CN203148908U - Gas bag-thermal desorption gas chromatography/mass spectrometry combined analyzing device system for analyzing all gas phase components in main stream smoke of cigarette - Google Patents
Gas bag-thermal desorption gas chromatography/mass spectrometry combined analyzing device system for analyzing all gas phase components in main stream smoke of cigarette Download PDFInfo
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- CN203148908U CN203148908U CN 201320124234 CN201320124234U CN203148908U CN 203148908 U CN203148908 U CN 203148908U CN 201320124234 CN201320124234 CN 201320124234 CN 201320124234 U CN201320124234 U CN 201320124234U CN 203148908 U CN203148908 U CN 203148908U
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Abstract
The utility model relates to a gas bag-thermal desorption gas chromatography / mass spectrometry combined analyzing device system for analyzing all gas phase components in main stream smoke of a cigarette. The system comprises a rotary disc smoking machine, a gas bag connected with the rotary disc smoking machine for collecting smoke, an injection pump, a thermal desorption instrument-gas chromatography/mass spectrometry combined instrument and an absorption sampling tube detachably connected with the gas bag, the injection pump and the thermal desorption instrument-gas chromatography/mass spectrometry combined instrument. The device system is applied to qualitative and quantitive analysis and detection of gas phase components in the smoke of the cigarette, and has the characteristics of simpleness and effectiveness. The system can analyze various gas phase components in the main stream smoke of the cigarette at the same time, so that the experimental repeatability is greatly improved, and the relative standard deviation of the objects to be detected in the large part of the all gas phase components is within 5%. The gas phase components in main stream smoke of the cigarette can be relatively completely captured. 67 components in the smoke of the cigarette can be identified qualitatively.
Description
Technical field
The utility model relates to a kind of for the sampling-analytical equipment to the full composition of cigarette mainstream flue gas gas phase, belongs to cigarette smoke analyzing and testing field.
Background technology
The analytical approach of the gas phase composition in the cigarette mainstream flue gas mainly contains at line spectrum, Mass Spectrometer Method method, cold solvent collecting method, absorption-thermal desorption method, sampler bag collecting method at present.Can carry out online, quick reaching by a mouthful analysis in line spectrum, Mass Spectrometer Method method, but these class methods only limit to conceptual phase at present, apply also to take day.Cold solvent collecting method composition changes little and reappearance is better relatively, and application report is more relatively, but troublesome poeration sensitivity is lower, only is suitable for the bigger volatile matter analyzing and testing of content.The sampler bag collecting method still has certain advantage, still has many people to adopt.In the sampler bag collecting method, partial fume directly can be imported GC, but sensitivity is lower, sample time, unsuitable strict control was unsuitable for batch quantity analysis.
This method is with airbag-thermal desorption-gas/matter coupling method combination, and the airbag method is collected, and absorption-thermal desorption method is carried out enrichment and detected.This technology has not only been expanded the analyst coverage of gas chromatography greatly, and has improved detection sensitivity (reaching the ng level).In case gas phase composition is adsorbed to Guan Zhonghou, can preserve at least more than the 24h, this just can make the operator after having captured the flue gas of all cigarette continuously, goes up the sample analysis more simultaneously, can increase work efficiency greatly.
The utility model content
The purpose of this utility model is to develop the device that can be used for the full composition of analysis of cigarette main flume gas phase in conjunction with the advantage of airbag sampling and thermal desorption technology, makes the more full composition of stability and high efficiency ground analyzing and testing cigarette mainstream flue gas gas phase of this device.
The utility model is achieved through the following technical solutions:
The airbag of the full composition of gas phase in a kind of analysis of cigarette main flume-thermal desorption gas/matter combined analysis device system, comprise that a rotating disk smoking machine, is connected in the airbag that the rotating disk smoking machine be used for to be collected flue gas, a syringe pump, thermal desorption instrument-gas chromatography instrument (ATD-GC/MS) and one with the detachable adsorption sampling pipe that is connected of described airbag, syringe pump and thermal desorption instrument-gas chromatography instrument.
Described rotating disk smoking machine is 20 duct rotating disk smoking machines, is preferably Borgwaldt200A type 20 duct rotating disk smoking machines.
Described airbag is the polyvinyl fluoride airbag, is preferably the Tedler airbag, can reduce the deposition of cigarette smoke on airbag; Described airbag links to each other with the gas outlet of rotating disk smoking machine by a sampling flexible pipe, is used for collecting the main flume of cigarette.
Described syringe pump is the LSP02-1B syringe pump.
The compound adsorption sampling pipe of described adsorption sampling Guan Weisan section Carbotrap300, two ends dispose the sealed copper cap, and described sealed copper cap is selected from Swagelok copper cap.
During sampling, described adsorption sampling Guan Yiduan inserts airbag, one end is tightly connected by silicone rubber tube and described syringe pump, by described syringe pump the cigarette smoke in the airbag is adsorbed onto in the adsorption sampling pipe, and is with the sealed copper cap that the adsorption sampling pipe is sealed at both ends after absorption is finished.
Described thermal desorption instrument is TurboMatrix ATD thermal desorption instrument; Described gas chromatography instrument adopts HP7890A gas chromatograph and the HP5975C mass spectrometer of coupling; Described thermal desorption instrument links to each other with the gas chromatography instrument by the transmission line of a heat tracing.
During detection, the cigarette smoke composition in the adsorption sampling pipe is by behind the thermal desorption instrument secondary desorption, transfers to the capillary column injection port of gas chromatography by the transmission line of described heat tracing, after gradient separations, enters mass spectrometer and detects.
With the airbag-thermal desorption gas/matter combined analysis device system applies of the full composition of gas phase in described a kind of analysis of cigarette main flume in the qualitative and quantitative analysis of the full composition of gas phase of cigarette smoke.
The airbag of the full composition of gas phase in described a kind of analysis of cigarette main flume-thermal desorption gas/matter combined analysis device System Utilization Procedure is: collect the cigarette smoke that the rotating disk smoking machine produces with airbag, then described adsorption sampling Guan Yiduan is inserted airbag, the other end is sealedly attached to described syringe pump by silicone rubber tube, by described syringe pump the cigarette smoke in the airbag is adsorbed onto in the adsorption sampling pipe, then the adsorption sampling pipe is sent into the thermal desorption instrument and carried out desorption and aging, use gas chromatography instrument analyzing and testing then.
Technique effect of the present utility model and advantage are:
(1) collect by airbag and the thermal desorption pipe captures sampling, can in time collect and preserve permanent advantage in conjunction with both, and make the operator continuous captured the flue gas of all cigarette after, go up the sample analysis more simultaneously, can increase work efficiency greatly
(2) sample time of syringe-type syringe pump, speed and volume height are controlled, the repeatability that can improve one's methods greatly.
(3) after the method that heats again by condensation of absorption-thermal desorption method/gas chromatography mass spectrometry is carried out the secondary desorption, transferred in the gas chromatograph by the transmission line of heat tracing, can reach highly enriched effect.
(4) gas circuit of used thermal desorption instrument is through redesign, no matter at which kind of state, outlet shunting gas purges the capillary column entrance always, reduces background signal greatly, for improving sensitivity and repeatability certain contribution is arranged also.
Description of drawings
The airbag of the full composition of gas phase in a kind of analysis of cigarette main flume of Fig. 1-thermal desorption gas/matter combined analysis device system
The separate colors spectrogram of Fig. 2 gas phase composition on the VOCOL analytical column
Reference numeral:
1. airbag; 2. flue gas injection port; 3. adsorption sampling pipe; 4. the sampling flexible pipe that connects airbag; 5. syringe; 6. syringe pump; 7. smoking machine; 8. cigarette props up clamper; 9. cigarette; 10. drip catcher (in cambridge filter is arranged); 11. pump unit; 12. the connecting tube to pump unit.
Embodiment
Below by specific instantiation explanation the technical solution of the utility model.Should understand these embodiment only is used for explanation the utility model and is not used in restriction scope of the present utility model.
Embodiment 1
The airbag of the full composition of gas phase in a kind of analysis of cigarette main flume-thermal desorption gas/matter combined analysis device system, comprise that a rotating disk smoking machine, is connected in the airbag that the rotating disk smoking machine be used for to be collected flue gas, a syringe pump, thermal desorption instrument-gas chromatography instrument and one with the detachable adsorption sampling pipe that is connected of described airbag, syringe pump and thermal desorption instrument-gas chromatography instrument.
Described rotating disk smoking machine is Borgwaldt200A type 20 duct rotating disk smoking machines.
Described airbag is the Tedler airbag, can reduce the deposition of cigarette smoke on airbag; Described airbag links to each other with the gas outlet of rotating disk smoking machine by a sampling flexible pipe, is used for collecting the main flume of cigarette.
Described syringe pump is the LSP02-1B syringe pump.
The compound adsorption sampling pipe of described adsorption sampling Guan Weisan section Carbotrap300, two ends dispose the sealed copper cap, and described sealed copper cap is selected from Swagelok copper cap.
During sampling, described adsorption sampling Guan Yiduan inserts airbag, one end is sealedly attached on the conehead of the syringe front end on the described LSP02-1B syringe pump by silicone rubber tube, by described syringe the cigarette smoke in the airbag is adsorbed onto in the adsorption sampling pipe, with the sealed copper cap that the adsorption sampling pipe is sealed at both ends after absorption is finished.
Described thermal desorption instrument is TurboMatrix ATD thermal desorption instrument; Described gas chromatography instrument adopts HP7890A gas chromatograph and the HP5975C mass spectrometer of coupling; Described thermal desorption instrument links to each other with the gas chromatography instrument by the transmission line of a heat tracing.
Cigarette smoke in the adsorption sampling pipe is by behind the thermal desorption instrument secondary desorption, transfers to the capillary column injection port of gas chromatography by the transmission line of heat tracing, after gradient separations, enters mass spectrometer and detects.
Airbag-thermal desorption gas/matter combined analysis device systematic analysis with the full composition of gas phase in the described analysis of cigarette main flume detects the qualitative analysis of certain commercial Virginian-type cigarette flue gas gas phase composition, and method step is:
(1) produces flue gas
At 22 ℃ ± 2 ℃, preheating 20min adjusts wind speed and the suction capacity of smoking machine with Borgwaldt200A type 20 duct rotating disk smoking machines, and the cigarette smoking mode is undertaken by iso standard.The wind speed 20cm/s of smoking machine; The suction capacity is 35mL, and suction time is 2s/puff, and be 58s every mouthful of interval time, collects the flue gas of 20 cigarette with the Tedler airbag.
(2) shift flue gas
Collected the flue gas of 20 cigarette with the Tedler airbag, behind the 2min, (the syringe pump range is 140mm, stroke resolution: 0.156 μ m, linear velocity scope: 5 μ m/min-130mm/min with the LSP02-1B syringe pump; 60mL/min) shift the 60mL flue gas and go into Carbontrap300 adsorption sampling pipe, after transfer finishes adsorption sampling pipe two ends are sealed with Swagelok copper cap, to be measured.
(3) smoke components detects
Adopt TurboMatrix ATD thermal desorption instrument that the adsorption sampling pipe is carried out desorption and aging, carry out flue gas analysis with HP7890A gas chromatograph and the coupling of HP5975C mass spectrometer then, the thermal desorption instrument links to each other with the gas chromatography instrument by the transmission line of a heat tracing; Desorption and the aging condition of adsorption sampling pipe on the thermal desorption instrument, the gas chromatography/mass spectrometry parameter arranges as follows:
Desorption conditions: He, 10.0psi; Valve: 200 ℃; Pre-blowing: 1min; The one-level desorption: 280 ℃ of temperature, 30min, desorption flow 40mL/min, import shunting 40mL/min, Tenax TA (60～80 order) adsorbent remains on-30 ℃ of following enrichments; The secondary desorption: 280 ℃ of temperature, keep 2min, 30mL/min is shunted in outlet; Transmission line temperature: 210 ℃.
Aging condition: He:10.0psi, valve: 220 ℃, pre-blowing: 1min, aging temperature: 300 ℃, digestion time: 30min, carrier gas flux: 40mL/min, import shunting: 40mL/min.
Gas chromatography-mass spectrum condition: Supelco VOCOL capillary column, 60m*0.32mm*1.8um; Temperature programme: 35 ℃ (10min), 3.5 ℃/min rise to 180 ℃, and 10 ℃/min rises to 210 ℃ (5min), gas chromatography and mass spectrometer transmission interface temperature: 230 ℃; Mass spectrometer detection mode: SCAN, sweep limit 10amu～300amu.
(4) qualitative analysis
The testing result spectrogram uses the Willey7n.1 storehouse to carry out the mass spectrum retrieval, identifies 67 kinds of chemical substances, sees shown in Fig. 2 and the table 1.
The full constituent analysis result of certain commercial Virginian-type cigarette flue gas gas phase of table 1
Embodiment 2
Present embodiment apparatus system and analytic process parameter arrange with embodiment 1, part gas phase composition 1 to the 2R4F standard cigarettes, the qualitative and quantitative analysis of 3-butadiene, iso pentane two floride, vinyl cyanide, benzene, toluene, styrene, acetone, crotonaldehyde etc., and compare with bibliographical information:
1, preparation standard working curve
When measuring in the mainstream smoke gas phase object the tested component of part with inner mark method ration, internal standard compound matter selects for use deuterium for benzene, joins the methanol solution of tested component and internal standard compound matter as work mother liquid concentration (the 5th grade of mark liquid sees Table 2); All the other mark liquid at different levels carry out stepwise dilution with methyl alcohol and obtain.The relative scale of measured matter concentration in mark liquid at different levels is in every grade of mark liquid: (1): (2): (3): (4): (5)=0.05:0.1:0.2:0.5:1.Every grade of interior scalar sum work mother liquor of marking in the liquid is identical.
Each amount of substance in the table 21 μ L work mother liquor
| Chemical substance | Content among the 1 μ L (μ g) |
| 1,3-butadiene | 7.2 |
| Iso pentane two floride | 172.6 |
| Vinyl cyanide | 8.1 |
| Benzene | 17.6 |
| Toluene | 34.6 |
| Styrene | 2.3 |
| Acetone | 80.0 |
| Crotonaldehyde | 8.6 |
| Two butanone | 32.4 |
| Butyraldehyde | 16.0 |
| Acetonitrile | 39.5 |
| The two methylfurans of 2,5- | 9.0 |
| Ethylbenzene | 4.3 |
| Deuterium is for benzene (interior mark) | 19.0 |
The adsorption sampling pipe is inserted gas chromatograph packed column injection port, utilize automatic sampler that 1-5 level mark liquid is introduced in the adsorption sampling pipe; Instrument parameter: He, constant current: 100mL/min, 20min, sample size: 1.0 μ L, injector temperature: 150 ℃, furnace temperature: 30 ℃.Utilize thermal desorption instrument-gas chromatograph/mass spectrometer coupling method to measure the response of each standard substance, set up the work song; The operating parameter of thermal desorption instrument and gas chromatography instrument arranges with embodiment 1.
Working curve checking situation sees Table 3:
Table 3 standard working curve checking situation
2, to the testing process of 2R4F standard cigarettes smoke components with embodiment 1.
3, quantitative test
Press computing formula:
Calculate the content that the gas phase in every cigarette mainstream flue gas is divided into;
Wherein, As: the chromatographic peak area of test substance; AIS: interior target chromatographic peak area; RF: the response factor of standard specimen; N: puff number; C: conversion factor,
The suction capacity is 35mL/min, the cigarette number is 20, sampling volume is 60mL, analysis result is as shown in table 4: wherein except cinnamic result is slightly on the low side, the analysis result of all the other each materials all drops in the coverage of 2R4F, and and the content mean bias of 2R4F is all in 20%, and wherein the result of iso pentane two floride and acetone and the content mean bias among the 2R4F are in 5%; And cinnamic result is less than normal, mainly is because it is two-phase in main flume distributes, and the analysis result of this paper is just at gas phase composition.In different cigarette smokes, cinnamic two-phase allocation proportion is calculated in this ratio approximately between 0.181～0.455, and cinnamic measurement result is just similar in appearance to the report result of 2R4F.The analysis result that shows apparatus of the present invention system still is reliable.
Part main flume gas phase composition analysis result in table 4 cigarette sample
Claims (6)
1. airbag-thermal desorption gas/matter combined analysis device the system of the full composition of gas phase in the analysis of cigarette main flume, comprise that a rotating disk smoking machine, is connected in the airbag that the rotating disk smoking machine be used for to be collected flue gas, a syringe pump, thermal desorption instrument-gas chromatography instrument and one with the detachable adsorption sampling pipe that is connected of airbag, syringe pump and thermal desorption instrument-gas chromatography instrument.
2. apparatus system as claimed in claim 1 is characterized in that, described rotating disk smoking machine is 20 duct rotating disk smoking machines.
3. apparatus system as claimed in claim 1 is characterized in that, described airbag is the polyvinyl fluoride airbag, and described airbag links to each other with the gas outlet of rotating disk smoking machine by a sampling flexible pipe.
4. apparatus system as claimed in claim 1 is characterized in that, described syringe pump is the LSP02-1B syringe pump.
5. apparatus system as claimed in claim 1 is characterized in that, the compound adsorption sampling pipe of described adsorption sampling Guan Weisan section Carbotrap300, and two ends dispose the sealed copper cap, and described sealed copper cap is selected from Swagelok copper cap.
6. apparatus system as claimed in claim 1 is characterized in that, described thermal desorption instrument is TurboMatrix ATD thermal desorption instrument; Described gas chromatography instrument adopts HP7890A gas chromatograph and the HP5975C mass spectrometer of coupling; Described thermal desorption instrument links to each other with the gas chromatography instrument by the transmission line of a heat tracing.
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| CN 201320124234 CN203148908U (en) | 2013-03-18 | 2013-03-18 | Gas bag-thermal desorption gas chromatography/mass spectrometry combined analyzing device system for analyzing all gas phase components in main stream smoke of cigarette |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104614464A (en) * | 2015-02-11 | 2015-05-13 | 安徽中烟工业有限责任公司 | Device for measuring oral cavity residual efficiency of gas-phase chemical components of main stream smoke of cigarette |
| CN106680405A (en) * | 2016-12-26 | 2017-05-17 | 无锡市环境监测中心站 | Fully automatic air bag type sample feeding heat desorption analysis gas chromatography mass spectrometry method |
| CN109164135A (en) * | 2018-08-22 | 2019-01-08 | 青岛颐中科技有限公司 | Electric heating low temperature cigarette comprehensive analysis experimental provision |
-
2013
- 2013-03-18 CN CN 201320124234 patent/CN203148908U/en not_active Expired - Lifetime
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104614464A (en) * | 2015-02-11 | 2015-05-13 | 安徽中烟工业有限责任公司 | Device for measuring oral cavity residual efficiency of gas-phase chemical components of main stream smoke of cigarette |
| CN104614464B (en) * | 2015-02-11 | 2016-06-01 | 安徽中烟工业有限责任公司 | The measuring apparatus of a kind of gaseous phase of main stream smoke of cigarette chemical composition oral cavity residual efficiency |
| CN106680405A (en) * | 2016-12-26 | 2017-05-17 | 无锡市环境监测中心站 | Fully automatic air bag type sample feeding heat desorption analysis gas chromatography mass spectrometry method |
| CN109164135A (en) * | 2018-08-22 | 2019-01-08 | 青岛颐中科技有限公司 | Electric heating low temperature cigarette comprehensive analysis experimental provision |
| CN109164135B (en) * | 2018-08-22 | 2021-11-16 | 青岛颐中科技有限公司 | Electric heating low-temperature cigarette comprehensive analysis experimental device |
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