JPS63177057A - Liquid specimen introducing apparatus - Google Patents

Abstract

PURPOSE:To extend the life of a specimen introducing port and to prevent the generation of the chips of a septum, by a method wherein a specimen introducing fine tube is allowed to pierce through the seal material of the specimen introducing port and the opening thereof is moved from the outside of the specimen introducing port to the inside thereof to introduce a specimen. CONSTITUTION:A specimen evaporation chamber 12 is provided so as to be adjacent to a specimen introducing port 2, and the gap between said chamber 12 and the introducing port 2 and that between said chamber 12 and the open air are respectively sealed by seal materials 14, 16 and an outlet 19 is provided to the chamber 12. Both ends of a cylindrical specimen sampling part 24 are sealed by seal materials 26, 28 and said sampling part 24 is placed on the upper part of a specimen bottle 40. A specimen introducing tube 18 is inserted in the evaporation chamber 12 in a movable manner in such a state that one end thereof pierces the holes of the seal materials 4, 16 of the evaporation chamber 12 and the leading end thereof is sealed to be present in the specimen introducing port 2 and an opening 20 is provided to the fine tube 18 at a proper position from the leading end thereof and the other end of the fine tube 18 pierces the seal materials 26, 28 of the specimen sampling part 24. A purge gas introducing fine tube 30 is provided so that the leading end thereof pierces the seal materials 26, 28 of the specimen sampling part 24. Then, purge gas is supplied into the sampling part 24 from the purge gas introducing fine tube 30 to wash the specimen introducing fine tube 18 and thereafter, the opening 20 of the specimen introducing fine tube 18 is moved from the outside of the specimen introducing port 12 to the inside thereof to introduce a specimen.

Description

DETAILED DESCRIPTION OF THE INVENTION (Field of Industrial Application) The present invention relates to a device for automatically introducing a liquid sample into an analytical instrument such as a gas chromatograph.

(Prior Art) FIG. 7 shows a method for automatically introducing a liquid sample into a gas chromatograph.

2 is a sample introduction port, the upper end of which is a rubber septum 4.
is sealed by. The sample inlet 2 is provided with a glass insert 6 leading to the column, and the carrier gas is flowed from the sample inlet through the glass insert to the column.

The liquid sample is drawn into the syringe 8 and the needle 10 of the syringe 8
is inserted through the septum 4 and into the glass insert 6, the plunger of the syringe 8 is pressed to inject the liquid sample.

(Problems to be Solved by the Invention) In the conventional liquid sample introduction device, the needle 10 of the syringe 8 pierces the septum 4 every time a sample is introduced into the sample introduction port 2, so the life of the septum 4 is shortened. , the septum 4 will have to be replaced frequently. The sample inlet 2 is often heated, and when replacing the septum 4, carrier gas is not supplied to the column, so it is necessary to lower the oven temperature of the gas chromatograph, so replacing the septum 4 is troublesome. This results in interruption of the analysis.

In addition, septum chips generated when the needle IO penetrates the septum 4 accumulate in the glass insert 6,
This causes tailing in gas chromatograms.

The present invention extends the life of the septum in the sample introduction port.

Another purpose is to prevent the generation of septum chips.

(Means for Solving Problems) In the present invention, instead of introducing the sample with a syringe, the sample introduction capillary is passed through the sealing material of the sample introduction port, and the opening of the sample introduction capillary is inserted into the sample introduction port. The sample is introduced by moving from the outside to the inside.

That is, the liquid sample introduction device of the present invention will be described with reference to FIG. 1 showing an embodiment.
) is provided adjacent to the sample inlet (2), and the first
A second sealing material (16) facing the first sealing material (14) is connected to the outside air.
) and has an outlet (19).
12), a cylindrical sample collection part (24) whose both ends are sealed with sealants (26, 28) and placed on the top of the sample bottle (40), and one end of which is the sample vaporization chamber (12). movably inserted through a hole in the material (14, 16);
The tip of one end is sealed and placed in the sample introduction port (2), has an opening (20) at an appropriate position from the tip, and the other end is sealed with both sealing materials (26, 28) of the sample collection part (24). A sample introduction thin tube (18) that can penetrate the
4), a purge gas introduction thin tube (30) that can penetrate both the sealing materials (26, 28), a solenoid valve (46) located upstream of the purge gas introduction thin tube (30) to supply and stop the purge gas, and a sample The position of the opening at one end of the introduction capillary (18) moves between the inside of the sample vaporization chamber (12) and the sample introduction port (2), and the position of the opening (36) at the other end of the sample introduction capillary (18) moves. The sample introduction capillary (1) moves between the sample collection section (24) and the sample liquid (42) in the sample bottle (40).
8), and the position of the opening (38) at the tip of the purge gas introduction capillary (30) is moved between the inside of the sample collection section (24) and the space above the sample (42) in the sample bottle (40). The purge gas introducing thin tube (30) is provided with a drive mechanism that moves the purge gas introduction thin tube (30), and a controller that controls the solenoid valve (46) and the drive mechanism in synchronization.

(Example) FIG. 1 is a schematic diagram showing an example in a state at the time of sample introduction.

A sample vaporization chamber 12 is provided adjacent to the sample introduction port 2 . The sample vaporization chamber 12 has a cylindrical shape, and the boundary with the sample introduction port 2 is sealed with a rubber septum I4, which is a first sealing material, and the upper end of the sample vaporization chamber 12 is sealed with a rubber septum I4, which is a second sealing material. It is sealed by a septum 16. The septum 14 and the septum 16 have holes through which the sample introduction tube 18 passes, and one end of the sample introduction tube 18 is inserted through both septa 14 and 16.

As shown in an enlarged view in FIG. 2, one end of the sample introduction capillary 18 is sealed at its tip, and an opening 20 is provided at an appropriate distance from the tip. The sample introduction capillary 18 can slide through the hole in the septum 14.16;
The position of the opening 20 is moved between being within the glass insert 6, as shown in FIG. 2, and within the sample vaporization chamber 12, as shown in FIG.

A purge gas outlet 19 is provided in the sample vaporization chamber 12 .

The sample introduction port 2 and the sample vaporization chamber 12 can be connected by screws, and a septum 14 is sandwiched and fixed between them. Further, the septum 16 is fixed at the upper end of the sample vaporization chamber 12 by a septum cap 22.

Returning to FIG. 1, reference numeral 24 is a cylindrical sample collection section, the openings at the upper and lower ends of which are sealed with a rubber septum 26, 28, which is a sealing material. Two holes are formed in each of the septa 26 and 28, and the other end of the sample introduction capillary tube 18 is inserted through one hole, and the purge gas introduction capillary tube 30 is inserted through the other hole. It has been inserted.

The sample collection section 24 is shown enlarged in FIG.
Septum 26.28 is a septum cap 32.
It is fixed by 34. At the tip of the other end of the sample introduction capillary 18, the tip is sealed and sharpened, and an opening 36 is provided at an appropriate distance from the tip. The same applies to the purge gas introduction thin tube 30, the tip of which is sealed and sharpened, and an opening 38 is provided at an appropriate distance from the tip. Sample introduction tube 1
8 and purge gas introduction thin tube 30 are both septum 26.2
It can slide through 8 holes.

Returning to FIG. 1, reference numeral 40 is a sample bottle in which a liquid sample 42 is accommodated. The opening of the sample bottle 40 is sealed with a rubber septum 44. A space exists above the liquid sample 42 within the sample bottle 40 .

On the upstream side of the purge gas introduction thin tube 30, there is a solenoid valve 46 for supplying purge gas or stopping the supply of purge gas.
is provided.

Although not shown in FIG. 1, a drive mechanism for vertically moving the sample introduction capillary 18 and the purge gas introduction capillary 30 is provided, and the operation of the drive mechanism and the solenoid valve 46 are
A controller is also provided to synchronize and control the opening and closing operations of the opening and closing operations.

The sample introduction capillary 18 and the purge gas introduction capillary 30 are made of stainless steel.

Next, the operation of this embodiment will be explained.

The standby state is shown in FIG. 5.Both the sample introduction capillary 18 and the purge gas introduction capillary 30 are pulled up by the drive mechanism, and the opening 20 at one end of the sample introduction capillary 18 is connected to the vaporization chamber 12.
The opening 36 at the other end is located inside the sampling section 24 , and the opening 38 at the tip of the purge gas introduction thin tube 30 is also located inside the sampling section 24 .

The electromagnetic valve 46 is open, and the purge gas is discharged from the purge gas introduction capillary 30, through the sample collection section 24, through the sample introduction capillary 18, and from the vaporization chamber 12 through the purge gas outlet 19 to the outside. As a result, the inside of the sample introduction capillary 18 is cleaned.

When introducing a sample, the tip of the sample introduction thin tube 18 on the vaporization chamber 12 side is first lowered, and the opening 20 is positioned within the glass insert 6 of the sample introduction port 2 as shown in FIG. 46 is closed, the other end of the sample introduction capillary 18 is lowered so that the opening 36 is immersed in the sample 42, and the purge gas introduction capillary 30 is also lowered so that the opening 38 at the tip is in the upper space of the sample 42 in the sample bottle 40. is positioned. Subsequently, the solenoid valve 46 is opened, and the sample 42 is introduced into the sample introduction capillary 18.
It is injected into the glass insert 6 through the process.

The movement of the sample introduction capillary 18 and the purge gas introduction capillary 30 and the opening and closing of the electromagnetic valve 46 are controlled by a controller.

After a certain period of time has elapsed, the tip of the sample bottle side of the sample introduction capillary 18 and the tip of the purge gas introduction capillary 30 are pulled up so that their respective openings 36 and 38 are in the sample collection section 24 as shown in FIG. is positioned. Thereafter, the first magnetic valve 46 is closed after a certain period of time has elapsed. This completes the introduction of the sample.

Next, the tip of the sample introduction thin tube 18 on the vaporization chamber side is pulled up so that the opening 20 is opened into the vaporization chamber 12 as shown in FIG.
The solenoid valve 46 is opened again to remove the sample remaining in the sample introduction capillary 18.

With the above operations, one cycle of the sample introduction operation is completed, and the next sample bottle is positioned at the sample collection position by the sample bottle feeding mechanism (path shown), and the above operations are repeated.

The sealing material on the sample bottle side in the sample collecting section 24 is not limited to the septum 26 shown in FIG. 4, but may also be an O-ring 48, 50 as shown in FIG. 6, for example.

In addition, the sealing material on the sample bottle side of the sample collection section 24 is not necessarily provided with a hole as in the embodiment, and the sample introduction thin tube 18
The purge gas introduction thin tube 30 is not limited to the structure in which a needle is inserted into the sealing material 26 on the sample bottle side each time a sample is introduced.
This is because the sealing material is easy to replace.

(Effects of the Invention) In the liquid sample introduction device of the present invention, instead of drilling a hole in the sealing material of the sample introduction port of the analytical instrument each time a sample is introduced,
Since a hole is pre-drilled and the sample introduction tube slides through the hole, the sealing material at the sample introduction port is less likely to be damaged even if the sample is introduced repeatedly, and chips of the sealing material can be removed from the glass. There is no accumulation on the insert. the result,
The life of the sealing material at the sample introduction port is extended, and the cause of tailing in the chromatogram can be reduced.

[Brief explanation of the drawing]

FIG. 1 is a schematic diagram showing one embodiment in a sample introduction state, and FIG. 2 is an enlarged sectional view showing the vaporization chamber portion of the same embodiment in a sample introduction state.
FIG. 3 is an enlarged cross-sectional view showing the vaporization chamber part in a standby state, FIG. 4 is an enlarged cross-sectional view showing the sample collection section of the same embodiment, and FIG. FIG. 6 is a sectional view showing the vicinity of the sample-side sealing material of the sample collection section of another embodiment, and FIG. 7 is a schematic diagram showing the vicinity of the sample introduction port of a conventional sample introduction device. 2... Sample introduction port, 12... Vaporization chamber, 14.16, 26, 28... Septum, 18.
...Sample introduction thin tube, 19...Purge gas outlet, 20.36, 38...Opening. 24... Sample collection section, 30... Purge gas introduction capillary, 46...
·solenoid valve.

Claims (1)

[Claims] (1) Provided adjacent to a sample introduction port of an analytical instrument, and sealed with the sample introduction port by a first sealing material;
a sample vaporization chamber sealed with the outside air by a second sealant facing the first sealant and having an outlet; and a cylindrical chamber with both ends sealed by the sealant and placed on the top of the sample bottle. The sample collecting part of the sample sampling part and one end of the sample vaporizing chamber are movably inserted through the holes of both sealing materials, and the tip of this one end is sealed and placed in the sample introduction port, and the sample is inserted into an appropriate position from the tip. a sample introduction capillary having an opening and having the other end capable of penetrating both sealing materials of the sample collection section; a purge gas introduction capillary having a tip end capable of penetrating both sealing materials of the sample collection section; and an upstream side of the purge gas introduction capillary. A solenoid valve located on the side for supplying and stopping purge gas and an opening at one end of the sample introduction capillary move between the sample vaporization chamber and the sample introduction port, and an opening at the other end of the sample introduction capillary moves between the sample vaporization chamber and the sample introduction port. The sample introduction capillary tube is moved so that the opening position moves between the inside of the sample collection section and the sample liquid in the sample bottle, and the position of the opening at the tip of the purge gas introduction capillary moves between the inside of the sample collection section and the sample liquid. A liquid sample introduction device comprising: a drive mechanism that moves the purge gas introduction capillary to move between spaces above the sample in a bottle; and a controller that synchronizes and controls the solenoid valve and the drive mechanism.