JPH02309252A - Specimen introducing apparatus for gas chromatograph - Google Patents

Abstract

PURPOSE:To enhance the injection efficiency of a specimen and the reliability of an analytical result by receiving the specimen from a syringe in a specimen receiving container to prevent the falling thereof and forcibly discharging the specimen evaporated by the carrier gas flowing in the receiving container to a capillary column. CONSTITUTION:The lower end of a case member 1 receiving a specimen receiver 2 is connected to the specimen injection port 3 of a capillary gas chromatograph and an opening 11 is provided to the case member 1 and a needle insertion port 4 and a carrier gas supply port 5 are provided to the side surface of the case member 1. The specimen receiver 2 is composed of a cylindrical body and received in the case member so as to be movable through a rod 6 and a through-hole 7 is provided to said specimen receiver 2 so as to be opposed to the needle insertion port 4 when the specimen receiver 2 is drawn upwardly and to the carrier gas supply port 5 when said receiver 2 is pushed downwardly and a vent hole 8 is provided to the upper part of the specimen receiver 2 and an opening 9 is provided to the lower part thereof through a tapered throttled part 2a.

Description

Detailed Description of the Invention (Field of Industrial Application) The present invention relates to a gas chromatograph-mass spectrometer suitable for analyzing a sample separated by a gas chromatograph using a capillary column using a mass spectrometer.
Regarding the sample introduction device.

(Prior art) Although a gas chromatograph equipped with a capillary column has extremely high separation performance, the sample volume that can be injected is extremely small. A needle-shaped body C is housed in a tube body A that is open and whose other end is connected to a gas chromatograph sample introduction device so as to be movable in the vertical direction, and a microsyringe needle Et! is inserted into this needle-shaped body C from the side. A sample introduction device was used that had a syringe needle insertion opening that allowed tactile insertion. Note that the symbol F in the figure indicates a carrier gas injection port.

(Problem to be Solved by the Invention) According to this sample introduction device, a sample dissolved in a solvent is applied to the surface of the needle-like body C using the needle E, and the needle-like body C is moved downward and heated. , the solvent can be quickly volatilized and the amount introduced can be kept as small as possible.

However, how far apart is the tip of the needle E and the needle C? Since the coating work is done after aligning the layers, not only does it require skill, but if excess coating is applied, it becomes droplets and falls into the gas chromatograph unit, remaining even after the analysis is completed and preventing subsequent analysis. There is a problem that errors occur.

The present invention was made in view of these problems, and its purpose is to provide a new gas chroma that can reliably inject a minute amount of sample into an analyzer while maintaining the volatility of the solvent. An object of the present invention is to provide a sample introduction device N for a tograph.

(Means for Solving the Problems) In order to solve such problems, in the present invention, the lower end is connected to the sample injection port of the gas chromatograph device,
In addition, the case member is equipped with a solvent discharge port on the top, a syringe needle insertion port and a carrier gas supply port on the side, and a constriction portion with an opening on the bottom end, and a first and second case member on the side. A cylindrical sample container having a through hole is movably accommodated in the case member to a position where the lower through hole faces the syringe needle insertion port and a position where the through hole faces the carrier gas supply port. I decided to do so.

(Function) When the needle of the syringe is inserted and a predetermined amount of sample is injected, the sample is held in the sample container without falling due to the surface tension with the nozzle, and in this state, the volatile components are dissipated to the outside through the through hole. will be done. When the sample container is pulled down 1 after the solvent has evaporated, the sample is vaporized by the heat from the thermostatic chamber, and is forcibly discharged to the sample supply port of the analyzer by the carrier gas flowing into the sample container.

(Example) The details of the present invention will be described below based on illustrated examples.

FIG. 1 shows an embodiment of the present invention, in which reference numeral 1 denotes a case member which movably accommodates a sample container 2, the lower end of which is a carrier and a rally for a sample of a gas chromatograph. It is connected to the injection port 3, and has an opening 11 at the upper end that is open to the outside through a resistance tube, and roughly on the side is a needle insertion port 4 that allows the needle of a microsyringe to be inserted therein. A carrier gas supply port 5 is provided below.

On the other hand, the sample container 2 is made of a cylindrical body as shown in FIG. A through hole 7 is provided at a position opposite to the needle insertion port 4 when the device is lowered, and a through hole 7 is provided at a position opposite to the carrier gas supply port 5 when the device is lowered. An opening 9 is provided through a tapered constriction portion 2a18.

In this embodiment, with the sample container 2 pulled up above the case member 1 and carrier gas being supplied from the supply port 5, the needle Eu insertion port 4 of the syringe is used as a guide from the needle insertion port 4 of the case member 1. When inserted, the tip of the needle E enters the through hole 7 and comes into contact with the wall surface of the container 2. In this state, when the syringe is operated to extrude an appropriate amount of sample, the sample is discharged from the needle E into the constriction section 2a.

The discharged sample spreads on the inner surface of the constricted portion 2a due to surface tension.

Of course, since the diameter of the through hole 9 formed in the lower part is extremely small, the sample is held in the nozzle part by surface tension and does not fall into the main body of the apparatus.

When lightning is struck in this state, the carrier gas flowing in from the lower hole of the sample container volatilizes the solvent contained in the sample and is discharged from the upper hole 8 into the case 1, and then to the outside of the case. .

When the solvent has finished volatilizing in this way, if the container is moved below the case member 1 (Fig. 2), the constriction section 2a will receive heat from the column constant temperature bath G, so the constriction The sample adhering to the surface of section 2a is vaporized.

By the way, when the sample container 2 is pulled downward, the through hole 7 faces the carrier gas injection port 5, and the lower passage hole 3 of the sample container 2 faces the sample injection port 3. Therefore, the sample vaporized from the constricted portion 2a of the sample container 2 is forcibly injected into the column H under the pressure of the carrier gas.

As a result, the sample injected into the sample container is efficiently discharged to the analyzer, in this example, column H of the gas chromatograph, so it can be analyzed with extremely high constant MWi degree and reproducibility. .

(Effects of the Invention) As explained above, in the present invention, the lower end is connected to the sample injection port of the gas chromatograph device, the upper part is provided with the solvent outlet, and the syringe needle insertion port and the carrier gas supply port are provided on the side. A case member provided with an opening, a cylindrical sample container having a constriction portion having an opening at the lower end, and first and second through holes at the side portions; Since the sample from the syringe is accommodated in the case member so as to be movable to a position facing the syringe needle insertion port and a position facing the carrier gas supply port, the sample from the syringe is received within the sample container to prevent it from falling.
The sample vaporized by the carrier gas that has flowed into the container can be forcibly discharged into the capillary column, making it possible to improve the injection efficiency of the sample into the analyzer and the reliability of the analysis results.

[Brief explanation of the drawing]

Fig. 1.2 is a sectional view showing an embodiment of the present invention in use, and Figs. 4(a) and 4(b) are diagrams showing an example of conventional sample introduction snowmaking in a gas chromatograph equipped with a catolar column.1... Case member 2... Sample container 2a.
・・Aperture part 3 ・・Sample injection port for gas chromatograph 4 ・・Needle insertion port 5 ・・Carrier gas injection lower, 8 ・・
・Through hole 9...-Opening hole E-...Needle
H-... Column G... Constant temperature bath

Claims (1)

[Claims] A case member whose lower end is connected to a sample injection port of a gas chromatograph device, which is equipped with a solvent outlet at its upper part, a syringe needle insertion port and a carrier gas supply port at its side, and a constrictor having an opening at its lower end. , and a cylindrical sample container equipped with first and second through holes on the side,
A sample introduction device for a gas chromatograph, wherein the through hole located below is movably housed in the case member to a position facing the syringe needle insertion port and a position facing the carrier gas supply port.