CN103713055B - High-concentration substance detection device and method - Google Patents
High-concentration substance detection device and method Download PDFInfo
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- CN103713055B CN103713055B CN201310755172.5A CN201310755172A CN103713055B CN 103713055 B CN103713055 B CN 103713055B CN 201310755172 A CN201310755172 A CN 201310755172A CN 103713055 B CN103713055 B CN 103713055B
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Abstract
The invention relates to a high-concentration substance detection device which comprises a feeding hole, a detector, a switching unit, a sample preparation unit, a chromatographic detection unit and a control unit, wherein the feeding hole is connected with the switching unit and the detector; the detector detects sample information which enters from the feeding hole in real time; the switching unit is connected with the sample preparation unit, the chromatographic detection unit and the control unit; the switching unit can perform connection and disconnection among the sample preparation unit, the chromatographic detection unit and the feeding hole under control of the control unit; the sample preparation unit is used for storing a sample when the sample preparation unit is communicated with the feeding hole; the chromatographic detection unit is used for detecting the sample information when the chromatographic detection unit is communicated with the feeding hole; the control unit is connected with the detector and is used for controlling a switching result according to the detection result of the detector. The invention also provides a high-concentration substance detection method. The device has the advantages of wide quantification range, information accuracy and comprehensiveness, high flexibility, high system integration level, and the like.
Description
Technical field
The present invention relates to a kind of pick-up unit and method, especially a kind of high-concentration substance detection device and method.
Background technology
In industrial processes, the waste gas of generation is discharged in air after effectively processing.But equipment in use, as there is the generation of the phenomenons such as the aging of equipment or fault, the high concentration components of generation is not also just discharged in air through effective process, can cause the pollution of air.
In industrial processes, the row's of stealing phenomenon also happens occasionally, the component of drain time and discharge is often difficult to controlled in time and trace to the source, good suggestion cannot be provided to production technology optimization and administrative law enforcement, time serious, larger impact and harm can be caused on the health of the mankind.
The early warning revealed for reply industry high-concentration component and detection, prior art has following several solution:
1, Electronic Nose
Electronic inductor is adopted to carry out early warning to leakage component.The method can only carry out early warning by super many finite concentrations to all components, cannot provide the material information and concentration information of revealing material one-component.
2, online analytical instrument
Online analytical instrument is applied to leakage component analysis, can only detect the component of finite concentration scope, detectable concentration is limited in scope, testing result can be caused to there is larger error, and there is certain analytical cycle in online analytical instrument, if leak case appears in analytical cycle, the trapping of sample cannot be carried out, the distortion and erroneous judgement that detect data can be caused.
3, timing sampling device
Adopt negative pressure sampler, arrange certain damping in conjunction with timing controller, fix a point to fixed location, regularly, determine volume sampling, the sample after collection is transported to laboratory and carries out analysis detection.The method can obtain original sample gas information, but cannot realize the collection that the on-fixed time reveals sample.Even and if reveal time sampling, if the leakage time is less than the timing sampling time of timing sampling device, after high concentration leakage sample collection completes, timing sampling device also will to ambient gas as air be sampled, and the ambient gas of collection is stored in sampling thief together, because ambient gas concentration is lower than sample concentration, the sample of samplers sample is caused to be diluted.
Summary of the invention
In order to solve above-mentioned deficiency of the prior art, the invention provides a kind of quantification range is wide, information accurate, comprehensive, flexibility ratio is high, level of integrated system is high high-concentration substance detection device and method.
For achieving the above object, the present invention adopts following technical scheme:
A kind of high-concentration substance detection device, comprising:
Injection port, described injection port is connected with detecting device with described switch unit;
Detecting device, described detecting device detects the sample message entered from injection port in real time;
Switch unit, described switch unit is also connected with control module with standby sample unit, chromatogram detecting unit, and described switch unit realizes the break-make between standby sample unit, chromatogram detecting unit, injection port under the control of the control unit;
Standby sample unit, at standby sample unit and stored sample when being connected between injection port;
Chromatogram detecting unit, described chromatogram detecting unit is used for detecting sample message at chromatogram detecting unit with when being connected between injection port;
Control module, described control module is also connected with detecting device, controls switch unit for the testing result according to detecting device.
Further, described high-concentration substance detection device also comprises alarm unit, and described control module sends warning message according to the working state control alarm unit of the testing result/standby sample unit of detecting device.
Further, described chromatogram detecting unit comprises quantitative loop and/or enrichment pipe.
As preferably, described standby sample unit comprises Soviet Union's code tank.
As preferably, the detecting device in described detecting device and chromatogram detecting unit is same detecting device.
Present invention also offers a kind of high-concentration substance detection method, comprise the following steps:
A, sample enter detecting device from injection port and detect;
Testing result is passed to control module by B, detecting device, and testing result and preset value compare by control module:
If testing result is higher than preset value, control module controls the stream between switch unit connection injection port and chromatogram detecting unit, detects sample message; Control module controls the stream between switch unit connection injection port and standby sample unit, and to sample storage for sample, until testing result is lower than preset value, control module controls the stream between switch unit disconnection injection port and standby sample unit, terminates for sample;
When switch unit switches stream, control module all gathers corresponding temporal information;
Return steps A.
Further, described testing result higher than preset value or standby sample unit can not standby sample time, control module controls alarm unit and sends warning message.
Further, in stepb, if testing result is lower than preset value, control module controls the stream between switch unit on-off injection port and chromatogram detecting unit chronologically, detects sample message.
Further, described high-concentration substance detection method also comprises step C, and control module controls switch unit and connects standby stream between sample unit and chromatogram detecting unit, and chromatogram detecting unit is detected the sample in standby sample unit.
Further, described chromatogram detecting unit comprises quantitative loop and/or enrichment pipe.
As preferably, described standby sample unit comprises Soviet Union's code tank.
As preferably, the detecting device in described detecting device and chromatogram detecting unit is same detecting device.
The present invention compared with prior art has following beneficial effect:
1, quantification range is wide
Adopt enrichment pipe and quantitative loop, reveal component to low concentration and high concentration respectively and carry out sample collection, quantification range is wide, and testing result is accurate.
2, information is comprehensive
Detecting device continues Real-Time Monitoring sample message, obtains the total concentration of sample, and concentration change trend;
Moment is revealed, the content of each composition in chromatogram detecting unit detection of leaks moment sample in high concentration;
Sample in standby sample unit is detected, the situation of sample in the whole leakage time period can be obtained, conveniently carry out sample and trace to the source;
Thus, can obtain the various sample messages corresponding with the time by the present invention, information is comprehensive, provides comprehensive and accurate reference to administrative service division.
3, information is accurate
Standby sample unit opens and closes in time according to Real-time Monitoring Data, avoid standby sample not in time or the opening time oversize and cause the dilution of sample; Make to carry out according to the testing result of standby sample unit the information that sample traces to the source more accurate.
4, flexibility ratio is high
System intialization can be arranged according to actual condition; Flexibility ratio is high.
5, level of integrated system is high
Valve road switched system can carry out the analysis of high-low-range concentration sample flexibly and switch, and can support that multiple standby original mold block in multiple standby sample unit is to the collection of sample.
Accompanying drawing explanation
Fig. 1 is embodiment 1 middle and high concentration substance detecting apparatus schematic diagram;
Fig. 2 is embodiment 2 middle and high concentration substance detecting apparatus schematic diagram.
Embodiment
Embodiment 1
Refer to Fig. 1, a kind of high-concentration substance detection device, comprise injection port 11, detecting device 21, switch unit 31, standby sample unit 41, chromatogram detecting unit 51 and control module (not marking in the drawings);
Described injection port 11 is connected with detecting device 21 by pump 211, and pump 211 continuous firing, is detected by detecting device 21 in real time to make the sample entered from injection port 11; Described detecting device 21 is connected with described control module, and real-time testing result is passed to control module, and control module record stores corresponding testing result, and gathers simultaneously, stores temporal information corresponding to corresponding testing result;
Described switch unit 31 is connected with control module with described injection port 11, standby sample unit 41, chromatogram detecting unit 51;
Described switch unit 31 realizes the break-make between standby sample unit 41, chromatogram detecting unit 51, injection port 11 under the control of the control unit;
Without restriction to the concrete device of switch unit, simultaneously also without restriction to the number of injection port, as long as the switch unit arranged and injection port can realize, by injection port, sample is passed into standby sample unit, chromatogram detecting unit.
Preferably, described control module can also control switch unit make standby sample unit detects with chromatogram between be connected, so that chromatogram detecting unit detects for the sample message in sample unit.
The present embodiment, injection port only has one, and injection port 11 is connected with chromatogram detecting unit 51 with described standby sample unit 41 by described switch unit 31;
Described switch unit 31 comprises multi-channel direction selecting valve 311 and solenoid valve 312; Described injection port 11 is connected with solenoid valve 312 one end, and solenoid valve 312 other end is connected with the public port O mouth of multi-channel direction selecting valve 311; Described chromatogram detecting unit 51 is connected with the 1st interface of multi-channel direction selecting valve 311;
Standby sample unit 41 comprises each standby sample device, without restriction to the number of standby sample device, can arrange according to actual condition; The each standby sample device of described standby sample unit 41 is connected with 2 ~ n interface of described multi-channel direction selecting valve 311.
Control module controls switch unit 31 according to the testing result of detecting device 21, realize standby sample unit 41, break-make between chromatogram detecting unit 51 with injection port 11: at standby sample unit with when being connected between injection port, control module controls switch unit makes the common interface O mouth of multi-channel direction selecting valve 311 be connected with the standby sample device of one of them sky, thus stored sample; Sample message is detected with when being connected between injection port at chromatogram detecting unit.
Standby sample unit can meet control module and control to close, and the sample gathered can realize stable existence wherein, the present embodiment, and described standby sample unit 41 comprises Soviet Union's code tank 411.Soviet Union's code tank inside surface, through polishing, plating or high cleaning, has the advantages such as chemical activity is low, stability is high, anti-collision is good, preferentially selects.Owing to being negative pressure in Soviet Union's code tank 411, then, when control module control switch unit 31 makes to be connected between injection port 11 and Soviet Union's code tank 411 of one of them sky, the sample in injection port is directly pressed into empty Soviet Union's code tank 411 and carries out standby sample.
Standby sample device in standby sample unit does not use, and can continue standby sample, and now, standby sample unit is in normal operating conditions; If the standby sample device in standby sample unit is finished, can not continue standby sample, now, standby sample unit is in abnormal operation, now just needs the standby sample device notifying that staff more renews.
The sample that in standby sample unit 41, standby sample device stores can detect as required in good time, detect as laboratory will be taken back for sample device, or be directly communicated with standby stream between sample unit 41 and chromatogram detecting unit 51, chromatogram detecting unit 51 is detected the sample in the standby sample device of stored sample in standby sample unit 41.
Further, described chromatogram detecting unit comprises quantitative loop and/or enrichment pipe.
If chromatogram detecting unit comprises quantitative loop and enrichment pipe, then, chromatogram detecting unit has quantitative loop detecting pattern and enrichment pipe detecting pattern, then control module also controls to select quantitative loop detecting pattern or enrichment pipe detecting pattern when injection port is connected with chromatogram detecting unit according to testing result.
The present embodiment chromatogram detecting unit 51 comprises multi-position valve 511, quantitative loop 512, pump 513, chromatographic column 514 and chromatographic detector 515.Device and the corresponding matching relationship of chromatogram detecting unit are the state of the art, do not repeat them here.
In order to know the testing result of detecting device in time, further, described high-concentration substance detection device also comprises alarm unit, and described control module sends warning message according to the working state control alarm unit of the testing result/standby sample unit of detecting device.
Preferably, the detecting device in described detecting device and chromatogram detecting unit is same detecting device, to improve level of integrated system.
Present invention also offers a kind of high-concentration substance detection method, comprise the following steps:
The high-concentration substance detection device of A, employing the present embodiment;
Sample continues to pass into detecting device 21 from injection port 11 and detects;
Testing result is passed to control module by B, detecting device 21, and testing result and preset value X compare by control module:
If testing result is higher than preset value X, control module control switch unit 31 connects the stream between injection port 11 and chromatogram detecting unit 51, and the sample after being sampled by quantitative loop 512 is passed into chromatographic column and detects; After quantitative loop 512 sampling terminates, control module controls switch unit 31 and disconnects the stream between injection port 11 and chromatogram detecting unit 51 and connect the stream between injection port 11 and standby sample unit 41, control module controls switch unit 31 makes the common interface O mouth of multi-channel direction selecting valve 311 be connected with the standby sample device of one of them sky, to sample storage for sample, until testing result is lower than preset value X, control module controls switch unit 31 and disconnects injection port 11 and for the stream between sample unit 41, terminate for sample;
When switch unit 31 switches stream, control module all gathers corresponding temporal information;
Return steps A.
Described preset value X can be arranged according to actual condition.
If desired obtaining sample leak case, can detect being taken back laboratory by the sample of the storage in sample unit.
The present embodiment is for detecting the benzene homologues in air, and X is 17mg/m
3(with reference to GB16297-1996).
This patent detecting device continues Real-Time Monitoring sample message, obtains the total concentration of sample, and concentration change trend; Moment is revealed, the content of each composition in chromatogram detecting unit detection of leaks moment sample in high concentration;
Sample in standby sample unit is detected, the situation of sample in the whole leakage time period can be obtained, conveniently carry out sample and trace to the source;
Thus, can obtain the various sample messages corresponding with the time by the present invention, information is comprehensive, provides comprehensive and accurate reference to administrative service division.
Standby sample unit opens and closes in time according to Real-time Monitoring Data, avoid standby sample not in time or the opening time oversize and cause the dilution of sample; Make to carry out according to the testing result of standby sample unit the information that sample traces to the source more accurate.
System intialization can be arranged according to actual condition; Flexibility ratio is high.
Valve road switched system can carry out the analysis of high-low-range concentration sample flexibly and switch, and can support that multiple standby original mold block in multiple standby sample unit is to the collection of sample.
Embodiment 2
Refer to Fig. 2, a kind of high-concentration substance detection device, with the high-concentration substance detection device described in embodiment 1 unlike:
1, the present embodiment chromatogram detecting unit 52 also comprises enrichment pipe 521.
Chromatogram detecting unit 52 has quantitative loop detecting pattern and enrichment pipe detecting pattern, then control module also controls to select quantitative loop detecting pattern or enrichment pipe detecting pattern when injection port 11 is connected with chromatogram detecting unit 52 according to testing result.
If testing result is lower than preset value X, control module controls the stream between switch unit 31 on-off injection port and chromatogram detecting unit chronologically, and controls selective enrichment pipe detecting pattern further.When enrichment pipe sampling pattern is to meet low concentration sample, the quantitative test carrying out one-component detects, and obtains the concentration information of one-component, conveniently monitors concentration of component variation tendency.
2, the present embodiment high-concentration substance detection device also comprises alarm unit (not marking in the drawings), and control module controls alarm unit according to the testing result of detecting device and sends warning message; Or control module also monitors the duty of standby sample unit for sample device, if standby sample device has been finished when can not continue standby sample, alarm unit has sent warning message.
The present embodiment additionally provides a kind of high-concentration substance detection method, with the high-concentration substance detection method described in embodiment 1 unlike:
1, in step, the high-concentration substance detection device of the present embodiment is adopted;
If 2 testing results are lower than preset value X, control module controls the stream between switch unit 31 on-off injection port and chromatogram detecting unit chronologically, and controls selective enrichment pipe detecting pattern further.
If testing result is higher than preset value X, control module controls alarm unit and generates warning message, and sends warning; Meanwhile, control switch unit 31 connects the stream between injection port 11 and chromatogram detecting unit 52, selects quantitative loop detecting pattern.
Control module also monitors the duty of standby sample unit for sample device, if standby sample unit is in abnormal operation, then, standby sample device is finished, and alarm unit sends warning message, and prompting staff changes standby sample device in time.
Adopt enrichment pipe and quantitative loop, reveal component to low concentration and high concentration respectively and carry out sample collection, quantification range is wide, and testing result is accurate.
Embodiment 3
A kind of high-concentration substance detection device, with the high-concentration substance detection device described in embodiment 2 unlike:
Control module also control switch unit make standby sample unit detects with chromatogram between be connected, so that chromatogram detecting unit detects for the sample message in sample unit.
The present embodiment additionally provides a kind of high-concentration substance detection method, with the high-concentration substance detection method described in embodiment 2 unlike: also comprise step C, control module control switch unit make standby sample unit detects with chromatogram between be connected, detect for the sample message in sample unit with chromatogram detecting unit.
Above-mentioned embodiment should not be construed as limiting the scope of the invention.Key of the present invention is: detect in real time sample message, if when detecting that high concentration is leaked, start chromatogram detect, simultaneously to sample for sample.Meet department for administrative supervision reveals sample detection requirement to high concentration.Without departing from the spirit of the invention, all should fall within protection scope of the present invention any type of change that the present invention makes.
Claims (12)
1. a high-concentration substance detection device, comprising:
Injection port, described injection port is connected with detecting device with switch unit;
Detecting device, described detecting device detects the sample message entered from injection port in real time;
Switch unit, described switch unit is also connected with control module with standby sample unit, chromatogram detecting unit, and described switch unit realizes the break-make between standby sample unit, chromatogram detecting unit, injection port under the control of the control unit;
Standby sample unit, at standby sample unit and stored sample when being connected between injection port, described standby sample unit comprises standby sample device;
Chromatogram detecting unit, described chromatogram detecting unit is used for detecting sample message at chromatogram detecting unit with when being connected between injection port;
Control module, described control module is also connected with detecting device, switch unit is controlled for the testing result according to detecting device, realize standby sample unit, chromatogram detecting unit and the break-make between injection port: at standby sample unit with when being connected between injection port, control module controls switch unit makes it be connected with the standby sample device of one of them sky, thus stored sample; Sample message is detected with when being connected between injection port at chromatogram detecting unit.
2. high-concentration substance detection device according to claim 1, it is characterized in that: described high-concentration substance detection device also comprises alarm unit, described control module sends warning message according to the working state control alarm unit of the testing result/standby sample unit of detecting device.
3. high-concentration substance detection device according to claim 1, is characterized in that: described chromatogram detecting unit comprises quantitative loop and/or enrichment pipe.
4. high-concentration substance detection device according to claim 1, is characterized in that: described standby sample unit comprises Soviet Union's code tank.
5. high-concentration substance detection device according to claim 1, is characterized in that: the detecting device in described detecting device and chromatogram detecting unit is same detecting device.
6. a high-concentration substance detection method, comprises the following steps:
A, sample enter detecting device from injection port and detect;
Testing result is passed to control module by B, detecting device, and testing result and preset value compare by control module:
If testing result is higher than preset value, control module controls the stream between switch unit connection injection port and chromatogram detecting unit, detects sample message; Control module controls the stream between switch unit connection injection port and standby sample unit, and to sample storage for sample, until testing result is lower than preset value, control module controls the stream between switch unit disconnection injection port and standby sample unit, terminates for sample;
When switch unit switches stream, control module all gathers corresponding temporal information;
Return steps A.
7. high-concentration substance detection method according to claim 6, is characterized in that: described testing result higher than preset value or standby sample unit can not standby sample time, control module controls alarm unit and sends warning message.
8. high-concentration substance detection method according to claim 6, it is characterized in that: in stepb, if testing result is lower than preset value, control module controls the stream between switch unit on-off injection port and chromatogram detecting unit chronologically, detects sample message.
9. high-concentration substance detection method according to claim 6, it is characterized in that: described high-concentration substance detection method also comprises step C, control module controls switch unit and connects standby stream between sample unit and chromatogram detecting unit, and chromatogram detecting unit is detected the sample in standby sample unit.
10. high-concentration substance detection method according to claim 6, is characterized in that: described chromatogram detecting unit comprises quantitative loop and/or enrichment pipe.
11. high-concentration substance detection method according to claim 6, is characterized in that: described standby sample unit comprises Soviet Union's code tank.
12. high-concentration substance detection method according to claim 6, is characterized in that: the detecting device in described detecting device and chromatogram detecting unit is same detecting device.
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| CN105749583B (en) * | 2014-12-16 | 2017-10-20 | 中国科学院大连化学物理研究所 | A kind of general preparative two-dimensional liquid chromatography device and its operating method |
| CN108489875B (en) * | 2018-02-06 | 2020-10-16 | 济宁中科云天环保科技有限公司 | Pollutant tracing system and method based on time period statistical analysis |
| CN108918899B (en) * | 2018-05-18 | 2021-12-28 | 北京大学深圳研究生院 | High-throughput screening system, device and method for chemical reaction |
| CN110208391A (en) * | 2018-06-12 | 2019-09-06 | 上海炫一电气有限公司 | It is a kind of for detecting the detection device of volatile organic matter in air |
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| JP2011141120A (en) * | 2008-10-07 | 2011-07-21 | Arkray Inc | Liquid chromatography device and liquid chromatography |
| US8707760B2 (en) * | 2009-07-31 | 2014-04-29 | Tricorntech Corporation | Gas collection and analysis system with front-end and back-end pre-concentrators and moisture removal |
| EP3185016B1 (en) * | 2010-10-29 | 2021-06-23 | Thermo Fisher Scientific OY | System layout for an automated system for sample preparation and analysis |
| CN102128896A (en) * | 2010-11-19 | 2011-07-20 | 聚光科技(杭州)股份有限公司 | Sampling method and device |
| JP5838866B2 (en) * | 2012-03-08 | 2016-01-06 | 株式会社島津製作所 | Liquid feeding mechanism and liquid chromatograph |
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