CN215339692U - Novel portable gas chromatography mass spectrometer - Google Patents
Novel portable gas chromatography mass spectrometer Download PDFInfo
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- CN215339692U CN215339692U CN202120604564.1U CN202120604564U CN215339692U CN 215339692 U CN215339692 U CN 215339692U CN 202120604564 U CN202120604564 U CN 202120604564U CN 215339692 U CN215339692 U CN 215339692U
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Abstract
The utility model discloses a novel portable gas chromatography-mass spectrometer which is characterized in that: the device comprises an open sample introduction unit, a chromatographic flow path and a mass spectrometer, wherein an outlet of the open sample introduction unit is connected with an inlet of the mass spectrometer through the chromatographic flow path, the chromatographic flow path comprises a six-way valve, a sampling pump, a three-way valve, a thermal desorption device and a chromatographic column, the sampling pump is connected with the six-way valve, a sample is pumped into the thermal desorption device during sampling, the six-way valve is switched and desorbed after the sampling is finished, the sample directly enters the mass spectrometer for detection after the separation of the sample, the three-way valve is connected between the sampling pump and the six-way valve and is connected with a carrier gas, the high-purity carrier gas can be reversely blown out when the sampling is finished, and the air remained in a pipeline is cleaned; the advantages are that: the flow path is simple, reduces because of risks such as gas leakage, multiple analysis cross contamination that the pipeline connecting piece is too much and leads to, makes things convenient for later maintenance, has reduced the volume of complete machine, more portable and use.
Description
Technical Field
The utility model relates to the field of gas chromatography-mass spectrometry combination, in particular to a novel portable gas chromatography-mass spectrometer.
Background
The gas chromatography-mass spectrometer is used for separating various mixed samples and then detecting the mixed samples through a mass detector, and the portable gas chromatography-mass spectrometer needs to be carried to a site to run for a certain time.
The direct sampling design of laboratory gas matter does not possess the gas sampling function for having the direct introduction port of gas tightness and reposition of redundant personnel, will realize that gas sampling needs external cold trap enrichment and thermal analysis device, and is simultaneously bulky, and the consumption is high, is unfavorable for the portable use in scene.
The portable gas chromatography flow path generally has two types, one type is an external direct sample inlet with a reduced plate, the mode is the same as a laboratory gas mode, an airtight needle is adopted for sample injection, and a carrier gas flow path is needed, so that a large amount of analysis gas is consumed, the gas cylinder is large in size, and the portability is poor. The other type is a direct sample inlet which is arranged in a flow path in the machine, a micro-extraction and direct sample introduction mode can be adopted, the flow path is complex in design, the air tightness requirement is high, the risk of whole machine pollution is high when a sample with a high boiling point enters, and the structure is complex and is not beneficial to maintenance. And the use of micro-extraction and direct liquid sample injection firstly needs to additionally carry other parts, and secondly, the two experiments need pretreatment to influence the experiment speed and cannot quickly obtain results.
After the gas instruments in the above modes are polluted by sample injection, some pollutants with low boiling points can be removed only by performing an air sample experiment or an aging experiment, and instrument components and parts need to be replaced for some residues with high boiling points, so that the experiment effect is influenced, and the maintenance cost is increased.
In summary, the internal chromatography flow path design of the conventional portable gas chromatography-mass spectrometer is designed by shrinking the laboratory-used large-scale instrument, so that the following problems exist in the small-scale portable instrument, and needs to be solved: 1) the sample introduction is assisted by carrier gas, and the maintenance is difficult after the sample introduction is polluted; 2) the complex integrated flow path leads to greater risk of airtightness in portable use and is more easily polluted by a sample for multiple times; 3) the self-cleaning function is limited after the instrument is polluted, and components and parts basically need to be replaced.
Disclosure of Invention
In order to solve the defects in the prior art, the utility model provides a novel portable gas chromatography mass spectrometer which is simple in chromatography flow path, small in size and convenient to carry.
The technical scheme adopted by the utility model for solving the technical problems is as follows: the utility model provides a novel portable gas chromatography mass spectrometer, includes uncovered appearance unit, chromatogram flow path and mass spectrometer, the export of uncovered appearance unit pass through the chromatogram flow path with mass spectrometer's access connection, the chromatogram flow path include sampling pump, six-way valve, three-way valve, thermal desorption device and chromatographic column, the a mouth of six-way valve with the access connection of uncovered appearance unit, the b mouth of six-way valve with thermal desorption device's first end be connected, the c mouth of six-way valve with chromatographic column's access connection, the outlet of chromatographic column with mass spectrometer's access connection, the d mouth and the outside carrier gas of six-way valve be connected, the e mouth of six-way valve with thermal desorption device's second end be connected, the f mouth of six-way valve with the first end of three-way valve be connected, the second end of the three-way valve is connected with the sampling pump, and the third end of the three-way valve is connected with external carrier gas.
In some embodiments, the open sample introduction unit includes an inerting sample introduction tube, a heating unit, heat-insulating cotton, an inerting adapter, and a protective sleeve, the heating unit is fixed outside the inerting sample introduction tube for heating the inerting sample introduction tube, the heat-insulating cotton is wrapped around the heating unit for heat insulation, the inerting adapter is hermetically connected to an outlet of the inerting sample introduction tube and an inlet of the chromatographic flow path, and the protective sleeve is sleeved on a sample introduction end of the inerting sample introduction tube for preventing scald. The uncovered appearance unit of advancing is convenient for clear up and maintain, uses the inertization adapter to link to each other gas circuit and instrument at the exit end of advancing the appearance pipe, and whole journey uses inertization spare part, pollution abatement.
In some embodiments, the open sample introduction unit is provided with a fixing clamp for fixing with an outer shell of the portable gas chromatography mass spectrometer. Therefore, the structure is reasonable, and the operation is convenient and fast.
In some embodiments, the third end of the three-way valve is connected with external carrier gas through a carrier gas pipeline, and a blowback damper for reducing the flow rate of the carrier gas is arranged on the carrier gas pipeline. The blowback is from clean function can be the air cleaning of residual in the pipeline, improves instrument sensitivity and pollution abatement, sets up the blowback damping on the gas circuit and can reduce carrier gas flow rate, makes the velocity of flow adjust to suitable scope, and the damped volume of blowback is less, the cost is lower, is fit for setting up in portable gas chromatography mass spectrograph's pipeline.
In some embodiments, the thermal desorption device employs an adsorption tube or a quantitative tube, and the tube diameter of the adsorption tube or the quantitative tube is smaller than that of the inerting sample injection tube. The pipe diameter of adsorption tube is less than the pipe diameter of inertization sampling tube, has better enrichment effect from this, when adopting the ration pipe, can improve the experimental speed to the higher sample of concentration.
In some embodiments, when the thermal desorption device employs an adsorption tube, the adsorption tube is a metal tube, a quartz tube or a capillary tube with a filler, and the filler employs an organic adsorbent. Thereby further enhancing the enriching effect.
In some embodiments, the inerted sample inlet tube is a metal tube or a quartz tube with a filler, and the filler is an organic adsorbent. Thereby further enhancing the enriching effect.
In some embodiments, the communication mode of the chromatography flow path specifically comprises: during sampling, the sampling pump is opened, the first end and the second end of the three-way valve are communicated, and the port a and the port b, the port c and the port d, and the port e and the port f of the six-way valve are communicated, so that air carrying samples enter the thermal desorption device for enrichment; during back flushing, the sampling pump is closed, the first end and the third end of the three-way valve are switched to be communicated, and the six-way valve is unchanged, so that carrier gas is swept from the reverse counter flow path and the thermal desorption device; and during thermal desorption, the port b and the port c, the port d and the port e, and the port f and the port a of the six-way valve are switched to be communicated, the thermal desorption device is heated and started, and a sample is desorbed from the thermal desorption device by carrier gas, enters the chromatographic column, is separated and then enters the mass spectrometer. The functions of enrichment, thermal desorption, sample injection detection and back flushing can be realized by switching the six-way valve, and the pipeline is simple and reasonable in arrangement, convenient to operate and small in occupied space.
In some embodiments, the open sample injection unit is used for injecting a sample in a manner selected from any one of a direct injection needle, solid phase microextraction, or gas joint injection.
In some embodiments, a flow controller is connected between the d port of the six-way valve and the external carrier gas, and is used for monitoring and controlling the flow rate of the carrier gas.
Compared with the prior art, the utility model has the advantages that: (1) the original chromatographic gas path is simplified on the basis of sample introduction of the open direct sample introduction unit, the whole machine flow path design can be completed only by arranging parts such as a six-way valve, a sampling pump, a three-way valve and the like, the risks of gas leakage, repeated analysis and cross contamination and the like caused by excessive pipeline connecting pieces are reduced, the later maintenance is facilitated, the size of the whole machine is reduced after the chromatographic flow path is simplified, and the whole machine is more convenient to carry and use; (2) the open direct sample introduction unit of the structure can directly drive a liquid sample into the device and then vaporize the liquid sample, and the sample is collected in the built-in thermal desorption device in a mode of collecting a gas sample through the sampling pump, so that later maintenance is facilitated; (3) compared with the traditional gas instrument, after a sample with high concentration or serious residue enters the traditional gas instrument, serious residual pollution exists in a pipeline, and the sample is difficult to remove without replacing components, the flow path back-flushing function of the design can reduce the interference of air through back flushing after sampling is finished, ensure the introduction of oxygen and water vapor in the analysis process of a mass spectrometer, simultaneously remove the cross contamination in the analysis through whole-process heating and back flushing, improve the repeatability of quantitative analysis, and play a self-cleaning function; (4) the structure can support the on-site sampling analysis of solid, liquid and gas, has wide application, less carried gas carrying capacity and convenient use.
Drawings
FIG. 1 is a schematic diagram of a piping structure of an embodiment of a novel portable gas chromatography mass spectrometer of the present invention;
FIG. 2 is a schematic diagram of a piping structure of another embodiment of the novel portable gas chromatography mass spectrometer of the utility model;
FIG. 3 is a schematic structural diagram of an open sample introduction unit in the novel portable gas chromatography-mass spectrometer.
The device comprises an open sample introduction unit 1, an inerting sample introduction pipe 11, a heating unit 12, heat preservation cotton 13, an inerting adapter 14, a protective sleeve 15, a fixing clamp 16, a chromatographic flow path 2, a sampling pump 21, a six-way valve 22, a three-way valve 23, a thermal desorption device 24, a chromatographic column 25, a carrier gas pipeline 26, a back flushing damper 27, a mass spectrometer 3, carrier gas 4 and a flow controller 5.
Detailed Description
The present invention will be described in further detail with reference to the following drawings and examples, but the present invention is not limited thereto.
Example one
As shown in the figure, the novel portable gas chromatography mass spectrometer comprises an open sample introduction unit 1, a chromatography flow path 2 and a Mass Spectrometer (MS) 3, wherein an outlet of the open sample introduction unit 1 is connected with an inlet of the mass spectrometer 3 through the chromatography flow path 2.
The chromatographic flow path 2 comprises a sampling pump 21, a six-way valve 22, a three-way valve 23, a thermal desorption device 24 and a chromatographic column 25, wherein an a port of the six-way valve 22 is connected with an outlet of the open sample injection unit 1, a b port of the six-way valve 22 is connected with a first end of the thermal desorption device 24, a c port of the six-way valve 22 is connected with an inlet of the chromatographic column 25, an outlet of the chromatographic column 25 is connected with an inlet of the mass spectrometer 3, a d port of the six-way valve 22 is connected with an external carrier gas 4, an e port of the six-way valve 22 is connected with a second end of the thermal desorption device 24, an f port of the six-way valve 22 is connected with a first end of the three-way valve 23, a second end of the three-way valve 23 is connected with the sampling pump 21, and a third end of the three-way valve 23 is connected with the external carrier gas 4.
Example two
The embodiment provides a novel portable gas chromatography mass spectrometer, which limits the specific structure of the open sample introduction unit 1 on the basis of the first embodiment. In this embodiment, the open sample introduction unit 1 includes an inerting sample introduction tube 11, a heating unit 12, heat preservation cotton 13, an inerting adapter 14, and a protective sleeve 15. The heating unit 12 is fixed outside the inerting sampling tube 11 and used for heating the inerting sampling tube, and the heat-insulating cotton 13 is made of high-temperature-resistant heat-insulating cotton and wrapped on the periphery of the heating unit 12 for heat insulation, so that the power consumption is reduced, and the inerting sampling tube can be heated to a sufficient temperature with low power. The inerting adapter 14 is hermetically connected with an outlet of the inerting sample inlet tube 11 and an inlet of the chromatographic flow path 2, and the protective sleeve 15 is sleeved on a sample inlet end of the inerting sample inlet tube 11 to prevent scalding. Because the metal tube is heated to a higher temperature, a small PEEK/PTFE protective sleeve 15 is sleeved on the open end to prevent scalding, an inerting adapter 14 is used at the other end of the metal tube to connect the gas path with the instrument, inerting parts are used in the whole process, and pollution is reduced.
In this embodiment, the inerting sample inlet tube 11 is made of 1/8 inerting metal tube or quartz tube with filler, the filler can be made of TENEX-TA, TENAX-GR or activated carbon, and in other embodiments, other combinations of fillers can be used according to different samples.
In this embodiment, the open sample introduction unit 1 is provided with a fixing clamp 16 for fixing with an outer shell of the portable gas chromatography mass spectrometer.
In this embodiment, the sample injection manner of the open sample injection unit 1 is selected from any one of a direct sample injection needle, solid phase micro-extraction, or gas joint sample injection.
EXAMPLE III
The present embodiment provides a novel portable gas chromatography-mass spectrometer, which is further supplemented with the specific structure of the chromatography flow path 2 on the basis of the first or second embodiment. In this embodiment, the third end of the three-way valve 23 is connected to the external carrier gas 4 through a carrier gas pipeline 26, and the carrier gas pipeline 26 is provided with a blowback damper 27 for reducing the flow rate of the carrier gas.
In this embodiment, the thermal desorption device 24 employs an adsorption tube, and the tube diameter of the adsorption tube is smaller than that of the inerting sample injection tube. The adsorption tube is a metal tube, a quartz tube or a capillary tube with a filler, and the filler can be TENEX-TA, TENAX-GR or activated carbon. In other embodiments, the thermal desorption device 24 may be a quantitative tube without filler, which may increase the experiment speed for samples with higher concentration.
Example four
The present embodiment provides a novel portable gas chromatograph-mass spectrometer, which is based on the above embodiments and describes in detail the communication manner of the chromatograph flow path 2. In this embodiment, during sampling, the sampling pump 21 is turned on, the first end a and the second end B of the three-way valve 23 are communicated, and the port a and the port B, the port c and the port d, and the port e and the port f of the six-way valve 22 are communicated, so that the air-carried sample enters the thermal desorption device 24 for enrichment; during back flushing, the sampling pump 21 is closed, the first end A and the third end C of the switching three-way valve 23 are communicated, and the six-way valve 22 is kept unchanged, so that the carrier gas is blown and swept from the reverse counter flow path and the thermal desorption device 24; during thermal desorption, the port b and the port c, the port d and the port e, and the port f and the port a of the six-way valve 22 are switched to be communicated, the thermal desorption device 24 is heated and started, and a sample is desorbed from the thermal desorption device 24 by carrier gas, enters the chromatographic column 25, is separated, and then enters the mass spectrometer 3.
In this embodiment, a flow controller 5 is further connected between the d port of the six-way valve 22 and the external carrier gas 4, and is used for monitoring and controlling the flow rate of the carrier gas.
The utility model relates to a novel portable gas chromatography-mass spectrometer, which has the following working principle:
a first stage: a sampling device such as a needle is used, a sample is injected into the inerting sample inlet pipe 11 from an opening, a filler in the pipe can adsorb the sample, the sample is rapidly heated by the heating unit 12 to be desorbed for primary separation, the sample is sent into the cooled thermal desorption device 24 for enrichment by starting the sampling pump 21, the sampling pump 21 is used for enabling the air carrying the sample to enter the thermal desorption device 24 for enrichment due to the fact that the sampling mode is opened, and the filler of the thermal desorption device 24 basically does not adsorb the air; and then, a small amount of high-purity carrier gas 4 is used for purging the sampling pipeline by switching a three-way valve 23 with a back flushing function, so that air remained in the pipeline and a thermal desorption device 24 is discharged, air interference is reduced, the sensitivity of the instrument is improved, and pollution is reduced.
And a second stage: after the sample is enriched, the six-way valve 22 is switched to switch the thermal desorption device 24 from the sampling gas circuit to the high vacuum detection gas circuit, wherein the desorption tube in the thermal desorption device can play a better enrichment and separation role by using a capillary desorption tube smaller than the first stage, and the sample is desorbed to be separated to the second stage through rapid temperature rise.
And a third stage: the thermal desorption device 24 sends the desorbed sample to the LTM chromatographic column 25, then the temperature of the chromatographic column 25 is linearly raised by program control, and the sample enters the mass spectrometer after the third-stage separation.
Wherein, the adsorption tube of the first stage can be selected not to be added with filler and can be only used as a liquid sample vaporizing chamber.
The adsorption tube in the second-stage thermal desorption device can be replaced by a quantitative tube without filler, and the experimental speed of samples with higher concentration can be increased when the quantitative tube is used as a high-concentration sample.
It should be noted that the above-mentioned embodiments are only preferred embodiments of the present invention, and the scope of the present invention is not limited thereby, and the present invention may be modified in materials and structures, or replaced with technical equivalents, in the constructions of the above-mentioned various components. Therefore, structural equivalents made by using the description and drawings of the present invention or by directly or indirectly applying to other related arts are also encompassed within the scope of the present invention.
Claims (10)
1. The utility model provides a novel portable gas chromatography mass spectrometer, its characterized in that includes uncovered introduction of sample unit, chromatogram flow path and mass spectrometer, the export of uncovered introduction of sample unit pass through the chromatogram flow path with mass spectrometer's access connection, the chromatogram flow path include sampling pump, six-way valve, three-way valve, thermal desorption device and chromatographic column, the a mouth of six-way valve with the access connection of uncovered introduction of sample unit, the b mouth of six-way valve with thermal desorption device's first end be connected, the c mouth of six-way valve with the access connection of chromatographic column, the export of chromatographic column with mass spectrometer's access connection, the d mouth and the outside carrier gas of six-way valve be connected, the e mouth of six-way valve with thermal desorption device's second end be connected, the f mouth of six-way valve with the first end of three-way valve be connected, the second end of the three-way valve is connected with the sampling pump, and the third end of the three-way valve is connected with external carrier gas.
2. The novel portable gas chromatography-mass spectrometer as claimed in claim 1, wherein the open sample introduction unit comprises an inerting sample introduction pipe, a heating unit, heat-insulating cotton, an inerting adapter and a protective sleeve, the heating unit is fixed outside the inerting sample introduction pipe and used for heating the inerting sample introduction pipe, the heat-insulating cotton is wrapped on the periphery of the heating unit and used for preserving heat, the inerting adapter is connected with the outlet of the inerting sample introduction pipe and the inlet of the chromatographic flow path in an airtight manner, and the protective sleeve is sleeved on the sample introduction end of the inerting sample introduction pipe and used for preventing scald.
3. The novel portable gas chromatography-mass spectrometer as claimed in claim 2, wherein the open sample introduction unit is provided with a fixing clamp for fixing with an outer shell of the portable gas chromatography-mass spectrometer.
4. The novel portable gas chromatography-mass spectrometer as claimed in claim 1, wherein the third end of the three-way valve is connected with external carrier gas through a carrier gas pipeline, and a back-blowing damper for reducing the flow rate of the carrier gas is arranged on the carrier gas pipeline.
5. The novel portable gas chromatography-mass spectrometer as claimed in claim 1, wherein the thermal desorption device is an adsorption tube or a quantitative tube, and the diameter of the adsorption tube or the quantitative tube is smaller than that of the inerting sample introduction tube.
6. The novel portable gas chromatography-mass spectrometer as claimed in claim 5, wherein when the thermal desorption device employs an adsorption tube, the adsorption tube is a metal tube, a quartz tube or a capillary tube with a filler, and the filler employs an organic adsorbent.
7. The novel portable gas chromatograph-mass spectrometer as recited in claim 2, wherein the inerting sample inlet tube is a metal tube or a quartz tube with a filler, and the filler is an organic adsorbent.
8. The novel portable gas chromatography mass spectrometer as claimed in claim 1, wherein the communication mode of the chromatography flow path specifically comprises: during sampling, the sampling pump is opened, the first end and the second end of the three-way valve are communicated, and the port a and the port b, the port c and the port d, and the port e and the port f of the six-way valve are communicated, so that air carrying samples enter the thermal desorption device for enrichment; during back flushing, the sampling pump is closed, the first end and the third end of the three-way valve are switched to be communicated, and the six-way valve is unchanged, so that carrier gas is swept from the reverse counter flow path and the thermal desorption device; and during thermal desorption, the port b and the port c, the port d and the port e, and the port f and the port a of the six-way valve are switched to be communicated, the thermal desorption device is heated and started, and a sample is desorbed from the thermal desorption device by carrier gas, enters the chromatographic column, is separated and then enters the mass spectrometer.
9. The novel portable gas chromatography-mass spectrometer as claimed in claim 2, wherein the open sample introduction unit is used in a sample introduction manner selected from any one of direct sample introduction needle, solid phase micro extraction or gas joint sample introduction.
10. The portable mass spectrometer as claimed in claim 1, wherein a flow controller is connected between the d port of the six-way valve and the external carrier gas for monitoring and controlling the flow rate of the carrier gas.
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| CN202120604564.1U CN215339692U (en) | 2021-03-25 | 2021-03-25 | Novel portable gas chromatography mass spectrometer |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114965737A (en) * | 2022-04-14 | 2022-08-30 | 北京佳分分析仪器技术有限公司 | Thermal cracking chromatographic analysis and detection method and device |
| CN115144493A (en) * | 2022-06-27 | 2022-10-04 | 山东光测环境科技有限公司 | Gas circuit structure of on-line monitoring analyzer |
| CN118837502A (en) * | 2024-07-30 | 2024-10-25 | 重庆黄嘉生物技术有限公司 | Chromatographic column incubator capable of being switched rapidly and switching method |
| WO2024250835A1 (en) * | 2023-06-06 | 2024-12-12 | 苏州智爱环境科技有限公司 | Online organic aerosol thermal desorption gas chromatography-mass spectrometry analysis system and method |
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2021
- 2021-03-25 CN CN202120604564.1U patent/CN215339692U/en active Active
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114965737A (en) * | 2022-04-14 | 2022-08-30 | 北京佳分分析仪器技术有限公司 | Thermal cracking chromatographic analysis and detection method and device |
| CN115144493A (en) * | 2022-06-27 | 2022-10-04 | 山东光测环境科技有限公司 | Gas circuit structure of on-line monitoring analyzer |
| WO2024250835A1 (en) * | 2023-06-06 | 2024-12-12 | 苏州智爱环境科技有限公司 | Online organic aerosol thermal desorption gas chromatography-mass spectrometry analysis system and method |
| CN118837502A (en) * | 2024-07-30 | 2024-10-25 | 重庆黄嘉生物技术有限公司 | Chromatographic column incubator capable of being switched rapidly and switching method |
| CN118837502B (en) * | 2024-07-30 | 2025-01-03 | 重庆黄嘉生物技术有限公司 | A fast-switching chromatographic column thermostat and switching method |
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