WO2016041348A1 - 一种转盘型吸烟机捕集装置及使用该装置分析卷烟烟气的方法 - Google Patents

一种转盘型吸烟机捕集装置及使用该装置分析卷烟烟气的方法 Download PDF

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WO2016041348A1
WO2016041348A1 PCT/CN2015/076486 CN2015076486W WO2016041348A1 WO 2016041348 A1 WO2016041348 A1 WO 2016041348A1 CN 2015076486 W CN2015076486 W CN 2015076486W WO 2016041348 A1 WO2016041348 A1 WO 2016041348A1
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Prior art keywords
adsorption
smoking machine
trap
adsorption block
adsorbent material
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PCT/CN2015/076486
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English (en)
French (fr)
Inventor
侯宏卫
姜兴益
罗彦波
庞永强
朱风鹏
李雪
张洪非
胡清源
陈再根
辛宝珺
黄卫东
常诚
曾波
牛罡
任静霞
孟科
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国家烟草质量监督检验中心
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Priority claimed from CN201410481831.5A external-priority patent/CN104266872B/zh
Priority claimed from CN201410482010.3A external-priority patent/CN104266873B/zh
Application filed by 国家烟草质量监督检验中心 filed Critical 国家烟草质量监督检验中心
Priority to EP15842509.0A priority Critical patent/EP3196630B1/en
Priority to JP2017534868A priority patent/JP6646674B2/ja
Publication of WO2016041348A1 publication Critical patent/WO2016041348A1/zh

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    • A—HUMAN NECESSITIES
    • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24C—MACHINES FOR MAKING CIGARS OR CIGARETTES
    • A24C5/00—Making cigarettes; Making tipping materials for, or attaching filters or mouthpieces to, cigars or cigarettes
    • A24C5/32—Separating, ordering, counting or examining cigarettes; Regulating the feeding of tobacco according to rod or cigarette condition
    • A24C5/34—Examining cigarettes or the rod, e.g. for regulating the feeding of tobacco; Removing defective cigarettes
    • A24C5/3406—Controlling cigarette combustion
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/02—Devices for withdrawing samples
    • G01N1/22—Devices for withdrawing samples in the gaseous state
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40—Concentrating samples
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/06—Preparation
    • G01N30/08—Preparation using an enricher

Definitions

  • the invention belongs to the technical field of cigarette smoke analysis and detection, and in particular relates to a rotary disk type smoking machine trapping device and a method for analyzing the cigarette smoke by using the same.
  • Cigarette mainstream smoke contains a lot of volatile organic compounds. Of the 44 hazardous ingredients listed in the Health Canada Health Check List, there are five volatile organic compounds: 1,3-butadiene, isoprene, acrylonitrile, benzene and toluene.
  • the carcinogenicity of 1,3-butadiene and isoprene is classified as a possible carcinogen in human body by IARC (2B); benzene is a human carcinogen, and its carcinogenicity is “full of animal experiments and human experimental data” (Group 1); IARC lists acrylonitrile as a carcinogen with "sufficient animal experiments and limited human experimental data”; toluene is irritating to the skin and mucous membranes, has an anesthetic effect on the central nervous system, and may cause cancer in long-term exposure. Therefore, the effective capture and accurate determination of volatile organic compounds in cigarette smoke has practical significance for smoking and health research.
  • a turntable type smoking machine trap apparatus and a method of analyzing the cigarette smoke using the same are provided.
  • the device of the invention has simple operation, good measurement repeatability, less organic solvent consumption, no significant difference between the sample test result and the standard method, and can realize the capture of volatile organic compounds at room temperature, and is suitable for large-volume samples. analysis.
  • the present invention provides a turntable type smoking machine trap device, which includes an adsorption block, The upper cover of the trap, the lower cover of the trap, the inner cavity of the hollow upper cover, the stopper and the Cambridge filter, the inner cover of the upper cover is disposed inside the upper cover of the trap, and the adsorption block is located in the inner cavity of the hollow upper cover.
  • the hollow body is formed inside.
  • the Cambridge filter is disposed at a cross section of the trap upper cover and the inner cavity of the trap lower cover.
  • the inner cavity of the upper cover of the trap is a hollow cavity
  • the adsorption block is located in the inner cavity of the upper cover
  • the lower end of the adsorption block is provided with a stopper.
  • the adsorption block comprises a solid adsorbent material and a sieve plate, wherein the middle portion of the adsorption block is a solid adsorbent material, and the sieve plate is disposed on the upper and lower sides of the solid adsorbent material.
  • the adsorbing material in the adsorption block is an activated carbon material, a magnetic adsorbing material or a molecular sieve material, and the particle diameter is 40-80 mesh; the sieve plate on the upper and lower sides of the adsorbing material is a sand core sieve plate having a pore diameter of 40-60 mesh.
  • the adsorption block may be an adsorption tube
  • the adsorption tube comprises: an outer tube, a adsorption tube adsorption block, a tapered interface and a gasket, wherein the outer tube is a hollow cylinder, and the adsorption tube adsorption block is located inside the outer tube, and the cone type
  • the interface is a hollow cylinder
  • the inner cavity of the inner cavity is tapered
  • the wide end of the inner cavity is connected to one side of the outer tube
  • the gasket is a hollow cylinder, which is located inside the cone-shaped interface and is in close contact with the adsorption block of the adsorption tube.
  • the middle portion of the adsorption tube adsorption block is a solid adsorption material, and the sieve plate is disposed on both sides of the solid adsorption material;
  • the adsorption material is an activated carbon material, a magnetic adsorption material or a molecular sieve material, and the adsorption material has a particle diameter of 40 - 80 ⁇ m, the two side sieve plates of the adsorbent material are sand core sieve plates having a pore size of 40-60 ⁇ m.
  • the present invention provides a method for analyzing volatile organic compounds in cigarette smoke using the above-described rotary type smoking machine trap, the method comprising the steps of:
  • Step 1 Perform sample balance according to the conditions specified in GB/T 16447, and select (the average mass ⁇ 0.02) g and (average suction resistance ⁇ 50) Pa cigarettes for sample testing:
  • Step 2 the carousel type smoking machine trapping device is installed on the smoking machine, and one pump is taken at a time;
  • Step 3 after the collection is completed, the rotary type smoking machine trapping device is removed, and the adsorption block is transferred to a container for extraction treatment;
  • Step 4 installing a blank sample in the rotary type smoking machine trap device, pumping one each time, and repeating step 3, comparing the obtained blank sample processing result with the cigarette sample processing result to analyze the cigarette smoke Volatile organic compounds in the gas.
  • the trapping device is installed on a smoking machine, and suction is performed under the conditions specified by the ISO standard, the suction capacity is 35 mL, the suction time is 2 s, the suction frequency is 60 s, and each suction is performed. 1 branch.
  • the invention provides a smoking machine capture device, the device comprising:
  • the adsorption device can be detachably sealed and connected with the clamping device for holding the cigarette cigarette, and the inside is placed with an adsorbing material for adsorbing substances in the cigarette smoke, such as volatile organic compounds;
  • a trapping chamber having two open ends, one end of which is in sealing communication with the adsorption device so as to enter the flue gas passing through the adsorption device, and the other end is connected to the smoking machine pump;
  • the smoking machine pumps the air, and the smoke of the cigarette smoke enters the adsorption device.
  • the substances in the smoke such as volatile organic compounds, are absorbed by the adsorbent material inside the adsorption device, and the unabsorbed substances are smoked through the trap chamber.
  • the pump is pumped out.
  • the composition and content of the substances in the adsorbent material in the adsorption device are detected, that is, the components of the cigarette smoke are measured.
  • the adsorption device and the trap chamber are arranged in an order from top to bottom, and wherein the trap chamber has a horizontal cross section that is circular.
  • the adsorption device can be detachably sealedly connected to the clamping device of the existing rotary type smoking machine trap.
  • the adsorption device and the trap chamber are integrally or detachably arranged, preferably in a detachable manner.
  • the adsorption device and the complementary chamber are detachably arranged, it is convenient to take out the adsorption device to determine the composition and content of the substance adsorbed therein.
  • a gasket is disposed between the adsorption device and the trap chamber to ensure that the two are in communication while maintaining a seal to the outside.
  • an openable and closable cover is provided on the adsorption device for taking out or replacing the adsorbent material in the adsorption device.
  • the adsorption device is further provided with two sieve plates inside, and the adsorption material placed inside the adsorption device is disposed between the two sieve plates; preferably, the two sieve plates are sand with a diameter of 40-60 ⁇ m. Core sieve plate.
  • the adsorbent material placed inside the adsorption device is a solid adsorbent material, preferably an activated carbon material, a magnetic adsorbent material or a molecular sieve material; preferably, the particle size of the adsorbent material is 40-80 ⁇ m.
  • the adsorption device is internally provided with an adsorption tube, the adsorption tube comprises an outer tube, and the adsorption material is placed inside the outer tube of the adsorption tube.
  • the outer tube of the adsorption tube is further provided with two sieve plates, and the adsorption material is disposed between the two sieve plates; preferably, the two sieve plates are sand core sieves with a diameter of 40-60 ⁇ m. board.
  • the smoking machine trap device further includes a stopper disposed under the adsorption device for abutting against the adsorption device.
  • the smoking machine capture device further comprises a Cambridge filter, the Cambridge filter being disposed inside the capture chamber.
  • the trap chamber has a volume of 10-20 mL, which is a cone chamber, and the narrow end of the cone chamber is in communication with the adsorption device, and the rough end is in communication with the smoking machine pump.
  • the Cambridge filter is disposed on a largest circular cross section of the cone chamber.
  • the present invention provides a method for analyzing volatile organic compounds in cigarette smoke using the aforementioned smoking machine trap, the method comprising the steps of:
  • Step 1 Perform sample balance according to the conditions specified in GB/T 16447, and select (the average mass ⁇ 0.02) g and (average absorption resistance ⁇ 50) Pa cigarettes for sample testing, wherein the average mass and average drag are the same The average of the mass and resistance of the 50 or more cigarettes of the grade;
  • Step 2 the carousel type smoking machine trapping device is installed on the smoking machine, and one pump is taken at a time;
  • Step 3 after the collection is completed, the rotary type smoking machine trapping device is removed, and the adsorption block is transferred to a container for extraction treatment;
  • Step 4 installing a blank sample in the rotary type smoking machine trap device, pumping one each time, and repeating step 3, comparing the obtained blank sample processing result with the cigarette sample processing result to analyze the cigarette smoke Volatile organic compounds in the gas.
  • the trapping device is installed on a smoking machine, and suction is performed under the conditions specified by the ISO standard, the suction capacity is 35 mL, the suction time is 2 s, the suction frequency is 60 s, and each suction is performed. 1 branch.
  • the present invention has at least the following beneficial technical effects:
  • the present invention adopts a novel flue gas trapping device, it is captured in comparison with a conventional absorber device.
  • the lower cover adds a cavity containing the solid adsorbent material, the escape of the flue gas is alleviated, the residence time in the trap is prolonged, and the adsorbent material between the frit plates is a volatile organic compound in the flue gas. It has better adsorption effect, can make the cigarette flue gas flow contact with the adsorbent sufficiently, and ensure the relevant components in the cigarette flue gas can be effectively absorbed, and meet the requirements of volatile organic compound analysis in cigarette flue gas.
  • the adsorption device equipped with the adsorbent material or the adsorption tube provided with the adsorbent material and disposed inside the adsorption device can be directly taken out, so that the adsorption therein can be easily taken out. Material or replace the adsorbent material therein.
  • the Cambridge filter is provided in the flue gas trap of the present invention, since the Cambridge filter is disposed between the adsorbent material and the pump, the cigarette flue gas passes through the adsorbent material and then passes through the Cambridge filter, so the adsorbent material It will fully adsorb volatile organic compounds in the flue gas, and the results will be more accurate.
  • the trap chamber of the present invention is a cone chamber
  • the other end is in communication with the pump because the tapered end of the cone communicates with the adsorbent material.
  • Figure 1 is a schematic view of a carousel type smoking machine trapping device with a lumen.
  • Figure 2 is a schematic diagram of the adsorption block.
  • Fig. 3 is a schematic view of a carousel type smoking machine trapping device with an adsorption tube.
  • Figure 4 is a schematic view of the adsorption tube.
  • Figure 5 is a graph of the suction curve under different volume chambers.
  • Figure 1 shows a carousel type smoking machine trap with a lumen, the device comprising: an adsorption block 1, a trap upper cover 2, a trap lower cover 3, a hollow upper cover inner chamber 4, a stopper 5 and The Cambridge filter 6 is provided with a hollow upper lid inner chamber 4 inside the trap upper cover 3, and the adsorption block 1 is located in the hollow upper lid inner chamber 4.
  • a hollow cavity body is formed inside.
  • a Cambridge filter 6 is disposed in a cross section of the trap upper cover 2 and the inner cavity of the trap lower cover 3.
  • the inner cavity 4 of the hollow upper cover is a hollow cavity, and the adsorption block 1 is located in the inner cavity 4 of the hollow upper cover, and the lower end of the adsorption block 1 is connected to the stopper 5.
  • the adsorption block 1 comprises a solid adsorbent material 11 and a sieve plate 12, wherein the middle of the adsorption block 1 is a solid adsorbent material 11, and the solid adsorbent material 11 is provided with sieve plates 12 on both upper and lower sides.
  • the adsorbing material 11 in the adsorbing block 1 is an activated carbon material, a magnetic adsorbing material or a molecular sieve material, and has a particle diameter of 40-80 mesh; the sieve plate 12 of the upper and lower sides of the adsorbing material 11 is a sand core sieve plate having a pore diameter of 40-60 mesh.
  • a hollow upper cover inner chamber 4 is disposed inside the upper cover 2 of the trap, and the adsorption tube 20 is located in the hollow upper cover inner chamber 4, wherein the adsorption tube 20 comprises: an outer tube 21 and an adsorption tube adsorption block 22
  • the wide mouth end is connected to one side of the outer tube 21, wherein the washer 24 is a hollow cylinder which is located inside the tapered interface 23 and is in close contact with the adsorption tube adsorption block 22.
  • the middle of the adsorption tube adsorption block 22 is a solid adsorption material 221, and the sieve plate 222 is disposed on both sides of the solid adsorption material 221;
  • the adsorption material 221 is an activated carbon material, a magnetic adsorption material or a molecular sieve material.
  • the particle size of the adsorbent material is 40-80 ⁇ m, and the two side sieve plates 222 of the adsorbent material are sand core sieve plates having a pore diameter of 40-60 ⁇ m.
  • the method for analyzing volatile organic compounds in cigarette smoke by using the rotary disk type smoke trap of the present invention includes the following steps:
  • Step 1 processing the cigarette sample, extracting the cigarette sample, performing sample balance according to the conditions specified in the GB/T 16447 standard, and selecting (the average mass ⁇ 0.02) g and the (average suction resistance ⁇ 50) Pa cigarette branch for the sample test;
  • Step 2 Install the turntable type smoking machine trapping device on the smoking machine, and draw one each time;
  • Step 3 after the collection is completed, the collecting device is removed, and the adsorption block 1 is transferred to a container for extraction treatment;
  • step 4 the blank sample is installed in a rotary type smoking machine trap, one pump is taken at a time, and step 3 is repeated, and the obtained blank sample processing result is compared with the cigarette sample processing result to analyze the cigarette smoke. Volatile organic compounds.
  • the column is an InertCap AQUATIC-2 column (length: 60 m, inner diameter: 0.25 mm, film thickness: 1.4 ⁇ m);
  • the temperature programming procedure is: The initial temperature is 40 ° C, maintained for 6.0 min, the temperature rise rate of 20 ° C / min is increased to 230 ° C for 10 min; the carrier gas is helium, the flow rate is 1.5 mL / min; the inlet temperature is 180 ° C, the injection volume is 1.0 ⁇ L, split ratio 10:1; transmission line temperature 230 ° C, ion source temperature 230 ° C, quadrupole temperature 150 ° C; mass spectrometry ionization voltage 70 eV; scanning mode: full scan and selected ion mode simultaneously.
  • Cigarette cigarettes in the cigarette holder During the suction process, the cigarette smoke enters the inner cavity of the upper cover of the trap, and two upper and lower sieve plates with a hole diameter of 20-60 ⁇ m are installed in the cavity, and 40-plates are installed between the two sieve plates.
  • the 80-mesh activated carbon is used as the adsorbent material, and the flue gas is dispersed into a plurality of small gas streams after passing through the upper sieve plate, buffered by the activated carbon material, and then discharged from the lower sieve plate, and the relevant components in the cigarette smoke are effectively absorbed in the process.
  • FIG. 5 This example uses the apparatus shown in Figure 1, in which different trap cavity sizes, such as 10-20 mL, ⁇ 10 mL, > 20 mL, are employed to investigate the effect of the trap cavity size and test results.
  • the result is shown in Figure 5.
  • the size of the trap cavity mainly affects the cigarette suction curve, which in turn affects the test results.
  • the volume of the trap chamber should be as small as possible to meet the processing requirements. It is recommended to limit it to 10-20 ml. If the volume is too large or too small, it will affect the suction curve.
  • the present invention adopts a novel flue gas trapping device, the inner cavity containing the solid adsorbent material is added to the rear cover of the trap as compared with the conventional absorber device, and the escape of the flue gas is alleviated, and the stay in the trap is stopped.
  • the time is prolonged, and the adsorbent material between the sieve plates has a good adsorption effect on the volatile organic compounds in the cigarette smoke, so that the cigarette flue gas flow can be fully contacted with the adsorbent, and the relevant components in the cigarette smoke are effectively ensured. Absorbed to meet the requirements of analysis of volatile organic compounds in cigarette smoke.
  • the detection limits of the five volatile organic compounds ranged from 0.03 ⁇ g/cig to 0.08 ⁇ g/cig; the recoveries ranged from 97.6% to 107.8%.
  • the device of the invention has the advantages of simple operation, good measurement repeatability, low consumption of organic solvent, no significant difference between the test results of the sample and the standard method, and the realization of the capture of volatile organic compounds at room temperature, and is suitable for analysis of large quantities of samples. .

Abstract

一种转盘型吸烟机捕集装置及使用该装置分析卷烟烟气的方法。该装置包括：吸附块（1）、捕集器上盖（2）、捕集器下盖（3）、中空上盖内腔（4）、档塞（5）和剑桥滤片（6），捕集器上盖（2）内部设置中空上盖内腔（4），吸附块（1）位于中空上盖内腔（4）中。本装置操作简便，并且测定重复性好，有机溶剂消耗量少，样品测试结果与标准方法无显著差异，且能在室温下实现对挥发性有机化合物的捕集，适用于大批量样品的分析。

Description

一种转盘型吸烟机捕集装置及使用该装置分析卷烟烟气的方法 技术领域
本发明属于卷烟烟气分析检测技术领域，尤其是涉及一种转盘型吸烟机捕集装置及使用该装置分析卷烟烟气的方法。
背景技术
随着吸烟与健康研究的深入开展，人们对卷烟烟气中的有害成分越来越关注。卷烟主流烟气中含有大量挥发性有机化合物。加拿大卫生部关注的检测名单列出的44种有害成分中，挥发性有机化合物有5种：1,3-丁二烯、异戊二烯、丙烯腈、苯和甲苯。1,3-丁二烯和异戊二烯的致癌性被IARC列为人体可能致癌物(2B)；苯为人体致癌物，其致癌性为“动物实验和人体实验数据充分”(Group1)；IARC把丙烯腈则列为“动物实验充分而人体实验数据有限”的致癌物；甲苯对皮肤和粘膜有刺激性，对中枢神经系统有麻醉作用，长期接触也可能致癌。因此，卷烟烟气中的挥发性有机化合物的有效捕集和准确测定对吸烟与健康研究具有现实意义。目前，已有许多采用GC-MS测定卷烟烟气中挥发性有机化合物的报道，主要采用冷溶液吸收法(-70℃左右的甲醇)和吸附管法进行捕集。冷溶液吸收法采用两个串联的装有15mL冷甲醇的收集瓶捕集，操作繁琐。吸附管法，吸烟机抽吸通道“死体积”和压降较大，测试结果重现性较差。
发明内容
为了克服现有技术的缺陷，提供一种转盘型吸烟机捕集装置及使用该装置分析卷烟烟气的方法。本发明的装置操作简便，并且测定重复性好，有机溶剂消耗量少，样品测试结果与标准方法无显著差异，且能在室温下实现对挥发性有机化合物的捕集，适用于大批量样品的分析。
本发明的上述目的是采用如下技术方案来实现的。
一方面，本发明提供一种转盘型吸烟机捕集装置，该装置包括吸附块、 捕集器上盖、捕集器下盖、中空上盖内腔、档塞和剑桥滤片，捕集器上盖内部设置中空上盖内腔，吸附块位于中空上盖内腔中。
优选地，捕集器上盖与捕集器下盖连接后，内部形成中空腔体。
优选地，剑桥滤片设置在捕集器上盖与捕集器下盖内部腔体的横截面处。
优选地，捕集器上盖内腔为中空腔体，吸附块位于上盖内腔中，吸附块下端设置档塞。
优选地，吸附块包括固体吸附材料、筛板，其中，吸附块中部为固体吸附材料，固体吸附材料上下两面设置筛板。
优选地，吸附块中吸附材料为活性炭材料、磁性吸附材料或分子筛材料，其粒径为40-80目；吸附材料上下两面的筛板为孔径40-60目的砂芯筛板。
优选地，吸附块可以为吸附管，所述吸附管包括：外管、吸附管吸附块、锥型接口和垫圈，其中，外管为中空圆柱体，吸附管吸附块位于外管内部，锥型接口为中空圆柱体，其内部中空腔为锥型，其内腔宽口端连接外管一侧，其中，垫圈为中空圆柱体，其位于锥型接口内部，并贴紧吸附管吸附块。
优选地，吸附管中，吸附管吸附块中部为固体吸附材料，固体吸附材料两侧设置筛板；所述吸附材料为活性炭材料、磁性吸附材料或分子筛材料，所述吸附材料的粒径为40-80μm，所述吸附材料的所述两个侧筛板为孔径40-60μm的砂芯筛板。
另一方面，本发明提供一种使用上述的转盘型吸烟机捕集装置分析卷烟烟气中的挥发性有机化合物的方法，该方法包括以下步骤：
步骤1，按照GB/T 16447标准规定条件进行样品平衡，挑选(平均质量±0.02)g与(平均吸阻±50)Pa的烟支用于样品测试：
步骤2，将所述转盘型吸烟机捕集装置安装在吸烟机上，每次抽吸1支；
步骤3，捕集完后取下所述转盘型吸烟机捕集装置，将所述吸附块转移至容器内进行萃取处理；和
步骤4，将空白样品安装在所述转盘型吸烟机捕集装置中，每次抽吸1支，并重复步骤3，将获得的空白样品处理结果与卷烟样品处理结果进行对照，以分析卷烟烟气中的挥发性有机化合物。
优选地，在所述步骤2中，将所述捕集装置安装在吸烟机上，在ISO标准规定条件下进行抽吸，抽吸容量35mL，抽吸时间2s，抽吸频率60s，每次抽吸1支。
本发明的技术方案也可以描述如下：
一方面，本发明提供一种吸烟机捕集装置，该装置包括：
吸附装置，可以与用于夹持卷烟烟支的夹持装置可拆卸式密封连通，内部放置有吸附材料，用于吸附卷烟烟气中的物质，例如挥发性有机化合物；
具有两个开口端的捕集腔，一端与所述吸附装置密封连通，以便经过所述吸附装置的烟气进入，另一端与吸烟机泵相连通；
运行时，吸烟机泵抽气，卷烟烟支的烟气进入吸附装置，烟气中的物质，例如挥发性有机化合物被吸附装置内部的吸附材料吸收，未被吸收的物质通过捕集腔被吸烟机泵抽出。检测吸附装置内吸附材料中的物质的成分及含量，即测出卷烟烟气的成分。
优选地，所述吸附装置和所述捕集腔以由上往下的顺序设置，且其中所述捕集腔的水平横截面为圆形。
优选地，所述吸附装置可以与现有的转盘型吸烟机捕集装置的夹持装置可拆卸式密封连接。
优选地，所述吸附装置和所述捕集腔为一体式设置或者可拆卸式设置，优选为可拆卸式设置。当所述吸附装置和补集腔为可拆卸式设置时，便于将吸附装置取出，以测定其中吸附的物质的成分及含量。
优选地，当所述吸附装置和捕集腔为可拆卸式设置时，所述吸附装置和捕集腔之间设置有垫圈，以保证二者在连通的同时，对外界保持密封。
优选地，当所述吸附装置和捕集腔为一体式设置时，在吸附装置上设置有可打开和封闭的盖，用于取出或者更换所述吸附装置中的吸附材料。
优选地，所述吸附装置内部还设置有两个筛板，吸附装置内部放置的吸附材料设置在所述两个筛板之间；优选地，所述两个筛板为孔径40-60μm的砂芯筛板。
优选地，所述吸附装置内部放置的吸附材料为固体吸附材料，优选为活性炭材料、磁性吸附材料或分子筛材料；优选地，所述吸附材料的粒径为 40-80μm。
优选地，所述吸附装置内部设置有吸附管，该吸附管包括外管，吸附材料放置在所述吸附管的外管内部。采用该吸附管形式时，在更换或者取吸附材料时，可以将吸附管直接取出，更为方便。优选地，所述吸附管的外管内部还设置有两个筛板，吸附材料设置在所述两个筛板之间；优选地，所述两个筛板为孔径40-60μm的砂芯筛板。
优选地，所述吸烟机捕集装置还包括档塞，设置在所述吸附装置下方，用于抵住所述吸附装置。
优选地，所述吸烟机捕集装置还包含剑桥滤片，所述剑桥滤片设置在所述捕集腔内部。
优选地，所述捕集腔体积为10～20mL，为锥体腔室，该锥体腔室细口端与吸附装置连通，粗口端与吸烟机泵连通。优选地，所述剑桥滤片设置在所述锥体腔室的最大圆截面上。
另一方面，本发明提供一种使用前述的吸烟机捕集装置分析测试卷烟烟气中挥发性有机化合物的方法，该方法包括以下步骤：
步骤1，按照GB/T 16447标准规定条件进行样品平衡，挑选(平均质量±0.02)g与(平均吸阻±50)Pa的烟支用于样品测试，其中平均质量和平均吸阻为同一种牌号的50支以上的卷烟的质量和吸阻的平均值；
步骤2，将所述转盘型吸烟机捕集装置安装在吸烟机上，每次抽吸1支；
步骤3，捕集完后取下所述转盘型吸烟机捕集装置，将所述吸附块转移至容器内进行萃取处理；和
步骤4，将空白样品安装在所述转盘型吸烟机捕集装置中，每次抽吸1支，并重复步骤3，将获得的空白样品处理结果与卷烟样品处理结果进行对照，以分析卷烟烟气中的挥发性有机化合物。
优选地，在所述步骤2中，将所述捕集装置安装在吸烟机上，在ISO标准规定条件下进行抽吸，抽吸容量35mL，抽吸时间2s，抽吸频率60s，每次抽吸1支。
与现有技术相比，本发明至少具有以下有益的技术效果：
1、由于本发明采用新型烟气捕集装置，与常规的吸收装置相比在捕集 器下盖增加了装有固体吸附材料的内腔，烟气的逸出得到缓和，在捕集器中的停留时间延长，而且筛板之间的吸附材料对卷烟烟气中的挥发性有机化合物具有较好的吸附效果，可以使卷烟烟气气流与吸附剂接触充分，保证卷烟烟气中的相关成分得到有效吸收，满足卷烟烟气中挥发性有机化合物分析的要求。
2、当本发明的烟气捕集装置采用可拆卸式时，装有吸附材料的吸附装置或者装有吸附材料的、设置在吸附装置内部的吸附管可以被直接取出，这样方便取出其中的吸附材料或者更换其中的吸附材料。
3、当本发明的烟气捕集装置中设置有剑桥滤片时，由于剑桥滤片设置在吸附材料与泵之间，卷烟烟气先经过吸附材料，再经过剑桥滤片，因此，吸附材料会全面吸附烟气中的挥发性有机物，从而测定的结果更准确。
4、当本发明的捕集腔为锥体腔室时，由于锥体细口端与吸附材料连通，另一端与泵连通。采用这样的结构，通过吸附材料的烟气会在锥体内缓冲一下，然后经过剑桥滤片，再被抽走，而不会直接穿透剑桥滤片。
附图说明
图1为带内腔的转盘型吸烟机捕集装置示意图。
图2为吸附块示意图。
图3为带吸附管的转盘型吸烟机捕集装置示意图。
图4为吸附管示意图。
图5为不同体积腔体下的抽吸曲线图。
具体实施方式
下面结合附图和具体实施例对本发明提供的一种带内腔的转盘型吸烟机捕集装置进行详细描述。
图1示出带有内腔的转盘型吸烟机捕集装置，该装置包括：吸附块1、捕集器上盖2、捕集器下盖3、中空上盖内腔4、档塞5和剑桥滤片6，捕集器上盖3内部设置中空上盖内腔4，吸附块1位于中空上盖内腔4中。
捕集器上盖2与捕集器下盖3连接后，内部形成中空腔体。
捕集器上盖2与捕集器下盖3内部腔体的横截面设置有剑桥滤片6。
中空上盖内腔4为中空腔体，吸附块1位于中空上盖内腔4中，吸附块1下端连接档塞5。
图2示出吸附块1包括固体吸附材料11、筛板12，其中，吸附块1中部为固体吸附材料11，固体吸附材料11上下两面设置筛板12。
吸附块1中吸附材料11为活性炭材料、磁性吸附材料或分子筛材料，其粒径为40-80目；吸附材料11上下两面的筛板12为孔径40-60目的砂芯筛板。
图3示出，捕集器上盖2内部设置中空上盖内腔4，吸附管20位于中空上盖内腔4中，其中，所述吸附管20包括：外管21、吸附管吸附块22、锥型接口23和垫圈24，其中，外管21为中空圆柱体，吸附管吸附块22位于外管21内部，锥型接口23为中空圆柱体，其内部中空腔为锥型，其内腔宽口端连接外管21一侧，其中，垫圈24为中空圆柱体，其位于锥型接口23内部，并贴紧吸附管吸附块22。
图4示出，吸附管20中，吸附管吸附块22中部为固体吸附材料221，固体吸附材料221两侧设置筛板222；所述吸附材料221为活性炭材料、磁性吸附材料或分子筛材料，所述吸附材料的粒径为40-80μm，所述吸附材料的所述两个侧筛板222为孔径40-60μm的砂芯筛板。
应用本发明带有内腔的转盘型吸烟机烟气捕集器分析测试卷烟烟气中的挥发性有机化合物的方法包括以下步骤：
步骤1，卷烟样品的处理，抽取卷烟样品，按照GB/T 16447标准规定条件进行样品平衡，挑选(平均质量±0.02)g与(平均吸阻±50)Pa的烟支用于样品测试；
步骤2，将转盘型吸烟机捕集装置安装在吸烟机上，每次抽吸1支；
步骤3，捕集完后取下捕集装置，将吸附块1转移至容器内进行萃取处理；
步骤4，将空白样品安装在转盘型吸烟机捕集装置中，每次抽吸1支，并重复步骤3，将获得的空白样品处理结果与卷烟样品处理结果进行对照，以分析卷烟烟气中的挥发性有机化合物。
根据本发明的分析测试方法的色谱/质谱(GC/MS)仪器条件：色谱柱为InertCap AQUATIC-2色谱柱(长度：60m，内径：0.25mm，膜厚：1.4μm)；程序升温程序为：初始温度为40℃，保持6.0min，20℃/min的升温速率升温至230℃，保持10min；载气为氦气，流速为1.5mL/min；进样口温度为180℃，进样体积为1.0μL，分流比为10:1；传输线温度230℃，离子源温度230℃，四极杆温度150℃；质谱离子化电压为70eV；扫描方式：全扫描和选择离子模式同时进行。
本发明在用于烟气分析时的工作过程为：
卷烟夹持器内的卷烟烟支在抽吸过程中，卷烟烟气进入捕集器上盖内腔体，腔内安装有孔径20～60μm上下两个筛板，两筛板之间装40～80目的活性炭作为吸附材料，烟气经过上筛板后分散为多股小气流，经活性碳材料缓冲，再由下筛板流出，在此过程中卷烟烟气中的相关成分被有效吸收。下置的剑桥滤片对其它的卷烟烟气粒相物进行截留。
各化合物的定量及定性离子如下表1所示：
表1各目标化合物的保留时间、定量及定性离子
Figure PCTCN2015076486-appb-000001
实施例1：
选取牌号A卷烟，按照GB/T 16447标准规定条件进行样品平衡，挑选(平均质量±0.02)g与(平均吸阻±50)Pa的烟支用于样品测试。将准备好的捕集器安装在吸烟机上，在ISO标准规定条件下进行抽吸，抽吸容量35.0mL，抽吸时间2s，抽吸频率60s。每次抽吸1支；捕集完后取下捕集器， 将吸附材料和前后筛板转移至相应容器进行萃取处理；同样的过程制作空白样品。结果如表2所示。
表2牌号A卷烟中挥发性有机化合物的测定结果-ISO模式
化合物 1,3-丁二烯 异戊二烯 丙烯腈 苯 甲苯
含量(μg/cig) 37.8 312.3 7.3 40.6 78.1
RSD(％)n＝5 3.9 2.7 4.1 4.5 2.6
实施例2：
选取牌号B卷烟，按照GB/T 16447标准规定条件进行样品平衡，挑选(平均质量±0.02)g与(平均吸阻±50)Pa的烟支用于样品测试。将准备好的捕集器安装在吸烟机上，在加拿大深度抽吸(HCI)标准规定条件下进行抽吸，抽吸容量55.0mL，抽吸时间2s，抽吸频率30s。每次抽吸1支；捕集完后取下捕集器，将吸附材料和前后筛板转移至相应容器进行萃取处理；同样的过程制作空白样品。结果如表3所示。
表3牌号B卷烟中挥发性有机化合物的测定结果-HCI
化合物 1,3-丁二烯 异戊二烯 丙烯腈 苯 甲苯
含量(μg/cig) 92.6 751.8 27.1 108.8 199.5
RSD(％) 3.1 2.6 3.7 2.4 1.5
实施例3：
选取牌号C卷烟，按照GB/T 16447标准规定条件进行样品平衡，挑选(平均质量±0.02)g与(平均吸阻±50)Pa的烟支用于样品测试。分别采用采用本发明的装置(剑桥滤片设置在吸附材料和泵之间，图1所示的装置)和吸附材料设置在剑桥滤片和泵之间的装置在ISO标准规定条件下进行抽吸，抽吸容量35mL，抽吸时间2s，抽吸频率60s，每次抽吸1支。卷烟抽吸捕集完成后取下捕集器，将吸附材料和前后筛板转移至相应容器进行萃取处理。比较两种装置的技术效果。结果见下表4。
表4应用两种装置测试挥发性有机化合物的效果比较
  1,3-丁二烯 异戊二烯 丙烯腈 苯 甲苯
本发明装置(μg/cig) 62.0 537.6 12.4 70.7 90.3
吸附设置在滤片后(μg/cig) 58.6 533.3 11.6 69.1 88.6
偏差(％) 2.8 0.4 3.1 1.2 1.0
上表的结果表明本发明将剑桥滤片设置在吸附材料和泵之间的装置具有相对较好的的吸附效果。
实施例4：
本实施例使用了图1所示的装置，其中，采用了不同的捕集器腔体大小，例如10-20mL，<10mL，>20mL，研究了捕集器腔体大小与测试结果的影响。结果如图5所示。根据该图5可知，捕集器腔体的大小主要影响卷烟抽吸曲线，进而对测试结果造成影响，捕集腔体积应在满足加工需求的前提下越小越好，建议限定在10～20ml之间，体积过大或过小均会对抽吸曲线产生影响。
由于本发明采用新型烟气捕集装置，与常规的吸收装置相比在捕集器后盖增加了装有固体吸附材料的内腔，烟气的逸出得到缓和，在捕集器中的停留时间延长，而且筛板之间的吸附材料对卷烟烟气中的挥发性有机化合物具有较好的吸附效果，可以使卷烟烟气气流与吸附剂接触充分，保证卷烟烟气中的相关成分得到有效吸收，满足卷烟烟气中挥发性有机化合物分析的要求。5种挥发性有机化合物的检出限在0.03μg/cig～0.08μg/cig；回收率在97.6％～107.8％之间。本发明装置操作简便，并且测定重复性好，有机溶剂消耗量少，样品测试结果与标准方法无显著差异，且能在室温下实现对挥发性有机化合物的捕集，适用于大批量样品的分析。
最后应说明的是，以上实施例仅用以描述本发明的技术方案而不是对本技术方法进行限制，本发明在应用上可以延伸为其他的修改、变化、应用和实施例，并且因此认为所有这样的修改、变化、应用、实施例都在本发明的精神和教导范围内。

Claims (9)

  1. 一种转盘型吸烟机捕集装置，该装置包括吸附块(1)、捕集器上盖(2)、捕集器下盖(3)、中空上盖内腔(4)、档塞(5)和剑桥滤片(6)，其特征在于，所述捕集器上盖(2)内部设置中空上盖内腔(4)，所述吸附块(1)位于所述中空上盖内腔(4)中。
  2. 根据权利要求1所述的转盘型吸烟机捕集装置，其特征在于，所述捕集器上盖(2)与所述捕集器下盖(3)连接后，内部形成中空腔体。
  3. 根据权利要求2所述的转盘型吸烟机捕集装置，其特征在于，所述剑桥滤片(6)设置在所述捕集器上盖(2)与所述捕集器下盖(3)形成的中空腔体的横截面处。
  4. 根据权利要求1或3所述的转盘型吸烟机捕集装置，其特征在于，所述吸附块(1)下端设置档塞(5)。
  5. 根据权利要求4所述的转盘型吸烟机捕集装置，其特征在于，所述吸附块(1)包括固体吸附材料(11)、筛板(12)，其中，所述吸附块(1)中部为固体吸附材料(11)，固体吸附材料(11)上下两面设置筛板(12)。
  6. 根据权利要求5所述的转盘型吸烟机捕集装置，其特征在于，所述吸附块(1)中吸附材料(11)为活性炭材料、磁性吸附材料或分子筛材料，其粒径为40-80目；吸附材料(11)上下两面的筛板(12)为孔径40-60目的砂芯筛板。
  7. 根据权利要求1所述的转盘型吸烟机捕集装置，其特征在于，所述吸附块(1)为吸附管(20)，所述吸附管(20)包括：外管(21)、吸附管吸附块(22)、锥型接口(23)和垫圈(24)，其中，外管(21)为中空圆柱体，吸附管吸附块(22)位于外管(21)内部，锥型接口(23)为中空圆柱体，其内部中空腔为锥型，其内腔宽口端连接外管(21)一侧，其中，垫圈(24)为中空圆柱体，其位于锥型接口(23)内部，并贴紧吸附管吸附块(22)。
  8. 根据权利要求7所述的带内腔的转盘型吸烟机捕集装置，其特征在于，吸附管(20)中，吸附管吸附块(22)中部为固体吸附材料(221)，固体吸附材料(221)两侧设置筛板(222)；所述吸附材料(221)为活性炭材 料、磁性吸附材料或分子筛材料，所述吸附材料的粒径为40-80μm，所述吸附材料的所述两个侧筛板(222)为孔径40-60μm的砂芯筛板。
  9. 一种使用权利要求1至8中任一项所述的转盘型吸烟机捕集装置分析卷烟烟气中的挥发性有机化合物的方法，该方法包括以下步骤：
    步骤1，按照GB/T 16447标准规定条件进行样品平衡，挑选(平均质量±0.02)g与(平均吸阻±50)Pa的烟支用于样品测试：
    步骤2，将所述转盘型吸烟机捕集装置安装在吸烟机上，每次抽吸1支；
    步骤3，捕集完后取下所述转盘型吸烟机捕集装置，将所述吸附块转移至容器内进行萃取处理；和
    步骤4，将空白样品安装在所述转盘型吸烟机捕集装置中，每次抽吸1支，并重复步骤3，将获得的空白样品处理结果与卷烟样品处理结果进行对照，以分析卷烟烟气中的挥发性有机化合物。
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