CN103226139B - Process for analyzing gas-phase total components in cigarette mainstream smoke through airbag-thermal desorption-gas chromatography/mass spectrometry method - Google Patents

Process for analyzing gas-phase total components in cigarette mainstream smoke through airbag-thermal desorption-gas chromatography/mass spectrometry method Download PDF

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CN103226139B
CN103226139B CN201310086878.7A CN201310086878A CN103226139B CN 103226139 B CN103226139 B CN 103226139B CN 201310086878 A CN201310086878 A CN 201310086878A CN 103226139 B CN103226139 B CN 103226139B
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airbag
gas
standard specimen
thermal desorption
sampling pipe
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CN103226139A (en
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郑赛晶
陈敏
刘百战
王磊君
张怡春
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Shanghai Tobacco Group Co Ltd
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Shanghai Tobacco Group Co Ltd
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Abstract

The invention relates to a process for analyzing gas-phase total components in a cigarette mainstream smoke through an airbag-thermal desorption-gas chromatography/mass spectrometry method. The process allows an airbag, an adsorption sampling tube, a syringe pump and a thermal desorber-gas chromatograph/mass spectrometer, utilizes the airbag to collect a cigarette mainstream smoke, allows the smoke in the airbag to be adsorbed to the adsorption sampling tube through the syringe pump, and utilizes the thermal desorber-gas chromatograph/mass spectrometer to desorb, age, detect and qualitatively and quantitatively analyze, so the advantages of each of above instruments are used, the repeatability is improved, the relative standard deviations of most measured substances in the gas-phase full components are below 5%, and the repeatability is substantially better than the previously-reported repeatability.

Description

The method of the full composition of gas phase in a kind of airbag-thermal desorption-gas/matter coupling method analysis of cigarette main flume
Technical field
The present invention relates to the method for the full composition of gas phase in a kind of airbag-thermal desorption-gas/matter coupling method analysis of cigarette main flume, belong to components in cigarette smoke gas phase composition detection analysis technical field.
Background technology
Cigarette smoke is the most complicated system of known composition, and the chemical composition identified from cigarette smoke at present, more than 5000 kinds, exists with gas, grain two-phase.According to research report both domestic and external, selective harm reduction technical difficulty for grain phase constituent is very large, and gas phase composition is through filter tip, because rate of propagation is very fast, have an opportunity to be adsorbed by the harm reduction material selectivity of filter tip, thus the emphasis of selective harm reduction should be placed on gas phase composition, but the reappearance of most of gas phase analysis method and sensitivity are all little desirable.In order to harm reduction material correctly can be evaluated, function is reduced to the selectivity of cigarette mainstream flue gas, be necessary very much the research test job of the full composition of gas phase carried out in cigarette mainstream flue gas.
The full composition of gas phase in application airbag-thermal desorption-gas/matter coupling method analysis of cigarette main flume, combine the advantage of airbag sampling and thermal desorption technology, first Tedler airbag is adopted to collect the main flume of 20 cigarette, and quantitatively shift certain volume flue gas with syringe-type syringe pump first and enter Carbotrap300 adsorption sampling pipe, recycling thermal desorption technology-gas/matter combined instrument (ATD-GC/MS) method carries out the qualitative and part of compounds quantitative test of the full composition of gas phase in cigarette mainstream flue gas.Because sample time of syringe-type syringe pump, speed and volume height are controlled and very accurate, considerably improve repeatability, in the full composition of gas phase, the relative standard deviation of most of measured object is all below 5%, and repeatability is significantly better than report in the past.
Summary of the invention
The object of the invention is to overcome above shortcoming, the method of the full composition of gas phase in a kind of airbag-thermal desorption-gas/matter coupling method analysis of cigarette main flume is provided, the method is by effectively combining airbag, syringe pump and thermal desorption instrument-Gc/ms Analyser, learn from other's strong points to offset one's weaknesses, considerably improve repeatability, in the full composition of gas phase, the relative standard deviation of most of measured object is all below 5%, and repeatability is significantly better than report in the past.
The present invention is achieved by the following technical solutions:
A method for the full composition of gas phase in airbag-thermal desorption-gas/matter coupling method analysis of cigarette main flume, comprises the following steps:
(1) airbag is connected on smoking machine, gathers the main flume that smoking machine produces;
(2) airbag is inserted in one end of adsorption sampling pipe, one end is sealedly attached to syringe pump, is evacuated in adsorption sampling pipe by the cigarette smoke in airbag by described syringe pump, has adsorbed rear sealed copper cap and has been sealed at adsorption sampling pipe two ends, for subsequent use;
(3) utilize thermal desorption instrument to carry out desorption and aging to the flue gas adsorbed in adsorption sampling pipe, then detect with Gc/ms Analyser;
(4) qualitative analysis is carried out to testing result;
(5) standard specimen of flue gas composition material to be measured is prepared, standard specimen is introduced in adsorption sampling pipe, then thermal desorption instrument-Gc/ms Analyser is utilized to measure the response of each standard specimen, set up the chromatographic peak area of each standard specimen composition and the ratio of interior mark peak area and the linear regression working curve of standard specimen concentration, and using the amount at 3 times of signal to noise ratio (S/N ratio) places as the detectability of assay method;
(6) quantitative test is carried out to testing result.
Wherein,
Preferably, described smoking machine is Borgwaldt200A type 20 duct rotating disk smoking machine; The correlation parameter of described rotating disk smoking machine is set as: the temperature of smoking machine preheating is 22 DEG C ± 2 DEG C, and the time of preheating is more than 20min; The wind speed of smoking machine is 10-50cm/s, is preferably 20-40cm/s; The pumping volume of described smoking machine is 10-90mL, is preferably 30-50mL.
Preferably, described airbag is Tedler airbag, can reduce the deposition of cigarette smoke on airbag; Described airbag is connected with the gas outlet of described smoking machine, for collecting the main flume of cigarette by a sampling flexible pipe.
Preferably, described syringe pump is LSP02-1B syringe pump; The range of described syringe pump is 140mm, stroke resolution: 0.156 μm, linear velocity scope: 5 μm/min-130mm/min.
Preferably, described adsorption sampling Guan Weisan section compound adsorption sampling pipe Carbotrap300, two ends are configured with sealed copper cap; Described sealed copper cap is selected from Swagelok copper cap.
Preferably, described thermal desorption instrument is TurboMatrix ATD thermal desorption instrument; Described Gc/ms Analyser adopts HP 7890A gas chromatograph and the HP 5975C mass spectrometer of coupling; Described thermal desorption instrument is connected with Gc/ms Analyser by the transmission line of a heating and thermal insulation.
Preferably, the condition of step (3) described desorption is: He:10.0psi; Valve: 200 DEG C; Pre-blowing: 1 ~ 3min; One-level desorption: temperature is 250 DEG C ~ 280 DEG C, 30min, and desorption flow is 40mL/min, the enrichment at-30 DEG C of import shunting 40mL/min, TenaxTA (60-80 order) adsorbent; Secondary desorption: temperature is 250 DEG C ~ 280 DEG C, 2min, outlet manifold 30mL/min.Transmission line temperature: 200 DEG C ~ 220 DEG C.
Preferably, the described aging condition of step (3) is: He:10.0psi; Valve: 220 DEG C; Pre-blowing: 1 ~ 3min; Aging temperature: 280 DEG C ~ 300 DEG C; Digestion time: 30min; Carrier gas flux: 40mL/min; Import is shunted: 40mL/min.
Preferably, the condition of work of step (3) described Gc/ms Analyser is: Supelco VOCOL capillary column, 60m*0.32mm*1.8um; Temperature programme: 35 DEG C (10min), 3.5 DEG C/min rises to 180 DEG C, and 10 DEG C/min rises to 210 DEG C (5min); Gas chromatography and mass spectrometer transmission interface temperature: 230 DEG C; Mass spectrometer detection mode: SCAN, sweep limit 10amu ~ 300amu.
In step (4), mass spectral database retrieval is adopted to carry out qualitative analysis.
In step (5), first prepare the methanol solution of certain density flue gas composition material to be measured and internal standard compound matter as working stocks, all the other each standard specimen methyl alcohol carry out stepwise dilution acquisition to working stocks, and in standard specimen at different levels, the relative scale of flue gas composition material concentration to be measured is 0.05:0.1:0.2:0.5:1; The content of the internal standard compound matter in every grade of standard specimen is identical; Then by adsorption sampling pipe access gas chromatograph packed column injection port, automatic sampler is utilized to introduce in adsorption sampling pipe by standard specimen at different levels; Then utilize thermal desorption instrument to carry out desorption and aging to the standard specimen material adsorbed in adsorption sampling pipe, then measure the response of each standard specimen with Gc/ms Analyser, set up working curve.
Preferably, described standard specimen introducing adsorption sampling pipe process instruments setting parameter is: He, constant current: 100mL/min, 20min, sample size: 1.0 μ L, injector temperature: 150 DEG C, furnace temperature: 30 DEG C; Described thermal desorption instrument and same step (3) is set for the operating parameter of the Gc/ms Analyser analyzed.
Preferably, described internal standard compound matter is deuterated benzene.
In step (5), described working curve is the linear regression working curve of flue gas composition material concentration in the ratio of the chromatographic peak area of flue gas composition material in standard specimen and the chromatographic peak area of internal standard compound matter and standard specimen.
In step (6), according to the chromatographic peak area of each composition of unknown sample and interior mark peak area ratio and linear regression working curve, calculate the content (μ g/cig) that the gas phase in every cigarette mainstream flue gas is divided into, computing formula is as follows:
Analyte ( μg / cig ) = ( A S A IS ) × RF × N × C
As: the chromatographic peak area of test substance; A iS: interior mark chromatographic peak area; RF: the response factor (calculating according to linear regression working curve) of standard specimen; N: puff number; C: conversion factor
Technique effect of the present invention and advantage are:
(1) to be collected by airbag and thermal desorption pipe trapping sampling, can in conjunction with both advantages that in time Collection and preservations are permanent, and make operator after having trapped the flue gas of all cigarette continuously, then while loading analysis, can greatly increase work efficiency
(2) sample time of syringe pump, speed and volume height are controlled, the repeatability that can greatly improve one's methods.
(3), after absorption-thermal desorption method/gas chromatography mass spectrometry carries out secondary desorption by the method that condensation is heated again, transfer in gas chromatograph by the transmission line of heating and thermal insulation, highly enriched effect can be reached.
(4) gas circuit of thermal desorption instrument used is through redesigning, no matter in which kind of state, outlet manifold gas purges capillary column entrance always, greatly reduces background signal, also has certain contribution for raising sensitivity and repeatability.
Accompanying drawing explanation
Airbag-thermal desorption gas/matter combined analysis device the system of the full composition of gas phase in a kind of analysis of cigarette of Fig. 1 main flume
Reference numeral:
1. airbag; 2. flue gas injection port; 3. adsorption sampling pipe; 4. connect the sampling flexible pipe of airbag; 5. syringe; 6. syringe pump; 7. smoking machine; 8. cigarette holder; 9. cigarette; 10. drip catcher (inside having cambridge filter); 11. pump units; The connecting tube of 12. to pump unit.
Embodiment
Below by way of specific instantiation, technical scheme of the present invention is described.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.
Embodiment 1
A method for the full composition of gas phase in airbag-thermal desorption-gas/matter coupling method analysis of cigarette main flume, for the qualitative analysis to certain trade mark cigarette, method step is as follows: (device as shown in Figure 1)
(1) flue gas is produced
By Borgwaldt200A type 20 duct rotating disk smoking machine at 22 DEG C ± 2 DEG C, preheating 20min, the wind speed of adjustment smoking machine and pumping volume, cigarette smoking mode is undertaken by iso standard.The wind speed 20cm/s of smoking machine; Pumping volume is 35mL, and suction time is 2s/puff, and every mouthful of interval time is 58s, collects the flue gas of 20 cigarette with Tedler airbag.
(2) flue gas is shifted
Collect the flue gas of 20 cigarette with Tedler airbag, after 2min, with LSP02-1B syringe pump, (syringe pump range is 140mm, stroke resolution: 0.156 μm, linear velocity scope: 5 μm/min-130mm/min; 60mL/min) shift 60mL flue gas and enter Carbontrap300 adsorption sampling pipe, after transfer terminates, adsorption sampling pipe two ends are sealed with Swagelok copper cap, to be measured.
(3) detection of exhaust gas compositions
TurboMatrix ATD thermal desorption instrument is adopted to carry out desorption and aging to adsorption sampling pipe, then carry out flue gas analysis with HP7890A gas chromatograph and the coupling of HP5975C mass spectrometer, thermal desorption instrument is connected with Gc/ms Analyser by the transmission line of a heating and thermal insulation; The desorption of adsorption sampling pipe on thermal desorption instrument and aging condition, gas chromatography/mass spectrometry optimum configurations is as follows:
Desorption conditions: He, 10.0psi; Valve: 200 DEG C; Pre-blowing: 1min; One-level desorption: temperature 280 DEG C, 30min, desorption flow 40mL/min, enrichment at import shunting 40mL/min, Tenax TA (60 ~ 80 order) adsorbent remains on-30 DEG C; Secondary desorption: temperature 280 DEG C, retains 2min, and shunting 30mL/min is carried out in outlet; Transmission line temperature: 210 DEG C.
Aging condition: He:10.0psi, valve: 220 DEG C, pre-blowing: 1min, aging temperature: 300 DEG C, digestion time: 30min, carrier gas flux: 40mL/min, import is shunted: 40mL/min.
Gas chromatography-mass spectrum condition: Supelco VOCOL capillary column, 60m*0.32mm*1.8um; Temperature programme: 35 DEG C (10min), 3.5 DEG C/min rises to 180 DEG C, and 10 DEG C/min rises to 210 DEG C (5min), gas chromatography and mass spectrometer transmission interface temperature: 230 DEG C; Mass spectrometer detection mode: SCAN, sweep limit 10amu ~ 300amu.
(4) qualitative analysis
Testing result spectrogram uses Willey7n.1 storehouse to carry out mass spectrum retrieval, identifies 67 kinds of chemical substances, as shown in table 1.
The full composition analysis result of table 1 gas phase
Embodiment 2
The method of the full composition of gas phase in a kind of airbag-thermal desorption-gas/matter coupling method analysis of cigarette main flume is used for the partial gas phase composition 1 to 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
During component tested with part in inner mark method ration mensuration main flume gas gas-phase objects, internal standard compound matter selects deuterated benzene, joins the methanol solution of tested component and internal standard compound matter as working stocks concentration (the 5th grade of mark liquid, in table 2); All the other mark liquid methyl alcohol at different levels carry out stepwise dilution acquisition.In every grade of mark liquid, the relative scale of measured matter concentration in mark liquid at different levels is: (1): (2): (3): (4): (5)=0.05:0.1:0.2:0.5:1.Interior scalar sum working stocks in every grade of mark liquid is identical.
Each amount of substance in table 21 μ L working stocks
Chemical substance Content (μ g) in 1 μ L
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 methylfuran of 2,5- 9.0
Ethylbenzene 4.3
Deuterated benzene (interior mark) 19.0
By adsorption sampling pipe access gas chromatograph packed column injection port, automatic sampler is utilized to introduce in adsorption sampling pipe by 1-5 level mark liquid; Instrument parameter: He, constant current: 100mL/min, 20min, sample size: 1.0 μ L, injector temperature: 150 DEG C, furnace temperature: 30 DEG C.Utilize thermal desorption instrument-gas chromatograph/mass spectrometer coupling method to measure the response of each standard substance, set up working curve; The operating parameter of thermal desorption instrument and Gc/ms Analyser arranges same embodiment 1.
Working curve checking situation is in 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
By computing formula: calculate the content of the gas phase composition in every cigarette mainstream flue gas;
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, pumping volume is 35mL/min, cigarette number is 20, sampling volume is 60mL, analysis result is as shown in table 4: wherein except cinnamic result slightly biased low except, the analysis result of all the other each materials all drops in the coverage of 2R4F, and with the content mean bias of 2R4F is all within 20%, the content mean bias wherein in the result of iso pentane two floride and acetone and 2R4F is within 5%; And cinnamic result is less than normal, mainly because it is two Entropy density deviation in main flume, and analysis result is herein just for gas phase composition.In different cigarette smokes, cinnamic two-phase partitioning ratio, approximately between 0.181 ~ 0.455, calculates in this ratio, and cinnamic measurement result is just similar in appearance to the report result of 2R4F.Show the analysis result of the inventive method or reliable.
Part main flume gas phase composition analysis result in table 4 cigarette sample

Claims (6)

1. a method for the full composition of gas phase in airbag-thermal desorption-gas/matter coupling method analysis of cigarette main flume, comprises the following steps:
(1) airbag is connected on smoking machine, gathers the main flume that smoking machine produces;
(2) airbag is inserted in one end of adsorption sampling pipe, one end is sealedly attached to syringe pump, is evacuated in adsorption sampling pipe by the cigarette smoke in airbag by described syringe pump, has adsorbed rear sealed copper cap and has been sealed at adsorption sampling pipe two ends, for subsequent use;
(3) utilize thermal desorption instrument to carry out desorption and aging to the flue gas adsorbed in adsorption sampling pipe, then detect with Gc/ms Analyser;
(4) qualitative analysis is carried out to testing result;
(5) standard specimen of flue gas composition material to be measured is prepared, standard specimen is introduced in adsorption sampling pipe, then thermal desorption instrument-Gc/ms Analyser is utilized to measure the response of each standard specimen, set up the chromatographic peak area of each standard specimen composition and the ratio of interior mark peak area and the linear regression working curve of standard specimen concentration, and using the amount at 3 times of signal to noise ratio (S/N ratio) places as the detectability of assay method;
(6) quantitative test is carried out to testing result;
Described airbag is Tedler airbag, and described airbag is connected with the gas outlet of described smoking machine, for collecting the main flume of cigarette by a sampling flexible pipe;
Described syringe pump is LSP02-1B syringe pump; The range of described syringe pump is 140mm, stroke resolution: 0.156 μm, linear velocity scope: 5 μm/min-130mm/min;
Described adsorption sampling Guan Weisan section compound adsorption sampling pipe Carbotrap300, two ends are configured with sealed copper cap; Described sealed copper cap is selected from Swagelok copper cap;
Described thermal desorption instrument is TurboMatrix ATD thermal desorption instrument; Described Gc/ms Analyser adopts HP7890A gas chromatograph and the HP5975C mass spectrometer of coupling; Described thermal desorption instrument is connected with Gc/ms Analyser by the transmission line of a heating and thermal insulation.
2. the method for claim 1, is characterized in that, described smoking machine is Borgwaldt200A type 20 duct rotating disk smoking machine; The correlation parameter of described rotating disk smoking machine is set as: the temperature of preheating is 22 DEG C ± 2 DEG C, and the time of preheating is more than 20min; Wind speed is 10-50cm/s; Pumping volume is 10-90mL.
3. the method for claim 1, is characterized in that, the condition of step (3) described desorption is: He:10.0psi; Valve: 200 DEG C; Pre-blowing: 1 ~ 3min; One-level desorption: temperature is 250 DEG C ~ 280 DEG C, 30min, and desorption flow is 40mL/min, the enrichment at-30 DEG C of import shunting 40mL/min, Tenax TA (60-80 order) adsorbent; Secondary desorption: temperature is 250 DEG C ~ 280 DEG C, 2min, outlet manifold 30mL/min; Transmission line temperature: 200 DEG C ~ 220 DEG C.
4. the method for claim 1, is characterized in that, the described aging condition of step (3) is: He:10.0psi; Valve: 220 DEG C; Pre-blowing: 1 ~ 3min; Aging temperature: 280 DEG C ~ 300 DEG C; Digestion time: 30min; Carrier gas flux: 40mL/min; Import is shunted: 40mL/min.
5. the method for claim 1, is characterized in that, the condition of work of step (3) described Gc/ms Analyser is: Supelco VOCOL capillary column, 60m*0.32mm*1.8um; Temperature programme: 35 DEG C (10min), 3.5 DEG C/min rises to 180 DEG C, and 10 DEG C/min rises to 210 DEG C (5min); Gas chromatography and mass spectrometer transmission interface temperature: 230 DEG C; Mass spectrometer detection mode: SCAN, sweep limit 10amu ~ 300amu.
6. the method for claim 1, it is characterized in that, in step (5), first prepare the methanol solution of certain density flue gas composition material to be measured and internal standard compound matter as working stocks, all the other each standard specimen methyl alcohol carry out stepwise dilution acquisition to working stocks, and in standard specimen at different levels, the relative scale of flue gas composition material concentration to be measured is 0.05:0.1:0.2:0.5:1; The content of the internal standard compound matter in every grade of standard specimen is identical; Then by adsorption sampling pipe access gas chromatograph packed column injection port, automatic sampler is utilized to introduce in adsorption sampling pipe by standard specimen at different levels; Then utilize thermal desorption instrument to carry out desorption and aging to the standard specimen material adsorbed in adsorption sampling pipe, then measure the response of each standard specimen with Gc/ms Analyser, set up working curve.
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