CN210803382U - Bag type direct sample introduction GC-O/MS test system - Google Patents
Bag type direct sample introduction GC-O/MS test system Download PDFInfo
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- CN210803382U CN210803382U CN201921569076.0U CN201921569076U CN210803382U CN 210803382 U CN210803382 U CN 210803382U CN 201921569076 U CN201921569076 U CN 201921569076U CN 210803382 U CN210803382 U CN 210803382U
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Abstract
The utility model relates to a pocket type method direct sampling GC-O/MS test system, this test system includes the oven, PVF sampling bag, the direct sampling device of pocket type method, gas chromatograph, the mass spectrograph, smell and distinguish the appearance, be provided with PVF sampling bag in the oven, PVF sampling bag is connected with the one end of the direct sampling device input tube of pocket type method through the interface, the direct sampling device input tube other end of pocket type method connects the air inlet of the direct sampling device of pocket type method, the gas outlet of the direct sampling device of pocket type method passes through the import of gas chromatography input tube connection gas chromatograph, gas chromatograph's export passes through the three-way valve and connects the mass spectrograph respectively, smell and distinguish the appearance input tube, smell and distinguish the appearance other end connection, the connection is smelled and is distinguished the appearance and pass through line connection smell recorder; the utility model discloses can realize that the pocket type method directly advances kind, reducible volatile substances loss is fit for the analysis of complex composition, is favorable to the smell material to be in the seizure and the discernment of distinguishing the port smelling.
Description
[ technical field ]
The utility model belongs to the technical field of gas chromatography-mass spectrometry allies oneself with technique and specifically relates to a pocket type method directly advances appearance GC-O/MS test system.
[ background art ]
The GC-O/MS technology formed by combining the gas chromatography-mass spectrometry (GC-MS) with the gas chromatography olfaction measurement method (GC-O) not only can qualitatively and quantitatively determine trace organic volatile substances (VOC) but also can combine sensory analysis, has high sensitivity and high selectivity, is combined with odor analysis caused by the volatile substances, and is commonly used for analyzing flavor substances in food and aroma substances in tobacco leaves. The most widely used forward mode of gas chromatographic analysis is a Thermal Desorption (TDS) sampling means, volatile substances emitted by a sample are trapped by using adsorption tubes such as TENAX or activated carbon, the substances in the sampling tube are thermally desorbed and enriched in a cold trap through the TDS, then the substances are conveyed into a Gas Chromatograph (GC) through carrier gas for separation, and the separated gas simultaneously enters a Mass Spectrum (MS) and a sniffer (sniffer) for qualitative and quantitative determination and odor identification. TDS sampling is mature at present, but is limited by adsorption packing of an adsorption tube, and some substances are lost in the adsorption and desorption processes; when the humidity of the objective environment is high, the column is damaged due to the fact that the water content of the sample is too large, and objective problems such as data result distortion are caused.
[ contents of utility model ]
The utility model aims at solving foretell not enough and providing a pocket type method and directly advancing kind GC-O MS test system, can realize that the pocket type method directly advances kind to reducible volatile substance loss is fit for the analysis of complex composition, is favorable to the smell material to be in the seizure and the discernment of distinguishing the port.
In order to realize the purpose, the bag-type direct sample introduction GC-O/MS testing system comprises an oven 1, a PVF sampling bag 2, a bag-type direct sample introduction device input tube 3, a bag-type direct sample introduction device 4, a gas chromatography input tube 5, a gas chromatograph 6, a mass spectrometer 7, a sniffing instrument input tube 8, a sniffing instrument 9 and a smell recording device 10, wherein the oven 1 is internally provided with the PVF sampling bag 2, the PVF sampling bag 2 is connected with one end of the bag-type direct sample introduction device input tube 3 through an interface, the other end of the bag-type direct sample introduction device input tube 3 is connected with an air inlet of the bag-type direct sample introduction device 4, an air outlet of the bag-type direct sample introduction device 4 is connected with an inlet of the gas chromatograph 6 through the gas chromatography input tube 5, an outlet of the gas chromatograph 6 is respectively connected with the mass spectrometer 7 and the sniffing instrument input tube 8 through a three-way valve, the other end of the sniffing instrument input tube 8 is connected with a sniffing instrument 9, and the connection sniffing instrument 9 is connected with a smell recording device 10 through a line.
Further, a chromatographic column inlet and a chromatographic column outlet for two ends of the chromatographic column to penetrate out are respectively formed in the top surface and the side surface of the gas chromatograph 6, the chromatographic column inlet is connected with the gas chromatograph input pipe 5, the chromatographic column outlet is connected with the three-way valve, and the middle part of the chromatographic column is coiled into a coiled pipe shape.
Further, be provided with gaseous direct sample inlet on the direct sampling device 4 of pocket type method, be equipped with cold trap device and carrier gas passageway in the direct sampling device 4 of pocket type method, gaseous direct sample inlet links to each other with the direct sampling device input tube 3 of pocket type method, the gas outlet of cold trap device links to each other with gas chromatography input tube 5, and the direct sampling device 4 of pocket type method and enrichment are in cold trap device through gaseous direct sample inlet to the sample gas of the direct sampling device input tube 3 input of pocket type method, after the sample gas lets in, blows in gas chromatography input tube 5 with the sample gas of enrichment in cold trap device along carrier gas passageway through the carrier gas.
Compared with the prior art, the utility model, pocket type method directly advances a kind GC-O MS test system and can realize that pocket type method directly advances a kind, and this pocket type method directly advances a kind method and compares the adsorption and desorption process that the adsorption tube mode has once lacked the sampling tube to can reduce volatile substances loss, be fit for the analysis of complex composition, be favorable to the smell material in the seizure and the discernment of distinguishing the port of smelling. Furthermore, the utility model discloses to sack additional heating device's design, can satisfy gaseous appearance mode of advancing under different temperature conditions.
[ description of the drawings ]
FIG. 1 is a spectrum of TDS and bag-based injection at 0-40 min;
FIG. 2 is a spectrum of TDS and bag-based injection at 0-10 min;
fig. 3 is a schematic diagram of the system of the present invention;
in the figure: 1. oven 2, PVF sampling bag 3, pocket type method direct sample introduction device input tube 4, pocket type method direct sample introduction device 5, gas chromatography input tube 6, gas chromatograph 7, mass spectrometer 8, smell distinguish appearance input tube 9, smell distinguish appearance 10, smell recorder.
[ detailed description of the invention ]
As shown in the attached figure 3, the utility model provides a GC-O/MS test system with direct bag-type sampling, which comprises an oven 1, a PVF sampling bag 2, a bag-type direct sampling device input tube 3, a bag-type direct sampling device 4, a gas chromatography input tube 5, a gas chromatograph 6, a mass spectrometer 7, an olfactory discrimination instrument input tube 8, an olfactory discrimination instrument 9 and an odor recording device 10, wherein the oven 1 is internally provided with the PVF sampling bag 2, the PVF sampling bag 2 is connected with one end of the bag-type direct sampling device input tube 3 through an interface, the other end of the bag-type direct sampling device input tube 3 is connected with an air inlet of the bag-type direct sampling device 4, an air outlet of the bag-type direct sampling device 4 is connected with an inlet of the gas chromatograph 6 through the gas chromatography input tube 5, an outlet of the gas chromatograph 6 is respectively connected with the mass spectrometer 7 and the olfactory discrimination instrument input tube 8 through a three-way valve, the other end of the input tube 8 of the sniffing instrument is connected with the sniffing instrument 9, and the sniffing instrument 9 is connected with the odor recording device 10 through a line. The top surface and the side surface of the gas chromatograph 6 are respectively provided with a chromatographic column inlet and a chromatographic column outlet for two ends of a chromatographic column to penetrate out, the chromatographic column inlet is connected with the gas chromatography input pipe 5, the chromatographic column outlet is connected with a three-way valve, and the middle part of the chromatographic column is coiled into a coil shape.
The direct bag-type sample introduction device 4 has a direct gas introduction port, a cold trap device, a carrier gas channel and other structures, collected sample gas is directly introduced into the sample introduction device through the gas introduction port and is enriched in the cold trap, and substances enriched in the cold trap are blown into the gas chromatography through the carrier gas for separation after the introduction of the sample gas is finished. The method specifically comprises the following steps: the direct bag-type sample introduction device 4 is provided with a direct gas injection port, the direct bag-type sample introduction device 4 is internally provided with a cold trap device and a carrier gas channel, the direct gas injection port is connected with the input pipe 3 of the direct bag-type sample introduction device, the gas outlet of the cold trap device is connected with the gas chromatography input pipe 5, sample gas input through the input pipe 3 of the direct bag-type sample introduction device is introduced into the direct bag-type sample introduction device 4 through the direct gas injection port and is enriched in the cold trap device, and after introduction of the sample gas is finished, the sample gas enriched in the cold trap device is blown into the gas chromatography input pipe 5 through the carrier gas along the carrier gas channel.
The test system is composed of the following parts: a sampling bag, a bag-type direct sample introduction device, a gas chromatographic column, a mass spectrometer, an olfactory analyzer (sniffer), a three-way valve, a connecting pipe and the like. The test method comprises the following steps: the method comprises the steps of collecting a gas sample to be collected into a PVF sampling bag, connecting the PVF sampling bag with a bag-type direct sampling device through an interface, introducing the sample gas into the bag-type direct sampling device, enriching the sample gas in a cold trap of the bag-type direct sampling device, heating the bag-type direct sampling device after the enrichment is finished, desorbing the sample gas, introducing carrier gas from the direction opposite to the sampling direction, and blowing the enriched substance into a GC for separation. After the separated sample gas passes through a three-way valve, one path of the sample gas enters an MS for qualitative and quantitative analysis, and the other path of the sample gas enters an odor identification instrument for odor identification by an odor evaluator. Compared with an adsorption tube sampling mode, the method adopting the bag type method for direct sample introduction reduces the adsorption and desorption processes of a sampling tube, thereby reducing the loss of volatile substances, being suitable for the analysis of complex components and being beneficial to the search of odor substances.
The above test method is further illustrated by comparative experiments as follows:
1. comparative experiment of standard solution
Will 2-butanone, dichloromethane, dimethyl disulfide, dipropenyl disulfide and butyl acetate mark liquid and be selected as the test material, use respectively the utility model discloses pocket method adds mark and advances kind and Tenax pipe adds two kinds of appearance modes of advancing of mark TDS appearance, and the test result shows (see table 1) above 5 kinds of materials all are detected in using the pocket type method to directly advance kind, nevertheless dimethyl disulfide, dipropenyl disulfide are not detected when using Tenax pipe to add mark TDS to advance kind.
TABLE 1 comparison of bag-based and TDS samples for standard solution testing
2. Comparative experiment of Material sample
A rubber sealing strip is selected as a test object, a sample is placed into a 10L PVF bag and is diffused for 2h at 65 ℃, the bag type direct sample introduction and Tenax sampling tube sampling (the sampling requirement refers to the requirements of HJ/T400-plus 2007) TDS method sample introduction are respectively used, and the peak emergence position and the intensity in the retention time of 10-40 minutes (see attached figure 1) are basically consistent from the comparison full spectrum of the two.
However, the peak patterns and intensities of the two samples are greatly different within the retention time of 0-10 minutes (see figure 2). The whole bag-type sampling method has the advantages that the sampling result of the TDS sampling method of sampling by the Tenax tube is superior to the sampling result of sampling by the bag-type sampling method in both the number and the intensity of peaks, and the bag-type sampling method has more obvious detection advantages in small molecular segments.
The bag-type method is applied to the odor tracing and modifying project by directly feeding a GC-O/MS method, and can be applied to the detection of the air quality and odor in the vehicle. For example, a certain automobile main engine plant has strict requirements on the quality and smell of air inside a produced vehicle, and it is expected to find out the idea of modifying the smell and Volatile Organic Compounds (VOC) of the product through VOC tests. The following are experiments applied to test the whole vehicle at normal temperature and at high temperature.
The test experiment of the whole vehicle at normal temperature comprises the following steps:
placing the sample car into the whole car cabin (25.0 +/-1.0 ℃, 50% +/-10% relative humidity, and ambient air flow rate less than or equal to 0.3m/s), opening the car door, standing for 6h, sealing for 16h after standing, and collecting the gas in the car by using a PVF bag.
And directly introducing the collected sample gas into a bag-type direct sample introduction GC-O test system. And (3) after the gas is subjected to GC separation, simultaneously entering an MS and a smell identification instrument for qualitative and manual smell identification, and finally obtaining component information in the sample gas and corresponding smell characteristics. As shown in table 2 below:
TABLE 2 results of normal temperature bag-type sample injection
Table 3 below is a description of olfactory ratings:
TABLE 3 olfactory discrimination Scale
From the above results, it can be seen that the odor detected by the bag-type sample injection method at normal temperature mainly comes from the acid odor of 2-butanone and the alcohol odor of n-butanol.
(II) high-temperature finished automobile test experiment:
and (3) placing the sample car into the whole car cabin, opening the car window, standing for 24 hours at normal temperature, sealing the sample car after standing, irradiating the car body by using 4 irradiation lamps, heating the measuring point to 65 +/-5 ℃ within 3 hours, and collecting the gas in the car by using a PVF bag in the 4 th hour.
And directly introducing the collected sample gas into a bag-type direct sample introduction GC-O test system. And (3) after the gas is subjected to GC separation, simultaneously entering an MS and a smell identification instrument for qualitative and manual smell identification, and finally obtaining component information in the sample gas and corresponding smell characteristics. As shown in table 4 below:
TABLE 4 high temperature bag method sample introduction test results
Table 5 below is a description of olfactory ratings:
TABLE 5 olfactory discrimination Scale
| Odor level/level | Description of the |
| 0 | Has no odor |
| 1 | Slight smell, requiring an effort to perceive |
| 2 | |
| 3 | Significant odor |
| 4 | |
| 5 | Very strong odor |
From the above results, it can be seen that more substances are detected at high temperature by the bag-type sample injection method than at normal temperature, and the concentration of most of the detected substances is also higher. The odor mainly comes from the acid odor of 2-butanone, the alcohol odor of n-butanol, and the gasoline odor and paint odor of styrene.
The present invention is not limited by the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be equivalent replacement modes, and are all included in the protection scope of the present invention.
Claims (3)
1. A GC-O/MS test system for direct sample introduction by a bag method is characterized in that: including oven (1), PVF sampling bag (2), the direct sampling device input tube of pocket type method (3), the direct sampling device of pocket type method (4), gas chromatography input tube (5), gas chromatograph (6), mass spectrograph (7), distinguish appearance input tube (8), distinguish appearance (9), smell recorder (10) smelly, be provided with PVF sampling bag (2) in oven (1), PVF sampling bag (2) is connected through the interface and the one end of the direct sampling device input tube of pocket type method (3), the air inlet of the direct sampling device of pocket type method (4) is connected to the direct sampling device of pocket type method input tube (3) other end, the import of gas chromatograph (6) is connected through gas chromatography input tube (5) in the gas outlet of the direct sampling device of pocket type method (4), the export of gas chromatograph (6) is connected mass spectrograph (7) respectively through the three-way valve, Sniff appearance input tube (8), sniff appearance input tube (8) other end connection and sniff appearance (9), connect and sniff appearance (9) and pass through line connection smell recorder (10).
2. The bag-on-bag direct-injection GC-O/MS test system according to claim 1, wherein: the top surface and the side surface of the gas chromatograph (6) are respectively provided with a chromatographic column inlet and a chromatographic column outlet which are used for penetrating out of two ends of the chromatographic column, the chromatographic column inlet is connected with the gas chromatograph input pipe (5), the chromatographic column outlet is connected with a three-way valve, and the middle part of the chromatographic column is coiled into a coiled pipe shape.
3. The bag-type direct-injection GC-O/MS test system according to claim 2, wherein: be provided with gaseous direct introduction port on the direct sampling device of pocket type method (4), be equipped with cold trap device and carrier gas passageway in the direct sampling device of pocket type method (4), gaseous direct introduction port links to each other with the direct sampling device input tube of pocket type method (3), the gas outlet and the gas chromatography input tube of cold trap device (5) link to each other, and the sample gas of the direct sampling device input tube of pocket type method (3) input lets in the direct sampling device of pocket type method (4) and enrichment in the cold trap device through gaseous direct introduction port, after the sample gas lets in, blows in gas chromatography input tube (5) along the carrier gas passageway with the sample gas of enrichment in the cold trap device through the carrier gas.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110531018A (en) * | 2019-09-20 | 2019-12-03 | 通标标准技术服务(上海)有限公司 | A kind of pocket type method direct injected GC-O/MS test macro and its test method |
| CN114062550A (en) * | 2021-11-16 | 2022-02-18 | 西南石油大学 | Natural gas all-component analysis device and method |
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2019
- 2019-09-20 CN CN201921569076.0U patent/CN210803382U/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110531018A (en) * | 2019-09-20 | 2019-12-03 | 通标标准技术服务(上海)有限公司 | A kind of pocket type method direct injected GC-O/MS test macro and its test method |
| CN114062550A (en) * | 2021-11-16 | 2022-02-18 | 西南石油大学 | Natural gas all-component analysis device and method |
| CN114062550B (en) * | 2021-11-16 | 2024-02-02 | 西南石油大学 | Natural gas full-component analysis device and method |
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