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CN104198628B - The shunting of a kind of capillary gas chromatograph/Splitless injecting samples mouth carrier gas control system - Google Patents

The shunting of a kind of capillary gas chromatograph/Splitless injecting samples mouth carrier gas control system Download PDF

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CN104198628B
CN104198628B CN201410464465.2A CN201410464465A CN104198628B CN 104198628 B CN104198628 B CN 104198628B CN 201410464465 A CN201410464465 A CN 201410464465A CN 104198628 B CN104198628 B CN 104198628B
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controller
injecting samples
shunting
splitless injecting
flow rate
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CN104198628A (en
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刘召贵
韩高锋
应刚
周立
张坤
蔡克亚
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Jiangsu Skyray Instrument Co Ltd
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Jiangsu Skyray Instrument Co Ltd
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Abstract

The invention discloses the shunting/Splitless injecting samples mouth carrier gas control system of capillary gas chromatograph, including in have the system control unit of the parts such as analog-digital converter, digital to analog converter, single-chip microcomputer and output serial ports;The inlet pressure controller being connected with analog-digital converter and described digital to analog converter;The dottle pin purge flow rate controller being connected with output serial ports;The bypass flow controller being connected with output serial ports;One end is connected with described inlet pressure controller, the shunting that the other end is connected with dottle pin purge flow rate controller/Splitless injecting samples mouth;Chromatographic column, described chromatographic column is connected with described shunting/Splitless injecting samples mouth;The invention enables overall structure to be easily understood, construct clear, capacity of resisting disturbance strong, it is simple to safeguard, it is to avoid a large amount of manpower and materials of the input such as the demarcation of sensor element and calibration in anti-interference, the problem such as debugging difficulty is big in discrete device design and production process.

Description

The shunting of a kind of capillary gas chromatograph/Splitless injecting samples mouth carrier gas control system
Technical field
The present invention relates to chromatograph devices field, it particularly relates to the injection port carrier gas control system of a kind of capillary gas chromatograph.
Background technology
Gas chromatogram (GC) is the experimental technique that a kind of mixture is separated into single component, and it is used to identify sample component and quantitative determine.Such as distilling with physical separation with similar technology difference gas chromatogram (GC) is that by the mixture of vaporization or gas, by the pipe containing certain material, based on material in pipe, to the retention property of different compounds is different, to obtain separating be thus that time-based difference carries out to compound separating that sample is recorded after detector is exactly chromatogram figure based on the other isolation technics of time difference, and each peak represents components different in initial biased sample.One gas chromatography system includes: controlled and pure carrier gas source it sample can be brought into GC system;Injection port, it is the most also as the vaporizer of fluid sample;Chromatographic column, it is achieved separation in time;Detector, when component is passed through, the output valve of the detector signal of telecommunication changes, thus responds component;Certain data processing equipment.
Injection port is exactly that the sample after volatilization is introduced the most frequently used sampling device of carrier gas stream is sample injection mouth and injection valve;And shunt/Splitless injecting samples capillary column has two kinds of operator schemes:
Shunt mode, capillary column has less sample capacity sample size necessary considerably less, generally far fewer than 1 microlitre to prevent chromatographic column from overloading, it is highly difficult that the least sample size operates, shunt mode provides a method that and solves this problem, common sample size is used to be injected into bushing pipe vaporization, then it is analyzed in only a portion being incorporated into chromatographic column, the ratio that remaining major part sets according to post flow and bypass flow also maintains this state through shunting outlet emptying, flow divider unlatching always.The sample of vaporization distributes between chromatographic column (gas-flow resistance is big) and shunting drain (gas-flow resistance is adjustable), as shown in Figure 1;
Splitless injecting samples pattern (such as Fig. 2), this pattern is particularly well-suited to the sample analysis of low concentration, and sample is captured in stigma within the Splitless injecting samples time by it, is vented by the sample gas remaining in injection port after the Splitless injecting samples time simultaneously.This pattern includes two steps: 1 closes flow divider, carrier gas stream distributes between the outlet of dottle pin purge gas and chromatographic column, and column head pressure is set by electronic pressure controller EPC regulation valve, thus sets the flow velocity flowing through chromatographic column;Injected sample, solvent and sample, at vaporizer, by entering chromatographic column in the shunting time requirement set under the promotion of carrier gas, and produce trapping at stigma;2, after the time that do not shunts terminates, open flow divider, the gaseous sample residual emptying that will remain in injection port.Stream and shunt mode are identical Fig. 1 now, GC post case raises column temperature, starts sample component and separates, and the method is effectively for the separation of the boiling point component higher than solvent, solvent peak will be very big, and the peak of target compound is separated by temperature programming to be used with solvent peak.
The carrier gas road control realization mode of the shunting of gas chromatograph/Splitless injecting samples mouth has various ways, main control mode to be divided into the manual regulative mode of mechanical valve and electronic valve automatic control mode.The manual regulative mode of mechanical valve the most substantially falls behind, and electronic valve automatic control mode is as commonly using in high-end gas chromatograph, implementation is the most diversified, control mode is to use discrete electronic components design, the shortcoming of discrete electronic components independent design is that reliability is the highest, safeguards that complicated, Control System Design and manufacture are complicated.
Summary of the invention
In view of this, need to overcome at least one in drawbacks described above of the prior art.The invention provides the shunting/Splitless injecting samples mouth carrier gas control system of a kind of capillary gas chromatograph, including:
System control unit, described system control unit includes analog-digital converter, digital to analog converter, single-chip microcomputer and output serial ports, described single-chip microcomputer is connected with described analog-digital converter and described digital to analog converter, and described output serial ports is connected with described single-chip microcomputer, and output signal;The function that described system is completed is cured in described single-chip microcomputer, forms specific functional circuit;
Inlet pressure controller, described inlet pressure controller is connected with described analog-digital converter and described digital to analog converter;
Dottle pin purge flow rate controller, described output serial ports is connected with dottle pin purge flow rate controller;
Bypass flow controller, described output serial ports is connected with bypass flow controller;
Shunting/Splitless injecting samples mouth, described shunting/Splitless injecting samples mouth one end is connected with described inlet pressure controller, and the other end is connected with dottle pin purge flow rate controller;
Chromatographic column, described chromatographic column is connected with described shunting/Splitless injecting samples mouth;
Wherein, described system control unit controls described split sampling and the realization of Splitless injecting samples function;Under split sampling pattern, described system control unit controls the output of pressure before described inlet pressure controller realizes post, controls described dottle pin purge flow rate controller and realize the output of dottle pin purge flow rate, control described bypass flow controller and realize the output of bypass flow;Under Splitless injecting samples pattern described system control unit control described inlet pressure controller realize post before pressure control, control described dottle pin purge flow rate controller realize dottle pin purge flow rate control, control described bypass flow controller to close in the Splitless injecting samples time arranged, according to the flow output arranged after completing the Splitless injecting samples time.
According in background of invention to described in prior art, the manual regulative mode of mechanical valve the most substantially falls behind, and electronic valve automatic control mode is as commonly using in high-end gas chromatograph, implementation is the most diversified, control mode is to use discrete electronic components design, the shortcoming of discrete electronic components independent design is that reliability is the highest, safeguards that complicated, Control System Design and manufacture are complicated;And the shunting/Splitless injecting samples mouth carrier gas control system of the capillary gas chromatograph that the present invention provides, by inlet pressure controller (EPC), the Integrated design of mass flow controller (MFC) achieves the control requirement of capillary gas chromatograph shunting/Splitless injecting samples mouth carrier gas, meet the pressure under split sampling and Splitless injecting samples and flow-control, system modular Integrated design makes shunting/Splitless injecting samples mouth carrier gas be easily understood, structure is clear, capacity of resisting disturbance is strong, safeguard simple, avoid discrete device design in anti-interference, a large amount of manpower and materials of the input such as the demarcation of sensor element and calibration in the problems such as debugging difficulty is big and production process.
It addition, according to the 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 double-serial port RE232.
Further, described inlet 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 the shunting of user setup/Splitless injecting samples pattern, according to sample injection time program, control instruction is sent to execution unit inlet pressure controller (EPC), dottle pin purge flow rate controller (MFC1), bypass flow controller (MFC2), each controller receive instruction is set after automated closed-loop perform corresponding pressure and flow-control.
System control unit is mainly made up of single-chip microcomputer (MCU), analog-digital converter (AD), digital to analog converter (DA) and double-serial port RE232, AD and DA mainly completes output setting and the feedback of status of inlet pressure controller (EPC), and double-serial port RE232 mainly completes and dottle pin purge flow rate controller (MFC1), the output setting of bypass flow controller (MFC2) and feedback of status.System control unit (MCU) is according to the state that arranges of user and parameter, according to shunting or shunt mode do not go to perform the setting of EPC, MFC1, MFC2 and the monitoring of feedback states, be the system requirement that meets the test sample sample introduction of capillary gas chromatograph split sampling mouth and Splitless injecting samples lancet pair.
Inlet pressure controller (EPC) is the miniature electronic pressure controller VSO-EP using the U.S., the simulation electronic control signal changing or fixing from system control unit is converted into change or fixing pneumatic output (gas pressure output) by controller, is i.e. inputted the gas pressure control realizing inlet pressure 0-50psi by the analogue signal of 0-5V.VOS-EP controller has that volume is little, control accuracy is high, response time is short, gas flow path is corrosion-resistant, internal closed loop controls and the feature such as pressure sensor output feedback, the internal closed loop control wherein possessed and pressure sensor output feedback function embody the integrated advantage of the design, decrease in system design design and the resource consumptions of production maintenance such as electronic circuitry design, maintenance and the pick up calibrations that EPC controls.
Dottle pin purge flow rate controller (MFC1) and bypass flow controller (MFC2) use the mass flow controller MFC(Mass Flow that Switzerland is advanced Controllers), change or the fixing digital and electronic control signal from system control unit is changed to change or fixing pneumatic output (gas flow output) by controller.MFC1 supplied with digital signal 0-100 mL/min, corresponding output flow 0-100mL/min, MFC2 supplied with digital signal 0-1250 mL/min, corresponding output flow 0-1250mL/min.MFC1 and MFC2 has that volume is little, control accuracy is high, response time is short, gas flow path is corrosion-resistant, internal closed loop controls and the feature such as output flow digital feedback, the internal closed loop control wherein possessed and pressure sensor output feedback function embody the integrated advantage of the design, decrease in system design design and the resource consumptions of production maintenance such as electronic circuitry design, maintenance and the pick up calibrations that MFC controls.
Aspect and advantage that the present invention adds will part be given in the following description, and part will become apparent from the description below, or is recognized by the practice of the present invention.
Accompanying drawing explanation
Above-mentioned and/or the additional aspect of the present invention and advantage will be apparent from easy to understand from the following description of the accompanying drawings of embodiments, wherein:
Schematic diagram under Fig. 1 shunting/Splitless injecting samples port system prior art SHUNT state;
Schematic diagram under Fig. 2 shunting/Splitless injecting samples port system prior art not SHUNT state;
The carrier gas control system schematic diagram of Fig. 3 present invention.
Wherein, 11 injection port flow control valves, 12 dottle pin nut and dottle pins, 13 dottle pin purge gass control parts, 14 bushing pipes, and 15 flow dividers (are opened), 16 shunting control of export parts, 17 flow dividers (close), 31 system control units, 32 inlet pressure controllers, 33 dottle pin purge flow rate controllers, 34 bypass flow controllers, A carrier gas (He), B chromatographic column flow LmL/min.
Detailed description of the invention
The embodiments described below is exemplary, is only used for explaining the present invention, and is not construed as limiting the claims.
Shunting/Splitless injecting samples mouth carrier gas the control system of the capillary gas chromatograph of the present invention, the wherein schematic diagram under Fig. 1 shunting/Splitless injecting samples port system prior art SHUNT state are described below with reference to accompanying drawings;Schematic diagram under Fig. 2 shunting/Splitless injecting samples port system prior art not SHUNT state;The carrier gas control system schematic diagram of Fig. 3 present invention.
According to embodiments of the invention, as it is shown on figure 3, the shunting/Splitless injecting samples mouth carrier gas control system of the capillary gas chromatograph of present invention offer, including:
System control unit 31, described system control unit 31 includes analog-digital converter AD, digital to analog converter DA, single-chip microprocessor MCU and output serial ports, described single-chip microprocessor MCU is connected with described analog-digital converter DA and described digital to analog converter AD, described output serial ports is connected with described single-chip microprocessor MCU, and output signal, the function that described system is completed is cured in described single-chip microprocessor MCU, forms specific functional circuit;
Inlet pressure controller EPC(32), described inlet pressure controller EPC(32) it is connected with described analog-digital converter AD and described digital to analog converter DA;
Dottle pin purge flow rate controller MFC1(33), described output serial ports and dottle pin purge flow rate controller are connected MFC1(33);
Bypass flow controller MFC2(34), described output serial ports and bypass flow controller MFC2(34) it is connected;
Shunting/Splitless injecting samples mouth, described shunting/Splitless injecting samples mouth one end and described inlet pressure controller EPC(32) it is connected, the other end and dottle pin purge flow rate controller MFC1(33) it is connected;
Chromatographic column, described chromatographic column is connected with described shunting/Splitless injecting samples mouth.
According in background of invention to described in prior art, the manual regulative mode of mechanical valve the most substantially falls behind, and electronic valve automatic control mode is as commonly using in high-end gas chromatograph, implementation is the most diversified, control mode is to use discrete electronic components design, the shortcoming of discrete electronic components independent design is that reliability is the highest, safeguards that complicated, Control System Design and manufacture are complicated;And the shunting/Splitless injecting samples mouth carrier gas control system of the capillary gas chromatograph that the present invention provides, by inlet pressure controller (EPC), the Integrated design of mass flow controller (MFC) achieves the control requirement of capillary gas chromatograph shunting/Splitless injecting samples mouth carrier gas, meet the pressure under split sampling and Splitless injecting samples and flow-control, system modular Integrated design makes shunting/Splitless injecting samples mouth carrier gas be easily understood, structure is clear, capacity of resisting disturbance is strong, safeguard simple, avoid discrete device design in anti-interference, a large amount of manpower and materials of the input such as the demarcation of sensor element and calibration in the problems such as debugging difficulty is big and production process.
According to some embodiments of the present invention, described output serial ports is double-serial port RE232.
According to some embodiments of the present invention, described inlet pressure controller EPC(32) it is 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) it is mass flow controller.
According to some embodiments of the present invention, as it is shown on figure 3, the shunting/Splitless injecting samples mouth injection port that to be capillary gas chromatograph the most frequently used, it both can be used as split sampling mouth, it is possible to as Splitless injecting samples mouth.The split sampling being implemented in combination with capillary gas chromatograph of shunting/Splitless injecting samples mouth and shunting/Splitless injecting samples mouth carrier gas control system and the realization of Splitless injecting samples function.Under split sampling pattern, described system control unit controls inlet pressure controller EPC(32) realize post before pressure 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 control inlet pressure controller EPC(32) realize post before pressure control, control dottle pin purge flow rate controller MFC1(33) realize dottle pin purge flow rate control, control bypass flow controller MFC2(34) close within the Splitless injecting samples time arranged, according to the flow output arranged after completing the Splitless injecting samples time.
System control unit 31 is after receiving the shunting of user setup/Splitless injecting samples pattern, according to sample injection time program, control instruction is sent to execution unit inlet 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 perform corresponding pressure and flow-control.
System control unit is mainly made up of single-chip microprocessor MCU, analog-digital converter AD, digital to analog converter DA and double-serial port RE232, AD and DA mainly completes inlet pressure controller EPC(32) output setting and feedback of status, double-serial port RE232 mainly completes 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 the state that arranges of user and parameter, according to shunting or shunt mode do not go to perform the setting of EPC, MFC1, MFC2 and the monitoring of feedback states, be the system requirement that meets the test sample sample introduction of capillary gas chromatograph split sampling mouth and Splitless injecting samples lancet pair.
Inlet pressure controller EPC(32) it is the miniature electronic pressure controller VSO-EP using the U.S., the simulation electronic control signal changing or fixing from system control unit is converted into change or fixing pneumatic output (gas pressure output) by controller, is i.e. inputted the gas pressure control realizing inlet pressure 0-50psi by the analogue signal of 0-5V.VOS-EP controller has that volume is little, control accuracy is high, response time is short, gas flow path is corrosion-resistant, internal closed loop controls and the feature such as pressure sensor output feedback, the internal closed loop control wherein possessed and pressure sensor output feedback function embody the integrated advantage of the design, decrease in system design design and the resource consumptions of production maintenance such as electronic circuitry design, maintenance and the pick up calibrations that EPC controls.
Dottle pin purge flow rate controller MFC1(33) and bypass flow controller MFC2(34) use the advanced mass flow controller MFC(Mass Flow of Switzerland Controllers), change or the fixing digital and electronic control signal from system control unit is changed to change or fixing pneumatic output (gas flow output) by controller.MFC1 supplied with digital signal 0-100 mL/min, corresponding output flow 0-100mL/min, MFC2 supplied with digital signal 0-1250 mL/min, corresponding output flow 0-1250mL/min.MFC1 and MFC2 has that volume is little, control accuracy is high, response time is short, gas flow path is corrosion-resistant, internal closed loop controls and the feature such as output flow digital feedback, the internal closed loop control wherein possessed and pressure sensor output feedback function embody the integrated advantage of the design, decrease in system design design and the resource consumptions of production maintenance such as electronic circuitry design, maintenance and the pick up calibrations that EPC controls.
Although the detailed description of the invention of the present invention is described in detail by the multiple illustrative examples with reference to the present invention, it must be understood that, those skilled in the art can be designed that multiple other improvement and embodiment, these improve and embodiment will fall within spirit and scope.Specifically, within the scope of aforementioned disclosure, accompanying drawing and claim, rational modification and improvement can be made in terms of the layout of parts and/or sub-combination layout, without departing from the spirit of the present invention.Except the modification in terms of parts and/or layout and improvement, its scope is defined by the appended claims and the equivalents thereof.

Claims (3)

1. the shunting of a capillary gas chromatograph/Splitless injecting samples mouth carrier gas control system, it is characterised in that including:
System control unit, described system control unit includes analog-digital converter, digital to analog converter, single-chip microcomputer and output serial ports, described single-chip microcomputer is connected with described analog-digital converter and described digital to analog converter, described output serial ports is connected with described single-chip microcomputer, and output signal, the function that described system is completed is cured in described single-chip microcomputer, forms specific functional circuit;
Inlet pressure controller, described inlet pressure controller is connected with described analog-digital converter and described digital to analog converter;
Dottle pin purge flow rate controller, described output serial ports is connected with dottle pin purge flow rate controller;
Bypass flow controller, described output serial ports is connected with bypass flow controller;
Shunting/Splitless injecting samples mouth, described shunting/Splitless injecting samples mouth one end is connected with described inlet pressure controller, and the other end is connected with dottle pin purge flow rate controller;
Chromatographic column, described chromatographic column is connected with described shunting/Splitless injecting samples mouth;
Wherein, described system control unit controls split sampling and the realization of Splitless injecting samples function;Under split sampling pattern, described system control unit controls the output of pressure before described inlet pressure controller realizes post, controls described dottle pin purge flow rate controller and realize the output of dottle pin purge flow rate, control described bypass flow controller and realize the output of bypass flow;Under Splitless injecting samples pattern described system control unit control described inlet pressure controller realize post before pressure control, control described dottle pin purge flow rate controller realize dottle pin purge flow rate control, control described bypass flow controller to close in the Splitless injecting samples time arranged, according to the flow output arranged after completing the Splitless injecting samples time
Wherein, described dottle pin purge flow rate controller and described bypass flow controller are mass flow controller.
The shunting of capillary gas chromatograph the most according to claim 1/Splitless injecting samples mouth carrier gas control system, it is characterised in that described output serial ports is double-serial port RE232.
The shunting of capillary gas chromatograph the most according to claim 2/Splitless injecting samples mouth carrier gas control system, it is characterised in that described inlet pressure controller is miniature electronic pressure controller.
CN201410464465.2A 2014-09-12 2014-09-12 The shunting of a kind of capillary gas chromatograph/Splitless injecting samples mouth carrier gas control system Active CN104198628B (en)

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