JPH0550648U - Mass spectrometer - Google Patents

Abstract

(57) [Summary] [Purpose] Gas chromatograph mass spectrometry is also possible using the ion source for atmospheric pressure ionization intended for liquid chromatographs. [Structure] In FIG. 1, a mobile phase solvent such as water or methanol flowing out from 1 is heated by 4 and reaches 3 which is heated by 4. A temperature of 3 and a pressure of 1 atomizes and then 6
It is vaporized at 5 and heated up to 7 parts of the atmospheric pressure ion source. The mobile phase solvent is ionized by corona discharge generated by applying a high voltage to 7. The sample components flowing out from here were controlled to a constant temperature by 10 9
Will be introduced at 7 At this time, the ion molecule reaction is repeated while passing through the ionized mobile phase solvent molecules 11 and 12, and the sample molecule is ionized and introduced into the mass spectrometer.

Description

[Detailed description of the device]

[0001]

[Industrial application]

 The present invention is directed to the components eluted from the gas chromatograph between the needle electrode part of the ion source for atmospheric pressure ionization or the first and second pores, which is intended only for the outflow sample from the liquid chromatograph. The present invention relates to a mass spectrometer capable of performing both gas chromatograph mass spectrometry and gas chromatograph mass spectrometry by introducing a gas chromatograph mass spectrometer.

[0002]

[Prior Art]

 The conventional atmospheric pressure ionization ion source is designed to ionize the outflow components from the liquid chromatograph. That is, the sample and mobile phase solvent flowing out from the liquid chromatograph reach the atomizer through the sample introduction pipe and become atomized due to the atomizer temperature and the pressure of the liquid chromatograph. Then, it is vaporized in the desolvation chamber to become solute molecules and reaches the atmospheric pressure ion source. The mobile phase solvent molecules are ionized by the corona discharge generated by applying a high voltage to the needle electrode of this atmospheric pressure ion source, and then the sample molecules are ionized by repeated ion molecule reactions and reach the mass spectrometric analysis section. To be done. However, since the sample that flows out from the liquid chromatograph is targeted, the coupling with the gas chromatograph is not considered, and in order to analyze the sample that flows out from the gas chromatograph, the ions for electron impact from the ion source for atmospheric pressure ionization It had to be replaced with a source, and it wasted time and effort for the replacement.

[0003]

[Problems to be solved by the device]

 In the atmospheric pressure chemical ionization method, the components separated by the liquid chromatograph pass through the sample introduction pipe together with the mobile phase solvent, reach the atomizer, and are atomized by the atomizer temperature and the pressure of the liquid chromatograph. Then, it is vaporized in the desolvation chamber to become solute molecules and reaches the atmospheric pressure ion source. Corona discharge generated by applying a high voltage to the needle electrode of this atmospheric pressure ion source ionizes mobile phase solvent molecules such as water and methanol, and then ionizes sample molecules by repeated ion molecule reactions to perform mass spectrometry. Reach the department. In this process, no consideration was given to introducing a component that separates from the gas chromatograph, and the change from liquid chromatograph mass spectrometry to gas chromatograph mass spectrometry was to change the ion source from the atmospheric pressure ion source to electron impact. Requires a change to the ion source. This switching work requires a lot of time and effort.

In the present invention, a sample from a gas chromatogram is introduced between a portion where an ionic molecule reaction required for ionization as liquid chromatograph mass spectrometry is occurring, that is, a needle electrode portion and first pores to second pores. This is characterized by the chemical ionization of gas chromatograph samples by mobile phase solvent ions from the liquid chromatograph. In chemical ionization, it is known that the quasi-molecular ion peak can be observed with high sensitivity even in a sample in which the molecular ion peak cannot be detected by the electron impact method. In addition, since substances that can be separated by liquid chromatograph and substances that can be separated by gas chromatograph do not necessarily match, it is an object of the present invention to make it possible to easily use both separation means with one mass spectrometer.

[0005]

[Means for Solving the Problems]

 The above object can be achieved by providing a needle electrode portion of the ion source for atmospheric pressure ionization or an introduction hole for the sample eluted from the gas chromatogram between the first pore and the second pore. That is, the mobile phase solvent from the liquid chromatograph is ionized by the corona discharge caused by the high voltage applied to the needle electrode and becomes the chemical ionization ion, and ionizes the inflowing measurement sample. At this time, the sample flowing out from the gas chromatograph is heated and vaporized, so it is necessary to heat the path between the gas chromatograph and the ion source for atmospheric pressure ionization to maintain a constant temperature. In the conventional device, only the sample from the liquid chromatograph was targeted, and in order to ionize the sample from the gas chromatograph, the ion source was changed to the electron impact method, but in the present invention, the transfer from the liquid chromatograph is performed. This is achieved by introducing the sample from the gas chromatograph into the chemical ionization section filled with the phase solvent ions and ionizing it by the chemical ionization method.

[0006]

[Action]

 In the above mass spectrometer, a mobile phase solvent such as water or methanol is always flown from the liquid chromatograph and used for ionization of the sample. The mobile phase solvent reaches the atomizer through the sample introduction pipe. It is atomized by the pressure of the atomizer and liquid chromatograph, then vaporized in the desolvation chamber and reaches the atmospheric pressure ion source. In the atmospheric pressure ion source, the mobile phase solvent is ionized by the corona discharge generated by applying a high voltage to the needle electrode. Some substances whose molecular ion peaks cannot be confirmed by the electron impact method because they pass through the first and second pores and are introduced into the mass spectrometer while repeating the ion-molecule reaction with the sample introduced from the gas chromatograph. Since it is possible to detect the quasi-molecular ion peak, it is effective in determining the molecular weight.

[0007]

【Example】

 Two embodiments of the present invention will be described below with reference to FIGS.

In FIG. 1, a mobile phase solvent such as water or methanol flowing out from the liquid chromatograph 1 passes through a sample introduction pipe 2 and reaches a sprayer 3 heated by a sprayer temperature controller 4. Atomized by the temperature of the atomizer 3 and the pressure of the liquid chromatograph 1, and then vaporized in the desolvation chamber 5 heated by the desolvation chamber temperature controller 6 and reaches the needle electrode 7 of the atmospheric pressure ion source. The mobile phase solvent is ionized by corona discharge generated by applying a high voltage to the needle electrode 7. The sample components flowing out from the gas chromatograph 8 are introduced into the needle electrode section 7 through the gas guide pipe or the capillary column 9 whose temperature is controlled by the temperature controller 10. At this time, the ion molecule reaction is repeated while passing through the first pore 11 and the second pore 12 together with the mobile phase solvent molecules which have been previously ionized, and the sample molecules are ionized and introduced into the mass spectrometric section.

In FIG. 2, a mobile phase solvent such as water or methanol flowing out from the liquid chromatograph 1 reaches a sprayer 3 heated by a sprayer temperature controller 4 via a sample introduction pipe 2. Atomized by the temperature of the atomizer 3 and the pressure of the liquid chromatograph 1, and then vaporized in the desolvation chamber 5 heated by the desolvation chamber temperature controller 6 and reaches the needle electrode 7 of the atmospheric pressure ion source. The mobile phase solvent is ionized by the corona discharge generated by applying a high voltage to the needle electrode 7, and passes through the first pores 11. The sample components flowing out from the gas chromatograph 8 are introduced into the gas through a gas guide pipe or a capillary column 9 whose temperature is controlled by a temperature controller 10. At this time, the ion molecule reaction is repeated while passing through the second pores 12 together with the mobile phase solvent molecules that have been previously ionized, and the sample molecules are ionized and introduced into the mass analysis unit.

According to the present embodiment, it is possible to perform gas chromatograph mass spectrometry and liquid chromatograph mass spectrometry using an atmospheric pressure ion source without a complicated exchange work of the ion source.

[0011]

[Effect of the device]

 According to the above invention, one device can be effectively used without complicated switching operation between liquid chromatograph mass spectrometry and gas chromatograph mass spectrometry. In gas chromatograph mass spectrometry, ion molecular reaction (chemical ionization; CI), which is a softer ionization than the electron impact method, is used, and pseudo molecular ions can be detected with high sensitivity even in samples in which detection of the molecular ion peak is not possible. Since it can be detected, it is effective in determining the molecular weight.

[Brief description of drawings]

FIG. 1 is a block diagram of an ion source for atmospheric pressure ionization, which is one embodiment of the present invention.

FIG. 2 is a configuration diagram of an ion source for atmospheric pressure ionization, which is one embodiment of the present invention.

[Explanation of symbols]

1 ... Liquid chromatograph, 2 ... Sample introduction pipe, 3 ... Atomizer, 4 ... Atomizer temperature controller, 5 ... Desolvation chamber,
6 ... Desolvation chamber temperature controller, 7 ... Needle electrode, 8 ... Gas chromatograph, 9 ... Gas guide pipe or capillary column, 10 ... Temperature controller, 11 ... First pore, 12 ... Second pore.

 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Yoko Kato, Inventor Yoko Kato 832, Nagakubo, Horiguchi, Katsuta, Ibaraki Pref. 2nd, within Ritsumei Engineering Engineering Co., Ltd. (72) Naoto Senda, 832 Nagakubo, Horiguchi, Katsuta, Ibaraki Measurement Engineering Co., Ltd. (72) Inventor Toshiaki Takahashi 832, Nagakubo, Horiguchi, Katsuta-shi, Ibaraki 2 days Hijiri Measurement Engineering Co., Ltd. (72) Kazuhiko Toyama, 832, Nagakubo, Horiguchi, Katsuta-shi, Ibaraki 2 days Measurement Engineering Within the corporation

Claims (3)

[Scope of utility model registration request] 1. A mass spectrometer characterized in that a component flowing out from a gas chromatograph is introduced into a needle electrode portion of an ion source for atmospheric pressure ionization. 2. A mass spectrometer characterized in that a component eluted from a gas chromatograph is introduced between the first pore and the second pore of the atmospheric pressure ionization ion source. 3. A mass spectrometer according to claim 1, wherein the gas chromatograph and the path to the ion source for atmospheric pressure ionization are temperature-controlled.