Integrated sol-gel matrix capillary column and preparation method thereof

A capillary monolithic column and sol-gel technology, applied in separation methods, chemical instruments and methods, and other chemical processes, can solve problems such as increased entropy, chaotic molecular motion, and complex actions, and achieve improved efficiency, tight combination, and heavy effect of guarantee

Active Publication Date: 2016-07-06
HENAN INST OF SCI & TECH
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  • Claims
  • Application Information

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Problems solved by technology

Another point of view is that the effect of microwaves on chemical reactions is very complicated. On the one hand, the reactant molecules absorb microwave energy, which increases the speed of molecular motion, resulting in chaotic molecular motions, resulting in an increase in entropy; in addition, the effect of microwaves on polar molecules, Forcing it to move in accordance with the action of the electromagnetic field leads to an increase in entropy. Therefore, the mechanism of microwave action on chemical reactions cannot be described only by the microwave heating effect.

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  • Integrated sol-gel matrix capillary column and preparation method thereof
  • Integrated sol-gel matrix capillary column and preparation method thereof
  • Integrated sol-gel matrix capillary column and preparation method thereof

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Embodiment Construction

[0021] The present invention will be described in detail below in conjunction with specific embodiments.

[0022] Experimental procedure

[0023] Reagents: methacryloxypropyltrimethoxysilane, sodium hydroxide, hydrochloric acid, methanol, toluene, sodium dodecylsulfonate, tris(Tris), acetonitrile, naphthalene, toluene, thiourea , Benzene, biphenyl.

[0024] making process:

[0025] 2.1 Preparation of polymerization solution: 1150 μL of methacryloxypropyltrimethoxysilane and 300 μL of 0.12M hydrochloric acid were stirred at room temperature for 30 minutes in the dark to obtain a monomer solution. Then, 800 μL of toluene and 50 mg of SDS (sodium dodecylsulfonate) were added to 200 μL of the monomer solution, and stirred at room temperature for 30 minutes to obtain a toluene-monomer solution mixture containing SDS.

[0026] 2.2 Capillary pretreatment: (1) sequentially use 0.1M NaOH, H 2 O, 0.1M HCl solution rinsed for 0.5h, and then rinsed with water to pH = 7; (2) rinsed wit...

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Abstract

The invention discloses an integrated sol-gel matrix capillary column and a preparation method thereof. The preparation method comprises the steps: filling 10cm polymerized solution into alkenylation capillary, and then microwave-polymerizing for 14.5min at 80 DEG C and 700W. According to the invention, the integrated sol-gel matrix capillary column is in-situ prepared in the capillary through a temperature-controlling microwave synthesizer. The prepared integrated column is subjected to chromatography performance evaluation under a pressurizing electrochromatography (P-CEC) separating mode; the four matters of thiourea, naphthalene, methylbenzene and biphenyl are subjected to baseline separation; the lowest theoretical plate height of naphthalene can reach 1.83 mu m; compared with an experimental result of a common microwave method, the result is that the theoretical plate quantity of naphthalene is increased to 54749 / m from 10000 / m and the separation column effect of the compound is greatly increased. A scanning electron microscope result shows that the integrated materials in the tube of the integrated sol-gel matrix capillary column prepared through the temperature-controlling microwave method are uniformly distributed and are tightly combined with the inner wall of the capillary.

Description

technical field [0001] The invention relates to capillary monolithic column technology, in particular to a sol-gel matrix capillary monolithic column and a preparation method thereof. Background technique [0002] Capillary electrochromatography (CEC) is a micro-column liquid chromatography separation technique driven by electroosmotic flow. It combines the high selectivity of high performance liquid chromatography (HPLC) with the high efficiency of capillary electrophoresis (CE), and is a new type of micro-separation technology. It has the characteristics of fast separation and less consumption of samples and reagents. It is not only used for the separation and analysis of ionic compounds, but also for the separation and analysis of neutral compounds. [0003] Capillary column is the core of capillary electrochromatography separation and analysis, and the preparation of capillary column is the key of capillary electrochromatography. Capillary electrochromatographic colum...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D15/22B01D15/20B01J20/281B01J20/30G01N30/60
CPCB01D15/20B01D15/22B01J20/281B01J2220/84B01J2220/86G01N30/6078
Inventor 张裕平许明录龚文君陈娜张毅军陈军李英杨靖华涂剑秋
Owner HENAN INST OF SCI & TECH
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