Use of double-phenyl hybridization silica gel material monolithic column in chromatogram

A monolithic column, silica gel technology, applied in the field of chromatographic analysis, can solve inevitable problems and achieve the effect of suitable pore size, good physical and chemical properties and separation characteristics, and high selectivity

Inactive Publication Date: 2009-02-11
NAT INST OF METROLOGY CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Although the above-mentioned technologies have improved the physical and chemical properties of the material to a certain extent, improved the separation performance, expanded the scope of ap

Method used

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  • Use of double-phenyl hybridization silica gel material monolithic column in chromatogram
  • Use of double-phenyl hybridization silica gel material monolithic column in chromatogram
  • Use of double-phenyl hybridization silica gel material monolithic column in chromatogram

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] 1) Capillary pretreatment

[0033] The capillary column was rinsed with 0.2mol / L hydrochloric acid and water for 30 minutes in sequence, then soaked with 10% HF at a volume concentration of 35°C for 3 hours, then washed with 1.0mol / L sodium hydroxide, water and methanol for 30 minutes, and finally placed in a gas chromatography furnace. Blow dry with nitrogen at 160°C and set aside.

[0034] 2) The monolithic column of bisphenyl hybrid silica gel material is prepared according to the following steps:

[0035] ①Preparation of biphenyl hybrid silica gel material: Using acid-base catalyzed sol-gel method, add 110 μL of silane precursor to 220 μL of methanol, 22 μL of hydrochloric acid and 20 μL of aqueous solution, mix well, vortex for 3 minutes, and After hydrolysis at room temperature for 4 h, add 4 mg of dodecylamine and mix well, and the silane precursors are 60 μL of phenyltriethoxysilane (PTES) and 50 μL of 1,4-bistriethoxysilylbenzene (BTEB) ( see figure 1 );

...

Embodiment 2

[0044] The difference from Example 1 is:

[0045] 1) The process of capillary pretreatment is as follows: wash the capillary column with 0.3mol / L hydrochloric acid and water for 45min, then treat it with HF with a volume concentration of 15% at 50°C for 5h, and then wash it with 1.0mol / L sodium hydroxide and water Rinse with methanol for 45 minutes, and finally blow dry in a gas chromatograph oven at 210°C with nitrogen for use.

[0046] 2) The monolithic column of bisphenyl hybrid silica gel material is prepared according to the following steps:

[0047] ①Preparation of biphenyl hybrid silica gel material: Using acid-base catalyzed sol-gel method, add 120 μL of silane precursor to 120 μL of methanol, 12 μL of hydrochloric acid and 10 μL of aqueous solution. After hydrolysis for 6 hours, add 7 mg of dodecylamine and mix well, and set aside, the silane precursors are 100 μL of phenyltriethoxysilane and 20 μL of 1,4-bistriethoxysilylbenzene;

[0048] ②Preparation of bisphenyl ...

Embodiment 3

[0050] The difference from Example 1 is:

[0051] 1) The process of capillary pretreatment is as follows: wash the capillary column with 0.2mol / L hydrochloric acid and water for 40 minutes, then treat it with HF with a volume concentration of 13% at 46°C for 4 hours, and then wash it with 1.5mol / L sodium hydroxide and water Rinse with methanol for 40 minutes, and finally blow dry in a gas chromatograph oven at 190°C with nitrogen for use.

[0052] 2) The monolithic column of bisphenyl hybrid silica gel material is prepared according to the following steps:

[0053] ①Preparation of bisphenyl hybrid silica gel material: Using acid-base catalyzed sol-gel method, add 140 μL of silane precursor to 160 μL of methanol, 18 μL of hydrochloric acid and 15 μL of aqueous solution. After hydrolyzing for 3 hours, add 5 mg of dodecylamine and mix well, and set aside, the silane precursors are 90 μL of phenyltriethoxysilane and 50 μL of 1,4-bistriethoxysilylbenzene;

[0054] ②Preparation of...

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Abstract

The invention relates to a chromatographic analysis technology, in particular to the application of bi-phenylene hybrid silica-gel monolithic column of bridge-bond organic-inorganic hybridization periodically meso-pore separation material in a chromatogram. The specified preparation method of bi-phenylene hybrid silica-gel material adopts a sol-gel method of acid-base catalysis. Under the condition of acid catalysis, hydrolysis reaction is carried out to a monomer, and an alkaline catalyst is added to carry out polycondensation reaction. The reaction rates of the hydrolysis reaction and the polycondensation reaction of the monomer are controlled by controlling and changing the pH value of a reaction system in the reaction process and the hydrolysis reaction and the polycondensation reaction of the monomer are effectively completely separated by the two-step catalysis method so as to obtain monolithic or particle material with uniform frame structure, suitable aperture and periodic meso-pores. Therefore, the chromatographic analysis technology meets the demands of separation, improves processing technology of the internal wall of quartz capillary, obtains stable monolithic separation material, is capable of separating acid, neutral and alkai compounds under the model of capillary electrochromatography, and shows that the material has excellent separation efficiency and separative selectivity.

Description

technical field [0001] The invention relates to chromatographic analysis technology, in particular to the application of a biphenyl hybrid silica gel material monolithic column of a bridging organic-inorganic hybrid periodic mesoporous separation material in chromatography. Background technique [0002] Separation materials are important components of chromatographic techniques including liquid chromatography and capillary electrochromatography, as well as the main materials for sample processing techniques such as solid phase extraction and solid phase microextraction. The characteristics of separation materials directly affect the analysis efficiency and application range. Wait. In recent years, with the development of chromatographic analysis technology and the improvement of practical application requirements, higher and higher requirements have been put forward for separation materials. [0003] Currently commonly used liquid chromatography and capillary electrochromat...

Claims

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Application Information

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IPC IPC(8): B01J20/285B01J20/286
Inventor 张庆合严丽娟
Owner NAT INST OF METROLOGY CHINA
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