CN104266874B - Linear pattern smoking machine capturing device and its analysis test method with adsorption tube - Google Patents

Linear pattern smoking machine capturing device and its analysis test method with adsorption tube Download PDF

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Publication number
CN104266874B
CN104266874B CN201410482059.9A CN201410482059A CN104266874B CN 104266874 B CN104266874 B CN 104266874B CN 201410482059 A CN201410482059 A CN 201410482059A CN 104266874 B CN104266874 B CN 104266874B
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CN
China
Prior art keywords
adsorption tube
trap
smoking machine
capturing
tube
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CN201410482059.9A
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Chinese (zh)
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CN104266874A (en
Inventor
李雪
朱风鹏
罗彦波
张洪非
陈再根
姜兴益
庞永强
侯宏卫
胡清源
黄卫东
辛宝珺
常诚
曾波
孟科
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国家烟草质量监督检验中心
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Publication of CN104266874A publication Critical patent/CN104266874A/en
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Abstract

The present invention provides a kind of linear pattern smoking machine capturing device and its analysis test method with adsorption tube, including Attraction block (1), artificial lip clamper (2), artificial lip (3), trap protecgulum (5), trap bonnet (6) and adsorption tube keeper (7), it is internal that the artificial lip (3) is arranged on the artificial lip clamper (2), the front end of the trap protecgulum (5) is inserted in the artificial lip clamper (2) and is resisted against on the artificial lip clamper, the present apparatus is easy to operate, and determine reproducible, organic solvent consumption is few, sample tests are with standard method without significant difference, and trapped while realizing at room temperature to VOC and carbonyls, suitable for the analysis of batch samples.

Description

Linear pattern smoking machine capturing device and its analysis test method with adsorption tube
Technical field
The present invention relates to cigarette smoke technical field of analysis and detection, more particularly to a kind of linear pattern smoking machine with adsorption tube Capturing device and the method that test cigarette smoke is analyzed using the capturing device.
Background technology
With carrying out in a deep going way for smoking and health research, people are increasingly paid close attention to the harmful components in cigarette smoke.Volume Contain a large amount of VOCs and carbonyls in cigarette main flume, the detection name of Her Majesty the Queen in right of Canada as represented by the minister of Healt's concern is single-row In the 44 kinds of harmful components gone out, VOC has 5 kinds:1,3- butadiene, isoprene, acrylonitrile, benzene and toluene; Carbonyls has 8 kinds:Formaldehyde, acetaldehyde, propionic aldehyde, acetone, methacrylaldehyde, crotonaldehyde, 2- butanone, butyraldehyde.Therefore, in cigarette smoke VOC and effective trapping of carbonyls and Accurate Determining there is reality to anticipate smoking and health research Justice.At present, existing many use combined gas chromatography mass spectrometries (GC-MS) determine VOC in cigarette smoke Report, it is main to be trapped using cold soln absorption process (- 70 DEG C or so of methanol) and sorbent tube method.Cold soln absorption process is used The trapping of the receiving flask equipped with 15mL cold methanols of two series connection, it is cumbersome.Sorbent tube method, smoking machine suction channel " dead volume " Larger with pressure drop, test result reappearance is poor.The collection of carbonyls mainly has two methods:One kind is that solution absorbs Method, another is by the way of superposition cambridge filter.Because solution absorption method is cumbersome, usual people use cambridge filter To trap the carbonyl complex in cigarette smoke.But, the mode of this filter disc trapping needs to be put into two in trap Cambridge filter, and the design of existing trap is, using a filter disc as standard, trap to be produced after two filter discs of superposition The problem of sealing loosely.Meanwhile, the derivating agent of acetontrile, which can be bonded on trap, to be difficult to clear up, and not only causes analyte to remain As a result forbidden also cause trap is contaminated to be difficult to clean up.
The content of the invention
To overcome existing defect, the present invention proposes a kind of linear pattern smoking machine capturing device with adsorption tube, including, inhale Attached pipe, artificial lip clamper, artificial lip, trap protecgulum, trap bonnet and adsorption tube keeper, it is characterised in that described Artificial lip is arranged on inside the artificial lip clamper, and the front end of the trap protecgulum is inserted in the artificial lip clamper simultaneously It is resisted against on the artificial lip clamper, the rear end of the trap protecgulum has before the first recess, the trap bonnet End is accommodated in first recess, and the rear end of the trap bonnet has the second recess, the adsorption tube keeper Front end is accommodated in second recess, and the adsorption tube keeper is provided with hollow cavity, and the Attraction block is located at described In hollow cavity, the front end of trapping chamber is connected to the Cigarette of the artificial lip insertion.
The first packing ring with through hole is arranged in the trap protecgulum, and the preceding surface connection of first packing ring is described Cigarette, after trap protecgulum is connected with trap bonnet, is internally formed hollow channel, wherein, the connection of the first packing ring rear end The passage.
Adsorption tube keeper is hollow cavity, and adsorption tube is located in adsorption tube keeper.
Adsorption tube includes outer tube, Attraction block, cone-shaped interface and packing ring, wherein, outer tube is hollow circular cylinder, and Attraction block is located at Outer tube, cone-shaped interface is hollow circular cylinder, and its inner hollow chamber is taper, and internal cavities wide mouth end connects outer tube side, Wherein second packing ring is hollow circular cylinder, and it is located inside cone-shaped interface, and is adjacent to Attraction block.
It is solid adsorption material in the middle part of Attraction block, solid adsorption material both sides set sieve plate.
It is solid adsorption material in the middle part of Attraction block, solid adsorption material both sides set sieve plate;The sorbing material is activity Carbon Materials, magnetic adsorptive material or molecular screen material, the particle diameter of the sorbing material is 40-80 μm, the institute of the sorbing material State the core sieve plate that two sieve plates are 40-60 μm of aperture.
Because the present invention uses Novel flue gas capturing device, added compared with conventional absorption plant in trap bonnet Pipe unit is adsorbed, the effusion of flue gas is relaxed, the extended residence time in trap, and the sorbing material between sieve plate There is preferable adsorption effect to the VOC in cigarette smoke, cigarette smoke air-flow can be made to be connect with adsorbent Touch abundant, it is ensured that the Related Component in cigarette smoke is effectively absorbed, meet in cigarette smoke VOC and The requirement trapped while carbonyls.
Brief description of the drawings
Fig. 1 is the linear pattern smoking machine capturing device schematic diagram with adsorption tube.
Fig. 2 is adsorption tube schematic diagram.
Embodiment
A kind of linear pattern smoking machine with adsorption tube provided below in conjunction with the accompanying drawings with specific embodiment the present invention is trapped Device is described in detail.
Fig. 1 shows a kind of linear pattern smoking machine capturing device with adsorption tube, including, adsorption tube 1, artificial lip clamper 2, people Work lip 3, trap protecgulum 5, trap bonnet 6 and adsorption tube keeper 7, according to the present invention, artificial lip 3 is clamped positioned at artificial lip Inside device 2, the front end insertion artificial lip clamper 2 of trap protecgulum 5 is interior and is resisted against on artificial lip clamper 2, before trap The rear end of lid 5 has the first recess, and the front end of trap bonnet 6 is accommodated in first recess.After trap bonnet 6 End has the second recess, and the front end of adsorption tube keeper 7 is accommodated in second recess.Attraction block keeper 7 is provided with Hollow cavity, adsorption tube 1 is located in the hollow cavity.
According to a preferred embodiment of the present invention, the first packing ring 4 with through hole is arranged on the trap protecgulum 5 In.The preceding surface connection Cigarette 8 of first packing ring 4, after trap protecgulum 5 is connected with trap bonnet 6, is internally formed hollow Passage, wherein, the rear end of packing ring 4 connects the passage.
Adsorption tube keeper 7 is hollow cavity, and adsorption tube 1 is located at adsorption tube keeper 7.
Fig. 2 shows, adsorption tube 1, including, outer tube 11, Attraction block 12, cone-shaped interface 13 and second packing ring 14, wherein, outer tube 11 be hollow circular cylinder, and Attraction block 12 is located inside outer tube 11, and cone-shaped interface 13 is hollow circular cylinder, and its internal cavities is cone Type, internal cavities wide mouth end connection outer tube 11 side, wherein second packing ring 14 are hollow circular cylinder, and it is located in cone-shaped interface 13 Portion, and it is adjacent to Attraction block 12.
The middle part of Attraction block 12 is solid adsorption material 121, and the both sides of solid adsorption material 121 set sieve plate 122.
Sorbing material 121 in adsorption tube 1 is absorbent charcoal material, magnetic adsorptive material or molecular screen material, and its particle diameter is 40-80μm.Two side sieve plates 122 are the core sieve plate in 40-60 μm of aperture.
Using the present invention with adsorption tube linear pattern smoking machine capturing device analysis test cigarette smoke method include with Lower step:
Step 1, the processing of cigarette sample, extracts cigarette sample, and sample is carried out according to the standard rated conditions of GB/T 16447 Balance, selecting average quality ± 0.02g and average resistance to suction ± 50Pa cigarette is used for sample test.
Step 2, linear pattern smoking machine capturing device is arranged on smoking machine, every time suction 1;
Step 3, capturing device is removed after having trapped, Attraction block 1 is transferred in container and carries out extraction processing;
Step 4, blank sample is arranged in linear pattern smoking machine capturing device, suction 1, and repeat step 3 every time, The blank sample result of acquisition is compareed with cigarette sample result, had with the volatility analyzed in cigarette smoke Machine compound and carbonyls.
According to Chromatography/Mass Spectrometry (GC/MS) instrument condition of the analysis test method of the present invention:Chromatographic column is InertCap AQUATIC-2 chromatographic column (length:60m, internal diameter:0.25mm, thickness:1.4μm);Temperature programming program is:Initial temperature is 40 DEG C, 6.0min is kept, 20 DEG C/min heating rate is warming up to 230 DEG C, keeps 10min;Carrier gas is helium, and flow velocity is 1.5mL/ min;Injector temperature is 180 DEG C, and sampling volume is 1.0 μ L, and split ratio is 10:1;230 DEG C of transmission line temperature, ion source temperature 230 DEG C, 150 DEG C of quadrupole rod temperature;Mass ions voltage is 70eV;Scan mode:Full scan and choice ion pattern are simultaneously Carry out.
Liquid phase chromatogram condition:Chromatographic column Explosive E2 250mm×4.6mmChromatographic column 5 μm of filler particle size (Dionex companies of the U.S.);Mobile phase A is acetonitrile/water (50/50, v/v), ammonium acetate containing 10mM, Mobile phase B For acetonitrile/water (80/20, v/v), the eluent gradient used keeps 5.0min for 100%A, linear in 50min afterwards Change turns to 100%B, and keeps 10.0min.Flow rate of mobile phase is 0.8mL/min;Chromatogram column temperature is 30 DEG C;Sampling volume is 5 μL。
The quantitative and qualitative ion of each compound is as shown in table 1 below:
The retention time of each target compound of table 1, quantitative and qualitative ion
The course of work of present invention when for flue gas analysis be:
Cigarette is in aspiration procedure, and cigarette smoke enters absorption pipe unit by cambridge filter, flows through adsorption tube Then flowed out from capturing device back outlet, cigarette smoke is efficiently absorbed in the process.
Next, illustratively illustrating to survey using the linear pattern smoking machine capturing device analysis of the present invention by embodiment The method for trying VOC and carbonyls in cigarette smoke.
Embodiment 1:
Trade mark A cigarette is chosen, Sample equilibration is carried out according to the standard rated conditions of GB/T 16447, select (average quality ± 0.02) g and (average resistance to suction ± 50) Pa cigarette are used for sample test.Ready capturing device is arranged on smoking machine, Aspirated under iso standard rated condition, pumping volume 35.0mL, suction time 2s, suction frequencies 60s.Suction 1 every time Branch;Capturing device is removed in suction trapping completion, and adsorption tube is taken out, cut off and corresponding container progress extraction processing is transferred to;Together The process of sample makes blank sample, and the result of blank sample is compareed with the result of A cigarette.
Measurement result-the ISO of VOC in the trade mark A cigarette of table 2
Measurement result-the ISO of carbonyls in the trade mark A cigarette of table 3
Embodiment 2:
Trade mark B cigarette is chosen, Sample equilibration is carried out according to the standard rated conditions of GB/T 16447, select (average quality ± 0.02) g and (average resistance to suction ± 50) Pa cigarette are used for sample test.Ready capturing device is arranged on smoking machine, Aspirated under Canadian depth suction (HCI) standard rated condition, pumping volume 55.0mL, suction time 2s, suction frequency Rate 30s.Suction 1 every time;Capturing device is removed in suction trapping completion, and adsorption tube is taken out, cut off and corresponding container is transferred to Carry out extraction processing;Same process makes blank sample, and the result of blank sample and the result of B cigarette are entered Row control.
Measurement result-the HCI of VOC in the trade mark B cigarette of table 4
Measurement result-the HCI of carbonyls in the trade mark B cigarette of table 5
Because the present invention uses Novel flue gas capturing device, added compared with conventional absorption plant in trap bonnet Pipe unit is adsorbed, the effusion of flue gas is relaxed, the extended residence time in trap, and the sorbing material between sieve plate There is preferable adsorption effect to the VOC in cigarette smoke, cigarette smoke air-flow can be made to be connect with adsorbent Touch abundant, it is ensured that the Related Component in cigarette smoke is effectively absorbed, meet in cigarette smoke VOC and The requirement of carbonyls analysis.Apparatus of the present invention are easy to operate, and determine reproducible, and organic solvent consumption is few, sample Product test result and standard method can be realized to VOC and carbonyls at room temperature without significant difference Trapping, it is adaptable to the analysis of batch samples.
Finally it should be noted that above example is only to describe technical scheme rather than to this technology method Limited, the present invention application can above extend to other modifications, change, using and embodiment, and it is taken as that institute Have such modification, change, using, embodiment all in the range of the spirit or teaching of the present invention.

Claims (6)

1. a kind of linear pattern smoking machine capturing device with adsorption tube, including adsorption tube (1), artificial lip clamper (2), artificial lip (3), trap protecgulum (5), trap bonnet (6) and adsorption tube keeper (7), it is characterised in that the artificial lip (3) is set Internal in the artificial lip clamper (2), the front end of the trap protecgulum (5) is inserted in the artificial lip clamper (2) simultaneously It is resisted against on the artificial lip clamper, the rear end of the trap protecgulum (5) has the first recess, the trap bonnet (6) front end is accommodated in first recess, and the front end of the trap bonnet (6) has the second recess, the absorption The front end of pipe keeper (7) is accommodated in second recess, and the adsorption tube keeper (7) is provided with hollow cavity, institute Adsorption tube (1) is stated in the hollow cavity, the front end of trapping chamber is connected to the Cigarette of the artificial lip insertion (8);
Wherein, the adsorption tube (1) includes outer tube (11), Attraction block (12), cone-shaped interface (13) and second packing ring (14), its In, outer tube (11) is hollow circular cylinder, and Attraction block (12) is located at outer tube (11) inside, and cone-shaped interface (13) is hollow circular cylinder, Its internal cavities is taper, and internal cavities wide mouth end connection outer tube (11) side, wherein second packing ring (14) are hollow circular cylinder, It is located at cone-shaped interface (13) inside, and is adjacent to Attraction block (12);Inhaled in the adsorption tube (1) in the middle part of Attraction block (12) for solid Enclosure material (121), solid adsorption material (121) both sides set sieve plate (122);The sorbing material (121) be absorbent charcoal material, Magnetic adsorptive material or molecular screen material, the particle diameter of the sorbing material is 40-80 μm, the sieve plate of the sorbing material both sides (122) it is the core sieve plate in 40-60 μm of aperture.
2. the linear pattern smoking machine capturing device according to claim 1 with adsorption tube, it is characterised in that with through hole First packing ring (4) is arranged in the trap protecgulum (5), and the preceding surface of first packing ring connects the Cigarette (8), After trap protecgulum (5) is connected with trap bonnet (6), hollow channel is internally formed, wherein, the connection of the first packing ring (4) rear end The passage.
3. the linear pattern smoking machine capturing device according to claim 1 with adsorption tube, it is characterised in that adsorption tube is kept Part (7) is hollow cavity, and adsorption tube (1) is located in adsorption tube keeper (7).
4. the side of cigarette smoke is tested by the analysis of the linear pattern smoking machine capturing device with adsorption tube described in claim 1 Method, comprises the following steps,
Step 1, Sample equilibration is carried out according to the standard rated conditions of GB/T 16447, selects average quality ± 0.02g and inhaled with average Resistance ± 50Pa cigarette is used for sample test:
Step 2, the linear pattern smoking machine capturing device is arranged on smoking machine, every time suction 1;
Step 3, the linear pattern smoking machine capturing device is removed after having trapped, the Attraction block is transferred in container and extracted Take processing;
Step 4, blank sample is arranged in the linear pattern smoking machine capturing device, suction 1, and repeat step 3 every time, The blank sample result of acquisition is compareed with cigarette sample result, had with the volatility analyzed in cigarette smoke Machine compound and carbonyls.
5. method according to claim 4, it is characterised in that in the step 2, the capturing device is arranged on and inhaled On cigarette machine, aspirated under iso standard rated condition, pumping volume 35mL, suction time 2s, suction frequencies 60s takes out every time Inhale 1.
6. method according to claim 4, it is characterised in that in the step 2, smoking machine is arranged on by capturing device On, aspirated under Canadian depth suction (HCI) standard rated condition, pumping volume 55mL, suction time 2s, suction frequency Rate 30s, every time suction 1.
CN201410482059.9A 2014-09-19 2014-09-19 Linear pattern smoking machine capturing device and its analysis test method with adsorption tube CN104266874B (en)

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