CN110879266B - Device and method for measuring heated migration quantity of filter stick additive - Google Patents
Device and method for measuring heated migration quantity of filter stick additive Download PDFInfo
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- CN110879266B CN110879266B CN201911083679.4A CN201911083679A CN110879266B CN 110879266 B CN110879266 B CN 110879266B CN 201911083679 A CN201911083679 A CN 201911083679A CN 110879266 B CN110879266 B CN 110879266B
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- 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
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- 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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
Abstract
The invention relates to a device and a method for measuring the heated migration quantity of a filter rod additive. The device comprises a hot air blower, a constant temperature box, a purging pipe, a purging component collector and a smoking machine; an air thermostatic tube is fixed in the incubator; the air inlet end of the air thermostatic tube is fixed at the air inlet, and the air outlet end is fixed at the air outlet; an air inlet of the incubator is connected with the air heater, and an air outlet of the incubator is connected with an air inlet end of the purging pipe; the sweeping component collector comprises a filter holder, a Cambridge filter and a refrigerant container; the air outlet end of the purging pipe is connected with one end of the filter disc holder; the other end of the filter disc holder is connected with a smoking machine; the filter disc holder is internally provided with a Cambridge filter disc in a clamping way and is arranged in the refrigerant container. The invention can simulate the cigarette suction to directly acquire the migration condition of the filter stick additive, and provides a simpler, more convenient and reliable method for evaluating the safety and efficacy of the filter stick additive.
Description
Technical Field
The invention belongs to the technical field of experimental instruments, and particularly relates to a novel device for simulating cigarette smoke flow eluting filter tip additives and measuring migration quantity of heated migration components and a novel method for measuring migration quantity of the heated migration components by adopting the novel device.
Background
At present, as people pay more and more attention to self health, low-tar cigarettes gradually become the main development flow of the cigarette market, but the low-tar cigarettes also bring about rapid reduction of cigarette aroma and loss of smoking comfort experience, and bring about great influence to cigarette consumers. Therefore, the flavoring of the filter tip becomes an important way for improving the smoking experience of the cigarette, different cigarette products such as a bead-blasting cigarette, a cigarette added with a flavoring line, a filter tip tow flavoring or a cigarette added with special flavor particles, especially a bead-blasting cigarette appear at home and abroad in recent years, and the bead-blasting cigarette has rapid development in domestic and foreign markets along with the increasing of the diversified and personalized demands of the products because the flavor of the cigarette consumer in the smoking process is controllable, different flavor characteristics can be highlighted, various smoking demands can be met, and the supplementing and modifying of the smoke flavor can be performed to a certain extent.
As filter perfuming technology has been widely used in cigarette products, the safety problem of filter additives has also attracted consumer attention. Different from food, the cigarette has a unique consumption mode, and the additive in the filter tip is eluted mainly through hot flow smoke so as to carry partial aroma components and improve functional components, and the main flow smoke enters the mouth of a consumer, so that the effects of enhancing aroma and improving flavor are achieved, the filter tip additive is not directly contacted with the mouth of the consumer, and the filter tip additive is always in the dynamic process of elution of the hot flow of smoke.
Most of the existing safety detection of the filter tip additive is to test the filter tip independently, and peel off the filter tip from the cigarette smoking process or analyze the smoke after the cigarette is burnt, wherein the former is disjointed from the actual smoking process of the cigarette, and the latter is interfered by complex background components generated after the tobacco shred burning of the cigarette, so that it is very difficult to obtain accurate analysis results. Although some filter stick additive migration amount detection devices and detection methods are reported; however, the device has a complicated structure, is inconvenient to operate, and has large measurement result deviation (such as CN 201810467715.6); the characteristic of volatile thermomigration components is not considered to collect the refrigerant, so that the volatile components are lost to influence analysis results (for example, CN201429591Y and CN 203365266U) and the like. Therefore, there is a need for a simpler, scientific, and rational analysis method and apparatus for simulated migration of filter additives and corresponding determination of migration.
Disclosure of Invention
The invention overcomes the defects in the prior art, and provides the device and the method for measuring the heated migration quantity of the filter stick additive, which are simple to operate and can truly simulate the elution of cigarette smoke flow. The method and the device not only can truly simulate the elution of the cigarette airflow on the filter tip, but also can avoid the influence of complex background generated by burning tobacco shreds in the traditional smoke analysis on the analysis result. The novel method and the device not only can objectively evaluate the efficacy and the safety of the filter tip additive, but also can provide better technical support for various aspects of cigarette product quality safety, smoke physiological feeling, smoking, health and the like.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a device for measuring the heated migration quantity of a filter stick additive comprises a hot air blower, an incubator, a purging pipe, a purging component collector and a smoking machine;
the constant temperature box is provided with an air inlet, an air outlet and an air outlet; an air thermostatic tube is fixed in the incubator; the air inlet end of the air thermostatic tube is fixed at the air inlet, and the air outlet end of the air thermostatic tube is fixed at the air outlet;
the air heater is connected with an air inlet of the constant temperature box; the air outlet of the incubator is connected with the air inlet end of the purging pipe;
the sweeping component collector comprises a filter holder, a Cambridge filter and a refrigerant container; the filter disc holder and the Cambridge filter disc are both arranged in the refrigerant container;
the air outlet end of the purging pipe is connected with one end of the filter disc holder; the other end of the filter disc holder is connected with a smoking machine;
the filter holder holds a Cambridge filter.
Further, it is preferable that temperature sensors are provided at both the air outlet and the air outlet.
Further, it is preferable that the dead volume of the connecting line between the air outlet end of the air thermostatic tube and the purge tube is not more than 1mL.
Further, it is preferable that the purge pipe includes a pipe body and a pipe cap connected to each other; the opening end of the tube body is provided with a seal ring bayonet; a sealing ring matched with the sealing ring bayonet is fixed in the pipe cap; the air inlet end of the purging pipe is arranged at the bottom of the pipe body, and the air outlet end of the purging pipe is arranged on the pipe cap.
Further, it is preferable that a screen plate is provided at an air inlet end of the purge pipe, and an air inlet direction is perpendicular to a plane in which the screen plate is located.
Further, it is preferable that the material of the purge tube is polypropylene plastic.
Further, it is preferable that the air thermostat pipe has an S-shape in the thermostat.
Further, it is preferable that the inner diameter of the purge tube is the same as the outer diameter of the filter rod, and the length of the space in the purge tube is the same as the length of the filter rod.
The invention also provides a method for measuring the thermal migration quantity of the filter rod additive, which adopts the device for measuring the thermal migration quantity of the filter rod additive and comprises the following steps:
and (3) opening the air heater, wrapping the filter stick additive to be tested by adopting acetate fibers after the temperatures at the air outlet and the air outlet are stable, loading the filter stick additive into a purging pipe, adding a refrigerant into a refrigerant container, immersing a filter holder into the refrigerant, starting a smoking machine for smoking, blowing out thermomigration components in a sample to be tested by air flow through the purging pipe in the smoking process of the smoking machine, capturing the thermomigration components by a Cambridge filter, and measuring the migration quantity of the captured thermomigration components by a static headspace-gas chromatography-mass spectrometry.
Further, it is preferable that the smoking mode of the smoking machine is an ISO standard smoking mode or a canadian deep smoking mode; the refrigerant is ice water, oil, dry ice or liquid nitrogen.
Further, it is preferred that the specific parameters of static headspace-gas chromatography-mass spectrometry are:
static headspace conditions: sample equilibrium temperature: 160. the temperature is lower than the temperature; sample ring: 3.0 mL; sample ring temperature: 160. the temperature is lower than the temperature; transmission line temperature: 180. the temperature is lower than the temperature; sample equilibration time: 30.0 min; sample bottle pressurization pressure: 138 kPa; pressurizing time: 0.20 min; inflation time: 0.20 min; sample loop equilibration time: 0.05 min; sample introduction time: 1.0 min;
gas chromatography conditions: chromatographic column: a VOC capillary column with the specification of 60 m multiplied by 0.32 mm multiplied by 1.8 mu m; carrier gas: helium with purity more than or equal to 99.999%; sample inlet temperature: 200 ℃; constant flow mode, column flow 2.0 mL/min, split ratio 1:1; programming temperature: the initial temperature is 40 ℃, and the temperature is kept for 2min; raising the temperature to 160 ℃ at a heating rate of 4 ℃/min; then the temperature is raised to 210 ℃ at the heating rate of 10 ℃/min, and the temperature is kept for 10 min;
mass spectrometry conditions: auxiliary interface temperature: 220. the temperature is lower than the temperature; ionization mode: an electron bombardment source (EI); ionization energy: 70 eV; ion source temperature: 230. the temperature is lower than the temperature; quadrupole temperature: 150. the temperature is lower than the temperature; solvent delay time: 4.0 min; the full-scanning monitoring mode is carried out, and the scanning range is 29 amu to 350 amu.
The analysis conditions are only commonly referred, and matched analysis conditions can be selected according to the actual conditions of the to-be-detected objects.
The working principle of the invention is as follows:
when the cigarette with the filter stick additive is smoked, the hot air flow of the cigarette passes through the cigarette body and enters the filter stick to carry out thermal elution on the filter stick additive, wherein partial matters capable of thermal migration gradually elute and are mixed in the smoke gas to enter human organs under the flushing of the dynamic hot air flow, the whole process is a dynamic migration process, and the device for measuring the thermal migration quantity of the filter stick additive is designed based on the process, so that the migration condition and the migration behavior of a smoker when smoking the cigarette with the filter stick additive are simulated.
The air heater and the incubator are used for providing hot air which simulates the actual smoking smoke flow temperature of the cigarettes. The temperature and air pressure of hot air blown out by the hot air blower alone are considered to fluctuate greatly. In the invention, an incubator is added behind the air heater. Hot air blown by the hot air blower enters an air thermostatic tube of the incubator from the air inlet, so that the further accurate control and stabilization of the temperature are realized. When the smoking machine is in a non-smoking state, hot air flows out from an air outlet of the incubator and is discharged to the external environment from an air outlet; when the smoking machine is in a smoking state, hot air passes through the purging pipe under the action of vacuum negative pressure, and the cigarette smoke flow is simulated to elute filter stick additives in the purging pipe. In addition to more accurate temperature control, the oven also serves to maintain a constant hot air pressure.
Temperature sensors are arranged at the air outlet and the air outlet of the incubator, so that the temperature and the temperature fluctuation of the air in the incubator can be accurately indicated. The hot air generated by the air heater and the incubator is heated by numerical control electricity, so that synchronous numerical control program heating (cooling) can be realized; different temperatures can be simulated for sucking cigarettes mouth by mouth, and the filter stick additive is purged mouth by heating through programming; the maximum risk principle of the migration is also followed, and each mouth simulates the highest temperature of the smoke flow of the cigarette to purge the filter stick additive.
The size of the purging pipe is matched with that of a cigarette filter tip (the purging pipe has various specifications such as a conventional cigarette filter tip, a middle-count cigarette filter tip, a fine-count cigarette filter tip, a long filter tip, a broken filter tip and the like), and purging pipes with different sizes can be freely replaced according to the simulated cigarette specifications.
The filter stick additives (the explosion beads, the aroma lines, the particles and the like) are wrapped in acetate fibers and then are rapidly filled into the purging pipe, and the explosion bead samples are wrapped, then are crushed and then are filled; the suction resistance of the filter stick can be simulated and adjusted by the dosage (packing tightness) of the acetate fiber.
The purging pipe is of a cutting sleeve structure with a sealing ring, after an object to be tested is filled in the purging pipe, the sealing ring is clamped on a bayonet of the sealing ring, so that a filter stick for simulation test can be formed and sealing is realized, and a screen plate is arranged at the air inlet end of the purging pipe, so that air flow can uniformly pass through the filled simulation filter stick when the smoking machine smokes.
In order to avoid the temperature loss of the air flow through the pipeline when the pipeline is connected, the purging pipe is preferably directly connected to the constant temperature box, the dead volume is avoided, and the temperature of the purging air flow and the set temperature can be kept completely consistent.
The filter holder of the present invention incorporates a Cambridge filter for capturing migrating agents. In order to more completely collect volatile components and reduce the loss of the volatile components in the analysis process, the filter holder is arranged in a refrigerant container. In actual test, different condensing mediums (such as ice water bath, oil bath, dry ice bath or liquid nitrogen bath) can be flexibly selected according to the volatility of the migration components to be tested, so that the required condensing temperature control of the filter disc holder is realized.
The smoking machine is a conventional smoking machine for cigarette smoke analysis, and can be a linear smoking machine, a rotary disc type smoking machine, a single-duct smoking machine and the like. The puff parameters of the smoking machine may be ISO standard puff pattern (1 puff per puff at 1 minute intervals, 35mL puff volume per puff duration of 2 seconds); the model Canadian deep-pumping mode (pumping 1 port every 0.5 minute interval, pumping capacity of 50 mL ports every 2 seconds duration) is also possible.
The thermomigration component trapped by the method is analyzed by a static headspace-gas chromatography-mass spectrometry method, the target compound is qualitatively determined according to the spectrum library retrieval result of chromatographic peaks, and the target compound is quantified according to the peak area.
To understand the mobility of the thermomigration component of the filter plug additive, the total content of thermomigration component in the filter plug additive is also determined. The total content was also determined by static headspace-gas chromatography-mass spectrometry. The filter rod additives were directly placed into headspace vials without purging for measurement under the same analytical conditions as above. The mobility of the migrating component is calculated by "actual mobility measurement value/total content".
Compared with the prior art, the invention has the beneficial effects that:
the analysis method and the device can attach the elution of the hot airflow of the actual simulated cigarette to the filter tip additive, and make up the problem that the analysis result is disjointed with the actual process of cigarette smoking when the filter tip is independently tested and separated from the cigarette smoking process in the prior art.
In the method, the hot air flow is adopted for purging, so that the adoption of the method in the analysis of the cigarette combustion smoke is avoided: the problem that the interference of complex background components is generated after the tobacco shred is combusted, and the accurate analysis result is very difficult to obtain is solved, the test result is more accurate and reliable, and the pretreatment of sample analysis is simplified.
The device has simple structure and convenient operation, can simulate the filter tip test of all cigarette specifications, can simulate the migration test of filter tip additives, and can simulate all cigarette smoking modes and smoke flow temperatures. Provides powerful technical support for the aspects of cigarette product quality safety, smoke physiological feeling, smoking, health and the like.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions of the prior art, the drawings which are used in the description of the embodiments or the prior art will be briefly described, it being obvious that the drawings in the description below are only some embodiments of the invention, and that other drawings can be obtained according to these drawings without inventive faculty for a person skilled in the art.
FIG. 1 is a schematic diagram of a filter rod additive heat migration measuring device;
FIG. 2 is a schematic view of the structure of the purge tube;
wherein, 1, an air heater; 2. a constant temperature box; 3. an air inlet; 4. an air outlet; 5. an air outlet; 6. an air thermostatic tube; 7. a purge tube; 8. a temperature sensor; 9. a smoking machine; 10. a seal ring bayonet; 11. a sieve plate; 12. a seal ring; 13. a filter holder; 14. a Cambridge filter; 15. a refrigerant container; 16 purging the ingredient collector; 17. a tube body; 18. a tube cap;
FIG. 3 is a full-sweep mass spectrum of the heat transfer component of a bead blasting product.
Detailed Description
The present invention will be described in further detail with reference to examples.
It will be appreciated by those skilled in the art that the following examples are illustrative of the present invention and should not be construed as limiting the scope of the invention. The specific techniques, connections, or conditions are not identified in the examples and are set forth in accordance with the techniques, connections, conditions, or in accordance with the product specifications described in the literature in this field. The materials, instruments or equipment used are conventional products available from commercial sources, not identified to the manufacturer.
As used herein, the singular forms "a", "an", "the" and "the" are intended to include the plural forms as well, unless expressly stated otherwise, as understood by those skilled in the art. It will be further understood that the terms "comprises" and/or "comprising," when used in this specification, specify the presence of stated features, integers, steps, operations, elements, and/or components, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, and/or groups thereof. It will be understood that when an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present.
In the description of the present invention, unless otherwise indicated, the meaning of "a plurality" is two or more. The orientation or state relationship indicated by the terms "inner", "upper", "lower", etc. are orientation or state relationship based on the drawings, are merely for convenience of description and simplification of description, and do not indicate or imply that the apparatus or element in question must have a specific orientation, be configured and operated in a specific orientation, and therefore should not be construed as limiting the invention.
In the description of the present invention, it should be noted that, unless explicitly stated and limited otherwise, the terms "mounted," "connected," and "provided" are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium. The specific meaning of the above terms in the present invention is understood by those of ordinary skill in the art according to the specific circumstances.
It will be understood by those skilled in the art that, unless otherwise defined, all terms (including technical and scientific terms) used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. It will be further understood that terms, such as those defined in commonly used dictionaries, should be interpreted as having a meaning that is consistent with their meaning in the context of the prior art and will not be interpreted in an idealized or overly formal sense unless expressly so defined herein.
Example 1
As shown in fig. 1, a device for measuring the thermal migration quantity of a filter rod additive comprises a hot air blower 1, a constant temperature box 2, a purging pipe 7, a purging component collector 16 and a smoking machine 9;
the incubator 2 is provided with an air inlet 3, an air outlet 4 and an air outlet 5; an air thermostatic tube 6 is fixed in the incubator 2; the air inlet end of the air thermostatic tube 6 is fixed at the air inlet 3, and the air outlet end of the air thermostatic tube 6 is fixed at the air outlet 4;
the air heater 1 is connected with an air inlet 3 of the incubator 2; the air outlet 4 of the incubator 2 is connected with the air inlet end of the purge pipe 7;
the sweeping component collector 16 comprises a filter holder 13, a Cambridge filter 14 and a refrigerant container 15; the filter holder 13 and the Cambridge filter 14 are both arranged in the refrigerant container 15;
the air outlet end of the purging pipe 7 is connected with one end of the filter disc holder 13; the other end of the filter holder 13 is connected with the smoking machine 9;
filter holder 13 holds a cambridge filter 14 therein.
Example 2
As shown in fig. 1, a device for measuring the thermal migration quantity of a filter rod additive comprises a hot air blower 1, a constant temperature box 2, a purging pipe 7, a purging component collector 16 and a smoking machine 9;
the incubator 2 is provided with an air inlet 3, an air outlet 4 and an air outlet 5; an air thermostatic tube 6 is fixed in the incubator 2; the air inlet end of the air thermostatic tube 6 is fixed at the air inlet 3, and the air outlet end of the air thermostatic tube 6 is fixed at the air outlet 4;
the air heater 1 is connected with an air inlet 3 of the incubator 2; the air outlet 4 of the incubator 2 is connected with the air inlet end of the purge pipe 7;
the sweeping component collector 16 comprises a filter holder 13, a Cambridge filter 14 and a refrigerant container 15; the filter holder 13 and the Cambridge filter 14 are both arranged in the refrigerant container 15;
the air outlet end of the purging pipe 7 is connected with one end of the filter disc holder 13; the other end of the filter holder 13 is connected with the smoking machine 9;
filter holder 13 holds a cambridge filter 14 therein.
Temperature sensors 8 are arranged at the air outlet 4 and the air outlet 5.
The dead volume of the connecting pipeline between the air outlet end of the air thermostatic tube 6 and the purging tube 7 is not more than 1mL.
The method for measuring the thermal migration quantity of the filter rod additive comprises the following steps of: after the temperature at the air outlet and the air outlet is stable, the filter stick additive to be tested is wrapped by acetate fibers and then is placed into a purging pipe (the explosion beads need to be pre-pinched and quickly placed in), a refrigerant is added into a refrigerant container, the whole filter holder is immersed into the refrigerant, a smoking machine is started to carry out smoking, air flow passes through the purging pipe in the smoking process of the smoking machine, thermomigration components in a sample to be tested are purged, the thermomigration components are trapped by a Cambridge filter, and the migration quantity of the trapped thermomigration components is measured by a static headspace-gas chromatography-mass spectrometry.
Example 3
As shown in fig. 1 and 2, a device for measuring the thermal migration quantity of a filter rod additive comprises a hot air blower 1, a constant temperature box 2, a purging pipe 7, a purging component collector 16 and a smoking machine 9;
the incubator 2 is provided with an air inlet 3, an air outlet 4 and an air outlet 5; an air thermostatic tube 6 is fixed in the incubator 2; the air inlet end of the air thermostatic tube 6 is fixed at the air inlet 3, and the air outlet end of the air thermostatic tube 6 is fixed at the air outlet 4;
the air heater 1 is connected with an air inlet 3 of the incubator 2; the air outlet 4 of the incubator 2 is connected with the air inlet end of the purge pipe 7;
the sweeping component collector 16 comprises a filter holder 13, a Cambridge filter 14 and a refrigerant container 15; the filter holder 13 and the Cambridge filter 14 are both arranged in the refrigerant container 15;
the air outlet end of the purging pipe 7 is connected with one end of the filter disc holder 13; the other end of the filter holder 13 is connected with the smoking machine 9;
filter holder 13 holds a cambridge filter 14 therein.
Temperature sensors 8 are arranged at the air outlet 4 and the air outlet 5.
The dead volume of the connecting pipeline between the air outlet end of the air thermostatic tube 6 and the purging tube 7 is not more than 1mL.
The purge tube 7 comprises a tube body 17 and a tube cap 18 which are connected with each other; the opening end of the tube body 17 is provided with a seal ring bayonet 10; a sealing ring 12 matched with the sealing ring bayonet 10 is fixed in the pipe cap 18; the air inlet end of the purging pipe 7 is arranged at the bottom of the pipe body 17, and the air outlet end is arranged on the pipe cap 18.
The air inlet end of the purging pipe 7 is provided with a sieve plate 11, and the air inlet direction is perpendicular to the plane of the sieve plate 11.
The purge tube 7 is made of polypropylene plastic.
The inner diameter of the purging tube 7 is the same as the outer diameter of the filter rod, and the length of the space in the purging tube 7 is the same as the length of the filter rod.
The air thermostat 6 is S-shaped in the thermostat 2.
The exhaust outlet 5 ensures the discharge of intermittent hot air during suction and avoids overheating of the air.
A method for measuring the thermal migration quantity of a filter rod additive, comprising the steps of:
after all the interfaces are connected, the air tightness of the connection part is ensured, and the suction capacity of the whole system is corrected according to the requirements of a smoking machine;
a. when analysis starts, the air heater is turned on, the corresponding power is regulated, the temperature of the thermostatic tube is determined to reach 100 ℃ and kept stable, a smoke suction machine is utilized to suck a mouth of hot air, and whether the temperatures at the air outlet and the air outlet of the thermostatic box reach 100 ℃ or not is monitored and kept stable;
b. the filter stick additives (explosion beads, fragrant threads, particles and the like) are put into a small amount of acetate fibers for wrapping, the explosion bead samples are wrapped by the acetate fibers in advance and are pinched, quickly put into a detachable purging pipe, covered with a bayonet and connected with an upper pipeline;
c. starting smoking machine sucking work, wherein the sucking capacity is 35mL, the sucking interval is 1min, the sucking duration is 2s, and when hot air is sucked, the hot air enters a blowing pipe through an outlet of the constant temperature box through the constant temperature pipe to blow the filter stick additive, and the hot air is directly discharged from an air outlet of the constant temperature box in a sucking gap;
d. after smoking, sucking two hot air ports again, and transferring the residual migration objects in the pipeline into a migration object collector;
e. the Cambridge filter in the migration collector was removed, the filter holder was rapidly wiped, the Cambridge filter was placed in a headspace vial and sealed, and migration was determined by static headspace-gas chromatography-mass spectrometry.
Specific parameters for static headspace-gas chromatography-mass spectrometry were:
static headspace conditions: sample equilibrium temperature: 160. the temperature is lower than the temperature; sample ring: 3.0 mL; sample ring temperature: 160. the temperature is lower than the temperature; transmission line temperature: 180. the temperature is lower than the temperature; sample equilibration time: 30.0 min; sample bottle pressurization pressure: 138 kPa; pressurizing time: 0.20 min; inflation time: 0.20 min; sample loop equilibration time: 0.05 min; sample introduction time: 1.0 min;
gas chromatography conditions: chromatographic column: a VOC capillary column with the specification of 60 m multiplied by 0.32 mm multiplied by 1.8 mu m; carrier gas: helium with purity more than or equal to 99.999%; sample inlet temperature: 200 ℃; constant flow mode, column flow 2.0 mL/min, split ratio 1:1; programming temperature: the initial temperature is 40 ℃, and the temperature is kept for 2min; raising the temperature to 160 ℃ at a heating rate of 4 ℃/min; then the temperature is raised to 210 ℃ at the heating rate of 10 ℃/min, and the temperature is kept for 10 min;
mass spectrometry conditions: auxiliary interface temperature: 220. the temperature is lower than the temperature; ionization mode: an electron bombardment source (EI); ionization energy: 70 eV; ion source temperature: 230. the temperature is lower than the temperature; quadrupole temperature: 150. the temperature is lower than the temperature; solvent delay time: 4.0 min; the full-scanning monitoring mode is carried out, and the scanning range is 29 amu to 350 amu.
Application example 1
Smoking parameters of the smoking machine are as follows: the suction capacity was 35mL, the suction interval was 1min, and the suction duration was 2s; the migration is collected by a 44 mm Cambridge filter disc, the sweeping thermomigration component of the suction 8 port is trapped,
and (5) carrying out data retrieval by using an NIS98 standard map library. FIG. 3 is a mass spectrum full scan chromatogram of a certain bead blasting product subjected to heat migration of components by a filter rod additive of the present invention.
The components with the similarity of more than 97% in the spectrum library are searched, the properties of the components are determined, and a list of the components for the heat migration of the explosive beads in the filter stick based on the method is shown in a table 1.
TABLE 1 results of static headspace analysis of thermomigration composition of burst sample
The main components of the bead explosion product after heat migration are solvents and essences, and no forbidden components exist as can be found from the chromatograms and the search results. The method can better monitor the heated migration components of the filter stick additive, analyze whether the forbidden components are added, and effectively prevent and pre-warn the safety risk of the filter stick additive.
Application example 2
The filter stick additive to be tested is ethyl acetate, ethyl butyrate and ethyl caproate, the boiling point difference of the 4 compounds is relatively obvious, and quantitative analysis and thermal migration analysis (the analysis method is the same as that of application example 1) are carried out on components with relatively high content in a sample by a standard curve method. The results are shown in Table 2, and Table 2 illustrates migration of different heated migrates after elution by a hot flue gas stream.
Table 2 quantitative migration test results of four ingredients in burst beads
As a result, the average quantitative mobility of the four components was found to be 27.04-37.75%. There is a substantial correlation between the quantitative mobilities of ethyl butyrate, ethyl n-hexanoate and benzyl alcohol and their boiling points, and the higher the boiling point, the lower the component mobility. The method can be used for examining the migration quantity and migration rate of various components in different filter stick additives, can be used for examining the migration performance of different substances, and can be used for effectively evaluating the migration risk of main components in the filter stick additives.
The foregoing has shown and described the basic principles, principal features and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (7)
1. The device for measuring the heated migration quantity of the filter stick additive is characterized by comprising a hot air blower (1), a constant temperature box (2), a purging pipe (7), a purging component collector (16) and a smoking machine (9);
an air inlet (3), an air outlet (4) and an air outlet (5) are arranged on the incubator (2); an air thermostatic tube (6) is fixed in the incubator (2); the air inlet end of the air thermostatic tube (6) is fixed at the air inlet (3), and the air outlet end of the air thermostatic tube (6) is fixed at the air outlet (4);
the air heater (1) is connected with an air inlet (3) of the incubator (2); an air outlet (4) of the constant temperature box (2) is connected with an air inlet end of the purging pipe (7);
the sweeping component collector (16) comprises a filter disc holder (13), a Cambridge filter disc (14) and a refrigerant container (15); the filter disc holder (13) and the Cambridge filter disc (14) are arranged in the refrigerant container (15);
the air outlet end of the purging pipe (7) is connected with one end of the filter disc holder (13); the other end of the filter disc holder (13) is connected with the smoking machine (9);
a Cambridge filter (14) is clamped in the filter holder (13);
the dead volume of a connecting pipeline between the air outlet end of the air thermostatic pipe (6) and the purging pipe (7) is not more than 1mL;
the purging pipe (7) comprises a pipe body (17) and a pipe cap (18) which are connected with each other; the opening end of the pipe body (17) is provided with a seal ring bayonet (10); a sealing ring (12) matched with the sealing ring bayonet (10) is fixed in the pipe cap (18); the air inlet end of the purging pipe (7) is arranged at the bottom of the pipe body (17), and the air outlet end is arranged on the pipe cap (18);
the air thermostatic tube (6) is S-shaped in the thermostatic box (2);
the temperature sensor (8) is arranged at the air outlet (4) and the air outlet (5) of the incubator (2).
2. The device for measuring the thermal migration quantity of filter rod additives according to claim 1, wherein a screen plate (11) is arranged at the air inlet end of the purging pipe (7), and the air inlet direction is perpendicular to the plane of the screen plate (11).
3. A filter rod additive heat migration measuring apparatus according to claim 1, wherein the material of the purge tube (7) is polypropylene plastic.
4. The device for measuring the thermal migration quantity of a filter rod additive according to claim 1, wherein the inner diameter of the purge tube (7) is the same as the outer diameter of the filter rod, and the length of the space in the purge tube (7) is the same as the length of the filter rod.
5. The method for measuring the thermal migration quantity of the filter rod additive, which is characterized by comprising the following steps of:
and (3) opening the air heater, wrapping the filter stick additive to be tested by adopting acetate fibers after the temperatures at the air outlet and the air outlet are stable, loading the filter stick additive into a purging pipe, adding a refrigerant into a refrigerant container, immersing a filter holder into the refrigerant, starting a smoking machine for smoking, blowing out thermomigration components in a sample to be tested by air flow through the purging pipe in the smoking process of the smoking machine, capturing the thermomigration components by a Cambridge filter, and measuring the migration quantity of the captured thermomigration components by a static headspace-gas chromatography-mass spectrometry.
6. The method of claim 5, wherein the smoking mode of the smoking machine is an ISO standard smoking mode or a canadian deep drawing mode; the refrigerant is ice water, oil, dry ice or liquid nitrogen.
7. The method of claim 5, wherein the specific parameters of static headspace-gas chromatography-mass spectrometry are:
static headspace conditions: sample equilibrium temperature: 160. the temperature is lower than the temperature; sample ring: 3.0 mL; sample ring temperature: 160. the temperature is lower than the temperature; transmission line temperature: 180. the temperature is lower than the temperature; sample equilibration time: 30.0 min; sample bottle pressurization pressure: 138 kPa; pressurizing time: 0.20 min; inflation time: 0.20 min; sample loop equilibration time: 0.05 min; sample introduction time: 1.0 min;
gas chromatography conditions: chromatographic column: a VOC capillary column with the specification of 60 m multiplied by 0.32 mm multiplied by 1.8 mu m; carrier gas: helium with purity more than or equal to 99.999%; sample inlet temperature: 200 ℃; constant flow mode, column flow 2.0 mL/min, split ratio 1:1; programming temperature: the initial temperature is 40 ℃, and the temperature is kept for 2min; raising the temperature to 160 ℃ at a heating rate of 4 ℃/min; then the temperature is raised to 210 ℃ at the heating rate of 10 ℃/min, and the temperature is kept for 10 min;
mass spectrometry conditions: auxiliary interface temperature: 220. the temperature is lower than the temperature; ionization mode: an electron bombardment source (EI); ionization energy: 70 eV; ion source temperature: 230. the temperature is lower than the temperature; quadrupole temperature: 150. the temperature is lower than the temperature; solvent delay time: 4.0 min; the full-scanning monitoring mode is carried out, and the scanning range is 29 amu to 350 amu.
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