CN109521121A - A kind of method of vapor in the VOC monitoring device and separation sample gas of separable vapor - Google Patents
A kind of method of vapor in the VOC monitoring device and separation sample gas of separable vapor Download PDFInfo
- Publication number
- CN109521121A CN109521121A CN201811639536.2A CN201811639536A CN109521121A CN 109521121 A CN109521121 A CN 109521121A CN 201811639536 A CN201811639536 A CN 201811639536A CN 109521121 A CN109521121 A CN 109521121A
- Authority
- CN
- China
- Prior art keywords
- interface
- way valve
- chromatographic column
- port
- vapor
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000000034 method Methods 0.000 title claims abstract description 38
- 238000012806 monitoring device Methods 0.000 title claims abstract description 35
- 238000000926 separation method Methods 0.000 title claims abstract description 11
- 230000018044 dehydration Effects 0.000 claims abstract description 59
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 59
- 238000005070 sampling Methods 0.000 claims abstract description 43
- 239000004615 ingredient Substances 0.000 claims abstract description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000007789 gas Substances 0.000 claims description 59
- 239000012159 carrier gas Substances 0.000 claims description 27
- 238000004587 chromatography analysis Methods 0.000 claims description 14
- 238000009835 boiling Methods 0.000 claims description 9
- 238000004140 cleaning Methods 0.000 claims description 7
- 238000004458 analytical method Methods 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- 238000001514 detection method Methods 0.000 claims description 5
- 238000007445 Chromatographic isolation Methods 0.000 claims description 4
- 230000005540 biological transmission Effects 0.000 claims description 3
- 238000000197 pyrolysis Methods 0.000 claims description 3
- 230000000694 effects Effects 0.000 abstract description 5
- 239000012855 volatile organic compound Substances 0.000 description 61
- 238000010586 diagram Methods 0.000 description 8
- 238000012544 monitoring process Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 4
- 238000005259 measurement Methods 0.000 description 3
- 239000005416 organic matter Substances 0.000 description 3
- 229920000557 Nafion® Polymers 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000003915 air pollution Methods 0.000 description 1
- 239000012491 analyte Substances 0.000 description 1
- -1 as shown in figure 4 Substances 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
Classifications
-
- 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
-
- 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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/16—Injection
- G01N30/20—Injection using a sampling valve
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The present invention relates to the methods of vapor in a kind of VOC monitoring device of separable vapor and separation sample gas, it is characterized in that, it is characterized in that, including dehydration sampler and multiple valve, the dehydration sampler includes ten-way valve, quantitative sampling ring, it is dehydrated chromatographic column, there are two types of operating modes for ten-way valve, quantitative sampling ring is used for the quantitative amount when ten-way valve is in operating mode two and samples gas, dehydration chromatographic column is used to be in operating mode in ten-way valve to be connected with quantitative sampling ring for the moment, and remove the vapor in sample gas, sample gas after removing water steams inputs enrichment pipe by multiple valve；VOC monitoring device provided by the present invention, using the vapor in the work column temperature separation sample gas of chromatographic column, separating rate is fast, and water removal effect is good, and other VOC ingredients in sample gas can input enrichment pipe and are enriched with, thus the drawbacks of effectively avoiding in the prior art.
Description
Technical field
The present invention relates to VOC monitoring technical fields, and in particular to a kind of the VOC monitoring device and separation of separable vapor
The method of vapor in sample gas.
Background technique
VOC is the english abbreviation of volatile organic compounds (volatile organic compounds)；Common meaning
On VOC be exactly to refer to volatile organic matter；But the VOC on environment protection significance refers to active a kind of volatile organic matter, i.e.,
That a kind of volatile organic matter of harm can be generated.
The air pollution agent ingredient on industrial park periphery becomes increasingly complex multiplicity, and environmental protection administration needs more online
VOC monitoring device, continuously to monitor the pollution factor ingredient and concentration of surrounding air on-line；Due to surrounding air VOC at
Divide concentration very low, usually less than 1ppbV causes existing instrument and equipment not measure directly.
In the prior art, conventional method is to flash heat using low temperature enrichment, high temperature using the enrichment pipe of filling enrichment material
The mode of parsing extracts the sample gas of a period of time, and the VOC ingredient being monitored in sample gas is trapped in enrichment pipe,
Then transient heating heat up by way of reversely blow to chromatographic column carry out chromatographic isolation, finally be sent to detector analysis ingredient and
Concentration；Existing VOC monitoring device is mainly used for analyzing low-carbon VOC ingredient (i.e. the ingredient of carbon atom number between 2 and 6), by
It is very low in the boiling point of low-carbon VOC ingredient, so when using enrichment pipe enrichment VOC ingredient, it usually needs enrichment pipe is dropped to
Low-down temperature, enrichment temperature are generally -10 DEG C~-20 DEG C.
During actual monitoring, since the content of water vapor in air can usually reach 3%, that is,
30000000ppbV, about three thousands of times of VOC ingredient, on the one hand, the enrichment material in enrichment pipe would generally be because excessive
Vapor and cause to be saturated, so that the VOC pollutant in air can not be trapped；On the other hand, due to enrichment pipe work in 0 degree with
Under, the vapor in air can be directly resulted in and freeze and block enrichment pipe, cause the even entire VOC monitoring device of enrichment pipe can not
It works normally；Therefore in practical application VOC monitoring device, need to remove the vapor in sample gas；And existing VOC monitoring is set
It is standby, it generallys use the vapor received and be in charge of in (nafion pipe, high molecular material) removal sample gas and common hydro carbons VOC is received
The good water removal effect being in charge of；However, for water solubility VOC (being such as highly soluble in the alcohols VOC of water) in sample gas, it will usually with
Vapor is removed together, and highest can lose 80% concentration, and so as to cause the measurement result of VOC monitoring device, there are larger mistakes
Difference.
Summary of the invention
To improve the deficiency in the presence of the prior art, the present invention provides a kind of VOC of separable vapor monitorings to set
Standby, using the vapor in the work column temperature separation sample gas of chromatographic column, separating rate is fast, and water removal effect is good, and its in sample gas
Its VOC ingredient can input enrichment pipe and is enriched with.
The technical scheme adopted by the invention is that:
A kind of VOC monitoring device of separable vapor, including dehydration sampler and multiple valve, the dehydration sampling
Device includes ten-way valve, quantitative sampling ring, dehydration chromatographic column, wherein
The ten-way valve includes ten interfaces, respectively interface one, interface two, interface three, interface four, interface five, interface
Six, interface seven, interface eight, interface nine and interface ten, interface one is for inputting sample gas, and interface two is for emptying, quantitative sampling
One end of ring is connected by pipeline with interface three, and the other end is connected with interface ten, and interface four and interface seven are respectively used to defeated
Enter carrier gas, be dehydrated one end of chromatographic column and be connected by pipeline with interface five, the other end is connected with interface nine, interface six with connect
Mouth eight is connected by pipeline with multiple valve respectively,
The ten-way valve is there are two types of operating mode, for the moment in operating mode, interface one is connected to interface two, interface three and
The connection of interface four, interface five is connected to interface six, interface seven is connected to interface eight connectivity, interface nine with interface ten, is in work
When mode two, interface one is connected to interface ten, interface two is connected to interface tee joint, interface four with interface five, interface six with connect
Seven connection of mouth, interface eight are connected to interface nine；
Quantitative sampling ring is used for the quantitative amount when ten-way valve is in operating mode two and samples gas, and dehydration chromatographic column is used for ten
Port valve is in operating mode and is connected for the moment with quantitative sampling ring, and removes the vapor in sample gas, the sample gas after removing water steaming
Enrichment pipe is inputted by multiple valve.
Preferably, the dehydration chromatographic column uses moderately polar resistance to steam chromatographic column.To flow out vapor quickly.
Preferably, the length of the dehydration chromatographic column is 15-20cm.
Preferably, the multiple valve is four-way valve or six-way valve or ten-way valve.
Preferably, the multiple valve be four-way valve, the four-way valve include four connectors, respectively connector one,
Connector two, connector three and connector four, the interface six and interface eight respectively by pipeline and the connector one and
Connector tee joint, connector two is for emptying, and connector four is for being connected to enrichment pipe；
Four-way valve is there are two types of working method, and for the moment in working method, connector one is connected with connector two, connector
Three are connected with connector four, and when being in working method two, connector one is connected with connector four, connector two and connector
Three are connected, and the work method control by controlling four-way valve is dehydrated chromatographic column Yes/No and is connected with enrichment pipe.
It further, further include enrichment resolver, the enrichment resolver includes six-way valve and enrichment pipe, and described six
Port valve includes six ports, respectively port one, port two, port three, port four, port five and port six, wherein
Port one is connected by pipeline with the connector four, and one end of the enrichment pipe passes through pipeline and port two-phase
Connection, the other end are connected by pipeline with port five, and port three is held for connecting chromatographic column, port four for inputting carrier gas
Mouth six is for emptying；
The six-way valve is there are two types of working condition, in running order a period of time, port one is connected to port two, port three and
The connection of port four, port five be connected tos with port six, when in running order two, port one is connected to port six, port two with hold
Mouth tee joint, port four are connected to port five；By adjusting the working condition of six-way valve, enrichment pipe Yes/No and chromatographic column are controlled
It is connected.
It further, further include chromatographic analysis device, the chromatographic analysis device includes chromatographic column and detector, the color
One end of spectrum column is connected by pipeline with the port three, and the other end is connected by pipeline with the detector, chromatographic column
For carrying out chromatographic isolation, detector is for detecting ingredient and content.
Preferably, the ten-way valve is ten-way valve sample injector, and/or, the six-way valve is six-way valve sample injector, and/or,
The four-way valve is four-way valve sample injector.
Further, the enrichment resolver further includes temperature controller, and the temperature controller is set at the enrichment pipe, temperature control
Device is used to adjust the temperature of enrichment pipe.
Preferably, the chromatographic column is analysis chromatographic column.
A method of using vapor in chromatography post separation sample gas, including aforementioned VOC monitoring device, using described quantitative
Ring quantitative collection sample gas is sampled, and sample gas collected is utilized into the work column of dehydration chromatographic column by the dehydration chromatographic column
Vapor in temperature removing sample gas.
Preferably, comprising the following steps:
Step 1: ten-way valve is in operating mode two, six-way valve in running order one, and four-way valve is in working method two,
Sample gas is inputted into quantitative sampling ring, and is full of quantitative sampling ring；
Blowback cleaning is carried out to dehydration chromatographic column using carrier gas；Enrichment pipe is cleaned using carrier gas；Utilize carrier gas pair
Chromatographic column is cleaned；
Step 2: after to be cleaned, switching the operating mode of ten-way valve, so that ten-way valve is in operating mode one, utilize
Sample pneumatic transmission in quantitative sampling ring is entered to be dehydrated chromatographic column by carrier gas, the low boiling using the work column temperature of dehydration chromatographic column, in sample gas
The fast VOC ingredient of point, flowing first flows out dehydration chromatographic column, and enters enrichment pipe, and enrichment pipe is in low temperature enrichment state；
Step 3: when vapor will flow out dehydration chromatographic column, switching four-way valve, four-way valve is made to be in working method one, water
Steam is emptied from dehydration chromatographic column outflow by four-way valve；
Step 4: after vapor flows completely out, switch the operating mode of ten-way valve, ten-way valve is made to be in operating mode two,
High-carbon, the higher boiling VOC ingredient being dehydrated in chromatographic column are gone out to be dehydrated chromatographic column, and flow into enrichment pipe by carrier gas blowback；
Sample gas inputs quantitative sampling ring again, and is full of quantitative sampling ring, completes sampling；
Step 5: when the VOC ingredient in dehydration chromatographic column is blown into enrichment pipe completely, and chromatographic column purged by carrier gas it is clean
Afterwards, circulation executes above-mentioned steps 2, step 3 and step 4；
Step 6: when the volume needed for the collection capacity of sample gas in enrichment pipe reaches detection, switch four-way valve and six-way valve,
Four-way valve and six-way valve is set to be respectively at working method two and working condition two,
Enrichment pipe is in high temperature pyrolysis analysis state, and the VOC ingredient being enriched in enrichment pipe is admitted to chromatographic column and is separated,
And it is sent into detector and is detected.
Compared with prior art, using a kind of the VOC monitoring device and separation sample of separable vapor provided by the invention
The method of vapor in gas, using the vapor in chromatography post separation sample gas, preventing vapor from entering enrichment pipe influences enrichment pipe
Low temperature Concentration Sampling process, not only separating rate is fast, and water removal effect is good, and other VOC ingredients to be monitored can be sent into enrichment
Pipe is enriched with, thus the drawbacks of effectively avoiding in the prior art, and may be implemented automatic water-removing, continuous enrichment parsing and
Measure function.
Detailed description of the invention
In order to illustrate the technical solution of the embodiments of the present invention more clearly, below will be to needed in the embodiment attached
Figure is briefly described, it should be understood that the following drawings illustrates only certain embodiments of the present invention, therefore is not construed as pair
The restriction of range for those of ordinary skill in the art without creative efforts, can also be according to this
A little attached drawings obtain other relevant attached drawings.
Fig. 1 is the structural schematic diagram of ten-way valve.
Fig. 2 is the structural schematic diagram of six-way valve.
Fig. 3 is the structural schematic diagram of four-way valve.
Fig. 4 is a kind of structural schematic diagram (step 1) of VOC monitoring device provided by the invention.
Fig. 5 is a kind of VOC monitoring device provided by the invention, schematic diagram when in step 2 (or being state 2).
Fig. 6 is a kind of VOC monitoring device provided by the invention, schematic diagram when in step 3 (or being state 3).
Fig. 7 is a kind of VOC monitoring device provided by the invention, schematic diagram when in step 4 (or being state 4).
Fig. 8 is a kind of VOC monitoring device provided by the invention, schematic diagram when in step 6 (or being state 6).
Description of symbols in figure
Dehydration sampler 101, ten-way valve 102, dehydration chromatographic column 103, quantitative sampling ring 104,
Four-way valve 201,
Enrichment resolver 301, enrichment pipe 302, six-way valve 303,
Port 1, port 2 402, port 3 403, port 4 404, port 5 405, port 6 406,
Interface 1, interface 2 502, interface 3 503, interface 4 504, interface 5 505, interface 6 506, interface seven
507, interface 8 508, interface 9 509, interface 10.
Connector 1, connector 2 602, connector 3 603, connector 4 604,
Chromatographic analysis device 701, chromatographic column 702, detector 703.
Specific embodiment
Below in conjunction with attached drawing in the embodiment of the present invention, technical solution in the embodiment of the present invention carries out clear, complete
Ground description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Usually exist
The component of the embodiment of the present invention described and illustrated in attached drawing can be arranged and be designed with a variety of different configurations herein.Cause
This, is not intended to limit claimed invention to the detailed description of the embodiment of the present invention provided in the accompanying drawings below
Range, but it is merely representative of selected embodiment of the invention.Based on the embodiment of the present invention, those skilled in the art are not doing
Every other embodiment obtained under the premise of creative work out, shall fall within the protection scope of the present invention.
Embodiment 1
Fig. 1, Fig. 2, Fig. 3 and Fig. 4 are please referred to, the VOC monitoring that a kind of separable vapor is provided in the present embodiment is set
It is standby, including dehydration sampler 101 and multiple valve, the dehydration sampler 101 include ten-way valve 102, quantitative sampling ring
104, it is dehydrated chromatographic column 103, wherein
Ten-way valve 102 include ten interfaces, respectively interface 1, interface 2 502, interface 3 503, interface 4 504,
Interface 5 505, interface 6 506, interface 7 507, interface 8 508, interface 9 509 and interface 10, interface 1 are used for
Sample gas is inputted, for emptying, one end of quantitative sampling ring 104 is connected by pipeline with interface 3 503 interface 2 502, another
End is connected with interface 10, and interface 4 504 and interface 7 507 are respectively used to input carrier gas, so as to using carrier gas as power,
It such as the VOC ingredient transfer for driving sample gas and being enriched with, or is cleaned using carrier gas, such as cleans enrichment pipe 302, chromatographic column 702
Deng；One end of dehydration chromatographic column 103 is connected by pipeline with interface 5 505, and the other end is connected with interface 9 509, interface
6 506 and interface 8 508 be connected respectively by pipeline with multiple valve；
In the present embodiment, multiple valve is mainly used for the flow direction of switching dehydration 101 output gas of sampler, a side
Face can empty vapor, on the other hand, the sample gas after water vapor removing can be transported in enrichment pipe 302；
In the present embodiment, there are two types of operating modes for the ten-way valve 102, for the moment in operating mode, interface 1 with
Interface 2 502 connection, interface 3 503 is connected to interface 4 504, interface 5 505 is connected to interface 6 506, interface 7 507 with connect
8 508 connection of mouth, interface 9 509 are connected to interface 10, and when being in operating mode two, interface 1 and interface 10 connect
Lead to, interface 2 502 is connected to interface 3 503, interface 4 504 is connected to interface 5 505, interface 6 506 and interface 7 507 connect
Logical, interface 8 508 is connected to interface 9 509；In actual application, two kinds of operating modes of ten-way valve 102 can pass through
Manually or automatically switch over.
In the present embodiment, quantitative sampling ring 104 is used for the quantitative amount sampling when ten-way valve 102 is in operating mode two
Gas, as shown in figure 4, sample gas can smoothly enter quantitative sampling ring 104 when ten-way valve 102 is in operating mode two；It is dehydrated color
Spectrum column 103 is used to be in operating mode in ten-way valve 102 to be connected with quantitative sampling ring 104 for the moment, and removes the water in sample gas
Steam, the sample gas after removing water steams inputs enrichment pipe 302 by multiple valve, to be enriched with；That is, as shown in figure 5, when fixed
It measuring after filling full sample gas in sample ring 104, ten-way valve 102 can be switched to operating mode one, at this point, using multiple valve, it can
So that quantitative sampling ring 104 is connected with dehydration chromatographic column 103, and removes sample gas using dehydration chromatographic column 103, it is fixed to make
It measures sample ring 104 and is connected via dehydration chromatographic column 103 with enrichment pipe 302, and the sample gas after water vapor removing is inputted into richness
Collector 302, to be enriched with.
VOC monitoring device provided by the present embodiment, can before enrichment, using chromatographic column 702 work when column temperature
Remove sample gas in vapor, thus prevent vapor enter enrichment pipe 302 influence enrichment pipe 302 low temperature Concentration Sampling mistake
Journey separates vapor using the column temperature of chromatographic column 702, and not only separating rate is fast, and water removal effect is good, moreover, in the process of water removal
In, other VOC ingredients to be monitored are not influenced, so that other VOC ingredients to be monitored can smoothly input enrichment pipe 302, and
Be enriched with, this VOC monitoring device not only it is possible to prevente effectively from the prior art the drawbacks of, but also may be implemented automatic water-removing,
Continuous enrichment parsing and measurement function.
In the present embodiment, dehydration chromatographic column 103 preferentially uses commonly used in the prior art, the moderately polar color of resistance to steam
Column 702 is composed, length is generally 15-20cm, to flow out vapor quickly during dehydration.
In the present embodiment, the multiple valve can be preferentially using four-way valve 201 or six-way valve 303 or ten-way valve 102.
Quantitative sampling ring 104 usually has certain internal cavities, to accommodate sample gas, in the present embodiment, quantitative
Sample ring 104 can use the common quantitative loop in chromatography field.
As an example, as shown in Figure 1, in the present embodiment, multiple valve is using four-way valve 201, wherein four-way valve
201 include four connectors, respectively connector 1, connector 2 602, connector 3 603 and connector 4 604, such as
Shown in Fig. 1, the interface 6 506 and interface 8 508 are connected by pipeline and the connector 1 and connector 3 603 respectively
Logical, connector 2 602 is for emptying, and connector 4 604 is for being connected to enrichment pipe 302；
There are two types of working methods for four-way valve 201, and for the moment in working method, connector 1 is connected with connector 2 602
Logical, connector 3 603 is connected with connector 4 604, when being in working method two, connector 1 and 4 604 phase of connector
Connection, connector 2 602 are connected with connector 3 603, in this VOC monitoring device, by the work for controlling four-way valve 201
Mode can control the emptying of dehydration chromatographic column 103 or be connected with enrichment pipe 302, for example, as shown in fig. 6, at four-way valve 201
For the moment in working method, dehydration chromatographic column 103 is emptied by four-way valve 201, so as to vent water vapor；As shown in Fig. 4 or Fig. 5,
When four-way valve 201 is in working method two, dehydration chromatographic column 103 is connected by four-way valve 201 with enrichment pipe 302, so as to
Dewatered sample gas is inputted into enrichment pipe 302.
As shown in figure 4, further including enrichment resolver 301, the enrichment resolver 301 in further embodiment
Including six-way valve 303 and enrichment pipe 302, the six-way valve 303 include six ports, respectively port 1, port 2 402,
Port 3 403, port 4 404, port 5 405 and port 6 406, wherein
Port 1 is connected by pipeline with the connector 4 604, and one end of the enrichment pipe 302 passes through pipeline
It is connected with port 2 402, the other end is connected by pipeline with port 5 405, and port 3 403 is used to connect chromatographic column 702,
Port 4 404 is for inputting carrier gas, and port 6 406 is for emptying；
There are two types of working condition, in running order a period of time, port 1 and ports 2 402 to connect for the six-way valve 303
It is logical, port 3 403 is connected to port 4 404, port 5 405 is connected to port 6 406, when in running order two, port one
401 are connected to port 6 406, port 2 402 is connected to port 3 403, port 4 404 is connected to port 5 405；In this VOC
In monitoring device, by adjusting the working condition of six-way valve 303, it can control 302 Yes/No of enrichment pipe and be connected with chromatographic column 702
It is logical, for example, as shown in Fig. 4 or Fig. 5 or Fig. 6 or Fig. 7, when the in running order a period of time of six-way valve 303, enrichment pipe 302 not with color
Column 702 is composed to be connected to；As shown in figure 8, enrichment pipe 302 is connected to chromatographic column 702 as six-way valve 303 in running order two, this
When can use carrier gas and will be transferred in chromatographic column 702 from the VOC ingredient parsed on enrichment pipe 302.
In further embodiment, this VOC monitoring device further includes chromatographic analysis device 701, the chromatographic analysis device
701 include chromatographic column 702 and detector 703, and one end of the chromatographic column 702 is connected by pipeline with the port 3 403,
The other end is connected by pipeline with the detector 703, and chromatographic column 702 is for carrying out chromatographic isolation, and detector 703 is for examining
Survey ingredient and content.
In the preferred scheme, in the present embodiment, ten-way valve 102 can be ten-way valve sample injector, and/or, six-way valve
303 can be six-way valve sample injector, and/or, four-way valve 201 can be four-way valve sample injector, four-way valve sample injector, six-way valve into
Sample device, ten-way valve sample injector, chromatographic column 702 and detector 703 are the common equipment in chromatography field, structure and tool
The function of body, is well known to those of ordinary skill in the art already, and which is not described herein again；In addition, dehydration chromatographic column 103 and chromatographic column
702, all there is corresponding column temperature in actual use, also no longer do excessively repeat here.
It is appreciated that in the present embodiment, chromatographic column 702 can be preferentially using analysis chromatographic column 702.
Since a duty cycle of enrichment pipe 302 generally includes low temperature enrichment, high temperature parsing, cleaning three ranks of aging
Section, therefore in more perfect scheme, this VOC monitoring device further includes temperature controller, and the temperature controller is set to the enrichment pipe 302
Place, temperature controller are used to adjust the temperature of enrichment pipe 302, so that enrichment pipe 302 can carry out low temperature enrichment and high temperature parsing；It is existing
In technology, in VOC monitoring technical field, there are many ready-made enrichment pipes 302 and corresponding temperature controller, not another here
One enumerates.
According to above-mentioned VOC monitoring device, the present embodiment additionally provide it is a kind of using chromatographic column 702 separate sample gas in vapor
Method removed in sample gas by sample gas collected by the dehydration chromatographic column using the work column temperature of dehydration chromatographic column
Vapor；Specific step is as follows:
Step 1: ten-way valve 102 is in operating mode two, and six-way valve 303 in running order one, four-way valve 201 is in work
Make mode two, as shown in figure 4, at this point,
Sample gas inputs quantitative sampling ring 104, and is full of quantitative sampling ring 104；
Blowback cleaning is carried out to dehydration chromatographic column 103 using carrier gas, i.e., dehydration chromatographic column 103 is in blowback cleaning state；
Enrichment pipe 302 is in cleaning ageing state, i.e., is cleaned using carrier gas to enrichment pipe 302；
Chromatographic column 702 is in cleaning state, i.e., is cleaned using carrier gas to chromatographic column 702；
Step 2: after the time to be cleaned, switching the operating mode of ten-way valve 102, so that ten-way valve 102 is in work
Mode one, as shown in figure 5, at this point,
Six-way valve 303 takes off still in working condition one, four-way valve 201 still in working method two, quantitative sampling ring 104
Water chromatographic column 103, enrichment pipe 302 are interconnected；
The sample pneumatic transmission in quantitative sampling ring 104 is entered to be dehydrated chromatographic column 103 using carrier gas, utilizes dehydration chromatographic column 103
Work column temperature, and the fast VOC ingredient of the low boiling point, flowing in sample gas first flows out dehydration chromatographic column 103, and enters enrichment pipe 302；
Enrichment pipe 302 is in low temperature enrichment state, to be enriched with；
In this step, the low boiling point, the fast VOC ingredient of flowing of first outflow dehydration chromatographic column 103 include water solubility VOC at
Point, it is such as highly soluble in the alcohols VOC of water, in conventional water-eliminating method, is in charge of (nafion pipe, high molecular material) as used to receive
When removing the vapor in sample gas, for such water solubility VOC at branch as vapor is removed together, highest can lose 80%
Concentration causes measuring result error very big, and utilizes VOC monitoring device and method provided by the present embodiment, low boiling point, flowing
Fast VOC ingredient can vapor flow out dehydration chromatographic column 103 before outflow dehydration chromatographic column 103, thus avoid and water steam
Gas is removed together.
Step 3: when vapor will flow out dehydration chromatographic column 103, switching four-way valve 201, four-way valve 201 is made to be in work
Mode one, as shown in fig. 6, at this point,
Ten-way valve 102 is still in operating mode one, and six-way valve 303 is still in working condition one；
Vapor is flowed out from dehydration chromatographic column 103, and is emptied by four-way valve 201；Vapor is avoided to enter enrichment pipe
302, so as to effectively avoid saturation caused by vapor and ice from blocking up problem；
Step 4: after vapor flows completely out, switching the operating mode of ten-way valve 102, so that ten-way valve 102 is in work
Operation mode two, as shown in fig. 7, at this point,
Four-way valve 201 is dehydrated chromatographic column 103 and richness still in working condition one still in working method one, six-way valve 303
Collector 302 is connected；
High-carbon, the higher boiling VOC ingredient being dehydrated in chromatographic column 103 are gone out to be dehydrated chromatographic column 103, and flow into richness by carrier gas blowback
Collector 302；
Sample gas inputs quantitative sampling ring 104 again, and is full of quantitative sampling ring 104, completes sampling；
Step 5: when the VOC ingredient in dehydration chromatographic column 103 is blown into enrichment pipe 302 completely, and chromatographic column 702 is by carrier gas
After purging is clean, circulation executes above-mentioned steps 2, step 3 and step 4.
Step 6: when sample gas collection capacity reaches the required volume of detection in enrichment pipe 302, switching four-way valve 201 and six and lead to
Valve 303 makes four-way valve 201 be in working method two, six-way valve 303 in running order two, as shown in figure 8, at this point,
Ten-way valve 102 is still in operating mode two；
Enrichment pipe 302 is connected with chromatographic column 702；
Enrichment pipe 302 is in high temperature pyrolysis analysis state, and the VOC ingredient being enriched in enrichment pipe 302 is admitted to chromatographic column 702
It is separated, and is sent into detector 703 and is detected；To complete primary quantitative enrichment, analyte detection process.
In step 6, after enrichment pipe 302 completes Thermal desorption, switch the working condition of six-way valve 303, so that six-way valve 303
In running order one, measurement process next time can be can smoothly enter into, in actual application, repeated the above steps
It is convenient to realize automatic water-removing, continuous enrichment parsing and continuous on-line detection function.
The above description is merely a specific embodiment, but scope of protection of the present invention is not limited thereto, any
Those familiar with the art in the technical scope disclosed by the present invention, can easily think of the change or the replacement, and should all contain
Lid is within protection scope of the present invention.
Claims (10)
1. a kind of VOC monitoring device of separable vapor, which is characterized in that including dehydration sampler and multiple valve, institute
Stating dehydration sampler includes ten-way valve, quantitative sampling ring, dehydration chromatographic column, wherein
The ten-way valve include ten interfaces, respectively interface one, interface two, interface three, interface four, interface five, interface six, connect
Mouth seven, interface eight, interface nine and interface ten, interface one is for inputting sample gas, and interface two is for emptying, and the one of quantitative sampling ring
End is connected by pipeline with interface three, and the other end is connected with interface ten, and interface four and interface seven are respectively used to input carrier gas,
One end of dehydration chromatographic column is connected by pipeline with interface five, and the other end is connected with interface nine, and interface six and interface eight divide
It is not connected by pipeline with multiple valve,
The ten-way valve is there are two types of operating mode, and for the moment in operating mode, interface one is connected to interface two, interface three and interface
Four connections, interface five is connected to interface six, interface seven is connected to interface eight connectivity, interface nine with interface ten, is in operating mode
When two, interface one is connected to interface ten, interface two is connected to interface tee joint, interface four with interface five, interface six and interface seven
Connection, interface eight are connected to interface nine；
Quantitative sampling ring is used for the quantitative amount when ten-way valve is in operating mode two and samples gas, and dehydration chromatographic column is used in ten-way valve
It is connected for the moment with quantitative sampling ring in operating mode, and removes the vapor in sample gas, the sample gas after removing water steams passes through
Multiple valve inputs enrichment pipe.
2. the VOC monitoring device of separable vapor according to claim 1, which is characterized in that the dehydration chromatographic column
Using moderately polar resistance to steam chromatographic column.
3. the VOC monitoring device of separable vapor according to claim 2, which is characterized in that the dehydration chromatographic column
Length be 15-20cm.
4. the VOC monitoring device of separable vapor according to claim 1, which is characterized in that the multiple valve is
Four-way valve or six-way valve or ten-way valve.
5. the VOC monitoring device of separable vapor according to claim 1, which is characterized in that the multiple valve is
Four-way valve, the four-way valve include four connectors, respectively connector one, connector two, connector three and connector four,
Respectively by pipeline and the connector one and connector tee joint, connector two is used to empty for the interface six and interface eight,
Connector four is for being connected to enrichment pipe；
Four-way valve is there are two types of working method, for the moment in working method, connector one is connected with connector two, connector three and
Connector four is connected, and when being in working method two, connector one is connected with connector four, connector two and connector three-phase
Connection, the work method control by controlling four-way valve are dehydrated chromatographic column Yes/No and are connected with enrichment pipe.
6. the VOC monitoring device of separable vapor according to claim 5, which is characterized in that further include enrichment parsing
Device, the enrichment resolver include six-way valve and enrichment pipe, and the six-way valve includes six ports, respectively port one,
Port two, port three, port four, port five and port six, wherein
Port one is connected by pipeline with the connector four, and one end of the enrichment pipe is connected by pipeline with port two
Logical, the other end is connected by pipeline with port five, and port three is for connecting chromatographic column, and port four is for inputting carrier gas, port
Six for emptying；
The six-way valve is there are two types of working condition, in running order a period of time, and port one is connected to port two, port three and port
Four connections, port five are connected to port six, and when in running order two, port one is connected to port six, port two and port three
Connection, port four are connected to port five；By adjusting the working condition of six-way valve, control enrichment pipe Yes/No is connected with chromatographic column
It is logical.
7. the VOC monitoring device of separable vapor according to claim 6, which is characterized in that further include chromatography
Device, the chromatographic analysis device include chromatographic column and detector, and one end of the chromatographic column passes through pipeline and the port three
It is connected, the other end is connected by pipeline with the detector, and chromatographic column is for carrying out chromatographic isolation, and detector is for detecting
Ingredient and content.
8. the VOC monitoring device of separable vapor according to claim 7, which is characterized in that the ten-way valve is ten
Port valve sample injector, and/or, the six-way valve is six-way valve sample injector, and/or, the four-way valve is four-way valve sample injector.
9. a kind of method using vapor in chromatography post separation sample gas, which is characterized in that including VOC according to any one of claims 8
Monitoring device passes through the dehydration chromatographic column, benefit using the quantitative sampling ring quantitative collection sample gas, and by sample gas collected
With the vapor in the work column temperature removing sample gas of dehydration chromatographic column.
10. the method according to claim 9 using vapor in chromatography post separation sample gas, which is characterized in that including with
Lower step:
Step 1: ten-way valve is in operating mode two, six-way valve in running order one, and four-way valve is in working method two,
Sample gas is inputted into quantitative sampling ring, and is full of quantitative sampling ring；
Blowback cleaning is carried out to dehydration chromatographic column using carrier gas；Enrichment pipe is cleaned using carrier gas；Using carrier gas to chromatography
Column is cleaned；
Step 2: after to be cleaned, switching the operating mode of ten-way valve, so that ten-way valve is in operating mode one, utilize carrier gas
Sample pneumatic transmission in quantitative sampling ring is entered to be dehydrated chromatographic column, the low boiling point, stream using the work column temperature of dehydration chromatographic column, in sample gas
It moves fast VOC ingredient and first flows out dehydration chromatographic column, and enter enrichment pipe, enrichment pipe is in low temperature enrichment state；
Step 3: when vapor will flow out dehydration chromatographic column, switching four-way valve, four-way valve is made to be in working method one, vapor
From dehydration chromatographic column outflow, and emptied by four-way valve；
Step 4: after vapor flows completely out, switching the operating mode of ten-way valve, ten-way valve is made to be in operating mode two, be dehydrated
High-carbon, higher boiling VOC ingredient in chromatographic column are gone out to be dehydrated chromatographic column by carrier gas blowback, and flow into enrichment pipe；
Sample gas inputs quantitative sampling ring again, and is full of quantitative sampling ring, completes sampling；
Step 5: after the VOC ingredient in dehydration chromatographic column is blown into enrichment pipe completely, and chromatographic column is purged completely by carrier gas, following
Ring executes above-mentioned steps 2, step 3 and step 4；
Step 6: when the volume needed for the collection capacity of sample gas in enrichment pipe reaches detection, switching four-way valve and six-way valve, make four
Port valve and six-way valve are respectively at working method two and working condition two,
Enrichment pipe is in high temperature pyrolysis analysis state, and the VOC ingredient being enriched in enrichment pipe is admitted to chromatographic column and is separated, and send
Enter detector to be detected.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811639536.2A CN109521121A (en) | 2018-12-29 | 2018-12-29 | A kind of method of vapor in the VOC monitoring device and separation sample gas of separable vapor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811639536.2A CN109521121A (en) | 2018-12-29 | 2018-12-29 | A kind of method of vapor in the VOC monitoring device and separation sample gas of separable vapor |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109521121A true CN109521121A (en) | 2019-03-26 |
Family
ID=65797290
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811639536.2A Pending CN109521121A (en) | 2018-12-29 | 2018-12-29 | A kind of method of vapor in the VOC monitoring device and separation sample gas of separable vapor |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109521121A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111044649A (en) * | 2020-03-18 | 2020-04-21 | 山东海慧环境科技有限公司 | Gas analysis device |
| CN111351882A (en) * | 2020-04-10 | 2020-06-30 | 苏州天蓝分析仪器有限公司 | High-low carbon concentration on-line analysis and detection device |
| CN113376302A (en) * | 2021-04-14 | 2021-09-10 | 必睿思(杭州)科技有限公司 | Expired gas chromatographic analysis system and expired gas chromatographic analysis method |
| CN113917054A (en) * | 2021-09-29 | 2022-01-11 | 苏州天蓝分析仪器有限公司 | Device for automatically measuring atmosphere trace-level VOC (volatile organic compound) components |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4234315A (en) * | 1978-09-29 | 1980-11-18 | Phillips Petroleum Company | Gas chromatographic analysis method and apparatus |
| JP2005249691A (en) * | 2004-03-05 | 2005-09-15 | Toyota Central Res & Dev Lab Inc | Gas chromatograph unit and exhaust gas analytical method |
| WO2013037182A1 (en) * | 2011-09-16 | 2013-03-21 | 武汉市天虹仪表有限责任公司 | Online volatile organic compound analyzer and using method thereof |
| CN104777261A (en) * | 2015-04-10 | 2015-07-15 | 中国科学院生态环境研究中心 | Low temperature gas chromatography system, low temperature gas chromatography method and low temperature gas chromatography device of volatile organic compound in atmosphere |
| CN205404512U (en) * | 2016-01-22 | 2016-07-27 | 李勘 | Freezing continuous on line analyzer of VOC that collects of electron refrigeration second grade |
| CN206489127U (en) * | 2017-01-19 | 2017-09-12 | 常州磐诺仪器有限公司 | A kind of environment VOCs monitors mass spectrometer apparatus on-line |
| US20170341056A1 (en) * | 2016-05-24 | 2017-11-30 | Max Analytical Technologies, Inc. | GC-FTIR and Mode of Operation to Address Water Interference |
-
2018
- 2018-12-29 CN CN201811639536.2A patent/CN109521121A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4234315A (en) * | 1978-09-29 | 1980-11-18 | Phillips Petroleum Company | Gas chromatographic analysis method and apparatus |
| JP2005249691A (en) * | 2004-03-05 | 2005-09-15 | Toyota Central Res & Dev Lab Inc | Gas chromatograph unit and exhaust gas analytical method |
| WO2013037182A1 (en) * | 2011-09-16 | 2013-03-21 | 武汉市天虹仪表有限责任公司 | Online volatile organic compound analyzer and using method thereof |
| CN104777261A (en) * | 2015-04-10 | 2015-07-15 | 中国科学院生态环境研究中心 | Low temperature gas chromatography system, low temperature gas chromatography method and low temperature gas chromatography device of volatile organic compound in atmosphere |
| CN205404512U (en) * | 2016-01-22 | 2016-07-27 | 李勘 | Freezing continuous on line analyzer of VOC that collects of electron refrigeration second grade |
| US20170341056A1 (en) * | 2016-05-24 | 2017-11-30 | Max Analytical Technologies, Inc. | GC-FTIR and Mode of Operation to Address Water Interference |
| CN206489127U (en) * | 2017-01-19 | 2017-09-12 | 常州磐诺仪器有限公司 | A kind of environment VOCs monitors mass spectrometer apparatus on-line |
Non-Patent Citations (2)
| Title |
|---|
| 谢裕焕 等: "污染源有机物在线监测技术", no. 25, pages 160 * |
| 陆德民 等: "石油化工自动控制设计手册", 中国医药科技出版社, pages: 221 - 224 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111044649A (en) * | 2020-03-18 | 2020-04-21 | 山东海慧环境科技有限公司 | Gas analysis device |
| CN111351882A (en) * | 2020-04-10 | 2020-06-30 | 苏州天蓝分析仪器有限公司 | High-low carbon concentration on-line analysis and detection device |
| CN113376302A (en) * | 2021-04-14 | 2021-09-10 | 必睿思(杭州)科技有限公司 | Expired gas chromatographic analysis system and expired gas chromatographic analysis method |
| CN113376302B (en) * | 2021-04-14 | 2024-06-18 | 必睿思(杭州)科技有限公司 | Exhaled breath gas chromatography analysis system and method |
| CN113917054A (en) * | 2021-09-29 | 2022-01-11 | 苏州天蓝分析仪器有限公司 | Device for automatically measuring atmosphere trace-level VOC (volatile organic compound) components |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109521121A (en) | A kind of method of vapor in the VOC monitoring device and separation sample gas of separable vapor | |
| CN107247108B (en) | Transformer oil on-line monitoring high-concentration vacuum oil-gas separation device and method | |
| CN102353724B (en) | On-line detection system and method of trace dissolved gas in organic oil | |
| CN101059525B (en) | Self-adaptive monitoring method for gas dissolved in oil of traction transformer, and the device thereof | |
| CN102650623A (en) | Device for detection of low-concentration Freon in seawater and production method thereof | |
| CN202676680U (en) | Device capable of detecting low-concentration freon in seawater | |
| KR100238384B1 (en) | Gas analyzer and gas analysis method | |
| CN209432755U (en) | A kind of VOC monitoring device of separable vapor | |
| US6497136B2 (en) | Trace-level gas analysis apparatus and method | |
| CN103134875A (en) | On-line pretreatment device of aquatic volatile organic compounds | |
| JP2000081422A (en) | Automated multipoint trace material analysis device and method and automated trace material analysis device and method | |
| CN203965453U (en) | A kind of oil dissolved gas on-Line Monitor Device | |
| CN108037217A (en) | A kind of Portable exhaust gas analyzer and its operating method | |
| CN209280647U (en) | A kind of continuous quadratic that multistage parallel takes turns to operate enrichment resolver | |
| CN112986442B (en) | Oil-gas integrated detection gas chromatograph for high-voltage electrical equipment | |
| CN103521480B (en) | A kind of cleaning method of the automatic clearing apparatus of sampling needle | |
| CN109406692A (en) | Continuous quadratic enrichment resolver that is a kind of multistage and running in turn | |
| CN109696495A (en) | A kind of VOC monitoring device and method that accurate quantification sampling may be implemented | |
| CN213780031U (en) | Online monitoring device for dissolved gas in transformer oil | |
| CN111842361A (en) | Sampling pump cleaning device with automatic control function and cleaning method | |
| CN110715926B (en) | Detection gas circuit for measuring automobile exhaust | |
| CN207992252U (en) | A kind of automatic sampling apparatus | |
| CN211602624U (en) | Pretreatment system of trace gas analysis equipment | |
| CN206362811U (en) | A kind of automatic sampler for quantitative capillary tube electrophoresis apparatus | |
| CN108169401A (en) | A kind of countryside portable gas-detecting device and its operating method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190326 |