CN103529152A - Self-feedback gasometry device based on mass spectrometer and application method thereof - Google Patents
Self-feedback gasometry device based on mass spectrometer and application method thereof Download PDFInfo
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- CN103529152A CN103529152A CN201310482967.3A CN201310482967A CN103529152A CN 103529152 A CN103529152 A CN 103529152A CN 201310482967 A CN201310482967 A CN 201310482967A CN 103529152 A CN103529152 A CN 103529152A
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Abstract
The invention discloses a self-feedback gasometry device based on a mass spectrometer and an application method thereof. The self-feedback gasometry device comprises a mass spectrometer, a control system, a gas distribution system, a pressure controller, a gas extractor, at least one control valve and at least one sample inlet, wherein the gas extractor is connected with the pressure controller through a connecting pipe; the gas distribution system and the sample inlet are respectively connected with the control valve through a connecting pipe; the control valve and the pressure controller are connected with the mass spectrometer through a first three-way joint; the mass spectrometer, the gas distribution system, the control valve and the pressure controller are respectively and electrically connected with the control system. The self-feedback gasometry device based on the mass spectrometer is simple and easy to operate, small in occupation space, convenient in maintenance, low in operation cost and wide in market prospect.
Description
Technical field
The present invention relates to one based on mass spectrometric gasometry device and using method thereof, be specifically related to gasometry device and the using method thereof of a kind of pressure based on mass spectrometer and the calibration of concentration THE DYNAMIC SELF-FEEDBACK.
Background technology
Gas analysis is significant to safety in production, process optimization, quality control and energy-saving and emission-reduction etc. with detection.A kind of as on-line analysis; mass spectrometry is by the mensuration of sample ion mass-to-charge ratio being analyzed to a kind of analytical approach of its composition; there is fast response time, measuring accuracy is high, range ability is wide, good stability, can carry out polycomponent detection simultaneously, can do the advantages such as qualitative and quantitative analysis, its application has related to petrochemical complex, Ferrous Metallurgy, bio-pharmaceuticals, new forms of energy and environmental protection etc.Mass spectrometer generally all requires to work under high vacuum, and gas analysis object much all can be with more high pressure operation, between mass spectrometer and analytic target, need the docking of suitable pressure buffer Interface realization, kapillary is a kind of conventional pressure buffer interface, there is cheapness, gas consumption is little, be easy to the advantages such as realization, but, because the complicacy of interface fluidised form can cause non-linear between pressure-response, the difference of background gas and the phase mutual interference meeting between gas cause departing from of concentration-response linear relation, thereby affected mass spectrometer quantitative result accurately and reliably, be not suitable for complex state sample analysis.
Summary of the invention
The present invention has overcome the deficiencies in the prior art, provide a kind of based on mass spectrometric self feed back gasometry device and using method thereof, to pressure and concentration calibration while utilizing mass spectrometer to carry out gasometric analysis to be solved, thereby obtain analysis result more accurately and reliably.
For solving above-mentioned technical matters, the present invention by the following technical solutions:
A mass spectrometric self feed back gasometry device, comprises mass spectrometer; Also comprise control system, gas distributing system, pressure controller, air extractor, at least one operation valve, at least one injection port; Described air extractor is connected with pressure controller by connecting pipe; Described gas distributing system is connected with described operation valve by connecting pipe; Described injection port is connected with described operation valve by connecting pipe; Described operation valve is connected with described mass spectrometer by the first three-way connection with described pressure controller; Described mass spectrometer and described control system electrically connect; Described gas distributing system and described control system electrically connect; Described operation valve and described control system electrically connect; Described pressure controller and described control system electrically connect.
Further technical scheme is by connecting pipe, to be connected with pressure unit between pressure controller and described the first three-way connection; Described pressure unit and described control system electrically connect.
Further technical scheme is to be provided with the second three-way connection between pressure unit and described pressure controller; Described the second three-way connection is connected with atmospheric valve by connecting pipe; Described atmospheric valve and described control system electrically connect.
Further technical scheme is also to comprise thermostat based on mass spectrometric self feed back gasometry device.
Further technical scheme is on thermostat, to be provided with temperature sensor, and described temperature sensor and described control system electrically connect.
Further technical scheme is that operation valve is that multichannel is switched motorized valve.
Further technical scheme is that control system is a kind of in computing machine, PLC, integrated circuit block; Described control system comprises I/O switch control unit and A/D converter.
Further technical scheme is that gas distributing system is a kind of in static gas distributing system or dynamic gas mixer.
Further technical scheme is that connecting pipe is the stable material of physico-chemical property.
Further technical scheme is a kind of using method based on mass spectrometric self feed back gasometry device, and described using method comprises the following steps:
Device is connected with testing sample container or pipeline, and initialization THE DYNAMIC SELF-FEEDBACK proportioning device, detects the sealing connecting;
Operation valve is switched to closed condition, start described air extractor, open the switch of pressure control device; While being vacuum in air-channel system, operation valve is switched to sample position, after pressure is stablized in air-channel system, start mass spectrometer the composition of the sample gas in air-channel system and response are tested, measure the pressure in air-channel system simultaneously;
According to the response recording, gas concentration is estimated, according to estimation result, adjust the concentration of calibrating gas, adjust calibrating gas sample introduction pressure consistent with sample feeding pressure, the response of measurement standard gas simultaneously;
Utilize external standard method to carry out quantitatively sample, if sample concentration and standard specimen concentration deviation do not meet the demands, concentration is adjusted calibrating gas concentration per sample again, repeats standard specimen test, until sample concentration and standard specimen concentration deviation meet the demands.
Compared with prior art, the invention has the beneficial effects as follows: the pressure controller on air-channel system of the present invention can be adjusted the sample introduction pressure of sample or standard specimen, by feedback system, make the sample introduction pressure of sample and standard specimen consistent, eliminated the impact of sample introduction pressure gap on quantitative result.The present invention can with gas distributing system collaborative work, the THE DYNAMIC SELF-FEEDBACK that state is realized standard specimen concentration per sample regulates, and makes composition and the concentration of standard specimen and sample consistent, has eliminated the impact of component difference on quantitative result.The collaborative work of vacuum extractor of the present invention, pressure controller and motorized valve, can realize the detection to the subatmospheric sample of pressure by Sample introduction sampling system, has avoided the interference of environmental gas.The coupling arrangement of air-channel system of the present invention all adopts the stable material of materialization, can effectively reduce the absorption of component in gas circuit in sample.Circuits System of the present invention has realized the data communication of each parts and computer control system, by the switching of motorized valve, and the adjusting of pressure controller, mass spectrometric control has realized auto injection.Can not only meet the analysis of negative-pressure gas sample, and energy automatic sampling, the unattended operation of Realization analysis instrument, saves human resources.
Accompanying drawing explanation
Fig. 1 is the structural representation of one embodiment of the invention.
Fig. 2 is the structural representation of another embodiment of the present invention.
Embodiment
Below in conjunction with accompanying drawing, the present invention is further elaborated.
As shown in Figure 1, Fig. 1 shows the structural representation of one embodiment of the invention.The mass spectrometric THE DYNAMIC SELF-FEEDBACK gasometry of one embodiment of the present of invention device comprises housing, and enclosure interior comprises air-channel system and Circuits System; Air-channel system comprises pressure controller 1, operation valve 2, air extractor 3, mass spectrometer 4, sampling receptacle or pipeline 8, gas distributing system 5.In the present embodiment, operation valve 2 can be solenoid valve or motorized valve, and preferably, in the present embodiment, operation valve is motorized valve.Air extractor in the present embodiment can be vacuum pump or the device with air extracting function, and the air extractor of this enforcement is vacuum pump.Air extractor is by conduit Bonding pressure controller one end, pressure controller 1 other end is connected with first interface of the first three-way connection 7 by first conduit, pressure controller 1 can be electrically connected to control system by data line, control system is controlled its operation automatically, realizes the automatic adjustment of pressure in pipeline; Second interface of the first three-way connection 7 is connected with mass spectrometer 4 by second conduit.The 3rd interface of the first three-way connection is connected with motorized valve by the 3rd conduit.As preferred embodiment, in the present embodiment, operation valve is that multichannel is switched motorized valve, control the 3rd conduit and be connected with sample or standard specimen, motorized valve is electrically connected to control system 6 by data line, and control system 6 is automatically controlled the 3rd conduit by motorized valve and is connected with sample or standard specimen.While analyzing, motorized valve switches, and sample gas is put into pipeline, by pressure controller, pressure is adjusted as required, mass spectrometer is analyzed, complete after analysis, according to analysis result, utilize 5 pairs of standard specimen concentration of gas distributing system to regulate, motorized valve switches, by standard specimen introduction pipeline, by pressure controller, pressure is adjusted as required, mass spectrometer is analyzed, and according to the analysis result of standard specimen, sample is carried out quantitatively.As preferred embodiment, the conduit in the present embodiment, jointing and sampling receptacle all adopt physico-chemical property stabilizing material, as glass, stainless steel material etc., wherein take stainless steel material as excellent.The air-channel system parts of the present embodiment are strictly sealing all, to keep the primary characteristic of gaseous sample, and shortens the pipeline that gaseous sample is carried as far as possible.Control system in the present embodiment can be computing machine, PLC or integrated circuit block, or is other devices that can realize data processing and Presentation Function.
As shown in Figure 2, Fig. 2 shows the structural representation of another embodiment of the present invention.As preferred embodiment, an alternative embodiment of the invention is implemented on the basis of above-described embodiment, the present embodiment comprises based on mass spectrometric THE DYNAMIC SELF-FEEDBACK gasometry device: pressure controller 21, operation valve 22, air extractor 23, mass spectrometer 24, gas distributing system 25, control system 26, the first three-way connection 27, the first sampling receptacle 28, the second three-way connection 9, the second sampling receptacle 10, temperature sensor 11, thermostat 12, pressure unit 13, atmospheric valve 14.Pressure controller 21, operation valve 22, air extractor 23, mass spectrometer 24, gas distributing system 25, connecting tee 27, the first sampling receptacle 28, the second three-way connection 9, the second sampling receptacle 10, pressure unit 13, atmospheric valve 14 connects by coupling arrangement.As preferred embodiment, in the present embodiment, pressure controller 1 is electronic pressure controller, a port of pressure controller 1 is connected with air extractor, another port is connected by conduit with first connector of the second three-way connection 9, between electronic pressure controller and control system 26, by signal wire, be connected, control system 26 can realize the automatic adjusting of pipeline inner pressure as required.As preferred embodiment, in the present embodiment, operation valve is that multichannel is switched motorized valve, specific embodiments is, it is No. 3 transfer valves that multichannel in the present embodiment is switched motorized valve, the first via is connected with the gas vent of gas distributing system, the second tunnel is connected with the first sampling receptacle 28, Third Road is connected with the second sampling receptacle 10, public road is connected by second conduit with second mouth of the first three-way connection 27, between No. 3 transfer valves and control system, by signal wire, be connected, control system can be controlled the switching of No. 3 transfer valves automatically.Air extractor 23 in the present embodiment is a vacuum pump, is connected with a port of pressure controller 21.Second connector and the atmospheric valve 14 of the second three-way connection 9 join, and atmospheric valve is motorized valve or solenoid valve, is connected by signal wire with control system, and control system opens or closes atmospheric valve automatically, realize being communicated with isolated of pipe system and environment.The 3rd interface of the second three-way connection 9 and first connector of the first three-way connection 27 join by second conduit, on second conduit, be connected to the pressure unit 13 that can accurately measure line pressure, pressure unit 13 transfers to control system by signal wire by the pressure signal recording.Gas distributing system 25 in the present embodiment can be static gas distributing system, can be also dynamic gas mixer, for the adjustment of calibrating gas composition and concentration.In the present embodiment, gas distributing system 25 is dynamic gas mixer, and this system is connected with control system by signal wire, and control system can be passed through composition and the concentration of gas distributing system adjustment criteria gas as required, and the concentration that realizes calibrating gas regulates automatically.Thermostat 12 in the present embodiment and the Main Function of temperature sensor 11 are to maintain pipe system temperature stabilization, and air-channel system is in thermostat, and then the gaseous tension in stable pipeline.In the present embodiment, the material of coupling arrangement adopts the stable material of physico-chemical property to make, and the stable material of materialization has multiple, and as pottery, stainless steel etc., as preferred embodiment, the material of the coupling arrangement in the present embodiment adopts stainless steel to make.Coupling arrangement adopts the stable stainless steel material of physico-chemical property, can effectively reduce the absorption of component in gas circuit in sample gas.Data processing equipment in the present embodiment can be PLC or integrated circuit block, and as preferred embodiment, in this enforcement, data processing equipment is the computing machine with display, adopts program controlled mode to carry out the automatic operation of system in control system.And comprise: I/O switch control unit, A/D converter.I/O switch control unit switches motorized valve with multichannel and is connected, for controlling the switching of motorized valve; A/D converter is connected with sensor electrical, for reading and record the measured value of described sensor.
According to another embodiment of the invention, the using method of the present embodiment based on mass spectrometric self feed back gasometry device, the course of work of the present embodiment using method is:
The first step, is connected device with testing sample container, initialization THE DYNAMIC SELF-FEEDBACK proportioning device detects the sealing connecting.
Second step, switches to closed condition by motorized valve, opens the switch of pressure controller completely; While being vacuum in air-channel system, motorized valve is switched to sampling receptacle link position, in air-channel system after pressure stability, start mass spectrometer the composition of the sample gas in air-channel system and response are tested, utilize pressure unit accurately to measure the pressure (sample feeding pressure) in air-channel system simultaneously.
The 3rd step, the signal recording according to mass spectrometer, estimates gas concentration, according to estimation result, utilize gas distributing system to adjust the concentration of calibrating gas, utilize pressure controller to adjust calibrating gas sample introduction pressure consistent with sample feeding pressure, by the response of mass spectrometer measurement standard gas simultaneously.
The 4th step, utilize external standard method to carry out quantitatively sample, if sample concentration and standard specimen concentration deviation do not meet the demands, concentration is adjusted calibrating gas concentration per sample again, the test of repetition standard specimen, until sample concentration and standard specimen concentration deviation meet the demands.
After above-mentioned 4 processes finish, complete the quantitative test of a sample.During next sample introduction, according to (2) (3) (4) step, operate.
The gasometric analysis device operation of the present embodiment is simple and easy, it is little, easy to maintenance to take up room, operating cost is low, automaticity is high, has wide market outlook.Under the prerequisite of not introducing secondary pollution, can effectively improve the utilization factor of gaseous sample, realize the object accurately detecting.Can not only meet the analysis of negative-pressure gas sample, and energy automatic sampling, automatic analysis, realizes the unattended operation of whole analytic process, saves human resources.
The present invention for the conventional sense of the scientific research of research institutions, government's part, for the gas analysis of carrying out in the laboratories such as process detection of industrial enterprise, can not only meet the analysis of gaseous sample, and energy automatic sampling, the unattended operation of Realization analysis instrument, saves human resources.
" embodiment " that spoken of in this manual, " another embodiment ", " embodiment ", etc., refer to specific features, structure or the feature in conjunction with this embodiment, described and be included at least one embodiment that the application's generality describes.In instructions, a plurality of local appearance statement of the same race is not necessarily to refer to same embodiment.Furthermore, while describing a specific features, structure or feature in conjunction with any embodiment, what advocate is in conjunction with other embodiment, to realize this feature, structure or feature also to fall within the scope of the invention.
Although with reference to a plurality of explanatory embodiment inventing, invention has been described here, but, should be appreciated that, those skilled in the art can design a lot of other modification and embodiments, and these are revised and within embodiment will drop on the disclosed principle scope and spirit of the application.More particularly, in the scope of the open claim of the application, can carry out multiple modification and improvement to the building block of subject combination layout and/or layout.Except modification that building block and/or layout are carried out with improving, to those skilled in the art, other purposes will be also obvious.
Claims (10)
1. based on a mass spectrometric self feed back gasometry device, comprise mass spectrometer; It is characterized in that: also comprise control system, gas distributing system, pressure controller, air extractor, at least one operation valve, at least one injection port; Described air extractor is connected with pressure controller by connecting pipe; Described gas distributing system is connected with described operation valve by connecting pipe; Described injection port is connected with described operation valve by connecting pipe; Described operation valve is connected with described mass spectrometer by the first three-way connection with described pressure controller; Described mass spectrometer and described control system electrically connect; Described gas distributing system and described control system electrically connect; Described operation valve and described control system electrically connect; Described pressure controller and described control system electrically connect.
2. according to claim 1 based on mass spectrometric self feed back gasometry device, it is characterized in that by connecting pipe, being connected with pressure unit between described pressure controller and described the first three-way connection; Described pressure unit and described control system electrically connect.
3. according to claim 2 based on mass spectrometric self feed back gasometry device, it is characterized in that being provided with the second three-way connection between described pressure unit and described pressure controller; Described the second three-way connection is connected with atmospheric valve by connecting pipe; Described atmospheric valve and described control system electrically connect.
4. according to claim 1 based on mass spectrometric self feed back gasometry device, it is characterized in that described based on mass spectrometric self feed back gasometry device, also comprising thermostat.
5. according to claim 4 based on mass spectrometric self feed back gasometry device, it is characterized in that being provided with temperature sensor on described thermostat, described temperature sensor and described control system electrically connect.
6. according to claim 1 based on mass spectrometric self feed back gasometry device, it is characterized in that described operation valve is that multichannel is switched motorized valve.
7. according to claim 1 based on mass spectrometric self feed back gasometry device, it is characterized in that described control system is a kind of in computing machine, PLC, integrated circuit block; Described control system comprises I/O switch control unit and A/D converter.
8. according to claim 1 based on mass spectrometric self feed back gasometry device, it is characterized in that described gas distributing system is a kind of in static gas distributing system or dynamic gas mixer.
9. according to claim 1 based on mass spectrometric self feed back gasometry device, it is characterized in that described connecting pipe is the stable material of physico-chemical property.
10. according to the using method based on mass spectrometric self feed back gasometry device described in the arbitrary claim of claim 1 to 9, it is characterized in that described using method comprises the following steps:
Device is connected with testing sample container or pipeline, and initialization THE DYNAMIC SELF-FEEDBACK proportioning device, detects the sealing connecting;
Operation valve is switched to closed condition, start described air extractor, open the switch of pressure control device; While being vacuum in air-channel system, operation valve is switched to sample position, after pressure is stablized in air-channel system, start mass spectrometer the composition of the sample gas in air-channel system and response are tested, measure the pressure in air-channel system simultaneously;
According to the response recording, gas concentration is estimated, according to estimation result, adjust the concentration of calibrating gas, adjust calibrating gas sample introduction pressure consistent with sample feeding pressure, the response of measurement standard gas simultaneously;
Utilize external standard method to carry out quantitatively sample, if sample concentration and standard specimen concentration deviation do not meet the demands, concentration is adjusted calibrating gas concentration per sample again, repeats standard specimen test, until sample concentration and standard specimen concentration deviation meet the demands.
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| CN108291892A (en) * | 2015-12-04 | 2018-07-17 | 株式会社岛津制作所 | Liquid sample analytic system |
| CN108844787A (en) * | 2018-07-10 | 2018-11-20 | 中国工程物理研究院化工材料研究所 | Self feed back seal chamber gas sampling device and its application |
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