CN103529152B - 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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- CN103529152B CN103529152B CN201310482967.3A CN201310482967A CN103529152B CN 103529152 B CN103529152 B CN 103529152B CN 201310482967 A CN201310482967 A CN 201310482967A CN 103529152 B CN103529152 B CN 103529152B
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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 with detect keeping the safety in production, process optimization, quality control and energy-saving and emission-reduction etc. are significant.As the one of on-line analysis; mass spectrometry is a kind of analytical approach by analyzing its composition to the mensuration of sample ion mass-to-charge ratio; have fast response time, measuring accuracy is high, range ability is wide, good stability, can carry out multi-analyte immunoassay 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 a high vacuum, and gas analysis object much all can with more high pressure operation, the docking of suitable pressure buffer Interface realization is needed between mass spectrometer and analytic target, 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, it is non-linear that complicacy due to interface fluidised form can cause between pressure-response, mutual interference between the difference of background gas and gas can cause departing from of concentration-response linear relation, thus have impact on mass spectrometer quantitative result accurately and reliably, be not suitable for complex state sample analysis.
Summary of the invention
Instant invention overcomes the deficiencies in the prior art, there is provided a kind of based on mass spectrometric self feed back gasometry device and using method thereof, to to be solved utilize mass spectrometer to carry out gasometric analysis time pressure and concentration calibration, thus obtain analysis result more accurately and reliably.
For solving above-mentioned technical matters, the present invention by the following technical solutions:
A kind of based on mass spectrometric self feed back gasometry device, comprise 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 connected with pressure unit by connecting pipe between pressure controller and described first three-way connection; Described pressure unit and described control system electrically connect.
Further technical scheme is provided with the second three-way connection between pressure unit and described pressure controller; Described second three-way connection is connected with atmospheric valve by connecting pipe; Described atmospheric valve and described control system electrically connect.
Further technical scheme also comprises thermostat based on mass spectrometric self feed back gasometry device.
Further technical scheme is that thermostat is provided with temperature sensor, and described temperature sensor and described control system electrically connect.
Further technical scheme is operation valve is multy-way switching motorized valve.
The further technical scheme one that to be control system be in computing machine, PLC, integrated circuit block; Described control system comprises I/O switch control unit and A/D converter.
One further in technical scheme to be gas distributing system be static gas distributing system or dynamic gas mixer.
The material that further technical scheme to be connecting pipe be physico-chemical property is stable.
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, initialization THE DYNAMIC SELF-FEEDBACK proportioning device, detects the sealing connected;
Operation valve is switched to closed condition, starts described air extractor, open the switch of pressure control device; When being vacuum in air-channel system, operation valve being switched to sample position, after pressure is stablized in air-channel system, starting mass spectrometer and the composition of the sample gas in air-channel system and response are tested, measuring the pressure in air-channel system simultaneously;
According to the response recorded, estimate gas concentration, according to estimation result, the concentration of adjustment calibrating gas, adjusts 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 adjusts standard 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 adjust the sample introduction pressure of sample or standard specimen, make sample consistent with the sample introduction pressure of standard specimen by feedback system, eliminate 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 realizes standard specimen concentration per sample regulates, make the composition of standard specimen and sample and concentration consistent, eliminate the impact of compositional difference on quantitative result.The collaborative work of vacuum extractor of the present invention, pressure controller and motorized valve, by Sample introduction sampling system, can achieve the detection to the subatmospheric sample of pressure, avoid the interference of environmental gas.The material that the coupling arrangement of air-channel system of the present invention all adopts materialization stable, effectively can reduce the absorption of component in gas circuit in sample.Circuits System of the present invention achieves the data communication of each parts and computer control system, by the switching of motorized valve, and the adjustment of pressure controller, mass spectrometric control realization auto injection.The analysis of negative-pressure gas sample can not only be met, 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.One embodiment of the present of invention mass spectrometric THE DYNAMIC SELF-FEEDBACK gasometry 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 tubes connection 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 with control system by data line, control system automatically controls it and runs, and 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.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 multy-way switching motorized valve, control the 3rd conduit to be connected with sample or standard specimen, motorized valve is electrically connected with control system 6 by data line, and control system 6 automatically controls the 3rd conduit by motorized valve and is connected with sample or standard specimen.When analyzing, motorized valve switches, and sample gas is put into pipeline, is adjusted as required by pressure controller to pressure, mass spectrometer is analyzed, after completing analysis, utilize gas distributing system 5 pairs of standard specimen concentration to regulate according to analysis result, motorized valve switches, by standard specimen introduction pipeline, adjusted pressure by pressure controller as required, mass spectrometer is analyzed, and the analysis result according to standard specimen carries out quantitatively sample.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., are wherein excellent with stainless steel material.The air-channel system parts of the present embodiment all strictly seal, and to keep the primary characteristic of gaseous sample, and shorten the pipeline of gaseous sample conveying as far as possible.Control system in the present embodiment can be computing machine, PLC or integrated circuit block, or is that other can realize the device of 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, first three-way connection 27, first sampling receptacle 28, second three-way connection 9, 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, first sampling receptacle 28, second three-way connection 9, second sampling receptacle 10, pressure unit 13, atmospheric valve 14 is connected 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, first connector of another port and the second three-way connection 9 passes through tubes connection, be connected by signal wire between electronic pressure controller with control system 26, control system 26 can realize the automatic adjustment of pipeline inner pressure as required.As preferred embodiment, in the present embodiment, operation valve is multy-way switching motorized valve, specific embodiments is, multy-way switching motorized valve in the present embodiment is No. 3 transfer valves, the first via is connected with the gas vent of gas distributing system, second tunnel is connected with the first sampling receptacle 28,3rd tunnel is connected with the second sampling receptacle 10, second mouth of public road and the first three-way connection 27 is by second tubes connection, No. 3 transfer valves are connected by signal wire with between control system, and control system can control 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 of the second three-way connection 9 connects with atmospheric valve 14, 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, realizes being communicated with isolated of pipe system and environment.3rd interface of the second three-way connection 9 is connected by second conduit with first connector of the first three-way connection 27, second conduit is connected to the pressure unit 13 accurately measuring line pressure, the pressure signal recorded is transferred to control system by signal wire by pressure unit 13.Gas distributing system 25 in the present embodiment can be static gas distributing system, also can be dynamic gas mixer, for calibrating gas composition and the adjustment of 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 as required by composition and the concentration of gas distributing system adjustment criteria gas, and the concentration realizing calibrating gas regulates automatically.Thermostat 12 in the present embodiment and the Main Function of temperature sensor 11 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 employing stainless steel of the coupling arrangement in the present embodiment is made.The stainless steel material that coupling arrangement adopts physico-chemical property stable, effectively can 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 preferably, 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 is connected with multy-way switching motorized valve, for controlling the switching of motorized valve; A/D converter is connected with sensor electrical, for reading and recording the measured value of described sensor.
According to another embodiment of the invention, the present embodiment is based on the using method of mass spectrometric self feed back gasometry device, and 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 connected.
Second step, switches to closed condition by motorized valve, opens the switch of pressure controller completely; When 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 to test the composition of the sample gas in air-channel system and response, utilize pressure unit accurately to measure pressure (sample feeding pressure) in air-channel system simultaneously.
3rd step, according to the signal that mass spectrometer records, 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.
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 adjusts standard gas concentration per sample again, repetition standard specimen is tested, till sample concentration and standard specimen concentration deviation meet the demands.
After above-mentioned 4 processes terminate, namely complete the quantitative test of a sample.During sample introduction next time, operate according to (2) (3) (4) step.
The present embodiment gasometric analysis device operation simple and easy, take up room little, easy to maintenance, operating cost is low, automaticity is high, has wide market outlook.Effectively can improve the utilization factor of gaseous sample under the prerequisite not introducing secondary pollution, realize the object accurately detected.The analysis of negative-pressure gas sample can not only be met, and energy automatic sampling, automatic analysis, realizes the unattended operation of whole analytic process, saves human resources.
The present invention is for the gas analysis carried out in the laboratory such as scientific research, the conventional sense of government's part, the process detection of industrial enterprise of research institutions, the analysis of gaseous sample can not only be met, and energy automatic sampling, the unattended operation of Realization analysis instrument, saves human resources.
Spoken of in this manual " embodiment ", " another embodiment ", " embodiment ", etc., refer to the specific features, structure or the feature that describe in conjunction with this embodiment and be included at least one embodiment of the application's generality description.Multiple place occurs that statement of the same race is not necessarily refer to same embodiment in the description.Furthermore, when describing specific features, structure or a feature in conjunction with any one embodiment, what advocate is also fall within the scope of the invention to realize this feature, structure or feature in conjunction with other embodiments.
Although with reference to the multiple explanatory embodiment of inventing, invention has been described here, but, should be appreciated that, those skilled in the art can design a lot of other amendment and embodiment, these amendments and embodiment will drop within spirit disclosed in the present application and spirit.More particularly, in the scope of the open claim of the application, multiple modification and improvement can be carried out to the building block of subject combination layout and/or layout.Except the modification of carrying out building block and/or layout is with except improvement, to those skilled in the art, other purposes also will be obvious.
Claims (8)
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; Pressure unit is connected with by connecting pipe between described pressure controller and described first three-way connection; Described pressure unit and described control system electrically connect; 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 being provided with the second three-way connection between described pressure unit and described pressure controller; Described second three-way connection is connected with atmospheric valve by connecting pipe; Described atmospheric valve and described control system electrically connect.
3. according to claim 1 based on mass spectrometric self feed back gasometry device, it is characterized in that described also comprising thermostat based on mass spectrometric self feed back gasometry device.
4. according to claim 3 based on mass spectrometric self feed back gasometry device, it is characterized in that described thermostat is provided with temperature sensor, described temperature sensor and described control system electrically connect.
5. according to claim 1 based on mass spectrometric self feed back gasometry device, it is characterized in that described operation valve is multy-way switching motorized valve.
6. according to claim 1 based on mass spectrometric self feed back gasometry device, it is characterized in that described control system is the one in computing machine, PLC, integrated circuit block; Described control system comprises I/O switch control unit and A/D converter.
7. according to claim 1 based on mass spectrometric self feed back gasometry device, it is characterized in that described gas distributing system is the one in static gas distributing system or dynamic gas mixer.
8. according to claim 1 based on mass spectrometric self feed back gasometry device, it is characterized in that described connecting pipe is that the stable material of physico-chemical property is made.
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| CN105181860B (en) * | 2015-08-11 | 2017-04-05 | 昆山禾信质谱技术有限公司 | The control method of the gas concentration quasistatic adjustment equipment fed back based on mass spectrum |
| EP3385709A4 (en) * | 2015-12-04 | 2019-01-02 | Shimadzu Corporation | Liquid sample analysis system |
| CN107065950B (en) * | 2017-03-28 | 2020-10-23 | 清华大学 | Control method based on air pressure change in vacuum cavity of mass spectrometer |
| CN108844787B (en) * | 2018-07-10 | 2024-02-13 | 中国工程物理研究院化工材料研究所 | Self-feedback sealed cavity gas sampling device and application thereof |
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| US4847493A (en) * | 1987-10-09 | 1989-07-11 | Masstron, Inc. | Calibration of a mass spectrometer |
| ATE408237T1 (en) * | 2000-12-15 | 2008-09-15 | V & F Analyse & Messtechnik | METHOD AND DEVICE FOR ASSESSING THE CONDITION OF ORGANISMS AND NATURAL PRODUCTS AND FOR ANALYZING A GASEOUS MIXTURE WITH MAIN AND SECONDARY COMPONENTS |
| US7531134B1 (en) * | 2002-03-08 | 2009-05-12 | Metara, Inc. | Method and apparatus for automated analysis and characterization of chemical constituents of process solutions |
| DE102006015535A1 (en) * | 2006-03-31 | 2007-10-04 | Thermo Electron (Bremen) Gmbh | Sample isotope ratio analysis, involves supplying sample gas and reference gas to analyzer over coupling, and regulating concentration of sample gas and/or reference gas through electronic flow regulation of carrier gas |
| CN102445498B (en) * | 2011-10-10 | 2013-06-05 | 上海科油石油仪器制造有限公司 | Automatic calibration method of process chromatograph |
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