CN208313912U - A kind of particulate organic matter on-line preconcentration resolver - Google Patents
A kind of particulate organic matter on-line preconcentration resolver Download PDFInfo
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- CN208313912U CN208313912U CN201820659356.XU CN201820659356U CN208313912U CN 208313912 U CN208313912 U CN 208313912U CN 201820659356 U CN201820659356 U CN 201820659356U CN 208313912 U CN208313912 U CN 208313912U
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- thermal desorption
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Abstract
The utility model relates to a kind of particulate organic matter on-line preconcentration resolver, described device includes the components such as thermal desorption unit, high temperature resistant four-way valve, capillary trapping column, semiconductor cold-trap, electronic three-way valve, gas chromatographic column.Particulate organic matter is through high temperature thermal desorption unit, successively pass through room temperature capillary trapping column and semiconductor cold trap trapping and empties, the organic matter of trapping then passes through the reversed sample introduction of Vavle switching, the low boiling component of semiconductor cold trap trapping Thermal desorption first discharges, and the high boiling component of capillary trapping column trapping enters gas chromatographic column separation detection as the temperature programming of gas-chromatography column oven gradually parses.The utility model improves thermal desorption flow, reduces the thermal desorption time, improve thermal desorption efficiency, avoid thermal desorption sample from being directly entered chromatographic column and cause the accumulative pollution of chromatographic column and detection unit by increasing emptying design.
Description
Technical field
The utility model belongs to environmental monitoring technology field, and in particular to a kind of particulate organic matter on-line preconcentration parsing dress
It sets.
Background technique
Organic matter in Atmospheric particulates is that it one of is mainly formed, and content can account for the 20%-80% of its total amount.Atmosphere
Organic components in grain object are considerably complicated, and concentration range span is big, and physicochemical properties are different, and the moment in atmospheric environment
Dynamic chemical occurs to develop.Therefore, line Measurement Technique becomes dynamic of the organic matter in atmospheric environment in cognition particulate matter
Law is of great significance.The line Measurement Technique of particulate organic matter molecular composition is both domestic and external to grind there are comparable difficulty
Study carefully the thermal desorption aerosol of exploitation in Williams for being based primarily upon Goldstein seminar of California, USA university et al. (2006)
Online gas chromatographic measurement system (TAG system).
Because the thermal desorption time is long, flow is big, it is generally the case that high temperature thermal desorption organic gas needs to first pass through cold trap trapping
Discharge into gas-chromatography (GC) analysis again afterwards.It is higher in view of particulate organic matter boiling point relative volatility organic matter (VOCs), it is main
It to volatilize (SVOC) with half, based on low volatile organic compounds (LVOC) and the portable demand of atmosphere online observation, report at present
The TAG system in road mainly uses capillary column to trap thermal desorption organic gas.In the TAG system of the exploitations such as Williams, thermal desorption
Organic gas is introduced directly into the chromatographic column being placed in 45 DEG C of incubators, and condenses and be enriched in column front end.The SV- of report in 2013
TAG is using one section of 15-50 centimetres of metal capillary as capture unit, and 40 DEG C of temperature, and joined emptying design, it is able to use
Higher thermal desorption flow is to improve thermal desorption efficiency.Number of patent application is the quartz filter TAG of CN201610847023.5,
First by low temperature (- 40 DEG C) semiconductor cold trap trapping, rear heating discharges into GC chromatogram column analysis, mentions organic gas after thermal desorption
The high arresting efficiency of low boiling component.
The trapping in TAG system about thermal desorption gas still has deficiency at present: sample be directly entered GC analytical column mode because
It is limited by column length and detector, thermal desorption flow is not high and the time is longer, and thermal desorption efficiency is lower, and long-term continuous sight
Survey can pollute chromatographic column and detector, influence the service life of chromatographic column and detector；Under normal temperature condition, capillary column is to low boiling point
The arresting efficiency of component is not high；Semiconductor cold-trap needs longer heating time and temperature to the release of high boiling component, seriously
In the service life for influencing trapping column, there are high boiling component analyzing efficiency is low and residue problem.
In fact, pre-concentration is one of the usual way of the on-line preconcentration parsing of VOC, ultralow temperature or adsorbent etc. are mostly used
Enrichment mode.Meanwhile in order to more fully trap VOC, it is commercialized at present and mostly uses multistage cold-trap, mixed adsorbent etc. grinding
Mode traps VOC to be segmented.This kind of enrichment analysis mode is applied in particulate matter and partly waves mainly for volatile organic matter
The on-line preconcentration parsing of hair, low volatile organic compounds there is also some problems.For example, cryotrap discharges not high boiling component
Completely, there is residue problem, improve analyzing efficiency and need to increase resolution temperature and time, will lead to the lost of life of trap tube；Quotient
Super low temperature refrigeration, electronic cooling and liquid nitrogen refrigerating mode are mostly used with cold-trap, volume is larger, needs to consume refrigerant, it is difficult to full
The portable demand observed enough；Adsorbent usually can selectively adsorb certain type organic, but continuous adsorbing base is complicated
Sample can cause serious pollution problem, meanwhile, the replacement of this kind of adsorption tube is often also quite cumbersome.
The problems such as to avoid caused chromatographic column/detection unit pollution during particulate matter thermal desorption, residual, this reality
With development of novel a kind of simple and practical particulate organic matter on-line preconcentration resolver and method.
Utility model content
To solve the above problems, the utility model is intended to provide a kind of particulate organic matter on-line preconcentration resolver, simply
Using chromatographic column incubator, high temperature resistant four-way valve and semiconductor cold-trap, is designed by emptying, carried out respectively for light high boiling component
The segmentation of room temperature and cryotrap traps, and reduces pollution of the thermal desorption in the process to chromatographic column and detection unit, improves chromatographic column
With the service life of detection unit；Sample thermal desorption efficiency and cold trap trapping efficiency are improved, improves system to light high boiling component
The sensitivity of detection；Device is simple, and replacement is convenient.Specific technical solution is as follows.
A kind of particulate organic matter on-line preconcentration resolver, comprising: thermal desorption unit 1, high temperature resistant four-way valve 2, capillary
The components such as trapping column 3A, semiconductor cold-trap 4, electronics three-way ball valve 5, gas chromatographic column 3B；The thermal desorption unit 1 and high temperature resistant
The A of four-way valve 2 is connected, and by Vavle switching, will be transmitted to capillary trapping column from the high-temperature gas of 1 thermal desorption of thermal desorption unit
3A and semiconductor cold-trap 4 are enriched with；The B of high temperature resistant four-way valve 2 is connected with capillary trapping column 3A, and capillary trapping column is placed in gas phase
In chromatographic column incubator 3, it is enriched with 30-40 DEG C of temperature, mainly traps high boiling component；Capillary trapping column 3A and semiconductor cold-trap 4
(0 to -40 DEG C) are connected, and the latter's enrichment fails the low boiling component captured by capillary trapping column 3A；Semiconductor cold-trap 4 and electronics
The B of three-way ball valve 5 is connected；The C of electronics three-way ball valve 5 is emptied, and 5 BC is for controlling emptying；The A and pressure of electronics three-way ball valve 5
The EPC or AUX of power flow controlling unit A6 is connected, and is used for reverse resolution sample introduction (5 AB)；The C and gas phase of high temperature resistant four-way valve 2
Chromatographic column 3B is connected；The D of high temperature resistant four-way valve 2 is connected with the EPC of pressure flow hybrid control unit B 7 or AUX, and the latter is gas phase color
Column 3B gas supply, the residual of transmission line between reverse blow thermal desorption unit 1 and high temperature resistant four-way valve 2 are composed, and is high temperature resistant four-way valve 2
Inertia protection is provided, it is prevented to be oxidized by oxygen.
The application method of above-mentioned apparatus, the device continuously automatically switch, handoff procedure are as follows: thermal desorption/Enrichment Mode-is reversed
Interpretive model-blowback mode；Under thermal desorption/Enrichment Mode, the AB of high temperature resistant four-way valve is connected to, thermal desorption in thermal desorption unit
High-temperature gas (2-150ml/min) capillary trapping column condensing trapping is entered by high temperature resistant four-way valve AB, collection at large
Group is diverted into semiconductor cooling trap and is enriched with, and the component that semiconductor cold-trap does not trap yet is emptied by the BC of electronics three-way ball valve；
Meanwhile the CD connection of high temperature resistant four-way valve, pressure flow hybrid control unit B provide carrier gas, 2ml/min to gas chromatographic column；Heat is de-
Enter reverse resolution mode after attached/Enrichment Mode, electronics three-way ball valve is in the position AB, with pressure flow hybrid control unit A
It is connected, the latter parses gas helium or nitrogen to semiconductor cold-trap and the conveying of capillary trapping column, and as gas chromatographic analysis
Carrier gas；The BC of high temperature resistant four-way valve is connected to, and the component parsed enters gas chromatographic column, by separation detection；Semiconductor cold-trap adds
By the low boiling component of cryogenic trapping, low boiling component is introduced into gas chromatographic column by separation detection for heat release；Gas chromatographic column
The heating of incubator start program gradually by the high boiling component Thermal desorption trapped in capillary trapping column and passes through gas chromatographic column point
From detection；Meanwhile the AD connection of high temperature resistant four-way valve, pressure flow hybrid control unit B are discharged remaining to thermal desorption unit blowback
Thermal desorption component simultaneously protects high temperature resistant four-way valve；After highest group of boiling point to be measured distributes capillary trapping column, in order to keep away
Exempt from heavier component pollution chromatographic column and detector, introduces blowback mode and remove interfering substance, electronics three-way ball valve is in AB
It sets, is connected with pressure flow hybrid control unit A, the AB of high temperature resistant four-way valve is connected to, and the residual in capillary trapping column is de- through overheating
The emptying of coupon member, meanwhile, the CD connection of high temperature resistant four-way valve, pressure flow hybrid control unit B provides carrier gas to gas chromatographic column.
Further, the transmission line between the thermal desorption unit 1 and high temperature resistant four-way valve 2 in system on-line sampling, cooled down
30-160 DEG C in journey, 305 DEG C are heated to during thermal desorption.
Further, high temperature resistant four-way valve 2, between high temperature resistant four-way valve 2 and capillary trapping column 3A and high temperature resistant four-way valve 2 with
Transmission line between chromatographic column 3B keeps 305 DEG C of constant temperature.
Further, stainless steel metal pipeline, gold that the capillary trapping column 3A and four-way valve 2B are handled by deactivation
Category two is logical to be connected, and is directly connected to semiconductor cold-trap 4, is easily attached and replaces.
Further, the preferred quartz capillary column of the capillary trapping column 3A, preferably 0.25 millimeter of internal diameter, 1 meter of length, benefit
With chromatographic column incubator temperature control.
Further, 0 to -40 DEG C of the cold-zone temperature of semiconductor cold-trap 4, the hot zone temperature 40 being connected with capillary trapping column 3A
To 200 DEG C.
Further, after the flow of thermal desorption unit is first low high (2-150ml/min), first low boiling component is captured in and is partly led
Then the low-temperature space of body cold-trap increases flow thermal desorption high boiling component.
Further, the thermal desorption unit 1, high temperature resistant four-way valve 2, gas-chromatography 3, semiconductor cold-trap 4, electronics three-way ball
Valve 5 is electrically connected respectively, by the unlatching of each component of real time computer control, close, and in real time record sampled data and
As a result, the online and automatic operating of realization device.
A kind of particulate organic matter on-line preconcentration resolver provided by the utility model, which has the advantages that, passes through increasing
Add emptying design, improve thermal desorption flow, reduce the thermal desorption time, improve thermal desorption efficiency, avoid thermal desorption sample directly into
Enter chromatographic column and causes the accumulative pollution of chromatographic column and detection unit；Utilize room temperature cold trap trapping high boiling component and low temperature cold
Trap traps the advantage of low boiling component, segmentation trapping low boiling point and high boiling point organic compound, reduces thermal desorption in the process to chromatographic column
With the pollution of detection unit；Sample thermal desorption efficiency and cold trap trapping efficiency are improved, the system of raising detects high low boiling component
Sensitivity.The utility model mainly solve accumulative pollution caused by particulate organic matter on-line measurement system continuous observation with
And the problem that cryotrap is difficult for high boiling component release, the service life of chromatographic column and cryotrap heating unit is improved, is extended
The time of continuous observation expands the boiling spread of analysis component, suitable for particulate matter half volatilization, low volatile organic
Line measurement.With it is compact-sized, convenient for integrated, the characteristics of being easily changed.
Detailed description of the invention
Fig. 1 is the utility model particulate organic matter on-line preconcentration resolver structural schematic diagram, in which:
1- thermal desorption unit 2- high temperature resistant four-way valve
3- gas-chromatography column oven 3A- capillary trapping column
3B- gas chromatographic column 4- semiconductor cold-trap
5- electronics three-way ball valve 6- pressure flow hybrid control unit A
7- pressure flow hybrid control unit B
Specific embodiment
The utility model is described in further details with specific embodiment with reference to the accompanying drawing:
Particulate organic matter on-line preconcentration resolver shown in the utility model has Three models, thermal desorption/enrichment mode
Formula, reverse resolution mode, blowback mode.
Under thermal desorption/Enrichment Mode, the AB of high temperature resistant four-way valve 2 is connected to, the high-temperature gas of thermal desorption in thermal desorption unit 1
(2-150ml/min) enters capillary trapping column 3A condensing trapping by the AB of high temperature resistant four-way valve 2, the group not trapped by 3A
It is enriched with when being diverted into semiconductor cold-trap 4, the component that semiconductor cold-trap 4 does not trap yet is arranged by the BC of electronics three-way ball valve 5
It is empty.Meanwhile the CD connection of high temperature resistant four-way valve 2, pressure flow hybrid control unit B 7 provide carrier gas (nitrogen to gas chromatographic column 3B
Or helium etc., 2 ml/min).
Enter reverse resolution mode after thermal desorption/enrichment (10-20min) mode.Electronics three-way ball valve 5 is in AB
Position is connected with pressure flow hybrid control unit A6, and the latter parses gas helium to semiconductor cold-trap 4 and capillary trapping column 3A conveying
Gas or nitrogen, and as gas chromatographic analysis carrier gas；The BC of high temperature resistant four-way valve 2 is connected to, and the component parsed enters gas phase color
Column 3B is composed by separation detection；The heating release of semiconductor cold-trap 4 by the low boiling component of cryogenic trapping, low boiling component retain compared with
It is weak, gas chromatographic column 3B is introduced by separation detection；The heating of 3 start program of gas-chromatography column oven, gradually traps capillary
The high boiling component Thermal desorption that traps in column 3A simultaneously passes through chromatographic column 3B separation detection.Meanwhile the AD of high temperature resistant four-way valve 2 connects
Logical, pressure flow hybrid control unit B 7 is discharged remaining thermal desorption component and protects high-temperature four-way valve 2 to 1 blowback of thermal desorption unit.
After highest group of boiling point to be measured distributes capillary trapping column 3A, in order to avoid heavier component pollutes chromatography
Column and detector introduce blowback mode and remove this kind of interfering substance.Electronics three-way ball valve 5 is still in the position AB and pressure flow control
Unit A6 processed is connected, and high temperature resistant four-way valve 2 switches to AB connection, and the residual in capillary trapping column 3A passes through thermal desorption unit 1
Emptying.Meanwhile the CD connection of high temperature resistant four-way valve 2, pressure flow hybrid control unit B 7 provide carrier gas to gas chromatographic column.
The technical solution of the utility model is described in detail above.Obviously, the utility model is not limited to institute
The above content of description.Above content based on the utility model, those skilled in the art can also make a variety of accordingly
Variation, but any be equal with the utility model or similar variation is fallen within the protection scope of the utility model.
Claims (4)
1. a kind of particulate organic matter on-line preconcentration resolver, which is characterized in that including thermal desorption unit, high temperature resistant four-way valve,
Capillary trapping column, semiconductor cold-trap, electronics three-way ball valve, gas chromatographic column；The thermal desorption unit and high temperature resistant four-way valve
A be connected, by Vavle switching, capillary trapping column and semiconductor cooling will be transmitted to from the high-temperature gas of thermal desorption unit thermal desorption
Trap enrichment；The B of the high temperature resistant four-way valve is connected with capillary trapping column；The capillary trapping column is placed in gas-chromatography column temperature
In case；The semiconductor cold-trap is connected with capillary trapping column, and enrichment fails the low boiling component captured by capillary trapping column；
The B of the electronics three-way ball valve is connected with semiconductor cold-trap；The C of the electronics three-way ball valve is emptied, and BC connection is for the row of control
It is empty；The A of the electronics three-way ball valve is connected with the EPC or AUX of pressure flow hybrid control unit A, and the latter is used for reverse resolution sample introduction；
The gas chromatographic column is connected with the C of high temperature resistant four-way valve；The D of the high temperature resistant four-way valve and pressure flow hybrid control unit B
EPC or AUX is connected, and the latter is used to supply for gas chromatographic column, transmits between reverse blow thermal desorption unit and high temperature resistant four-way valve
The residual of line, and inertia protection is provided for high temperature resistant four-way valve, prevent it to be oxidized by oxygen.
2. the apparatus according to claim 1, which is characterized in that the high temperature resistant four-way valve and capillary trap intercolumniation and resistance to
The equal deactivation of transmission line of high-temperature four-way valve and gas-chromatography intercolumniation handles and is kept for 305 DEG C of high temperature.
3. the apparatus according to claim 1, which is characterized in that the capillary trapping column is quartz capillary column, internal diameter
0.25 millimeter, 1 meter of length, utilize gas-chromatography column oven temperature control.
4. the apparatus according to claim 1, which is characterized in that the thermal desorption unit, high temperature resistant four-way valve, gas-chromatography
Column oven, semiconductor cold-trap, electronics three-way ball valve are electrically connected respectively, pass through opening for each component of real time computer control
It opens, close, and record sampled data in real time and as a result, realize the online and automatic operating of described device.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201820659356.XU CN208313912U (en) | 2018-05-04 | 2018-05-04 | A kind of particulate organic matter on-line preconcentration resolver |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201820659356.XU CN208313912U (en) | 2018-05-04 | 2018-05-04 | A kind of particulate organic matter on-line preconcentration resolver |
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| CN208313912U true CN208313912U (en) | 2019-01-01 |
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| CN201820659356.XU Withdrawn - After Issue CN208313912U (en) | 2018-05-04 | 2018-05-04 | A kind of particulate organic matter on-line preconcentration resolver |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110333309A (en) * | 2019-07-24 | 2019-10-15 | 清华大学 | A kind of particulate matter organic component on-line measurement system and method based on Two way chromatograms |
| WO2023115636A1 (en) * | 2021-12-22 | 2023-06-29 | 云南中烟工业有限责任公司 | Substance pyrolysis real-time online analysis device and method for using same |
-
2018
- 2018-05-04 CN CN201820659356.XU patent/CN208313912U/en not_active Withdrawn - After Issue
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110333309A (en) * | 2019-07-24 | 2019-10-15 | 清华大学 | A kind of particulate matter organic component on-line measurement system and method based on Two way chromatograms |
| WO2023115636A1 (en) * | 2021-12-22 | 2023-06-29 | 云南中烟工业有限责任公司 | Substance pyrolysis real-time online analysis device and method for using same |
| US11740250B2 (en) | 2021-12-22 | 2023-08-29 | China Tobacco Yunnan Industrial Co., Ltd. | Device for real-time online analysis of substance pyrolysis and method of using the same |
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| AV01 | Patent right actively abandoned |
Granted publication date: 20190101 Effective date of abandoning: 20230411 |
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| AV01 | Patent right actively abandoned |
Granted publication date: 20190101 Effective date of abandoning: 20230411 |
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| AV01 | Patent right actively abandoned | ||
| AV01 | Patent right actively abandoned |