JPS59210358A - Analyzing device coupled with liquid chromatograph-atmospheric ionizing mass spectrometer - Google Patents

Abstract

PURPOSE:To enable measurement of a non-volatile sample, etc. which are previously difficult to measure by atomizing the outflow liquid from a liquid chromatograph and analyzing the same with an atm. ionizing mass spectrometer. CONSTITUTION:The outflow liquid from an LC column 1 is fed through a guide wire 10 onto an ultrasonic oscillating element 9, by which the liquid is atomized. The atomized liquid is fed together with the carrier gas from a carrier gas introducing port 2 into the ionizing part of a mass spectrometer. The carrier gas is heated to assist the disintegration of the fine particles contg. the atomized sample to the cluster attached with several molecules or down to the molecule itself and at the same time the ionizing part is also heated by a heater 5 according to need so that the condenstation of the solvent by the inside wall of the ionizing part is prevented. If the device is constituted in such a way, the material susceptible to thermal decomposition or the material which is hardly evaporatable by heating is fed together with the carrier gas into the ionizing part and is ionized. The easy analysis of such material is thus made possible.

Description

DETAILED DESCRIPTION OF THE INVENTION [Field of Application of the Invention] The present invention relates to an analysis device that combines a liquid chromatograph and an atmospheric pressure ionization quality analyzer.

[Background of the invention]

Atmospheric pressure ionization mass spectrometer (hereinafter abbreviated as APIMS) is a mass spectrometer that efficiently ionizes a sample under atmospheric pressure using corona discharge or beta rays emitted from Ni, and is capable of analyzing extremely trace components. Liquid chromatographs (hereinafter abbreviated as LC) are the only instruments capable of separating and detecting non-volatile substances or thermally unstable substances, and have become widely used.

However, there is currently no highly sensitive LC detector;
Since information regarding the molecular structure such as the mass of the sample cannot be obtained, attempts have been made to combine it with a mass spectrometer (A
nal, Chem, 51L, 682 A (19
79)),.

By the way, the atmospheric pressure ionization mass spectrometer (APIMS) is highly sensitive and ionization is performed under atmospheric pressure, so it is very convenient to combine with LC. Horning et al. (Anal.

Chem, 4 7, 2369 (1975),
J, Chromatogr, 99.

13 (1974)) proposed an analysis device that combined LC and APIMS. FIG. 1 shows the general configuration of this device. The LC effluent is introduced through the LC column 1 into a glass vaporizer tube 4 heated by a heater 5, where it is heated and vaporized. The vaporized solution is introduced from the carrier gas introducing vibe 2, sent to the ionization chamber together with the heated carrier gas, ionized by corona discharge by the corona discharge electrode 6, and taken out into the vacuum through the pores and analyzed. Note that 3 is glass wool, which has the function of removing large particles and making small particles smaller. 8 is a gas outlet.

This configuration has the disadvantage that since the solution is heated and vaporized, it is not possible to measure substances that are easily thermally decomposed or substances that do not vaporize even when heated.

[Purpose of the invention]

Accordingly, an object of the present invention is to provide an analysis device that combines a liquid chromatograph and an atmospheric pressure ionization mass spectrometer, which can easily handle even substances that are easily thermally decomposed or that are difficult to heat and vaporize.

[Summary of the invention]

To achieve the above object, the present invention is characterized in that the effluent from a liquid chromatograph is atomized by an ultrasonic atomizer and analyzed by an atmospheric pressure ionization mass spectrometer. Hereinafter, the present invention will be described in detail using the drawings.

[Embodiments of the invention]

FIG. 2 is an example of a configuration of a coupling section of an analysis device combining an LC and an APIMS according to the present invention. The effluent from the LC column 1 is continuously sent onto the ultrasonic oscillation element 9 along the LC solution guide wire 10.

The effluent from the LC column 1 is atomized on the surface of the ultrasonic oscillation element 9, and sent to the ionization section together with the carrier gas from the carrier gas inlet 2. Although the wire 10 and the ultrasonic oscillation element 9 are in contact with each other,
are in very close condition. The carrier gas is heated to help the fine particles containing the atomized sample become finer and become clusters with several molecules attached or even molecules themselves, and the ionization section is also heated by the heater 5 as necessary. This prevents the solvent from condensing on the inner wall of the ionization section. The sample is efficiently ionized in the ionization section and introduced into the analyzer, but excess solvent and carrier gas are discharged to the outside from the gas outlet 8. According to the present invention, since the sample is not vaporized by heating, there is an advantage that even heat-sensitive substances or non-volatile samples can be sent to the ionization section together with a carrier gas and analyzed as ions. In the present invention, the ionization section is also heated, but this is to prevent condensation of the solvent, and generally a sufficiently low temperature may be used as long as a solvent that is easily vaporized can be vaporized.

FIG. 3 shows a modification of the analyzer of the present invention, in which an ultrasonic oscillation element 9
' is attached to the end of the LC column 1, and has the feature of being able to perform even more effective atomization.

〔Effect of the invention〕

As described above, according to the present invention, in order to atomize a nonvolatile sample in solution form using ultrasonic waves and suspend it in the air,
Even non-volatile samples or samples that are unstable to heat, which have been difficult to measure up until now, can now be ionized at atmospheric pressure and their mass spectra measured.

[Brief explanation of drawings]

FIG. 1 is a schematic diagram of a conventional LC-A and PI bond analyzer, and FIGS. 2 and 3 are schematic diagrams of an LC-APIMS bond analyzer according to an embodiment of the present invention. DESCRIPTION OF SYMBOLS 1... LC column, 2... Carrier gas introduction pipe, 3... Glass wool, 4... Vaporizer glass tube, 5... Heater, 6... Corona discharge electrode, 7...
...Vacuum flange, 8...Gas outlet, 9...Ultrasonic oscillation element, Fig. γ 2 Fig. 3 Z

Claims (1)

[Claims] (1) A liquid chromatograph, an atomizer that converts the effluent from the liquid chromatograph into θ, and an atmospheric pressure ionization mass spectrometer that introduces and analyzes the mist from the atomizer. A combined chromatograph-atmospheric pressure ionization pawnshop analyzer analyzer, characterized in that it is equipped with: 2. The liquid chromatograph-atmospheric pressure ionization mass spectrometer coupled analysis device according to claim 1, wherein the atomization device is provided in the ionization section of the atmospheric pressure ionization mass spectrometer. 3. The atomizing device is characterized by comprising a solution guide wire for guiding the effluent from the liquid chromatograph and an ultrasonic oscillation element provided near the tip of the wire or in contact with the wire. A liquid chromatograph-atmospheric pressure ionization mass spectrometer coupled analysis device according to claim 2. 4. Claim 2, wherein the atomizing device comprises a column that guides the effluent from the liquid chromatograph from below, and an ultrasonic vibration element provided at the end of the column. Liquid chromatograph-atmospheric pressure ion mass spectrometer coupled analysis device.