CN108845064A - A kind of full smoke pH method for measuring of cigarette mainstream - Google Patents

A kind of full smoke pH method for measuring of cigarette mainstream Download PDF

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Publication number
CN108845064A
CN108845064A CN201810697606.3A CN201810697606A CN108845064A CN 108845064 A CN108845064 A CN 108845064A CN 201810697606 A CN201810697606 A CN 201810697606A CN 108845064 A CN108845064 A CN 108845064A
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Prior art keywords
full
series connection
cigarette
cold
mainstream
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张峻松
张博
李瑞丽
朱远洋
黄贵元
彭周舟
何山
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Zhengzhou University of Light Industry
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Zhengzhou University of Light Industry
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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
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/06Preparation
    • 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
    • G01N30/88Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86

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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)
  • General Physics & Mathematics (AREA)
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Abstract

The invention belongs to tobacco chemistry analysis fields, particularly relate to a kind of full smoke pH method for measuring of cigarette mainstream.Complete technical problem cannot be trapped using general measure cigarette mainstream flue gas pH value in the prior art by solving, and be included the following steps:10-60 branch cigarette is aspirated under standard smoking conditions using smoking machine, by the full flue gas of mainstream using XAD-2 adsorption tube and series connection cold-trap device trapping;The adsorbent taken out in XAD-2 adsorption tube carries out oscillation extraction, obtains extract liquor;Merge the absorbing liquid in series connection cold-trap device in each series connection absorption bottle, the absorbing liquid after merging is merged with extract liquor, obtains amalgamation liquid;Amalgamation liquid, the as pH value of the full flue gas of cigarette mainstream are measured with Accurate pH meter.The present invention traps better effect, can accurately more reflect the pH value of the full flue gas of cigarette mainstream using solid particle absorption, three kinds of solvent trapping, cold trap trapping Trapping ways.

Description

A kind of full smoke pH method for measuring of cigarette mainstream
Technical field
The invention belongs to tobacco chemistry analysis fields, particularly relate to a kind of full smoke pH method for measuring of cigarette mainstream.
Background technique
Cigarette mainstream flue gas refers in aspiration procedure, from the flue gas stream of cigarette tail end evolution.Main flume enters smoking The oral cavity of person sucks lung by throat, has the function that stimulation nerve, generates physiological strength.
Main flume pH value is one of the important reference indicator of cigarette total quality, can reflect out main flume chemistry at / equilibrium relation, measurement method also constantly improving, and the pH value of flue gas, pH examination are originally measured using pH test paper Paper measurement result has some limitations, subjective factor is larger, then occurs a variety of measurement sides such as pH meter, electrode method again Method.The method for mainly using room temperature cold-trap to the measurement of the full smoke pH of mainstream at present, there are more easily to wave in main flume Ingredient is sent out, there are biggish disputes for the effect of trapping.Therefore, this research is using XAD-2 adsorption tube and series connection cold trap trapping method The full flue gas of mainstream is trapped, its pH value is measured, it is intended to provide a kind of accurate, convenient and fast method for the measurement of the full smoke pH of mainstream.
Measuring method about the full smoke pH of mainstream is it has been reported that focus primarily upon absorption bottle trapping and Cambridge under room temperature Filter disc trapping, but the loss of cigarette smoke volatile materials is easily caused under room temperature, this has the authenticity of measurement result biggish Deviation does not find the pH value of the full flue gas of measurement mainstream of document identical with the method for the present invention by literature search.
Mao Duobin et al. traps cigarette mainstream smoke condensate, oscillation extraction grain using cambridge filter using at normal temperature Ingredient in phase object traps gaseous phase of main stream smoke of cigarette object using series connection absorption bottle, by the extract liquor of granule phase substance and gas gas-phase objects Absorbing liquid is merged and is measured to its pH value, the pH value as the full flue gas of cigarette mainstream.
Journey passes tinkling of pieces of jade et al. and utilizes RM20H rotating disc type smoking machine Impinger 5box Trapping ways, at normal temperature, trapping master Smoke Particulate and gas gas-phase objects are flowed, the absorbing liquid of the extract liquor of granule phase substance and gas gas-phase objects is merged and its pH value is carried out Measurement.
It is reported based on existing research, room temperature is mainly used for the capture method of gaseous phase of main stream smoke of cigarette object at present The trapping of lower absorption bottle and measure respectively granule phase substance and gas gas-phase objects pH value method, but trap completely whether, not can determine that.
Summary of the invention
The present invention proposes a kind of full smoke pH method for measuring of cigarette mainstream, solves and is surveyed in the prior art using conventional Amount cigarette mainstream flue gas pH value cannot trap complete technical problem, and providing one kind being capable of the full flue gas pH of Accurate Determining cigarette mainstream Method.
The technical proposal of the invention is realized in this way:
A kind of full smoke pH method for measuring of cigarette mainstream, includes the following steps:
(1)Cigarette smoking
10-60 branch cigarette is aspirated under standard smoking conditions using smoking machine, and the full flue gas of mainstream is used into XAD-2 adsorption tube and string Join cold-trap device trapping;
(2)Oscillation extraction
The adsorbent taken out in XAD-2 adsorption tube carries out oscillation extraction, obtains extract liquor;
(3)The merging of extract liquor and absorbing liquid
Merge the absorbing liquid in series connection cold-trap device in each series connection absorption bottle, the absorbing liquid after merging is closed with extract liquor And obtain amalgamation liquid;
(4)The measurement of pH value
Amalgamation liquid, the as pH value of the full flue gas of cigarette mainstream are measured with Accurate pH meter.
The step(1)Middle series connection cold-trap device includes cold-trap and the 2-6 series connection absorption bottle in cold-trap, each string Connection absorption bottle opening is equipped with air inlet pipe and exhaust pipe, the other end opening setting for the exhaust pipe that tail end is connected in absorption bottle.
Absorbing liquid is equipped in each series connection absorption bottle.
The step(1)The environment temperature of cold-trap device is subzero 10-100 DEG C in middle series connection cold-trap device.
The step(2)The time of middle oscillation extraction is 10-70min, temperature is 10-25 DEG C, frequency 150-210r/ min。
The absorbing liquid and absorbing liquid are secondary distilled water and organic solvent is 2 by volume:(1-4)It mixes; Wherein organic solvent is isopropanol, methanol, ethyl alcohol or acetone.
The step(2)Middle absorbing liquid is the 1/3-2/3 of series connection absorption bottle volume.
The beneficial effects of the present invention are:
One, the present invention is to propose that one kind being capable of the full cigarette of Accurate Determining cigarette mainstream on the basis of existing pertinent literature report The method of gas pH value, and to experimental factor(Duration of oscillation, frequency of oscillation, oscillation extraction liquid product)It optimizes, utilizes turntable Formula smoking machine aspirates the cigarette of certain number, and mainstream full flue gas XAD-2 adsorption tube and concatenated cold-trap absorption bottle are trapped, Adsorbent in adsorption tube is transferred in triangular flask after suction, it is molten that certain density secondary distilled water-organic solvent is added Liquid carries out oscillation extraction, the absorbing liquid in extract liquor extracted and absorption bottle is merged, and measure its pH value.
Two, the pH value for determining the full flue gas of cigarette mainstream that the present invention can be more accurate, to be smoke chemistry ingredient The exploration of knowledge relationship between sensory experience provides more scientific comprehensive analysis data and theories integration.
Three, the measurement of existing main flume pH value individually uses solvent absorption main flume, many important volatilizations Property ingredient be not easy trapping completely, the present invention using solid particle absorption, solvent trapping, three kinds of Trapping ways of cold trap trapping, trapping Better effect can accurately more reflect the pH value of the full flue gas of cigarette mainstream.
Detailed description of the invention
Fig. 1 is mainstream whole smoke trapping process device schematic diagram, wherein 1- smoking machine, 2-XAD-2 adsorption tube, and 3- series connection is cold Trap device, 4- fixing clamp, 5- series connection absorption bottle, 6- cold-trap.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical solution of the present invention is clearly and completely described, it is clear that institute The embodiment of description is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, Those of ordinary skill in the art's every other embodiment obtained under that premise of not paying creative labor, belongs to this hair The range of bright protection.
One, test portion
1. instrument and reagent
Cigarette is purchased by market;Secondary distilled water(Modulating pH value with sodium hydroxide solution after abjection carbon dioxide is 7);PH value is slow Electuary:Mixed phosphate saline solution that hydrogen phthalate sodium water solution that pH value is 4, pH value are 6.86, pH value are 9.18 Sodium tetraborate aqueous solution(Shanghai INESA Scientific Instrument Co., Ltd.);XAD-2 adsorption tube(Beijing Lake Tai Rui instrument and equipment Co., Ltd).
RM20H carousel-type smoking machine(German Borgwalt KC company);Agilent 7890B/5977A gas-chromatography/ Mass spectrometer(Agilent company of the U.S.);Full temperature shaken cultivation case(Taicang experimental facilities factory);MODEL868 type Accurate pH Meter(Ao Lilong company of the U.S.).
2. test procedure
Specially:(1)Cigarette smoking
20 cigarette are aspirated under standard smoking conditions using rotating disc type smoking machine, and the full flue gas of mainstream is used into XAD-2 adsorption tube With series connection cold-trap device trapping;
(2)Oscillation extraction
The adsorbent taken out in XAD-2 adsorption tube carries out oscillation extraction, and the time of oscillation extraction is 10-70min, temperature 10- 25 DEG C, frequency 150-210r/min, obtain extract liquor(As shown in Figure 1);
(3)The merging of extract liquor and absorbing liquid
Adsorbent in adsorption tube is transferred in triangular flask after suction, secondary distilled water-organic solvent is added(Isopropanol, Methanol, ethyl alcohol or acetone)Oscillation extraction is carried out, the absorbing liquid in the extract liquor and absorption bottle after oscillation is merged, is obtained Amalgamation liquid;
(4)The measurement of pH value
Amalgamation liquid, the as pH value of the full flue gas of cigarette mainstream are measured with Accurate pH meter.
Two, results and discussion
1. condition optimizing
1.1 duration of oscillation
Influence of the different duration of oscillation of table 1 to the full smoke pH of mainstream
As can be seen from the table, preferable when duration of oscillation 30-50min.
1.2 frequency of oscillation
Influence of the different frequencies of oscillation of table 2 to the full smoke pH of mainstream
As can be seen from the table, it is preferable when frequency of oscillation is 170-200r/min.
1.3 oscillation extraction liquid product
Influence of the different oscillation extraction liquid products of table 3 to the full smoke pH of mainstream
As can be seen from the table, it is preferable when oscillation extraction extract liquor volume is 40-70ml.
3. the repeatability of method
Using the good method of above-mentioned optimization, measure gaseous phase of main stream smoke of cigarette object pH value 10 times, the relative standard of measurement result is inclined Difference(RSD)It is 1.57, thus illustrates that repeatability is good for this method.
4. sample analysis result
Using the scheme optimized, commercially available 20 kinds of gaseous phase of main stream smoke of cigarette object pH value is measured, and is surveyed with current ambient temperature method of trapping Determine the full smoke pH of cigarette mainstream to compare.Room temperature capture method:It is used 70ml 50% 2 time through smoking machine trapping granule phase substance Distilled water-isopropanol carries out oscillation extraction(Time:30min, frequency of oscillation:175r/min);It is logical by the flue gas of cambridge filter Enter 2 series connection absorption bottles(Normal temperature environment), absorption bottle is provided with 50mL absorbing liquid(Secondary distilled water-isopropanol), suction finishes, Merge absorbing liquid and granule phase substance extract liquor in absorption bottle and measures its pH value, the as full smoke pH of mainstream.Comparing result such as 4 institute of table Show.
The pH value measurement result of 4 20 kinds of commercial cigarettes main flume gas gas-phase objects of table
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.

Claims (7)

1. a kind of full smoke pH method for measuring of cigarette mainstream, which is characterized in that include the following steps:
(1)Cigarette smoking
10-60 branch cigarette is aspirated under standard smoking conditions using smoking machine, and the full flue gas of mainstream is used into XAD-2 adsorption tube and string Join cold-trap device trapping;
(2)Oscillation extraction
The adsorbent taken out in XAD-2 adsorption tube carries out oscillation extraction, obtains extract liquor;
(3)The merging of extract liquor and absorbing liquid
Merge the absorbing liquid in series connection cold-trap device in each series connection absorption bottle, the absorbing liquid after merging is closed with extract liquor And obtain amalgamation liquid;
(4)The measurement of pH value
Amalgamation liquid, the as pH value of the full flue gas of cigarette mainstream are measured with Accurate pH meter.
2. the full smoke pH method for measuring of cigarette mainstream as described in claim 1, it is characterised in that:The step(1)In Cold-trap device of connecting includes that cold-trap and the 2-6 series connection absorption bottle in cold-trap, each series connection absorption bottle opening are equipped with Air inlet pipe and exhaust pipe, the other end opening setting for the exhaust pipe that tail end is connected in absorption bottle.
3. the full smoke pH method for measuring of cigarette mainstream as claimed in claim 2, it is characterised in that:Each series connection absorption bottle Inside it is equipped with absorbing liquid.
4. the full smoke pH method for measuring of cigarette mainstream as described in claim 1, it is characterised in that:The step(1)In The environment temperature of cold-trap device is subzero 10-100 DEG C in series connection cold-trap device.
5. the full smoke pH method for measuring of cigarette mainstream as described in claim 1, it is characterised in that:The step(2)In The time of oscillation extraction is 10-70min, temperature is 10-25 DEG C, frequency 150-210r/min.
6. the full smoke pH method for measuring of cigarette mainstream as described in claim 1, it is characterised in that:The absorbing liquid and suction Receipts liquid is secondary distilled water and organic solvent is 2 by volume:(1-4)It mixes;Wherein organic solvent is isopropanol, first Alcohol, ethyl alcohol or acetone.
7. the full smoke pH method for measuring of cigarette mainstream as described in claim 1, it is characterised in that:The step(2)In Absorbing liquid is the 1/3-2/3 of series connection absorption bottle volume.
CN201810697606.3A 2018-06-29 2018-06-29 A kind of full smoke pH method for measuring of cigarette mainstream Pending CN108845064A (en)

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CN110320292A (en) * 2019-06-28 2019-10-11 河南中烟工业有限责任公司 The measuring method of volatile component in a kind of full flue gas of electronic cigarette
WO2020253561A1 (en) * 2019-06-19 2020-12-24 湖北中烟工业有限责任公司 Method for measuring aluminum release amount in smoke of heat-not-burn cigarette
CN114259081A (en) * 2021-12-02 2022-04-01 吉林烟草工业有限责任公司 Method for regulating and controlling pH of flue gas by utilizing volatile acid adsorbed by porous material

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2020253561A1 (en) * 2019-06-19 2020-12-24 湖北中烟工业有限责任公司 Method for measuring aluminum release amount in smoke of heat-not-burn cigarette
CN110320292A (en) * 2019-06-28 2019-10-11 河南中烟工业有限责任公司 The measuring method of volatile component in a kind of full flue gas of electronic cigarette
CN114259081A (en) * 2021-12-02 2022-04-01 吉林烟草工业有限责任公司 Method for regulating and controlling pH of flue gas by utilizing volatile acid adsorbed by porous material
CN114259081B (en) * 2021-12-02 2024-01-26 吉林烟草工业有限责任公司 Method for regulating and controlling pH of flue gas by utilizing volatile acid adsorbed by porous material

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