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Ionization method for analyzing sample, and dedicated ionization source

An ionization source and ionization technology are applied in the direction of material analysis using wave/particle radiation, analyzing materials, and parts of particle separator tubes. It can solve the problem that ionization equipment is not the most convenient, reduces the service life of electrodes, and is not Miniaturization of instruments and other issues to achieve the effect of reducing the discharge range, avoiding pollution, and simple design

Inactive Publication Date: 2010-03-10
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the above two new ion sources still have certain shortcomings: for example, in the ionization process of DESI, high voltage and ionization solvent are required, which will pollute the environment to a certain extent, and the high flow rate of gas is not conducive to Reduce the detection cost; although DART saves the solvent, it still needs high voltage and high flow ionization gas, and also needs a gas heating device, so the ionization equipment is not the most convenient, and it is not suitable to realize the miniaturization of the instrument. still needs further research
For example, many reports have used glow discharge (glow discharge, GD) for ionization ([1] Newman, K.; Mason, R.S. Gas Chromatography Combined with Fast Flow Discharge Mass Spectrometry (GC-FFGD-MS). J .Anal.At.Spectrom.2004,19,1134-1140.[2] Belkin, M.A.; Olson, L.K.; Caruso, J.A.Radiofrequency Glow Discharge as an Ion Source for GasChromatography with Mass Spectrometric Detection.J.Anal.At.Spectrom .1997, 12, 1255-1261.]), the method is simple and convenient, and the operating cost is low, but it requires a certain degree of vacuum, so vacuum equipment is necessary, which leads to the complexity of the instrument design and increases the operating cost. cost; and, the electrode of glow discharge should be in direct contact with the sample, which will pollute the electrode and reduce the service life of the electrode

Method used

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  • Ionization method for analyzing sample, and dedicated ionization source
  • Ionization method for analyzing sample, and dedicated ionization source
  • Ionization method for analyzing sample, and dedicated ionization source

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Such as figure 1 As shown, the ionization source 1 is composed of a hollow needle electrode 11 (inner diameter 0.1-0.5mm, about 50mm in length) and a copper plate 12 to form a counter electrode. The carrier gas 3 passes through the hollow needle electrode 11 at a flow rate of 20-200mL / min. The flow rate of gas 3 is measured by a gas flow meter, and the size can be adjusted by a needle valve. A flat insulating medium layer 13 (1-5 mm thick) is placed between the two counter electrodes, and for the convenience of operation, the insulating medium can be slightly in contact with the copper plate electrodes. Different samples are respectively arranged on the flat insulating medium, and the diameter of the sample point can be as small as the diameter of the needle tip; the distance between the hollow needle electrode 11 and the flat insulating medium layer 13 is about 5-15 mm. The power supply device is a 5-30W AC power supply, and the size of the device is small (6cm×4cm×3c...

Embodiment 2

[0036] Ordinary glass (thickness 2mm) was selected as the insulating medium, and the glass was corroded with hydrofluoric acid before the experiment to obtain a rough surface. Take 3 μL of the mixed solution of four amino acids (L-valine, L-proline, L-serine and L-alanine) and spot on the insulating medium. Align the hollow needle electrode with this area, and the needle electrode is fed with helium at a flow rate of 50mL / min, and the discharge power is 30W, which are respectively connected to the two electrodes. When the power is turned on, discharge ionization starts. The ionization device is 40mm away from the sampling port of the mass spectrometer, so that the sample ions can be analyzed. Such as figure 2 , for the analysis of four amino acid mixed samples of L-valine (Mr=117), L-proline (Mr=115), L-serine (Mr=105) and L-alanine (Mr=89) mass spectrum. In the figure, the protonated molecular ion peaks of each amino acid can be clearly distinguished, indicating that the...

Embodiment 3

[0038] Taking amino acids as an example again, ionize L-glutamic acid (Mr 147) and L-serine (Mr 105). Ordinary glass (thickness 2mm) was selected as the insulating medium, and the glass was corroded with hydrofluoric acid before the experiment to obtain a rough surface. Taking amino acid as an example, take 3 μL of the sample solution and spot it on the insulating medium. Aim the hollow needle electrode at this area, and pass through the needle electrode with helium gas at a flow rate of 50mL / min; the power of the discharge power supply is 30W, connected to the two electrodes respectively, and the discharge ionization starts when the power is turned on. The ionization device is 40mm away from the sampling port of the mass spectrometer, so that the sample ions can be analyzed. Such as image 3 A, are the mass spectra of L-glutamic acid at different times; image 3 B, are the total ion chromatograms of different ions of L-serine and the ion chromatograms of fragment ions resp...

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Abstract

A special ionization source is prepared for connecting hollow needle electrode to planar electrode by power supply unit, setting planar insulation media layer between hollow needle electrode and planar electrode and hanging hollow needle electrode above planar insulation media layer in angle of 60-90 degree.

Description

technical field [0001] The invention relates to an ionization method for analyzing samples and a special ionization source thereof. Background technique [0002] Mass spectrometry is one of the most sensitive analytical methods and has a wide range of applications. The ionization source is an important part of the mass spectrometer. At present, there are several ion sources, such as electron bombardment ion source (EI), chemical ionization source (CI), field ionization / field desorption ionization source (FI / FD), Fast atom bombardment source (FAB), electrospray ionization source (ESI), laser desorption source (LD), atmospheric pressure chemical ionization source (APCI), etc. are suitable for the ionization of a wide variety of organic compounds with different properties. However, no matter which of the above ion sources is used, most of the samples cannot save the cumbersome pretreatment process, and it is more difficult to be used for continuous, real-time monitoring, high-...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N23/225H01J49/02
Inventor 张新荣那娜张四纯
Owner TSINGHUA UNIV
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