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CN108490097A - A kind of detection method of the volatile organic compounds burst size of nanometer of filter tip - Google Patents

A kind of detection method of the volatile organic compounds burst size of nanometer of filter tip Download PDF

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CN108490097A
CN108490097A CN201810470152.6A CN201810470152A CN108490097A CN 108490097 A CN108490097 A CN 108490097A CN 201810470152 A CN201810470152 A CN 201810470152A CN 108490097 A CN108490097 A CN 108490097A
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temperature
filter
heating chamber
smoke
air
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王晋
陈章玉
李天飞
李晶
张承明
孔维松
刘欣
李雪梅
许�永
黄海涛
杨光宇
杨叶昆
陈建华
耿永勤
张涛
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China Tobacco Yunnan Industrial Co Ltd
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China Tobacco Yunnan Industrial Co Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/06Preparation

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
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  • General Health & Medical Sciences (AREA)
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  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)

Abstract

本发明涉及一种纳米滤嘴的挥发性有机化合物释放量的检测方法,包括如下步骤:步骤(1)、抽吸口数确定;步骤(2)、根据抽吸口数设定所需加热腔的温度;步骤(3)、抽吸;步骤(4)、纳米滤嘴中成分分析。本发明避免了复杂的背景干扰,测定结果的精密度和准确性显著提高。本发明结构简单,操作方便,减少复杂烟气的影响,可作为纳米滤嘴的挥发性有机化合物释放量的新的分析方法。

The invention relates to a method for detecting the release of volatile organic compounds from a nano filter, comprising the following steps: step (1), determining the number of suction ports; step (2), setting the temperature of the required heating chamber according to the number of suction ports ; Step (3), suction; Step (4), component analysis in the nano-filter. The invention avoids complex background interference, and the precision and accuracy of the measurement results are significantly improved. The invention has the advantages of simple structure, convenient operation and reduced influence of complex smoke, and can be used as a new analysis method for the emission of volatile organic compounds of the nanometer filter.

Description

一种纳米滤嘴的挥发性有机化合物释放量的检测方法A method for detecting the emission of volatile organic compounds from nano-filters

技术领域technical field

本发明涉及一种挥发性有机化合物释放量的检测方法,具体涉及一种纳米滤嘴的挥发性有机化合物释放量的检测方法,属于烟用辅料的理化检验领域。The invention relates to a method for detecting the release amount of volatile organic compounds, in particular to a method for detecting the release amount of volatile organic compounds of a nano-filter, and belongs to the field of physical and chemical inspection of cigarette auxiliary materials.

背景技术Background technique

挥发性有机化合物(Volatile Organic Compounds,VOCs)是指沸点在50~260 ℃之间、室温下饱和蒸气压超过133.32 Pa 的易挥发性化合物。挥发性有机化合物的存在不仅存在安全风险,含量过高时也会对卷烟的抽吸品质产生不良影响。因此。对滤嘴的挥发性有机化合物进行定量分析,无论是在安全性评价还是品质控制方面都有着重要的意义。Volatile Organic Compounds (Volatile Organic Compounds, VOCs) refer to volatile compounds with a boiling point between 50 and 260 °C and a saturated vapor pressure exceeding 133.32 Pa at room temperature. The existence of volatile organic compounds not only poses safety risks, but also has adverse effects on the smoking quality of cigarettes when the content is too high. therefore. Quantitative analysis of volatile organic compounds in filters is of great significance both in safety evaluation and quality control.

目前纳米滤嘴添加成分向卷烟烟气中迁移的测试方法通常采用吸烟机抽吸卷烟,再捕集烟气成分进行分析。由于卷烟燃烧时产生非常复杂的背景,会对纳米滤嘴迁移成分的测定造成严重干扰,其成分的测定非常困难,分析结果的误差也非常大。如何真实准确的对纳米滤嘴安全性成分进行准确的分析和检测成为烟草分析研究的重点。At present, the test method for the migration of the added components of the nano-filter into the cigarette smoke usually uses a smoking machine to suck the cigarette, and then capture the components of the smoke for analysis. Due to the very complex background generated when the cigarette is burned, it will seriously interfere with the determination of the migration components of the nano-filter, the determination of its components is very difficult, and the error of the analysis results is also very large. How to truly and accurately analyze and detect the safety components of nano-filters has become the focus of tobacco analysis research.

发明内容Contents of the invention

为了解决上述技术问题,本发明的目的在于提供一种纳米滤嘴的挥发性有机化合物释放量的检测方法。In order to solve the above-mentioned technical problems, the object of the present invention is to provide a method for detecting the emission of volatile organic compounds from nano-filters.

本发明目的通过下列技术方案予以实现:The object of the invention is achieved through the following technical solutions:

一种纳米滤嘴的挥发性有机化合物释放量的检测方法,其特征在于:A method for detecting the emission of volatile organic compounds from a nano-filter, characterized in that:

包括如下步骤:Including the following steps:

步骤(1)、抽吸口数确定Step (1), determine the number of suction ports

在待测卷烟的含有纳米滤嘴的远唇端加料起始部位插入测温探针,在常规吸烟机上抽吸,通过测温探针测定每口抽吸时通过纳米滤嘴起始部位烟气的温度,并确定整支卷烟的抽吸口数;Insert a temperature measuring probe at the starting part of the far lip end of the cigarette to be tested that contains nano-filters, smoke on a conventional smoking machine, and use the temperature-measuring probe to measure the smoke that passes through the starting part of the nano-filter during each puff. temperature and determine the number of puffs for the whole cigarette;

步骤(2)、根据抽吸口数设定所需加热腔的温度Step (2), set the temperature of the required heating chamber according to the number of suction ports

按卷烟实际抽吸温度设定检测装置的若干加热腔中的空气温度,并设定抽吸口数,抽吸口数为7-8口,空气温度为36-51℃;Set the air temperature in several heating chambers of the detection device according to the actual smoking temperature of the cigarette, and set the number of suction ports, the number of suction ports is 7-8, and the air temperature is 36-51°C;

步骤(3)、抽吸Step (3), suction

将吸烟机、烟气捕集器和滤嘴夹持器依次连接,把纳米滤嘴卷烟的过滤嘴从卷烟上取下,安装到滤棒夹持器上,启动吸烟机按标准条件抽吸,抽吸的空气来自不同温度的加热腔,根据抽吸口数依次切换,每口抽吸通过过滤嘴的气流温度均和卷烟吸烟机实际抽吸时的气流温度一致;烟气捕集器采用三乙胺-甲醇混合溶液进行捕集气流;Connect the smoking machine, the smoke trap and the filter holder in sequence, remove the filter tip of the nano-filter cigarette from the cigarette, install it on the filter rod holder, start the smoking machine and smoke according to the standard conditions. The air sucked comes from heating chambers of different temperatures, which are switched in turn according to the number of suction ports. The temperature of the airflow through the filter tip is consistent with the actual airflow temperature of the cigarette smoking machine; the smoke trap adopts triethylamine- The mixed solution of methanol is used to capture the air flow;

步骤(4)、成分分析Step (4), component analysis

对捕集液进行顶空-气质分析。Headspace-gas-gas analysis was performed on the trapping fluid.

进一步地,使用芳香胺释放量的检测装置进行检测,所述检测装置包括若干加热腔,加热腔一端连接进气口,另一端连接出气管,出气管围绕转盘设置,转盘上包括第一进气管,第一进气管随转盘转动,第一进气管一端在某一时刻与其中一个出气管连通,第一进气管另一端与第二进气管一端连通,第二进气管固定,另一端与滤嘴夹持器连接,滤嘴夹持器连接烟气捕集器,烟气捕集器连接吸烟机。Further, a detection device for release of aromatic amines is used for detection, the detection device includes several heating chambers, one end of the heating chamber is connected to the air inlet, and the other end is connected to the air outlet pipe, the air outlet pipe is arranged around the turntable, and the first air inlet pipe is included on the turntable , the first air intake pipe rotates with the turntable, one end of the first air intake pipe communicates with one of the air outlet pipes at a certain moment, the other end of the first air intake pipe communicates with one end of the second air intake pipe, the second air intake pipe is fixed, and the other end is connected with the filter The holder is connected, the filter holder is connected with the smoke trap, and the smoke catcher is connected with the smoking machine.

进一步地,加热腔为10个,加热腔上均设有温度调节装置,加热温度范围为30-200℃。Further, there are 10 heating chambers, each of which is equipped with a temperature regulating device, and the heating temperature range is 30-200°C.

进一步地,步骤(4)中,色谱条件:60 m×0.32 mm×1μm DB-5MS柱;载气:氦气;进样量3μL;进样口温度220 ℃;分流比15:1;柱温箱温度40 ℃;载气流速1 ml/min;程序升温:从40 ℃保持6 min,然后以10 ℃/min 的速率升至160 ℃,保持3 min,最后以20 ℃/min 的速率升至220 ℃,保持3 min。Further, in step (4), chromatographic conditions: 60 m×0.32 mm×1 μm DB-5MS column; carrier gas: helium; injection volume 3 μL; inlet temperature 220 °C; split ratio 15:1; column temperature Oven temperature 40 °C; carrier gas flow rate 1 ml/min; temperature program: keep at 40 °C for 6 min, then increase to 160 °C at a rate of 10 °C/min, maintain for 3 min, and finally increase at a rate of 20 °C/min to 220°C, keep for 3 minutes.

进一步地,步骤(4)中,质谱条件:电离方式EI,电离能量70 eV,传输线温度200℃,离子源温度240 ℃,溶剂延迟时间3 min,扫描范围:m/z 40.0-200.0。Further, in step (4), mass spectrometry conditions: ionization mode EI, ionization energy 70 eV, transfer line temperature 200 °C, ion source temperature 240 °C, solvent delay time 3 min, scan range: m/z 40.0-200.0.

进一步地,步骤(3)中,三乙胺用量为50 ml,甲醇用量为20ml。Further, in step (3), the amount of triethylamine used is 50 ml, and the amount of methanol used is 20 ml.

与现有技术相比,本发明具有以下有益效果:Compared with the prior art, the present invention has the following beneficial effects:

(1)、本发明的检测装置设置若干加热腔,设置不同的温度,可以非常好的人体口腔的抽吸温度,避免常规的温度一致不能真实反映口腔抽吸温度的情形,设置转盘,操作方便,容易切换,减少复杂烟气的影响,使得挥发性有机化合物的测定变得非常容易。(1) The detection device of the present invention is equipped with several heating chambers and different temperatures, which can improve the suction temperature of the human oral cavity, avoiding the situation that the conventional temperature cannot truly reflect the suction temperature of the oral cavity, and is equipped with a turntable, which is easy to operate , easy to switch, reducing the influence of complex flue gas, making the determination of volatile organic compounds very easy.

(2)、本发明采用净化空气流进行洗脱,消除了实际卷烟燃烧过程中产生的复杂烟气成分背景干扰,测定结果的精密度和准确性显著提高,且测试周期缩短15分钟左右。(2) The present invention adopts purified air flow for elution, which eliminates the background interference of complex smoke components generated in the actual cigarette burning process, significantly improves the precision and accuracy of the measurement results, and shortens the test period by about 15 minutes.

(3)、采用简单的顶空或溶剂提取就可直接进行分析;避免了常规纳米滤嘴成分向烟气迁移分析检测中的复杂样品净化和富集操作。(3) Simple headspace or solvent extraction can be used for direct analysis; it avoids the complicated sample purification and enrichment operations in the analysis and detection of conventional nano-filter component migration to flue gas.

附图说明Description of drawings

图1为本发明的检测装置的结构示意图;Fig. 1 is the structural representation of detection device of the present invention;

图1中:I为转盘;II为滤嘴夹持器;III为烟气捕集器;IV为吸烟机;V为空气入口;In Figure 1: I is the turntable; II is the filter holder; III is the smoke trap; IV is the smoking machine; V is the air inlet;

1-第一连通口,1’-第一加热腔;2-第二连通口,2’-第二加热腔;3-第三连通口,3’-第三加热腔;4-第四连通口,4’-第四加热腔;5-第五连通口,5’-第五加热腔;6-第六连通口,6’-第六加热腔;7-第七连通口,7’-第七加热腔;8-第八连通口,8’-第八加热腔;9-第九连通口,9’-第九加热腔;10-第十连通口,10’-第十加热腔;11-第一进气管;12-第二进气管。1-the first communication port, 1'-the first heating chamber; 2-the second communication port, 2'-the second heating chamber; 3-the third communication port, 3'-the third heating chamber; 4-the fourth communication 4'-the fourth heating chamber; 5-the fifth communication port, 5'-the fifth heating chamber; 6-the sixth communication port, 6'-the sixth heating chamber; 7-the seventh communication port, 7'- Seventh heating chamber; 8-eighth communication port, 8'-eighth heating chamber; 9-ninth communication port, 9'-ninth heating chamber; 10-tenth communication port, 10'-tenth heating chamber; 11-the first air intake pipe; 12-the second air intake pipe.

具体实施方式Detailed ways

下面结合附图和实施例对本发明作进一步的详细说明,但不以任何方式对本发明加以限制,基于本发明教导所做的任何变换或改进,均落入本发明的保护范围。实施例中未注明具体技术或条件者,按照本领域内的文献所描述的技术或条件或者按照产品说明书进行。所用材料或设备未注明生产厂商者,均为可以通过购买获得的常规产品。The present invention will be described in further detail below in conjunction with the accompanying drawings and examples, but the present invention is not limited in any way, and any changes or improvements based on the teachings of the present invention fall within the protection scope of the present invention. If no specific technique or condition is indicated in the examples, it shall be carried out according to the technique or condition described in the literature in this field or according to the product specification. The materials or equipment used are not indicated by the manufacturer, and they are all conventional products that can be obtained through purchase.

实施例1Example 1

本实施例的挥发性有机化合物释放量的检测装置,包括第一加热腔1’、第二加热腔2’、第三加热腔3’、第四加热腔4’、第五加热腔5’、第六加热腔6’、第七加热腔7’、第八加热腔8’、第九加热腔9’、第十加热腔10’,每个加热腔一端均连接进气口,另一端连接出气管,出气管围绕转盘I设置,形成围绕转盘I设置的第一连通口1、第二连通口2、第三连通口3、第四连通口4、第五连通口5、第六连通口6、第七连通口7、第八连通口8、第九连通口9、第十连通口10,转盘I上包括第一进气管11,第一进气管11随转盘I转动,第一进气管11一端在某一时刻与其中一个连通口连通,第一进气管11另一端与第二进气管12一端连通,第二进气管12固定,第二进气管12另一端与滤嘴夹持器II连接,滤嘴夹持器II连接烟气捕集器III,烟气捕集器III连接吸烟机IV,进气口一端可以设置进气管,进气管一端连接空气入口V。The detection device for the emission of volatile organic compounds in this embodiment includes a first heating chamber 1', a second heating chamber 2', a third heating chamber 3', a fourth heating chamber 4', a fifth heating chamber 5', The sixth heating chamber 6', the seventh heating chamber 7', the eighth heating chamber 8', the ninth heating chamber 9', and the tenth heating chamber 10', one end of each heating chamber is connected to the air inlet, and the other end is connected to the outlet The air pipe and the air outlet pipe are arranged around the turntable 1 to form the first communication port 1, the second communication port 2, the third communication port 3, the fourth communication port 4, the fifth communication port 5, and the sixth communication port 6 arranged around the turntable 1. , the seventh communication port 7, the eighth communication port 8, the ninth communication port 9, the tenth communication port 10, the first air intake pipe 11 is included on the rotating disk 1, and the first air intake pipe 11 rotates with the rotating disk 1, and the first air intake pipe 11 One end communicates with one of the communication ports at a certain moment, the other end of the first air intake pipe 11 communicates with one end of the second air intake pipe 12, the second air intake pipe 12 is fixed, and the other end of the second air intake pipe 12 is connected to the filter holder II , the filter holder II is connected to the smoke trap III, the smoke trap III is connected to the smoking machine IV, an air intake pipe can be arranged at one end of the air inlet, and one end of the air intake pipe is connected to the air inlet V.

加热腔上均设有温度调节装置,加热温度范围为30-200℃。加热腔上设有电子加热组件,可以迅速加热腔内空气至指定温度,精确控温。The heating chamber is equipped with a temperature regulating device, and the heating temperature range is 30-200°C. There is an electronic heating component on the heating chamber, which can quickly heat the air in the chamber to the specified temperature and control the temperature precisely.

转盘、抽烟机与控制系统连接,控制系统控制转盘自动旋转切换,且与抽烟机卷烟抽吸过程保持一致,即抽吸第一口时,第一连通口与第一进气管11相通;抽吸第二口时,切换至第二连通口,使得第二连通口与第一进气管11相通;依此类推,至抽吸第N口时,第N连通口与第一进气管11相通,转盘切换时,外界空气不会直接进入第一进气管,整个抽吸过程的空气均来自各个加热腔,高度真实模拟人体吸烟。The turntable and the smoking machine are connected with the control system, and the control system controls the automatic rotation and switching of the turntable, and is consistent with the cigarette smoking process of the smoking machine, that is, when the first puff is taken, the first communication port communicates with the first intake pipe 11; When the second port is used, switch to the second communication port so that the second communication port communicates with the first air intake pipe 11; When switching, the outside air will not directly enter the first air intake pipe, and the air in the entire suction process comes from each heating chamber, which highly simulates human smoking.

滤棒夹持器为圆周可调型滤嘴夹持器,其圆周可调,满足市售卷烟所有圆周规格。烟气捕集器为剑桥滤片捕集。所有组件间的气路为金属或玻璃隔热管路。The filter rod holder is a filter tip holder with adjustable circumference, and its circumference can be adjusted to meet all the circumference specifications of commercially available cigarettes. The smoke trap is a Cambridge filter. The gas paths between all components are metal or glass heat-insulated pipelines.

使用上述检测装置检测挥发性有机化合物释放量,按以下进行:Use the above-mentioned detection device to detect the emission of volatile organic compounds, as follows:

在A卷烟人工添加1号纳米滤嘴,在装有纳米滤嘴的起始部位插入测温探针,在普通吸烟机上抽吸,通过测温探针测定每口抽吸时通过纳米滤嘴起始部位的烟气的温度,并确定整支卷烟的抽吸口数。Artificially add No. 1 nano-filter to cigarette A, insert a temperature-measuring probe at the beginning of the nano-filter, smoke it on an ordinary smoking machine, measure the starting point of each puff through the nano-filter through the temperature-measuring probe Determine the temperature of the smoke at the starting point and determine the number of puffs for the entire cigarette.

根据测得的抽吸温度及抽吸口数,设定模拟装置中空气加热腔中的空气温度,温度加热腔1’(第一口36.5 ℃)、加热腔2’(第二口37.9 ℃)、加热腔3’(第三口41.2 ℃)、加热腔4’(第四口43.8 ℃)、加热腔5’(第五口45.1 ℃)、加热腔6’(第六口46.7 ℃)、加热腔7’(第七口48.4 ℃)、加热腔8’(第八口50.3 ℃)。设定抽吸口数共8口。According to the measured suction temperature and the number of suction ports, set the air temperature in the air heating chamber in the simulation device, temperature heating chamber 1' (first port 36.5 ℃), heating chamber 2' (second port 37.9 ℃), Heating chamber 3' (third port 41.2 ℃), heating chamber 4' (fourth port 43.8 ℃), heating chamber 5' (fifth port 45.1 ℃), heating chamber 6' (sixth port 46.7 ℃), heating chamber 7' (7th port 48.4 ℃), heating chamber 8' (eighth port 50.3 ℃). Set the number of suction ports to 8 in total.

把纳米过滤嘴从卷烟上取下,安装到滤棒夹持器上,启动吸烟机按标准条件进行抽吸,抽吸第一口时,通过滤棒的为第一加热腔中的热空气;然后通过转盘切换,抽吸第二口时,通过滤棒的为第二加热腔中的热空气,依此类推,根据口数依次切换。通过过滤嘴的空气流模拟卷烟抽吸时的烟气流,把纳米滤嘴成分洗脱。Remove the nano-filter from the cigarette, install it on the filter rod holder, start the smoking machine to smoke according to the standard conditions, and when you take the first mouthful, the hot air in the first heating chamber passes through the filter rod; then Switching through the turntable, when sucking the second port, the hot air in the second heating chamber passes through the filter rod, and so on, switching in turn according to the number of ports. The air flow through the filter simulates the smoke flow when the cigarette is smoked, and the nano-filter components are eluted.

采用50ml三乙胺-20ml甲醇混合溶液进行捕集气流。对捕集液进行顶空-气质分析。A 50ml triethylamine-20ml methanol mixed solution was used to capture the gas flow. Headspace-gas-gas analysis was performed on the trapping fluid.

色谱条件:60 m×0.32 mm×1μm DB-5MS柱;进样量3μL;进样口温度220 ℃;分流比15:1;柱温箱温度40 ℃;载气流速1 ml/min;程序升温:从40 ℃保持6 min,然后以10℃/min 的速率升至160 ℃,保持3 min,最后以20 ℃/min 的速率升至220 ℃,保持3 min。Chromatographic conditions: 60 m×0.32 mm×1 μm DB-5MS column; injection volume 3 μL; inlet temperature 220 ℃; split ratio 15:1; column oven temperature 40 ℃; carrier gas flow rate 1 ml/min; temperature program : Keep from 40°C for 6 minutes, then increase to 160°C at a rate of 10°C/min, hold for 3 minutes, and finally increase to 220°C at a rate of 20°C/min, and hold for 3 minutes.

质谱条件:电离方式EI,电离能量70 eV,传输线温度200 ℃,离子源温度 240 ℃,溶剂延迟时间3 min,扫描范围:m/z 40.0-200.0。Mass spectrometry conditions: ionization mode EI, ionization energy 70 eV, transfer line temperature 200 ℃, ion source temperature 240 ℃, solvent delay time 3 min, scan range: m/z 40.0-200.0.

分析结果如表1所示。The analysis results are shown in Table 1.

实施例2Example 2

本实施例的检测装置与实施例1相同,使用上述检测装置检测挥发性有机化合物释放量,按以下进行:The detection device of the present embodiment is the same as that of Example 1, and the above-mentioned detection device is used to detect the emission of volatile organic compounds, as follows:

在B卷烟人工添加2号纳米滤嘴,在装有纳米滤嘴起始部位插入测温探针,在普通吸烟机上抽吸,通过测温探针测定每口抽吸时通过纳米滤嘴起始部位烟气的温度,并确定整支卷烟的抽吸口数。Artificially add No. 2 nano-filters to B cigarettes, insert a temperature measuring probe at the beginning of the nano-filters, smoke on an ordinary smoking machine, and use the temperature-measuring probe to measure the start of each puff through the nano-filters The temperature of the smoke at the site and determine the number of puffs for the whole cigarette.

根据测得的抽吸温度及抽吸口数,设定装置中空气加热腔中的空气温度,温度加热腔1’(第一口35.4℃)、加热腔2’(第二口36.5 ℃)、加热腔3’(第三口40.1 ℃)、加热腔4’(第四口41.5 ℃)、加热腔5’(第五口43.6 ℃)、加热腔6’(第六口45.2 ℃)、加热腔7’(第七口47.1 ℃)。设定抽吸口数共7口。According to the measured suction temperature and the number of suction ports, set the air temperature in the air heating chamber in the device, temperature heating chamber 1' (first port 35.4°C), heating chamber 2' (second port 36.5°C), Chamber 3' (third port 40.1 ℃), heating chamber 4' (fourth port 41.5 ℃), heating chamber 5' (fifth port 43.6 ℃), heating chamber 6' (sixth port 45.2 ℃), heating chamber 7 ' (7th mouth 47.1 ℃). Set the number of suction ports to 7 in total.

把纳米过滤嘴从卷烟上取下,安装到滤棒夹持器上,启动吸烟机按标准条件进行抽吸,抽吸第一口时,通过滤棒的为第一加热腔中的热空气;然后通过转盘切换,抽吸第二口时,通过滤棒的为第二加热腔中的热空气,依此类推,根据口数依次切换。通过过滤嘴的空气流模拟卷烟抽吸时的烟气流,抽吸结束后,把纳米滤嘴成分洗脱。Remove the nano-filter from the cigarette, install it on the filter rod holder, start the smoking machine to smoke according to the standard conditions, and when you take the first mouthful, the hot air in the first heating chamber passes through the filter rod; then Switching through the turntable, when sucking the second port, the hot air in the second heating chamber passes through the filter rod, and so on, switching in turn according to the number of ports. The air flow through the filter simulates the smoke flow when the cigarette is smoked, and the nano-filter components are eluted after the suction is over.

采用50ml三乙胺-20ml甲醇混合溶液捕集气流。对捕集液进行顶空-气质分析。A 50ml triethylamine-20ml methanol mixed solution was used to capture the gas flow. Headspace-gas-gas analysis was performed on the trapping fluid.

色谱条件:60 m×0.32 mm×1 μm DB-5MS柱。进样量3μL;进样口温度220 ℃;分流比15:1;柱温箱温度40 ℃;载气流速1 ml/min;程序升温:从40 ℃保持6 min,然后以10℃/min 的速率升至160 ℃,保持3 min,最后以20 ℃/min 的速率升至220 ℃,保持3 min。Chromatographic conditions: 60 m×0.32 mm×1 μm DB-5MS column. Injection volume 3 μL; inlet temperature 220 °C; split ratio 15:1; column oven temperature 40 °C; carrier gas flow rate 1 ml/min; The rate was increased to 160 °C and maintained for 3 min, and finally increased to 220 °C at a rate of 20 °C/min and maintained for 3 min.

质谱条件:电离方式EI,电离能量70 eV,传输线温度200 ℃,离子源温度 240 ℃,溶剂延迟时间3 min,扫描范围:m/z 40.0-200.0。Mass spectrometry conditions: ionization mode EI, ionization energy 70 eV, transfer line temperature 200 ℃, ion source temperature 240 ℃, solvent delay time 3 min, scan range: m/z 40.0-200.0.

其余与实施例1相同,分析结果如表1所示。All the other are identical with embodiment 1, analysis result is as shown in table 1.

实施例3Example 3

本实施例的检测装置与实施例1相同,使用上述检测装置检测挥发性有机化合物释放量,按以下进行:The detection device of the present embodiment is the same as that of Example 1, and the above-mentioned detection device is used to detect the emission of volatile organic compounds, as follows:

在C卷烟人工添加3号纳米滤嘴,在装有纳米滤嘴的起始部位插入测温探针,在普通吸烟机上抽吸,通过测温探针测定每口抽吸时通过纳米滤嘴起始部位的烟气的温度,并确定整支卷烟的抽吸口数。Artificially add No. 3 nano-filter to cigarette C, insert a temperature-measuring probe at the beginning of the nano-filter, smoke it on an ordinary smoking machine, measure the starting point of each puff through the nano-filter through the temperature-measuring probe Determine the temperature of the smoke at the starting point and determine the number of puffs for the entire cigarette.

根据测得的抽吸温度及抽吸口数,设定模拟装置中空气加热腔中的空气温度,温度加热腔1’(第一口36.5 ℃)、加热腔2’(第二口37.9 ℃)、加热腔3’(第三口41.2 ℃)、加热腔4’(第四口43.8 ℃)、加热腔5’(第五口45.1 ℃)、加热腔6’(第六口46.7 ℃)、加热腔7’(第七口48.4 ℃)、加热腔8’(第八口50.3 ℃)。设定抽吸口数共8口。According to the measured suction temperature and the number of suction ports, set the air temperature in the air heating chamber in the simulation device, temperature heating chamber 1' (first port 36.5 ℃), heating chamber 2' (second port 37.9 ℃), Heating chamber 3' (third port 41.2 ℃), heating chamber 4' (fourth port 43.8 ℃), heating chamber 5' (fifth port 45.1 ℃), heating chamber 6' (sixth port 46.7 ℃), heating chamber 7' (7th port 48.4 ℃), heating chamber 8' (eighth port 50.3 ℃). Set the number of suction ports to 8 in total.

把纳米过滤嘴从卷烟上取下,安装到滤棒夹持器上,启动吸烟机按标准条件进行抽吸,抽吸第一口时,通过滤棒的为第一口加热腔中的热空气;然后通过转盘切换,抽吸第二口时,通过滤棒的为第二加热腔中的热空气,依此类推,根据口数依次切换。通过过滤嘴的空气流模拟卷烟抽吸时的烟气流,抽吸结束后,把纳米滤嘴成分洗脱。Remove the nano-filter from the cigarette, install it on the filter rod holder, start the smoking machine to smoke according to the standard conditions, and when the first puff is taken, the hot air in the heating chamber of the first puff passes through the filter rod; Then switch through the turntable, when the second port is sucked, the hot air in the second heating chamber passes through the filter rod, and so on, switching in turn according to the number of ports. The air flow through the filter simulates the smoke flow when the cigarette is smoked, and the nano-filter components are eluted after the suction is over.

采用50ml三乙胺-20ml甲醇混合溶液进行捕集气流。对捕集液进行顶空-气质分析。A 50ml triethylamine-20ml methanol mixed solution was used to capture the gas flow. Headspace-gas-gas analysis was performed on the trapping fluid.

色谱条件:60 m×0.32 mm×1 μm DB-5MS柱。进样量3μL;进样口温度220 ℃;分流比15:1;柱温箱温度40 ℃;载气流速1 ml/min;程序升温:从40 ℃保持6 min,然后以10℃/min 的速率升至160 ℃,保持3 min,最后以20 ℃/min 的速率升至220 ℃,保持3 min。Chromatographic conditions: 60 m×0.32 mm×1 μm DB-5MS column. Injection volume 3 μL; inlet temperature 220 °C; split ratio 15:1; column oven temperature 40 °C; carrier gas flow rate 1 ml/min; The rate was increased to 160 °C and maintained for 3 min, and finally increased to 220 °C at a rate of 20 °C/min and maintained for 3 min.

质谱条件:电离方式EI,电离能量70 eV,传输线温度200 ℃,离子源温度 240 ℃,溶剂延迟时间3 min,扫描范围:m/z 40.0-200.0。Mass spectrometry conditions: ionization mode EI, ionization energy 70 eV, transfer line temperature 200 ℃, ion source temperature 240 ℃, solvent delay time 3 min, scan range: m/z 40.0-200.0.

其余与实施例1相同,分析结果如表1所示。All the other are identical with embodiment 1, analysis result is as shown in table 1.

实施例4Example 4

本实施例的检测装置与实施例1相同,使用上述检测装置检测挥发性有机化合物释放量,按以下进行:The detection device of the present embodiment is the same as that of Example 1, and the above-mentioned detection device is used to detect the emission of volatile organic compounds, as follows:

在D卷烟人工添加4号纳米滤嘴,在装有纳米滤嘴起始部位插入测温探针,在普通吸烟机上抽吸,通过测温探针测定每口抽吸时通过纳米滤嘴烟气的温度,并确定整支卷烟的抽吸口数。Artificially add No. 4 nano-filters to D cigarettes, insert a temperature-measuring probe at the beginning of the nano-filters, smoke on an ordinary smoking machine, and use the temperature-measuring probes to measure the smoke that passes through the nano-filters during each puff. temperature and determine the number of puffs for the entire cigarette.

根据测得的抽吸温度及抽吸口数,设定模拟装置中空气加热腔中的空气温度,温度加热腔1’(第一口35.4℃)、加热腔2’(第二口36.5 ℃)、加热腔3’(第三口40.1 ℃)、加热腔4’(第四口41.5 ℃)、加热腔5’(第五口43.6 ℃)、加热腔6’(第六口45.2 ℃)、加热腔7’(第七口47.1 ℃)。设定抽吸口数共7口。According to the measured suction temperature and the number of suction ports, set the air temperature in the air heating chamber in the simulation device, temperature heating chamber 1' (first port 35.4 °C), heating chamber 2' (second port 36.5 °C), Heating chamber 3' (third port 40.1 ℃), heating chamber 4' (fourth port 41.5 ℃), heating chamber 5' (fifth port 43.6 ℃), heating chamber 6' (sixth port 45.2 ℃), heating chamber 7' (7th port 47.1 °C). Set the number of suction ports to 7 in total.

把纳米过滤嘴从卷烟上取下,安装到滤棒夹持器上,启动吸烟机按标准条件进行抽吸,抽吸第一口时,通过滤棒的为第一加热腔中的热空气;然后通过转盘切换,抽吸第二口时,通过滤棒的为第二加热腔中的热空气,依此类推,其口数依次切换。通过过滤嘴的空气流模拟卷烟抽吸时的烟气流,抽吸结束后,把纳米滤嘴成分洗脱。Remove the nano-filter from the cigarette, install it on the filter rod holder, start the smoking machine to smoke according to the standard conditions, and when you take the first mouthful, the hot air in the first heating chamber passes through the filter rod; then Switching through the turntable, when the second port is sucked, the hot air in the second heating chamber passes through the filter rod, and so on, and the number of ports is switched in turn. The air flow through the filter simulates the smoke flow when the cigarette is smoked, and the nano-filter components are eluted after the suction is over.

采用50ml三乙胺-20ml甲醇混合溶液进行捕集气流。对捕集液进行顶空-气质分析。A 50ml triethylamine-20ml methanol mixed solution was used to capture the gas flow. Headspace-gas-gas analysis was performed on the trapping fluid.

色谱条件:60 m×0.32 mm×1 μm DB-5MS柱。进样量3μL;进样口温度220 ℃;分流比15:1;柱温箱温度40 ℃;载气流速1 ml/min;程序升温:从40 ℃保持6 min,然后以10℃/min 的速率升至160 ℃,保持3 min,最后以20 ℃/min 的速率升至220 ℃,保持3 min。Chromatographic conditions: 60 m×0.32 mm×1 μm DB-5MS column. Injection volume 3 μL; inlet temperature 220 °C; split ratio 15:1; column oven temperature 40 °C; carrier gas flow rate 1 ml/min; The rate was increased to 160 °C and maintained for 3 min, and finally increased to 220 °C at a rate of 20 °C/min and maintained for 3 min.

质谱条件:电离方式EI,电离能量70 eV,传输线温度200 ℃,离子源温度 240 ℃,溶剂延迟时间3 min,扫描范围:m/z 40.0-200.0。Mass spectrometry conditions: ionization mode EI, ionization energy 70 eV, transfer line temperature 200 ℃, ion source temperature 240 ℃, solvent delay time 3 min, scan range: m/z 40.0-200.0.

其余与实施例1相同,分析结果如表1所示。All the other are identical with embodiment 1, analysis result is as shown in table 1.

实施例5Example 5

本实施例的检测装置与实施例1相同,使用上述检测装置检测挥发性有机化合物释放量,按以下进行:The detection device of the present embodiment is the same as that of Example 1, and the above-mentioned detection device is used to detect the emission of volatile organic compounds, as follows:

在E卷烟人工添加5号纳米滤嘴,在装有纳米滤嘴的部位插入测温探针,在普通吸烟机上抽吸,通过测温探针测定每口抽吸时通过纳米滤嘴烟气的温度,并确定整支卷烟的抽吸口数。Artificially add No. 5 nano-filters to E cigarettes, insert a temperature-measuring probe into the part where the nano-filters are installed, smoke on an ordinary smoking machine, and use the temperature-measuring probe to measure the amount of smoke that passes through the nano-filters during each puff. temperature, and determine the number of puffs taken throughout the cigarette.

根据测得的抽吸温度及抽吸口数,设定模拟装置中空气加热腔中的空气温度,温度加热腔1’(第一口36.5 ℃)、加热腔2’(第二口37.9 ℃)、加热腔3’(第三口41.2 ℃)、加热腔4’(第四口43.8 ℃)、加热腔5’(第五口45.1 ℃)、加热腔6’(第六口46.7 ℃)、加热腔7’(第七口48.4 ℃)、加热腔8’(第八口50.3 ℃)。设定抽吸口数共8口。According to the measured suction temperature and the number of suction ports, set the air temperature in the air heating chamber in the simulation device, temperature heating chamber 1' (first port 36.5 ℃), heating chamber 2' (second port 37.9 ℃), Heating chamber 3' (third port 41.2 ℃), heating chamber 4' (fourth port 43.8 ℃), heating chamber 5' (fifth port 45.1 ℃), heating chamber 6' (sixth port 46.7 ℃), heating chamber 7' (7th port 48.4 ℃), heating chamber 8' (eighth port 50.3 ℃). Set the number of suction ports to 8 in total.

把纳米过滤嘴从卷烟上取下,安装到滤棒夹持器上,启动吸烟机按标准条件进行抽吸,抽吸第一口时,通过滤棒的为第一加热腔中的热空气;然后通过转盘切换,抽吸第二口时,通过滤棒的为第二加热腔中的热空气,依此类推,其口数依次切换。通过过滤嘴的空气流就模拟卷烟抽吸时的烟气流,抽吸结束后,把纳米滤嘴成分洗脱。Remove the nano-filter from the cigarette, install it on the filter rod holder, start the smoking machine to smoke according to the standard conditions, and when you take the first mouthful, the hot air in the first heating chamber passes through the filter rod; then Switching through the turntable, when the second port is sucked, the hot air in the second heating chamber passes through the filter rod, and so on, and the number of ports is switched in turn. The air flow through the filter simulates the smoke flow when the cigarette is smoked, and the nano-filter components are eluted after the smoke is finished.

模拟气流采用50ml三乙胺-20ml甲醇混合溶液进行捕集。对捕集液进行顶空-气质分析。The simulated gas flow is captured by a mixed solution of 50ml triethylamine-20ml methanol. Headspace-gas-gas analysis was performed on the trapping fluid.

色谱条件:60 m×0.32 mm×1 μm DB-5MS柱。进样量3μL;进样口温度220 ℃;分流比15:1;柱温箱温度40 ℃;载气流速1 ml/min;程序升温:从40 ℃保持6 min,然后以10℃/min 的速率升至160 ℃,保持3 min,最后以20 ℃/min 的速率升至220 ℃,保持3 min。Chromatographic conditions: 60 m×0.32 mm×1 μm DB-5MS column. Injection volume 3 μL; inlet temperature 220 °C; split ratio 15:1; column oven temperature 40 °C; carrier gas flow rate 1 ml/min; The rate was increased to 160 °C and maintained for 3 min, and finally increased to 220 °C at a rate of 20 °C/min and maintained for 3 min.

质谱条件:电离方式EI,电离能量70 eV,传输线温度200 ℃,离子源温度 240 ℃,溶剂延迟时间3 min,扫描范围:m/z 40.0-200.0。Mass spectrometry conditions: ionization mode EI, ionization energy 70 eV, transfer line temperature 200 ℃, ion source temperature 240 ℃, solvent delay time 3 min, scan range: m/z 40.0-200.0.

其余与实施例1相同,分析结果如表1所示。All the other are identical with embodiment 1, analysis result is as shown in table 1.

实施例6Example 6

本实施例的检测装置与实施例1相同,使用上述检测装置检测挥发性有机化合物释放量,按以下进行:The detection device of the present embodiment is the same as that of Example 1, and the above-mentioned detection device is used to detect the emission of volatile organic compounds, as follows:

在F卷烟人工添加6号纳米滤嘴,在装有纳米滤嘴起始部位插入测温探针,在普通吸烟机上抽吸,通过测温探针测定每口抽吸时通过纳米滤嘴烟气的温度,并确定整支卷烟的抽吸口数。Artificially add No. 6 nano-filter to F cigarette, insert a temperature-measuring probe at the beginning of the nano-filter, smoke on an ordinary smoking machine, and use the temperature-measuring probe to measure the smoke that passes through the nano-filter during each puff. temperature and determine the number of puffs for the entire cigarette.

根据测得的抽吸温度及抽吸口数,设定模拟装置中空气加热腔中的空气温度,温度加热腔1’(第一口35.4℃)、加热腔2’(第二口36.5 ℃)、加热腔3’(第三口40.1 ℃)、加热腔4’(第四口41.5 ℃)、加热腔5’(第五口43.6 ℃)、加热腔6’(第六口45.2 ℃)、加热腔7’(第七口47.1 ℃)。设定抽吸口数共7口。According to the measured suction temperature and the number of suction ports, set the air temperature in the air heating chamber in the simulation device, temperature heating chamber 1' (first port 35.4 °C), heating chamber 2' (second port 36.5 °C), Heating chamber 3' (third port 40.1 ℃), heating chamber 4' (fourth port 41.5 ℃), heating chamber 5' (fifth port 43.6 ℃), heating chamber 6' (sixth port 45.2 ℃), heating chamber 7' (7th port 47.1 °C). Set the number of suction ports to 7 in total.

把纳米过滤嘴从卷烟上取下,安装到滤棒夹持器上,启动吸烟机按标准条件进行抽吸,抽吸第一口时,通过滤棒的为第一加热腔中的热空气;然后通过转盘切换,抽吸第二口时通过滤棒的为第二加热腔中的热空气,依此类推,根据口数依次切换。通过过滤嘴的空气流就模拟卷烟抽吸时的烟气流,抽吸结束后,把纳米滤嘴成分洗脱。Remove the nano-filter from the cigarette, install it on the filter rod holder, start the smoking machine to smoke according to the standard conditions, and when you take the first mouthful, the hot air in the first heating chamber passes through the filter rod; then Switching through the turntable, the hot air in the second heating chamber passes through the filter rod when sucking the second port, and so on, switching in turn according to the number of ports. The air flow through the filter simulates the smoke flow when the cigarette is smoked, and the nano-filter components are eluted after the smoke is finished.

采用50ml三乙胺-20ml甲醇混合溶液进行捕集气流。对捕集液进行顶空-气质分析。A 50ml triethylamine-20ml methanol mixed solution was used to capture the gas flow. Headspace-gas-gas analysis was performed on the trapping fluid.

色谱条件:60 m×0.32 mm×1 μm DB-5MS柱。进样量3μL;进样口温度220 ℃;分流比15:1;柱温箱温度40 ℃;载气流速1 ml/min;程序升温:从40 ℃保持6 min,然后以10℃/min 的速率升至160 ℃,保持3 min,最后以20 ℃/min 的速率升至220 ℃,保持3 min。Chromatographic conditions: 60 m×0.32 mm×1 μm DB-5MS column. Injection volume 3 μL; inlet temperature 220 °C; split ratio 15:1; column oven temperature 40 °C; carrier gas flow rate 1 ml/min; The rate was increased to 160 °C and maintained for 3 min, and finally increased to 220 °C at a rate of 20 °C/min and maintained for 3 min.

质谱条件:电离方式EI,电离能量70 eV,传输线温度200 ℃,离子源温度 240 ℃,溶剂延迟时间3 min,扫描范围:m/z 40.0-200.0。Mass spectrometry conditions: ionization mode EI, ionization energy 70 eV, transfer line temperature 200 ℃, ion source temperature 240 ℃, solvent delay time 3 min, scan range: m/z 40.0-200.0.

其余与实施例1相同,分析结果如表1所示。All the other are identical with embodiment 1, analysis result is as shown in table 1.

实施例7Example 7

本实施例的检测装置与实施例1相同,使用上述检测装置检测挥发性有机化合物释放量,按以下进行:The detection device of the present embodiment is the same as that of Example 1, and the above-mentioned detection device is used to detect the emission of volatile organic compounds, as follows:

在G卷烟人工添加7号纳米滤嘴,在装有纳米滤嘴的起始部位插入测温探针,在普通吸烟机上抽吸,通过测温探针测定每口抽吸时通过纳米滤嘴起始部位的烟气的温度,并确定整支卷烟的抽吸口数。Artificially add No. 7 nano-filters to G cigarettes, insert a temperature-measuring probe into the initial part equipped with nano-filters, smoke on an ordinary smoking machine, and measure the starting point of each puff through the nano-filters through the temperature-measuring probe. Determine the temperature of the smoke at the starting point and determine the number of puffs for the entire cigarette.

根据测得的抽吸温度及抽吸口数,设定模拟装置中空气加热腔中的空气温度,温度加热腔1’(第一口36.5 ℃)、加热腔2’(第二口37.9 ℃)、加热腔3’(第三口41.2 ℃)、加热腔4’(第四口43.8 ℃)、加热腔5’(第五口45.1 ℃)、加热腔6’(第六口46.7 ℃)、加热腔7’(第七口48.4 ℃)、加热腔8’(第八口50.3 ℃)。设定抽吸口数共8口。According to the measured suction temperature and the number of suction ports, set the air temperature in the air heating chamber in the simulation device, temperature heating chamber 1' (first port 36.5 ℃), heating chamber 2' (second port 37.9 ℃), Heating chamber 3' (third port 41.2 ℃), heating chamber 4' (fourth port 43.8 ℃), heating chamber 5' (fifth port 45.1 ℃), heating chamber 6' (sixth port 46.7 ℃), heating chamber 7' (7th port 48.4 ℃), heating chamber 8' (eighth port 50.3 ℃). Set the number of suction ports to 8 in total.

把纳米滤嘴的卷烟的过滤嘴从卷烟上取下,安装到滤棒夹持器上,启动吸烟机按标准条件进行抽吸,抽吸第一口时,通过滤棒的为第一加热腔中的热空气;然后通过转盘切换,抽吸第二口时,通过滤棒的为第二加热腔中的热空气,依此类推,根据口数依次切换。通过过滤嘴的空气流就模拟卷烟抽吸时的烟气流,抽吸完成后,把纳米滤嘴成分洗脱。Remove the filter tip of the nano-filter cigarette from the cigarette, install it on the filter rod holder, start the smoking machine and smoke according to the standard conditions. the hot air in the second heating chamber; and then switch through the turntable. When the second port is sucked, the hot air in the second heating chamber passes through the filter rod, and so on, switching in turn according to the number of ports. The air flow through the filter simulates the smoke flow when the cigarette is smoked. After the suction is completed, the nano-filter components are eluted.

采用50ml三乙胺-20ml甲醇混合溶液进行捕集气流。对捕集液进行顶空-气质分析。A 50ml triethylamine-20ml methanol mixed solution was used to capture the gas flow. Headspace-gas-gas analysis was performed on the trapping fluid.

色谱条件:60 m×0.32 mm×1 μm DB-5MS柱。进样量3μL;进样口温度220 ℃;分流比15:1;柱温箱温度40 ℃;载气流速1 ml/min;程序升温:从40 ℃保持6 min,然后以10℃/min 的速率升至160 ℃,保持3 min,最后以20 ℃/min 的速率升至220 ℃,保持3 min。Chromatographic conditions: 60 m×0.32 mm×1 μm DB-5MS column. Injection volume 3 μL; inlet temperature 220 °C; split ratio 15:1; column oven temperature 40 °C; carrier gas flow rate 1 ml/min; The rate was increased to 160 °C and maintained for 3 min, and finally increased to 220 °C at a rate of 20 °C/min and maintained for 3 min.

质谱条件:电离方式EI,电离能量70 eV,传输线温度200 ℃,离子源温度 240 ℃,溶剂延迟时间3 min,扫描范围:m/z 40.0-200.0。Mass spectrometry conditions: ionization mode EI, ionization energy 70 eV, transfer line temperature 200 ℃, ion source temperature 240 ℃, solvent delay time 3 min, scan range: m/z 40.0-200.0.

其余与实施例1相同,分析结果如表1所示。All the other are identical with embodiment 1, analysis result is as shown in table 1.

表1 VOCs分析结果Table 1 VOCs analysis results

由表1可以看出,本实施例的装置和方法能有效提升纳米滤嘴中挥发性有机化合物释放量的分析结果准确性,使样品的分析灵敏度提高,样品不受复杂的烟气影响,真实反映了滤嘴中挥发性有机化合物成分,检测周期短,具有推广应用价值。It can be seen from Table 1 that the device and method of this embodiment can effectively improve the accuracy of the analysis results of the release of volatile organic compounds in the nano-filter, improve the analysis sensitivity of the sample, and the sample is not affected by complex smoke, and the real It reflects the composition of volatile organic compounds in the filter, has a short detection period, and has the value of popularization and application.

以上所述仅为本发明的较佳实施例而已,并不用以限制本发明,凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。The above descriptions are only preferred embodiments of the present invention, and are not intended to limit the present invention. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principles of the present invention shall be included in the scope of the present invention. within the scope of protection.

Claims (6)

1.一种纳米滤嘴的挥发性有机化合物释放量的检测方法,其特征在于: 包括如下步骤:1. A method for detecting the release of volatile organic compounds from a nano-filter, characterized in that: comprising the steps: 步骤(1)、抽吸口数确定Step (1), determine the number of suction ports 在待测卷烟的含有纳米滤嘴的远唇端加料起始部位插入测温探针,在常规吸烟机上抽吸,通过测温探针测定每口抽吸时通过纳米滤嘴起始部位烟气的温度,并确定整支卷烟的抽吸口数;Insert a temperature measuring probe at the starting part of the far lip end of the cigarette to be tested that contains nano-filters, smoke on a conventional smoking machine, and use the temperature-measuring probe to measure the smoke that passes through the starting part of the nano-filter during each puff. temperature and determine the number of puffs for the whole cigarette; 步骤(2)、根据抽吸口数设定所需加热腔的温度Step (2), set the temperature of the required heating chamber according to the number of suction ports 按卷烟实际抽吸温度设定检测装置的若干加热腔中的空气温度,并设定抽吸口数,抽吸口数为7-8口,空气温度为36-51℃;Set the air temperature in several heating chambers of the detection device according to the actual smoking temperature of the cigarette, and set the number of suction ports, the number of suction ports is 7-8, and the air temperature is 36-51°C; 步骤(3)、抽吸Step (3), suction 将吸烟机、烟气捕集器和滤嘴夹持器依次连接,把纳米滤嘴卷烟的过滤嘴从卷烟上取下,安装到滤棒夹持器上,启动吸烟机按标准条件抽吸,抽吸的空气来自不同温度的加热腔,根据抽吸口数依次切换,每口抽吸通过过滤嘴的气流温度均和卷烟吸烟机实际抽吸时的气流温度一致;烟气捕集器采用三乙胺-甲醇混合溶液进行捕集气流;Connect the smoking machine, the smoke trap and the filter holder in sequence, remove the filter tip of the nano-filter cigarette from the cigarette, install it on the filter rod holder, start the smoking machine and smoke according to the standard conditions. The air sucked comes from heating chambers of different temperatures, which are switched in turn according to the number of suction ports. The temperature of the airflow through the filter tip is consistent with the actual airflow temperature of the cigarette smoking machine; the smoke trap adopts triethylamine- The mixed solution of methanol is used to capture the air flow; 步骤(4)、成分分析Step (4), component analysis 对捕集液进行顶空-气质分析。Headspace-gas-gas analysis was performed on the trapping fluid. 2.根据权利要求1所述的检测方法,其特征在于:使用芳香胺释放量的检测装置进行检测,所述检测装置包括若干加热腔,加热腔一端连接进气口,另一端连接出气管,出气管围绕转盘设置,转盘上包括第一进气管,第一进气管随转盘转动,第一进气管一端在某一时刻与其中一个出气管连通,第一进气管另一端与第二进气管一端连通,第二进气管固定,另一端与滤嘴夹持器连接,滤嘴夹持器连接烟气捕集器,烟气捕集器连接吸烟机。2. The detection method according to claim 1, characterized in that: a detection device for release of aromatic amine is used for detection, the detection device includes several heating chambers, one end of the heating chamber is connected to the air inlet, and the other end is connected to the air outlet pipe, The air outlet pipe is arranged around the turntable, and the turntable includes a first air inlet pipe, which rotates with the turntable, and one end of the first air inlet pipe communicates with one of the air outlet pipes at a certain moment, and the other end of the first air inlet pipe connects with one end of the second air inlet pipe. The second air intake pipe is fixed, the other end is connected with the filter holder, the filter holder is connected with the smoke trap, and the smoke catcher is connected with the smoking machine. 3.根据权利要求1所述的检测方法,其特征在于:加热腔为10个,加热腔上均设有温度调节装置,加热温度范围为30-200℃。3. The detection method according to claim 1, characterized in that there are 10 heating chambers, each of which is equipped with a temperature adjustment device, and the heating temperature range is 30-200°C. 4.根据权利要求1所述的检测方法,其特征在于:步骤(4)中,色谱条件:60 m×0.32 mm×1μm DB-5MS柱;载气:氦气;进样量3μL;进样口温度220 ℃;分流比15:1;柱温箱温度40℃;载气流速1 ml/min;程序升温:从40 ℃保持6 min,然后以10 ℃/min 的速率升至160℃,保持3 min,最后以20 ℃/min 的速率升至220 ℃,保持3 min。4. The detection method according to claim 1, characterized in that: in step (4), chromatographic conditions: 60 m×0.32 mm×1 μm DB-5MS column; carrier gas: helium; injection volume 3 μL; injection Inlet temperature 220 °C; split ratio 15:1; column oven temperature 40 °C; carrier gas flow rate 1 ml/min; temperature program: keep from 40 °C for 6 min, then increase to 160 °C at a rate of 10 °C/min, keep 3 min, and finally increased to 220 °C at a rate of 20 °C/min and kept for 3 min. 5.根据权利要求1所述的检测方法,其特征在于:步骤(4)中,质谱条件:电离方式EI,电离能量70 eV,传输线温度200 ℃,离子源温度 240 ℃,溶剂延迟时间3 min,扫描范围:m/z40.0-200.0。5. The detection method according to claim 1, characterized in that: in step (4), mass spectrometry conditions: ionization mode EI, ionization energy 70 eV, transmission line temperature 200 °C, ion source temperature 240 °C, solvent delay time 3 min , Scanning range: m/z40.0-200.0. 6.根据权利要求1所述的检测方法,其特征在于:步骤(3)中,三乙胺用量为50 ml,甲醇用量为20ml。6. The detection method according to claim 1, characterized in that: in step (3), the amount of triethylamine used is 50 ml, and the amount of methanol used is 20 ml.
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