JPH05157742A - Analyzing apparatus of gas chromatograph or the like - Google Patents

Abstract

PURPOSE:To improve sensitivity and to enable detection of a peak of high resolution by connecting a volatile component concentrating device with a thermal decomposition device removably by a connecting pipe. CONSTITUTION:A gas chromatograph mass analyzer 1 has a detector 3 with a capillary column 2 interposed. A sample is set on a sample stage 12 and charged in a heating chamber 13 of a thermal decomposition device 10 and it is heated to a desired necessary temperature through the intermediary of a temperature controller 14 so that a thermally decomposed component be produced. On the occasion, a solenoid operated valve 24 is opened beforehand. An inactive carrier gas is sent in from a carrier gas inlet passage 15 and thereby a product in the heating chamber 13 is discharged from an outlet passage 16 and sent into a connecting pipe 18 provided removably. In the connecting pipe 18, a volatile component made adsorbed on a collector is desorbed by heat or vaporized. The component volatilized or desorbed is sent into a trap tube 5 of a volatile component concentrating device 4 and cooled down by liquid nitrogen 9 to be trapped. By closing the valve 24 on the occasion, the temperature is raised rapidly and each component is introduced into a gas chromatograph and detected.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a gas chromatograph and a gas chromatograph mass spectrometer, and more particularly, it is equipped with a thermal decomposition device for pretreating a sample and a volatile component concentrating device.

[0002]

2. Description of the Related Art Conventionally, various methods have been proposed as a method for analyzing a gas chromatograph or a gas chromatograph mass spectrometer, in which various pretreatment devices are connected and a component which cannot be detected by conventional gas chromatograph analysis is detected. There is.

For example, there is a case in which a thermal decomposition device is connected to a gas chromatograph mass spectrometer and used as a method for structural analysis of a polymer. In addition, a trace amount volatile component concentrator is connected to a gas chromatograph mass spectrometer for use in volatile component analysis, headspace gas analysis, residual monomer analysis in polymers and the like.

In the conventional method of using a thermal decomposition apparatus, the thermal decomposition apparatus is directly connected to the injection part of an analyzer such as a gas chromatograph, the carrier gas is split, and the decomposition products are diffused in the dead space of the thermal decomposition chamber. The analysis was done to prevent this.

[0005]

The split method has a merit, but has a problem in detecting a trace amount of components because the analysis has a split ratio of about 50: 1. In addition, these pretreatment devices are built into the gas chromatograph body and cannot be easily replaced once assembled.
Also, it takes 1 to 2 days for stable treatment and use even if it is replaced over time.

Further, when the pretreatment device is replaced, there is a possibility that glass products such as sample tubes and trap tubes and other thin tubes may be damaged, or microanalysis may be hindered by contamination of the device.

[0007]

Therefore, in the present invention,
The thermal decomposition device and the volatile component concentrator are connected so that they can be mounted on the gas chromatograph or the gas chromatograph mass spectrometer, and further, the thermal decomposition device, the gas chromatograph mass spectrometer, the volatile component concentrator and the gas chromatograph mass spectrometer. It can be used by simply exchanging only the connecting part without exchanging each device, and it can be used in an extremely short time, and in the analysis of thermal decomposition components, the thermal decomposition components are cold traps and instantaneous vaporization. The volatile component concentrator connected to a gas chromatograph or the like and the thermal decomposition device are connected so that the band can be prevented from spreading and the amount of information from the obtained pyrogram can be abundant.

[0008]

Embodiment 1 is an analyzer showing a gas chromatograph or a gas chromatograph mass spectrometer, which is equipped with a detector 3 via a capillary column 2. Reference numeral 4 denotes a volatile component concentrator, which is composed of a SUS tube 6 having a trap tube 5 built therein, a pipe 7 for covering them, and liquid nitrogen 9 supplied by a communication pipe 8 communicating with the pipe 7.

Reference numeral 10 denotes a pyrolyzer, which allows a sample stage 12 provided with a platinum heater 11 to be inserted into a heating chamber 13, and the platinum heater 11 is connected to a temperature controller 14. The heating chamber 13 communicates with a carrier gas inlet 15 and a carrier gas outlet 16.

Between the end of the carrier gas outlet 16 and the pipe 7, a connecting pipe 18 constituted by a glass lining pipe or the like housed in the oven block 17 is detachably provided. The connecting pipe 18 is preferably a stainless pipe having a glass lining because it is less likely to adsorb a sample and there is no risk of breakage due to repeated attachment and detachment.

To connect the connecting tube 18 to the trap tube 5 and the carrier gas outlet 16, the packing 19 inserted into the connecting tube 18 is screwed from above and below with a union 20 and a nut 21, and further from above, a graphite Vespel ferrule 22. And the nut 23 is screwed.

Next, the use and operation thereof will be described. The sample is placed on the sample table 12 and loaded into the heating chamber 13, and the temperature is adjusted via the temperature controller 14 to heat the sample to a desired temperature, Generate decomposition components. At this time, the solenoid valve 24 is opened.

An inert carrier gas is fed through the carrier gas inlet passage 15, the product in the heating chamber 13 is discharged through the carrier gas outlet passage 16 and fed into the connecting pipe 18 . In the connecting pipe 18 , the volatile components adsorbed by the scavenger are heated to be desorbed or vaporized. However, by adsorbing the selective adsorbent to analyze the specific element compound and filling the catalyst with water, It can be used for addition chromatography, derivatization chromatography of polar compounds and the like.

The thus volatilized components or desorbed components are sent to the trap tube 5, cooled by the liquid nitrogen 9 to the liquid nitrogen temperature (-130 ° C.) and trapped. At that time, the solenoid valve 24 is closed. Then, the temperature is rapidly raised and introduced into a gas chromatograph to detect each component.

[0015]

According to the present invention as described above, since the volatile component concentrating device connected to the gas chromatograph and the thermal decomposition device are connected, it has the functions of only thermal decomposition analysis and only volatile component analysis, In the component analysis, the pyrolyzed components can be cold-lapped and instantly vaporized, and the sensitivity can be increased by concentrating, and the obtained pyrogram is, for example, as shown in FIGS. In the pyrogram, and as shown in FIGS. 5 and 6, as shown in the polystyrene pyrograms, the spread of the bunt is eliminated, and the pyrogram obtained by a simple pyrolysis and gas chromatograph coupling device has a high resolution. The peak could be detected and the amount of information became rich.

Further, it is not necessary to replace a pyrolysis device and a concentrating device in one gas chromatograph, and the number of adjustment days is not required, and the glass tube and the like are not damaged and the practical effect is remarkable.

[Brief description of drawings]

FIG. 1 is a schematic explanatory view of an embodiment of the present invention.

FIG. 2 is a partially enlarged explanatory view of the same.

FIG. 3 is a conventional polymethylmethacrylate pyrogram.

FIG. 4 is a polymethylmethacrylate pyrogram according to this example.

FIG. 5 is a polystyrene pyrogram according to a conventional example.

FIG. 6 is a polystyrene pyrogram according to this example.

[Explanation of reference numerals] 1 gas chromatograph or gas chromatograph mass spectrometer 3 detector. 4 Volatile component concentrator. 8 communication tubes. 10 Pyrolysis device. 13 heating chamber. 14 Temperature controller. 18 Connection pipe.

 ─────────────────────────────────────────────────── ─── Continuation of front page (72) Torurou Tsuneto, 1-8 Kasumi, Yokkaichi-shi, Mie Tosoh Co., Ltd. Petrochemical Research Laboratory (72) Inventor, Kimitoshi Nagata 745, 2-5, Sakuradai, Yokkaichi-shi, Mie

Claims (2)

[Claims] 1. An analyzer for a gas chromatograph or the like, wherein a volatile component concentrator connected to the gas chromatograph or the like is connected to a thermal decomposition device. 2. An analyzer such as a gas chromatograph according to claim 1, wherein the volatile component concentrating device and the thermal decomposition device are detachably connected by a sample pipe.