CN109342617B - Sample pretreatment device for gas chromatograph-mass spectrometer - Google Patents
Sample pretreatment device for gas chromatograph-mass spectrometer Download PDFInfo
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- CN109342617B CN109342617B CN201811306896.0A CN201811306896A CN109342617B CN 109342617 B CN109342617 B CN 109342617B CN 201811306896 A CN201811306896 A CN 201811306896A CN 109342617 B CN109342617 B CN 109342617B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/14—Preparation by elimination of some components
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/16—Injection
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/16—Injection
- G01N30/20—Injection using a sampling valve
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/14—Preparation by elimination of some components
- G01N2030/146—Preparation by elimination of some components using membranes
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Abstract
The invention provides a sample pretreatment device for a gas chromatograph-mass spectrometer, which comprises a box body, a first separation tube and a second separation tube, wherein the first separation tube and the second separation tube are arranged above the box body in parallel; the first separation pipe and the second separation pipe are spirally coiled, two ports of the first separation pipe are respectively connected with a first sample inlet pipe and a first sample outlet pipe, two ports of the second separation pipe are respectively connected with a second sample inlet pipe and a second sample outlet pipe, and the bottoms of the first separation pipe and the second separation pipe are both communicated with a waste discharge branch pipe; the box lateral wall is equipped with into appearance pipe and prefiltration appearance pipe, is equipped with first filter membrane and second filter membrane in the box, and the filtration pore of second filter membrane is less than the filtration pore of first filter membrane, and prefiltration appearance union coupling has the water pump, and the output of water pump is connected with the passage, and the end of passage divide into two and links to each other with first appearance pipe and second appearance pipe respectively. The method is suitable for pretreatment of different samples, and has the advantages of high pretreatment efficiency, good pretreatment effect and simple operation.
Description
Technical Field
The invention relates to a sample pretreatment device for a gas chromatograph-mass spectrometer.
Background
The gas chromatograph/mass spectrometer refers to an apparatus in which a gas chromatograph and a mass spectrometer are used in combination. Mass spectrometry can carry out effective qualitative analysis, but cannot analyze complex organic compounds; chromatography is an effective method for separating and analyzing organic compounds, and is particularly suitable for quantitative analysis of organic compounds, but qualitative analysis is difficult. Therefore, the effective combination of the two must provide a highly effective qualitative and quantitative analysis tool for chemists and biochemists to carry out complex organic compounds.
The gas chromatograph-mass spectrometer has higher requirements on the purification degree of a measured sample, if the gas chromatograph-mass spectrometer cannot contain suspended matters, heavy components, water and the like, the sample must be pretreated before entering the sample analyzer, and the sample can be injected into a sample cell of the sample analyzer only if the purification degree of the sample meets the sample introduction condition, but the gas chromatograph-mass spectrometer in the market at present cannot completely pretreat the sample, has low treatment efficiency, is difficult to operate and has a small application range.
Disclosure of Invention
The invention aims to provide a sample pretreatment device for a gas chromatograph-mass spectrometer, which is suitable for pretreatment of different samples, and has the advantages of high pretreatment efficiency, good pretreatment effect and simple operation.
The invention provides the following technical scheme:
a sample pretreatment device for a gas chromatograph-mass spectrometer comprises a box body, a first separation tube and a second separation tube, wherein the first separation tube and the second separation tube are arranged above the box body in parallel;
the first separation pipe and the second separation pipe are spirally coiled, ports at the lower part and the upper part of the first separation pipe are respectively connected with a first sample inlet pipe and a first sample outlet pipe, ports at the lower part and the upper part of the second separation pipe are respectively connected with a second sample inlet pipe and a second sample outlet pipe, and the bottoms of the first separation pipe and the second separation pipe are both communicated with a waste discharge branch pipe;
one side top of box is equipped with into appearance pipe, and the opposite side below is equipped with and just strains out appearance pipe, top-down is equipped with first filter membrane and second filter membrane in proper order in the box, first filter membrane with the second filter membrane all is equipped with evenly distributed's filtration pore, just the filtration pore of second filter membrane is than the filtration pore of first filter membrane is little, advance the appearance pipe and be located first filter membrane top, just it is located to strain out the appearance pipe second filter membrane below, it is connected with the water pump just to strain out the appearance union coupling, the output of water pump is connected with the passage, the end of passage divide into two and respectively with first appearance pipe with the second advances the appearance pipe and links to each other.
Preferably, the first filter membrane and the second filter membrane are both obliquely arranged and are inclined in the direction from the sample feeding pipe to the primary filtering sample pipe.
Preferably, the bottom of the box body is provided with a bottom plate parallel to the second filter membrane.
Preferably, a first sample injection valve is arranged on the first sample injection pipe, a second sample injection valve is arranged on the second sample injection pipe, and a sample outlet valve is arranged on the first sample outlet pipe.
Preferably, the top port of first separator tube is equipped with two branches, one branch with first appearance pipe links to each other, and another branch is connected with the back flow, the other end of back flow with the bottom port of second separator tube links to each other, the both ends of back flow all are equipped with the backward flow valve.
Preferably, the ends of the first sample outlet pipe and the second sample outlet pipe are combined to form a sample outlet header pipe.
Preferably, the ends of the waste branch pipes communicated with the first separation pipe and the second separation pipe are combined into a waste header pipe.
Preferably, a side face, far away from by the first separating tube and the second separating tube, is fixedly connected with a first side supporting rod and a second side supporting rod respectively, and the bottoms of the first side supporting rod and the second side supporting rod are fixedly connected with the top surface of the box body.
Preferably, one side face of the first separation pipe opposite to one side face of the second separation pipe is fixedly connected with a connecting plate, and the bottom of the connecting plate is fixedly connected with the top face of the box body.
The invention has the beneficial effects that:
(1) after a sample to be treated is filtered by two layers of filter membranes in a box body, primary filtration is completed; then the sample is further processed by leading the sample into the first separation pipe and the second separation pipe through a water pump, and the effect of pretreatment can be improved through double treatment.
(2) The sample after just straining rotates at first separator tube and second separator tube spiral, and under the effect of gravity, suspended solid, heavy ends, water etc. in the sample all can sink to the branch pipe that wastes discharge, and first separator tube and second separator tube can carry out further processing to the sample simultaneously, and the preliminary treatment is efficient.
(3) Different filter membranes can be selected for primary filtration according to different samples, and the application range is wide.
(4) And the water pump is started, the sample to be processed is put into the sample inlet pipe, the pretreatment of the sample can be waited for, and the operation is simple.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
fig. 1 is a schematic structural view of the present invention.
Labeled as: 1. a box body; 2. a sample inlet pipe; 3. primarily filtering out a sample tube; 4. a first filter membrane; 5. a second filter membrane; 6. a base plate; 7. a water pump; 8. a material guide pipe; 9. a first sample introduction pipe; 10. a first sample injection valve; 11. a second sample injection pipe; 12. a second sample injection valve; 13. a first separation tube; 14. a second separation tube; 15. a return pipe; 16. a reflux valve; 17. a first sample outlet pipe; 18. a sample outlet valve; 19. a second sample outlet pipe; 20. a waste discharge branch pipe; 21. a first side strut; 22. a second side support bar; 23. a connecting plate; 24. a waste header pipe.
Detailed Description
As shown in fig. 1, a sample pretreatment device for a gas chromatograph-mass spectrometer comprises a box body 1, and a first separation tube 13 and a second separation tube 14 which are arranged above the box body 1 in parallel; the first separation pipe 13 and the second separation pipe 14 are spirally coiled, ports at the lower part and the upper part of the first separation pipe 13 are respectively connected with a first sample inlet pipe 9 and a first sample outlet pipe 17, ports at the lower part and the upper part of the second separation pipe 14 are respectively connected with a second sample inlet pipe 11 and a second sample outlet pipe 19, and the tail ends of the first sample outlet pipe 17 and the second sample outlet pipe 19 are converged into a sample outlet header pipe, so that samples can be conveniently taken out and collected after pretreatment; the bottoms of the first separation pipe 13 and the second separation pipe 14 are communicated with a waste discharge branch pipe 20, and the tail ends of the waste discharge branch pipes 20 are converged into a waste discharge main pipe 24, so that the collection of substances such as suspended matters, heavy components, water and the like settled in the sample is facilitated.
One side top of box 1 is equipped with into appearance pipe 2, the opposite side below is equipped with prefiltration appearance pipe 3, top-down is equipped with first filter membrane 4 and second filter membrane 5 in proper order in the box 1, first filter membrane 4 and second filter membrane 5 all are equipped with evenly distributed's filtration pore, and the filtration pore of second filter membrane 5 is less than the filtration pore of first filter membrane 4, it is located first filter membrane 4 top to advance appearance pipe 2, prefiltration appearance pipe 3 is located second filter membrane 5 below, prefiltration appearance pipe 3 is connected with water pump 7, the output of water pump 7 is connected with passage 8, the end of passage 8 divide into two and link to each other with first appearance pipe 9 and second appearance pipe 11 respectively.
The first sample inlet pipe 9 is provided with a first sample inlet valve 10, the second sample inlet pipe 11 is provided with a second sample inlet valve 12, the first sample outlet pipe 17 is provided with a sample outlet valve 18, and the first separation pipe 13/the second separation pipe 14 can be used independently or the first separation pipe 13 and the second separation pipe 14 can be used simultaneously by controlling the opening of the first sample inlet valve 10 and the second sample inlet valve 11 so as to adapt to different sample requirements. The top port of the first separation pipe 13 is provided with two branches, one branch is connected with the first sample outlet pipe 17, the other branch is connected with the return pipe 15, the other end of the return pipe 15 is connected with the bottom port of the second separation pipe 14, and both ends of the return pipe 15 are provided with return valves 16.
A side face, far away from the first separation pipe 13 and the second separation pipe 14, is fixedly connected with a first side supporting rod 21 and a second side supporting rod 22 respectively, the bottoms of the first side supporting rod 21 and the second side supporting rod 22 are fixedly connected with the top face of the box body 1, the positions of the first separation pipe 13 and the second separation pipe 14 are fixed, and the stability and the structural strength of the device are improved. The opposite side surfaces of the first separation pipe 13 and the second separation pipe 14 are fixedly connected through the connecting plate 23, and the bottom of the connecting plate 23 is fixedly connected with the top surface of the box body 1, so that the fixing strength of the first separation pipe 13 and the second separation pipe 14 and the stability of the device can be improved.
The working principle of the invention is as follows: the sample to be processed is put into the sample inlet pipe 2, and is fully filtered by the first filter membrane 4 and the second filter membrane 5, so that part of impurities in the sample are filtered, the sample after primary filtration flows out from the primary filtration sample outlet pipe 3, and is conveyed to the first separation pipe 13 and the second separation pipe 14 through the water pump 7 and the material guide pipe 8 for further processing. When the impurities in the sample to be treated are less and rapid pretreatment is needed, closing 2 backflow valves 16, opening a first sample injection valve 10, a second sample injection valve 12 and a sample outlet valve 18, enabling the sample after primary filtration to simultaneously flow into a first separation pipe 13 and a second separation pipe 14 for spiral motion, enabling suspended matters, heavy components, water and the like in the sample to sink to a waste discharge branch pipe 20 and a waste discharge main pipe 24 to flow out under the action of gravity, and enabling the pretreated sample to flow out of a first sample outlet pipe 17 and a second sample outlet pipe 19; when the sample to be processed has more impurities and needs to be fully preprocessed, the second sample injection valve 12 and the sample outlet valve 18 are closed, the first sample injection valve 10 and the return valve 16 are opened, the primarily filtered sample enters the second separation pipe 14, flows to the lower port of the first separation pipe 13 along the return pipe 15 after being spirally moved, and flows out of the fully preprocessed sample from the first sample outlet pipe 17 after being spirally moved again.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (5)
1. A sample pretreatment device for a gas chromatograph-mass spectrometer is characterized by comprising a box body, a first separation tube and a second separation tube, wherein the first separation tube and the second separation tube are arranged above the box body in parallel;
the first separation pipe and the second separation pipe are spirally coiled, ports at the lower part and the upper part of the first separation pipe are respectively connected with a first sample inlet pipe and a first sample outlet pipe, ports at the lower part and the upper part of the second separation pipe are respectively connected with a second sample inlet pipe and a second sample outlet pipe, the bottoms of the first separation pipe and the second separation pipe are both communicated with a waste discharge branch pipe, the first sample inlet pipe is provided with a first sample inlet valve, the second sample inlet pipe is provided with a second sample inlet valve, the first sample outlet pipe is provided with a sample outlet valve, a top port of the first separation pipe is provided with two branches, one branch is connected with the first sample outlet pipe, the other branch is connected with a return pipe, the other end of the return pipe is connected with a bottom port of the second separation pipe, and two ends of the return pipe are both provided with return valves;
a sample inlet pipe is arranged above one side of the box body, a primary filtering sample outlet pipe is arranged below the other side of the box body, a first filter membrane and a second filter membrane are sequentially arranged in the box body from top to bottom, the first filter membrane and the second filter membrane are respectively provided with uniformly distributed filter holes, the filter holes of the second filter membrane are smaller than those of the first filter membrane, the sample inlet pipe is positioned above the first filter membrane, the primary filtering sample outlet pipe is positioned below the second filter membrane, the primary filtering sample outlet pipe is connected with a water pump, the output end of the water pump is connected with a guide pipe, and the tail end of the guide pipe is divided into two branches and is respectively connected with the first sample inlet pipe and the second sample inlet pipe; the first filter membrane and the second filter membrane are obliquely arranged and are inclined along the direction from the sample inlet pipe to the primary filtering sample outlet pipe; and a bottom plate parallel to the second filter membrane is arranged at the bottom of the box body.
2. The apparatus of claim 1, wherein the ends of the first sample outlet tube and the second sample outlet tube are combined to form a sample outlet manifold.
3. The apparatus of claim 1, wherein the ends of the waste branch pipes communicated with the first separation pipe and the second separation pipe are combined into a waste header pipe.
4. The gas chromatograph-mass spectrometer sample pretreatment device according to claim 1, wherein a first side supporting rod and a second side supporting rod are fixedly connected to one side surface of the first separation tube and the second separation tube away from each other, and the bottoms of the first side supporting rod and the second side supporting rod are fixedly connected to the top surface of the box body.
5. The apparatus of claim 4, wherein a side surface of the first separation tube opposite to a side surface of the second separation tube opposite to the second separation tube is fixedly connected with a connecting plate, and the bottom of the connecting plate is fixedly connected with the top surface of the box body.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811306896.0A CN109342617B (en) | 2018-11-05 | 2018-11-05 | Sample pretreatment device for gas chromatograph-mass spectrometer |
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| CN201811306896.0A CN109342617B (en) | 2018-11-05 | 2018-11-05 | Sample pretreatment device for gas chromatograph-mass spectrometer |
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| CN109342617A CN109342617A (en) | 2019-02-15 |
| CN109342617B true CN109342617B (en) | 2021-11-09 |
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| CN110455969A (en) * | 2019-08-28 | 2019-11-15 | 山东工业职业学院 | A kind of gas chromatograph-mass spectrometer sample pretreatment apparatus |
| CN112241132A (en) * | 2020-09-20 | 2021-01-19 | 杭州谱育科技发展有限公司 | Control device and method for scanning speed of quadrupole mass spectrometer |
| CN114803614B (en) * | 2022-06-20 | 2022-09-06 | 浙江恒达仪器仪表股份有限公司 | Full-automatic pretreatment device of aerosol sampling filter membrane |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0618377A (en) * | 1992-06-30 | 1994-01-25 | Shimadzu Corp | Pretreatment and injection of sample |
| WO2016082126A1 (en) * | 2014-11-26 | 2016-06-02 | 四川九章生物科技有限公司 | Device for enriching and purifying compounds and use method therefor |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN202562898U (en) * | 2012-04-17 | 2012-11-28 | 武汉钢铁(集团)公司 | Sample pretreatment device of gas chromatography and mass spectrometer |
| CN205691558U (en) * | 2016-04-21 | 2016-11-16 | 武汉华正环境检测技术有限公司 | A kind of gas chromatograph-mass spectrometer sample pretreatment apparatus |
| CN105784455B (en) * | 2016-05-16 | 2018-08-17 | 张起香 | Extract structure and liquid preprocessing device |
| CN206715435U (en) * | 2016-12-30 | 2017-12-08 | 商丘师范学院 | A kind of drawing and pulling type filter |
| CN206710392U (en) * | 2017-04-27 | 2017-12-05 | 苏州康恒检测技术有限公司 | A kind of gas chromatograph-mass spectrometer sample pretreatment apparatus |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0618377A (en) * | 1992-06-30 | 1994-01-25 | Shimadzu Corp | Pretreatment and injection of sample |
| WO2016082126A1 (en) * | 2014-11-26 | 2016-06-02 | 四川九章生物科技有限公司 | Device for enriching and purifying compounds and use method therefor |
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