CN115483087B - Gas sample feeding and sampling method capable of adjusting wide-pressure-variation accurate sample feeding - Google Patents
Gas sample feeding and sampling method capable of adjusting wide-pressure-variation accurate sample feeding Download PDFInfo
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- CN115483087B CN115483087B CN202211108605.3A CN202211108605A CN115483087B CN 115483087 B CN115483087 B CN 115483087B CN 202211108605 A CN202211108605 A CN 202211108605A CN 115483087 B CN115483087 B CN 115483087B
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- 238000005070 sampling Methods 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 title claims abstract description 13
- 238000002347 injection Methods 0.000 claims abstract description 79
- 239000007924 injection Substances 0.000 claims abstract description 79
- 238000001514 detection method Methods 0.000 claims abstract description 15
- 230000035484 reaction time Effects 0.000 claims abstract description 6
- 238000001819 mass spectrum Methods 0.000 claims description 23
- 238000005086 pumping Methods 0.000 claims description 9
- 230000006837 decompression Effects 0.000 claims description 8
- 238000005202 decontamination Methods 0.000 claims description 7
- 230000003588 decontaminative effect Effects 0.000 claims description 7
- 230000001105 regulatory effect Effects 0.000 claims description 6
- 238000004401 flow injection analysis Methods 0.000 claims description 3
- 230000009467 reduction Effects 0.000 claims description 2
- 239000007789 gas Substances 0.000 abstract description 68
- 238000012360 testing method Methods 0.000 abstract description 9
- 230000035945 sensitivity Effects 0.000 abstract description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 3
- 238000013461 design Methods 0.000 abstract description 3
- 238000007664 blowing Methods 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 abstract description 2
- 238000005201 scrubbing Methods 0.000 abstract 5
- 229910001873 dinitrogen Inorganic materials 0.000 abstract 1
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 231100000331 toxic Toxicity 0.000 description 3
- 230000002588 toxic effect Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 150000002222 fluorine compounds Chemical class 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 231100000206 health hazard Toxicity 0.000 description 1
- 238000004949 mass spectrometry Methods 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/0027—Methods for using particle spectrometers
- H01J49/0031—Step by step routines describing the use of the apparatus
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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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/04—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components
- H01J49/0422—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components for gaseous samples
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Physics & Mathematics (AREA)
- Electrochemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Electron Tubes For Measurement (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses a gas sample feeding and sampling method capable of adjusting wide-pressure-variation accurate sample feeding, which is applied to a sample feeding system of a gas mass spectrometer and realizes the functions of directly sampling a gas sample from the atmosphere and reducing pressure to working pressure. In the invention, a wide variable pressure adjusting range can be realized through the micro-adjusting valve, and the test environment pressure can be from vacuum to one atmosphere; the sample injection valve with the sample injection pipe and the micropores can enable the gas sample to accurately enter the ionization region of the ionization source, so that the sample ionization rate, the gas sample utilization rate and the detection sensitivity are improved; the design of scrubbing valve can realize the quick scrubbing function of residual gas sample, if cooperate nitrogen gas blowing and advance the heating of appearance pipeline, can more fully realize equipment scrubbing, reduce test interference, improve the detection accuracy, use the combination of fine setting valve and scrubbing valve, realized accurate regulation gas sample introduction volume, the design of reposition of redundant personnel simultaneously can shorten detection reaction time, and quick scrubbing function has reduced the detection influence that residual gas brought.
Description
Technical Field
The invention relates to the technical field of gas sample feeding and sampling methods, in particular to a gas sample feeding and sampling method capable of adjusting wide-pressure-variation accurate sample feeding.
Background
There are many enclosed spaces in the working environment, and various harmful gases exist in the environments of the enclosed spaces, for example, human metabolism, degassing of nonmetallic materials, pyrolysis of materials, accidental leakage, running of equipment and the like, and harmful gases are generated. These hazardous gases can present a health hazard to personnel in the enclosed space, even if some toxic gases directly endanger the life safety of the personnel. Therefore, test instruments for monitoring toxic and harmful gases, especially benzene substances, fluorides, chlorides and other substances, are arranged in the working environment of the closed space.
The equipment for monitoring the toxic and harmful gas mainly comprises a mass spectrometer, and the type and the concentration of the toxic and harmful gas are monitored in real time by means of mass spectrometry. The working pressure required by the gas mass spectrometer is generally 1×10 -5Pa～1×10-2 Pa, so that a special sample inlet and sampling system needs to be developed, and the gas sample can be directly sampled from the atmospheric pressure environment, and the gas sample entering the test chamber can not cause pressure fluctuation through a series of measures of diversion and decompression. Meanwhile, in order to adapt to different detection environments and higher detection sensitivity, the sample feeding and taking system also needs to have the functions of adjustable gas sample feeding amount, wider pressure change range, accurate sample feeding and the like.
Disclosure of Invention
The invention aims at: in order to solve the problems, a gas sample feeding and sampling method capable of adjusting wide-pressure-variation accurate sample feeding is provided.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
A gas sample feeding and sampling method capable of adjusting wide-pressure and accurate feeding comprises the following steps:
s1: the flow rate range and the inner diameter size of the fine tuning valve are selected appropriately, the larger the opening of the fine tuning valve is, the more the flow is divided, the lower the pressure at the outlet of the capillary tube is, the about 1000Pa is, namely the inlet pressure of the fine tuning valve is obtained, and the flow conductance value of the fine tuning valve in the full-open state can be calculated by combining the pumping speed of the flow dividing pump and the extreme vacuum value, so that the flow rate range and the inner diameter size of the fine tuning valve are determined;
S2: the method comprises the steps of selecting proper inner diameter and length of a capillary, wherein the capillary is a gas sample inlet, inlet pressure is atmospheric pressure, outlet pressure is 1000 Pa-10000 Pa, calculating conductance of the capillary by combining with inlet pumping speed of a fine tuning valve, and determining the inner diameter and length of the capillary according to a calculation formula of conductance of a long straight-through pipe;
S3: selecting proper diameter and thickness of the current-limiting micropore, wherein the air inlet end of the current-limiting micropore is the air outlet end of the capillary, and the pressure is 1000 Pa-10000 Pa; the gas outlet end of the flow-limiting micropore is a mass spectrum chamber; according to the pumping speed of a main pump group of the gas mass spectrometer and the pressure difference between two ends of the flow-limiting micropore, the conductance of the flow-limiting micropore can be calculated; combining with a circular section long tube model of the current-limiting micropore, and calculating to obtain the diameter and thickness of the current-limiting micropore;
s4: the sample injection valve is arranged, and consists of the flow-limiting micropore, the electromagnetic valve and the sample injection pipe, and according to the pipe diameter of the sample injection pipe, the mass spectrometer is provided with an interface with the same caliber, and the sample injection pipe is arranged to extend from the interface to the ionization region of the ionization source, so that the accurate sample injection of the sample injection gas sample is facilitated, and the gas sample can be fully ionized;
S5: the gas sample injection quantity is regulated by adopting three decompression modes of capillary injection, pump set diversion and micropore flow limiting, and under the condition of ensuring gas small-flow injection, the rapid detection reaction time and the wide regulation pressure range can be still maintained;
s6: and the residual gas sample in the sample injection pipeline can be rapidly removed by opening the decontamination valve.
Preferably, the capillary tube in the capillary sample injection adopts a capillary tube with the inner diameter not exceeding 0.5 millimeter and the length of the meter magnitude, and the sample injection amount of the gas sample is sufficiently reduced by reducing the conductance, so that the purpose of first-stage decompression is achieved.
Preferably, the pump group split flow adopts a mechanical pump group and a fine tuning valve to realize the split flow, and the split flow gas quantity is adjusted by adjusting the opening of the fine tuning valve, so that the gas quantity entering the mass spectrum chamber and the vacuum pressure in the mass spectrum chamber are adjusted.
Preferably, the sample inlet of the mass spectrum chamber in the micropore flow-limiting adopts a micron-sized flow-limiting micropore, a gas sample enters the mass spectrum chamber from the flow-limiting micropore after the pressure reduction measures of the front two weights, and the pressure required to maintain the working in the mass spectrum chamber is achieved through flow limitation.
In summary, due to the adoption of the technical scheme, the beneficial effects of the invention are as follows:
1. The gas mass spectrometer can be suitable for a wide sampling pressure range and a testing environment from vacuum pressure to atmospheric pressure through multiple decompression and diversion measures;
2. According to the application, the high-precision fine tuning valve is adopted to effectively control the sample injection split ratio of the gas sample, accurately adjust the sample injection pressure, control the sample injection quantity of the gas sample, improve the accuracy of pressure control in a mass spectrum chamber, effectively shorten the reaction time of mass spectrometer detection under the split action, and rapidly remove the residual gas sample through the decontamination valve, thereby reducing the test interference;
3. according to the application, the sample injection valve is optimally designed, the sample injection position of the gas sample is effectively controlled by adopting a sample injection pipe mode, the ionization efficiency of the gas sample is improved, and the detection sensitivity of the gas mass spectrometer is further improved.
Drawings
FIG. 1 illustrates a schematic diagram of an in-sample sampling system provided in accordance with an embodiment of the present invention;
Fig. 2 is a schematic perspective view of a sample injection valve according to an embodiment of the present invention;
Fig. 3 shows a front view of a sample injection valve structure according to an embodiment of the present invention.
Legend description:
1. A sample injection valve port I; 2. a sample injection valve port II; 3. and (5) feeding a sample tube.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Referring to fig. 1-3, the present invention provides a technical solution:
A gas sample feeding and sampling method capable of adjusting wide-pressure and accurate feeding comprises the following steps:
s1: the flow rate range and the inner diameter size of the fine tuning valve are selected appropriately, the larger the opening of the fine tuning valve is, the more the flow is divided, the lower the pressure at the outlet of the capillary tube is, the about 1000Pa is, namely the inlet pressure of the fine tuning valve is obtained, and the flow conductance value of the fine tuning valve in the full-open state can be calculated by combining the pumping speed of the flow dividing pump and the extreme vacuum value, so that the flow rate range and the inner diameter size of the fine tuning valve are determined;
S2: the method comprises the steps of selecting proper inner diameter and length of a capillary, wherein the capillary is a gas sample inlet, inlet pressure is atmospheric pressure, outlet pressure is between 1000Pa and 10000Pa, calculating the conductance of the capillary by combining the inlet pumping speed of a fine tuning valve, and determining the inner diameter and length of the capillary according to a calculation formula of the conductance of a long straight-through pipe, wherein the inner diameter of the capillary is about 0.2 millimeter, and the length of the capillary is about meter;
S3: selecting proper diameter and thickness of the current-limiting micropore, wherein the air inlet end of the current-limiting micropore is the air outlet end of the capillary, and the pressure is 1000 Pa-10000 Pa; the gas outlet end of the flow-limiting micropore is a mass spectrum chamber, and the pressure is about 10 -3 Pa; according to the pumping speed of a main pump group of the gas mass spectrometer and the pressure difference between two ends of the flow-limiting micropore, the conductance of the flow-limiting micropore can be calculated; the diameter and thickness of the current-limiting micropore can be calculated by combining a circular section long tube model of the current-limiting micropore, and the aperture of the current-limiting micropore is generally between 10 and 100 mu m;
S4: the sample injection valve is arranged, the sample injection valve consists of a flow limiting micropore, an electromagnetic valve and a sample injection pipe 3, an interface with the same caliber is reserved on the mass spectrometer according to the pipe diameter of the sample injection pipe 3, the sample injection pipe 3 is arranged to extend from the interface to the ionization region position of the ionization source, the accurate sample injection of a sample injection gas sample is facilitated, the gas sample can be fully ionized, the utilization rate of the gas sample is improved, and the detection sensitivity of the gas mass spectrometer is further improved;
S5: the gas sample injection quantity is regulated by adopting three decompression modes of capillary injection, pump set diversion and micropore flow limiting, under the condition of ensuring gas small-flow injection, the rapid detection reaction time and the wide regulation pressure range can be still maintained, the diversion quantity of the gas sample is regulated by regulating the opening of a fine tuning valve, the larger the opening of the fine tuning valve is, the more the diversion quantity is, the less the gas sample quantity enters a mass spectrum chamber is, and the accurate sample injection quantity regulation can be carried out by the pressure value of a low vacuum gauge;
S6: during the test interval of different gas samples, the capillary, the sample injection pipe 3 and the mass spectrum chamber are required to be fully cleaned, the interference influence of residual gas samples on the test is avoided, the residual gas samples in the capillary and the sample injection pipe 3 can be rapidly pumped out by opening the decontamination valve, the influence of residual substances can be more rapidly and fully removed if the nitrogen is matched for blowing out and heating the sample injection pipe 3, particularly, the liquefiable gas samples are realized, the equipment decontamination is realized, the test interference is reduced, and the detection accuracy is improved.
Specifically, as shown in fig. 1, fig. 2 and fig. 3, the capillary tube in capillary sample injection adopts a capillary tube with the inner diameter not exceeding 0.5 millimeter and the length of meter magnitude, the sample injection amount of the gas sample is sufficiently reduced by reducing the conductance, the purpose of first-stage decompression is achieved, the pump group is shunted by adopting a mechanical pump group and a fine tuning valve to realize the purpose of shunting, the fine tuning valve is a continuously adjustable flow control valve, the amount of shunted gas is adjusted by adjusting the opening of the fine tuning valve, and then the amount of gas entering a mass spectrum chamber and the vacuum pressure in the mass spectrum chamber are adjusted, so that the device is suitable for different use environments; the combination of the fine tuning valve and the decontamination valve is used, so that the gas sample injection amount is accurately regulated, the accuracy of quantitative analysis of the gas mass spectrometer is increased, meanwhile, the detection reaction time can be shortened due to the design of flow division, and the detection influence caused by residual gas is reduced due to the rapid decontamination function.
As shown in fig. 2 and 3, the sample injection valve is mainly used for controlling a small dose of gas sample to accurately enter the mass spectrum chamber and directly reach an ionization source ionization region of the mass spectrometer, so that the ionization efficiency of the gas sample is improved; the sample injection valve is a three-position two-way valve seat, a flow-limiting micropore with a micron-order aperture is arranged in the valve seat, the flow-limiting micropore and the valve seat are sealed by the sample inlet pipe 3, then a coil and a valve core of a standard electromagnetic valve are arranged on the valve seat to form the sample injection valve, and the flow-limiting micropore can be designed and replaced according to actual requirements, so that the applicability is enhanced.
As shown in fig. 2 and 3, the first sample injection valve port 1 and the second sample injection valve port 2 are in a normally-open state, the opening and closing of the sample injection pipe 3 are controlled by an electromagnetic valve, the sample injection valve is arranged at the sample injection end of the mass spectrum chamber, the sample injection pipe 3 is directly arranged in an ion source ionization region of the mass spectrometer, the sample injection pipe 3 is opened in the power-on state of the sample injection valve, a gas sample enters the mass spectrum chamber through the sample injection pipe 3, the sample injection pipe 3 is closed in the power-off state of the sample injection valve, and the gas sample flows between the first sample injection valve port 1 and the second sample injection valve port 2.
The previous description of the embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (2)
1. A gas sample feeding and sampling method capable of adjusting wide-pressure and accurate feeding is characterized by comprising the following steps:
s1: the flow rate range and the inner diameter size of the fine tuning valve are selected appropriately, the larger the opening of the fine tuning valve is, the more the flow is divided, the lower the pressure at the outlet of the capillary tube is, the about 1000Pa is, namely the inlet pressure of the fine tuning valve is obtained, and the flow conductance value of the fine tuning valve in the full-open state can be calculated by combining the pumping speed of the flow dividing pump and the extreme vacuum value, so that the flow rate range and the inner diameter size of the fine tuning valve are determined;
S2: the method comprises the steps of selecting proper inner diameter and length of a capillary, wherein the capillary is a gas sample inlet, inlet pressure is atmospheric pressure, outlet pressure is 1000 Pa-10000 Pa, calculating conductance of the capillary by combining inlet pumping speed of a fine tuning valve, and determining the inner diameter and length of the capillary according to a calculation formula of conductance of a long straight-through pipe;
S3: selecting proper diameter and thickness of the current-limiting micropore, wherein the air inlet end of the current-limiting micropore is the air outlet end of the capillary, and the pressure is 1000 Pa-10000 Pa; the gas outlet end of the flow-limiting micropore is a mass spectrum chamber; according to the pumping speed of a main pump group of the gas mass spectrometer and the pressure difference between two ends of the flow-limiting micropore, the conductance of the flow-limiting micropore can be calculated; combining with a circular section long tube model of the current-limiting micropore, and calculating to obtain the diameter and thickness of the current-limiting micropore;
s4: the sample injection valve is arranged, and consists of the flow-limiting micropore, the electromagnetic valve and the sample injection pipe, and according to the pipe diameter of the sample injection pipe, the mass spectrometer is provided with an interface with the same caliber, and the sample injection pipe is arranged to extend from the interface to the ionization region of the ionization source, so that the accurate sample injection of the sample injection gas sample is facilitated, and the gas sample can be fully ionized;
S5: the gas sample injection quantity is regulated by adopting three decompression modes of capillary injection, pump set diversion and micropore flow limiting, and under the condition of ensuring gas small-flow injection, the rapid detection reaction time and the wide regulation pressure range can be still maintained;
S6: the residual gas sample in the sample injection pipeline can be rapidly removed by opening the decontamination valve;
The pump group split flow adopts a mechanical pump group and a fine tuning valve to realize the split flow, and the split flow gas quantity is adjusted by adjusting the opening of the fine tuning valve, so that the gas quantity entering a mass spectrum chamber and the vacuum pressure in the mass spectrum chamber are adjusted;
The sample inlet of the mass spectrum chamber in the micropore flow-limiting is provided with a micron-sized flow-limiting micropore, a gas sample enters the mass spectrum chamber from the flow-limiting micropore after the pressure reduction measures of the front two weights, and the pressure required to work in the mass spectrum chamber is maintained through flow limitation;
The sample injection valve is a three-position two-way valve seat, a flow-limiting micropore with a micron-sized aperture is arranged in the valve seat, the flow-limiting micropore and the valve seat are sealed by a sample inlet pipe, and then a coil and a valve core of the standard electromagnetic valve are arranged on the valve seat to form the sample injection valve;
The first sample injection valve port and the second sample injection valve port are in a normally-on state, the opening and closing of the sample injection pipe are controlled by an electromagnetic valve, the sample injection valve is arranged at the sample injection end of the mass spectrum chamber, the sample injection pipe is directly arranged in an ionization region of an ion source of the mass spectrometer, the sample injection pipe is opened in an electrified state of the sample injection valve, a gas sample enters the mass spectrum chamber through the sample injection pipe, the sample injection pipe is closed in a power-off state of the sample injection valve, and the gas sample circulates between the first sample injection valve port and the second sample injection valve port.
2. The method for sampling gas samples by adjustable wide-pressure-variation accurate sampling according to claim 1, wherein the capillary tube in the capillary sampling adopts a capillary tube with an inner diameter not more than 0.5 mm and a length of m-order, and the sampling amount of the gas samples is sufficiently reduced by reducing the conductance, so that the purpose of first-stage decompression is achieved.
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| CN202211108605.3A CN115483087B (en) | 2022-09-13 | 2022-09-13 | Gas sample feeding and sampling method capable of adjusting wide-pressure-variation accurate sample feeding |
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| CN208208713U (en) * | 2018-06-19 | 2018-12-07 | 中国科学院光电研究院 | A kind of detection device of high-precision mass spectrum detection limit |
| CN210014951U (en) * | 2019-03-14 | 2020-02-04 | 四川宏胜杰机电设备有限公司 | Multifunctional sample gas distribution and sample introduction system |
| CN112782264B (en) * | 2020-12-14 | 2023-10-24 | 兰州空间技术物理研究所 | Device and method for detecting and calibrating trace harmful gas in closed space |
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| 基于飞行时间质谱计的微型气体分析仪技术研究;韩琰 等;真空与低温;20201116;第27卷(第2期);第127-131页 * |
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