Device for supplying samples for gas analysis

 

(57) Abstract:

The invention relates to analytical instrumentation. The device includes an inner tube, one end of which is open, while the other is connected through the detector by means of motive gas flow, an intermediate tube, one end of which is open, while the other has a plug, through which is threaded open end of the inner tube, outer tube, one end of which is open, while the other is docked with the open end of the intermediate tube, injector tube with the sample material, one end of which is placed in the outer tube with a gap relative to its inner walls, and the other is placed outside the outer tube and connected through quick release tight joints and flexible pipe to the pump flow of carrier gas or gaseous samples. Moreover, the open end of the inner tube is passed through the intermediate tube and is installed inside the injector tube and the intermediate tube is connected through a pipe with a pump flow of carrier gas. The technical result of the present invention is expressed in increasing the reliability of the qualitative and quantitative analysis. 1 C.p. f-crystals, 2 Il.

Izopet asnyk samples and samples of volatile substances, capable in terms of conducting the analysis proceed in the gas phase, from solid and liquid materials, in particular, high-resolution qualitative and quantitative microanalysis of gas chromatography and mass spectrometry.

A device for supplying volatile materials from solid materials for analysis in a gas chromatograph (U.S. Patent N 5065614, MKI G 01 N 30/18 publ. 19.11.91 g), including removable injector tube with the sample material, one end of which is connected through quick release tight joints and flexible pipe to the source of the impulses of the flow of carrier gas, and the other end has a removable needle. The device is equipped with a thermal desorption unit, made of a material with high heat conductivity and having a channel located coaxial injector tube and the open end of the chromatographic column. Around the canal to the heating element. The injector tube with a needle equipped with a mechanism for reciprocating movement and fixing it accordingly in three positions: the injector tube with the needle withdrawn from the channel of thermal desorption unit (preparatory phase); the injector tube with the needle placed in the channel of thermal desorption unit (heating of the sample); the injection needle Nogo device is the narrow scope of its use in micro-analytical technique because of the large number of restrictions on the use, as well as the lack of representativeness of the sample due to a change in its qualitative and quantitative composition due to the duration of the interaction of its components with the heated solid material and with each other. The injector tube with the needle, due to the complexity of its construction, has a relatively large mass, resulting in its solid material may be quickly heated (heating rate of not more than 100oC/min heating time of at least 0.5 min). This, on the one hand, it is not possible to combine the procedure of heating the solid material and sampling procedure the sample from the injector tube for analysis, and on the other hand can lead to a change in the qualitative and quantitative composition of the sample.

The closest technical solution (prototype) is a device for supplying gas analysis of samples of volatile substances from solid materials in the form of filter (US Patent N 5109710, MKI G 01 N 30/20, publ. 05.05.92 g) comprising an inner tube, which is a chromatographic column, one end of which is open and the other end connected through the detector to the booster gas stream representing a channel connecting the detector with the environment; the intermediate tube, the morning of the tube; the outer tube, one end of which is connected with the open end of the intermediate tube, and the outer and intermediate tubes is provided with each of his pipe with a valve; a heating device and temperature control, located around the intermediate tube with the nozzle and part of the outer tube adjacent to the intermediate tube; an injector tube with the sample material, one end of which is perforated, provided with a perforated cover and placed in the outer tube with a gap relative to its inner wall and its other end located outside the outer tube and connected through quick release tight joints and flexible pipe, to stimulate a flow of carrier gas; node isolation channel of the outer tube from the environment, representing the seal Assembly in the form of an elastic cuffs placed on the end of the outer tube, through which omitted the injector tube with the possibility of reciprocation without depressurization of the outer tube; a cooling device outer tube in the area of the seal node representing a section of outer tube made of ceramics.

The device prototype has disadvantages for use, osobennoy before entering the open end of the inner tube and the large contact surface of the sample components with the elements of the outer and intermediate tubes, there is an increase in the duration of feeding them into the inner tube and, accordingly, increase the width of the chromatographic peaks, and also changes the qualitative and quantitative composition of the reactive components of the sample;

- when placing the sample in the injector tube environment penetrates, due to diffusion, in the outer, intermediate and inner tubes;

- at the time of submitting samples for analysis of pollution from the field site seal outer tube penetrate, due to diffusion, intermediate and inner tubes. All the above-mentioned disadvantages reduce the reliability of the quantitative and qualitative analysis.

In the prototype is not considered the possibility of filing for analysis of samples when the pressure in the sample is equal to or below the ambient pressure and the possibility to apply for the analysis of gaseous samples, which limits the scope of application of the device.

Disclosure of the invention

Object of the present invention is to provide such a device which would provide the feed gas analysis gas samples and samples of volatile substances in the conditions of the analysis proceed in the gas phase, from solid and liquid materials, when the pressure of the reliability of the qualitative and quantitative analysis due to:

- sample feeding the shortest path in the channel connecting the device with the detector, without intermediate contact of its components with most of the elements of device:

in all modes except penetration in the channel connecting the device with the detector, contamination of the elements of the device and the environment.

This task is solved in that the device for supplying samples for gas analysis, including the inner tube, one end of which is open and the other end connected through the detector by means of motive gas flow; an intermediate tube, one end of which is open and the other end has a plug, through which is threaded open end of the inner tube; an outer tube, one end of which is open and the other end connected with the open end of the intermediate tube; heating device and temperature control, located around the outer tube and the intermediate tube; an injector tube with sample one end is placed in the outer tube with a gap relative to its inner walls, and the other end is placed outside the outer tube and connected through quick release tight joints and flexible pipe, to the s, according to the invention, the end of the injector tube, placed in the outer tube, is made open; the open end of the inner tube is passed through the intermediate tube and is installed inside the injector tube; node isolation channel of the outer tube from the external environment is made in the form of a booster flow of carrier gas connected through a pipe to the intermediate pipe.

Node isolation channel of the outer tube from the external environment can be further provided with a removable rotary tube, one end of which is connected to the open end of the outer tube by means of the detachable sealed connection and the other end provided with a site seal, executed, for example, elastic cuff, through which missed the end of the injection tube located outside the outer tube, with the possibility of reciprocating movement of the injector tube without the depressurization of the rotary tube. When this Gating tube is connected through a pipe to pump gas stream, and around it in the area of the site seal is a cooling device, for example, in the form of a heat sink with forced ventilation. The booster flow of gas from the rotary tube can be made in the form of Pobediteli gas from the rotary tube, you can use the valve, connected with the environment.

New distinctive features of the prototype characteristics of the proposed device provide:

- submission of samples in the shortest way into the inner tube without intermediate contact of its components with the elements of the outer and intermediate tubes by placing the open end of the inner tube inside the injector tube;

- submission of samples for analysis at a pressure in the layout area of the sample, both above and below and equal to the ambient pressure due to the supply of the carrier gas in the intermediate tube and the supply device removable rotary tube;

in all modes except penetration into the inner tube of the environment or the environment of a rotary tube through the open end of the outer tube and the outer tube by creating a flow of carrier gas from the pump flow of carrier gas through the pipe intermediate tube, an intermediate tube, the outer tube and through the open end of the outer tube into the environment or into the lock tube.

Brief description of drawings

The invention is further explained in the description of specific variants of its implementation and the accompanying drawings, on which:

Fig. 1 - diagram of the device for poda"ptx2">

In Fig. 1, 2 characters "A", Q1 - Q4 marked material containing the sample, and the absolute value of the cost of the gas streams, the arrows indicate the direction of the gas streams.

Option 1.

According Fig. 1, the device for supplying the samples in the first embodiment includes the inner tube 1, which represents a quartz capillary column for gas chromatography, the end 2 of which is open and the other end connected through the detector 3 to the pump gas flow (not shown), a vacuum pump. The intermediate tube 4 has an open end 5 and at the other end of the installed plug 6. Through the cover 6 is missing from the end 2 of the inner tube 1. The outer tube 7 has an open end 8 and its other end 9 docked with the end 5 of the tube 4. Node isolation channel of the outer tube 7 from the external environment is made in the form of pump flow 10 carrier gas connected, through a pipe 11, with the intermediate tube 4. The pump flow 10 carrier gas is a container with a carrier gas under pressure, fitted with a valve for regulating the gas supply. Around the tube 7 and the tube 4 with the pipe 11 posted by device 12 heating and maintaining the temperature, vypolnennoe and power supply unit (not shown). The injector tube 13 is made in the form of thin-walled tubes (outer diameter 2 mm, wall thickness - 0.15 mm) stainless steel. Material "A", containing the sample, representing, for example, aerosol glass fiber filter or sorbent "Tenax between two wads of glass wool or the sorbent in the form of a thin layer of polydimethylsiloxane deposited on the inner wall of the tube 13, is placed near the end 14 of the tube 13. The end 14 of the tube 13 is placed in the tube 7 with a gap relative to its inner walls. The end 2 of the inner tube 1 is passed through the tube 4 and is installed inside the injector tube 13 before the material "A". The end 15 of the injector tube 13 is connected through a quick-detachable sealed connection 16 and a flexible pipe 17 (not fully shown) to the pump 18 of the flow of carrier gas or gaseous samples, representing the vessel containing the carrier gas or gaseous sample under pressure, fitted with a valve for regulating the gas supply. The ends of the injector tube 13 provided with removable plugs, PTFE (diagrams not shown), which are used to avoid prolonged contact of the sample contained in the tube 13, with the environment.

Option 2.

With the second tube 19. One end of the tube 19 is connected to the end 8 of the tube 7, through detachable sealed connection 20, made in the form of an elastic cuffs. The other end of the tube 19 is provided with a seal node 21, also made in the form of an elastic cuffs, skipped through which the end 15 of the tube 13, with the possibility of reciprocating movement of the tube 13 without depressurization of the tube 19. The tube 19 is connected by pipe 22 to the pump 23 of the gas stream, representing a valve connected to a vacuum pump (not shown) or with the environment. Around the tube 19 in the area of the site seal 21 is located, the device 24 cooling performed, for example, in the form of a heat sink with forced ventilation. At an operating pressure in the sample above ambient pressure tube 1 may be connected through the detector 3 with the environment.

The device works in the following way

Option 1.

Feed analysis is preceded by a procedure of selection, preparation and storage of samples. The gaseous sample is injected into the vessels. Aerosols from the air are selected on the filter by passing through it a certain amount of air, then put it in the injector tube 13. Pair of organic substances air volume. Organic matter from volatile solvents selected from the sorbent, which is equipped with the injector tube, by applying to it an aliquot of the solution and subsequent removal of the solvent from the adsorbent by passing through the injector tube 13 a sufficient volume of carrier gas. When storing samples of the ends of the injector tube 13 is closed with plugs. The number of injection tubes corresponds to the number of samples.

To maintain the device (Fig. 1) operable in all modes include: booster (not shown) of the gas flow (vacuum pump) connected through the detector 3 to the tube 1, which provides a continuous flow of gas from the device to the detector 3 through the open end 2 and the channel inner tube 1 with a flow rate Q1; served continuously with a flow rate Q2>Q1 carrier gas from the pump 10 into the pipe 11, the tubes 4, 7 and from the tube 7 through the end 8 into the environment, what prevents the penetration of the environment into the tube 1 through the end 8 and the tube 7. In addition, include the device 12 heating and maintaining the temperature.

In the first stage, the stage of preparation for submission of samples for analysis, the ends of the injector tube 13 is released from the stub; end 15 is connected, via a connection 16 to patrol is 17 and tube 13 gas; place the end 14 of the tube 13 (depicted by the dotted line) before the end of the 8 outside of the tube 7.

In the second stage, the stage of submitting samples for analysis, the tube 13 is rapidly injected inside the outer tube 7, the material "A" is before the end 2 of the tube 1, and a gaseous sample surrounds the end 2 of the tube 1. The end 14 of the tube 13, as a result of contact with the walls of the tube 7 and the carrier gas, and thermal radiation, is heated together with the material "A" and the breakdown. The tube 13 is held in the tube 7 within the time necessary to heat the end 14 of the tube 13 with the material "A" and feed samples with a flow of carrier gas from the tube 13 through the end 2 of the tube 1. The duration of injection of the sample into the tube 1 can be reduced by preheating the tube 13 with the sample in the tube 7 and reduce the retention time of the tube 13 in the tube 7, as well as due to increase in Q3. When Q1>Q3 sample feed tube 1 is lossless. The duration of injection of the gaseous sample may be arbitrary.

At the third stage, the stage of analysis of the sample injector tube 13 is removed from the tube 7 and turn off the pump 18 of the gas flow. Volatile components of the sample continue to move in the flow of carrier gas in the tube 1 in the direction of the detector 3. what to submit for analysis of the next sample.

Option 2.

Selection, preparation and storage of samples perform as described in the first embodiment. To maintain the device (Fig. 2) operable in all modes include: booster (not shown) of the gas flow (vacuum pump) connected through the detector 3 to the tube 1, which provides a continuous flow of gas from the device to the detector 3 through the open end 2 and the channel inner tube 1 with a flow rate Q1; served continuously with a flow rate Q2>Q1 carrier gas from the pump 10 into the pipe 11, the tubes 4, 7 and from the tube 7 through the end 8 of the tube 19, what prevents the penetration of the medium from the tube 19 into the tube 1 through the end 8 and the tube 7. In addition, include the device 12 heating and maintaining the temperature and the device 24 cooling.

In the first stage, the stage of preparation for submission of samples for analysis, the ends of the injector tube 13 is released from the plugs; plug end 15 of the tube 13 to the nozzle 17; enter the end 14 of the tube 13 (shown dashed) in the tube 19 through the node 21 and set before the end of the 8 outside of the tube 7; includes boosters 18 and 23 of the gas stream with expenses Q3 and Q4, respectively; expect some time required to fill the gas pipe 17 and the tube 13 and establish the working pressure in the tube 23 is Liz, the tube 13 is rapidly injected inside the outer tube 7, the material "A" is before the end 2 of the tube 1, and a gaseous sample surrounds the end 2 of the tube 1. The end 14 of the tube 13, is due to contact with the walls of the tube 7 and the carrier gas, and thermal radiation, is heated together with the material "A" and the breakdown. The tube 13 is held in the tube 7 within the time required for heating the end 14 of the tube 13 with the material "A" and feed samples with a flow of carrier gas from the tube 13 through the end 2 of the tube 1. When Q1>Q3 sample feed tube 1 is lossless. The duration of injection of the gaseous sample may be arbitrary. At the third stage, the stage of analysis of the sample, the end 14 of the tube 13 is removed from the tube 7 into the tube 19. The sample components continue to move in the flow of the carrier gas inside the tube 1 in the direction of the detector 3. When all components of the sample from the tube 1 will arrive at the detector 3, the end 14 of the tube 13 is removed from the tube 19 and disable the boosters 18 and 23 of the thread. Stage of the analysis is finished and the device is ready for submission to the analysis of the next sample.

New distinctive features of the prototype characteristics of the proposed device provide:

- decrease the duration of the submission of samples to 1 second or less, which is practically not this penetration of dirt into the chromatographic column of elements of the device and the environment in all modes of operation of the device, that reduces the accuracy of quantitative measurements.

Industrial applicability. The invention can be used in analytical instrumentation.

1. Device for supplying samples for gas analysis, including the inner tube, one end of which is open and the other end connected through the detector by means of motive gas flow, an intermediate tube, one end of which is open and the other end has a plug, through which is threaded open end of the inner tube, outer tube, one end of which is open and the other end connected with the open end of the intermediate tube, the heating device and the temperature control, located around the outer and intermediate tubes, injector tube with sample one end is placed in the outer tube with a gap relative to its inner walls, and the other end is placed outside the outer tube and connected through quick release tight joints and flexible pipe to the pump flow of carrier gas or gaseous samples, the node isolation channel of the outer tube from the external environment, characterized in that the end of the injector tube, placed in the outer tube made of QCD the tube, node isolation channel of the outer tube from the external environment is made in the form of a booster flow of carrier gas connected through a pipe to the intermediate pipe.

2. The device under item 1, characterized in that the node isolation channel of the outer tube from the external environment is further provided with a removable rotary tube, one end of which is connected to the open end of the outer tube by means of the detachable sealed connection and the other end has a seal Assembly through which missed the end of the injection tube located outside the outer tube with the possibility of reciprocating movement of the injector tube without the depressurization of the rotary tube, while the Gating tube is connected through a pipe to pump gas stream and around a rotary tube in the area of the site seal is a cooling device.

 

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