CN101377469B - Method and apparatus for real-time detecting mixing gas component content by thermal conductivity detector - Google Patents
Method and apparatus for real-time detecting mixing gas component content by thermal conductivity detector Download PDFInfo
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- CN101377469B CN101377469B CN2008100294669A CN200810029466A CN101377469B CN 101377469 B CN101377469 B CN 101377469B CN 2008100294669 A CN2008100294669 A CN 2008100294669A CN 200810029466 A CN200810029466 A CN 200810029466A CN 101377469 B CN101377469 B CN 101377469B
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Abstract
The invention discloses a method for real-time detecting component content of mixed gas with thermal conductivity detector, and a device thereof. The computer data acquisition system of the device is connected with the signal output end of the thermal conductivity detector; one of the gas cylinders, one of the pressure regulating valves, and one of the mass flow controllers are orderly connected with the thermal conductivity detector; and a sampling probe is connected with the to-be-detected gas inlet of the thermal conductivity detector through a pipeline. The method comprises the following steps: firstly, scaling the gas content and voltage output value of the TCD detecting system before detection; secondly, introducing the to-be-detected gas into the sampling system through the sampling probe during detection; thirdly obtaining the content of a certain component of the to-be-detected mixed gas by referring to the concentration relation between the voltage and the concentration of the certain component in the mixed gas generated during the scaling step. The invention is an effective method for detecting the concentration variation of a certain component within the mixed gas with fast detection, simple and convenient operation, accurate analysis result, wide application range and good stability.
Description
Technical field
The present invention relates to the detection of mixing gas component content, particularly relate to a kind of method and device that utilizes a certain component concentration in the thermal conductivity detector (TCD) real-time detecting mixing gas.
Background technology
In industries such as chemical industry, the energy, often need certain component in the real-time detecting mixing gas to reach the situation of change of locus in time.For example in the research reactor, in the mixing rule of gas, often need in the cold conditions model of reactor, inject tracer gas, detect the regularity of distribution of tracer gas in reactor.The time that the concentration of traditional gas chromatographic analysis technique test gas needs is longer, is difficult to reach the requirement of real-time detection.The present invention utilizes the difference of the coefficient of heat conductivity of gas with various, adopt thermal conductivity detector (TCD) (ThermalConductivity Detector, TCD) coefficient of heat conductivity of real-time detecting mixing gas, and output correspondent voltage value, relation according to certain concentration of component in the thermal conductivity detector (TCD) output voltage of scale and the mixed gas obtains this component concentrations in the gas to be measured.
Chinese invention patent 96190402.X discloses a kind of device of measuring component of mixture concentration, has first's volume, and in this volume, concentration of component is not subjected to keep invariable by the influence that concentration in diffusional resistance and the mixed gas is coupled.The solid electrolyte as aspirator is compensated above-mentioned coupling influence between first's volume and the gaseous mixture by being in by a controllable component pump electric current.The pump current's intensity is the measuring of the concentration that requires in the gaseous mixture.The said pump electric current can be used as the departure function of the Nernst sensor output voltage between first's volume and the reference gas volume and is subjected to the control of ratings.This device characteristic is on purpose to influence the ratings that depends on aspirator solid electrolyte two ends voltage-measurable.But this patented technology need fill the gas that has benchmark gas concentration to be measured in the second portion volume in test process, and promptly this patented technology must be used standard gas simultaneously when the gas concentration of test outside the oxygen, and this just makes the test process complexity.
Summary of the invention
The objective of the invention is to overcome the shortcoming of prior art, provide that a kind of test specification is wide, applicability is strong, the method for component concentration in the real-time detection mixed gas fast.
Another object of the present invention is to provide the thermal conductivity detector (TCD) that utilizes of realizing said method to detect the device of certain component concentration in the mixed gas.
The method of certain concentration of component is to utilize the difference of gas with various coefficient of heat conductivity in the real-time detecting mixing gas of the present invention, adopt thermal conductivity detector (TCD) (TCD) to detect the coefficient of heat conductivity of mixed gas, and output correspondent voltage value, relation according to certain concentration of component in the thermal conductivity detector (TCD) output voltage of scale and the mixed gas obtains this component concentrations in the gas to be measured.
Purpose of the present invention realizes by adopting following technical scheme:
Utilize the method for thermal conductivity detector (TCD) real-time detecting mixing gas component content, comprise the steps:
(1) standard gas proportioning is determined: with gas cylinder two in the pure gas that contains certain component in the gas to be measured and gas cylinder three in gas to be measured in all the other components gas respectively through pressure-regulating valve two, three the drawing of pressure-regulating valve, use four its flows of control of three and mass rate controller of mass rate controller more respectively, the standard gas proportioning mixed gas that obtains;
(2) scale of gas concentration to be measured and TCD voltage: the mixing tank that sampling probe is inserted the good standard gas of proportioning, one of service property (quality) flow quantity control instrument control reference gas flow, two control criterion airsheds of service property (quality) flow quantity control instrument, the magnitude of voltage of TCD output when detecting gas variable concentrations to be measured respectively;
(3) detection of gas concentration to be measured: sampling probe is inserted respectively in the sample to be detected, flow when one of service property (quality) flow quantity control instrument control reference airshed such as step (2) scale, standard airshed when the two controls airshed to be measured of service property (quality) flow quantity control instrument is step (2) scale, the magnitude of voltage of record TCD output, contrast step (2) voltage that scale produced and the concentration relationship of gas component in mixed gas can obtain detecting certain component concentrations in the mixed gas.
Utilize the device of thermal conductivity detector (TCD) real-time detecting mixing gas component content, comprise the sub-system of reference source of the gas and flow control, sampling system, thermal conductivity detector (TCD) and data acquisition system (DAS) and standard gas matching system;
Described thermal conductivity detector (TCD) and data acquisition system (DAS) comprise thermal conductivity detector (TCD) and computer data acquisition system, and computer data acquisition system is connected with the signal output part of thermal conductivity detector (TCD);
Described reference source of the gas and flow control system comprise one of one of gas cylinder that connects successively, pressure-regulating valve and one of mass rate controller, and one of mass rate controller is connected with the reference gas import of thermal conductivity detector (TCD); Described sampling system comprises by two of the sampling probe of pipeline connection and makings amount flow quantity control instrument to be measured; Sampling probe is connected with the gas import to be measured of thermal conductivity detector (TCD) by pipeline, and two of mass rate controller is connected with the gas to be measured outlet of thermal conductivity detector (TCD);
Standard gas matching system comprise the gas cylinder that contains component gas A to be measured two, pressure-regulating valve two, the mass rate controller three, contain all the other B component in the mixed gas gas cylinder three, pressure-regulating valve three, the mass rate controller four, gas A and gas B mixing tank, aciculiform variable valve; Gas cylinder two, two being connected successively of pressure-regulating valve with three of mass rate controller, and be connected with mixing tank; Three of gas cylinder, three of pressure-regulating valve is connected successively with four of mass rate controller, and is connected with mixing tank; The aciculiform variable valve is connected with mixing tank; Mixing tank is provided with thief hatch.
With respect to prior art, the present invention has following advantage and beneficial effect:
1. for certain concentration of component in the test mixing gas, compare, cancelled the chromatographic column separating process, make test process to carry out in real time fast with traditional chromatogram gas concentration analytical technology.
2. contain scaling system and test macro, to the variation of a certain concentration of component in the mixed gas, all can obtain the corresponding relation of its concentration change and thermal conductivity detector (TCD) output voltage by scaling system, the gas scope that test adapts to is wide, highly versatile
Description of drawings
Fig. 1 is the apparatus structure synoptic diagram that utilizes the thermal conductivity detector (TCD) real-time detecting mixing gas component content.
Fig. 2 is the thermal conductivity detector (TCD) fundamental diagram.
Fig. 3 is a standard gas matching system.
Fig. 4 is the device synoptic diagram that utilizes gas mixing situation in the helium research fluidized-bed reactor.
Embodiment
The present invention is further illustrated below in conjunction with drawings and embodiments, but the scope of protection of present invention is not limited to the scope that embodiment is expressed.
As shown in Figure 1, utilize the pick-up unit of certain component concentration in the thermal conductivity detector (TCD) real-time detecting mixing gas to comprise reference source of the gas and the sub-system of flow control, sampling system and thermal conductivity detector (TCD) and data acquisition system (DAS).
Described thermal conductivity detector (TCD) and data acquisition system (DAS) comprise: thermal conductivity detector (TCD) 1 and computer data acquisition system 2, computer data acquisition system 2 is connected with the signal output part 112 of thermal conductivity detector (TCD) 1.As shown in Figure 2, a kind of pick-up unit that thermal conductivity detector (TCD) is made up of thermal resistance sensor, it is made up of two conductance cells and testing circuit, and two conductance cells have the import and export of gas.Wherein the gas feed of one of conductance cell 106 is reference gas import 108, exports to be reference gas outlet 109.2 107 gas feed of conductance cell is gas import 110 to be measured, and exporting is gas outlet 111 to be measured.Testing circuit is typical whiston bridge circuit, i.e. one of fixed resistance 102 and reference arm resistance 104 serial connections, and 2 103 of fixed resistance is connected in series with gage beam resistance 105, is connected with power supply 101 after the two sequential circuit parallel connections.Different according to the flow of 2 107 reference gas that enters one of conductance cell 106 and conductance cell and gas to be measured and coefficient of heat conductivity, the output terminal 112 exportable different voltages of testing circuit.The gas of considering oxidisability may cause the oxidation of reference arm resistance 104, so the reference gas among the present invention is selected non-oxidizing gas for use, as nitrogen, hydrogen, argon gas etc.
Reference source of the gas and flow control system comprise one of one of one of gas cylinder of connection successively 7, pressure-regulating valve 8, mass rate controller 9 and thermal conductivity detector (TCD) 1.Reference gas is successively by one of one of one of gas cylinder 7, pressure-regulating valve 8 and mass rate controller 9, and the flow of regulating control reference gas keeps stable back to insert the reference gas import 108 of thermal conductivity detector (TCD) 1, is discharged by reference gas outlet 109.
Sampling system comprises by 25 of the sampling probe 3 of pipeline connection and makings amount flow quantity control instrument to be measured.Gas to be measured by 25 of sampling probe 3 and makings amount flow quantity control instrument to be measured, is connected to the gas import 110 to be measured of thermal conductivity detector (TCD) 1 successively, and discharges from gas outlet 111 to be measured.If contain dust in the gas to be measured, then filtrator 4 is installed in sampling probe 3 backs; If atmospheric pressure to be measured is low excessively, can not guarantee that sample gas crosses thermal conductivity detector (TCD) 1 with certain velocity flow, then vacuum pumps 6 are installed, for gas flow to be measured provides power in 25 backs of mass rate controller.To be sampling probe 3 need adopt tubule footpath pipeline (internal diameter is less than 2 millimeters) to the pipeline of thermal conductivity detector (TCD) 1 for the real-time that detects for guaranteeing, the connecting line of sampling system; And pipeline will be lacked as far as possible, and gas communication speed will be as quickly as possible, with guarantee gas to be measured from sampling probe 3 to thermal conductivity detector (TCD) 1 flowing time short as far as possible, usually less than 1 second.
The present invention also comprises standard gas matching system, is used for the scale of mixed gas component concentration and TCD detection system output voltage values.According to the component concentration scope of gas to be checked in mixed gas, the mixed gas of a series of known gas concentrations to be measured of proportioning (being called standard gas), the standard gas of serial concentration known is fed test macro, read the magnitude of voltage of the output terminal 112 of thermal conductivity detector (TCD) 1, obtain the relation (being generally linearity) of gas content to be measured in voltage and the standard gas, when detecting, can concern that the magnitude of voltage correspondence that reads by detection system calculates a certain components contents in the mixed gas according to this.
As shown in Figure 3, standard gas matching system comprise the gas cylinder that contains component gas A to be measured 2 201, pressure-regulating valve 2 203, the mass rate controller 3 204, contain all the other B component in the mixed gas gas cylinder 3 202, pressure-regulating valve 3 207, the mass rate controller 4 208, gas A and gas B mixing tank 205, aciculiform variable valve 206.The filling material of filling glass pearl and so in the mixing tank 205, so that gas is fully mixed, mixing tank 205 is provided with thief hatch 209.Gas cylinder 2 201,2 203 being connected successively of pressure-regulating valve with 3 204 of mass rate controller, 3 204 of mass rate controller is connected with mixing tank 205; 3 202 of gas cylinder, 3 207 of pressure-regulating valve is connected successively with 4 208 of mass rate controller, and 4 208 of mass rate controller is connected with mixing tank 205; Aciculiform variable valve 206 is connected with mixing tank 205.
During scale,, obtain the mixed gas of known gas A concentration with the flow of accurate pilot-gas A of mass rate controller and gas B.Sampling probe 3 is inserted thief hatch 209, stability of flow with one of mass rate controller 9 control reference gas, stability of flow with 25 control criterion gas of mass rate controller, read in the TCD output voltage values of the standard gas when containing gas with various A concentration from data acquisition system (DAS) 2, obtain the corresponding relation of voltage and A gas concentration.
When using in the said apparatus real-time detecting mixing gas A component concentration, sampling probe 3 is inserted in the gas that needs to detect, and the flow when one of quality of regulation flow quantity control instrument 9 and 25 of mass rate controller make the flow scale of reference gas and gas to be measured is consistent.Magnitude of voltage by data acquisition system (DAS) 2 record TCD outputs contrasts voltage and the concentration relationship of gas composition A in mixed gas that scale produced, can obtain detecting the concentration of component A in the mixed gas.
The present invention utilizes the difference of gas with various coefficient of heat conductivity, provides efficient ways for certain component concentrations in the real-time detecting mixing gas changes.Do not need during test gas to be separated, so detect rapidly, fast with chromatographic column.To the mensuration of certain component concentrations in any mixed gas, the variation of its concentration will inevitably cause the variation of coefficient of heat conductivity, and is so all available method of the present invention is tested the variation of its concentration, applied widely.
Embodiment: the test of concentrations of helium in certain fluidized-bed reactor
Application background: utilize gas flow rule in the concentration change rule research fluidized-bed reactor of tracer gas helium in bed.
As shown in Figure 3, certain fluidized-bed reactor is made up of following components: fluidizing gas (using air herein) inlet 301, bellows 302, gas distribution grid 303, fluidized bed body 304, helium distributor 305, gas filter 306, gas vent 313.Mean grain size be housed be 60 microns solid particle in the bed 312.Gas distribution grid 303 is a sintered porous metal plate.Helium distributor 305 is the stainless-steel tube of 6 millimeters of diameters, and it inserts the hole that the interior part of reactor is drilled with 0.5 millimeter of 5 diameter, is used for introducing in fluidized bed helium.Filtrator 306 is a sintered metal tube, is used to discharge the gas in the fluidized bed, prevents catalyst loss simultaneously.Five thief hatchs of gas 307,308,309,310,311 have been disposed at the differing heights place on the bed body 304.Helium distributor 305 is 0.5 meter apart from the distance of gas distribution grid 303, and thief hatch 308,309,310,311 distances from gas distribution grid 303 are respectively 0.4,0.3,0.2,0.1 meter.Thief hatch 307 is positioned at the free spatial domain of catalyst-free at 1.5 meters, distribution of gas aerofoil top.From helium distributor 305 helium is introduced the fluidized bed bed, insert sampling probe 3 at thief hatch 307,308,309,310,311 places, the concentrations of helium of test each point can reflect the characteristics of motion of introducing gas the fluidized bed from helium distributor 305.
Among this embodiment, utilize the thermal conductivity detector (TCD) 1 of the detection system of certain component concentration in the thermal conductivity detector (TCD) real-time detecting mixing gas to select the built-in thermal conductivity detector (TCD) of Shanghai Kechuang GC910 type chromatogram for use; The mass rate controller is all selected Beijing remittance Bo Long S49-33MT of company mass flow controller for use; Vacuum pump 6 selects for use the Wenling city to leap the FY-1C of instrument company type vacuum pump; Filtrator 4 is selected Beijing Xiong Chuan SS-2237 type filter for use; Needle valve 26 is selected Beijing Xiong Chuan SS-3M6F type for use; Reference gas is high pure nitrogen; Gas A is high-purity helium; Gas B is an air.
Detection comprises following two steps
(1) standard gas proportioning is determined.With helium in one of gas cylinder 201 and gas cylinder 2 202 in air two-way gas respectively from gas cylinder through pressure-regulating valve 2 203,3 207 the drawing of variable valve, again respectively with the mass rate controller 3 204,4 208 its flows of control of mass rate controller, the standard gas of the concentration known that obtains at mixing tank 205.
(2) scale of concentrations of helium and TCD voltage: as shown in Figure 1, 2, the sampling probe 3 of test macro is inserted the mixing tank 205 of the good standard gas of proportionings, one of service property (quality) flow quantity control instrument 9 control reference gas nitrogen flow 10ml/min; Open vacuum pump 6, the standard airshed 80ml/min that air that 25 controlled step (1) of service property (quality) flow quantity control instrument obtain and helium are formed is by the magnitude of voltage of computer data acquisition system 2 detection TCD signal output parts 112.
(3) repeating step (1) and (2), respectively the proportioning concentrations of helium be 1%, 2%, the standard gas (as shown in table 1) of 3%...9%, and detect the magnitude of voltage that TCD exports respectively when above-mentioned standard gas concentration, the result is as shown in table 2:
Table 1
Table 2 the 6th row are 4 replicate determination results to standard gas concentration, and the 7th has listed the measurement maximum deviation.The analysis result maximum deviation is less than 2.0% as can be seen from Table 2.
Table 2
(4) detection of concentrations of helium in the fluidized bed cold conditions model: fluidized bed as shown in Figure 4, from 301 air mass flows that enter that enter the mouth is 10.5 normal cubic metres/hour (gas space velocity is 0.05 meter per second the bed), the helium gas flow of introducing from helium distributor 305 be 0.3 normal cubic metre/hour.Sampling probe 3 is inserted respectively in the thief hatch 307,308,309,310,311, pop one's head in 3 ends from 135 millimeters of bed body 304 inwalls, flow 10ml/min when one of service property (quality) flow quantity control instrument 9 control reference gas nitrogen flows such as step (2) TCD scale, standard airshed 80ml/min when the 25 controls airshed to be measured of service property (quality) flow quantity control instrument is step (2) scale, detect each sampled point concentrations of helium, obtain data such as following table 3:
Table 3
The tracer gas helium will move downward in the bright fluidized bed of table 3 tables of data, but more down, concentrations of helium is low more.The thief hatch 307 places measured concentrations of helium of probe meets the concentrations of helium in Theoretical Calculation exit.
Find during test that when the helium gas flow of introducing when helium distributor 305 changed, the output voltage of thermal conductivity detector (TCD) 1 changed immediately, the response time is in 0.5 second, but the i.e. variation of certain component concentration in the present invention's real-time detecting mixing gas.If carry out the gas chromatographic analysis of spectrogram, then general about 15 minutes time of needs of chromatographic column just can be finished the separation to gas composition, can not detect in real time component concentrations.Measuring technology of the present invention is separated the scale of gas concentration with test process, needn't use standard gas in test process, makes the test process simple possible that becomes.
Claims (5)
1. utilize the method for thermal conductivity detector (TCD) real-time detecting mixing gas component content, it is characterized in that comprising the steps:
(1) standard gas proportioning is determined: with gas cylinder two in the pure gas that contains certain component in the gas to be measured and gas cylinder three in gas to be measured in all the other components gas respectively through pressure-regulating valve two, three the drawing of pressure-regulating valve, use four its flows of control of three and mass rate controller of mass rate controller more respectively, the standard gas proportioning mixed gas that obtains; The mixed gas of a series of known gas concentrations to be measured of proportioning;
(2) scale of gas concentration to be measured and thermal conductivity detector (TCD) voltage: reference gas is successively by one of one of gas cylinder, pressure-regulating valve and one of mass rate controller, the flow of regulating control reference gas keeps stable back to insert the reference gas import of thermal conductivity detector (TCD), is discharged by the outlet of reference gas; Sampling system comprises by two of the sampling probe of pipeline connection and makings amount flow quantity control instrument to be measured; Sampling probe is connected with the gas import to be measured of thermal conductivity detector (TCD) by pipeline, and two of mass rate controller is connected with the gas to be measured outlet of thermal conductivity detector (TCD); Sampling probe is inserted the mixing tank of the good standard gas of proportioning, one of service property (quality) flow quantity control instrument control reference gas flow, two control criterion airsheds of service property (quality) flow quantity control instrument, the magnitude of voltage of thermal conductivity detector (TCD) output when detecting gas variable concentrations to be measured respectively;
(3) detection of gas concentration to be measured: sampling probe is inserted in the sample to be detected, flow when one of service property (quality) flow quantity control instrument control reference airshed such as step (2) scale, standard airshed when the two controls airshed to be measured of service property (quality) flow quantity control instrument is step (2) scale, the magnitude of voltage of record thermal conductivity detector (TCD) output, the magnitude of voltage and the concentration relationship of gas component in mixed gas of the output of contrast step (2) scale thermal conductivity detector (TCD) can obtain detecting certain component concentrations in the mixed gas.
2. utilize the device of thermal conductivity detector (TCD) real-time detecting mixing gas component content, it is characterized in that: comprise the sub-system of reference source of the gas and flow control, sampling system, thermal conductivity detector (TCD) and data acquisition system (DAS) and standard gas matching system;
Described thermal conductivity detector (TCD) and data acquisition system (DAS) comprise thermal conductivity detector (TCD) and computer data acquisition system, and computer data acquisition system is connected with the signal output part of thermal conductivity detector (TCD);
Described reference source of the gas and flow control system comprise one of one of gas cylinder that connects successively, pressure-regulating valve and one of mass rate controller, and one of mass rate controller is connected with the reference gas import of thermal conductivity detector (TCD); Described sampling system comprises by two of the sampling probe of pipeline connection and makings amount flow quantity control instrument to be measured; Sampling probe is connected with the gas import to be measured of thermal conductivity detector (TCD) by pipeline, and two of mass rate controller is connected with the gas to be measured outlet of thermal conductivity detector (TCD);
Standard gas matching system comprise the gas cylinder that contains component gas A to be measured two, pressure-regulating valve two, the mass rate controller three, contain all the other B component in the mixed gas gas cylinder three, pressure-regulating valve three, the mass rate controller four, all the other B component mixing tanks, aciculiform variable valve in gas A and the mixed gas; Gas cylinder two, two being connected successively of pressure-regulating valve with three of mass rate controller, and be connected with mixing tank; Three of gas cylinder, three of pressure-regulating valve is connected successively with four of mass rate controller, and is connected with mixing tank; The aciculiform variable valve is connected with mixing tank; Mixing tank is provided with thief hatch.
3. the device that utilizes the thermal conductivity detector (TCD) real-time detecting mixing gas component content according to claim 2 is characterized in that: when treating that examining system is normal pressure, described mass rate controller two after vacuum pump is installed.
4. the device that utilizes the thermal conductivity detector (TCD) real-time detecting mixing gas component content according to claim 2, it is characterized in that: when treating that examining system contains granule foreign, described sampling probe be provided with filtrator with two pipelines that are connected of makings amount flow quantity control instrument to be measured.
5. the device that utilizes the thermal conductivity detector (TCD) real-time detecting mixing gas component content according to claim 2 is characterized in that: described sampling probe to the pipeline of thermal conductivity detector (TCD) adopts internal diameter less than 2 millimeters tubule footpath pipeline.
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