CN107727780A - The electron pressure control device and method of on-line chromatograph - Google Patents
The electron pressure control device and method of on-line chromatograph Download PDFInfo
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- CN107727780A CN107727780A CN201710763949.0A CN201710763949A CN107727780A CN 107727780 A CN107727780 A CN 107727780A CN 201710763949 A CN201710763949 A CN 201710763949A CN 107727780 A CN107727780 A CN 107727780A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/32—Control of physical parameters of the fluid carrier of pressure or speed
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- Treatment Of Liquids With Adsorbents In General (AREA)
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Abstract
The present invention relates to a kind of electron pressure control device and method of on-line chromatograph, the electron pressure control device includes chromatographic column, electron pressure/flow-control module, the electron pressure/flow-control module are arranged on the upstream of the chromatographic column, and pressure before post or flow are controlled；Detection process unit, the detection process unit are arranged on the downstream of the chromatographic column, and testing sample is analyzed and exports testing result, while the actual retention time of selected compound is sent into feedback control module；Feedback control module, the feedback control module carries out function correction according to pressure before post or the controlling value of flow with actual retention time, and retention time to be locked is substituted into the pressure of the next testing sample of correction function acquisition or the controlling value of flow and is sent to electron pressure/flow-control module.There is the present invention retention time to correct automatically, and measurement result is accurate, stably, instrument for a long time effectively operation the advantages that.
Description
Technical field
The present invention relates to chromatography field, the electron pressure control device and method of more particularly to a kind of on-line chromatograph.
Background technology
On-line chromatograph longtime running automatic progress sampled measurements analysis, calculates to be measured in analyzer house according to establishing method
Concentration of component, and record transmission measurement result.Existing on-line chromatograph can often ensure each material retention time within a couple of days
Repeatability, accurately material is carried out it is qualitative and quantitative, but after running the several months, due to operation condition of chromatogram (such as flow rate of carrier gas,
Column temperature, capillary column specification and detector type) and chromatogram column bleed aging etc. influence, material retention time will drift about,
Moieties retention time front and rear difference tens of seconds, cause to perplex for qualitative and further quantitative calculate of peak identification, export
The measurement result of mistake.To solve this problem, existing on-line chromatograph is often through the confidential interval for expanding peak window, part
Increase the adaptability of measuring method, in combination with periodic calibrating, by setting calibration result threshold value, prompt custom system to exist and ask
Topic, and then carry out manual maintenance.However, aforesaid way still has following defect：
1st, peak window is set with limit range, and the scope tends not to the range of drift for including peak；2nd, calibration frequency is high, mark
Gas consumption is big；3rd, it is only capable of being solved after problem occurs, the accuracy of measurement result can not be ensured for a long time；4th, need artificial
On-site maintenance, the effective run time of instrument are short；5th, after being changed to instrument condition, debug time length；6th, different instruments it
Between, method can not transplant；7th, automaticity is low, is not suitable for networking multiple instruments test platform.
The content of the invention
It is high the invention provides a kind of automaticity in order to solve the deficiency in above-mentioned prior art, calibration frequency
Rate is low, the electron pressure control device for the on-line chromatograph that instrument is effectively run for a long time.
The purpose of the present invention is achieved through the following technical solutions：
A kind of electron pressure control device of on-line chromatograph, including chromatographic column, the electron pressure control device also include：
Electron pressure/flow-control module, the electron pressure/flow-control module are arranged on the upper of the chromatographic column
Trip, is controlled to pressure before post or flow；
Detection process unit, the detection process unit are arranged on the downstream of the chromatographic column, testing sample are divided
Analyse and export testing result, while the actual retention time of selected compound is sent to feedback control module；
Feedback control module, the feedback control module is according to pressure before post or the controlling value of flow and actual retention time
Function correction is carried out, and retention time to be locked is substituted into correction function and obtains the pressure of next testing sample or the control of flow
It is worth and is sent to electron pressure/flow-control module.
The present invention also provide a kind of retention time correct automatically, the electron pressure of the on-line chromatograph of measurement result accurate stable
Control method, the electron pressure control method comprise the following steps：
(A1) compound is selected, the retention time to be locked of the compound is tR0；
(A2) feedback control module by retention time to be locked substitute into first function obtain testing sample post before pressure or
Flow control value is simultaneously sent to electron pressure/flow-control module；
(A3) pressure before post or flow are adjusted to the controlling value by electron pressure/flow-control module, and test sample is treated in analysis
Product, the actual retention time of the selected compound of detection process unit output to feedback control module；
(A4) feedback control module is carried out according to Pressure control or flow control value before post and actual retention time to first function
Correct and then obtain second function, and retention time to be locked is substituted into second function and obtains pressure before the post of next testing sample
Or flow control value；
(A5) (A3) step is repeated, reduces the gap of actual retention time and retention time to be locked.
According to above-mentioned compress control method, it is preferable that the compress control method further comprises：
(B1) pressure or flow before change post, the data group of pressure or flow and retention time carries out secondary song before obtaining post
Line is fitted, and obtains first function：
(B1) step is located at before (A1) step.
According to above-mentioned compress control method, it is preferable that the second function is translated by first function and obtained.
According to above-mentioned compress control method, alternatively, retention time t to be lockedR0Debugged for on-line chromatograph and complete to carry out
When testing sample is analyzed, the actual retention time of compound is selected.
Compared with prior art, the device have the advantages that being：
1st, the present invention is corrected using pressure before post or the controlling value of flow with actual retention time to function so that is protected
Stay time continuous approach locking retention time, it is ensured that Stability and veracity during on-line chromatograph longtime running qualitatively and quantitatively,
So as to reduce calibration frequency, gas usage amount is reduced；
2nd, automatic adjusting method of the present invention, safeguarded without manual site, improve the effective run time of instrument；Automate journey
Degree is high, is adapted to networking multiple instruments test platform；
3rd, electron pressure control method of the invention can directly take back use, improve debugging effect for different instruments
Rate.
Brief description of the drawings
Referring to the drawings, the disclosure will be easier to understand.Skilled addressee readily understands that be：This
A little accompanying drawings are used only for illustrating technical scheme, and are not intended to and protection scope of the present invention is construed as limiting.
In figure：
Fig. 1 is the structural representation of the on-line chromatograph pressure control device of the embodiment of the present invention 1.
Embodiment
Fig. 1 and following description describe the present invention optional embodiment with instruct those skilled in the art how to implement and
Reproduce the present invention.In order to instruct technical solution of the present invention, simplify or eliminate some conventional aspects.Those skilled in the art should
The understanding is derived from the modification of these embodiments or replacement will within the scope of the invention.Under those skilled in the art should understand that
Stating feature can combine to form multiple modifications of the present invention in a variety of ways.Thus, the invention is not limited in it is following can be real
Mode is applied, and is only limited by claim and their equivalent.
Embodiment 1
Fig. 1 schematically illustrates the structure diagram of the on-line chromatograph electron pressure control device of the present embodiment, such as Fig. 1 institutes
State, the pressure control device includes：
Chromatographic column, testing sample is separated；
Electron pressure/flow-control module, the electron pressure/flow-control module are arranged on the upper of the chromatographic column
Trip, is controlled to pressure before post or flow；
Detection process unit, the detection process unit are arranged on the downstream of the chromatographic column, testing sample are divided
Analyse and export testing result, while the actual retention time of selected compound is sent to feedback control module；
Feedback control module, the feedback control module is according to pressure before post or the controlling value of flow and actual retention time
Function correction is carried out, and retention time to be locked is substituted into correction function and obtains the pressure of next testing sample or the control of flow
It is worth and is sent to electron pressure/flow-control module.
The present embodiment also provides the compress control method of above-mentioned electron pressure control device, the electron pressure control method
Comprise the following steps：
(A1) compound is selected, the retention time to be locked of the compound is tR0；
(A2) feedback control module by retention time to be locked substitute into first function obtain testing sample post before pressure or
Flow control value is simultaneously sent to electron pressure/flow-control module；
(A3) pressure before post or flow are adjusted to the controlling value by electron pressure/flow-control module, and test sample is treated in analysis
Product, the actual retention time of the selected compound of detection process unit output to feedback control module；
(A4) feedback control module is carried out according to Pressure control or flow control value before post and actual retention time to first function
Correct and then obtain second function, and retention time to be locked is substituted into second function and obtains pressure before the post of next testing sample
Or flow control value；
(A5) (A3) step is repeated, reduces the gap of actual retention time and retention time to be locked.
Further, the second function is translated by first function and obtained.
During testing sample on-line checking, by being constantly changing pressure or flow before post, carry out compensation apparatus fortune
Influence caused by various condition changes during row, such as aging of flow rate of carrier gas, column temperature, chromatographic column, so that when retaining
Between constantly restrain, become closer to lock retention time.Each testing sample detection, is all the compensation to condition variable quantity
Journey, is the correction of linear function relation, and the correction of each functional relation all obtains via the translation of last functional relation.
The first function is to lead in feedback control module before default functional relation or on-line chromatograph operation
Cross the test of multigroup testing sample and be fitted test data acquisition, specifically, the compress control method further comprises：
(B1) pressure or flow before change post, the data group of pressure or flow and retention time carries out secondary song before obtaining post
Line is fitted, and obtains first function：
(B1) step is located at before (A1) step.
The present embodiment is had an advantage that：Function is carried out with actual retention time using pressure before post or the controlling value of flow
Correction so that the continuous approach locking retention time of retention time, it is ensured that qualitatively and quantitatively accurate during on-line chromatograph longtime running
Property and stability, so as to reduce calibration frequency, improve the effective run time of instrument；The compress control method of the present embodiment is not to
It directly can directly be used between same instrument, improve debugging efficiency.
Embodiment 2
The present embodiment is the on-line chromatograph electron pressure control device and method of the embodiment of the present invention 1 in VOCs detection fields
Application examples.
In the application examples, electron pressure/flow-control module is electron pressure control module (EPC), including pressure passes
Sensor, proportioning valve and circuit board, pressure before post is adjusted the pressure needed for controlling and then exporting.Certainly, the electronics
Pressure/flow control module can also use electronic flow control module (EFC), including flow sensor, proportioning valve and electricity
Road plate, pressure before post is adjusted the flow needed for control output.
The electron pressure control method of the on-line chromatograph of the application example, it is real by pressure before electron pressure module control column
It is existing, comprise the following steps that：
S1. a kind of compound is selected in test substance, the retention time of the compound is locked；
S2. pressure before different posts is controlled, test substance is detected before 5 groups of different posts under pressure, obtains 5 groups of institutes
State the different retention times of compound；
S3. the data of the pressure different to 5 groups and retention time carry out conic fitting, obtain fitting function：
S4. test substance is detected under the stream pressure of itself into on-line chromatograph, selectes the actual guarantor of compound
The time is stayed as retention time t to be lockedR0；According to the fitting function, pressure control values are before obtaining post：
Pressure is p before S5.EPC module control columns1, now detection process unit output retention time do not have it is complete etc.
In tR0, but tR1, then point (t is obtainedR1, p1)；Pass through point (tR1, p1) do one and fitting function：
The curve 2 of translation, the functional relation of the curve 2 are：P=a [tR-(tR1-tR0)]2+b[tR-(tR1-tR0)]+c, in order to obtain
tR0Retention time, pressure control values are before the post that need to be set：p2=a [tR0-(tR1-tR0)]2+b[tR0-(tR1-tR0)]+c；
Pressure is p before S6.EPC module control columns2, the retention time of now detection process unit output is still without complete etc.
In tR0, but tR2, then point (t is obtainedR2, p2)；Pass through point (tR2, p2) do a curve 3 translated with curve 2, the curve 3
Functional relation be：P=a [tR-(tR1-tR0)-(tR2-tR0)]2+b[tR-(tR1-tR0)-(tR2-tR0)]+c, in order to obtain tR0's
Retention time, pressure control values are before the post that need to be set：p3=a [tR0-(tR1-tR0)-(tR2-tR0)]2+b[tR0-(tR1-tR0)-
(tR2-tR0)]+c；
S7. S5, S6 step are repeated, constantly changes pressure before post so that retention time constantly restrains, and becomes closer to tR0。
Claims (5)
1. a kind of electron pressure control device of on-line chromatograph, including chromatographic column, it is characterised in that：The electron pressure control dress
Putting also includes：
Electron pressure/flow-control module, the electron pressure/flow-control module is arranged on the upstream of the chromatographic column, right
Pressure or flow are controlled before post；
Detection process unit, the detection process unit are arranged on the downstream of the chromatographic column, testing sample are analyzed simultaneously
Testing result is exported, while the actual retention time of selected compound is sent to feedback control module；
Feedback control module, the feedback control module are carried out according to pressure before post or the controlling value of flow with actual retention time
Function correction, and by the pressure of the next testing sample of retention time to be locked substitution correction function acquisition or the controlling value of flow simultaneously
It is sent to electron pressure/flow-control module.
A kind of 2. electron pressure control method of on-line chromatograph, it is characterised in that：The electron pressure control method includes following
Step：
(A1) compound is selected, the retention time to be locked of the compound is tR0；
(A2) feedback control module by retention time to be locked substitute into first function obtain testing sample post before pressure or flow
Controlling value is simultaneously sent to electron pressure/flow-control module；
(A3) pressure before post or flow are adjusted to the controlling value by electron pressure/flow-control module, analyze testing sample, inspection
The actual retention time of the selected compound of processing unit output is surveyed to feedback control module；
(A4) feedback control module is corrected according to Pressure control or flow control value before post with actual retention time to first function
And then second function is obtained, and retention time to be locked is substituted into second function and obtains pressure or stream before the post of next testing sample
Measure controlling value；
(A5) (A3) step is repeated, reduces the gap of actual retention time and retention time to be locked.
3. electron pressure control method according to claim 2, it is characterised in that：The electron pressure control method enters one
Step includes：
(B1) pressure or flow before change post, the data group of pressure or flow and retention time carries out conic section plan before obtaining post
Close, obtain first function：
(B1) step is located at before (A1) step.
4. electron pressure control method according to claim 3, it is characterised in that：The second function passes through first function
Translation obtains.
5. electron pressure control method according to claim 2, it is characterised in that：Retention time t to be lockedR0For online color
When spectrum debugging completes to carry out testing sample analysis, the actual retention time of compound is selected.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710763949.0A CN107727780A (en) | 2017-08-30 | 2017-08-30 | The electron pressure control device and method of on-line chromatograph |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201710763949.0A CN107727780A (en) | 2017-08-30 | 2017-08-30 | The electron pressure control device and method of on-line chromatograph |
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| CN107727780A true CN107727780A (en) | 2018-02-23 |
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Citations (6)
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| US5987959A (en) * | 1996-10-10 | 1999-11-23 | Hewlett-Packard Company | Automated retention time locking |
| US6494078B1 (en) * | 2001-06-25 | 2002-12-17 | Agilent Technologies, Inc. | Retention-time locked comprehensive multidimensional gas chromatography |
| CN102016568A (en) * | 2008-04-17 | 2011-04-13 | 帝斯曼知识产权资产管理有限公司 | Comprehensive two-dimensional gas chromatography |
| CN102798684A (en) * | 2011-05-21 | 2012-11-28 | 中国科学院大连化学物理研究所 | Chemical profile analysis method based on retention time locking-gas chromatography-quadrupole mass spectrometry-selected ion monitoring mode |
| CN106233209A (en) * | 2014-02-17 | 2016-12-14 | 株式会社岛津制作所 | Feed back control system |
-
2017
- 2017-08-30 CN CN201710763949.0A patent/CN107727780A/en active Pending
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|---|---|---|---|---|
| US5987959A (en) * | 1996-10-10 | 1999-11-23 | Hewlett-Packard Company | Automated retention time locking |
| US5827946A (en) * | 1997-04-30 | 1998-10-27 | Hewlett-Packard Company | Method for sample identification using a locked retention time database |
| US6494078B1 (en) * | 2001-06-25 | 2002-12-17 | Agilent Technologies, Inc. | Retention-time locked comprehensive multidimensional gas chromatography |
| CN102016568A (en) * | 2008-04-17 | 2011-04-13 | 帝斯曼知识产权资产管理有限公司 | Comprehensive two-dimensional gas chromatography |
| CN102798684A (en) * | 2011-05-21 | 2012-11-28 | 中国科学院大连化学物理研究所 | Chemical profile analysis method based on retention time locking-gas chromatography-quadrupole mass spectrometry-selected ion monitoring mode |
| CN106233209A (en) * | 2014-02-17 | 2016-12-14 | 株式会社岛津制作所 | Feed back control system |
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| 王宇成 主编: "《最新色谱分析检测方法及应用技术实用手册 第2卷》", 31 December 2004, 银声音像出版社 * |
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Application publication date: 20180223 |