WO2020253561A1 - 一种检测加热不燃烧卷烟烟气中铝释放量的方法 - Google Patents

一种检测加热不燃烧卷烟烟气中铝释放量的方法 Download PDF

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WO2020253561A1
WO2020253561A1 PCT/CN2020/094851 CN2020094851W WO2020253561A1 WO 2020253561 A1 WO2020253561 A1 WO 2020253561A1 CN 2020094851 W CN2020094851 W CN 2020094851W WO 2020253561 A1 WO2020253561 A1 WO 2020253561A1
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aluminum
solution
standard working
standard
heat
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PCT/CN2020/094851
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English (en)
French (fr)
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黄龙
罗诚浩
陈义坤
柯炜昌
张敦铁
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湖北中烟工业有限责任公司
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Priority to EP20827519.8A priority Critical patent/EP3957971B1/en
Priority to KR1020217037056A priority patent/KR102563685B1/ko
Publication of WO2020253561A1 publication Critical patent/WO2020253561A1/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
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
    • 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
    • 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
    • G01N1/38—Diluting, dispersing or mixing samples
    • 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
    • G01N1/4022—Concentrating samples by thermal techniques; Phase changes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/02—Details
    • H01J49/10—Ion sources; Ion guns
    • H01J49/105—Ion sources; Ion guns using high-frequency excitation, e.g. microwave excitation, Inductively Coupled Plasma [ICP]
    • A—HUMAN NECESSITIES
    • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24D—CIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
    • A24D1/00—Cigars; Cigarettes
    • A24D1/20—Cigarettes specially adapted for simulated smoking devices
    • A—HUMAN NECESSITIES
    • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24F—SMOKERS' REQUISITES; MATCH BOXES; SIMULATED SMOKING DEVICES
    • A24F40/00—Electrically operated smoking devices; Component parts thereof; Manufacture thereof; Maintenance or testing thereof; Charging means specially adapted therefor
    • A24F40/80—Testing
    • 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
    • G01N1/2202—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling
    • G01N1/2214—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling by sorption
    • 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
    • G01N1/2202—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling
    • G01N1/2214—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling by sorption
    • G01N2001/2217—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling by sorption using a liquid

Definitions

  • the invention relates to a method for detecting the amount of aluminum released in heat-not-burn cigarette smoke, and belongs to the technical field of tobacco detection.
  • Low-temperature cigarettes that is, heat-not-burn cigarettes (heat-not-burn cigarettes)
  • the tobacco material is heated by an external heat source, and the atomization medium, flavor components and additional fragrances in the tobacco material are heated to produce smoke similar to traditional cigarettes.
  • the heating temperature 250°C ⁇ 350°C(°C)
  • the burning temperature of traditional cigarettes 800°C ⁇ 900°C
  • the harmful components and biological The toxicity is greatly reduced, and the sidestream smoke and environmental smoke are also greatly reduced.
  • the composition of mainstream smoke is significantly different from that of traditional cigarettes.
  • JECFA Joint Expert Committee on Food Additives under the Food and Agriculture Organization of the United Nations and the World Health Organization
  • WHO Expert Committee on Food Additives has formulated the "Tentative Weekly Tolerable Intake" of aluminum.
  • the oral intake of aluminum per kilogram of body weight per person shall not exceed 2mg per kilogram of body weight per week (calculated based on 50kg body weight, Each person consumes about 15mg per day), it will not cause health hazards.
  • Heat-not-burn cigarettes are a new thing. There is no detection method for the smoke components of heat-not-burn cigarettes in the prior art, and there is no verified and approved special smoking machine for heat-not-burn cigarettes, and there is no detection of heat-not-burn cigarettes. The method of aluminum release in flue gas.
  • the purpose of the present invention is to provide a method for detecting the amount of aluminum released in heat-not-burn cigarette smoke, which can detect the amount of aluminum released in heat-not-burn cigarette smoke aerosol, with good stability and good linear correlation , Good practicability, high sensitivity and good repeatability.
  • a method for detecting the amount of aluminum released in the smoke of heat-not-burn cigarettes including the following steps: preparing a standard working solution of aluminum; obtaining aluminum according to the standard working solution of aluminum Element standard working curve; smoke heat not burn cigarettes, and collect the total smoke components of the heat not burn cigarettes; obtain sample preparation solutions according to the collected total smoke components; determine and analyze the sample preparation solutions, Combined with the standard working curve of the aluminum element, the release amount of aluminum in the total flue gas composition is determined.
  • the aluminum single element standard solution is diluted step by step to obtain the aluminum standard working solution, and the aluminum standard working solution includes aluminum single element series standard working solutions.
  • the external standard method or the internal standard method is used to obtain the aluminum standard working curve.
  • the aluminum standard working curve is obtained.
  • the internal standard working solution is obtained by diluting with a 45 Sc element standard solution.
  • the medium of the aluminum single element standard solution and the 45 Sc element standard solution are both the first nitric acid solution.
  • a solution capture method is used to collect the full smoke components.
  • a plurality of absorption bottles are used to sequentially collect the full smoke components in series.
  • collecting the total smoke components includes the following steps: (1) determining a cigarette smoking machine, (2) connecting a plurality of the absorption bottles connected in series to the clamp of the cigarette smoking machine Between the rear end of the cigarette holder and the suction mechanism; (3) insert the end of the heat-not-burn cigarette into the heating device, and insert the end of the mouthpiece into the holder of the cigarette smoking machine; (4) use the The heating device is heated, and the cigarette smoking machine starts smoking to the completion of smoking, and collects all smoke components.
  • the number of puffs is determined according to the smoking mode of the cigarette smoking machine and the heating time set by the heating device, and when the number of puffs is reached, the cigarette smoking machine completes smoking.
  • the smoking mode of the cigarette smoking machine is a Canadian deep smoking mode or a standard smoking mode.
  • the cigarette smoking machine adopts the Canadian deep puffing mode including a puffing capacity of 55 milliliters, a puffing time of 2 seconds, and an interval time between adjacent puffs of 28 seconds; so The Canadian deep suction mode sucks 2 puffs per minute.
  • the cigarette smoking machine adopts a standard smoking mode including a suction volume of 35 milliliters per puff, a puffing time of 2 seconds, and an interval time between adjacent puffs of 58 seconds; the standard smoking The suction mode sucks 1 puff per minute.
  • the cigarette smoking machine is a linear smoking machine.
  • an oxidant is added to the absorption bottle, the absorption liquid in the absorption bottle is completely transferred into the volumetric flask, and the sample preparation solution is obtained after constant volume.
  • the absorption bottle is a quartz absorption bottle
  • the absorption liquid in the quartz absorption bottle is a second nitric acid solution.
  • the oxidant is added to the quartz absorption bottle to completely oxidize the aluminum element in the full flue gas composition, and after shaking, the absorption liquid in the quartz absorption bottle is combined with The detergent is completely transferred into the volumetric flask, the first nitric acid solution is used to make the volume to the mark, and the sample preparation solution is obtained by shaking.
  • the volume fraction of the first nitric acid solution is 2%-8%; the volume of the second nitric acid solution is 15-25 ml, and the volume fraction of the second nitric acid solution is 5%- 15%.
  • an inductively coupled plasma mass spectrometer is used to measure the sample preparation solution.
  • the aluminum single element series standard working solution includes aluminum single element series standard working solutions with concentrations of 0, 0.5, 1.0, 2.0, 5.0, 10.0, 20.0, and 50.0 micrograms per liter.
  • the concentration of the internal standard working solution can be determined according to the concentration gradient of the aluminum single element series standard working solution and the content range of the actual test sample.
  • the concentration of the internal standard working solution is 10 micrograms per liter.
  • the present invention establishes a method for detecting the amount of aluminum released in the mainstream smoke of heat-not-burn cigarettes, with good precision, high accuracy, and high aluminum recovery rate. It is suitable for the quantitative analysis of aluminum emission in mainstream smoke of heat-not-burn cigarettes.
  • the method of the present invention can make full use of the linear smoking machine for smoking of heat-not-burn cigarettes and the collection of all smoke components, without the need for a special heat-not-burn cigarette smoking machine, which is simple and efficient.
  • the present invention adopts a series of multi-stage absorption bottles, which can realize the collection of all smoke components and the determination of the amount of aluminum released. 4.
  • the operation of smoking, full smoke trapping and absorption liquid treatment of the heating non-combustion cigarette of the present invention is simple and convenient, and the sample preparation solution is measured by inductively coupled plasma mass spectrometer, which is convenient, stable and has good linearity. Relevant and practical. 5.
  • the method of the present invention has high sensitivity and good repeatability.
  • Fig. 1 is a schematic flow diagram of a specific embodiment of the method for detecting the amount of aluminum released in heat-not-burn cigarette smoke of the present invention
  • Figure 2 is a schematic diagram of a linear smoking machine holder, a suction unit and a series-connected absorption bottle in a specific embodiment of the present invention
  • Fig. 3 is a schematic structural diagram of a quartz absorption bottle in a specific embodiment of the present invention.
  • the method for detecting the amount of aluminum released in the heat of non-combustion cigarette smoke includes the following steps:
  • the aluminum single element standard solution is determined as the standard stock solution; the aluminum single element standard solution is gradually diluted to obtain the aluminum single element series standard working solution. According to actual needs, the aluminum standard working solution is ready to use.
  • the preparation of the standard working solution of aluminum element includes the following content: the medium of the standard solution of aluminum element is determined to be the first nitric acid solution, and its standard value is 10 mg/L (milligrams/liter).
  • the concentration gradient of the aluminum single element series standard working solution can be determined according to the content range of the actual test sample.
  • the concentration of the aluminum single element series standard working solution is 0, 0.5, 1.0, 2.0, 5.0, 10.0, 20.0 and 50.0 ⁇ g/L (micrograms/liter), respectively.
  • the volume fraction of the first nitric acid solution is 2%-8%.
  • the volume fraction of the first nitric acid solution is 5%.
  • the external standard method is opposite to the internal standard method. It refers to adding a certain amount of standard substance (reference substance) to the blank sample to make a control sample, and the sample is processed and tested in parallel with the unknown sample. According to the response value of the control sample
  • the functional relationship of the concentration of the added standard (reference) is a quantitative method to estimate the concentration of the tested component in the unknown sample. For example, in chromatography, you want to know the concentration of the test sample. You can use the external standard method to first draw a working curve with the standard sample of the component to be tested, measure the peak height or peak area of each peak, and draw the standard curve.
  • the sample concentration can be obtained by measuring the peak height or peak area corresponding to the standard curve.
  • the aluminum standard working curve is obtained.
  • the internal standard working solution was added online, and the multi-level aluminum single element series standard working solutions were drawn into the ICP-MS (inductively coupled plasma mass spectrometer) for determination.
  • the ratio of the aluminum element content to the internal standard element content was taken as the horizontal Coordinates, the ratio of the mass-to-charge intensity of aluminum element to the internal standard element mass-to-charge ratio intensity is the ordinate, and the aluminum element work curve is established. Then, linear regression is performed on the calibration data to obtain the standard working curve and correlation coefficient.
  • the aluminum single element standard working solution with a concentration of 0.5 ⁇ g/L is injected multiple times, the standard deviation of the measurement result is calculated, and the detection limit and quantification limit of aluminum are determined by 3 times and 10 times the standard deviation, respectively.
  • the results show that the working curve of aluminum has good linearity, and the correlation coefficient is higher than 0.999; the quantitative limit of aluminum is much lower than the content of the target in the sample preparation solution, which is suitable for quantitative analysis.
  • a 45 Sc element standard solution is used to dilute to obtain an internal standard working solution.
  • the preparation of the internal standard working solution includes the following content: the medium of the 45 Sc element standard solution is determined to be the first nitric acid solution with a standard value of 10 mg/L (milligrams per liter).
  • the concentration of the internal standard working solution can be determined according to the concentration gradient of the aluminum single element series standard working solution and the content range of the actual test sample.
  • the concentration of the internal standard working solution is 10.0 ⁇ g/L (micrograms per liter).
  • the measurement conditions of the inductively coupled plasma mass spectrometer are determined (as shown in Table 1).
  • the RF power of the inductively coupled plasma mass spectrometer is 1280w (watts)
  • the flow rate of the carrier gas is 1.11L/min (liters/min)
  • the injection rate is 0.1mL/min (ml/min)
  • the acquisition mode is full quantitative Analysis, the number of repetitions is 3 times.
  • the detection limit of aluminum is determined to be 0.39 ng/L.
  • the quantitative limit of aluminum is determined to be 1.31 ng/L.
  • the mass number of aluminum is 27. Determine the internal standard element to be 45 Sc. Determine the integration time to be 0.5 seconds (as shown in Table 2).
  • Smoking heat-not-burn cigarettes and collecting all smoke components include the following steps:
  • the number of puffing ports is determined according to the smoking mode of the cigarette smoking machine 1 and the heating time set by the heating device 7, and when the number of puffing ports is reached, the cigarette smoking machine 1 completes smoking.
  • the smoking mode of the cigarette smoking machine 1 is the Canadian deep smoking mode or the ISO standard smoking mode.
  • the cigarette smoking machine 1 adopts the Canadian deep puffing mode, including a puffing capacity of 55 milliliters, a puffing time of 2 seconds, and an interval time between adjacent puffs of 28 seconds. Determine the Canadian deep suction mode to pump 2 puffs per minute.
  • the cigarette smoking machine 1 adopts the ISO standard smoking mode including a suction volume of 35 ml per puff, a puffing time of 2 seconds, and an interval time between adjacent puffs of 58 seconds. Determine the ISO standard suction mode to pump 1 puff per minute.
  • the heating device 7 is set for a continuous heating time of 3-6 minutes, 6-12 mouths are sucked in the Canadian deep suction mode, and 3-6 mouths are sucked in the ISO standard suction mode to achieve After the number of suction ports, the suction is completed.
  • the cigarette smoking machine 1 is a linear smoking machine (as shown in Figure 2).
  • the smoking mode of the cigarette smoking machine is independently designed according to actual needs.
  • the absorption bottle 3 contains a second nitric acid solution as an absorption liquid for absorbing smoke.
  • the volume of the second nitric acid solution is 15-25 ml, and the volume fraction of the second nitric acid solution is 5%-15%.
  • the volume of the second nitric acid solution is 20 milliliters, and the volume fraction of the second nitric acid solution is 10%.
  • the absorption bottle 3 is a quartz absorption bottle (a porous glass plate absorption bottle), and the absorption liquid of the quartz absorption bottle 3 is a second nitric acid solution.
  • the quartz absorption bottle 3 includes a bottle body 31, and an air inlet 32 is provided on the first side of the bottle body 31, and the collected smoke components enter from the air inlet 32. .
  • An air outlet 33 is provided on the second side of the bottle body 31, and the flue gas absorbed by the second nitric acid solution escapes from the air outlet 33.
  • the inside of the bottle body 31 is provided with a straight glass tube 34, the top of the straight glass tube 34 is connected to the air inlet 32, and the bottom of the straight glass tube 34 is provided with a half glass sphere 35, which can increase the total smoke composition and absorption The contact area of the liquid reduces the speed of smoke escape.
  • a sand core filter plate 36 is provided at the bottom of the semi-glass sphere 35.
  • the sand core filter plate 36 can increase the resistance of the flue gas to escape, and at the same time, the flue gas is dispersed into a plurality of small bubbles to escape after passing through the sand core filter plate 36.
  • the flue gas more fully contacts the quartz absorption bottle 3, so that the absorption is faster and safer.
  • a frosted standard port 37 is provided on the side wall of the bottle body 31 to improve the sealing performance.
  • the sand core filter plate 36 is configured as a quartz sand core filter plate.
  • the diameter of the quartz sand core filter plate 36 is 100-160 microns.
  • quartz absorption bottles 3 each added with a second nitric acid solution are connected in series, and the content of aluminum in each quartz absorption bottle 3 is measured. It was determined that aluminum was detected in the first and second quartz absorption bottles 3, and aluminum was not detected in the third, fourth and fifth quartz absorption bottles 3.
  • the number of quartz absorption bottles 3 is two, which can effectively trap aluminum in mainstream smoke.
  • the two quartz absorption bottles 3 are connected by a connecting pipe 2.
  • the air inlet 32 of the first quartz absorption bottle 3 is connected to the outlet end of the full flue gas composition (the rear end of the holder 4, as shown in FIG. 2) through the connecting pipe 2, and the outlet of the first quartz absorption bottle 3
  • the air port 33 is connected to the air inlet 32 of the second quartz absorption bottle 3 through the connecting pipe 2, and the air outlet 33 of the second quartz absorption bottle 3 is connected to the suction unit 5, so that the whole smoke can be fully absorbed by the absorption liquid.
  • An oxidant is added to the absorption bottle 3 to fully oxidize the aluminum element in the total flue gas composition, and the absorption liquid in the absorption bottle 3 is completely transferred into a volumetric flask, and after constant volume, a sample preparation solution is obtained.
  • an oxidant is added to the quartz absorption flask 3 to fully oxidize the aluminum element in the total flue gas composition. After ultrasonic vibration, the absorption liquid and washing liquid of the quartz absorption flask 3 are completely transferred into the volumetric flask together, and the first Dilute the nitric acid solution to the mark, shake well, and obtain a sample preparation solution.
  • the oxidant is hydrogen peroxide.
  • the volume of hydrogen peroxide is 5-10 mL (milliliter).
  • the volume of hydrogen peroxide is 5 ml.
  • the ultrasonic vibration time is 20-50 minutes.
  • the ultrasonic vibration time is 30 minutes.
  • the volumetric flask is a plastic volumetric flask.
  • the volume of the plastic volumetric flask is 100 milliliters.
  • An inductively coupled plasma mass spectrometer was used to measure the sample preparation solution. Specifically, determine the measurement conditions of the inductively coupled plasma mass spectrometer (as shown in Table 1). Determine the mass number of aluminum as 27. Determine the internal standard element to be 45 Sc. Determine the integration time to be 0.5 seconds (as shown in Table 2).
  • the ratio of the mass-to-charge intensity of aluminum element to the mass-to-charge ratio intensity of the internal standard element is substituted into the aluminum standard working curve to obtain the content of aluminum in the flue gas aerosol in the sample preparation solution.
  • the aluminum single element standard solution is a standard stock solution
  • the medium of the aluminum single element standard solution is 5% (volume fraction) nitric acid solution
  • the standard value is 10 mg/L.
  • the medium of the standard solution of 45 Sc is 5% (volume fraction) nitric acid solution, and its standard value is 10 mg/L.
  • the parameters of the inductively coupled plasma mass spectrometer (as shown in Table 1), the mass of aluminum element, the corresponding internal standard elements and the integration time (as shown in Table 2). Then, take the ratio of aluminum element content to internal standard element content as the abscissa, and the ratio of the mass-to-charge ratio of aluminum element to the internal standard element's mass-to-charge ratio as the ordinate to establish a working curve for aluminum. Linear regression was performed on the calibration data to obtain the standard working curve and correlation coefficient; the 0.5 ⁇ g/L aluminum single element standard working solution was injected 8 times, and the standard deviation of the measurement result was calculated, and the standard deviation was determined by 3 times and 10 times respectively.
  • the detection limit and the quantification limit are determined by the calculation results (as shown in Table 3).
  • Table 3 The results show that the working curve of aluminum has good linearity, and the correlation coefficient is higher than 0.999; the limit of quantification of aluminum is lower than the content of the target in the sample preparation solution, which is suitable for quantitative analysis.
  • the linear smoking machine 1 After determining the traditional cigarette linear smoking machine 1 (as shown in 2), connect the two quartz absorption bottles 3 with 20 ml of 10% (volume fraction) nitric acid solution through the connecting pipe 2, and connect the two quartz absorption bottles 3 Connect between the rear end of the holder 4 and the suction unit 5. After all the connecting pipes 2 are connected, check the air tightness; then, insert the end of the heat-not-burn cigarette sample A into the heating device 7, the mouthpiece The end is inserted into the holder 4, and the heating device 7 is turned on to preheat for 30 seconds. After the preheating time is reached, the linear smoking machine 1 starts to smoke and collects all smoke components. Among them, the linear smoking machine 1 adopts the Canadian deep suction mode, the heating time of the heating device is 4 minutes, and the suction is completed after 8 puffs are drawn.
  • sample preparation solution is measured by inductively coupled plasma mass spectrometer, and the instrument conditions and parameters, detection method and step (2) are consistent. Then, the ratio of the mass-to-charge intensity of aluminum element to the mass-to-charge ratio intensity of the internal standard element was substituted into the standard working curve to obtain the content of aluminum element in the smoke aerosol of heat-not-burn cigarette sample A (as shown in Table 4).
  • this example tests the heat-not-burn cigarette sample B. All the steps are the same as those in the first example, to determine the amount of aluminum released in the mainstream smoke of the heat-not-burn cigarette sample B (as shown in Table 4). Show).
  • this example tests the heat-not-burn cigarette sample C.
  • the linear smoking machine 1 adopts the ISO standard smoking mode, the heating time is set to 4 minutes, and after 4 puffs, The suction is complete.
  • the other steps are the same as in the first embodiment, and the amount of aluminum released in the mainstream smoke of the heat-not-burn cigarette sample C is determined (as shown in Table 4).
  • the method of the present invention utilizes the traditional cigarette linear smoking machine for smoking of heat-not-burn cigarettes and the collection of full smoke components, without a special heat-not-burn cigarette smoking machine; multi-stage absorption bottles are connected in series to achieve full smoke composition capture Collection and determination of the amount of aluminum released; sample extraction, full smoke capture and absorption liquid treatment of heating non-combustion cigarettes are easy to operate, and the inductively coupled plasma mass spectrometer is convenient to determine, good stability, and good linear correlation , Good practicability, high sensitivity, and good repeatability.

Abstract

一种检测加热不燃烧卷烟烟气中铝释放量的方法，包括以下步骤：制备铝元素标准工作溶液；根据铝元素标准工作溶液，获取铝元素标准工作曲线；抽吸加热不燃烧卷烟，收集加热不燃烧卷烟的全烟气成分；根据收集的全烟气成分，获取样品制备溶液；根据样品制备溶液的测定分析，结合铝元素标准工作曲线，确定全烟气成分中的铝释放量。利用直线型吸烟机(1)进行加热不燃烧卷烟的抽吸和全烟气成分的捕集，无需加热不燃烧卷烟专用吸烟机；采用多级吸收瓶(3)串联，实现了全烟气成分捕集，并进行铝释放量的测定；简洁高效，稳定性好，具有线性相关性好、实用性好、灵敏度高以及重复性好的优点。

Description

一种检测加热不燃烧卷烟烟气中铝释放量的方法 技术领域
本发明涉及一种检测加热不燃烧卷烟烟气中铝释放量的方法，属于烟草检测技术领域。
背景技术
低温卷烟，即加热不燃烧卷烟(heat-not-burn cigarette)，通过外部热源对烟草物质进行加热，烟草物质中的雾化介质、香味成分和外加香通过加热产生类似于传统卷烟燃吸的烟雾，使消费者得到生理满足感。由于低温卷烟中的烟草物质只加热而不燃烧，且加热温度(250℃～350℃(摄氏度))远低于传统卷烟的燃烧温度(800℃～900℃)，因此，烟气有害成分和生物毒性大幅降低，侧流烟气和环境烟气也大幅度降低，主流烟气组成和传统卷烟有着明显差异。
为防止雾化剂甘油和丙二醇向卷烟纸表面的渗漏影响加热不燃烧卷烟烟支外观，同时能够更好的集聚热量，保持烟草原料的水分不发生较大的变化，在实际的加热不燃烧卷烟烟支生产过程中，很多企业采用铝箔纸作为卷烟纸卷制烟支，如飞利浦莫里斯公司的HEET烟支、湖北中烟工业有限责任公司的COO烟支等。铝和其化合物经常被用于食品添加剂，但是过量使用也会对人体健康造成一定的危害。世界卫生组织建议，每人每日Al(铝)的摄入量控制在0.004g(即4mg(毫克))以下，JECFA(联合国粮农组织和世界卫生组织下的食品添加剂联合专家委员会(Joint FAO/WHO Expert Committee on Food Additives))制定了铝的“暂定每周耐受摄入量”，人(全人群)终生每周每公斤体重经口摄入的铝不超过2mg(按照50kg体重计算，每人每天摄入约15mg)，就不会引起身体健康危害。
加热不燃烧卷烟作为新生事物，现有技术中还没有针对于加热不燃烧卷烟烟气组分的检测方法，也没有经过验证和认可的加热不燃烧卷烟专用吸烟机，更没有检测加热不燃烧卷烟烟气中铝释放量的方法。
发明内容
本发明的目的在于，提供一种检测加热不燃烧卷烟烟气中铝释放量的方法，其能够对加热不燃烧卷烟烟气气溶胶中的铝释放量进行检测，稳定性好，线性相关性好，实用性好，灵敏度高，重复性好。
为实现上述目的，本发明采取以下技术方案：一种检测加热不燃烧卷烟烟气中铝释放量的方法，包括以下步骤：制备铝元素标准工作溶液；根据所述铝元素标准工作溶液，获取铝元素标准工作曲线；抽吸加热不燃烧卷烟，收集所述加热不燃烧卷烟的全烟气成分；根据收集的所述全烟气成分，获取样品制备溶液；根据所述样品制备溶液的测定分析，结合所述铝元素标准工作曲线，确定所述全烟气成分中的铝释放量。
在一个具体实施例中，采用铝单元素标准溶液逐级稀释得到所述铝元素标准工作溶液，所述铝元素标准工作溶液包括铝单元素系列标准工作溶液。
在一个具体实施例中，根据铝元素标准工作溶液，采用外标法或内标法，获取铝元素标准工作曲线。
在一个具体实施例中，根据所述铝元素标准工作溶液，结合内标工作溶液，获取铝元素标准工作曲线。
在一个具体实施例中，采用 45Sc元素标准溶液稀释得到所述内标工作溶液。
在一个具体实施例中，所述铝单元素标准溶液和所述 45Sc元素标准溶液的介质均为第一硝酸溶液。
在一个具体实施例中，采用溶液捕集方式收集所述全烟气成分。
在一个具体实施例中，采用多个吸收瓶依次串联收集所述全烟气成分。
在一个具体实施例中，收集所述全烟气成分，包括以下步骤：(1)确定卷烟吸烟机，(2)将串联好的多个所述吸收瓶连接于所述卷烟吸烟机的夹持器后端与抽吸机构之间；(3)将所述加热不燃烧卷烟的烟支端插入加热器具，嘴棒端插入所述卷烟吸烟机的所述夹持器内；(4)利用所述加热器具进行加热，所述卷烟吸烟机开始抽吸至抽吸完成，收集全烟气成分。
在一个具体实施例中，根据所述卷烟吸烟机的抽吸模式和所述加热器具设 置的加热时间确定抽吸口数，达到所述抽吸口数后，所述卷烟吸烟机抽吸完成。
在一个具体实施例中，所述卷烟吸烟机的所述抽吸模式为加拿大深度抽吸模式或标准抽吸模式。
在一个具体实施例中，所述卷烟吸烟机采用所述加拿大深度抽吸模式包括每口抽吸容量55毫升，每口抽吸时间2秒，相邻抽吸口数之间间隔时间28秒；所述加拿大深度抽吸模式每分钟抽吸2口。
在一个具体实施例中，所述卷烟吸烟机采用标准抽吸模式包括每口抽吸容量35毫升，每口抽吸时间2秒，相邻抽吸口数之间间隔时间58秒；所述标准抽吸模式每分钟抽吸1口。
在一个具体实施例中，所述卷烟吸烟机为直线型吸烟机。
在一个具体实施例中，向所述吸收瓶中加入氧化剂，将所述吸收瓶中的吸收液完全转入容量瓶中，定容后，获取所述样品制备溶液。
在一个具体实施例中，所述吸收瓶为石英吸收瓶，所述石英吸收瓶内的吸收液为第二硝酸溶液。
在一个具体实施例中，向所述石英吸收瓶中加入所述氧化剂将所述全烟气成分中的所述铝元素完全氧化，震荡后，将所述石英吸收瓶中的所述吸收液和洗涤剂一并完全转入所述容量瓶中，采用所述第一硝酸溶液定容至刻度，摇匀，获取所述样品制备溶液。
在一个具体实施例中，所述第一硝酸溶液的体积分数为2％～8％；所述第二硝酸溶液的体积为15～25毫升，所述第二硝酸溶液的体积分数为5％～15％。
在一个具体实施例中，采用电感耦合等离子体质谱仪对所述样品制备溶液进行测定。
在一个具体实施例中，所述铝单元素系列标准工作溶液包括浓度为0、0.5、1.0、2.0、5.0、10.0、20.0和50.0微克每升的铝单元素系列标准工作溶液。
在一个具体实施例中，所述内标工作溶液的浓度能够根据所述铝单元素系列标准工作溶液的浓度梯度和实际检测样品的含量范围确定。
在一个具体实施例中，所述内标工作溶液的浓度为10微克每升。
本发明由于采取以上技术方案，其具有以下优点：1、本发明建立了一种检测加热不燃烧卷烟主流烟气中铝释放量的方法，精密度好，准确度高，铝元素回收率高，适合加热不燃烧卷烟主流烟气中铝元素释放量的定量分析。2、本发明的方法能够充分利用直线型吸烟机进行加热不燃烧卷烟的抽吸和全烟气成分的捕集，无需加热不燃烧卷烟专用吸烟机，简洁高效。3、本发明根据加热不燃烧卷烟的特点，采用多级吸收瓶串联，能够实现全烟气成分捕集，并进行铝释放量的测定。4、本发明加热不燃烧卷烟的抽吸、全烟气捕集和吸收液处理操作简捷，以及采用电感耦合等离子体质谱仪对样品制备溶液进行测定，便捷，稳定性好，具有较好的线性相关性，实用性好。5、本发明的方法灵敏度高，重复性好。
本发明的其它特征和优点将在随后的说明书中阐述，并且部分的从说明书中变得显而易见，或者通过实施本发明而了解。本发明的目的和其他优点可通过在说明书、权利要求书以及附图中所特别指出的结构来实现和获得。
附图说明
为了更清楚的说明本发明实施例中的技术方案，下面将对实施例描述中所需要的附图做简单的介绍：
图1是本发明的检测加热不燃烧卷烟烟气中铝释放量的方法的一个具体实施例的流程示意图；
图2是本发明的一个具体实施例中直线型吸烟机夹持器、抽吸单元与串联的吸收瓶相连接的示意图；
图3是本发明的一个具体实施例中石英吸收瓶的结构示意图。
具体实施方式
以下将结合附图及实施例来详细说明本发明的实施方式，借此对本发明如何应用技术手段来解决技术问题，并达成技术效果的实现过程能充分理解并据以实施。需要说明的是，只要不构成冲突，本发明中的各个实施例以及各实施例中的各个特征可以相互结合，所形成的技术方案均在本发明的保护范围之内。
如图1所示，本发明提出的检测加热不燃烧卷烟烟气中铝释放量的方法，包括以下步骤：
(1)制备铝元素标准工作溶液
确定铝单元素标准溶液为标准储备液；采用铝单元素标准溶液逐级稀释得到铝单元素系列标准工作溶液。根据实际需要，铝元素标准工作溶液即配即用。
进一步地，铝元素标准工作溶液的配制包括以下内容：确定铝单元素标准溶液的介质为第一硝酸溶液，其标准值为10mg/L(毫克/升)。其中，铝单元素系列标准工作溶液的浓度梯度能够根据实际检测样品的含量范围确定。优选的，铝单元素系列标准工作溶液的浓度分别为0、0.5、1.0、2.0、5.0、10.0、20.0和50.0μg/L(微克/升)。
在一个具体的实施例中，第一硝酸溶液的体积分数为2％～8％。优选的，第一硝酸溶液的体积分数为5％。
(2)根据铝元素标准工作溶液，获取铝元素标准工作曲线，确定铝元素的检测限和定量限
根据铝元素标准工作溶液，采用外标法或内标法，获取铝元素标准工作曲线。外标法是与内标法相对，指添加一定量的标准品(对照品)于空白检材中制成对照样品，与未知检材平行地进行样品处理并检测，根据对照样品响应值与其中所添加标准品(对照品)浓度的函数关系推算未知检材中被测组分浓度的定量方法。例如，在色谱法中，想知道被测样品浓度。可以用外标法首先用待测组份的标准样品绘制工作曲线，测出各峰的峰高或峰面积对应的样品浓度，绘制出标准曲线。实际应用时，测出峰高或峰面积对应标准曲线，就可以得到样品浓度。优选的，根据铝元素标准工作溶液，结合内标工作溶液，获取铝元素标准工作曲线。具体的，在线加入内标工作溶液，分别吸取多级铝单元素系列标准工作溶液注入ICP-MS(电感耦合等离子体质谱仪)中进行测定，以铝元素含量与内标元素含量的比值为横坐标，铝元素质荷比强度与内标元素质荷比强度的比值为纵坐标，建立铝元素工作曲线。接着，对校正数据进行线性回归得到标准工作曲线和相关系数。优选的，将浓度为0.5微克/升的铝单元素标准工作溶液进样多次，计算测定结果的标准偏差，分别以标准偏差的3倍和10倍 确定铝元素的检测限和定量限。结果表明，铝元素的工作曲线线性良好，相关系数高于0.999；铝元素的定量限远低于样品制备溶液中目标物的含量，适合定量分析。优选的，采用 45Sc元素标准溶液稀释得到内标工作溶液。
进一步地，内标工作溶液的配制包括以下内容：确定 45Sc元素标准溶液的介质为第一硝酸溶液，其标准值10mg/L(毫克每升)。其中，内标工作溶液的浓度能够根据铝单元素系列标准工作溶液的浓度梯度和实际检测样品的含量范围确定。优选的，内标工作溶液的浓度为10.0μg/L(微克每升)。
在一个优选的实施例中，确定电感耦合等离子体质谱仪的测定条件(如表1所示)。其中，电感耦合等离子体质谱仪的射频功率为1280w(瓦)，载气流速为1.11L/min(升/分钟)，进样速率为0.1mL/min(毫升/分钟)，获取模式为全定量分析，重复次数为3次。
在一个具体的实施例中，确定铝元素的检测限为0.39纳克/升。
在一个具体的实施例中，确定铝元素的定量限为1.31纳克/升。
表1电感耦合等离子体质谱仪测定条件
参数 工作条件
射频功率 1280w
载气流速 1.11L/min
进样速率 0.1mL/min
获取模式 全定量分析
重复次数 3
在一个具体的实施例中，测定铝元素的质量数为27。确定内标元素为 45Sc。确定积分时间为0.5秒(如表2所示)。
表2元素测定质量数、内标元素、积分时间
元素 测定质量数 内标元素 积分时间/s
Al 27 45Sc 0.5
(3)抽吸加热不燃烧卷烟，收集加热不燃烧卷烟的全烟气成分
抽吸加热不燃烧卷烟，收集全烟气成分包括以下步骤：
①确定卷烟吸烟机1(如图2所示)，
②通过连接管路2将串联好的多个吸收瓶3连接于卷烟吸烟机1的夹持器4后端与抽吸单元5之间，所有连接管路2连接好后，进行气密性检查；
③将加热不燃烧卷烟烟支6的烟支端插入加热器具7中，嘴棒端插入卷烟吸烟机1的夹持器4内；
④开启加热器具7的开关预热，达到预热时间后，卷烟吸烟机1开始抽吸至抽吸完成，收集全烟气成分。
进一步地，根据卷烟吸烟机1的抽吸模式和加热器具7设置的加热时间确定抽吸口数，达到抽吸口数后，卷烟吸烟机1抽吸完成。
在一个具体的实施例中，卷烟吸烟机1的抽吸模式为加拿大深度抽吸模式或ISO标准抽吸模式。
在一个具体的实施例中，卷烟吸烟机1采用加拿大深度抽吸模式包括每口抽吸容量55毫升，每口抽吸时间2秒，相邻抽吸口数之间间隔时间28秒。确定加拿大深度抽吸模式每分钟抽吸2口。
在一个具体的实施例中，卷烟吸烟机1采用ISO标准抽吸模式包括每口抽吸容量35毫升，每口抽吸时间2秒，相邻抽吸口数之间间隔时间58秒。确定ISO标准抽吸模式每分钟抽吸1口。
在一个具体的实施例中，加热器具7设置的持续加热的时间为3～6分钟，采用加拿大深度抽吸模式抽吸6～12口，采用ISO标准抽吸模式抽吸3～6口，达到抽吸口数后，抽吸完成。
在一个具体的实施例中，卷烟吸烟机1为直线型吸烟机(如图2所示)。
在一个具体的实施例中，根据实际需要，自主设计卷烟吸烟机的抽吸模式。
在一个具体的实施例中，吸收瓶3内盛放有第二硝酸溶液作为吸收液，用于吸收烟气。
在一个具体的实施例中，第二硝酸溶液的体积为15～25毫升，第二硝酸溶液的体积分数为5％～15％。优选的，第二硝酸溶液的体积为20毫升，第二硝酸溶液的体积分数10％。
在一个优选的实施例中，吸收瓶3为石英吸收瓶(多孔玻板吸收瓶)，石英吸收瓶3的吸收液为第二硝酸溶液。
在一个具体的实施例中，如图3所示，石英吸收瓶3包括瓶体31，在瓶体31的第一侧设置有进气口32，收集的全烟气成分从进气口32进入。在瓶体31的第二侧设置有出气口33，被第二硝酸溶液吸收后的烟气从出气口33逸出。瓶体31的内部设置有直玻璃管34，直玻璃管34的顶部与进气口32连通，直玻璃管34的底部设置有半玻璃球体35，半玻璃球体35能够增加全烟气成分与吸收液的接触面积，缓解烟气逸出的速度。在半玻璃球体35的底部设置有砂芯滤板36，砂芯滤板36能够增加烟气逸出的阻力，同时使烟气经过砂芯滤板36后分散为多个小气泡逸出，使烟气更充分接触石英吸收瓶3，使吸收更快速、安全。在瓶体31的侧壁上设置有磨砂标准口37，能够提高密封性。
在一个具体的实施例中，砂芯滤板36设置成石英砂芯滤板。
在一个具体的实施例中，石英砂芯滤板36的直径为100～160微米。
在一个具体的实施例中，将5个分别加有第二硝酸溶液的石英吸收瓶3进行串联，测定每个石英吸收瓶3中铝的含量。确定第1和第2个石英吸收瓶3中检出了铝元素，第3、第4以及第5个石英吸收瓶3中均未检出铝。
在一个优选的实施例中，石英吸收瓶3的数目为两个，能够实现主流烟气中铝元素的有效捕集。
在一个优选的实施例中，如图2、图3所示，两个石英吸收瓶3之间通过连接管路2连接。其中，第一石英吸收瓶3的进气口32通过连接管路2与全烟气成分的出口端(夹持器4后端，如图2所示)连接，第一石英吸收瓶3的出气口33通过连接管路2连接第二石英吸收瓶3的进气口32，第二石英吸收瓶3的出气口33与抽吸单元5连接，能够使全烟气充分被吸收液吸收。
(4)根据收集的全烟气成分，获取样品制备溶液
向吸收瓶3中加入氧化剂将全烟气成分中的铝元素充分氧化，将吸收瓶3中的吸收液完全转入容量瓶中，定容后，获取样品制备溶液。具体的，向石英吸收瓶3中加入氧化剂将全烟气成分中的铝元素充分氧化，超声震荡后，将石英吸收瓶3的吸收液和洗涤液一并完全转入容量瓶中，采用第一硝酸溶液定容 至刻度，摇匀，获取样品制备溶液。
在一个具体的实施例中，氧化剂为过氧化氢。
在一个具体的实施例中，过氧化氢的体积为5～10mL(毫升)。优选的，过氧化氢的体积为5毫升。
在一个具体的实施例中，超声震荡的时间为20～50分钟。优选的，超声震荡的时间为30分钟。
在一个具体的实施例中，容量瓶为塑料容量瓶。优选的，塑料容量瓶体积为100毫升。
(5)根据样品制备溶液的测定分析，结合铝元素标准工作曲线，确定全烟气成分中的铝释放量
采用电感耦合等离子体质谱仪对样品制备溶液进行测定。具体的，确定电感耦合等离子体质谱仪的测定条件(如表1所示)。确定铝元素质量数为27。确定内标元素为 45Sc。确定积分时间为0.5秒(如表2所示)。
以铝元素质荷比强度与内标元素质荷比强度的比值代入铝元素标准工作曲线，求得样品制备溶液中烟气气溶胶中铝元素的含量。
下面列举三个具体的实施例
实施例一
(1)制备铝元素标准工作溶液
确定铝单元素标准溶液为标准储备液，铝单元素标准溶液的介质为5％(体积分数)硝酸溶液，其标准值为10毫克/升。接着，准确移取1.0毫升铝单元素标准溶液于100毫升塑料容量瓶，并采用5％(体积分数)硝酸溶液定容，得到浓度为100微克/升的工作溶液。然后，取8个50毫升的塑料容量瓶，分别准确移取一定体积的铝单元素标准溶液，并采用5％(体积分数)硝酸溶液定容，逐级稀释得到0、0.5、1.0、2.0、5.0、10.0、20.0和50.0微克/升的铝单元素系列标准工作溶液。
(2)根据铝元素标准工作溶液，结合内标工作溶液，获取铝元素标准工作曲线
确定 45Sc元素标准溶液的介质为5％(体积分数)硝酸溶液，其标准值为10毫克/升。准确移取0.1毫升的 45Sc元素标准溶液于100毫升塑料容量瓶内，得到浓度为10.0微克/升的内标工作溶液。接着，在线加入内标工作溶液，分别吸取上述8级铝单元素系列标准工作溶液(浓度为0、0.5、1.0、2.0、5.0、10.0、20.0和50.0微克/升的铝单元素系列标准工作溶液)注入电感耦合等离子体质谱仪中进行测定。其中，电感耦合等离子体质谱仪的参数(如表1所示)，铝元素质量数、对应内标元素及积分时间(如表2所示)。然后，以铝元素含量与内标元素含量的比值为横坐标，铝元素质荷比强度与内标元素质荷比强度的比值为纵坐标，建立铝元素工作曲线。并对校正数据进行线性回归得到标准工作曲线和相关系数；将0.5微克/升的铝单元素标准工作溶液进样8次，计算测定结果的标准偏差，分别以标准偏差的3倍和10倍确定检测限和定量限，确定计算结果(如表3所示)。结果表明，铝元素的工作曲线线性良好，相关系数高于0.999；铝元素的定量限低于样品制备溶液中目标物的含量，适合定量分析。
表3铝元素的标准工作曲线与检测限
Figure PCTCN2020094851-appb-000001
(3)抽吸加热不燃烧卷烟，收集加热不燃烧卷烟的全烟气成分
确定好传统卷烟直线型吸烟机1(如2所示)后，将2个加有20毫升10％(体积分数)硝酸溶液的石英吸收瓶3通过连接管路2连接，将2个石英吸收瓶3连接于夹持器4后端与抽吸单元5之间，所有连接管路2连接好之后检查气密性；接着，将加热不燃烧卷烟样品A的烟支端插入加热器具7，嘴棒端插入夹持器4，开启加热器具7开关预热30s，达到预热时间后，直线型吸烟机1开始抽吸，并收集全烟气成分。其中，直线型吸烟机1采用加拿大深度抽吸模式，加热器具设置的加热时间为4min，抽吸8口后，抽吸完成。
(4)根据收集的全烟气成分，获取样品制备溶液
向串联好的2个石英吸收瓶3中分别加入5毫升过氧化氢，超声震荡30分钟；将2个石英吸收瓶3中的吸收液和洗涤液一并转入100毫升塑料容量瓶中， 并用5％(体积分数)硝酸溶液定容至刻度，摇匀，得到样品制备溶液。
(5)根据样品制备溶液的测定分析，结合铝元素标准工作曲线，确定全烟气成分中的铝释放量
对样品制备溶液进行电感耦合等离子体质谱仪测定，仪器条件和参数、检测方法和步骤(2)一致。然后，以铝元素质荷比强度与内标元素质荷比强度的比值代入标准工作曲线，求取加热不燃烧卷烟样品A的烟气气溶胶中铝元素的含量(如表4所示)。
表4三个实施例加热不燃烧卷烟样品分析结果(ng/支)
Figure PCTCN2020094851-appb-000002
(6)精密度与回收率实验
将样品制备溶液分为四份，其中1份为参比，另外3份分别加入高、中、低三种不同浓度水平的铝单元素标准工作溶液，每个添加水平重复测定2个样品制备溶液。对样品制备溶液进行测定，并由样品制备溶液中的原含量、加标量以及加标测定量计算回收率(如表5所示)。结果表明，铝元素的加标回收率在98.8％～102.4％之间。将加入中等浓度铝单元素标准工作溶液的萃取液样品重复分析6次，确定铝元素的相对标准偏差(RSD)的计算结果为1.17％。
表5分析方法的加标回收率
Figure PCTCN2020094851-appb-000003
实施例二
在上述实施例的基础上，本实例对加热不燃烧卷烟样品B进行检测，所有骤与实施例一均相同，确定加热不燃烧卷烟样品B的主流烟气中铝元素释放 量(如表4所示)。
实施例三
在上述实施例的基础上，本实例对加热不燃烧卷烟样品C进行检测，其中，直线型吸烟机1采用ISO标准抽吸模式，加热器具设置的加热时间为4分钟，抽吸4口后，抽吸完成。其它步骤与实施例一均相同，确定加热不燃烧卷烟样品C主流烟气中铝元素释放量(如表4所示)。
本发明方法利用传统卷烟直线型吸烟机进行加热不燃烧卷烟的抽吸和全烟气成分的捕集，无需加热不燃烧卷烟专用吸烟机；采用多级吸收瓶串联，实现了全烟气成分捕集，并进行铝释放量的测定；加热不燃烧卷烟的样品抽吸、全烟气捕集和吸收液处理操作简单，采用电感耦合等离子体质谱仪测定便捷，稳定性好，具有线性相关性好，实用性好、灵敏度高、重复性好的优点。
虽然本发明所公开的实施方式如上，但所述的内容只是为了便于理解本发明而采用的实施方式，并非用以限定本发明。任何本发明所属技术领域内的技术人员，在不脱离本发明所公开的精神和范围的前提下，可以在实施的形式上及细节上作任何的修改与变化，但本发明的专利保护范围，仍须以所附的权利要求书所界定的范围为准。

Claims (22)

  1. 一种检测加热不燃烧卷烟烟气中铝释放量的方法，其特征在于，包括以下步骤：
    制备铝元素标准工作溶液；
    根据所述铝元素标准工作溶液，获取铝元素标准工作曲线；
    抽吸加热不燃烧卷烟，收集所述加热不燃烧卷烟的全烟气成分；
    根据收集的所述全烟气成分，获取样品制备溶液；
    根据所述样品制备溶液的测定分析，结合所述铝元素标准工作曲线，确定所述全烟气成分中的铝释放量。
  2. 根据权利要求1所述的方法，其特征在于，采用铝单元素标准溶液逐级稀释得到所述铝元素标准工作溶液，所述铝元素标准工作溶液包括铝单元素系列标准工作溶液。
  3. 根据权利要求1或2所述的方法，其特征在于，根据铝元素标准工作溶液，采用外标法或内标法，获取铝元素标准工作曲线。
  4. 根据权利要求3所述的方法，其特征在于，根据所述铝元素标准工作溶液，结合内标工作溶液，获取铝元素标准工作曲线。
  5. 根据权利要求4所述的方法，其特征在于，采用 45Sc元素标准溶液稀释得到所述内标工作溶液。
  6. 根据权利要求5所述的方法，其特征在于，所述铝单元素标准溶液和所述 45Sc元素标准溶液的介质均为第一硝酸溶液。
  7. 根据权利要求1所述的方法，其特征在于，采用溶液捕集方式收集所述全烟气成分。
  8. 根据权利要求7所述的方法，其特征在于，采用多个吸收瓶依次串联收集所述全烟气成分。
  9. 根据权利要求8所述的方法，其特征在于，收集所述全烟气成分，包括以下步骤：
    (1)确定卷烟吸烟机，
    (2)将串联好的多个所述吸收瓶连接于所述卷烟吸烟机的夹持器后端与抽吸机构之间；
    (3)将所述加热不燃烧卷烟的烟支端插入加热器具，嘴棒端插入所述卷烟吸烟机的所述夹持器内；
    (4)利用所述加热器具进行加热，所述卷烟吸烟机开始抽吸至抽吸完成，收集全烟气成分。
  10. 根据权利要求9所述的方法，其特征在于，根据所述卷烟吸烟机的抽吸模式和所述加热器具设置的加热时间确定抽吸口数，达到所述抽吸口数后，所述卷烟吸烟机抽吸完成。
  11. 根据权利要求10所述的方法，其特征在于，所述卷烟吸烟机的所述抽吸模式为加拿大深度抽吸模式或标准抽吸模式。
  12. 根据权利要求11所述的方法，其特征在于，所述卷烟吸烟机采用所述加拿大深度抽吸模式包括每口抽吸容量55毫升，每口抽吸时间2秒，相邻抽吸口数之间间隔时间28秒；所述加拿大深度抽吸模式每分钟抽吸2口。
  13. 根据权利要求11所述的方法，其特征在于，所述卷烟吸烟机采用标准抽吸模式包括每口抽吸容量35毫升，每口抽吸时间2秒，相邻抽吸口数之间间隔时间58秒；所述标准抽吸模式每分钟抽吸1口。
  14. 根据权利要求9所述的方法，其特征在于，所述卷烟吸烟机为直线型吸烟机。
  15. 根据权利要求9所述的方法，其特征在于，向所述吸收瓶中加入氧化剂，将所述吸收瓶中的吸收液完全转入容量瓶中，定容后，获取所述样品制备溶液。
  16. 根据权利要求15所述的方法，其特征在于，所述吸收瓶为石英吸收瓶，所述石英吸收瓶内的吸收液为第二硝酸溶液。
  17. 根据权利要求16所述的方法，其特征在于，向所述石英吸收瓶中加入所述氧化剂将所述全烟气成分中的所述铝元素完全氧化，震荡后，将所述石英吸收瓶中的所述吸收液和洗涤剂一并完全转入所述容量瓶中，采用所述第一硝酸溶液定容至刻度，摇匀，获取所述样品制备溶液。
  18. 根据权利要求17所述的方法，其特征在于，所述第一硝酸溶液的体积分数为2％～8％；所述第二硝酸溶液的体积为15～25毫升，所述第二硝酸溶液的体积分数为5％～15％。
  19. 根据权利要求1所述的方法，其特征在于，采用电感耦合等离子体质谱仪对所述样品制备溶液进行测定。
  20. 根据权利要求2所述的方法，其特征在于，所述铝单元素系列标准工作溶液包括浓度为0、0.5、1.0、2.0、5.0、10.0、20.0和50.0微克每升的铝单元素系列标准工作溶液。
  21. 根据权利要求2所述的方法，其特征在于，所述内标工作溶液的浓度能够根据所述铝单元素系列标准工作溶液的浓度梯度和实际检测样品的含量范围确定。
  22. 根据权利要求21所述的方法，其特征在于，所述内标工作溶液的浓度为10微克每升。
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