JPS62191753A - Mass analyser - Google Patents

Abstract

PURPOSE:To prevent thermal cracking due to the excessive rising in temp. or an adsorption phenomenon due to the excessive lowering in temp., by applying program control to the rising in the temps. of an interface, a gaseous specimen introducing pipe and an ionizing chamber in matching relation to the rising in the temp. of a GC column thermostatic tank. CONSTITUTION:In an analytical apparatus consisting of a gas chromatograph and a mass analyser, the temps. of a GC interface 2, a gaseous specimen introducing pipe 4 and an ionizing chamber 5 is raised in synchronous relation to the rising in the temp. of a GC column thermostatic tank 1 by program control. By this method, the temp. raising program from the outlet of the column thermostatic tank 1 to the ionizing chamber 5 can be freely set and, therefore, a situation such that dehydration or demethylation is generated by heat before ionization and the molecular ion on a mass spectrum is not detected is eliminated. The high b.p. compound in a high mass region can be also detected and, because the specimen is not adsorbed, the detection of a minute amount can be performed.

Description

DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to a mass spectrometer, in particular an interface,
The present invention relates to a mass spectrometer suitable for synchronizing the temperature control of a sample gas introduction pipe and an ionization chamber with a GC column constant temperature bath to program a temperature increase for each part.

[Conventional technology]

In the conventional apparatus, as described in JP-A-53-49492, the temperature of the interface is controlled in conjunction with the temperature of the column constant temperature bath.

However, no consideration was given to the ability to control the temperature rise of the sample gas introduction pipe and ionization chamber via the interface.

[Problem that the invention seeks to solve]

In the above-mentioned prior art, the part of the carrier gas separator that removes the carrier gas of the gas sent from the GC to the MS and concentrates the sample gas was damaged at the interface. Even if the temperature increase control of this interface is linked to the GC column constant temperature bath, if it is not synchronized to the ionization chamber, the sample will undergo phenomena such as thermal decomposition, and molecular ions will not be detected on the mass spectrum and only fragments will be measured in the mass spectrum. There was a problem with doing this.

An object of the present invention is to program the temperature increase of the interface, sample gas introduction pipe, and ionization chamber in accordance with the temperature increase control of the GC column constant temperature bath.

[Means for resolving the gap]

The above purpose is to set each flow path (INOTERFACE, sample gas introduction pipe, ionization chamber) until the sample components separated and eluted by GC are ionized by MS to the optimum temperature conditions for the gas sample. [Operation] The interface, sample gas introduction pipe, and ionization chamber operate synchronously by temperature raising programming of the GC column thermostat. As a result, the temperature of each flow path can be controlled freely, so the temperature is raised according to the composition of the sample to be analyzed, and the sample gas components are introduced into the ionization chamber, resulting in stable ionization and accurate mass spectra. Can be measured.

〔Example〕

Hereinafter, one embodiment of the present invention will be explained with reference to FIG. G
The components separated and eluted by the column attached to the CO column constant temperature bath (1) are led to the sample gas introduction pipe (4) via the carrier gas separator (3) Th in the interface (2) section, and then to the ionization chamber (5). ) is ionized. The ionized ions are scanned by an electric field (6) and a magnetic field (7), and the signal entering the collector (8) is output through an amplifier (9).

According to this embodiment, when performing a series of measurements, in synchronization with the temperature program (10) of the GC column constant temperature bath (1),
Interface (2), sample gas introduction pipe (4),
The temperature of each part of the ionization chamber (5) is adjusted according to the heating program curve (1).
The temperature is increased at the rate shown in 1). Therefore, it is effective to prevent thermal decomposition due to excessively high temperature K and adsorption phenomenon due to excessively low temperature.

〔Effect of the invention〕

According to the present invention, a heating program can be set freely from the column outlet to the ionization chamber, so it is possible to prevent molecular ions from being detected in mass spectra due to thermal dehydration, demethylation, etc. before ionization. lost.

It is also possible to detect high boiling point compounds in the high mass range fn/Z of 100O or more, and since the sample is not adsorbed, trace amounts of 10"g can be measured using the multiple ion detector (MID) method. It is effective because it was able to reduce the amount of water used.

[Brief explanation of drawings]

FIG. 1 is a plan view of a temperature program using the GC-MS method and GC temperature increase control.

Claims (1)

[Claims] 1. GC consisting of a gas chromatograph and a mass spectrometer
A mass spectrometer characterized by increasing the temperature of the GC interface, sample gas introduction pipe, and ionization chamber in synchronization with the temperature increase of the GC column constant temperature bath in MS. 2. The mass spectrometer according to claim 1, characterized in that the temperature of the GC interface, sample gas introduction pipe, and ionization chamber can be programmed to be raised from a temperature different from that of the GC column thermostat.