CN107643350A - Full two dimension and the apparatus and method of one-dimensional gas chromatograph switching - Google Patents
Full two dimension and the apparatus and method of one-dimensional gas chromatograph switching Download PDFInfo
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- 230000000737 periodic effect Effects 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
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Abstract
The invention discloses full two dimension and the apparatus and method of one-dimensional gas chromatograph switching, the switching device includes tonifying Qi module, switching switch, the oneth the 4th interface, the first and second vapour locks；The first end of second interface is connected with the first end of the second vapour lock by the first pipeline, and the second end of the second vapour lock is connected by the second pipeline with the first end of the 3rd interface；The outlet of tonifying Qi module is connected by the 3rd pipeline with switching switch, switching switch first outlet is connected by the 4th pipeline with the first pipeline in first node, and the both ends that switching switch second outlet connects first vapour lock in section point connect the 4th pipeline and the 5th pipeline respectively；First interface first end is connected by the first pipeline between pipeline and first node and section point, and the 4th interface first end is connected by pipeline with the second pipeline.The present invention can automatically switch between complete two peacekeepings one-dimensional gas chromatograph, meet the demand that complete two peacekeepings one-dimensional gas chromatograph is used alternatingly with an instrument.
Description
Technical field
It is specifically a kind of comprehensive two dimensional gas chromatography instrument in complete two peacekeeping one the present invention relates to technical field of analytical instruments
The device switched between dimension.
Background technology
Comprehensive two dimensional gas chromatography (Comprehensive Two-dimensional Gas Chromatography, referred to as
GC × GC) it is a kind of new chromatography skill that last century the nineties grow up on the basis of traditional one-dimensional gas chromatograph
Art.Its cardinal principle is that separating mechanism is different and independent two chromatographic columns connect in a series arrangement mutually, and centre is equipped with
One modulator, all distillates after first pillar separates are carried out after concentration aggregation in modulator with periodic arteries and veins
The form of punching is discharged into second pillar and carries out continuing to separate, and finally enters chromatographic detector.It is so incomplete in the first dimension
Separated component (distillate altogether) is further separated in the second dimension, has reached the effect of orthogonal separation.But some situations
Lower user wants to close the complete two-dimentional function of this comprehensive two dimensional gas chromatography instrument, and tradition is run using only the first root chromatogram column
The method of one-dimensional gas chromatograph.But due to comprehensive two dimensional gas chromatography more than traditional one-dimensional gas-chromatography modulator and second post
Son, hamper the method that user directly runs traditional one-dimensional gas-chromatography：
1. the stationary phase for second pillar being connected in stream, internal diameter size often have huge difference with first pillar
Not, directly operation traditional one-dimensional gas-chromatography method the separating resulting of first pillar can be re-mixed, separated, produce compared with
Big interference, cause component retention time compare the result of a pillar purely with elution order not it is contemplated that；
2. modulator part is connected in stream, analyte necessarily flows through modulator.Its stream of some modulators
Outside by burner hearth, non-operating state can not keep proper temperature, cause the analyte in stream to be arrested in the modulation of cooling
In device pipeline, can not smoothly it flow out.
The present invention proposes a kind of comprehensive two dimensional gas chromatography instrument can between comprehensive two dimensional gas chromatography and one-dimensional gas chromatograph
Automatically switch, change the scheme of stream without dismounting.Greatly facilitate user and complete two-dimentional gas phase color is used alternatingly with an instrument
The demand of spectrum and one-dimensional gas chromatograph.
The content of the invention
The present invention proposes switching device and method of a kind of comprehensive two dimensional gas chromatography instrument between complete two peacekeeping is one-dimensional
Scheme, deficiency of the prior art is overcome, there is switching simplicity, separating resulting is reliable, avoids component retention time and outflow
The advantages that result generation significant change or analyte retardance of the order compared to a pure pillar can not smoothly flow out.
First, when the present invention switches comprehensive two dimensional gas chromatography instrument between complete two peacekeeping is one-dimensional, stream is changed without dismounting
Road, only it need to switch the state for once switching switch.The switching action can easily manually, electronic, pneumatic or other are automatic
Change means are completed, if implementation is proper, switching switch can be controlled by software, completes to automatically switch.If dismounting changes stream,
Pipeline can be caused to be truncated, hermetic collar failure need to change and gas leakage risk, this programme have evaded above-mentioned deficiency；
Secondly, when being switched to one-dimensional gas chromatograph, analyte is not passed through two-dimensional columns, will not be disturbed by two-dimensional columns, changes
Separation sequence, reliable results, analyze it is contemplated that being equal to the standard one-dimensional gas chromatograph carried out using only an one-dimensional post；
Furthermore when being switched to one-dimensional gas chromatograph, analyte avoids flowing through modulator so as to avoid causing in stream
Analyte, which is arrested in the modulator pipeline of cooling, smoothly to flow out.
To realize the purpose of the present invention, it is achieved using following technical scheme：
It is a kind of to be used for full two dimension and the switching device of one-dimensional gas chromatograph switching, including tonifying Qi module, switching switch, first
Interface, second interface, the 3rd interface, the 4th interface, the first vapour lock and the second vapour lock, wherein：
The first end of second interface is connected with the first end of the second vapour lock by the first pipeline, and the second end of the second vapour lock leads to
The first end that the second pipeline is crossed with the 3rd interface is connected；The import phase that the outlet of tonifying Qi module passes through the 3rd pipeline and switching switch
Even, the first outlet for switching switch is connected by the 4th pipeline with the first pipeline in first node, switches the second outlet of switch
It is connected by the 5th pipeline with the first pipeline in section point, the both ends of first vapour lock connect the 4th pipeline and the 5th respectively
Pipeline, and the tie point of the first end of the first vapour lock and the 4th pipeline is switched between first outlet and first node positioned at switching,
Second end of the first vapour lock and the tie point of the 5th pipeline are between switching switch second outlet and section point；First interface
First end connected by the first pipeline between pipeline and first node and section point, the first end of the 4th interface passes through pipe
Road is connected with the second pipeline, and tie point is between the first end of the 3rd interface and the second end of the second vapour lock.
Described switching device, wherein：The first node is compared with section point more close to second interface.
Described switching device, wherein：The switching switch is used to switch air-flow between first outlet and second outlet
Output；Or exported for switching to the air-flow of first node or section point.
Described switching device, wherein：Second end of first interface is used to be connected with the outlet of one-dimensional post by pipeline, the
Second end of two interfaces is used for the entrance that modulator is connected by pipeline, and the outlet of modulator is used for the import for connecting two-dimensional columns,
Second end of the 3rd interface is used for the outlet for connecting two-dimensional columns, and the second end of the 4th interface is used for by pipeline connecting detection device
Import.
A kind of gas chromatograph, including one of as above described in switching device, injection port, one-dimensional post, modulator, two-dimensional columns
And detector, it is characterised in that：Second end of the first interface is connected by pipeline with the outlet of one-dimensional post, and one-dimensional post enters
Mouth is connected with injection port, and the second end of second interface connects the entrance of modulator by pipeline, and the outlet of modulator passes through pipeline
It is connected with the import of two-dimensional columns, the second end of the 3rd interface of outlet connection of two-dimensional columns；Second end of the 4th interface passes through pipeline
The import of connecting detection device.
A kind of method of comprehensive two dimensional gas chromatography and one-dimensional gas chromatograph switching, this method use gas phase color as described above
Spectrometer, this method include：
Comprehensive two dimensional gas chromatography detecting step：Tonifying Qi module provides carrier gas, and carrier gas is opened under switching switch guiding from switching
The second outlet of pass enters lower stream, and wherein trickle tonifying Qi flows to first node through the first vapour lock, remaining most air-flow stream
To section point, be divided into two-way here, the first via flows downwardly through the second vapour lock, another way upwards with flow into first interface after
One-dimensional post sample gas is converged, then upwards at first node with flowing through the sample gas that the trickle tonifying Qi of vapour lock is merged into as, flows
Modulated device and two-dimensional columns, then and flow through the second vapour lock carrier gas converge after through the 4th interface flow into detector, complete full two dimension
Gas chromatographic detection；Or：
One-dimensional gas chromatograph detecting step：Tonifying Qi module provides carrier gas, under switching switch guiding, from the of switching switch
One outlet enters upper stream, and wherein trickle tonifying Qi flows to section point through the first vapour lock, remaining most air flow direction first
Node, it is divided into two-way here, the first via flows up through modulator and two-dimensional columns, leads to the 4th interface；Another way downwards with stream
Enter the one-dimensional post sample gas after first interface to converge, the trickle tonifying Qi with flowing through the first vapour lock at section point still further below converges
Synthesize sample gas, flow through the second vapour lock, the pure carrier gas stream with flowing through modulator converge after through the 4th interface flow into detector, it is complete
Detected into one-dimensional gas chromatograph.
Described comprehensive two dimensional gas chromatography and the method for one-dimensional gas chromatograph switching, wherein：The carrier gas of tonifying Qi module output
Air pressure determined by below equation (1)：
Wherein：
Pi：Superfeed pressure, it is absolute pressure,
Po：Detector end pressure, it is absolute pressure,
Tref：Reference temperature,
F：Modulator or the target flow of the second vapour lock are flowed through,
η：Viscosity of the carrier gas under Current Temperatures,
pref：Reference pressure,
T：Carrier gas temperature, it is absolute temperature,
R:The vapour lock of vapour lock value, modulator and two-dimensional columns altogether；Or second vapour lock vapour lock value.
Described comprehensive two dimensional gas chromatography and the method for one-dimensional gas chromatograph switching, wherein flowing through the flow F of the first vapour lock
Calculated according to below equation (2)：
Wherein：
Pi：Superfeed pressure, it is absolute pressure,
Po：Detector end pressure, it is absolute pressure,
Tref：Reference temperature,
η：Viscosity of the carrier gas under Current Temperatures,
pref：Reference pressure,
T：Carrier gas temperature, it is absolute temperature,
R is the vapour lock value of first vapour lock.
Described comprehensive two dimensional gas chromatography and the method for one-dimensional gas chromatograph switching, wherein first vapour lock is regular
Round pipe, its vapour lock value R are calculated by following formula：
L：Vapour lock duct length,
r：Vapour lock internal diameter of the pipeline.
Brief description of the drawings
Accompanying drawing 1 is the switching device (part in dotted box) of comprehensive two dimensional gas chromatography of the present invention and one-dimensional gas chromatograph
The schematic diagram being installed in comprehensive two dimensional gas chromatography system；
Accompanying drawing 2 is switching device schematic diagram in comprehensive two dimensional gas chromatography working condition；
Accompanying drawing 3 is switching device schematic diagram in one-dimensional gas chromatograph working condition.
Embodiment
Fig. 1-3 and the optional embodiment of the present invention is following description described to instruct how those skilled in the art implement
It is of the invention with reproducing.In order to instruct technical solution of the present invention, simplify or eliminate some conventional aspects, and lifted with concrete numerical value
Example explanation.Those skilled in the art should understand that modification or replacement from these embodiments, the change of parameter will be in this hair
In bright scope.Those skilled in the art should understand that following characteristics can combine to form the multiple of the present invention in a variety of ways
Modification.Thus, the invention is not limited in following optional embodiments, and only limited by claim and their equivalent.
The present invention is described in further detail by embodiment below in conjunction with accompanying drawing：
As shown in figure 1, the two-dimentional and one-dimensional switching device of the comprehensive two dimensional gas chromatography of the present invention is dashed rectangle inframe
Part, the device is installed in comprehensive two dimensional gas chromatography system in figure.The switching device includes tonifying Qi module, switching
Switch, interface 1, interface 2, interface 3, interface 4, vapour lock 1 and vapour lock 2.The first end of interface 2 passes through the first pipe with the first end of vapour lock 2
Road is connected, and the end of vapour lock 2 second is connected by the second pipeline with the first end of interface 3；The outlet of tonifying Qi module passes through the 3rd pipeline
Import with switching switch is connected, and the first outlet for switching switch is connected by the 4th pipeline with the first pipeline in first node,
The second outlet of switching switch is connected by the 5th pipeline with the first pipeline in section point, and the first node is compared with section point
More close to interface 2, the both ends of vapour lock 1 connect the 4th pipeline and the 5th pipeline and (switch the first outlet of switch and the respectively
Vapour lock 1 is connected between two outlets).The first end of interface 1 is connected by the pipeline between pipeline and node 1 and node 2, interface
4 first end is connected by pipeline with the second pipeline.Second end of interface 1 is connected by pipeline with the outlet of one-dimensional post, one-dimensional
The import of post is connected with injection port, and the second end of interface 2 connects the first end (entrance) of modulator by pipeline, and the of modulator
Two ends (outlet) are connected by the import of pipeline and two-dimensional columns, the second end of the outlet connecting interface 3 of two-dimensional columns；The of interface 4
The import that two ends pass through pipeline connecting detection device.The switching switch can switch gas between first outlet and second outlet
Stream.
To sum up, comprehensive two dimensional gas chromatography system of the invention from injection port connection first dimension analytical column (first capillary column,
Referred to as one-dimensional post) entrance, one-dimensional column outlet is connected to the interface 1 of switching device, and the interface 2 of switching device is connected to modulator
Entrance.Modulator outlet connects the second dimension analytical column (second capillary column, abbreviation two-dimensional columns) entrance, and two-dimentional column outlet, which is connected to, to be cut
The interface 3 of changing device, the interface 4 of switching device are connected to detector.
Tonifying Qi module, what the air-flow that the tonifying Qi module provides switching was set with driving the component flow direction of one-dimensional post outflow
Direction, supplemental air flow is provided to the second dimension analytical column when doing complete two-dimentional.Its upstream connects source of the gas, and downstream connection is singly entered to one
The switchings switch of the double outlets of mouth.Switching switch, it has single import and double outlet, manually, electronic, pneumatic mode or other
Type of drive switches between two outlets.Its entrance is tonifying Qi module, exports the gas piping for both direction, leads to all the way
Node 1, interface 2, and then connect the entrance of the hot modulator of comprehensive two dimensional gas chromatography；Another way leads to node 2, vapour lock 2, makes part
Gas is directly communicated to detector without modulator, two-dimensional columns.
Vapour lock 1, between the exit gas pipeline of switching switch both direction, its role is to can make switching
Valve do not import make-up gas that also there is a small amount of make-up gas to flow into all the way, referred to as trickle tonifying Qi, avoid analyzed gas
Spread to that of importing make-up gas at two-way pipeline river conjunction, so as to cause peak stretching, hangover, or even be brought into down all the way
Once analyze, disturb result.Depending on the size of vapour lock 1 is by make-up gas air pressure and the target flow size of trickle tonifying Qi.
Vapour lock 2, between the gas exit line all the way of switching valve and the interface 4 of switching device.Its role is to
Match the vapour lock of modulator and two-dimensional columns, can make flow through modulator, two-dimensional columns supplemental air flow and eventually enter into detector
Air-flow under the two states of switching valve, i.e., switching pass through 2 two kinds of paths of modulator or vapour lock, its flow, pressure are maintained at
In zone of reasonableness.
The method of comprehensive two dimensional gas chromatography and the one-dimensional gas chromatograph switching of the embodiment of the present invention is as follows：
When comprehensive two dimensional gas chromatography method to be implemented, direction and the air flow direction for switching switch are as shown in Figure 2.For side
Just illustrate, the uninterrupted mark of citing is in fig. 2.Tonifying Qi module gives outflow 5mL/min, under switching switch guiding, enters
Enter lower stream, wherein 0.1mL/min trickles tonifying Qi flows to node 1 through vapour lock 1, remaining most air-flow 4.9mL/min flow direction
Node 2, be divided into 2 tunnels here, 3mL/min flows downwardly through vapour lock 2 all the way, another way 1.9mL/min upwards with flow into interface 1 after
One-dimensional post sample gas flow 1mL/min converge, turn into 2.9mL/min air-flow, then upwards at node 1 with flowing through vapour lock 1
Trickle tonifying Qi be merged into as 3mL/min sample gas, flow through modulator and two-dimensional columns, complete sample analyte in modulator
Trapping, analyze in release and two-dimensional columns.The flow 3mL/min for flowing through modulator and the flow 3mL/min for flowing through vapour lock 2 converge
Detector is flowed into by interface 4, completes comprehensive two dimensional gas chromatography detection.
When one-dimensional gas chromatograph method to be implemented, direction and the air flow direction for switching switch are as shown in Figure 3.Now by
Analyte produces interference without two-dimensional columns, separation that will not be to one-dimensional post；The stream of vapour lock 2 is completely disposed in burner hearth, so complete
Avoid analyte entirely to be arrested in the modulator pipeline of cooling, the problem of can not smoothly flowing out.For convenience of description, illustrate
Uninterrupted mark in figure 3.Tonifying Qi module gives outflow 5mL/min, under switching switch guiding, into upper stream, its
Middle 0.1mL/min trickles tonifying Qi flows to node 2 through vapour lock 1, and remaining most air-flow 4.9mL/min flows to node 1, here
It is divided into 2 tunnels, 3mL/min, which is flowed up through, all the way flows through modulator and two-dimensional columns, leads to interface 4；Another way 1.9mL/min downwards with
The one-dimensional post sample gas flow 1mL/min flowed into after interface 1 converges, and turns into 2.9mL/min air-flow, still further below at node 2
Trickle tonifying Qi with flowing through vapour lock 1 is merged into as 3mL/min sample gas, flows through vapour lock 2, the pure tonifying Qi stream with flowing through modulator
Amount 3mL/min is detected after converging through the inflow detector of interface 4, completion one-dimensional gas chromatograph.
The flow of above-mentioned setting is realized, the air pressure and vapour lock 1, the size of vapour lock 2 of tonifying Qi need to be controlled.The air pressure of tonifying Qi by
Following formula decision,
Pi：Superfeed pressure (absolute pressure), unit：Pa
Po：Detector end pressure (absolute pressure), unit：Pa
Tref：Reference temperature, usually 25 degrees Celsius of room temperature, i.e. 298K
F：Flow through the target flow of modulator (or vapour lock 2), unit：mL/min
η：Viscosity of the carrier gas under Current Temperatures, unit：poise
pref：Reference pressure, usually an atmospheric pressure, 1.013*10^5Pa
T：Carrier gas temperature (absolute temperature), unit：K
R:The vapour lock (or vapour lock of vapour lock 2) of vapour lock, modulator and two-dimensional columns altogether
For the modulator of determination and two-dimensional columns, the decision of above-mentioned air pressure is relevant with flow and temperature, need to give and mend
The pressure curve that gas module is set is calculated by above formula.
The size of vapour lock 2 is determined under given tonifying Qi module pressure by the uninterrupted of vapour lock 2, is also related to entrance
The total flow of detector.Vapour lock 2 should not be too small, so that the flow into detector is excessive, influences performance, and waste gas；Gas
Resistance 2 should not be too big, so that too small by the flow of vapour lock 2, when switching to one-dimensional mode, the outflow flow of one-dimensional post can not be complete
It is complete to enter the stream of vapour lock 2, and the stream for thering is part to be spilled over to modulator, cause to switch one-dimensional mode failure.Pass through vapour lock 2
The scope that flow should follow is：1) it is more than one-dimensional column flow；2) it is less than detector and suggests that flow subtracts modulator flow all the way.
Flowing through the flow of vapour lock 1 can calculate according to following formula,
Vapour lock leads to the round pipe of common rule, such as empty vitreous silica capillary column to serve as, and its big I passes through following formula
Calculate：
L：Vapour lock duct length, unit：m
r：Vapour lock internal diameter of the pipeline, unit：m
The size of vapour lock 1 can also be calculated by above formula.
Claims (4)
1. a kind of be used for two dimension entirely and the switching device of one-dimensional gas chromatograph switching, including tonifying Qi module, switching switch, first connects
Mouth, second interface, the 3rd interface, the 4th interface, the first vapour lock and the second vapour lock, it is characterised in that：
The first end of second interface is connected with the first end of the second vapour lock by the first pipeline, and the second end of the second vapour lock passes through
Two pipelines are connected with the first end of the 3rd interface；The outlet of tonifying Qi module is connected by the 3rd pipeline with the import of switching switch,
The first outlet of switching switch is connected by the 4th pipeline with the first pipeline in first node, and the second outlet for switching switch passes through
5th pipeline is connected with the first pipeline in section point, and the both ends of first vapour lock connect the 4th pipeline and the 5th pipe respectively
Road, and the tie point of the first end of the first vapour lock and the 4th pipeline is switched between first outlet and first node positioned at switching, the
Second end of one vapour lock and the tie point of the 5th pipeline are between switching switch second outlet and section point；First interface
First end is connected by the first pipeline between pipeline and first node and section point, and the first end of the 4th interface passes through pipeline
It is connected with the second pipeline, and tie point is between the first end of the 3rd interface and the second end of the second vapour lock.
2. switching device according to claim 1, it is characterised in that：The first node is compared with section point more close to
Two interfaces.
3. a kind of gas chromatograph, including switching device as described in one of claim 1-2, injection port, one-dimensional post, modulation
Device, two-dimensional columns and detector, it is characterised in that：Second end of the first interface is connected by pipeline with the outlet of one-dimensional post,
The import of one-dimensional post is connected with injection port, and the second end of second interface connects the entrance of modulator by pipeline, and modulator goes out
Mouth is connected by the import of pipeline and two-dimensional columns, the second end of the 3rd interface of outlet connection of two-dimensional columns；The second of 4th interface
The import that end passes through pipeline connecting detection device.
4. a kind of comprehensive two dimensional gas chromatography and the method for one-dimensional gas chromatograph switching, it is characterised in that this method uses right such as will
The gas chromatograph described in 3 is sought, this method includes：
Comprehensive two dimensional gas chromatography detecting step：Tonifying Qi module provides carrier gas, and carrier gas is under switching switch guiding, from switching switch
Second outlet enters lower stream, and wherein trickle tonifying Qi flows to first node through the first vapour lock, remaining most air flow direction
Two nodes, are divided into two-way here, and the first via flows downwardly through the second vapour lock, another way upwards with flow into it is one-dimensional after first interface
Post sample gas is converged, then upwards at first node with flowing through the sample gas that the trickle tonifying Qi of vapour lock is merged into as, flows through tune
Device processed and two-dimensional columns, then and flow through the second vapour lock carrier gas converge after through the 4th interface flow into detector, complete complete two-dimentional gas phase
Chromatogram detects；Or：
One-dimensional gas chromatograph detecting step：Tonifying Qi module provides carrier gas, under switching switch guiding, goes out from the first of switching switch
Mouth enters upper stream, and wherein trickle tonifying Qi flows to section point through the first vapour lock, remaining most air flow direction first node,
It is divided into two-way here, the first via flows up through modulator and two-dimensional columns, leads to the 4th interface；Another way is downwards with flowing into first
One-dimensional post sample gas after interface is converged, and the trickle tonifying Qi with flowing through the first vapour lock at section point still further below is merged into as
Sample gas, the second vapour lock is flowed through, the pure carrier gas stream with flowing through modulator is one-dimensional through the 4th interface inflow detector, completion after converging
Gas chromatographic detection.
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| CN109580852A (en) * | 2019-02-03 | 2019-04-05 | 南京九岚纹仪器科技有限公司 | A kind of comprehensive two dimensional gas chromatography instrument and modulator approach |
| CN113804782A (en) * | 2021-09-06 | 2021-12-17 | 中国环境监测总站 | Quantitative testing method and device for volatile organic compounds |
| CN115308348A (en) * | 2022-09-02 | 2022-11-08 | 中国石油化工股份有限公司 | Full-two-dimensional gas chromatography analysis method for unconventional additives in gasoline |
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| CN109580852A (en) * | 2019-02-03 | 2019-04-05 | 南京九岚纹仪器科技有限公司 | A kind of comprehensive two dimensional gas chromatography instrument and modulator approach |
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| CN109580852B (en) * | 2019-02-03 | 2022-04-22 | 南京九岚纹仪器科技有限公司 | Full-two-dimensional gas chromatograph and modulation method |
| US11940425B2 (en) | 2019-02-03 | 2024-03-26 | Nanjing Nine Max Instrument Co. Ltd. | Modulation method using a comprehensive two-dimensional gas chromatograph |
| CN113804782A (en) * | 2021-09-06 | 2021-12-17 | 中国环境监测总站 | Quantitative testing method and device for volatile organic compounds |
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