CN104198628A - Flow distribution/non-flow distribution sample inlet carrier gas control system of capillary gas chromatograph instrument - Google Patents
Flow distribution/non-flow distribution sample inlet carrier gas control system of capillary gas chromatograph instrument Download PDFInfo
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- CN104198628A CN104198628A CN201410464465.2A CN201410464465A CN104198628A CN 104198628 A CN104198628 A CN 104198628A CN 201410464465 A CN201410464465 A CN 201410464465A CN 104198628 A CN104198628 A CN 104198628A
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Abstract
The invention discloses a flow distribution/non-flow distribution sample inlet carrier gas control system of a capillary gas chromatograph instrument. The system comprises a system control unit in which parts such as an analog-digital converter, a digital-analog converter, a single chip and an output serial port are arranged, a sample inlet pressure controller connected with the analog-digital converter and the digital-analog converter, a spacing cushion purge flow controller connected with the output serial port, a flow distribution/non-flow distribution sample inlet with one end connected with the sample inlet pressure controller and the other end connected with the spacing cushion purge flow controller, and a chromatographic column connected with the flow distribution/non-flow distribution sample inlet. The system is simple and easy to understand in overall structure, clear in construction, good in anti-jamming capability and easy to maintain; the problems of jamming resistance, high debugging difficulty and the like in the design of a discrete device and a large amount of manpower and material resources in calibration and the like of a sensor part in a production process are avoided.
Description
Technical field
The present invention relates to chromatograph apparatus field, specifically, relate to a kind of injection port carrier gas control system of capillary gas chromatograph.
Background technology
Gas chromatography (GC) is a kind of experimental technique that potpourri is separated into single component, and it is used to sample component to identify and quantitative measurement.With physical separation such as distillation and similarly the different gas chromatographies of technology (GC) be that by the potpourri of vaporization or gas, the pipe by containing certain material obtains to the retention property difference of different compounds based on material in pipe that separated to be exactly time-based difference like this carry out to compound that sample separation is recorded after detecting device is exactly chromatogram figure based on other isolation technics of mistiming, each peak represents components different in initial biased sample.A gas chromatography system comprises: it can bring sample into GC system controlled and pure carrier gas source; Injection port, it is simultaneously also as the vaporizer of fluid sample; Chromatographic column, realizes separation in time; Detecting device, when component is passed through, the output valve of detecting device electric signal changes, thereby component is made to response; Certain data processing equipment.
Injection port is exactly the sample after volatilization to be introduced to carrier gas to flow the most frequently used sampling device be sample injection mouth and sampling valve; And shunt/Splitless injecting samples has two kinds of operator schemes with capillary column:
Shunt mode, capillary column has less sample capacity sample size necessary considerably less, conventionally far fewer than 1 microlitre, to prevent chromatographic column, overload, it is very difficult that little sample size like this operates, shunt mode provides a kind of method to solve this problem, adopt common sample size to be injected into bushing pipe vaporization, then only a part is wherein incorporated in chromatographic column and is analyzed, the ratio that all the other major parts are set according to post flow and bypass flow is through shunting outlet emptying, and this state is opened and maintained always to diverting valve.The sample of vaporization distributes between chromatographic column (gas-flow resistance is large) and shunting drain (gas-flow resistance is adjustable), as shown in Figure 1;
Splitless injecting samples pattern (as Fig. 2), this pattern is specially adapted to the sample analysis of low concentration, and it is captured in column cap at Splitless injecting samples in the time by sample, will remain in the sample gas emptying of injection port later in the Splitless injecting samples time simultaneously.This pattern comprises two steps: 1 closes diverting valve,, carrier gas stream distributes between the outlet of dottle pin sweep gas and chromatographic column, and column head pressure is set by electronic pressure controller EPC variable valve, thereby sets the flow velocity that flows through chromatographic column; Injected sample, solvent and sample be at vaporizer, under the promotion of carrier gas, by entering chromatographic column in the shunting time requirement of setting, and produces trapping at column cap; 2 after the not shunting time finishes, and opens diverting valve, by the residual emptying of gaseous sample remaining in injection port.Stream and shunt mode are identical Fig. 1 now, GC post case rising column temperature, starts sample component separation, and the method is effectively for the separation of the boiling point component higher than solvent, solvent peak will be very large, adopt temperature programme that the peak of target compound is separated with solvent peak.
Implementation is controlled on the carrier gas road of shunting/Splitless injecting samples mouth of gas chromatograph various ways, and main control mode is divided into mechanical valve manual adjustments mode and electrovalve automatic control mode.Mechanical valve manual adjustments mode obviously falls behind in some aspects, and electrovalve automatic control mode is as generally using in high-end gas chromatograph, implementation is variation also, control mode is to adopt discrete electronic components design, the shortcoming of discrete electronic components independent design is that reliability is not high, safeguards that complexity, Control System Design and manufacture are complicated.
Summary of the invention
In view of this, need to overcome at least one in above-mentioned defect of the prior art.Shunting/Splitless injecting samples mouth carrier gas the control system that the invention provides a kind of capillary gas chromatograph, comprising:
System control unit, described system control unit comprises analog to digital converter, digital to analog converter, single-chip microcomputer and output serial ports, described single-chip microcomputer and described analog to digital converter and described digital to analog converter are connected, and described output serial ports and described single-chip microcomputer are connected, and output signal; Described single-chip microcomputer is the single-chip microcomputer with the specific function circuit of described system, and the function that described system completes is cured in described single-chip microcomputer, forms specific functional circuit;
Injection port pressure controller, described injection port pressure controller be connected with described analog to digital converter and described digital to analog converter;
Dottle pin purge flow rate controller, described output serial ports and dottle pin purge flow rate controller are connected;
Bypass flow controller, described output serial ports and bypass flow controller are connected;
Shunting/Splitless injecting samples mouth, described shunting/Splitless injecting samples mouth one end and described injection port pressure controller are connected, and the other end and dottle pin purge flow rate controller are connected;
Chromatographic column, described chromatographic column and described shunting/Splitless injecting samples mouth are connected;
Wherein, described system control unit is controlled the realization of described split sampling and Splitless injecting samples function; Under split sampling pattern, described system control unit is controlled described injection port pressure controller and is realized the output of pressure before post, controls described dottle pin purge flow rate controller and realize the output of dottle pin purge flow rate, control the output that described bypass flow controller is realized bypass flow; Under Splitless injecting samples pattern, described system control unit is controlled described injection port pressure controller and is realized the control of pressure before post, controls described dottle pin purge flow rate controller and realize dottle pin purge flow rate and control, control described bypass flow controller and close in the Splitless injecting samples time arranging, complete than split sampling and according to the flow arranging, export after the time.
According to the present invention in background technology to described in prior art, mechanical valve manual adjustments mode obviously falls behind in some aspects, and electrovalve automatic control mode is as generally using in high-end gas chromatograph, implementation is variation also, control mode is to adopt discrete electronic components design, the shortcoming of discrete electronic components independent design is that reliability is not high, safeguards that complexity, Control System Design and manufacture are complicated, and shunting/Splitless injecting samples mouth carrier gas control system of capillary gas chromatograph provided by the invention, by injection port pressure controller (EPC), the Integrated design of mass flow controller (MFC) has been realized the control requirement of capillary gas chromatograph shunting/Splitless injecting samples mouth carrier gas, meet pressure and flow control under split sampling and Splitless injecting samples, system modular Integrated design is easily understood the carrier gas of shunting/Splitless injecting samples mouth, it is clear to construct, antijamming capability is strong, safeguard simple, avoided anti-interference in discrete device design, a large amount of manpower and materials that in the problems such as debugging difficulty is large and production run, the demarcation of sensor element and calibration etc. drop into.
In addition, according to shunting/Splitless injecting samples mouth carrier gas control system of capillary gas chromatograph disclosed by the invention, also there is following additional technical feature:
Further, described output serial ports is two serial ports RE232.
Further, described injection port pressure controller is miniature electronic pressure device.
Further, described dottle pin purge flow rate controller and described bypass flow controller are mass flow controller.
System control unit is after receiving shunting/Splitless injecting samples pattern of user's setting, according to sample injection time program, steering order is sent to execution unit injection port pressure controller (EPC), dottle pin purge flow rate controller (MFC1), bypass flow controller (MFC2), each controller receive instruction is set after automated closed-loop carry out corresponding pressure and flow control.
System control unit is mainly comprised of single-chip microcomputer (MCU), analog to digital converter (AD), digital to analog converter (DA) and two serial ports RE232, AD and DA mainly complete output setting and the feedback of status of injection port pressure controller (EPC), and two serial ports RE232 mainly complete output setting and the feedback of status with dottle pin purge flow rate controller (MFC1), bypass flow controller (MFC2).System control unit (MCU) is according to user's the state that arranges and parameter, according to shunting or not shunt mode go to carry out the setting of EPC, MFC1, MFC2 and the monitoring of feedback states, be the requirement that system meets capillary gas chromatograph split sampling mouth and the right test sample feeding of Splitless injecting samples lancet.
Injection port pressure controller (EPC) is the miniature electronic pressure controller VSO-EP that adopts the U.S., controller is converted into the variation from system control unit or fixing simulation electronic control signal to change or fixing pneumatic output (gaseous tension output), and the gaseous tension of realizing injection port pressure 0-50psi by the simulating signal input of 0-5V is controlled.The features such as VOS-EP controller has that volume is little, control accuracy is high, the response time is short, gas flow path is corrosion-resistant, inner closed-loop control and pressure sensor output feedback, the inside closed-loop control wherein possessing and pressure sensor output feedback function have embodied the design's integrated advantage, have reduced in system the designs such as electronic circuitry design, maintenance and pick up calibration of EPC control and the resource consumption of production maintenance.
Dottle pin purge flow rate controller (MFC1) and bypass flow controller (MFC2) adopt Switzerland advanced person's mass flow controller MFC(Mass Flow Controllers), controller is changed to variation or fixing pneumatic output (gas flow output) by the variation from system control unit or fixing digital and electronic control signal.MFC1 supplied with digital signal 0-100 mL/min, corresponding delivery rate 0-100mL/min, MFC2 supplied with digital signal 0-1250 mL/min, corresponding delivery rate 0-1250mL/min.The features such as MFC1 and MFC2 have that volume is little, control accuracy is high, the response time is short, gas flow path is corrosion-resistant, inner closed-loop control and delivery rate digital feedback, the inside closed-loop control wherein possessing and pressure sensor output feedback function have embodied the design's integrated advantage, have reduced in system the designs such as electronic circuitry design, maintenance and pick up calibration of MFC control and the resource consumption of production maintenance.
The aspect that the present invention is additional and advantage in the following description part provide, and part will become obviously from the following description, or recognize by practice of the present invention.
Accompanying drawing explanation
Above-mentioned and/or additional aspect of the present invention and advantage will become from the following description of the accompanying drawings of embodiments and obviously and easily understand, wherein:
Fig. 1 shunting/Splitless injecting samples port system prior art is divided the schematic diagram under stream mode;
Fig. 2 shunting/Splitless injecting samples port system prior art is regardless of the schematic diagram under stream mode;
Fig. 3 carrier gas control system of the present invention schematic diagram.
Wherein, 11 injection port flowrate control valves, 12 dottle pin nut and dottle pins, 13 dottle pin sweep gas control assemblies, 14 bushing pipes, 15 diverting valves (opening), 16 shunting outlet control assemblies, 17 diverting valves (pass), 31 system control units, 32 injection port pressure controllers, 33 dottle pin purge flow rate controllers, 34 bypass flow controllers, A carrier gas (He), B chromatographic column flow LmL/min.
Embodiment
The embodiment the following describes is exemplary, only for explaining the present invention, and can not be interpreted as limitation of the present invention.
Shunting/Splitless injecting samples mouth carrier gas control system of describing below with reference to accompanying drawings capillary gas chromatograph of the present invention, wherein Fig. 1 shunting/Splitless injecting samples port system prior art is divided the schematic diagram under stream mode; Fig. 2 shunting/Splitless injecting samples port system prior art is regardless of the schematic diagram under stream mode; Fig. 3 carrier gas control system of the present invention schematic diagram.
According to embodiments of the invention, as shown in Figure 3, shunting/Splitless injecting samples mouth carrier gas control system of capillary gas chromatograph provided by the invention, comprising:
System control unit 31, described system control unit 31 comprises analog to digital converter AD, digital to analog converter DA, single-chip microprocessor MCU and output serial ports, described single-chip microprocessor MCU and described analog to digital converter DA and described digital to analog converter AD are connected, described output serial ports and described single-chip microprocessor MCU are connected, and output signal;
Injection port pressure controller EPC(32), described injection port pressure controller EPC(32) be connected with described analog to digital converter AD and described digital to analog converter DA;
Dottle pin purge flow rate controller MFC1(33), described output serial ports and the dottle pin purge flow rate controller MFC1(33 that is connected);
Bypass flow controller MFC2(34), described output serial ports and bypass flow controller MFC2(34) be connected;
Shunting/Splitless injecting samples mouth, described shunting/Splitless injecting samples mouth one end and described injection port pressure controller EPC(32) be connected, the other end and dottle pin purge flow rate controller MFC1(33) be connected;
Chromatographic column, described chromatographic column and described shunting/Splitless injecting samples mouth are connected.
According to the present invention in background technology to described in prior art, mechanical valve manual adjustments mode obviously falls behind in some aspects, and electrovalve automatic control mode is as generally using in high-end gas chromatograph, implementation is variation also, control mode is to adopt discrete electronic components design, the shortcoming of discrete electronic components independent design is that reliability is not high, safeguards that complexity, Control System Design and manufacture are complicated, and shunting/Splitless injecting samples mouth carrier gas control system of capillary gas chromatograph provided by the invention, by injection port pressure controller (EPC), the Integrated design of mass flow controller (MFC) has been realized the control requirement of capillary gas chromatograph shunting/Splitless injecting samples mouth carrier gas, meet pressure and flow control under split sampling and Splitless injecting samples, system modular Integrated design is easily understood the carrier gas of shunting/Splitless injecting samples mouth, it is clear to construct, antijamming capability is strong, safeguard simple, avoided anti-interference in discrete device design, a large amount of manpower and materials that in the problems such as debugging difficulty is large and production run, the demarcation of sensor element and calibration etc. drop into.
According to some embodiments of the present invention, described output serial ports is two serial ports RE232.
According to some embodiments of the present invention, described injection port pressure controller EPC(32) be miniature electronic pressure device.
According to some embodiments of the present invention, described dottle pin purge flow rate controller MFC1(33) and described bypass flow controller MFC2(34) be mass flow controller.
According to some embodiments of the present invention, as shown in Figure 3, shunting/Splitless injecting samples mouth is the most frequently used injection port of capillary gas chromatograph, and it both can be used as split sampling mouth, also can be used as Splitless injecting samples mouth.The combination of shunting/Splitless injecting samples mouth and shunting/Splitless injecting samples mouth carrier gas control system has realized the split sampling of capillary gas chromatograph and the realization of Splitless injecting samples function.Under split sampling pattern, described system control unit is controlled injection port pressure controller EPC(32) realize pressure before post output, control dottle pin purge flow rate controller MFC1(33) realize the output of dottle pin purge flow rate, control bypass flow controller MFC2(34) realize the output of bypass flow.Under Splitless injecting samples pattern, system control unit is controlled injection port pressure controller EPC(32) realize pressure before post control, control dottle pin purge flow rate controller MFC1(33) realize dottle pin purge flow rate and control, control bypass flow controller MFC2(34) at the Splitless injecting samples arranging, in the time, close, complete after sample introduction according to the flow output arranging.
System control unit 31 is after receiving shunting/Splitless injecting samples pattern of user's setting, according to sample injection time program, steering order is sent to execution unit injection port pressure controller EPC(32), dottle pin purge flow rate controller MFC1 (33), bypass flow controller MFC2 (34), each controller receive instruction is set after automated closed-loop carry out corresponding pressure and flow control.
System control unit is mainly comprised of single-chip microprocessor MCU, analog to digital converter AD, digital to analog converter DA and two serial ports RE232, AD and DA mainly complete injection port pressure controller EPC(32) output setting and feedback of status, two serial ports RE232 mainly complete and dottle pin purge flow rate controller MFC1(33), bypass flow controller MFC2(34) output setting and feedback of status.Single-chip microprocessor MCU in system control unit 31 is according to user's the state that arranges and parameter, according to shunting or not shunt mode go to carry out the setting of EPC, MFC1, MFC2 and the monitoring of feedback states, be the requirement that system meets capillary gas chromatograph split sampling mouth and the right test sample feeding of Splitless injecting samples lancet.
Injection port pressure controller EPC(32) be the miniature electronic pressure controller VSO-EP that adopts the U.S., controller is converted into the variation from system control unit or fixing simulation electronic control signal to change or fixing pneumatic output (gaseous tension output), and the gaseous tension of realizing injection port pressure 0-50psi by the simulating signal input of 0-5V is controlled.The features such as VOS-EP controller has that volume is little, control accuracy is high, the response time is short, gas flow path is corrosion-resistant, inner closed-loop control and pressure sensor output feedback, the inside closed-loop control wherein possessing and pressure sensor output feedback function have embodied the design's integrated advantage, have reduced in system the designs such as electronic circuitry design, maintenance and pick up calibration of EPC control and the resource consumption of production maintenance.
Dottle pin purge flow rate controller MFC1(33) and bypass flow controller MFC2(34) adopt Switzerland advanced person's mass flow controller MFC(Mass Flow Controllers), controller is changed to variation or fixing pneumatic output (gas flow output) by the variation from system control unit or fixing digital and electronic control signal.MFC1 supplied with digital signal 0-100 mL/min, corresponding delivery rate 0-100mL/min, MFC2 supplied with digital signal 0-1250 mL/min, corresponding delivery rate 0-1250mL/min.The features such as MFC1 and MFC2 have that volume is little, control accuracy is high, the response time is short, gas flow path is corrosion-resistant, inner closed-loop control and delivery rate digital feedback, the inside closed-loop control wherein possessing and pressure sensor output feedback function have embodied the design's integrated advantage, have reduced in system the designs such as electronic circuitry design, maintenance and pick up calibration of EPC control and the resource consumption of production maintenance.
Although the specific embodiment of the present invention is described in detail with reference to a plurality of illustrative examples of the present invention, but it must be understood that, those skilled in the art can design multiple other improvement and embodiment, and these improve and within embodiment will drop on spirit and scope.Particularly, within the scope of aforementioned open, accompanying drawing and claim, can aspect the layout of parts and/or subordinate composite configuration, make rational modification and improvement, and can not depart from spirit of the present invention.Except modification and the improvement of parts and/or layout aspect, its scope is limited by claims and equivalent thereof.
Claims (4)
1. shunting/Splitless injecting samples mouth carrier gas control system of capillary gas chromatograph, is characterized in that, comprising:
System control unit, described system control unit comprises analog to digital converter, digital to analog converter, single-chip microcomputer and output serial ports, described single-chip microcomputer and described analog to digital converter and described digital to analog converter are connected, described output serial ports and described single-chip microcomputer are connected, and output signal, described single-chip microcomputer is the single-chip microcomputer with the specific function circuit of described system;
Injection port pressure controller, described injection port pressure controller be connected with described analog to digital converter and described digital to analog converter;
Dottle pin purge flow rate controller, described output serial ports and dottle pin purge flow rate controller are connected;
Bypass flow controller, described output serial ports and bypass flow controller are connected;
Shunting/Splitless injecting samples mouth, described shunting/Splitless injecting samples mouth one end and described injection port pressure controller are connected, and the other end and dottle pin purge flow rate controller are connected;
Chromatographic column, described chromatographic column and described shunting/Splitless injecting samples mouth are connected;
Wherein, described system control unit is controlled the realization of described split sampling and Splitless injecting samples function; Under split sampling pattern, described system control unit is controlled described injection port pressure controller and is realized the output of pressure before post, controls described dottle pin purge flow rate controller and realize the output of dottle pin purge flow rate, control the output that described bypass flow controller is realized bypass flow; Under Splitless injecting samples pattern, described system control unit is controlled described injection port pressure controller and is realized the control of pressure before post, controls described dottle pin purge flow rate controller and realize dottle pin purge flow rate and control, control described bypass flow controller and close in the Splitless injecting samples time arranging, complete than split sampling and according to the flow arranging, export after the time.
2. shunting/Splitless injecting samples mouth carrier gas control system of capillary gas chromatograph according to claim 1, is characterized in that, described output serial ports is two serial ports RE232.
3. shunting/Splitless injecting samples mouth carrier gas control system of capillary gas chromatograph according to claim 2, is characterized in that, described injection port pressure controller is miniature electronic pressure device.
4. shunting/Splitless injecting samples mouth carrier gas control system of capillary gas chromatograph according to claim 1, is characterized in that, described dottle pin purge flow rate controller and described bypass flow controller are mass flow controller.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107561200A (en) * | 2017-10-13 | 2018-01-09 | 江苏天瑞仪器股份有限公司 | A kind of pressure flow electronic control system for injection port of chromatograph |
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| CN104198628B (en) | 2016-11-23 |
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