CN110531018A - A kind of pocket type method direct injected GC-O/MS test macro and its test method - Google Patents
A kind of pocket type method direct injected GC-O/MS test macro and its test method Download PDFInfo
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- CN110531018A CN110531018A CN201910891327.5A CN201910891327A CN110531018A CN 110531018 A CN110531018 A CN 110531018A CN 201910891327 A CN201910891327 A CN 201910891327A CN 110531018 A CN110531018 A CN 110531018A
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- 238000000034 method Methods 0.000 title claims abstract description 91
- 238000012360 testing method Methods 0.000 title claims abstract description 30
- 238000010998 test method Methods 0.000 title claims abstract description 9
- 230000035943 smell Effects 0.000 claims abstract description 63
- 238000004817 gas chromatography Methods 0.000 claims abstract description 32
- 241001062472 Stokellia anisodon Species 0.000 claims abstract description 15
- 239000000126 substance Substances 0.000 claims abstract description 14
- 230000008676 import Effects 0.000 claims abstract description 9
- 238000004458 analytical method Methods 0.000 claims abstract description 8
- 239000007789 gas Substances 0.000 claims description 74
- 238000005070 sampling Methods 0.000 claims description 16
- 239000012159 carrier gas Substances 0.000 claims description 13
- 238000002347 injection Methods 0.000 claims description 11
- 239000007924 injection Substances 0.000 claims description 11
- 239000000470 constituent Substances 0.000 claims description 6
- 238000001514 detection method Methods 0.000 claims description 6
- 238000007664 blowing Methods 0.000 claims description 3
- 238000004587 chromatography analysis Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000005259 measurement Methods 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 7
- 239000004615 ingredient Substances 0.000 abstract description 4
- 238000001819 mass spectrum Methods 0.000 description 16
- 238000002474 experimental method Methods 0.000 description 6
- 238000003795 desorption Methods 0.000 description 5
- 238000001179 sorption measurement Methods 0.000 description 5
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- WQOXQRCZOLPYPM-UHFFFAOYSA-N dimethyl disulfide Chemical compound CSSC WQOXQRCZOLPYPM-UHFFFAOYSA-N 0.000 description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000796 flavoring agent Substances 0.000 description 3
- 235000019634 flavors Nutrition 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 239000005864 Sulphur Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- PYGSKMBEVAICCR-UHFFFAOYSA-N hexa-1,5-diene Chemical group C=CCCC=C PYGSKMBEVAICCR-UHFFFAOYSA-N 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 238000004949 mass spectrometry Methods 0.000 description 2
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 description 1
- 240000008067 Cucumis sativus Species 0.000 description 1
- 235000010799 Cucumis sativus var sativus Nutrition 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 244000061176 Nicotiana tabacum Species 0.000 description 1
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 208000011117 substance-related disease Diseases 0.000 description 1
- 238000006467 substitution reaction Methods 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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/16—Injection
- G01N30/20—Injection using a sampling valve
-
- 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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
-
- 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
- G01N2030/201—Injection using a sampling valve multiport valves, i.e. having more than two ports
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- 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)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The present invention relates to a kind of pocket type method direct injected GC-O/MS test macro and its test methods, the test macro includes baking oven, PVF sampler bag, pocket type method direct injected device, gas chromatograph, mass spectrograph, it smells and distinguishes instrument, PVF sampler bag is provided in baking oven, PVF sampler bag is connected by interface with one end of pocket type method direct injected device input pipe, the air inlet of pocket type method direct injected device input pipe other end connection pocket type method direct injected device, the gas outlet of pocket type method direct injected device connects the import of gas chromatograph by gas-chromatography input pipe, the outlet of gas chromatograph is separately connected mass spectrograph by triple valve, it smells and distinguishes instrument input pipe, it smells and distinguishes that the connection of the instrument input pipe other end smells and distinguishes instrument, connection, which is smelt, distinguishes that instrument passes through connection smell recording device；The present invention can be realized pocket type method direct injected, can reduce volatile materials loss, be suitble to the analysis of complicated ingredient, be conducive to odoring substance and smelling the capture and identification for debating port.
Description
[technical field]
The present invention relates to gas chromatography combined with mass spectrometry technical field, specifically a kind of pocket type method direct injected GC-O/
MS test macro and its test method.
[background technique]
Gas chromatography combined with mass spectrometry technology (GC-MS) combines gas-chromatography olfactometry (GC-O) to be formed by GC-O/
MS technology micro volatile organic substance (VOC) can not only be carried out it is qualitative and quantitative, more can organoleptic analysis combine, there is height
It is sensitivity, highly selective, and the analysis of the smell caused by volatile materials combines, and is usually used in analyzing the flavor in food
Flavor matter in substance and tobacco leaf.What wherein the preceding input mode application of gas chromatographic analysis was most is thermal desorption (TDS) sample introduction
Means trap the volatile materials that sample distributes using adsorption tubes such as TENAX or active carbons, by TDS to sampling pipe
In substance carry out thermal desorption and be enriched with into cold-trap, later by carrier gas by substance feeding gas-chromatography (GC) separate,
The gas isolated while entering mass spectrum (MS) and distinguish that instrument (sniffer) carries out qualitative, quantitative and smell is smelt and distinguished with smelling.TDS sample introduction mesh
It is preceding to apply comparative maturity, however limited by adsorption tube adsorption stuffing, Cucumber can adsorbed and lost in desorption process；
When the humidity of objective environment is higher, sample moisture content is excessive also to be damaged pillar, cause the visitors such as data result distortion
Sight problem.
[summary of the invention]
A kind of pocket type method direct injected GC-O/MS test system is provided present invention aim to solve above-mentioned deficiency
System, can be realized pocket type method direct injected, so as to reduce volatile materials loss, is suitble to the analysis of complicated ingredient, is conducive to
Odoring substance debates the capture and identification of port smelling.
A kind of pocket type method direct injected GC-O/MS test macro, including baking oven 1, PVF sampling are designed to achieve the above object
Bag 2, pocket type method direct injected device input pipe 3, pocket type method direct injected device 4, gas-chromatography input pipe 5, gas chromatograph
6, mass spectrograph 7, smell and distinguish instrument input pipe 8, smell and distinguish instrument 9, smell recording device 10, PVF sampler bag 2, institute are provided in the baking oven 1
State PVF sampler bag 2 and be connected by interface with one end of pocket type method direct injected device input pipe 3, the pocket type method directly into
3 other end of sampling device input pipe connects the air inlet of pocket type method direct injected device 4, the pocket type method direct injected device 4
Gas outlet connects the import of gas chromatograph 6 by gas-chromatography input pipe 5, and the outlet of the gas chromatograph 6 passes through threeway
Valve is separately connected mass spectrograph 7, smells and distinguish instrument input pipe 8, and described smell distinguishes that the connection of 8 other end of instrument input pipe smells and distinguishes instrument 9, and the connection is smelt
Distinguish that instrument 9 passes through connection smell recording device 10.
Further, the top surface and side of the gas chromatograph 6 offer the chromatography being pierced by for chromatographic column both ends respectively
Column import and column outlet, the chromatographic column import are connected with gas-chromatography input pipe 5, and the column outlet connects threeway
Valve is coiled into the middle part of the chromatographic column coil-like.
Further, it is provided with gas direct injection port on the pocket type method direct injected device 4, the pocket type method is direct
Cold-trap device and carrier gas passage are equipped in sampling device 4, the gas direct injection port and pocket type method direct injected device input
Pipe 3 is connected, and the gas outlet of the cold-trap device is connected with gas-chromatography input pipe 5, through pocket type method direct injected device input pipe 3
The sample gas of input is passed through pocket type method direct injected device 4 by gas direct injection port and is enriched in cold-trap device, the sample
After gas is passed through, the sample air-blowing being enriched in cold-trap device is entered along carrier gas passage by gas-chromatography input pipe 5 by carrier gas.
The present invention also provides a kind of test methods of pocket type method direct injected GC-O/MS test macro, including following step
It is rapid: first the gas sample collection acquired will to be needed into PVF sampler bag 2, then PVF sampler bag 2 is straight by interface and pocket type method
It taps into sampling device 4 to be connected, sample gas is passed through pocket type method direct injected device 4 and is enriched in its cold-trap first, rises after the completion of enrichment
Temperature be desorbed and is passed through carrier gas from the opposite direction of sample introduction, and the substance of enrichment is blown into gas chromatograph 6 and is separated；Separation
After sample gas afterwards passes through triple valve, enter mass spectrograph 7 all the way and carry out qualitative and quantitative analysis, another way, which enters to smell, at the same time distinguishes instrument
9 are smelt with to carry out smell and distinguish.
Application of the test method of the present invention in the air quality and odor detection to vehicle interior.
Further, the step of present invention application at normal temperature tests vehicle are as follows: sample car is put into vehicle cabin,
Keeping temperature is 25.0 DEG C ± 1.0 DEG C, and relative humidity is 50% ± 10%, and it is quiet to open car door for ambient windstream speed≤0.3m/s
6h is set, standing terminates rear enclosed 16h, and the acquisition of interior gas is carried out with PVF sampler bag；The sample gas being collected is directly logical
Enter pocket type method direct injected device, then by gas after gas-chromatography separates, while entering mass spectrograph and smelling and distinguishing that instrument is determined
Property and manually smell and distinguish, finally obtain constituent information and its corresponding odor characteristics in sample gas.
Further, the step of present invention application at high temperature tests vehicle are as follows: sample car is put into vehicle cabin,
It opens and is stood under vehicle window room temperature for 24 hours, standing terminates rear enclosed sample car makes measurement point in 3h with 4 irradiation light irradiation vehicle bodies
65 DEG C ± 5 DEG C are warming up to, 4h carries out the acquisition of interior gas with PVF sampler bag；The sample gas being collected is passed directly into
Pocket type method direct injected device then by gas after gas-chromatography separates, while entering mass spectrograph and smelling and distinguishing that instrument progress is qualitative
And manually smell and distinguish, finally obtain constituent information and its corresponding odor characteristics in sample gas.
Compared with the existing technology, it is direct that pocket type method direct injected GC-O/MS test macro can be realized pocket type method to the present invention
Sample introduction, the method for the pocket type method direct injected have lacked the absorption and desorption process of a sampling pipe compared to adsorption tube mode, thus
Volatile materials loss can be reduced, is suitble to the analysis of complicated ingredient, is conducive to odoring substance and is smelling the capture and knowledge for debating port
Not.In addition, design of the present invention to sack additional heating device, can satisfy sample introduction side of the gas under condition of different temperatures
Formula.
[Detailed description of the invention]
Fig. 1 is the spectrogram of TDS and pocket type method sample introduction in 0-40min；
Fig. 2 is the spectrogram of TDS and pocket type method sample introduction in 0-10min；
Fig. 3 is system schematic of the invention；
In figure: 1, baking oven 2, PVF sampler bag 3, pocket type method direct injected device input pipe 4, pocket type method direct injected dress
5, gas-chromatography input pipe 6 is set, gas chromatograph 7, mass spectrograph 8, smells and distinguishes instrument input pipe 9, smells and distinguish instrument 10, smell record
Device.
[specific embodiment]
As shown in Fig. 3, the present invention provides a kind of pocket type method direct injected GC-O/MS test macro, including baking oven 1,
PVF sampler bag 2, pocket type method direct injected device input pipe 3, pocket type method direct injected device 4, gas-chromatography input pipe 5, gas phase
Chromatograph 6, mass spectrograph 7 are smelt and distinguish instrument input pipe 8, smell and distinguish instrument 9, smell recording device 10, are provided with PVF sampler bag 2 in baking oven 1,
PVF sampler bag 2 is connected by interface with one end of pocket type method direct injected device input pipe 3, pocket type method direct injected device
3 other end of input pipe connects the air inlet of pocket type method direct injected device 4, and the gas outlet of pocket type method direct injected device 4 passes through
Gas-chromatography input pipe 5 connects the import of gas chromatograph 6, and the outlet of gas chromatograph 6 is separately connected mass spectrum by triple valve
Instrument 7 is smelt and distinguishes instrument input pipe 8, smells and distinguishes that the connection of 8 other end of instrument input pipe smells and distinguishes instrument 9, and connection, which is smelt, distinguishes that instrument 9 passes through connection smell
Recording device 10.The top surface and side of gas chromatograph 6 offer the chromatographic column import being pierced by for chromatographic column both ends and color respectively
Column outlet is composed, chromatographic column import is connected with gas-chromatography input pipe 5, and column outlet connects triple valve, the middle part disk of chromatographic column
It is coiled into coil-like.
Wherein, pocket type method direct injected device 4 has the structures such as gas direct injection port, cold-trap device, carrier gas passage, adopts
The sample gas collected is passed directly into sampling device by injection port and is enriched in cold-trap, and sample gas will be rich by carrier gas after being passed through
Substance of the collection in cold-trap is blown into gas-chromatography and is separated.Specifically: it is straight that gas is provided on pocket type method direct injected device 4
Injection port is connect, is equipped with cold-trap device and carrier gas passage in pocket type method direct injected device 4, gas direct injection port and pocket type method are straight
It taps into sampling device input pipe 3 to be connected, the gas outlet of cold-trap device is connected with gas-chromatography input pipe 5, through pocket type method direct injected
The sample gas that device input pipe 3 inputs is passed through pocket type method direct injected device 4 by gas direct injection port and is enriched in cold-trap dress
In setting, after sample gas is passed through, it is defeated that the sample air-blowing being enriched in cold-trap device along carrier gas passage is entered by gas-chromatography by carrier gas
Enter pipe 5.
The test macro will partially be constituted by as follows: sampler bag, pocket type method direct injected device, gas chromatographic column, mass spectrum
Instrument is smelt and distinguishes instrument (sniffer), triple valve and connecting tube etc..Its test method are as follows: the gaseous sample for needing to acquire is collected first
Into PVF sampler bag, PVF sampler bag is connected by interface with pocket type method direct injected device, it is direct that sample gas is passed through pocket type method
Sampling device is simultaneously enriched in its cold-trap first, and heating be desorbed and is passed through load from the opposite direction of sample introduction after the completion of enrichment
The substance of enrichment is blown into GC and separated by gas.Sample gas after separation carries out qualitative, quantitative by after triple valve, entering MS all the way
Analysis, another way, which enters to smell, at the same time distinguishes instrument, is smelt and is distinguished by Odor Evaluations person's progress smell.Using the side of pocket type method direct injected
Method reduces the absorption and desorption process of a sampling pipe compared to adsorption tube sample mode, so as to reduce volatile materials damage
It loses, is suitble to the analysis of complicated ingredient, is conducive to the searching of odoring substance.
Below by way of comparative experiments, the invention will be further described:
1. standard liquid comparative experiments
2- butanone, methylene chloride, dimethyl disulfide, two sulphur of diallyl and butyl acetate standard liquid are chosen for testing
Substance uses pocket type method mark-on sample introduction of the present invention and Tenax pipe mark-on TDS two kinds of input modes of sample introduction, test result table respectively
5 kinds of substances more than bright (being shown in Table 1) are detected in using pocket type method direct injected, but are using Tenax pipe mark-on TDS sample introduction
When dimethyl disulfide, two sulphur of diallyl it is undetected.
The comparison of table 1, standard liquid test pocket type method sample introduction and TDS sample introduction
2. material sample comparative experiments
Selecting a kind of rubber weather strip is test object, and sample is put into PVF bag of 10L and distributes 2h at 65 DEG C, is distinguished
Use pocket type method direct injected of the present invention and the sampling of Tenax sampling pipe (sampling request is with reference to HJ/T400-2007 requirement) side TDS
Method sample introduction, from the comparison of the two compose entirely in it can be found that going out peak position and strong at retention time 10-40 minutes (see attached drawing 1)
It spends substantially coincident.
But the spectral peak peak type and intensity that two kinds of input modes obtain (see attached drawing 2) in retention time 0-10 minutes have very
Big difference.On the whole the number at pocket type method sample introduction either peak or the intensity at peak be better than Tenax pipe sample TDS mode into
Sample as a result, pocket type method sample introduction small molecule section have more significantly detection advantage.
Pocket type method direct injected GC-O/MS method of the present invention is traced to the source the application in rectification project in smell, Ji Keying
For the air quality and odor detection to vehicle interior.For example, air matter of certain automobile main frame maker to the vehicle interior of production
Amount and smell have strict requirements, are expected that by organic volatile (VOC) test and look for what its product was rectified and improved for smell and VOC
Thinking.The following are applications to be tested at normal temperature vehicle and using the experiment tested at high temperature vehicle.
(1) room temperature vehicle test experiments:
Sample car is put into vehicle cabin (25.0 DEG C ± 1.0 DEG C, 50% ± 10% relative humidity, ambient windstream speed≤
0.3m/s), it opens car door and stands 6h, standing terminates rear enclosed 16h, and the acquisition of interior gas is carried out with PVF bags.
The sample gas being collected is passed directly into pocket type method direct injected GC-O test macro.Gas is same after GC is separated
When enter MS and distinguish that instrument carries out qualitative and manually smells and distinguish, finally obtains constituent information and its corresponding smell in sample gas with smelling
Feature.It is as shown in table 2 below:
Table 2, room temperature pocket type method sample introduction test result
The following table 3 is to smell to distinguish that grade illustrates:
Table 3 is smelt and distinguishes grade explanation
| Oder levels/level | Description |
| 0 | Odorlessness |
| 1 | Slight smell needs to make great efforts to perceive |
| 2 | Clearly smell |
| 3 | Significant smell |
| 4 | Strong smell |
| 5 | Ferocious smell |
2- butanone is mostly come from from the peculiar smell that can be seen that pocket type sampling system sample detection under room temperature in result above
The alcohol stink of acid smell and n-butanol.
(2) high temperature vehicle test experiments:
Sample car is put into vehicle cabin, opens and is stood under vehicle window room temperature for 24 hours, standing terminates rear enclosed sample car, is irradiated with 4
Light irradiation vehicle body makes measurement point be warming up to 65 DEG C ± 5 DEG C in 3h, and 4h carries out the acquisition of interior gas with PVF bags.
The sample gas being collected is passed directly into pocket type method direct injected GC-O test macro.Gas is same after GC is separated
When enter MS and distinguish that instrument carries out qualitative and manually smells and distinguish, finally obtains constituent information and its corresponding smell in sample gas with smelling
Feature.It is as shown in table 4 below:
Table 4, high-temperature bag method sample introduction test result
The following table 5 is to smell to distinguish that grade illustrates:
Table 5 is smelt and distinguishes grade explanation
| Oder levels/level | Description |
| 0 | Odorlessness |
| 1 | Slight smell needs to make great efforts to perceive |
| 2 | Clearly smell |
| 3 | Significant smell |
| 4 | Strong smell |
| 5 | Ferocious smell |
From in result above as can be seen that high temperature under pocket type sampling system sample detection than having detected more objects under room temperature
Matter, the concentration for detecting substance mostly are also higher.Its peculiar smell mostlys come from the alcohol stink and benzene of the acid smell of 2- butanone, n-butanol
The smell of petrol and paint-like flavour of ethylene.
The present invention is simultaneously not limited to the embodiments described above, other any without departing from spiritual essence and principle of the invention
Changes, modifications, substitutions, combinations, simplifications made by lower, should be equivalent substitute mode, are included in protection model of the invention
Within enclosing.
Claims (7)
1. a kind of pocket type method direct injected GC-O/MS test macro, it is characterised in that: including baking oven (1), PVF sampler bag (2),
Pocket type method direct injected device input pipe (3), pocket type method direct injected device (4), gas-chromatography input pipe (5), gas-chromatography
Instrument (6), mass spectrograph (7) are smelt and distinguish instrument input pipe (8), smell and distinguish instrument (9), smell recording device (10), setting in the baking oven (1)
Have PVF sampler bag (2), the PVF sampler bag (2) passes through one end phase of interface and pocket type method direct injected device input pipe (3)
Connection, the air inlet of pocket type method direct injected device input pipe (3) other end connection pocket type method direct injected device (4),
The gas outlet of the pocket type method direct injected device (4) by gas-chromatography input pipe (5) connection gas chromatograph (6) into
Mouthful, the outlet of the gas chromatograph (6) is separately connected mass spectrograph (7) by triple valve, smells and distinguish instrument input pipe (8), described to smell
It distinguishes that the connection of instrument input pipe (8) other end is smelt to distinguish instrument (9), the connection, which is smelt, distinguishes that instrument (9) pass through connection smell recording device
(10)。
2. pocket type method direct injected GC-O/MS test macro as described in claim 1, it is characterised in that: the gas-chromatography
The top surface and side of instrument (6) offer the chromatographic column import being pierced by for chromatographic column both ends and column outlet, the chromatography respectively
Column import is connected with gas-chromatography input pipe (5), and the column outlet connects triple valve, is coiled into the middle part of the chromatographic column
It is coil-like.
3. pocket type method direct injected GC-O/MS test macro as claimed in claim 2, it is characterised in that: the pocket type method is straight
Tap on sampling device (4) and be provided with gas direct injection port, be equipped in the pocket type method direct injected device (4) cold-trap device and
Carrier gas passage, the gas direct injection port are connected with pocket type method direct injected device input pipe (3), and the cold-trap device goes out
Port is connected with gas-chromatography input pipe (5), and the sample gas through pocket type method direct injected device input pipe (3) input is straight by gas
It connects injection port to be passed through pocket type method direct injected device (4) and be enriched in cold-trap device, after the sample gas is passed through, passes through load
The sample air-blowing being enriched in cold-trap device is entered gas-chromatography input pipe (5) along carrier gas passage by gas.
4. a kind of test method of pocket type method direct injected GC-O/MS test macro as claimed in claim 1,2 or 3, special
Sign is, comprising the following steps: will first need the gas sample collection that acquires in PVF sampler bag (2), then by PVF sampler bag
(2) it is connected by interface with pocket type method direct injected device (4), sample gas is passed through pocket type method direct injected device (4) and exists first
It is enriched in its cold-trap, heating be desorbed and is passed through carrier gas from the opposite direction of sample introduction after the completion of enrichment, and the substance of enrichment is blown
Enter gas chromatograph (6) to be separated；Sample gas after separation by the way that it is qualitative fixed to enter mass spectrograph (7) progress after triple valve all the way
Amount analysis, another way enters to smell and distinguishes instrument (9) and smelt with to carry out smell and distinguish at the same time.
5. a kind of application of test method as claimed in claim 4 in the air quality and odor detection to vehicle interior.
6. application as claimed in claim 5, it is characterised in that: the step of testing at normal temperature vehicle are as follows: by sample car
It is put into vehicle cabin, keeping temperature is 25.0 DEG C ± 1.0 DEG C, and relative humidity is 50% ± 10%, ambient windstream speed≤0.3m/
S opens car door and stands 6h, and standing terminates rear enclosed 16h, and the acquisition of interior gas is carried out with PVF sampler bag；The sample that will be collected
Product gas is passed directly into pocket type method direct injected device, then by gas after gas-chromatography separates, while enter mass spectrograph with
It smells and distinguishes that instrument carries out qualitative and artificial smell and distinguishes, finally obtain constituent information and its corresponding odor characteristics in sample gas.
7. application as claimed in claim 5, it is characterised in that: the step of testing at high temperature vehicle are as follows: by sample car
It is put into vehicle cabin, opens and stood under vehicle window room temperature for 24 hours, standing terminates rear enclosed sample car is made with 4 irradiation light irradiation vehicle bodies
Measurement point is warming up to 65 DEG C ± 5 DEG C in 3h, and 4h carries out the acquisition of interior gas with PVF sampler bag；The sample that will be collected
Product gas is passed directly into pocket type method direct injected device, then by gas after gas-chromatography separates, while enter mass spectrograph with
It smells and distinguishes that instrument carries out qualitative and artificial smell and distinguishes, finally obtain constituent information and its corresponding odor characteristics in sample gas.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910891327.5A CN110531018A (en) | 2019-09-20 | 2019-09-20 | A kind of pocket type method direct injected GC-O/MS test macro and its test method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910891327.5A CN110531018A (en) | 2019-09-20 | 2019-09-20 | A kind of pocket type method direct injected GC-O/MS test macro and its test method |
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| CN110531018A true CN110531018A (en) | 2019-12-03 |
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| CN111087830A (en) * | 2020-01-09 | 2020-05-01 | 山东道恩高分子材料股份有限公司 | Research and analysis method for improving odor and VOC (volatile organic compounds) of automobile material |
| CN113588819A (en) * | 2021-07-27 | 2021-11-02 | 重庆长安汽车股份有限公司 | Quantitative evaluation method for odor of automobile interior part |
| CN114414703A (en) * | 2022-02-28 | 2022-04-29 | 海南红塔卷烟有限责任公司 | Essence component artificial smell device synchronous with instrument analysis and synchronization method |
| CN114487223A (en) * | 2022-01-19 | 2022-05-13 | 青岛科大新橡塑检测服务有限公司 | Method for measuring VOC content in EPS foam |
| CN115932115A (en) * | 2023-01-03 | 2023-04-07 | 中化泉州能源科技有限责任公司 | Method for analyzing identification of odor substances in polyolefin |
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Cited By (6)
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|---|---|---|---|---|
| CN111087830A (en) * | 2020-01-09 | 2020-05-01 | 山东道恩高分子材料股份有限公司 | Research and analysis method for improving odor and VOC (volatile organic compounds) of automobile material |
| CN113588819A (en) * | 2021-07-27 | 2021-11-02 | 重庆长安汽车股份有限公司 | Quantitative evaluation method for odor of automobile interior part |
| CN114487223A (en) * | 2022-01-19 | 2022-05-13 | 青岛科大新橡塑检测服务有限公司 | Method for measuring VOC content in EPS foam |
| CN114414703A (en) * | 2022-02-28 | 2022-04-29 | 海南红塔卷烟有限责任公司 | Essence component artificial smell device synchronous with instrument analysis and synchronization method |
| CN114414703B (en) * | 2022-02-28 | 2023-08-01 | 海南红塔卷烟有限责任公司 | Artificial smell device for essence components synchronous with instrument analysis and synchronization method |
| CN115932115A (en) * | 2023-01-03 | 2023-04-07 | 中化泉州能源科技有限责任公司 | Method for analyzing identification of odor substances in polyolefin |
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