Unlock instant, AI-driven research and patent intelligence for your innovation.

Capillary open tubular column based on silicon dioxide zeolite nanoparticles as well as preparation and application thereof

A nano-zeolite and silica technology, applied in the field of nanotechnology and micro-separation, to achieve the effect of small sample volume, good analysis reproducibility and high chemical stability

Inactive Publication Date: 2018-07-24
EAST CHINA NORMAL UNIVERSITY
View PDF10 Cites 2 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are few reports on the combination of open-column capillary electrochromatography and amperometric detection technology

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Capillary open tubular column based on silicon dioxide zeolite nanoparticles as well as preparation and application thereof
  • Capillary open tubular column based on silicon dioxide zeolite nanoparticles as well as preparation and application thereof
  • Capillary open tubular column based on silicon dioxide zeolite nanoparticles as well as preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0059] Preparation of capillary open-tubular column based on silica nano-zeolite particles with an average particle size of 50 nm

[0060] Mix ethyl orthosilicate, tetrapropylammonium hydroxide and water, according to the molar ratio of 1:0.3:20, stir and react at room temperature for 2 hours, then evaporate and remove ethanol in a water bath at 70°C, and then fill the tank with water. Hydrothermal crystallization at 175°C for 3 days, suction filtration, washing, and drying of the obtained mixed solution at 100°C to obtain white powdery silica nano-zeolite particle material with an average particle diameter of 50 nm.

[0061] Get 5 mg of the obtained silica nano-zeolite particles and disperse them in 1 milliliter of absolute ethanol, and ultrasonicate for 45 minutes to obtain a white emulsion, and fill the white emulsion to the pre-prepared volume at a flow rate of 2 milliliters per hour with a syringe pump. In the treated bare fused silica capillary, the filling time was 15 m...

Embodiment 2

[0063] Preparation of capillary open-tubular column based on silica nano-zeolite particles with an average particle size of 200 nm

[0064] Mix ethyl orthosilicate, tetrapropylammonium hydroxide and water, according to the molar ratio of 1:0.18:20, stir and react at room temperature for 2 hours, then evaporate ethanol in a water bath at 70°C, and then fill the tank with water. Hydrothermal crystallization at 175° C. for 3 days, suction filtration, washing and drying of the obtained mixed solution to obtain a white powdery silicon dioxide nano-zeolite material with an average particle diameter of 200 nanometers.

[0065] Get 5 mg of the obtained silica nano-zeolite particles and disperse them in 1 milliliter of absolute ethanol, and ultrasonicate for 45 minutes to obtain a white emulsion, and fill the white emulsion to the pre-prepared volume at a flow rate of 2 milliliters per hour with a syringe pump. In the treated bare fused silica capillary, the filling time was 15 minutes...

Embodiment 3

[0070]Experimental conditions: the length of the bare fused silica capillary is 30 cm, the inner diameter is 50 microns, and the outer diameter is 360 microns; The bare fused silica capillary is prepared, and each end is cut off by 5 cm before use. The average particle size of silica nano-zeolite particles is 50 nm. Amperometric detection adopts a three-electrode system, with a saturated calomel electrode or silver chloride electrode as a reference electrode, a platinum wire as a counter electrode, and a carbon disc electrode with a diameter of 300 microns as a working electrode, with an oxidation potential of 950 millivolts. The electroosmotic flow marker is absolute ethanol; the running buffer solution is 80 mmol / L boric acid-borax buffer solution (pH=8.00); the running voltage is 5 kV; the injection time is 8 seconds (injection voltage is 5 kV).

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
The average particle sizeaaaaaaaaaa
Lengthaaaaaaaaaa
The inside diameter ofaaaaaaaaaa
Login to View More

Abstract

The invention discloses a preparation method of a capillary open tubular column based on silicon dioxide zeolite nanoparticles. The preparation method comprises the following steps: mixing a silicon source, an alkali source and water according to certain proportion, stirring, clarifying, removing ethanol through water bath, and performing hydrothermal crystallization to obtain silicalite-1 silicondioxide zeolite nanoparticles; dispersing the prepared silicon dioxide zeolite nanoparticles into a solvent, adding into a bare fused quartz capillary, sealing the two ends of the capillary, and sintering at high temperature to prepare the capillary open tubular column based on the silicon dioxide zeolite nanoparticles. A capillary electrochromatography of the capillary open tubular column basedon the silicon dioxide zeolite nanoparticles is combined with an amperometric detection system, separation and analysis of homologous compounds and multiple groups of isomers such as branched chain isomerism, position isomerism and conformation isomerism can be realized. The capillary open tubular column is simple in preparation process, good in separation effect and low in analysis cost; by adoption of an amperometric detection technology, the detection sensitivity of the capillary electrochromatography technology can be further improved.

Description

technical field [0001] The invention belongs to the intersection field of nanometer technology and micro-separation technology, and specifically relates to the preparation and application of a capillary open-tube column based on silica nanometer zeolite particles. Background technique [0002] Capillary Electrochromatography (CEC) combines the high separation efficiency of Capillary Electrophoresis (CE) and the high selectivity of High Performance Liquid Chromatography (HPLC), and is a promising electrophoretic separation mode. CEC can improve the separation selectivity of similar compounds by filling different stationary phases in the capillary, or directly bonding various ligands to the inner wall. Compared with the pressure-driven flow of HPLC, the plug-flow-driven mode in CEC mode allows the use of smaller particles (submicron or even nanoscale) in the packed column, which can provide higher column efficiency. At the same time, as a miniaturized separation technology, C...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): G01N30/60G01N27/447B01D15/22
CPCB01D15/22G01N27/44704G01N30/6078
Inventor 楚清脆刘琳珍赵小双李娜杨紫悦陈丽叶建农
Owner EAST CHINA NORMAL UNIVERSITY