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Philip Morris

Triacetin Content of Cigarette Filters

Date: 19590000/EP
Length: 3 pages
2028435304-2028435306
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Page 1: iqq46e00
~' ~'~~~~~P~~ ~~ ~~ ~ ' ~~~'~a~cet,ini ~~ Content ~~ ~~ of Cigarette ~~~~ Filters ~~~ IWargqretl E. Bill, Gunars Vilcins and Frank E. Resnik Research and Development Department,, Philip Iwlorris, Iinc. Richrnoncl, Virginia, W.S.A.- ----- ___ _ Triacetin is commonly used as a plasticizer for cellulose acetiate fibers in cigarette filters, and its, determi- nat'ion is important for good quality control oni the final filter product. For this reason an infrared method has been developed for the determina- tion of triacetin in the cigarette filters. The triacetin is extracted from the filters with benzene andI the extract examined withi an infrared spectrophotometer. Recovery values of known amounts of triacetin added to the untreated cellulose acetate fibers average 99%, Ctrndiff' (1959) reports a method in which triacetin is extractedl from the filters and saponified with ethanolic potassium hydroxide: The saponified ester is titrated with a hydrochloric acid' so- lution to determine the t'riacetin concentration. It is believed that an 0.8 0.7 0.6 W u z 0 5 Q m cr p . 0.4 N m Q 0:3 0.2 O:f 2.0 Figure 1: Tiriace6n calibrartiomcurve. infrared method is more rapidi as: it does not require the repeated prepa- ration or standardization of solu- tions. The method which, is, reported in this paper is more specific for triacetin, and is applicable even. in the presence of other filter additives. Apparatus and. Reagents Perkin-Elmer Model' 21 double- beam infrared spectrophotometer equipped wit'h a sodium chloride prism. Perkin-Elmer matched 200 ±50 microns fixed liquid cells with sodi- um chloride windows. Benzene, Spectro grade obtaine& from Distillation Products Indus- tries: Triacetin, obtained from Tennes- see Eastman Company. 3.0 4:0 CONCENTRATION (mq\ml) 5.0 (Tobacco Scie.nr,e 26) 6. 0 Cellulose acetate fibers obtained from Tennessee Eastman Company. AnaHftical Procedore Preparation of Calibration Curve: Prepare & series of' standard solu- tions of triacetin ini benzene with the triacetini concentrations ranging from one to five milligrams per milli- liter. Analyze these solutions with the infrared spectrophotometer using two matched fixed thickness cells which are 200, -_t50 microns. Fill one eelli with the sample and place it in the sample beam. Fill the other cell with benzene andi place it in the ref- erence beam to compensate for the solvent in the sample. Obtaini the in- frared spectrum~ of t'his standaQ-.diand draav the base 1'ine. firom 7.5 to 9.0 microns to compute the corrected' ab- sorbance of'the 8.2 micron band. De- termine the calibration curve by analyzing a series of' these standard solutions: Analysis of Sample: Remove twenty filters from the test ciga- rettes and strip the paper from the filters. Weigh these: filters and place them in a thimble in a Soxhlet ex- traction apparatus with approxi- mately 75 ml benzene. Wrap the ex- traction tube andl flask with alumi- numl foiil to facilitate reHuxing. Re- flux for one hour. Quantitatively transfer the extract to & 100 mU volumetric flask and dilute to volume with benzene. Analyze this solution with the infrared spectrophotometer using the two matched fixed thick- ness cells which were usedl for the calibrationn curve. From this spec- trumi draw the base line from 7.5 to 9.0 microns and compute the cor- rected absorbance of the 8.2 mirroio band. Read the concentration of the triacetin in mg!mll from the calibra- tion curve.
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. Calculafions The following formula was used for calculating the triacetini content ufcigarette filters: Ar....... d = A....: - A.,,.:. where : A,.,,,,~,,, = corrected absorb- ance at 8.2 mi- crons . A,,,,: = maximum absorb- u 7 ance at 8.2 mi - crons Q ~. U As,,. = minimum absorb- m' ance at 8.2 mi- crons A typical sample calculation is as follows: = 8.6% triaeetin The specific extinctioni coef6cient' may be used' in, the calculations rather than the standard graph. The following formula was used for cal- culating the specific extinction co- effiicient: Aro..R.... = Am .- Aa„,«. 2 4 6 = 0.244 - 0:085 = 0.159 . The corrected absorbance (0.159)) is equivalent to, 1.15 mg/ml (Figure 1)'. a i ------ f-• 8' 10 12' 14 WAVELENGTiNI (IMHCRONS). Figure 2. Infrared!spectrum of triecetim mg/ml X total ml 1 g ~o triacetin =sa mple weight (g) X 1000 mg X 100 _ 1.15 mg/.ml X 100 1ml X 1 g_ X 100 1.33' g 1000 mg. micron fixed thickness cell was filled with benzene and'placed in the ref- erence beam to compensate for the solvent in the sample. The base linee was drawn from 7.5 to 9.0 microns. Specific extinction coefficient A.,,r. at 82' microns (A/mg/ml) • - mg triacetin/ml benzene An example of the calculation is as follotivs : Sp: ext: coeff. = 0.695 5.0 mg/mI = 0.139 A/mg/ml A typical sample ealculation is as follows: Acorr. total ml I g % trlacetln - X X X, 100' sp: ext. coeff: sample wt. (g) 1000 mg (A/mg/ml). 0.159. 100m1 I g ~X ~X~ X~ 100 0.139 A f mg/ml 1.33 g, 1000 mg, = 8.6% triacetin Results and I Discussion Ttvo~ standard solutions of triace- tin in benzene were prepared. From the first solution (1.004 g/100 ml) four dilutions were made, while from, the second solution, (0:800' g/1100 ml) three dilutions were pre- pared. These soiutions were analyzed using the 191.7 micron fixed thick- wtth the infrared spectrophotometer ness cell for the samplc. The 1'78.00 and the corrected absorbance of the 8.2 micron bandl computed (Table 1). The calibration curve prepared from these values was linear in the range investigated from one to five milligrams per milliliter (IFigure 1). The benzene exfract' of the cellu- lose acetate fibers did not show ab- sorption in the seven to nine micron region where the triacetin content was measured. Therefore, no cor- (Tobacco Science 27) rection for a blank hadl to be made in the calculs.t'ions. The recovery experiments were carried out by adding triacetin to untreated cellulose acetate fibers in the following manner: the cellulose acetate fibers were placed in a Soxh- let extraction thimble and a known amount of triacetin placed on the fibers. The compositions rangedl from seven to nine percent, by weight. After the addition of the triacetin, the sample stood for one hour, to simulate more elosely the conditions used in preparing, cigarette filters. The sample was extracted with 75 ml I benzene for one hour in a Soxhlett extraction apparatus which was wrapped with aluminum foil. The extract was transferred quantita- tively to a 100 ml volumetric flask, di- luted to volume with benzene, and analyzed in the 1911.7 micron fixed thickness celli The 178.0 micron fixed thickness cell filled withi benzene was placedl in the reference beam: The infraredl spectrum of this sam- ple was obtainedl and the triacetin calculated. The percent recovery of added triacetin is shown in Table 2. To determine the triacetin content't of filters oni commercial cigarettes five brands werQ examined. Three samples of twenty cigarettes each were takeni for e-ieh brandI examined. The filters were removed from the cigarettes, the paper was stripped from around the filters, and the fll- ~ ters were weighed. They were ex- tracted and treated' in , the same man- W ner as the cellulose acetate fibers in ~ the recovery experiments. The infra- red spect'ral were examined, and the ~ t calculated' results are shown ini Table 3. ~ A major advantage of this methodl O i i ifi i Th b enzene ex- s ts spec e c ty. tracts of the filt'ers from the eom-
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Table 1. Concentration and Absorbance Values of Solutions Used to Prepare Calibration Curvee mg triacetin/ mfbenzene 5.0 4.0 3.0 1.6 1.0 Sample Number 1 2' 3' 4 corrected absorbance at 8.2 microns 0.695 ' 0.548' 0.414 0.223' 0.140 Table 2. Recovery Values of'Triacet'in Amount' Added i Amount Found (mg) 1'45' 98 90 97 (mg) 145 98 90 94' Specific extinction coefficient' 0.139 0.137 0.138 0.139 0.14!0 Percent Recovery 100 100 100 97 Table 3. Triacetin Content of Filters from Various Cigarette Brands Det'ermina- Determina- Determina- Standard Brand tion # I tion #2 tuon #3I Average Deviation "A" 8.8°fo, 8.5% 8.9% 8.7% 0:21 "B" u n 9.0 8.8' 9.1 9.0 0.16' C 3.0 2.9' 2:9 2.91 0.07 "Dy, 5.2 5.5' 5.11 5.3 0.21 "E„ 9.1 9.4 9.3 9.3 0.16 (Tobacco Science 28) mercial cigarettes were examined initially from two to fifteen microns. This approach immediately will show whether any other additives are, present which would interfere with the triacetin analysis. No other compound or combination of com- pounds will give the identical infra- red spectrum of triacetin. In the titration method a separate qualita- tive analysis would have to be per- formed to verify the presence of'tri' acetin and' determine whether any interfering compounds are present. Summary. The benzene extraction procedure waa found to be rapid, precise, and accurate. Analyses of samples con- taining known amounts of triacetin showed a recovery of 99%. Good! pre- cision1was obtained for the analyses of' commercially available cigarette brctnd§: In comparison to the method described by Cundiff (1'959); it was not necessary to prepare standardi solutions other than the initial solu- tions required to obtain the calibra- tion curve for triacetin in benzene:. The method described in this paper is specific for triacetin and allows the, possible quantitative analysis of' other filter additfives, Literature Cited Ctindiff, Robert' H., "Determination of Triacetin in Filter Plugs,"' To- bacco Science, 148: 20-21 (1959). ikd~44

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