX polymer na...

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Abstract

The invention relates to a preparation method of a hollow capillary tubular gas chromatographic column in a GDX porous polymer series. The method comprises the following steps that (1), HF is used for washing the inner wall of an elastic capillary tubular column in a dripping mode, then blowing is carried out, and a pre-processed elastic capillary tubular column is obtained; (2), polymer micro-sphere seed suspension liquid is prepared; (3), the two ends of the pre-processed elastic capillary tubular column are connected with buffer columns respectively, then the polymer micro-sphere seed suspension liquid is pressed into the buffer columns through nitrogen, and an elastic capillary tubular column of which the inner wall is coated with polymer seeds is obtained; (4), a polymerization reaction monomer suspension liquid is prepared; (5), the polymerization reaction monomer suspension liquid and a cross-linking agent are evenly mixed according to a proportion, and then stable suspension liquid is obtained; (6), the stable suspension liquid is pressed into the elastic capillary tubular column of which the inner wall is coated with the polymer seeds through nitrogen, after a coating is deposited in a water bath and then is blown dry, and then a hollow capillary tubular chromatographic column is obtained; (7), chromatographic column aging processing is carried out on the hollow capillary tubular chromatographic column, and chromatographic column testing evaluation is carried out after aging processing is finished. The method is low in column loss and stable in performance.

Description

technical field [0001] The invention relates to a preparation method of a GDX series porous polymer stationary phase quartz capillary chromatographic column, in particular to a preparation method of a GDX porous polymer series hollow capillary gas chromatographic column. Background technique [0002] The GDX series stationary phase is a domestic porous polymer bead gas chromatography stationary phase. GDX is a cross-linked polymer porous polymer ball obtained by suspension copolymerization of styrene-divinylbenzene. After heat treatment, it forms a polymer ball with a porous structure. The current commodity types are: GDX-101, GDX-102, 103, 201, 301, 401, 501, 601, etc. This type of stationary phase has good thermal stability, high temperature resistance, no loss after long-term use, and good selectivity to alcohols, acids, vinegars, aldehydes, alkanes, aromatics, nitriles, halogenated alkanes and nitrogen oxides. It is suitable for separating homologues with a high boilin...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/285B01J20/30
Inventor 雷晓强马金婵景海生
Owner 兰州东立龙信息技术有限公司
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