Silica gel integral open-tube capillary column with metal wire as template and preparation method thereof

An open-tube capillary column and capillary technology, applied in separation methods, alkali metal compounds, chemical instruments and methods, etc., can solve the problems of difficult to prepare stationary phase, capillary blockage, uneven distribution of stationary phase, etc.

Active Publication Date: 2022-06-07
ANHUI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in capillary tubes with larger diameters (≥20 μm), there are problems such as silica sol being affected by gravity, which can easily lead to capillary clogging, uneven distribution of stationary phase, and difficulty in preparing thicker stationary phases.

Method used

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  • Silica gel integral open-tube capillary column with metal wire as template and preparation method thereof
  • Silica gel integral open-tube capillary column with metal wire as template and preparation method thereof
  • Silica gel integral open-tube capillary column with metal wire as template and preparation method thereof

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preparation example Construction

[0037] The invention provides a preparation method of a silica gel integral open-tube capillary column using a metal wire as a template, the preparation method comprising:

[0038] 1) introducing the metal wire into the first capillary as a template, then filling the sol solution into the capillary, and then capping both ends of the first capillary;

[0039] 2) heat-treating the capillary, then carrying out temperature-programmed treatment, then removing the template, then sequentially cleaning, drying and calcining the first capillary to obtain an integral open-tube capillary column of silica gel;

[0040] Wherein, the sol solution includes polyethylene glycol, urea, methyl orthosilicate, and acetic acid solution.

[0041] In the above preparation method, the content of each component in the sol solution can be selected in a wide range, but in order to further optimize the shrinkage rate, mechanical strength and porosity of the stationary phase of the integral open capillary ...

preparation example 1

[0068] like Figure 12 As shown in a-d, place the spotting capillaries of various sizes vertically, cover the lower end with a 20 μL pipette tip, burn the spotting capillary in the middle, and the glass is heated and softened and pulled down naturally. The inner diameter of the cauterized spotting capillary is gradually reduced, and is cut with a capillary cutter at the place where the metal filament 4 cannot penetrate to form a second capillary of various specifications.

Embodiment 1

[0070] 1) Dissolve 0.124g PEG-10000 and 0.09g urea in 1mL acetic acid solution (pH is 3.4), stir under ice-water bath for 10 minutes, add 400μL of methyl orthosilicate TMOS to it, stir under ice-water bath for 40min, keep Shake for 10 min in an ice-water bath and sonicate at 50 KHz for degassing.

[0071] The metal wires were sonicated in high-purity water and ethanol for 8-10 min, respectively, and then dried.

[0072] The capillary of the chromatographic column was successively washed with sodium hydroxide solution with a concentration of 1 mol / L, hydrochloric acid solution with a concentration of 0.1 mol / L, high-purity water and acetone at 60 °C for 5 h.

[0073] 2) Filter the above sol solution with a 0.45 μm syringe filter, and fill it into a chromatographic column capillary (inner diameter 75 μm, outer diameter 365 μm) pierced with template gold wire (50 μm in diameter).

[0074] After positioning the template (the maximum diameter of the wide end of the second capillar...

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Abstract

The invention discloses a silica gel integral open-tube capillary column with a metal wire as a template and a preparation method thereof. The preparation method comprises: 1) introducing the metal wire into the first capillary as a template, and then filling the sol solution into the capillary , and then both ends of the first capillary are capped; 2) The capillary is heat-treated, and then the temperature is programmed, and then the template is removed, and then the first capillary is cleaned, dried and calcined in order to obtain a whole silica gel An open-tube capillary column; wherein, the sol solution includes polyethylene glycol, urea, methyl orthosilicate, and acetic acid solution. The preparation method can make the silica gel in the open-tube capillary column evenly and thickly distributed, and at the same time make the open-tube capillary column not easy to be blocked.

Description

technical field [0001] The invention relates to a capillary column, in particular to a silica gel integral open-tube capillary column using a metal wire as a template and a preparation method thereof. Background technique [0002] Chromatography is a physical separation method in which the mixed components are dispersed between two phases, a stationary phase (SP) encapsulated in a tube and a mobile phase (MP) passing in a certain direction within the tube. Miniaturized instrumentation and green chemistry are two very important topics in modern analytical science, both of which are influencing the future development of chromatography, reflected in the current need for portable instruments and reducing solvent consumption. Chromatographic analysis columns in the form of capillary columns of 5-500 μm inner diameter have attracted research interest in the field due to their reduced sample capacity requirements and greatly reduced solvent consumption. [0003] Capillary columns ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D15/22G01N30/60B01J20/283B01J20/28B01J20/30
CPCB01D15/22G01N30/6078B01J20/283B01J20/2805B01J20/3057B01J20/3078
Inventor 蒋晨陆波王亚娟朱昌青
Owner ANHUI NORMAL UNIV
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