CN102590198A - Method for determining total volatile phenol in smoke of cigarettes by using spectrophotometer - Google Patents
Method for determining total volatile phenol in smoke of cigarettes by using spectrophotometer Download PDFInfo
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- CN102590198A CN102590198A CN2012100248351A CN201210024835A CN102590198A CN 102590198 A CN102590198 A CN 102590198A CN 2012100248351 A CN2012100248351 A CN 2012100248351A CN 201210024835 A CN201210024835 A CN 201210024835A CN 102590198 A CN102590198 A CN 102590198A
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Abstract
The invention relates to a method for determining total volatile phenol in the smoke of cigarettes by using a spectrophotometer, which belongs to the technical field of tobacco. The method comprises the following steps that: under the alkaline condition of pH (Potential Of Hydrogen) equal to 10 and the existence of potassium ferricyanide, a volatile phenol compound can react with 4-aminoantipyrine to generate orange red antipyrine dye, the colored compound is extracted by chloroform, the spectrophotometer is then used for determining absorbance at 460nm, a graph is drawn with the phenol concentration as the abscissa and the absorbance as the ordinate, the conventional linear regression is adopted to fit a straight line, and thereby, a standard curve for phenol is obtained. After being soaked in sulfuric acid, a cigarette smoke sample Cambridge filter is distilled by vapor, the distilled part undergoes the same chromogenic reaction, and is then determined by the spectrophotometer, and thereby, the total volatile phenol content is obtained. The method is used for determining the total volatile phenol in the smoke of the cigarettes, and when only the total volatile phenol in the smoke of cigarettes rather than a single phenol substance needs to be determined, the method has the advantages of rapidness, simplicity in operation and relatively simple instruments.
Description
Technical field:
The present invention relates to a kind of method, belong to technical field of tobacco with total volatile phenol in the spectrophotometric determination cigarette smoke.
Background technology:
Can steam with water vapor according to aldehydes matter, be divided into volatile phenol and non-volatile phenol, it has been generally acknowledged that boiling point is being to be generally monohydric phenol by volatile phenol below 230 ℃, boiling point is being non-volatile phenol more than 230 ℃, is generally polyhydric phenol.Aldehydes matter is a protoplasm poison, belongs to highly toxic substance, and human body is taken in a certain amount of meeting and the acute poisoning symptom occurred.The volatile phenol material big city that produces during cigarette burning produces dull fragrance and suction beastly flavor, is one type of important objectionable constituent in the cigarette mainstream flue gas, also is important assorted pneumatolytic/one who experiences when smokeing panel test.Because the volatile phenol compound is under the alkali condition about pH=10; In the presence of the potassium ferricyanide; Can generate orange-red antipyrine dyestuff with the reaction of 4-amino-antipyrine; Conventional method behind chloroform extraction, at 460nm place is measured absorbance with spectrophotometer with colored compound, reaches the purpose of the total volatile phenol of quantitative measurement (in phenol).
Summary of the invention:
The object of the invention in provide a kind of quick, easy and simple to handle with the spectrophotometric determination cigarette smoke in the method for total volatile phenol.
Research shows: the volatile phenol compound is under the alkali condition about pH=10; In the presence of the potassium ferricyanide; Can generate orange-red antipyrine dyestuff with the reaction of 4-amino-antipyrine; Conventional method behind chloroform extraction, at 460nm place is measured absorbance with spectrophotometer with colored compound, reaches the purpose of the total volatile phenol of quantitative measurement (in phenol).Its reaction equation is following:
The inventive method is under the prerequisite that need not measure single aldehydes matter such as phenol, methylphenol etc.; Adopt steam distillation flue gas cambridge filter, use total volatile phenol in the spectrophotometric determination cigarette smoke again, be used for measuring cigarette gas index, judge that cigarette is good and bad.
The inventive method is the improvement on total volatile phenol detection method basis in existing cigarette smoke, and its improvement is following:
1, the phenol typical curve is drawn: the phenol standard solution (10ug/mL) of in one group of 7 250mL volumetric flask, add 0,2,4,6,8,10 respectively, 12mL preparing the same day, each adding distil water 20mL; The buffer solution that adds 5mL pH=10, mixing, this moment, the pH value was 10.0 ± 0.2; Add 1mL4-amino-antipyrine solution again, 1mL potassium ferricyanide solution, mixing; After placing 20min, with twice of chloroform extraction nonferrous layer (15mL+5mL), standing demix; Connect common conical hopper below the separating funnel, conical hopper neck tube inwall is absorbent cotton or filter paper beyond the Great Wall, covers anhydrous sodium sulfate drying above.Filtrating is directly inserted in the 25mL volumetric flask, and it is colourless to filtrating to wash anhydrous sodium sulfate and cotton or filter paper with methenyl choloride, is settled to scale with methenyl choloride then.Do contrast with blank test solution (0mL phenol standard solution), measure absorbance in photometer 460nm place with the 10mm cuvette.With the phenol concentration is horizontal ordinate, is that ordinate is figure with the absorbance, adopts conventional linear regression fit straight line, obtains the typical curve of phenol.
What 2, qualified cigarette propped up selects: import cigarette and homemade commodity cigarette, cigarette length is 84mm.Cigarette sample is positioned over temperature (22 ± 1) ℃, balance 48h under relative humidity (60 ± 2) the % condition, selecting average quality ± 0.02g/ to prop up the cigarette that props up with average resistance to suction ± 5Pa/ then is that qualified cigarette props up.
3, suction method: according to standard mode smoking, each sample is inhaled 20, each cigarette sample triplicate.
4, specimen preparation: will aspirate one whole good of cambridge filter and put into the special-purpose cucurbit bottom of steam distillation device; Adding the 30mL sulfuric acid solution soaks; Ultrasonic concussion 10min distills with water vapour then, collects about 200mL cut (the about 8min of distillation time).Pipette 20mL collection liquid and go in the 250mL separating funnel, add the buffer solution of 5mL pH=10, mixing, this moment, the pH value was 10.0 ± 0.2; 1mL4-amino-antipyrine solution again, 1mL potassium ferricyanide solution, mixing; After placing 20min, with twice of chloroform extraction nonferrous layer (15mL+5mL), standing demix; Connect common conical hopper below the separating funnel, conical hopper neck tube inwall is absorbent cotton or filter paper beyond the Great Wall, covers anhydrous sodium sulfate drying above.Filtrate and insert in the 25mL volumetric flask, filter is finished, and it is colourless to filtrating to continue to wash anhydrous sodium sulfate and cotton or filter paper with methenyl choloride, is settled to scale with methenyl choloride again.It is a to do blank test solution simultaneously.
5, sample determination: do reference with blank test solution, survey absorbance in 460nm photometer place with the 10mm cuvette.According to the phenol typical curve, calculate the quality of contained total volatile phenol (in phenol) in the sample solution.
Method of the present invention is used for the mensuration of the total volatile phenol of cigarette smoke; For not measuring to single aldehydes matter; Only need measure the total volatile phenol in the cigarette smoke, have quick, easy and simple to handle and the simple relatively advantage of instrument, good prospects for application is arranged.
Description of drawings:
The mensuration technology of Fig. 1 the inventive method.
The response curve of Fig. 2 phenol concentration and absorbance
The practical implementation method:
Below in conjunction with accompanying drawing the present invention is carried out detailed description repeatedly.
1 key instrument and reagent
UV-2450 ultraviolet-visible pectrophotometer (Japanese Shimadzu company), the rotary smoking machine in 20 ducts (German Borgwaldt company), steam distillation device (Switzerland Buchi company) automatically.It is pure that agents useful for same is analysis, and institute's water is no phenol water.
Phenol (C
6H
5OH) standard reserving solution: 1mg/mL is diluted to 10ug/mL standard operation liquid during use, preparation on the same day, and used the same day.Purifying phenol: get phenol in cucurbit, add air set pipe, add thermal distillation, collect 182 ℃～184 ℃ cut, cooling.This cut is a clear crystal, in brown bottle, seals and keeps in Dark Place.
PH=10 buffer solution: take by weighing 20g ammonium chloride (NH
4C
l), with 100mL strong aqua (NH
3H
2O) dissolving adds water and is settled to 500mL, jumps a queue, and places refrigerator to preserve.
The potassium ferricyanide (K
3[Fe (CN)
6]) solution: take by weighing the 8g potassium ferricyanide, the water dissolving, constant volume places in the refrigerator and preserves to 100mL, can use a week.
4-amino-antipyrine (C
11H
13ON
3) solution: take by weighing 2g 4-amino-antipyrine, the water dissolving adds the water constant volume to 100mL, places in the refrigerator and preserves, and can use a week.The purification of 4-amino-antipyrine: the 4-amino-antipyrine solution for preparing is placed dry beaker, add 10g florisil silica (60 orders～80 orders are smoked 4h for 600 ℃); Stir fully with glass bar; Leave standstill a moment, solution is used the middling speed filter paper filtering, collect filtrating; In brown bottle, seal, refrigerator is preserved.
No phenol distilled water: add 1g copper sulphate (CuSO at 1000mL water
4), to think highly of the steaming first water with quartzy sub-boiling distillation and obtain, whole process avoids using rubber tube, down together.
Or in 1000mL, adding the active carbon powder of 0.2g through 200 ℃ of activation 0.5h, behind the shake well, placement is spent the night.With double-deck middling speed filter paper filtering, filtrating is kept in the Pyrex bulb subsequent use.
Or hydro-oxidation sodium (NaOH) makes water be strong basicity, and drips liquor potassic permanganate to aubergine, moves in the cucurbit to add thermal distillation, and it is subsequent use to collect distillate.
Sulfuric acid solution: 1+4, the concentrated sulphuric acid (H of 1 part of volume
2SO
4) add the water of 4 parts of volumes, cooling.
Anhydrous sodium sulfate (Na
2SO
4): 550 ℃ of baking 4h in muffle furnace.
Methenyl choloride (CHCl
3).
2 experimental techniques
2.1 the drafting of typical curve: the phenol standard solution (10ug/mL) of in one group of 7 250mL volumetric flask, add 0,2,4,6,8,10 respectively, 12mL preparing the same day, each adding distil water 20mL.The buffer solution that adds 5mL pH=10, mixing, this moment, the pH value was 10.0 ± 0.2; 1mL4-amino-antipyrine solution again, 1mL potassium ferricyanide solution, mixing; After placing 20min, with twice of chloroform extraction nonferrous layer (15mL+5mL), standing demix; Connect common conical hopper below the separating funnel, conical hopper neck tube inwall is absorbent cotton or filter paper beyond the Great Wall, covers anhydrous sodium sulfate drying above.Filtrating is directly inserted in the 25mL volumetric flask, and it is colourless to filtrating to wash anhydrous sodium sulfate and cotton or filter paper with methenyl choloride, is settled to scale with methenyl choloride then.Do contrast with blank test solution (0mL phenol standard solution), survey absorbance in the 460nm place with the 10mm cuvette.With phenol concentration y is horizontal ordinate, is the ordinate curve plotting with the absorbance reading x of instrument, the Regression Equations y=0.0027x that obtains, coefficient R
2=0.9992, like Fig. 2.
2.2 sample determination:
What qualified cigarette propped up selects: import cigarette and homemade commodity cigarette, cigarette length is 84mm.Cigarette sample is positioned over temperature (22 ± 1) ℃, balance 48h under relative humidity (60 ± 2) the % condition, selecting average quality ± 0.02g/ to prop up the cigarette that props up with average resistance to suction ± 5Pa/ then is that qualified cigarette props up.
Suction method: according to standard mode smoking, each sample is inhaled 20, each cigarette sample triplicate.
Specimen preparation: will aspirate one whole good of cambridge filter and put into the special-purpose cucurbit bottom of steam distillation device, and add the 30mL sulfuric acid solution and soak, ultrasonic concussion 10min distills with water vapour then, collects about 200mL cut (the about 8min of distillation time).Pipette 20mL collection liquid and go in the 250mL separating funnel, add the buffer solution of 5mL pH=10, mixing, this moment, the pH value was 10.0 ± 0.2; 1mL4-amino-antipyrine solution again, 1mL potassium ferricyanide solution, mixing; After placing 20min, with twice of chloroform extraction nonferrous layer (15mL+5mL), standing demix; Connect common conical hopper below the separating funnel, conical hopper neck tube inwall is absorbent cotton or filter paper beyond the Great Wall, covers anhydrous sodium sulfate drying above.Filtrate and insert in the 25mL volumetric flask, filter is finished, and it is colourless to filtrating to continue to wash anhydrous sodium sulfate and cotton or filter paper with methenyl choloride, is settled to scale with methenyl choloride again.It is a to do blank test solution simultaneously.
Sample determination: do reference with blank test solution, survey absorbance in the 460nm place with the 10mm cuvette.According to typical curve, calculate the quality of contained total volatile phenol (in phenol) in the sample solution.
3 measure the result
Measure the total volatile phenol in homemade Virginian-type cigarette and each flue gas of three kinds of import blended type cigarette with the method, the results are shown in Table 1.The repeatability and the recovery of standard addition of the method have been tested.Find out that from table 1 relative standard deviation (RSD) is 1.89%～4.11%, recovery of standard addition is 96.88%～103.59%, explains that the recovery of this method is high, good reproducibility.Find out also that from table 1 the total volatile phenol content in the Virginian-type cigarette flue gas will obviously exceed 2～4 times than blended type cigarette.
The content of total volatile phenol in table 1 cigarette smoke
Claims (1)
1. method with total volatile phenol in the spectrophotometric determination cigarette smoke, the improvement on existing method basis, its improvement is following:
A. the phenol typical curve is drawn: in one group of 7 250mL volumetric flask; The 10ug/mL phenol standard solution of add 0,2,4,6,8,10 respectively, 12mL preparing the same day, each adding distil water 20mL adds 5mL pH=10 buffer solution; Mixing, pH value are 10.0 ± 0.2; Add 1mL4-amino-antipyrine solution again, 1mL potassium ferricyanide solution, mixing; After placing 20min, with chloroform extraction nonferrous layer twice, i.e. 15mL+5mL; Standing demix; Connect common conical hopper below the separating funnel, conical hopper neck tube inwall is absorbent cotton or filter paper beyond the Great Wall, covers anhydrous sodium sulfate drying above; Filtrating is directly inserted in the 25mL volumetric flask, and it is colourless to filtrating to wash anhydrous sodium sulfate and cotton or filter paper with methenyl choloride, is settled to scale with methenyl choloride then; With 0mL phenol standard solution is that blank test solution is done contrast, measures absorbance in luminosity 460nm place with the 10mm cuvette; With the phenol concentration is horizontal ordinate, is ordinate with the absorbance, with conventional linear regression fit straight line, obtains the typical curve of phenol;
What b. qualified cigarette propped up selects: import cigarette and homemade commodity cigarette, and cigarette length is 84mm; Cigarette sample is positioned over 22 ± 1 ℃ of temperature, balance 48h under relative humidity 60 ± 2% conditions, selecting average quality ± 0.02g/ to prop up the cigarette that props up with average resistance to suction ± 5Pa/ is that qualified cigarette props up;
C. suction method: press the smoking of conventional criteria mode, each sample is inhaled 20, each cigarette sample triplicate;
D. specimen preparation: will aspirate the cucurbit bottom that one whole good of cambridge filter is put into conventional steam distillation device, and add the 30mL sulfuric acid solution and soak ultrasonic concussion 10min; Distill 8min with water vapour then; Collect the 200mL cut, pipette 20mL collection liquid and go in the 250mL separating funnel, add 5mL pH=10 buffer solution; Mixing, pH value are 10.0 ± 0.2; Add 1mL4-amino-antipyrine solution again, 1mL potassium ferricyanide solution, mixing; After placing 20min, with chloroform extraction nonferrous layer twice, i.e. 15mL+5mL; Standing demix; Connect common conical hopper below the separating funnel, conical hopper neck tube inwall is absorbent cotton or filter paper beyond the Great Wall, covers anhydrous sodium sulfate drying above; Filtrate and insert in the 25mL volumetric flask, filter is finished, and it is colourless to filtrating to continue to wash anhydrous sodium sulfate and cotton or filter paper with methenyl choloride, is settled to scale with methenyl choloride again, and the blank test solution of doing 0mL phenol standard solution simultaneously is a;
E. sample determination: do reference with blank test solution, survey absorbance in 460nm photometer place,, calculate in the sample solution quality in the contained total volatile phenol of phenol according to the phenol typical curve with the 10mm cuvette.
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Cited By (8)
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| CN103091382A (en) * | 2013-01-15 | 2013-05-08 | 云南烟草科学研究院 | Determination method for content of total volatile alkali in cigarette smoke |
| FR3031592A1 (en) * | 2015-01-13 | 2016-07-15 | Commissariat Energie Atomique | MATERIAL FOR DETECTING PHENOL COMPOUNDS AND ITS APPLICATIONS |
| FR3031593A1 (en) * | 2015-01-13 | 2016-07-15 | Commissariat Energie Atomique | ANALYSIS OF PHENOL IN LIQUID PHASE |
| CN107144539A (en) * | 2017-06-29 | 2017-09-08 | 深圳安吉尔饮水产业集团有限公司 | The detection method of water dispenser product volatile phenol content |
| CN108548811A (en) * | 2018-03-15 | 2018-09-18 | 成都市排水有限责任公司 | A method of measuring volatile phenol in water with continuous flow method |
| CN111220601A (en) * | 2018-11-27 | 2020-06-02 | 上海尚湾信息技术有限公司 | Rapid detection method for pesticide residues in vegetables and fruits |
| CN111380821A (en) * | 2018-12-29 | 2020-07-07 | 贵州中烟工业有限责任公司 | Method for measuring copper in tobacco or tobacco products by using continuous flow method |
| CN112697785A (en) * | 2020-11-10 | 2021-04-23 | 红云红河烟草(集团)有限责任公司 | Method for testing and evaluating gluing uniformity of cigarette roll joint lap |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103091382A (en) * | 2013-01-15 | 2013-05-08 | 云南烟草科学研究院 | Determination method for content of total volatile alkali in cigarette smoke |
| FR3031592A1 (en) * | 2015-01-13 | 2016-07-15 | Commissariat Energie Atomique | MATERIAL FOR DETECTING PHENOL COMPOUNDS AND ITS APPLICATIONS |
| FR3031593A1 (en) * | 2015-01-13 | 2016-07-15 | Commissariat Energie Atomique | ANALYSIS OF PHENOL IN LIQUID PHASE |
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| CN107144539A (en) * | 2017-06-29 | 2017-09-08 | 深圳安吉尔饮水产业集团有限公司 | The detection method of water dispenser product volatile phenol content |
| CN108548811A (en) * | 2018-03-15 | 2018-09-18 | 成都市排水有限责任公司 | A method of measuring volatile phenol in water with continuous flow method |
| CN111220601A (en) * | 2018-11-27 | 2020-06-02 | 上海尚湾信息技术有限公司 | Rapid detection method for pesticide residues in vegetables and fruits |
| CN111380821A (en) * | 2018-12-29 | 2020-07-07 | 贵州中烟工业有限责任公司 | Method for measuring copper in tobacco or tobacco products by using continuous flow method |
| CN112697785A (en) * | 2020-11-10 | 2021-04-23 | 红云红河烟草(集团)有限责任公司 | Method for testing and evaluating gluing uniformity of cigarette roll joint lap |
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Application publication date: 20120718 |