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Method for preparing quartz needle by etching capillary tube by hydrofluoric acid

A technology of capillary and hydrofluoric acid, which is applied in the parts of particle separator tubes, sample introduction/extraction, instruments, etc., can solve the problems of difficulty in automation, low usage of hydrofluoric acid, and poor service life. It is not easy to achieve Effects of clogging stability, reduced usage, and long service life

Active Publication Date: 2017-03-08
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The tip of the needle prepared by laser ablation is closed and needs to be cut before it can be used, which will make it difficult to control the outer diameter, and as the tip of the electrospray needle, it is easy to block, has a short life, and poor reproducibility (Oleschuk, R.D.et.al.Rapid Commun.Mass Spectrom.2005,19,2671-2680; Oleschuk, R.D.et.al.Anal.Chem.2004,76,6456-6460) The method for preparing quartz needles by traditional hydrofluoric acid etching is cumbersome, and needs to pass water inside the capillary, Gas or oil (R.D.Smith et.al.Anal.Chem.2006,78,7796-7801), and the etching must be observed in real time, it is difficult to automate
Therefore, we designed a device based on the hydrofluoric acid etching method to realize the preparation of quartz needles, with good reproducibility, less hydrofluoric acid usage, and poor service life. It is expected to realize automatic preparation

Method used

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  • Method for preparing quartz needle by etching capillary tube by hydrofluoric acid
  • Method for preparing quartz needle by etching capillary tube by hydrofluoric acid
  • Method for preparing quartz needle by etching capillary tube by hydrofluoric acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Preparation of quartz needles with different inner diameters:

[0028] Take 2 capillaries with a length of 10 cm and an inner diameter of 3 μm, 10 μm, 15 μm, and 20 μm respectively. After scraping off the polyamide coating with a blade, fix them in the designed device respectively, such as figure 1 As shown (the porous plate is fixed on the iron stand, the capillary is fixed in the hole of the porous plate, the lower end of the capillary passes through the hole at the bottom center of the hydrofluoric acid storage tube, the hole wall is closely attached to the outer wall of the capillary, and the capillary passes through the hole The silica gel plug, the wall of the silica gel plug hole is closely attached to the outer wall of the capillary, and the silica gel plug is used to fix the capillary outside the bottom of the hydrofluoric acid storage tube); add 20 μL of 40% hydrofluoric acid, etch at room temperature until the capillary breaks, and the prepared Quartz needles...

Embodiment 2

[0030] Application of quartz needles in liquid chromatography-mass spectrometry:

[0031] Select the quartz needle of 10 μm inner diameter that embodiment 1 makes as electrospray needle, investigate its spray stability and life: flow rate: 100nL / min; Mobile phase: the aqueous solution of 2% acetonitrile, 0.1% formic acid; Spray voltage: 1.9 kV. Depend on Figure 4 It can be seen that the spray stability is very good, and after 60 hours of continuous spraying, it still has good stability, which fully proves the potential value of the quartz needle in electrospray application.

Embodiment 3

[0033] Preparation of microinjection needles:

[0034] Take a 10cm 3μm capillary tube, use an alcohol lamp to carbonize the polyamide coating, then wipe off the carbonized polyamide layer with absorbent cotton soaked in alcohol, and fix it in the designed device (the porous plate is fixed on the iron stand, and the hole in the porous plate The capillary is internally fixed, and the lower end of the capillary passes through the hole in the center of the bottom of the hydrofluoric acid storage tube. The hole wall is closely attached to the outer wall of the capillary. A silicone stopper secures the capillary outside the bottom of the hydrofluoric acid reservoir), such as figure 1 As shown; add 20 μL of 40% hydrofluoric acid, etch at room temperature until the capillary breaks, and the prepared quartz needle is as follows: image 3 shown. The outer diameter of the microinjection needle is controllable (only 10.0±0.3 μm), and capillaries with different inner diameters are select...

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Abstract

The invention relates to a method for preparing a quartz needle by etching a capillary tube by hydrofluoric acid. The method specifically comprises the steps of removing polymer coating from a to-be-etched position of the capillary tube; then fixing the capillary tube on a designed apparatus (figure 1); and adding a certain volume of hydrofluoric acid to etch the capillary tube until the capillary tube is broken due to etching. A conical surface is formed in the etched position of the quartz capillary tube due to a volatilization effect of the hydrofluoric acid and an affinity interaction with the surface of quartz. The method can be widely applied to preparation of quartz materials, the outer diameters and conical surfaces of which need to be controlled, used in the fields of a mass spectrum electronic injection needle, a genetic engineering micro-injection needle and the like.

Description

technical field [0001] The invention relates to a method for preparing a quartz needle by etching a capillary tube with hydrofluoric acid, specifically a designed fixing device, which adopts a hydrofluoric acid etching method to form a tapered surface. The method can be widely used in the preparation of electrospray needles, microinjection needles and other quartz materials that need to control the outer diameter and cone surface. Background technique [0002] With the development of mass spectrometry technology, electrophoresis-mass spectrometry, liquid phase-mass spectrometry, etc. are widely used as high-efficiency separation and high-sensitivity detection systems in proteomics, lipidomics, glycomics, and metabolomics (Simpson, D.C. ; Smith, R.D. Electrophoresis 2005, 26, 1291-1305; Smith, R.D.; Shen, Y.; Tang, K. Acc. Chem. Res. 2004, 37, 269–278). The electrospray needle is used as the interface between CE or LC and mass spectrometry, and its spray effect directly affe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01J49/04H01J49/26G01N27/62
Inventor 张丽华朱旭东蒋好梁玉杨开广梁振张玉奎
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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