CN104833719A - Mono-photon time of flight mass spectrum on-line puff-by-puff analysis on 7 volatile organic compounds in mainstream cigarette smoke of thin cigarette - Google Patents
Mono-photon time of flight mass spectrum on-line puff-by-puff analysis on 7 volatile organic compounds in mainstream cigarette smoke of thin cigarette Download PDFInfo
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Abstract
The invention discloses mono-photon time of flight mass spectrum on-line puff-by-puff analysis on 7 volatile organic compounds in mainstream cigarette smoke of thin cigarette, and belongs to the field of cigarette smoke gas component detection and analysis. The mono-photon time of flight mass spectrum on-line puff-by-puff technology is adopted to analyze seven volatile organic compounds in the mainstream cigarette smoke of thin cigarettes. Under the conditions of international standardization organization (ISO) and Canadian intense smoking regime (HCI), 7 volatile organic compounds released from thin cigarettes of 9 brands are quantitatively and qualitatively analyzed online puff-by-puff. Under the ISO conditions, 7 volatile organic compounds released from 20 conventional cigarettes including flue-cured type cigarettes and blended type cigarette are quantitatively and qualitatively analyzed online; wherein the 7 volatile compounds are acetaldehyde, 1,3-butadiene, acetone, isoprene, 2-butanone, benzene, and toluene.
Description
Technical field
The invention belongs to components in cigarette smoke gas phase composition detection analysis technical field, be specifically related to a kind of single photon flight time mass spectrum and analyze 7 kinds of volatile organic compounds in ramuscule cigarette main flume by mouth online.
Background technology
Ramuscule cigarette and ultra-fine cigarette are the tobacco products that circumference is less than conventional cigarette, and the general circumference of ultra-fine cigarette is down to below 17mm, usually adopts longer filter tip, and cigarette pipe tobacco amount is lower, and the market share of these products constantly increases in recent years.This product design mainly for young man and female consumer, and often gives the impression of less harmful.Therefore, European Union, World Health Organization (WHO) intend taking measure of control to it.But the research of ramuscule cigarette flue gas releaser level is also less at present, is necessary to carry out the correlative study of ramuscule cigarette releaser, for the work of honouring an agreement provides scientific basis.
2012, May Siu etc. analyzes the mainstream smoke constituents of the ramuscule cigarette of six trades mark, and contrast with the commercially available stock size cigarette product of Canada, result shows, the carbon monoxide of ramuscule cigarette, carbonyls, volatile organic compounds and aromatic amine burst size are starkly lower than traditional cigarette, and formaldehyde, ammonia, phenol release amount are high.The tobacco-specific nitrosamine burst size of mixed type ramuscule cigarette is significantly higher than fire-cured tobacco type.In this article, under testing ISO and the degree of depth two kinds of suction modes, reach the burst size of 32 kinds of compositions, need the Canadian Official Analytical's method of use nine kinds in ramuscule cigarette main flume, experiment needs at substantial time and resource.2013, Coggins etc. have detected releaser level and the biology toxicity thereof of 9 kinds of compositions in different circumference cigarette sample.Result shows, the multiple smoke components comprising tobacco-specific nitrosamine reduces with the reduction of circumference, and hydrogen cyanide has rising trend, but this rising and circumferential variation non-correlation.The different detection technique of use 4 kinds is needed to realize the detection of 9 kinds of objects in experiment.At present, China's tobacco business uses the volatile organic compounds (GB/T 27523-2011) in gas chromatography/mass spectrometry main flume usually, uses the carbonyls (YC/T 254-2008) in high performance liquid chromatography derivatization method mensuration main flume.In addition, the deep propelling of honouring an agreement along with international Tobacco Control, the objectionable constituent inventory of flue gas releaser control is also in continuous expansion.Therefore, develop and use efficient, high-throughout flue gas releaser constituent analysis technology to scientific research and work of honouring an agreement significant.
At present, smoking machine manufacturer Borgwaldt company and Photonion company have combined and have released commercial one channel smoke sucking machine coupling single photon time of-flight mass spectrometer LMX2-TOFMS.But the flight time mass spectrum of this type of application mostly is Algorithm, in flue gas complex matrices, to a large amount of gas phase of Simultaneously test and semi-volatile organic compounds, often needs to be connected in series with gas chromatography multidimensional.
Summary of the invention
A kind of single photon flight time mass spectrum is the object of the present invention is to provide to analyze 7 kinds of volatile organic compounds in ramuscule cigarette main flume by mouth online.
Based on above-mentioned purpose, this invention takes following technical scheme:
Single photon flight time mass spectrum analyzes 7 kinds of volatile organic compounds in ramuscule cigarette main flume by mouth online, it comprises the detection system adopting smoking machine to be connected with single photon time of-flight mass spectrometer and carries out analyzing 7 kinds of volatile organic compounds in ramuscule cigarette main flume by mouth online respectively under International standardization (ISO 3308:2012) suction mode and Canadian degree of depth suction (HCI T-115) pattern, concrete steps are: (1) opens smoking machine, mass spectrometric power supply, setting mass spectrometric transmission line temperature is 180 DEG C, interface temperature is 250 DEG C, injector temperature is 250 DEG C, after mass spectrometer reaches the temperature of setting, standard correction disulfonic gas is used to carry out automatic calibration to instrument, (2) correct by rear, use the ramuscule cigarette after smoking machine suction balance, acetaldehyde in ramuscule cigarette main flume is analyzed online by mouth, 1, 3-butadiene, acetone, isoprene, 2-butanone, this volatile organic compounds in 7 of Benzene and Toluene, the gas flow making flue gas enter ionized region is 0.7 mL/min, standard correction gas concentration is 100ppm toluene/nitrogen, resolution is >500, use argon lamp, photon energy is at 9.8 ± 0.4eV, soft ionization is carried out to object, qualitative with molion mass-to-charge ratio m/z, with effective ion rate and response signal intensity, be each object instrumental correction factor with the ratio of the response signal intensity of calibration gas, directly carry out quantitatively, often wheel experiment smoking cigarette cigarette number is 5, after often wheel suction terminates, carry out 5 suctions to clean gas circuit.
Preferably, in described step (1), smoking machine is Borgwaldt Gui 2 duct smoking machine; Described mass spectrometer is Smoke Analyser LMX2-TOFMS single photon time of-flight mass spectrometer.
In described step (2), the balance of ramuscule cigarette is temperature is 22 ± 1 DEG C, and relative humidity is under the standard conditions of (60 ± 3) %, balance 48h.
In described step (2) under ISO (International Standards Organization) suction mode: pumping volume is 35mL, puff interval 60s, puff duration phase 2s, does not close filter tip air vent; Under Canadian degree of depth suction mode: pumping volume is 55mL, puff interval 30s, puff duration phase 2s, closes filter tip air vent.
The present invention establishes a kind of method being applicable to ramuscule cigarette mainstream smoke constituents on-line analysis, compared with existing other technologies, has following advantage:
1. the inventive method does not need to trap volatile organic compounds in main flume, can on-line analysis;
2. the present invention is with volatile organic compounds effective ion rate (γ) and response signal intensity PICS in main flume, with the ratio of calibration gas (usually using benzene or toluene) the signal intensity correction factor as target compound, directly carry out qualitative and quantitative analysis, do not need to set up evaluating objects thing standard working curve;
3. the inventive method is to ramuscule cigarette mainstream smoke constituents online by mouth analysis, can obtain every mouthful of mainstream smoke drawn releaser and send rule, investigates cigarette circumference to the impact of multiple main flume volatile organic compounds burst size simultaneously.
Accompanying drawing explanation
Fig. 1 is the comparison (all using method of the present invention) of conventional smoke and ramuscule cigarette 7 kinds of compound burst sizes under ISO, HCI condition in embodiment;
Fig. 2 is that ramuscule cigarette/conventional size cigarette smoke releaser level compares under ISO and HCI pattern;
Fig. 3 be under HCI condition in 1# sample main flume acetaldehyde by mouth burst size;
Fig. 4 be under HCI condition in 1# sample main flume 1,3-butadiene by mouth burst size;
Fig. 5 be under HCI condition in 1# sample main flume acryl aldehyde by mouth burst size;
Fig. 6 be under HCI condition in 1# sample main flume acetone by mouth burst size;
Fig. 7 be under HCI condition in 1# sample main flume isoprene by mouth burst size;
Fig. 8 be under HCI condition 1# sample crotonaldehyde in mainstream smoke by mouth burst size;
Fig. 9 be under HCI condition in 1# sample main flume 2-butanone by mouth burst size;
Figure 10 be under HCI condition in 1# sample main flume benzene by mouth burst size;
Figure 11 be under HCI condition in 1# sample main flume toluene by mouth burst size;
Figure 12 be under HCI condition in 1# sample main flume phenol by mouth burst size.
Embodiment
Below in conjunction with specific embodiment, technical scheme of the present invention is described in further detail, but protection scope of the present invention is not limited thereto.
Embodiment 1
Single photon flight time mass spectrum analyzes 7 kinds of volatile organic compounds in the ramuscule cigarette main flume of 9 trades mark online by mouth, step is:
(1) open smoking machine, mass spectrometric power supply, setting mass spectrometric transmission line temperature is 180 DEG C, and interface temperature is 250 DEG C, and injector temperature is 250 DEG C, after mass spectrometer reaches the temperature of setting, uses standard correction disulfonic gas to carry out automatic calibration to instrument, (2) correct by rear, use the ramuscule cigarette after smoking machine suction balance, acetaldehyde in ramuscule cigarette main flume is analyzed online by mouth, 1, 3-butadiene, acetone, isoprene, 2-butanone, these 7 kinds of volatile organic compounds of Benzene and Toluene, the gas flow making flue gas enter ionized region is 0.7 mL/min, standard correction gas concentration is 100ppm toluene/nitrogen, resolution is >500, use argon lamp, photon energy is at 9.8 ± 0.4eV, soft ionization is carried out to object, qualitative with molion mass-to-charge ratio m/z, with effective ion rate and response signal intensity, be each object instrumental correction factor (the instrumental correction factor of 7 kinds of compounds is in table 2) with the ratio of the response signal intensity of calibration gas, directly carry out quantitatively, computing formula is as follows:
Wherein:
PICS
arepresent and analyze object light ionization cross section;
PICS
brepresent calibration gas photoionization cross section;
f a represent correction factor;
γrepresent rate of ionization;
s a represent and analyze thing response signal intensity;
s b represent calibration gas response signal intensity;
n a represent and analyze thing molal quantity;
n b represent calibrating gas molal quantity.
Often wheel experiment smoking cigarette cigarette number is 5, and after often wheel suction terminates, carry out 5 suctions to clean gas circuit, smoking parameters is in table 1.
Smoking parameters under table 1 ISO and HCI suction mode
Volatile organic compounds correction factor (relative to toluene) in table 2 ramuscule cigarette main flume
1,under ISO and Canadian degree of depth suction mode, ramuscule cigarette 7 kinds of volatile organic compounds measurement results of 9 trades mark are in table 3, table 4
Table 3 ramuscule cigarette is ramuscule cigarette mainstream smoke constituents content at iso conditions
Unit: microgram/
Table 4 ramuscule cigarette is ramuscule cigarette mainstream smoke constituents content under HCI condition
Unit: microgram/
2,under ISO pattern, 7 kinds of volatile organic compounds average measurement of 20 kinds of traditional cigarette (comprising fire-cured tobacco type and blended type cigarette) the results are shown in Table 5.
Table 5 conventional size cigarette mainstream smoke constituents content at iso conditions
Unit: microgram/
3,the test result of context of methods to ramuscule cigarette and conventional smoke is used to compare
Use context of methods, ramuscule cigarette is in the degree of depth suction of ISO, HCI(Canada) the mainstream smoke constituents releaser content that measures under condition and average are in table 3, table 4, and the main flume releaser average that conventional size cigarette records at iso conditions is in table 5.The burst size of the acetaldehyde of ramuscule cigarette under ISO and HCI condition, 1,3-butadiene, acetone, isoprene, 2-butanone, Benzene and Toluene all lower than conventional smoke, as shown in Figure 1.
,compared with ramuscule cigarette (context of methods) and conventional size cigarette (universaling analysis method) 7 kinds of volatile organic compounds burst sizes
Acetaldehyde, 1,3-butadiene, acetone, isoprene, 2-butanone, the content of Benzene and Toluene in flue gas compare with the conventional size cigarette using universaling analysis method to record, and investigate under ISO and HCI different mode, and releaser level changes situation.As shown in Figure 2, ISO ratio refers at iso conditions, ramuscule cigarette flue gas releaser content/conventional size cigarette smoke releaser content, and display ramuscule cigarette smoke delivery is all lower than conventional size cigarette, and under HCI condition, this reduction is more remarkable.
In bibliographical information about ramuscule cigarette flue gas releaser level, show a lot of smoke components content lower than traditional cigarette, although can not think that its harmfulness reduces accordingly, but propose according to tobacco product control research group of World Health Organization No. 951 scientific literature---Chemical Components in Cigarette Smoke setting the highest limitation " median " measure, correlative study should be carried out, obtain ramuscule cigarette every milligram of nicotine flue gas releaser level condition, based on scientific basis, formulate the control requirement to ramuscule cigarette.
, main flume analyzes by mouth burst size
With 1# sample for legend, under the dark suction mode of Canada (Fig. 3-12), in ten kinds of objects of this experimental analysis, present certain release rule by mouth suction, first is higher, and second mouthful minimum, 3rd mouthful and the 4th mouthful increases again to some extent, particularly 1,3-butadiene and benzene, first burst size is apparently higher than later mouth number.In the end a bite burst size is lower for some cigarettes, is because last a bite puff number is imperfect.
Under ISO pattern, several ultra-fine smoke release is consistent with above-mentioned rule, and the sample that circumference is larger, the composition firsts such as toluene, 2-butanone, not higher than second mouthful, show by the mouth release rule property of there are differences.Analyzing this phenomenon Producing reason, may be because the reduction gas velocity increase along with circumference under identical suction flow causes.
Claims (5)
1. single photon flight time mass spectrum analyzes 7 kinds of volatile organic compounds in ramuscule cigarette main flume by mouth online, it is characterized in that, the detection system adopting smoking machine to be connected with single photon time of-flight mass spectrometer carries out analyzing 7 kinds of volatile organic compounds in ramuscule cigarette main flume by mouth online respectively under ISO (International Standards Organization) suction mode and Canadian degree of depth suction mode, concrete steps are: (1) opens smoking machine, mass spectrometric power supply, setting mass spectrometric transmission line temperature is 180 DEG C, interface temperature is 250 DEG C, injector temperature is 250 DEG C, after mass spectrometer reaches the temperature of setting, standard correction disulfonic gas is used to carry out automatic calibration to instrument, (2) correct by rear, use the ramuscule cigarette after smoking machine suction balance, acetaldehyde, 1 in ramuscule cigarette main flume is analyzed online by mouth, this volatile organic compounds in 7 of 3-butadiene, acetone, isoprene, 2-butanone, Benzene and Toluene, soft ionization is carried out to object, qualitative with molion mass-to-charge ratio m/z, with effective ion rate and response signal intensity, be each object instrumental correction factor with the ratio of the response signal intensity of calibration gas, directly carry out quantitatively, often wheel experiment smoking cigarette cigarette number is 5.
2. single photon flight time mass spectrum according to claim 1 analyzes 7 kinds of volatile organic compounds in ramuscule cigarette main flume by mouth online, it is characterized in that, in described step (1), smoking machine is Borgwaldt Gui 2 duct smoking machine; Described mass spectrometer is Smoke Analyser LMX2-TOFMS single photon time of-flight mass spectrometer.
3. single photon flight time mass spectrum according to claim 1 analyzes 7 kinds of volatile organic compounds in ramuscule cigarette main flume by mouth online, it is characterized in that, in described step (2), the balance of ramuscule cigarette is temperature is 22 ± 1 DEG C, relative humidity is under the standard conditions of (60 ± 3) %, balance 48h.
4. single photon flight time mass spectrum according to claim 1 analyzes 7 kinds of volatile organic compounds in ramuscule cigarette main flume by mouth online, it is characterized in that, in described step (2), flue gas enters the gas flow of ionized region is 0.7 mL/min, standard correction gas concentration is 100ppm toluene/nitrogen, resolution is >500, use argon lamp, photon energy is 9.8 ± 0.4eV.
5. single photon flight time mass spectrum according to claim 1 analyzes 7 kinds of volatile organic compounds in ramuscule cigarette main flume by mouth online, it is characterized in that, in described step (2) under ISO (International Standards Organization) suction mode: pumping volume is 35mL, puff interval 60s, puff duration phase 2s, does not close filter tip air vent; Under Canadian degree of depth suction mode: pumping volume is 55mL, puff interval 30s, puff duration phase 2s, closes filter tip air vent.
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| CN102636556A (en) * | 2012-04-23 | 2012-08-15 | 上海烟草集团有限责任公司 | Ion molecule mass-spectrometric method for on-line detection of gas phase composition of cigarette smoke mouth by mouth |
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| CN104201085A (en) * | 2014-08-25 | 2014-12-10 | 暨南大学 | Direct mass spectrometric analysis method for stinking organic matters discharged from landfill |
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