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A method for preparing quartz needles by etching capillaries with hydrofluoric acid

A technology of capillary and hydrofluoric acid, which is applied to parts, instruments, and measuring devices of particle separator tubes, can solve problems such as difficulty in automation, poor service life, and low usage of hydrofluoric acid, and achieve stability that is not easy to clog Sexuality, long service life, and the effect of reducing the amount of use

Active Publication Date: 2019-01-04
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 cause the outer diameter to be difficult to control, 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.MassSpectrom .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 it is necessary to pass water and gas inside the capillary Or oil (R.D.Smithet.al.Anal.Chem.2006,78,7796-7801), and the etching situation must be observed in real time, it is difficult to realize automation
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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  • A method for preparing quartz needles by etching capillaries with hydrofluoric acid
  • A method for preparing quartz needles by etching capillaries with hydrofluoric acid
  • A method for preparing quartz needles by etching capillaries with 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 applications.

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 dipped 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. 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 microinjection needles is controllable (only 10.0±0.3 μm), and capillaries with different inner diameters are selected for preparation according to different needs.

[0035] The microinjec...

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Abstract

The invention relates to a novel method for preparing a quartz needle by etching a capillary with hydrofluoric acid. Specifically, the polymer coating on the capillary tube to be etched is removed, then the capillary tube is fixed in the designed device (Figure 1), and a certain volume of hydrofluoric acid is added to etch the capillary tube until the capillary tube is etched and broken. The volatilization of hydrofluoric acid and the affinity with the quartz surface make the etched part of the quartz capillary form a conical surface. The method can be widely used in the preparation of quartz materials such as mass spectrometry electrospray needles and genetic engineering microinjection needles that need to control the outer diameter and the cone surface.

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 Patents(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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