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Silica gel integral open tubular capillary column taking metal wire as template and preparation method thereof

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

Active Publication Date: 2020-09-04
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 tubular capillary column taking metal wire as template and preparation method thereof
  • Silica gel integral open tubular capillary column taking metal wire as template and preparation method thereof
  • Silica gel integral open tubular capillary column taking metal wire as template and preparation method thereof

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preparation example Construction

[0037] The invention provides a method for preparing a silica gel integral open-tube capillary column with a metal wire as a template. The preparation method comprises:

[0038] 1) introducing a 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 performing a temperature-programmed treatment, then removing the template, and then sequentially cleaning, drying and calcining the first capillary to obtain a silica gel integral open-tube capillary column;

[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, mechanical strength and porosity of the stationary phase of the integral open-tube capillary colum...

preparation example 1

[0068] Such as Figure 12 As shown in a-d of a, place the spotting capillary tubes of various specifications vertically, put a 20 μL pipette tip on the lower end, burn in the middle of the spotting capillary tube, and the glass is heated and softened and pulled down naturally. The inner diameter of the burnt spotting capillary gradually decreases, and the place where the metal filament 4 cannot penetrate is cut off with a capillary cutter to form second capillaries of various specifications.

Embodiment 1

[0070] 1) Dissolve 0.124g PEG-10000 and 0.09g urea in 1mL acetic acid solution (pH 3.4), stir for ten minutes in an ice-water bath, then add 400μL of methyl orthosilicate TMOS, stir for 40min in an ice-water bath, keep Ice-water bath, ice bath, 50KHz ultrasonic conditions vibration 10min degassing.

[0071] Sonicate the metal wire in high-purity water and ethanol for 8-10 minutes, and then dry.

[0072] Wash the capillary of the chromatographic column through 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 hours.

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

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

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Abstract

The invention discloses a silica gel integral open tubular capillary column taking a metal wire as a template and a preparation method thereof. The preparation method comprises the steps: 1), introducing a metal wire into a first capillary to serve as the template, then filling the capillary with a sol solution, and then capping the two ends of the first capillary; (2) carrying out heat treatmenton the capillary tube, then carrying out temperature programming treatment, then removing the template, and then sequentially cleaning, drying and calcining the first capillary tube to prepare the silica gel integral open tubular capillary column; wherein the sol solution comprises polyethylene glycol, urea, tetramethyl orthosilicate and an acetic acid solution. According to the preparation method, silica gel in the open tubular capillary column can be uniformly distributed and is relatively thick, and meanwhile, the open tubular capillary column is not easy to block.

Description

technical field [0001] The invention relates to a capillary column, in particular to a silica gel integral open-tube capillary column with 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, one is the stationary phase (SP) encapsulated in a tube, and the other is the mobile phase (MP) passing through the tube in a certain direction. Miniaturized instrumentation and green chemistry are two very important topics in modern analytical science, both of which influence the future development of chromatography, reflected in the current demand for portable instruments and reduced solvent consumption. Chromatographic columns in the form of capillary columns with an internal diameter of 5-500 μm have attracted research interest in this field due to their reduced sample volume requirements and greatly reduced solvent consumption. [000...

Claims

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Application Information

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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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