CN112946308A - Sampling device integrating gas, liquid and solid sampling functions - Google Patents
Sampling device integrating gas, liquid and solid sampling functions Download PDFInfo
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- CN112946308A CN112946308A CN201911266834.6A CN201911266834A CN112946308A CN 112946308 A CN112946308 A CN 112946308A CN 201911266834 A CN201911266834 A CN 201911266834A CN 112946308 A CN112946308 A CN 112946308A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
- G01N35/10—Devices for transferring samples or any liquids to, in, or from, the analysis apparatus, e.g. suction devices, injection devices
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
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Abstract
The invention discloses a gas-collecting, liquid and solid sample-feeding function integrated sample-feeding device, which comprises a surface-passivated stainless steel liquid sample-feeding pipe, a sample-feeding chamber body, a purge gas air inlet, a purge gas stainless steel pipe, a sample-feeding screw cap, a liquid sample-feeding port, a purge gas air outlet, a heat-conducting aluminum groove block, a heat-insulating tetrafluoro sleeve, a heating rod, a temperature-sensing element, a quartz enrichment pipe, enrichment fillers and quartz cotton. After a gas sample is enriched by a quartz enrichment tube filled with fillers, taking down a sample introduction nut, inserting the sample introduction nut into the quartz enrichment tube, locking the sample introduction nut, carrying out thermal desorption and gasification, and then, allowing the gas sample to enter a detection unit through a purge gas outlet by a purge gas carrier band for detection; sampling liquid sample by using a sample injection needle and then injecting the sample from a liquid sample injection port, wherein a purge gas carrier band enters a detection unit through a purge gas outlet for detection; the solid sample is dissolved and diluted by a solvent to become liquid, the sample is injected from a liquid injection port after being sampled by a sample injection needle, and the sample enters a detection unit for detection through a purge gas outlet by a purge gas carrier band.
Description
Technical Field
The invention relates to a simple sample introduction device capable of introducing samples of gas, liquid and solid, belonging to the sample introduction technology in the analysis technology.
Background
The sample introduction technology is a precondition for ensuring whether a sample can be accurately measured, the sample introduction technology with excellent performance must ensure high accuracy and good repeatability, a sample introduction device is also stable and reliable correspondingly, the sample application has wide variation range, good sealing performance and the like. At present, the sample injection modes are mainly four, namely capillary direct sample injection, diaphragm pump collection sample injection, valve sample injection and automatic sample injector sample injection.
Capillary direct sampling is a common sampling mode in the existing small-sized mass spectrometry, and is mainly used for directly analyzing components of a gaseous sample under the atmospheric pressure condition.
The collection and sample introduction of the diaphragm pump is to pump a gaseous sample into a quantitative ring or an enrichment pipe filled with enrichment filler, and then the gaseous sample is brought into a separation or detection unit through air flow purging;
the valve sample introduction is that the sample introduction operation of sample introduction is completed by using a sample introduction valve in the column chromatography, a quantitative ring of a sample is arranged on a bypass of the sample introduction valve for conveying a gas or liquid mobile phase, and the gas or liquid sample in the quantitative ring is brought into a separation or detection unit by using the gas or liquid mobile phase through the switching of the valve;
generally, an automatic sampler comprises a sample arm, a sample needle, a sample tray, a cleaning system, a driving system, a control system, and the like, which cooperate with each other to drive the automatic sampler to operate normally. A sample injection needle is loaded on a sample injection arm, and different sample stations are uniformly distributed on a circular sample disc at different radiuses by the circle center of a rotating shaft of the circular sample disc; after the sample introduction arm and the sample tray obtain control commands and signals, coordinated sample introduction action is generated; the sample disc rotates a sample station to generate a signal, and the sample arm can suck samples after obtaining the signal, thereby ensuring that a sample needle on the sample arm can accurately suck target samples on different radiuses of the sample disc and sample in a liquid sample mode.
The on-line monitoring technology is to continuously or regularly monitor the surrounding environment or the actual sample under the condition that the analyzer is in normal operation, the object to be detected is often a plurality of samples with low-concentration gaseous state, liquid state and solid state different states discharged by the surrounding environment or pollution, and how to develop a sample injection device integrating gas, liquid and solid sample injection functions is urgent.
Disclosure of Invention
The invention discloses a gas-collecting, liquid and solid sample-feeding function integrated sample-feeding device, which comprises a surface-passivated stainless steel liquid sample-feeding pipe, a sample-feeding chamber body, a purge gas air inlet, a purge gas stainless steel pipe, a sample-feeding screw cap, a liquid sample-feeding port, a purge gas air outlet, a heat-conducting aluminum groove block, a heat-insulating tetrafluoro sleeve, a heating rod, a temperature-sensing element, a quartz enrichment pipe, enrichment fillers and quartz cotton.
The invention adopts the following specific technical scheme:
the upper side and the lower side of the heat-conducting aluminum groove block are respectively provided with a through hole, the sample introduction chamber body is sleeved in the through hole at the lower side of the heat-conducting aluminum groove block, a heating rod is placed in the through hole at the upper side of the heat-conducting aluminum groove block, and a heat-insulating polytetrafluoroethylene sleeve is sleeved outside the heat-conducting aluminum groove block; the sample introduction chamber body is a cylinder, a blind hole for accommodating a liquid sample introduction pipe is arranged on the right end face of the cylinder, a through hole is arranged on the left bottom surface of the blind hole, a sealing cap with a through hole in the middle is arranged at the right opening end, and the through hole in the middle is used as a liquid sample introduction port; a purge gas inlet is arranged in the middle of the sample injection chamber body, and a purge gas stainless steel pipe penetrates through the heat-insulating tetrafluoro sleeve and the heat-conducting aluminum groove block to be connected with the purge gas inlet; the liquid sample inlet pipe is sleeved in the blind hole of the sample inlet chamber body, the end face of the right opening of the liquid sample inlet pipe is closely attached to the sealing cap, and the left opening end of the liquid sample inlet pipe is used as a purge gas outlet and is connected with the right end of the through hole of the sample inlet chamber body. The liquid sample inlet pipe is a passivated stainless steel sample inlet pipe with a passivated inner surface, the surface passivated stainless steel liquid sample inlet pipe is a round pipe with openings at the left end and the right end, wherein a semicircular hole is formed at a position 1.5cm away from the right end port, and the hole is used for carrying a sample after the purge gas in the purge gas stainless steel pipe flows into the surface passivated stainless steel liquid sample inlet pipe through a purge gas inlet; the sample introduction chamber body is a cylinder with an external thread at the right end, a blind hole for accommodating a liquid sample introduction pipe is arranged on the right end surface of the cylinder, a through hole is arranged on the left bottom surface of the blind hole, an internal thread is arranged on the inner wall surface of the left end of the through hole, and the right end is tightly screwed with a sample introduction screw cap with an internal thread and a through hole in the middle through part through a sealing gasket; a scavenging gas inlet is arranged at the position of the sampling chamber body from the right end 1/3, and a scavenging gas stainless steel pipe is completely welded with the scavenging gas inlet through a heat-insulating tetrafluoro sleeve and a heat-conducting aluminum groove block. The surface-passivated stainless steel liquid sample inlet pipe can be inserted into the sample inlet chamber body, liquid sample is introduced from the liquid sample inlet after being sampled by the sample introduction needle, and the purge gas carrier band enters the detection unit through the purge gas outlet for detection; the solid sample is dissolved and diluted by a solvent to become liquid, the sample is injected from a liquid injection port after being sampled by a sample injection needle, and the sample enters a detection unit for detection through a purge gas outlet by a purge gas carrier band. According to the property of a sample needing to be enriched, the device also comprises a quartz enrichment tube, one or more enrichment fillers in enrichment fillers 1, enrichment fillers 2 and the like can be sequentially filled in the quartz enrichment tube along the axial direction, and quartz cotton is used for isolation among different enrichment fillers and blocking two ends; after a gas sample is subjected to off-line enrichment by adopting a quartz enrichment tube internally provided with a filler, a sample injection nut is taken down, the quartz enrichment tube enriched with the sample is inserted into a stainless steel liquid sample injection tube with a passivated surface, the sample injection nut is locked, and a purge gas carrier band enters a detection unit through a purge gas outlet after thermal desorption and gasification for detection. The heat conduction aluminum groove block respectively fixes the sample injection chamber body, the heating rod and the temperature sensing element groove through jackscrews. The heat-insulating PTFE sleeve is used for insulating heat of the heat-conducting aluminum groove block; the purging flow rate of the purging air flow is 100-1000 mL/min according to different detectors connected to the rear end. A heating rod groove for accommodating the electric heating rod and a groove for accommodating a temperature sensing element of a temperature sensor or a thermocouple are respectively arranged at the two opposite sides of the through hole of the sample introduction chamber body in the heat conduction aluminum groove block.
The invention has the advantages that:
the invention discloses a sample injection device integrating three sample injection modes of gas, liquid and solid, which is a hotspot content of research all the time, most of the sample injection modes are limited to liquid, solid and gas which can not be injected in two ways at present, and the device solves the problem of realizing the three sample injection modes of gas, liquid and solid at the same time. The device has the characteristics of low cost and simple operation.
Drawings
FIG. 1 is a schematic cross-sectional view of a sample injection device integrating gas, liquid and solid sample injection functions;
FIG. 2 is a schematic diagram of a gas sample introduction enrichment tube in a sample introduction device integrating gas, liquid and solid sample introduction functions;
in FIG. 1, 1 is a purge gas outlet; 2 is a heat-conducting aluminum groove block; 3 is a heat-insulating tetrafluoro sleeve; 4, a stainless steel liquid sampling pipe with a passivated surface; 5 is a sample introduction chamber body; 6 is a sampling screw cap; 7 is a heating rod; 8 is a temperature sensing element; 9 is a purge gas inlet; 10 is a semi-circular hole; 11 is a stainless steel tube for purging; 16 is a liquid sample inlet;
in FIG. 2, 12 is a quartz enrichment tube; 13 is enriched filler 1; 14 is quartz wool; 15 is an enrichment packing 2.
Detailed Description
The upper side and the lower side of the heat-conducting aluminum groove block are respectively provided with a through hole, the sample introduction chamber body is sleeved in the through hole at the lower side of the heat-conducting aluminum groove block, a heating rod is placed in the through hole at the upper side of the heat-conducting aluminum groove block, and a heat-insulating polytetrafluoroethylene sleeve is sleeved outside the heat-conducting aluminum groove block; the sample introduction chamber body is a cylinder, a blind hole for accommodating a liquid sample introduction pipe is arranged on the right end face of the cylinder, a through hole is arranged on the left bottom surface of the blind hole, a sealing cap with a through hole in the middle is arranged at the right opening end, and the through hole in the middle is used as a liquid sample introduction port; a purge gas inlet is arranged in the middle of the sample injection chamber body, and a purge gas stainless steel pipe penetrates through the heat-insulating tetrafluoro sleeve and the heat-conducting aluminum groove block to be connected with the purge gas inlet; the liquid sample inlet pipe is sleeved in the blind hole of the sample inlet chamber body, the end face of the right opening of the liquid sample inlet pipe is closely attached to the sealing cap, and the left opening end of the liquid sample inlet pipe is used as a purge gas outlet and is connected with the right end of the through hole of the sample inlet chamber body. The liquid sample inlet pipe is a passivated stainless steel sample inlet pipe with a passivated inner surface, the surface passivated stainless steel liquid sample inlet pipe is a round pipe with openings at the left end and the right end, wherein a semicircular hole is formed at a position 1.5cm away from the right end port, and the hole is used for carrying a sample after the purge gas in the purge gas stainless steel pipe flows into the surface passivated stainless steel liquid sample inlet pipe through a purge gas inlet; the sample introduction chamber body is a cylinder with an external thread at the right end, a blind hole for accommodating a liquid sample introduction pipe is arranged on the right end surface of the cylinder, a through hole is arranged on the left bottom surface of the blind hole, an internal thread is arranged on the inner wall surface of the left end of the through hole, and the right end is tightly screwed with a sample introduction screw cap with an internal thread and a through hole in the middle through part through a sealing gasket; a scavenging gas inlet is arranged at the position of the sampling chamber body from the right end 1/3, and a scavenging gas stainless steel pipe is completely welded with the scavenging gas inlet through a heat-insulating tetrafluoro sleeve and a heat-conducting aluminum groove block. The surface-passivated stainless steel liquid sample inlet pipe can be inserted into the sample inlet chamber body, liquid sample is introduced from the liquid sample inlet after being sampled by the sample introduction needle, and the purge gas carrier band enters the detection unit through the purge gas outlet for detection; the solid sample is dissolved and diluted by a solvent to become liquid, the sample is injected from a liquid injection port after being sampled by a sample injection needle, and the sample enters a detection unit for detection through a purge gas outlet by a purge gas carrier band. According to the property of a sample needing to be enriched, the device also comprises a quartz enrichment tube, one or more enrichment fillers in enrichment fillers 1, enrichment fillers 2 and the like can be sequentially filled in the quartz enrichment tube along the axial direction, and quartz cotton is used for isolation among different enrichment fillers and blocking two ends; after a gas sample is subjected to off-line enrichment by adopting a quartz enrichment tube internally provided with a filler, a sample injection nut is taken down, the quartz enrichment tube enriched with the sample is inserted into a stainless steel liquid sample injection tube with a passivated surface, the sample injection nut is locked, and a purge gas carrier band enters a detection unit through a purge gas outlet after thermal desorption and gasification for detection. The heat conduction aluminum groove block respectively fixes the sample injection chamber body, the heating rod and the temperature sensing element groove through jackscrews. The heat-insulating PTFE sleeve is used for insulating heat of the heat-conducting aluminum groove block; the purging flow rate of the purging air flow is 100-1000 mL/min according to different detectors connected to the rear end. A heating rod groove for accommodating the electric heating rod and a groove for accommodating a temperature sensing element of a temperature sensor or a thermocouple are respectively arranged at the two opposite sides of the through hole of the sample introduction chamber body in the heat conduction aluminum groove block.
A sampling device integrating gas, liquid and solid sampling functions has the following specific operation flow:
when the sample is 1ppm sulfur dioxide with air as balance gas, a diaphragm pump is utilized, the flow is controlled to be 0.5L/min through a flow meter, the sample is sucked into a quartz enrichment tube for enrichment for 1min, a sample introduction screw cap is opened, the quartz enrichment tube is inserted into a surface passivated stainless steel liquid sample introduction tube, a heating rod and a temperature sensing element are utilized to rapidly heat a heat conduction aluminum groove block, so that the sample introduction chamber body, the surface passivated stainless steel liquid sample introduction tube and the quartz enrichment tube are rapidly heated, the sample is heated and desorbed, and purge gas in a purge gas stainless steel tube is rapidly carried into a purge gas outlet under the carrying of the flow of 1L/min and then enters a mass spectrum detector for detection;
when the sample is 1ppm benzene with methanol as a solvent, 1ul sample is taken by using a trace sample injection needle, the sample injection chamber body is heated to 100 ℃, the trace sample injection needle is inserted into a liquid sample injection port, the sample is pushed into a stainless steel liquid sample injection pipe with a passivated surface, and the liquid sample is instantly gasified and then is rapidly carried into a gas outlet of a purge gas by the purge gas under the carrying of a flow rate of 1L/min so as to enter a mass spectrum detector for detection;
when the sample is explosive TNT, dissolving TNT in acetone to obtain 1ppm liquid, taking 1ul sample with micro sample introduction needle, heating the sample introduction chamber to 180 deg.C, inserting the micro sample introduction needle into the liquid sample introduction port, pushing the sample into the stainless steel liquid sample introduction pipe with passivated surface, instantly gasifying the liquid sample, carrying the gas with 1L/min flow, and rapidly introducing into the gas outlet of the gas, and detecting with ion mobility spectrometry detector.
Claims (8)
1. A sample introduction device integrating gas, liquid and solid sample introduction functions comprises a liquid sample introduction pipe (4), a sample introduction chamber body (5), a purge gas inlet (9), a purge gas stainless steel pipe (11), a liquid sample introduction port (16), a purge gas outlet (1), a heat conduction aluminum groove block (2) and a heat preservation tetrafluoro sleeve (3);
the upper side and the lower side of the heat conduction aluminum groove block (2) are respectively provided with a through hole, the sample introduction chamber body (5) penetrates through the through hole at the lower side of the heat conduction aluminum groove block (2), the through hole at the upper side of the heat conduction aluminum groove block (2) is used for placing a heating rod (7), and a heat preservation polytetrafluoroethylene sleeve (3) is sleeved outside the heat conduction aluminum groove block (2);
the sample introduction chamber body (5) is a cylinder, a blind hole for accommodating the liquid sample introduction pipe (4) is arranged on the right end face of the cylinder, a through hole is arranged on the left bottom surface of the blind hole, a sealing cap with a through hole in the middle is arranged at the right opening end, and the through hole in the middle is used as a liquid sample introduction port (16); a purge gas inlet (9) is arranged in the middle of the sample introduction chamber body (5), and a purge gas stainless steel pipe (11) penetrates through the heat-insulating tetrafluoro sleeve (3) and the heat-conducting aluminum groove block (2) to be connected with the purge gas inlet (9);
the liquid sample inlet pipe (4) is sleeved in the blind hole of the sample inlet chamber body (5), the end face of the right opening of the liquid sample inlet pipe is closely attached to the sealing cap, and the left opening end of the liquid sample inlet pipe is used as a purge gas outlet (1) and is connected with the right end of the through hole of the sample inlet chamber body (5).
2. The sample introduction device according to claim 1, wherein: the liquid sample inlet pipe (4) is a passivated stainless steel sample inlet pipe with a passivated inner surface, the surface passivated stainless steel liquid sample inlet pipe (4) is a round pipe with openings at the left end and the right end, wherein a semicircular hole (10) is formed at a position 1.5cm away from the right end port, and the hole is used for carrying a sample after purge gas in a purge gas stainless steel pipe (11) flows into the surface passivated stainless steel liquid sample inlet pipe (4) through a purge gas inlet (9).
3. The sample introduction device according to claim 1, wherein: the sample introduction chamber body (5) is a cylinder with external threads at the right end, a blind hole for accommodating the liquid sample introduction pipe (4) is arranged on the right end surface of the cylinder, a through hole is arranged on the bottom surface of the left side of the blind hole, internal threads are arranged on the inner wall surface of the left end of the through hole, and the right end is tightly screwed with a sample introduction screw cap (6) with an internal thread and a through hole in the middle part through a sealing gasket; a scavenging gas inlet (9) is arranged at the position of the sampling chamber body (5) far from the right end 1/3, and a scavenging stainless steel pipe (11) is completely welded with the scavenging gas inlet (9) through a heat-insulating tetrafluoro sleeve (3) and a heat-conducting aluminum groove block (2).
4. The sample introduction device according to claim 1, wherein: the surface-passivated stainless steel liquid sample inlet pipe (4) can be inserted into the sample inlet chamber body (5), the liquid sample is sampled by using a sample injection needle and then is injected from a liquid sample inlet (16), and a purge gas carrier belt enters the detection unit through a purge gas outlet (1) for detection; the solid sample is dissolved and diluted by a solvent to become liquid, the sample is sampled by a sample injection needle and then is injected from a liquid sample injection port (16), and the sample enters a detection unit for detection through a purge gas outlet (1) by a purge gas carrier band.
5. The sample introduction device according to claim 1, wherein: according to the property of a sample needing to be enriched, the device also comprises a quartz enrichment tube (12), one or more enrichment fillers in enrichment fillers 1(13), enrichment fillers 2(15) and the like can be sequentially filled in the quartz enrichment tube (12) along the axial direction, and quartz wool (14) is used for isolating different enrichment fillers and blocking two ends;
after a gas sample is offline enriched by adopting a quartz enrichment tube (12) internally provided with a filler, a sample injection nut (6) is taken down, the quartz enrichment tube (12) enriched with the sample is inserted into a stainless steel liquid sample injection tube (4) with a passivated surface, the sample injection nut is locked, and the gas sample enters a detection unit for detection through a purge gas outlet (9) by a purge gas carrier band after thermal desorption and gasification.
6. The sampling device of claim 1, which integrates gas, liquid and solid sampling functions, and is characterized in that: the heat conduction aluminum groove block (2) respectively fixes the sample introduction chamber body (5), the heating rod (7) and the temperature sensing element groove (8) through jackscrews; the heat-insulating tetrafluoro sleeve (3) is used for heat insulation of the heat-conducting aluminum groove block.
7. The sample introduction device according to claim 1, wherein: the purging flow rate of the purging air flow is 100-1000 mL/min according to different detectors connected to the rear end.
8. The sample introduction device according to claim 1, wherein: a heating rod groove of an electric heating rod (7) and a groove of a temperature sensing element (8) of which the inside is provided with a temperature sensor or a thermocouple are respectively arranged in the heat conduction aluminum groove block (2) and the two opposite sides of the through hole for accommodating the sample introduction chamber body (5).
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911266834.6A CN112946308A (en) | 2019-12-11 | 2019-12-11 | Sampling device integrating gas, liquid and solid sampling functions |
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| CN201911266834.6A CN112946308A (en) | 2019-12-11 | 2019-12-11 | Sampling device integrating gas, liquid and solid sampling functions |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114994224A (en) * | 2022-07-06 | 2022-09-02 | 核工业理化工程研究院 | Liquid sample introduction device and method for gas isotope mass spectrometer |
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2019
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| JPS61180136A (en) * | 1985-02-06 | 1986-08-12 | Mitsubishi Heavy Ind Ltd | Sample introducing device for gas chromatograph |
| CN1803252A (en) * | 2005-01-14 | 2006-07-19 | 中国科学院大连化学物理研究所 | Sample-taking adsorption tube and its hydrolyzed adsorption device |
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| CN114994224A (en) * | 2022-07-06 | 2022-09-02 | 核工业理化工程研究院 | Liquid sample introduction device and method for gas isotope mass spectrometer |
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Application publication date: 20210611 |