JPS5835459A - Method and device for injecting sample into gas chromatograph - Google Patents

Abstract

(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to gas chromatography, and more particularly to a method and apparatus for introducing a sample into a gas chromatograph. The present invention can be applied to the analysis of trace contaminants in solid, gaseous, and liquid mixtures of organic and inorganic compounds.

Methods are known in the art for injecting a sample into the evaporator of a chromatograph, which is continuously blown through with an inert carrier by a stream of gas, but which is sealed so that no pressure escapes. The sample is introduced by piercing the syringe needle through a septum of self-sealing material that seals and obstructs the inlet of the evaporator, thus injecting the liquid sample into the interior volume of the evaporator. The sample vapor created in the internal volume of the evaporator is carried by a carrier gas to the chromatograph column. Chromatography performed by virtually all hitherto known gas chromatographs uses a sample injector. The accuracy of the graphical analysis is significantly affected by the use of a septum of self-sealing material, such as silicone im, which closes off the evaporator inlet, which is pierced by the syringe needle. There are two main problems that arise in connection with the use of self-sealing septa.

They interfere with analysis inside sensitive instruments during temperature programming. Contamination of the clove 1 togelaf device by septum material, and usually 10 to 2
Loss of self-sealing ability of the septum after several perforations up to 0. The septum generally causes a "yeast beak" to appear on the chromatogram during temperature programming of the column even when no sample is introduced. There are at least four reasons for such contamination. They are the release of gaseous substances by the partition walls that are affected by the high temperatures that occur in the evaporator.

It is grabbed by the needle of the syringe and placed into the evaporator along with the sample. The discharge of the volatile components of the strip broken off from the 11Mw, the residue of the previous sample absorbed by the septum by back-diffusion of the volatiles in the evaporator, and the septum material inside the syringe needle. sample and the residue of the sample before it accumulates during the reaction.

Since 1967, a number of inventions directed to preventing the above factors from interfering with the accuracy of chromatographic measurements have been granted patents in various countries.

Among the very first such inventions were polytetrafluor overlying the surface of the septum, exposed inside the evaporator, and intended for the septum and shield to be moved after each piercing. Consider the use of a barrier in the form of a strip of inert material such as ethylene: U.S. Pat. No. 3,581,573, issued in 1971, C1, 7.
There was one indicated by 3-422.

Another invention, patented in 1972 and disclosed in U.S. Pat. The shield is slidably placed, the hole is properly aligned with the inlet in the head of the evaporator before piercing the septum with the needle of the syringe, and then the septum is inserted into the heated zone of the evaporator. from its position in proper alignment with the perforations in the septum so that it is completely insulated from the

Another invention that sought to prevent septa from adversely affecting the results of chromatographic analysis was U.S. Pat. No. 3,959.713, CJ, issued in 1976, 7
3-422. An improved feature of the invention is that by turning the evaporator off after each sample injection, the septum is completely shielded from the interior volume of the evaporator.

However, the inventions cited so far provide only partial solutions to the problem of bulkheads. Although they prevent contamination caused by volatiles of the septum, they do not eliminate the ingress of some of the septum material that is introduced into the evaporator by, for example, a syringe needle. Furthermore, other problems such as the pressure tightness of the partition walls were not completely resolved.

To reduce the drawbacks of self-sealing septa, new devices have been developed that introduce sealed samples into capsules of inert metals such as aluminum, gold, etc. The capsule is introduced into the evaporator through the inlet and pierced with a hollow needle, after which the contents of the capsule are blown r-rr-r by the heated transport stream into the chromatography column. carried.

(See U.S. Pat. No. 3,783,794, C1,75-422, issued in 1974).

What is unique about this device is that there are too many moving elements to be rubbed and its structure is complex.

More recently, methods have been proposed for introducing the sample into a gas chromatograph, in which the liquid sample is injected into the evaporator of the chromatograph through an inlet that is sealed by a one-turn shutoff valve. Before inserting the syringe needle into the evaporator, the evaporator is depressurized. After the sample has been injected and the needle has been withdrawn from the vaporizer, the inlet is again hermetically closed by the rotatable valve.

That device has the disadvantage that the rotatable valve is placed in close proximity to the heated zone of the evaporator.The valve is operated without lubrication only by the high precision bonding of its polished surfaces. It is intended to ensure that the inlet of the evaporator is sealed and closed, which has a negative impact on the reliability of the gas chromatograph.

This is especially true when analyzing substances with high boiling points, such as those exceeding 450°C. Another disadvantage is that only a syringe must be used as a sample carrier, limiting the range of substances that can be analyzed since only liquid or gaseous samples can be introduced with a hypodermic syringe.

(K. Grob, Grob II 1978 Journal of Chromatography, No. 151, 611
(see page).

The present invention provides a method for transferring a sample to a gas chromatograph, which allows reliable and accurate chromatographic analysis results to be obtained by preventing contaminants from entering the sample being analyzed. It is directed to a method and apparatus for introducing a sample of the substance under analysis into the evaporator of a gas chromatograph by means of a sample probe or carrier, and then generating vapors of the substance. According to the invention, in a method for transferring a gas into a gas chromatograph (7) chromatography column by a flow of carrier gas,
The evaporator of a gas chromatograph is sealed only during sample injection, after physically communicating the evaporator to the sample carrier.
The vapor of the substance under analysis is transferred from the evaporator via a flow constrictor of constant cross-sectional diameter into the chromatographic column, the evaporator being open to the atmosphere after such transfer.

The method is advantageous in that the evaporator is sealed only during sample injection, and the vapor is passed through a flow constrictor of constant cross-section to the black thornfish placement ram, after which the evaporator is opened to the atmosphere. until the next sample is introduced into the evaporator.
During the chromatographic analysis of the sample thus introduced,
Since the material emanating from the evaporator does not enter the column of black thornfish, the internal volume of the evaporator is flushed out, ie, blown away, by a portion of the carrier gas stream entering the column inlet. This prevents contaminants from entering the injected sample and ensures more reliable and accurate results of the chromatographic analysis.

In one simple form of carrying out and carrying out the method according to the invention, the liquid sample is injected into the vaporizer by means of a sample probe or carrier, such as a hypodermic syringe, the part of the syringe being inserted into the vaporizer; For example, the physical volume of the needle is
The internal volume of the evaporator is somewhat smaller, or almost equal to it.A liquid sample introduced into the evaporator evaporates and rapidly increases its volume, thereby forcing the sample to flow out of the evaporator. An overpressure of vapor is created inside the evaporator sufficient to transfer it through the evaporator into the carrier gas stream that enters the chromatography column.

Preferably, the substance under analysis is carried from the evaporator into the chromatographic column by a flow of carrier gas which is fed into the evaporator after it has been sealed. At the same time, after the vapor is transferred from the evaporator to the chromatography column, the flow of dialysis gas supplied to the evaporator is cut off, and this flow is then passed downstream of the flow constrictor to the inlet of the chromatography column. directed towards.

According to the invention, there is further provided an apparatus for carrying out the method according to the invention, in which a sample carrier & The evaporator is periodically connected to the evaporator having a passageway conveying the substance vapor from the evaporator to the chromatography column. According to another feature of the invention, a flow restriction of constant cross-sectional diameter is provided between the passage leading the sample carrier to the evaporator and the passage carrying the vapor of the substance under analysis from the evaporator to the chromatography column. The sample carrier on which the vessel is placed is equipped with a sealing element that sealingly engages the sample carrier with the evaporator during sample injection.

The main advantages of this device for injecting samples it.

It does not use self-sealing septa, it prevents contaminants and septum volatiles from penetrating into the sample material, thereby improving the reliability and accuracy of chromatography analysis. Significantly different from prior art devices such as those in This improves the reliability of the device, especially when operating at the high temperatures (above 400°C) encountered in the evaporator. The device can use various known types of sample carriers such as syringes, pipettes, ambles, etc., which allows a wide surround of sample material to be introduced by the device proposed herein.

A less complex modification of the device according to the present invention, which can be used with any known American chromatograph without redesigning its structure, is placed inside the evaporator and allows the liquid to flow through the sample. Another modified form of the O sample injector uses a constant cross-sectional diameter flow constrictor in the form of a capillary extending the passageway into the evaporator. ° is bulked at the outlet of the evaporator so that it becomes part of the passageway that excludes the vapor of the substance under analysis from the evaporator into the chromatography column. This modification is particularly advantageous for use with temperature programmable chromatography columns. The flow restrictor is preferably placed in the furnace of the column.

Another example of a sample injection device uses a flow constrictor or flow restrictor in the form of a tube filled with particulate absorbent. The absorbent is the same as that used in chromatography columns. This modification is preferably used in conjunction with a chromatograph equipped with a blow-off device to wash away the heavier sample components to speed up the analysis of the lighter components.

One preferred embodiment of the apparatus includes a flow divider attached to the carrier gas supply pipe, one outlet pipe of the flow divider having a
A passage leads the sample vapor from the evaporator and into the chromatography column upstream of the flow constrictor, the outlet tube of which is equipped with a shutoff valve. Another outlet tube of the flow divider leads to a passageway that rejects sample vapor from the evaporator and into the chromatography column downstream of the flow restrictor and is equipped with an adjustable flow restrictor. This device is
A carrier gas is intended to drag the substances under analysis and transport them from the evaporator into the chromatography column, thereby increasing the reproducibility of sample injections.

Additionally, this embodiment includes another controllable isolation valve located in the outlet pipe with an adjustable flow restrictor connected to the flow divider.

A further modification of the device is contemplated in which a hollow long tube with a pointed end extending from the evaporator is used to inject a sample in the gas phase that is in thermodynamic equilibrium with the liquid or solid substance being analyzed. The extended needle flea serves as a passageway for the sample carrier to the evaporator.

The sample carrier is generally an ampoule partially filled with the substance under analysis, the top or neck of which is closed by a septum, or membrane, of self-sealing material. The ampoule is made to move towards the end of the pointed needle so that the needle pierces the self-sealing septum, opening the internal volume of the ampoule to the evaporator at the moment the introduction of the gas phase sample begins. To prevent vapor condensation, the hollow needle is preferably enclosed within a temperature-controlled I housing, and the pointed end of the needle extends therefrom.

During the measured yellow injection of liquid samples, in order to improve the reliability of the action, the sample carrier has the form of a capillary tube with a hermetically closed end attached to the holder, and the capillary tube is closed. It has a horizontal hole adjacent to the section. Capillaries are also
It has a sealing sleeve of inert deformable material.

This structure is particularly advantageous for introducing small liquid samples (up to 1 microliter), since it prevents fractionation of sample components. - Improved reliability of the device is obtained with the construction hitherto described by the capillary retainer having a spring-biased grip in the form of a wavy bar with a corrugated hooked end. It will be done. The head portion of the evaporator has a collar in fixed engagement with the corrugated end of said plate, the head collar tapers outwardly, and the tapered portion of the head collar carries a longitudinal or axial force along it. It has a group that extends in the direction. Additionally, a microswitch is placed very close to the evaporator head to automate the sample injection action. Its structure is also.

The control device includes a control device for controlling a shut-off valve, the control device being electrically connected to a microswitch, one of the spring-biased gripping plates is arranged so that the passageway is opened before passing the sample carrier to the evaporator. It has a resin which cooperates with said microswitch at the time of actuation to be sealed.

Instead, in order to introduce a sample of solid material, the sample carrier has a rod-like shape made of ferromagnetic material, and the two sides of the evaporator are surrounded by an induction coil.

Disclosed below are various embodiments of a sample injection device according to the present invention. The method according to the invention.

This will be better understood by considering the structure and operating method of the device.

Referring to Figures 1 and 2, there are two less complex positions of the sample injector: before injecting the sample (Figure 81) and during injection (Figure 2 #XJ). A preferred embodiment is shown. Referenced generally by numbers 1.2 and 3 are the evaporator, sample carrier, and chromatography column, respectively. The chromatographic column 3 may be of any known suitable construction and has the form of a tube 4 of inert material, such as glass, filled with particulate absorbent 5. The sample carrier 2, which is part of the sample injection device, may also be of any known conventional design, and in this modification is generally a syringe with a diameter 6 made of a transparent material such as glass. , the internal passage of which is provided with a mandrel 7 that can be moved longitudinally along a passage in the axial direction of the syringe. The hollow needle 8 is the 11e day 6 of the syringe.
, whose internal passage is actually an extension of the internal passage of the body 6 .

The evaporator 1, which is essential to the sample injector proposed here, includes a cylindrical body 9 and a heater 10 made of an inert, heat-resistant material such as stainless steel. The sample carrier 2 is placed inside the evaporator 1.
There is a tubular element 11 forming a passage leading to. In the embodiment disclosed here, the communication between the sample tube 2 and the vaporizer 1 is obtained by inserting the hollow needle 8 of a hypodermic syringe into the internal volume of the tubular element 11, the size of the tube 11 being is such that the internal volume of the needle 8 is approximately equal to the internal volume of the tube 11, but somewhat smaller than the internal volume of the tube 11, so that the needle 8 is placed with a minimum clearance to the inner wall of the tube 11. To be elected. The tube 11 is provided with a sealing ring 12 of soft material, such as aluminum or copper, which is pushed into sealing engagement by a coupling nut 14 towards the head 13 of the body 9 of the evaporator 1. The sealing ring 12 is
It is joined to the pipe 11 by welding or the like.

Inside the evaporator 1 there is provided a flow constrictor 15 in the form of a capillary, ie of constant area cross-sectional diameter, extending from the tubular element 11 . A conduit 16 serves to convey an inert carrier gas, such as nitrogen, to the evaporator 1.
It is placed so that it leads to the evaporation chamber. Conduit 16 includes a bypass line 17 having a controllable disconnect valve 18, such as an electromagnetically controlled valve. Inside the evaporator 1, the vapor of the substance being analyzed is passed from the evaporator 1 into the chromatography column 3 through an annular gap created between the wall of the evaporator 9 and the tubular element 11. There is a tube 19 forming a passage for exclusion. In the embodiment shown in FIGS. 1 and 2,
The chromatographic column 3 is in fact an extension of the evaporator passageway which excludes vapors from the evaporator 1 and is separated from the evaporator by a filter 20 of inert fibrous material such as glass fiber. The pressure tightness at the point where the pipe 19 extends away from the evaporator 1 is ensured by the coupling nut 22.
This is ensured by providing a sealing element 21 which is pressed into a sealing fit on the end face of the cylindrical tube 9 of the evaporator 10 facing the chromatography column 3. Alternatively, other known suitable sealing elements may be used for tube 19 and evaporator 10.
It may be used to create a pressure-tight space. The sample carrier 2 also comprises a sealing element 23, which in this embodiment is actually a guide 25 for aligning the needle 8 with the tubular element 11 when inserted into the internal volume of the evaporator 1. an annular sleeve of deformable material, such as rubber, surrounded by a metal cup 24, having a

The described modification of the sample injector according to the invention operates as follows.

Initially, i.e. before sample injection, a stream of carrier gas is conveyed continuously along conduit 16 to evaporator 1, from where the bulk of the gas enters chromatography column 3 and then to detection. A small portion of the carrier gas, from 1 milliliter to 6 milliliters per minute, may flow, although it tends to deviate from the carrier gas (not shown since it is not relevant to the invention and its construction and use are well known to those skilled in the art). It escapes to the atmosphere via the wringer 15 and the tubular element 11.

The introduction of the sample is carried out by means of a syringe 2 and for this purpose the needle 8 of the hypodermic syringe is inserted into the passage of the tubular element 11 until the end of the tube 11 extending from the vaporizer 1 is made pressure tight by the sealing element 23. inserted inside. The length of the tube 11 is such that the tip of the needle 8 enters the heated zone of the evaporator 1 at the moment pressure tightness is obtained, and the temperature of the heated zone is equal to the evaporation point of the mixture to be analyzed. maintained to reach or exceed. Tubular element 11 and sealed element 2
When a pressure of between 3 and 3 is obtained, the liquid sample.

By pushing the stem 7 of the hypodermic syringe 2 it is injected into the heated zone of the vaporizer 1. The instantaneous evaporation of the sample in the passage of tube 11 creates an overpressure of about 10 to 20 times the pressure of the carrier gas at the inlet of chromatography column 3. The pressure difference between the pressure in the passage of tube 11 and the pressure at the inlet of column 3 of the chromatography directs most of the sample vapor from the passage of tube 11 through the constrictor 15 and into the column 3 of the chromatography.
The sample vapor, which is then entrained by the carrier stream, is admitted to the chromatographic column 3 for separation.

The amount of sample received in column 3 of chromatography is determined by the pressure difference thus created, the resistance of constrictor 15 and the retention time of syringe needle 8 in tubular element 11. Following injection of the sample, the isolation valve 18 is automatically switched from the position shown in FIG. 1 to the position shown in FIG. 2 so that the carrier gas escapes to the atmosphere. , otherwise flowed along bypass pipe 17 into a buffer vessel (not shown). This position of the valve 18 (FIG. 2) reduces the pressure at the inlet of the column 3, which increases the amount of sample forced from the passage of the tube 11 through the constrictor 15 into the chromatography column 3. work. After the sample is injected, the needle 8 of the syringe is inserted into the tube 1.
It is extracted from passage 1. This is accompanied by a loss of pressure tightness in the evaporation chamber 1, with the result that the °C valve 18 is automatically switched from the position shown in FIG. 2 to the position shown in FIG. Valve 1
In this position of 8, a flow of carrier gas is allowed to be conveyed continuously along conduit 16 into the evaporator 1, from where the majority of the flow passes through conduit 19, where the sample is separated into its components. As such, a small portion of the stream entering the chromatographic column 3 is discharged to the atmosphere through the constrictor 15 and the passage of the tubular element 11, thereby blowing away sample residues therefrom.

Therefore, the previously described modification of the sample injection device is such that the introduction of the vapor of the sample during the analysis is carried out by the pressure generated in the passage of the tubular element 11 during the evaporation of the sample and by the pressure in the column 3 of the chromatography. It is characterized in that it is carried out by a pressure difference between the pressure at the inlet and the pressure at the inlet. Blowing away the structure with a carrier gas escaping to the atmosphere helps prevent sample vapor from settling on the structure elements, thus rendering subsequent analyzes independent of previous sample elements. I can do it.

This improves the accuracy of the analysis.

Next, referring to FIGS. 6 and 4, which show approximately two working positions of another modified example of the sample injection device according to the present invention, in which the same elements are indicated by the same numbers, the embodiment shown in these drawings will be described. is a combination of schematic and cross-sectional views formed by tube 19.

It is characterized by having a flow constrictor 315 of a certain preselected cross-sectional diameter placed between the passage for eliminating vapors of the mixture to be analyzed and the chromatography column 3. Moreover, the conduit 16 carrying the carrier gas has a flow regulator 26 and a flow divider 27 placed in series.
Contains.

An outlet tube 28 of one of the flow dividers 27 leads to a passage which excludes the vapor of the substance under analysis from the evaporator 1 and conveys it through a flow constrictor 315 into the chromatography column 3, and with an electric field. A shutoff valve 29 is provided as a controlled valve. Another outlet pipe 30 of the flow divider 2T leads to the AM which rejects the vapor from the evaporator 1 to the chromatography column 3. It is connected downstream of the flow restrictor 315 and includes an adjustable flow restrictor 31 in the tail. A detector 32, such as a flame ionization detector, is attached to the outlet of the chromatography column 3.

The modified sample injector according to the invention shown in FIGS. 3 and 4 operates as follows.

Prior to liquid sample injection (FIG. 6), the flow of carrier gas is passed from the flow regulator 26 into the outlet tube 30 of the flow divider 27 1 and then through the adjustable flow restrictor 31 to the inlet of the chromatography column 3. carried continuously. Most of the flow enters column 3 of the chromatography (2/min).
(in proportions from 0 ml to 30 ml),
It then reaches a detector 32. The remainder or small portion of the flow (
From 1 mm to 3 milliliters per minute enters the evaporator 1 via the flow constrictor 315 and is then discharged to the atmosphere through the tubular element 11.

In this path of carrier gas, valve 29 is closed and a moderate flow rate enters the chromatography column 3, while a small portion of the carrier gas flow passes through the evaporator 1, i.e. Move to blow it away. Sample collection is then carried out by means of a syringe 2 acting as a sample carrier, and the liquid mixture under analysis is determined
The measured quantity is thus introduced.

The syringe 2 is equipped with a sealing element 23 at the point of contact of the needle 8 with the syringe sleeve 6, the sealing element 23 being in the form of a bim sleeve that is slipped onto the syringe 20 needle 8 before sample injection. be. The needle 8 of the syringe 2 is then carefully inserted into the passage of the tubular element 11, which is facilitated by the passage having a larger diameter than the outer diameter of the needle 8.

The needle 8 is inserted once into the passageway of the tube 11 so that the rubber sleeve 23 completely blocks the entrance to the passageway.

Following this, valve 29 is switched to the position shown in FIG. In this position the valve 29 is open so that the carrier gas flow leaving the flow divider 2T passes along both of its ports 28 and 30, and one of the carrier gas flows passes through the outlet 3o and is regulated. One stream of carrier gas enters the chromatography column 3 via the flow constrictor 31, while another carrier gas stream enters the evaporator 1 through the outlet 28.
From there it moves along the path of tube 19 and through constrictor 315 which also enters column 3. By pushing the stem 7 of the hypodermic syringe 2, the liquid sample under analysis is injected into the passage of the tube 19 placed in the heated zone of the vaporizer 1.

The liquid sample mixture is then evaporated, whereby the vapor is entrained by the flow of carrier gas entering the evaporator 1 from the outlet 2B of the flow divider 27 and transported to the chromatography column 3 via the flow constrictor 315. , where they are separated at the outlet of chromatographic column 3 and detected by detector 23 .

After the sample has been injected and the sample mixture has been separated into components in the chromatographic column 3, the valve 29 is closed (FIG. 6) and the hypodermic needle 8 is removed from the passageway of the tubular element 11. Can be pulled out. The sample injector is thus configured such that a large part of the carrier gas stream leaving the outlet 30 of the flow divider 27 enters the chromatography column 3 and a small portion is carried through the flow constrictor 315 into the evaporator 1. It is returned to the operating system shown in Figure 6,
Thereby, the passageways of tubes 19 and 11 are flushed or blown to remove sample residue therefrom.

Gaseous samples can likewise be injected by means of the syringe 2, in which case the rubber sleeve 23 is attached to the needle (before injection).
Used as a protective shield to close side holes.

Referring now to FIG. 5, there is shown, in part schematically and in part in cross-section, a liquid mixture according to the invention intended for the fractional injection of a liquid mixture sample consisting of the lightest mixture components. Another modified form of sample injector is shown. Heavy components are placed in chromatography column 30.
It is not injected into the air but is released into the atmosphere through the evaporator 1.

The elements in Figure 5 are the same as those in Figures 3vl and 4.

The modified example shown in FIG. 5, designated by the same numerals, differs from the embodiment of FIGS. It has the shape of a filled tube. Chromatography column 3
An absorbent similar to that used in the flow restrictor 515 or any other suitable absorbent may be used as the absorbent for the flow restrictor 515.

Another feature of this modification that differs from the embodiments shown in FIGS. 6 and 4 is that the outlet pipe 30 extending from the flow divider 27 has an open position of the valve 29 corresponding to a closed position of the valve 34; In order to do the opposite, another controllable connection valve 34 is provided which operates simultaneously with the isolation valve 29.

The modified example shown in FIG. 5 operates as follows.

Pressure tightness of the internal volume of the evaporator 1 is achieved by blocking the passage of the tubular element 11 with a rubber sleep-shaped kidney sealing element 23, which is slipped onto the hollow needle 8 of the syringe 2. obtained before. Following this, a liquid sample is injected into the passageway of tube 19.

At the same time, valve 29 is opened while valve 34 is closed. The stream of carrier gas leaving outlet 2B of flow divider 2T is carried into evaporator 1, dragging vapors of the substance being analyzed along the passage of tube 19 and transporting them to flow restrictor 515. Take it inside. Separation of the sample mixture into two or more fractions or components then occurs in flow restrictor 515. This is because the restrictor 515 tube contains particulate absorbent. After the light fraction has been transferred from the flow restrictor 515 to the chromatography column 3, a switching between valves 29 and 34 takes place, with valve 29 assuming the closed position and valve 34 open. Following the switching, the pressure in the vaporizer 1 is relieved by withdrawing the syringe 20 needle 8 from the passage of the tubular element 11, thus moving the sealing element 23 away from the entrance of the passage of the tube 11. In this mode of operation, the flow of carrier gas (the path of the carrier gas flow is shown by the dashed arrow) leaving the outlet tube 30 of the flow divider 27 and entering the inlet of the chromatography column 3 is divided into two Divided into streams. One stream enters column 3 of the chromatography, carrying with it the lighter fractions of the sample mixture being analyzed along the length of the column, and they pass into a separate emission pan P ( 5epa
It is further separated and detected by a detector 32 in the form of rate omission bands). Another flow of carrier gas enters flow restrictor 515;
The particulate absorbent 33 is washed away and the heavy fractions, which are not analyzed, are blown away through the passages of tubes 19 and 11 to the atmosphere. The blowing of the particulate sorbent filling the flow restrictor 515 causes all components of the light fraction to be forced from the chromatography column 3 into the detector 32 and all the heavy components to fill the flow restrictor 515. This continues until it is removed from the atmosphere.

The above-mentioned modifications of the sample injector according to the invention are:

Prevents heavy fractions of the mixture under analysis from entering the chromatography column, thereby reducing the time required for chromatography analysis.

Referring now to Figures 6 and 7, they show, partly schematically and partly in cross-section, a sample of the gaseous phase remaining in equilibrium with the sample of liquid or solid being analysed. An embodiment of a sample injector according to the invention intended for injection into a gas chromatograph is also shown. Figure 6 shows an example of the proposed modification before sample injection.

FIG. 7 shows it during injection of the gas phase. The embodiment of FIGS. 6 and 7 differs from the modification shown in FIG. , and the pointed end 36 of the needle 35 is sufficiently spaced from the evaporator 1. The needle 35 is enclosed in a temperature controlled housing 3T equipped with a heating wire 38. The pointed end 36 of the hollow needle 35 is fixed to the housing 37 and extends a distance therefrom. The sample carrier has the form of an ampoule 39 partially filled with the liquid or solid substance under analysis. The upper or neck portion of the ampoule 39 is hermetically closed by a septum or membrane 41 of self-sealing material such as silicone im, the surface of which is covered by a layer of polytetrafluoroethylene. Ampoule 39 was placed opposite the pointed end 36 of hollow needle 35 and provided along its periphery with a plurality of similar ampoules 39 partially filled with the liquid or solid sample to be analyzed. The ampoule 39 is rigidly mounted in a temperature-controlled, rotatable, cartridge-shaped holder 42. The hollow needle 35 is held in a retainer 42 which can be moved axially towards the pointed end 36 so as to communicate the internal volume of the hollow needle 39 to the evaporator 1. , an electric heating m43 intended to maintain a predetermined temperature is placed inside the ampoule 39.

In that preferred embodiment of the sample injector according to the invention shown in FIGS. 6 and 7FA, the flow constrictor 15 has the form of a capillary tube extending from a hollow needle 35, and the constrictor is placed in the evaporator. ing. The outlet tube 28 of the flow divider 27 opens into the internal passage of the hollow needle 35 via a valve 29, and the outlet 3 of the flow divider 21
0 communicates via a valve 34 and an adjustable flow restrictor 31 with the internal volume of the evaporator 1 and into the passage of the tube 19 which serves to convey the sample vapor into the chromatography column 3. Instead, a flow constrictor 15 is placed outside the evaporator 1 and serves as part of the passage of the tube 19 to exclude the sample vapor from the evaporator 1 or the chromatography column 3. Examples are also possible.

The presently described preferred embodiment of the sample injection device according to the invention operates as follows.

Prior to sample injection, the holder 42 of the ampoule 39 is in its lowest position, indicated by the dashed line in FIG. At this point in operation, valve 29 is closed and valve 34 is open. The carrier gas is conveyed from the outlet pipe 30 of the flow divider 27 into the internal volume of the evaporator 1.

The majority of the carrier gas flow passes through the passage of tube 19 into the chromatography column 3, while a small portion (from 10% to 30%) passes through the passage of tube 19 and enters the constrictor 15. It enters the hollow needle 35 and is released into the atmosphere. This operative position is such that the pointed end of the hollow needle 35 is axially aligned with the ampoule 40 and
so that it is placed 41 blocks above the bulkhead. Upon receiving a signal from a zologramming device (not shown), the ampoule 39
The retainer 42 is raised to the highest position. needle 35
The pointed end 36 pierces the septum 41 of the ampoule 39 and enters the interior of the flask 39 filled with sample vapor. At this moment, receiving a signal from the zolograming device, valve 29 opens and valve 34 closes. carrier gas (
jIspiJ) flows along the outlet pipe 2B of the flow divider 2T and enters the passage of the needle 35. The carrier gas follows the path of the needle 35 and passes through the flow constrictor 15 into the chromatography column 3. The carrier also
It follows the passage formed by the inside of the needle 35 and enters the internal volume of the ampoule 39, into which the needle 3 is placed.
50 pressure at the inlet of the passage (in this case from 2 atm to 4 atm)
(up to atmospheric pressure) produces a pressure that is woody equivalent to The medium is then saturated with vapor of the liquid to be analyzed in the internal volume of the ampoule 39. After sample injection, valve 29
and 34 automatically assume the position shown in FIG. 7 upon receiving a signal from the Zorogramming device. That is, valve 34 is closed and valve 29 is open (in this position of the valve the pressure value at the inlet of chromatography column 3 is equal to ampoule 39).
The difference between those pressure values is essentially lower than the pressure value inside the internal volume of .

Determined by the pressure differential created by the adjustable flow constrictor 31, the vapor and gas mixture then passes from the internal volume of the aldel 39 along the passage of the needle 35 and constrictor 15 to the chromatography column 3. Enter. The amount of vapor and gas entering the column depends on the time of exposure. 5
After a preselected period of time ranging from 1 to 60 seconds, upon receiving a signal from the zologramming device, valves 29 and 34 are switched to the positions shown in FIG. 6, with valve 29 in the open position and valve 34 in the open position. Closed. The flow of carrier gas conveyed from the outlet tube 2B of the flow divider 27 into the passage of the hollow needle 35 is interrupted to prevent the flow of the vapor and gas mixture from entering the column 3.

After the sample injection has taken place, a signal received by the programming device causes ampoule holder 42 to be lowered and subsequently (with a delay of less than 1 second) valves 29 and 34 are moved to the position shown in FIG. 7 (valve 29 is closed). , valve 34 is open). In this position of the valve, the carrier gas passes along the flow divider 27 and its outlet tube 30 and enters the column 3 of the chromatograph 2 for separation, a small fraction of the gas flow, from 10% to For up to 20%, enter the wringer 15 and press the needle 3.
It is released into the atmosphere through the passage No.5. The passage of the needle 35 is heated to a temperature that prevents condensation of the vapor of the sample mixture, so that the carrier gas escaping to the atmosphere washes the residue of the previous sample from the passage of the needle 35. The separation of the components of the sample mixture is The ampoule holder 42 is rotated at the same time by a predetermined angle to place another sample flask 39 towards the pointed end of the hollow needle 35. This can be done in the order described so far.

Referring now to FIGS. 8 and 9, there is shown, partly in schematic diagram and partly in cross-section, another preferred embodiment of an apparatus for injecting a liquid sample into a schromatograph. , where a micropipette is used as a sample carrier. Elements of the same device as shown in previous figures are designated with the same numbers. The sample carrier of the apparatus of FIGS. 8 and 9 is in the form of a capillary tube 44 made of an inert, heat-resistant material such as glass or stainless steel. The solid or solid end 45 of the capillary tube 44
is one force connected to the retainer 46, and the horizontal hole 4T is the capillary tube 4.
4 directly adjacent the end 45 of the entity. The capillary tube 44 further comprises a seal 123 in the form of a sleeve of deformable inert material, such as a tube. The capillary retainer 46 comprises a grip 49 biased by a spring 48,
9 has the form of a plate of flexible material, such as steel, with a corrugated hooked end 50. The evaporator 1 has a head 51 extending away from the zone to be heated and tightly connected to the tubular element 11, the passage of the tubular element 11, together with the passage in the head 51, evaporating the capillary tube 44. The evaporator head 51 further includes a tab 52 into which the corrugated end 50 of the spring-biased tab 49 is firmly engaged.

The collar 52 is on its side facing towards the inserted capillary when the capillary 44 is introduced into the passage 1151 of the evaporator 1 and further into the passage of the tube 11.

and when this passage is sealed against pressure escape by sealing engagement with the sealing element 23.

It has a tapered surface that serves as a guide for the hooked end 50 of the holder 49. The tapered collar 52 further extends longitudinally therethrough and is used to release the hooked end 50 of the gripper 49 to depressurize the evaporator 1 after the sample has been injected into the gas chromatograph. The head 52 of the evaporator 1 is provided with a group 53 (FIG. 9) intended to
There is a micro switch 4 electrically connected to a control device 55 that controls the operation of the quick-release valves 29 and 34 in the immediate vicinity of the
5 is placed, and the control device is generally a timed relay. From one of the plates of the spring-biased grip 49 extends a retainer 56 which cooperates with a trigger microswitch 54 for pressurizing or depressurizing the evaporator 1.

Another feature of this modification that differs from the previously described embodiments is that the flow restrictors 57 and 58 of constant area cross-section, which serve as a bypass for the outlet pipes 2B and 30 of the flow divider 27, are connected to the quick-acting valves 29 and 30, respectively. and are connected in parallel.

Furthermore, an outlet pipe 28 of the flow divider 27 is connected to a device for monitoring the pressure therein, such as a pressure gauge 59.

The embodiment described herein operates in a first order manner.

Sample fluid is delivered into the calibrated passage of capillary tube 44 by one capillary force. A sealing machine that can move! X23
closes the lateral hole 47 of the capillary tube 44.

Initially, i.e. before injecting the sample into the evaporator 1,
Valve 29 is closed and valve 34 is open. The carrier gas passes along the outlet tube 30 of the flow divider 27 into the internal volume of the evaporator podium 9, from where the bulk of the gas flow, from 30 fml to 60 ml per minute, is directed into the passage of the tube 19. A small portion, from 1 sililiter to 5 ml per minute, is transported along the chromatography column 3 through the flow constrictor 15 and tube 1.
1 passage and through an evaporator 51 to the atmosphere. At the same time, a small portion of the flow sent through the flow constrictor 57, from 1 liter to 2 milliliters per minute, is blown away from a portion of the outlet pipe 28 of the flow divider 2T downstream of the valve 29 to remove 7 liters of gas. Acts to release into the atmosphere.

At the moment of sample injection, the capillary tube 44 is inserted into the passage of the evaporator head 51 and moved as far as possible. The movable sealing element 23 is thereby biased by a spring-biased catch 49 which is pushed towards the head 51 and blocks the entrance to the passage of the evaporator head 51 in sealing engagement therewith.
The corrugated end 50 of the evaporator 1 is fixed to the ridge 52 of the head 51 of the evaporator 1.

A riser 56 extending from one of the plates of the holder 49 is forcefully engaged with a microswitch 54 to close its contacts, and a controller 55 has electrically controlled valves 29 and 34 shown in FIG. Send a signal to both valves so that they can be switched to the position shown. In this position of the valve, a large portion of the carrier flow proceeding along the outlet pipe 28 of the flow divider 27 is directed to the evaporator head 5, which is placed opposite the transverse hole 47 of the capillary tube 44.
1 into the passageway of tube 11 and transfer the measured amount of liquid sample into the tube 11.
, where it evaporates and its vapor, entrained by the flow of carrier gas, then passes through a flow constrictor 15 and a passage in tube 19 to be separated at the outlet of the clotgelafy column 3. transported to a column for detection. Following sample injection, a small portion of the carrier gas flow.

Via a flow restrictor 5B of constant cross-sectional diameter and an adjustable flow restrictor 31, it passes into the internal volume of the body 9 of the evaporator 1, whereby the sample vapor passes through the outlet pipe 3o of the flow divider 2T.
shutoff valves 29 and 3.
4. Upon completion of the injection as indicated by an optical signal indicator 11 (not shown) electrically connected to a control device 55 for regulating the operation, the retainer 46 of the capillary tube 44 is activated by the plate of the capillary tube 49 or the evaporator. 9 until aligned with group 53 of head 51, counterclockwise as best seen in FIG. At the same time, the reso 56 of the hook 49 releases the contact of the microswitch 54 in order to switch the valves 29 and 34 to their initial positions before sample injection (valve 29 is closed and valve 34 is open); The capillary tube is then drawn up from the passage in the evaporator head 51.

Thereby, the pressure in the evaporator 1 is released. This position of the valve is
When the carrier stream is carried by the outlet 30 of the flow divider 21 and enters the evaporator 1 and further along the passage of the tube 19 into the chromatography column 3, a small fraction of the flow is 1 milliliter per minute. or up to 5 milliliters, flow constrictor 15 and tube 11 and evaporator type 510
It is released into the atmosphere through the passageway, and the gas thus released washes away any sample residue from the passageway.

Sample injection can then be resumed, with subsequent liquid samples being injected in the order previously described.

The pressure gauge 59 is used to check the tightness of the passageway of the evaporator head 51 after the sealing element 23 is pressed into sealing engagement with the black generator head 51 during sample injection. Useful. If grip 49 is the evaporator @510 is 52
If the needle of the pressure gauge 59 changes its position after it has become stuck, this indicates that a force has not been obtained that does not provide adequate pressure tightness. In order to correct this situation and completely seal the evaporator, the position of the head 51 relative to the diameter 9 of the evaporator 1 must be adjusted or the sealing element 23 must be replaced.

Another modified form of the sample injector, shown in FIG. 10, is intended for injecting solid sample material. Referring to FIG. 10, the sample injector includes a sample carrier 1 made as a bar member 60 of ferromagnetic material, while an induction coil 61, used in place of the heating wire of the previous preferred embodiment, It is fitted into the body 9 of the vessel 1, that is, it surrounds it.

A ferromagnetic rod 60 is attached to a standby 62 by sliding the sealing element 23 onto it. A sample of a solid substance is
It is dissolved in a volatile solvent and a measured amount of the solution is applied to the end face of the ferromagnetic rod 60, such as with a syringe. The thus coated sample is then swept away for 5K so that the solvent vapor leaves a thin film of solid material on the surface of the rod 60.

Dry in a stream of inert gas or by an infrared radiator. The rod 60 is then installed in the evaporator and closes the entrance to the passage of the tube 11 by means of a sealing element 2'3. Valve 29 is opened such that pyrolysis of the sample of solid material is effected by pulses of high frequency current induced by coil 61.

Valve 34 remains closed during this operation.

At the position of the valve shown in FIG. 10, the entire flow of carrier gas exiting the flow divider 27 is directed along the outlet tube 28 to the tube 11 in order to draw with it the gaseous and vaporized products of pyrolysis. and convey them through the flow constrictor 15 and tube 19 passages into the chromatography column 3. After the products of pyrolysis are sent to chromatography column 3, valves 29 and 34 are connected to valve 2.
9 assumes the closed position and the valve 34 is switched open. Therewith, the entire flow of carrier gas is directed from the flow divider 27 along its outlet pipe 30 and the valve 34 is switched open. It enters the chromatography column 3 via the valve 34 and the adjustable flow restrictor 31 through the valve 190 passage.The rod 60 is then withdrawn from the passage of the tube 11 and a small portion of the middle gas flows through the passage. It escapes into the atmosphere through the wringer 15.

The use of a sample injector according to the present invention prevents errors in chromatographic analysis that commonly occur when septa are used in prior art sample injectors. In other words, the method and apparatus proposed here can be used to detect
``Ghost Peak'' will appear.
This helps prevent particles of the material from entering the internal volume of the evaporator. Another advantage of the sample injection device according to the invention is that the device consists of largely standard conventional elements and can be used with any known suitable gas chromatograph without substantial modification to the 70-piece set-up. Low production cost due to

Finally, the sample injector according to the invention is capable of injecting samples in various phases, such as liquid, gas, and gas phase.

Disclosed herein were various embodiments of the invention.

However, such embodiments may be modified without departing from the spirit and scope of the present invention (various changes and modifications may be made thereto).
It will be clear to those skilled in the art.

[Brief explanation of the drawing]

1 shows a sectional view of the sample injection device according to the invention in its simplest form at the moment just before sample introduction; FIG. 2 shows the device of FIG. 1 with a sample carrier inserted; 3 &; ! J is another embodiment of the sample injection device,
4 shows the apparatus of FIG. 3 with a sample carrier inserted, and FIG. Schematically and partly in cross-section - one modified form of the device according to the invention having a flow restrictor in the cross-section, i.e. simply in the form of a tube filled with particulate absorbent; FIG. 6 shows, partly schematically and partly in cross-section, at the moment just before sample introduction.
7 shows an embodiment of the device according to the invention, intended to introduce a gas phase in equilibrium with a liquid or solid phase;
The figure is at the time of gas phase introduction. The device of FIG. 5, FIG. 8 shows an embodiment of the device according to the invention with a sample carrier in the form of a pipette, FIG. 98u is a partial top view of FIG. 8, and FIG. 1 shows an example of a device according to the invention intended for introducing solid samples; The reference number 1 in the drawing is "Evaporator J," 2.3!1 is "Sample carrier J," 3 is "Chromatography column," and 6 is "
9 is the evaporator body, 11 is the syringe body, and 11 is the evaporator body.
19 is a passage leading the sample carrier to the evaporator, and 19 is a passage for eliminating vapor. 15.315 is "flow constrictor", 23 is "sealing element",
2T is the "shunter", 28.30 is the "shunter outlet pipe",
29 and 34 are "controllable shutoff valves". 31 is "Adjustable flow constrictor" %35 is "Hollow needle"
, 36 is the "pointed end of the needle", 37 is the "temperature-controlled housing J", 35Htr antill 141 is the "bulkhead"
, 44 is the "capillary", 45 is the "capillary end J, 49 is the "grip", 50 is the hook-shaped end of the grip, 51 is the "Ir1J of the evaporator, 52 is the "boxwood", 53 is the "vertical" group of
, 54 is a "micro switch", 55 is a "control device",
56 is "Reso", 60 is "rod", 61 is "induction coil"
, 62 indicates a "retainer", and 515 indicates a "flow restrictor". Table of reference numbers used in the claims of the invention 1 - Evaporator 2 - Sample carrier 3 - Chromatography column 11 - Channel leading the sample carrier to the evaporator 1 - 5, 3
15,515 - Flow restrictor of constant cross section 19 - Passage for excluding steam 23 - Sealing element 27 - Flow divider 28 - Outlet pipe of the flow divider 29 - 4 valve cutoff 30 - Outlet pipe of the flow divider 3l - fI11 Articulating flow constrictor 34 - Sliding valve 35 - Hollow needle 36 - Pointed end of needle 39 - Ensol 41 - Septum 44 - Capillary tube 45 - Capillary body end 46 - Retainer 47 - Transverse hole 49 A handful 50 One hooked end 51 - Evaporator head 52 One barb 53 - Vertical group 54 - Micro switch 56 - Rib 60 - Rod 61 - Induction coil 62 - Retainer representative Asamura Hiroshige Page 1 Continuation of 0 Inventor Yuri Abramovich Sultanopitch Soviet State Moscow Provsoyuznaya Ulitsa 3 Corps 3 Cavy 53 0 Inventor Vrushimir Mikhailopich Posiemansky Soviet State Moscow 2 Pavlovsky Pereulok 20 Cavy 80 0 Inventor Karl Ivanovich Sakodinsky Soviet Union Moscow Ulitsa Babilova 12 Cave 29 Inventor Semen Samuilopich Berlin Soviet Union Moscow Sovkoznaya Ulitsa 53 Corpus 1 Cave 33 0 Inventor Vrashim Ivanovich・Ogurtosov Soviet State Moscow Fergansky 2 Proezd 14 Corpus 2 Cavy 81 0 Inventor Vrushimir Vasilyepich Alekhine Soviet State Moscow Ulitosa Ku'Sinena 6 Corpus 7 Cavi 79 The Commissioner of the Patent Office 1, of the case Display Patent Application No. 132545 of 1982 3, Relationship with the case of the person making the amendment Patent applicant 4, Agent 5, Date of amendment order Showa Year Month i

Claims (1)

Claims: (11) A method of injecting a sample into a gas chromatograph in which a sample of the substance under analysis is introduced by a sample carrier into the evaporator of the gas chromatograph, and the resulting The vapor is transferred into a stream of gas as the carrier advances toward the chromatography column of the gas chromatograph. After physically communicating the evaporator with the sample carrier, only during the introduction of the sample. After sealing the evaporator against pressure escape and transferring the vapor to be analyzed into the chromatographic column via a flow constrictor of constant, ie constant cross-section. A method for injecting a sample into a chromatograph, characterized in that the evaporator is connected to the atmosphere. (2) In the method according to claim 1, the temperature is 0.degree. The introduction of the sample into the evaporator is carried out by a sample carrier, the physical volume of the part of the sample carrier inserted into the evaporator being somewhat smaller than or approximately equal to the internal volume of the evaporator. , during the evaporation of the liquid sample in the internal volume of the evaporator and due to the overpressure of the vapor of the substance under analysis that occurs, the vapor of the substance to be analyzed is directed from the evaporator towards the column of the chromatography. It is characterized in that the advancing carrier can be transferred into a stream of water. A method of injecting a sample into a gas chromatograph. (3) In the method according to claim 1. The vapor of the sample material is transferred from the evaporator to the chromatography column by a flow of the carrier gas that is directed into the evaporator after the evaporator is sealed against pressure escape. After such transfer, the flow of the carrier gas fed into the evaporator is interrupted and the flow is directed downstream of the flow constrictor to the population of the chromatography column. A method of injecting a sample into a chromatograph. (4) An apparatus for injecting a sample into a chromatograph for carrying out the method according to claim 1, wherein the sample carrier is connected to a passage leading to the evaporator, the carrier gas into the evaporator, and a passageway for rejecting vapors of the substance under analysis from the evaporator to the chromatography column. after the passageway (11) leading the sample carrier (2) to the evaporator (1) and the vapor of the substance under analysis from the evaporator (1) to the chromatographic column (3). VC, in front of said passageway (19) to exclude, a flow constrictor or flow restrictor (15, 315, 5) of constant loss cross section;
15) is essentially arranged such that said sample carrier (2) is provided with a hermetic seal which hermetically closes said passageway (11) leading said sample carrier (2) to said evaporator (1) during sample injection. An apparatus for injecting a sample into a gas chromatograph, comprising an element (23). (5) The apparatus according to claim 4,
The flow constrictor (15) is connected to the sample carrier (2).
A device for injecting a sample into a schromatograph, characterized in that the channel (11) leading to the evaporator (1) is in the form of an elongated capillary tube and is placed inside the evaporator. (61 #! f In the device according to claim 4,
The flow constrictor (315) is placed at the outlet of the evaporator (1) to be part of the passageway, through which the vapor of the substance under analysis flows from the evaporator (1) to the gas chromatography. An apparatus for injecting a sample into a gas chromatograph, characterized in that the sample is rejected by the column (3) of (7) Device according to claims 4 and 6, characterized in that the flow restrictor is made as a tube (515) filled with particulate absorbent (33). A device that injects a sample into a gas chromatograph. +8)! Apparatus according to claims 4 to 7, in which the carrier gas conduit (16
) is equipped with a flow divider (27), one outlet (28) of said flow divider (27) leading to said passageway (19) rejecting vapors from said evaporator (1) to said chromatography column (3). ) having a controllable isolation valve (29) essentially located upstream of the flow and before the flow constrictor or flow restrictor (15, 315, 515);
Another outlet (3o) of the flow divider (27) is. Essentially after said flow restrictor (15, 315, 515) and downstream of said flow therethrough said passageway (1
9) and having an adjustable flow restrictor (31). (9) A device according to claim 8, which is located in the outlet pipe (30) of the flow divider (27), provided with the adjustable flow restrictor (31). Apparatus for injecting a sample into a gas chromatograph, characterized in that it further comprises a controllable shut-off valve (34). αI In the apparatus according to claim 9. A hollow needle (35) is used as a passage through the sample carrier to the evaporator (1), said needle having a pointed end (36) extending away from the evaporator (1); The sample gear (2) is an ampoule (3).
9) and its top or neck is made of self-sealing material with a spacing of 1! (41), said ampoule (39) is sealed so that said needle (35) is placed in said flask (39) at a point immediately prior to sample introduction.
moving towards the pointed end (36) of the hollow needle (35) so as to pierce the septum (41) of self-sealing material to communicate the internal volume of the needle to the evaporator (1). An apparatus for injecting a sample into a gas chromatograph, characterized in that: (37) and said pointed end (36) of said needle
) extends from the apparatus for injecting a sample into a gas chromatograph. 02, the apparatus according to claim 9, wherein the sample carrier (2) has a hermetically closed end (45
) in the form of a capillary tube (44) attached to a retainer (46), and furthermore, said hermetically closed end (4
5) has a lateral hole (47) adjacent to said capillary tube (44);
Device for injecting a sample into a gas chromatograph, characterized in that the device comprises a movable sealing sleeve (23) of inert deformable material. Q3 In the device described in claim 12,
The retainer (46) of the capillary tube (44) is provided with a spring-biased grip (49) in the form of a plate of flexible material with a corrugated hooked end (50); The evaporator has a head It (51) with a head (52) adapted to securely engage the corrugated end (50) of said plate;
The head (51) of the evaporator (1) is (52)
] Apparatus for injecting a sample into a gas chromatograph, characterized in that it has a tapered surface, through which the longitudinal groups (53) extend. (141% In the device according to claim 13,
It was electrically connected to the microswitch (54) located in the immediate vicinity of the head member (51) of the evaporator (1). one of the plates of the spring-biased grip (4s) is equipped with a control device (55) for controlling the sample carrier (2) in the evaporator (34);
1) while the passage (11) leading to the microswitches (5, 4) is sealed to prevent pressure from escaping.
) and has a Rizzo (56) that cooperates with it. A device for injecting a sample into a gas chromatograph, characterized by: a9 An apparatus according to claim 9, wherein the sample carrier (2) has the form of a rod (6o) of ferromagnetic material mounted on the holder (62), and the sample carrier (2) The day (9) is equipped with an induction coil (61),
A device for injecting a sample into a gas chromatograph, characterized by: