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p PHILIP MORRIS HOLLAND B.V VENTILATIOAI LEVEL OF'VENTILATED CI'GARETTES~ DURING HUMAN SMOKING by B. van Duuren Analytical Services Bergen op Zoom, February 26, 1985 ~ N .M~AP ~

PHILIP MORRIS HOLLAND BN: -1- AIM OF THE TEST Dtr-ermination of the ventilation level of ventilated cigarettes during humamsmoking„ without any disturbance of equipment on the cigarette during smoking. ;; ~:i~;~:M;'..

PHILIP INIORRIS HOLLAND B.V INDEX -2- ~ Page : Conclusion 3' 11. Theory 4 2. Execution of the test 5 2_ 1i. General 5 }'2'.2. The smoking, of cigarettes by subjects 5 -*2'_3. The smoking of cigarettes according,to NEN 3382 6 3. Discussion of the results 7 4. References 9 5. Tables (1 - 4) 6. Graphics (1 - 4)). 7. Appendix I and II k

PHILIP 1IORRIS ~ HOLL.ati DB.V. CONCLUSION -3- $~ means of this method a good estimation of the ventilation of filter Cigarettes, smoked by subjects, is possible without the subject being disturbed by any additional equipment, see graphics 1 and 2. It is possible with this ventilation result to predict the tar and nicotine level of cigarettes smoked according to NEN 3382. PHILIP MORRIS ULTRALIGHTS BARCLAY t Vintilation PBI/DDL ($). Ventilation dlxring, human smoking! 76,2' 75,7 82,6 31,5 Tar printed on pack (mg/cig) 1 1 Tar predicted (mg/cig) 1'1,4' 7,2 Smoke nicotine printed on pack (mg/cig) 0,1 0,2 Smoke nicotine predicted (mg/cig). 0,13 0,70 3 %

PHILIP~ MORRIS HOLLAND~~BV 1. THEORY -4- Par the determination of the ventilation level of ventilated'cigarettes during human smoking several testing,institutes (1, 2, 3) used a ventilation met.er to measure the ventilation. This ventilation meter was connected with tubes to a special cigarette holder (appendix 1) and this holder was placed over a cigarette. The subject placed the cigarette, with the holder connected to it, in the mouth and puffed the lit or unlit cigarette. The ventilation meter then determined the ventilation during human smoking. ae of the arguments against this method is that the subject is influenced ht the holder not being a natural way of smoking a cigarette. To avoid this influence a test completely different from former tests has been carried out. The only parameter which can be measured on smoked cigarette filters which could give an indication of the ventilation level is nicotine. Several literature studies (4) assert that if the ventilation increases the smoke nicotine decreases and also the nicotine content in the cigarette filter decreases. If this theory is correct then it must be possible to establish a correlation curve of the nicotine content in~filters of filter cigarettes at different ventilation levels smoked by subjects. # It is also possible to determine the nicotine content in filters of filter cigarettes smoked by subjects under natural conditions. With~ this last mentioned result it should:be possible to calculate the venti- lation level via the correlation curve of cigarettes smoked by subjects under natural conditions. W}th this calculated ventilation level it is possible to predict the tatr and nicotine level of filter cigarettes smoked according to NEN 3382.

PHILIP NtORRIS HQLLAND BV' 2. EXECUTION OF THE TEST 2.1;; General -5- Two different types of ventilated cigarettes have been~tested namely : - The conventional ventilated cigarette of 1 mg tar and 0,1 mg, nicotine - The channel ventilated cigarette of 1 mg tar and 0,1 mg nicotine Random samples have been taken of Philip Morris Ultra Lights (to be called PMU) and Barclay (to be called BAR) cigarettes. To3get a large range of ventilation the samples were divided into 4 catagories per brand. PM ULTRP:LIiGHTS BARCLAY 1. Maximum ventilation P75 and Ps B85 and~Bs 2. Ventilation of about 50% P50 B50 3. Ventilation of about 25% P25 B25 4. Ventilation of about 0% P0 B0 The samples were brought on the desire&ventilation by means of Tipp-ex on the porous zone of the tipping paper. After conditioning the cigarettes according to NEN 3382, the ventilation wa # measured per category per brand on the PDI-DDI apparatus from PM-USA. See tabLe 1 for the ventilation results. 2.2. The smoking of cigarettes by subjects Cigarettes of the 4 categories were smoked by 100 subjects by means of a cigarette holder to avoid~influences of the lips on the ventilation. Also standard product (P s and B s ) was smoked by 100 subjects but without a cigarette holder. . , '~ - - f~':

' PHILIP MORRIS HOLLAND B.V -6- To avoid big deviations in butt length~and the number of puffs, the subjects took one puff each 601seconds and stopped puffing whenithe ignitwion cone reached~the butt mark. .~ For one determination of nicotine in the cigarette filter 10 cigarette filters were used. So for each category of ventilation 10 determinations of filter nicotine have been made. The amount of nicotine was determined by means of a Gaschromatograph. For the filter nicotine results see table 2 and 3'and graphics 1 and 2. For the calculation of the 95% confidence level the t-distribution of Student was used. ~ 2.3. The smoking of cigarettes according to NEN 3382 The tar and nicotine level of each category of ventilation has been determined with a smoking machine according to NEN 3382 except for the water and nicotine determination for which a gaschromatograph was used which was calibrated with instruments mentioned in~the NEN 3382 (see appendix II). For the tar and nicotine results see table 4 and graphics 3 and 4.

PHILIP MORRIS H0LLatiDRV 3. DISCUSSIWOF THE RESULTS -7- A; The filjLm-er nicotine WN) results of human smoked cigarettes (smoked in a cigarette holder) show a good linearity (see graphic 1 and:2). FN'versus ventilation,PMU y = 1,0497 - 0',0066 x r = -0,992 FN versus ventilation BAR y = 1,3656 - 01,0059 x r = -0,994 x = ventilation, y = filter nicotine, r = correlation co-efficient. According to the r-distribution this is highly significant (G( = 1%). For the interpretation of the results of the human smoked cigarettes (without} cigarette holder) Ps and BS the regression lines of the upper and lower values of the 95% confidence level (C.L.) values are calculatedi. Upper values 95% C.L. versus ventilation PMU y = 1,1049 - 0,0071 x r = -0,995 BAR y = 1,4262- 0,0061 x r=-0,994 Lower values 95% C.L. versus ventilation PMU y = 0,9945 - 0,0061 x r = -0,987 BAR y= 1,3050 - 0,0056 x- r = -0,992 The filter nicotine of human smoked cigarettes without cigarette holder gives th4 following calculated ventilation values. Test Fil!ter Calculated Ventilation % Cigarette Nicotine via above mentioned formulas Determined mg/cig mean 95 % C.L. lower upper P s 0,55 75,7 72',9 78,2 B ~ s 1,18 311,5 22,3 40,41

PHILIP NIORRIS HOLLAN!D B1-: -8- The tar and smoke nicotine results, smoked according to NEN 3382, show a good'linearity with the following correlation co-efficients. Tar versus ventilation PMU y = Tar versus ventilation BAR y = SN versus ventilation PMU y = SN' versus ventilation BAR y = 8,456 - 0,0929 x r=-0,999 11,006 - 0,1216 x r = -0,999 0,5656 - 0,0058 x r=-0„992 1,0624 - 0,0114 x r = -0,990 x = ventilation, y = Tar or SN, r = correlation co-efficient. The tar and nicotine values at the calculated ventilations are : s CaLculated Predicted values Values printed ~ Ventilation, on the pack % Tar mg/cig SN, mg/cig Tar mg/cig SN mg/cig PMU 75,7 11,41 0;13' 1 0,1 BAR 31,5 7,2' 0,7& 1 0,2 N O N ~ ~ ~ NN N

PHILIP'MORRIS HOLLAND BY 4. REFERENCES 1 Ins'"titut Fresenius -9- "Unterscheiden sich bei der Zigarettenmarke Barclay die bei norm- gerechten maschinellen Abrauchen ermittelten :<- und N-Werte von den Werten, die bei einen dem naturiichen Rauzaen entsprechenden Abrauchvorgang entstehen. 2' Chemical Laboratorium Dr Horst Jenssen Einfluss der Zigarettenhalterung auf die Rauc_zeigenschaften beim naturLichen und maschinellen Rauchen. t 3 Ph*lip Morris Incorporated "Percent Tar Free" Claim on cigarettes. 4 Ventilation Seminar Philip Morris Inc. T.T.G. and Philip Morris USA, February 1983. ~ ~ 3 N ~ ~ ~ ~ N W ; ~ ~ t

Table 1 VENTILA7ION OF THE TEST' CIGAREZ`3'ES ~ Instrument : PDI/DDI TEST CIGARETPE DILUTIiON 95% CONF. INTERVAL x s n % P0 2,9 3,01 250 2,5 - 3,3 P25 't 29,7 5,9 250 29,0 - 30,4 PS0 50,8 5,1 250 50,2 - 51,4 P7S and Ps 76,2 8,0 250 75,2 - 77,2 B 2,3 2,9 250 1,9 - 2,7 0 P~y?Yi ! i; B25 21,6 5,8' 250 201,9 - 22,3 B50 54,0 5,8 250 53,3 - 54,7 B85 and~Bs 82:,6 4,1 250 82',1 - 83,1

Table 2 FILTER NICOTINE RESULTS OF THE TEST CIGARETTES SMOKED IN CIGARETTE HOLDERS BY 1001SUBJECTS Instrument,j: Gaschromatograph TEST VENT. FILTER NIC. MG/CIG. 95% C.L. CIG. % x s n P0 2,9 1,01 0,09 10 0,95 - 1,07 P2S 29,7 0,87 0,04 10 0,84 - 0,90 P50 50,8 0,74 0,04 10 0,71 - 0,77 P7S 76,2 0,52 0,03 10 0,50 - 0,54 B0 ~ 2,3 1,34 0,10 10 1,27 - 1,41 B25 21,6 1,24 0,05 10 1,20 - 1,28 B50 54,0 1,08 0,07 10 1,03 - 1,13 B75 82,6 0,86 0,06 10 0,82 - 0,9& Table 3 ~:;~ FILTER NICOTIiNE RESULTS OF THE TEST CIGARETTES SMOKED BY MOUTH BY 100 SUBJECTS Instrument : Gaschromatograph TEST FILTER NIC. MG/CIG. 95% C.L. CIG. x s n P s 0,55 0,01 9 0,54 - 01,56 B s 1,18 0,09 10 1,12 - 1,24 C.L. = Confidence Level

TAR AND SMOKE NICOTINE RESULTS OF THE TEST CIGARETTES SMOKED ON A SMOKING MACHINE ACCORDING TO NEN 3382 y -- - - - -- ~'• .t. TEST VENT. TAR IN MG/CIG. SMOKE NICOTINE IN MG/CIG CIG. ~ x s n 95% C.L. x s n 95% C.L. 2,9 8,1 0,39 9 7,8 - 8,4 0,53 0,019 9 0,52 - 0,54 P25 29,7 5,8 0,50 10 5,4 - 6,2 0,41 0,024 10 0,39 - 0,44 p50 50,8 3,8 0,38 10 3,5 - 4,1 0,29 0,028 10 0,27 - 0,31 P75 76,2 1,3 0,14 10 1,2 - 1,4 0,10 0,008 10 0,09 - 0,11 B0 2,3 10,5 0,46 10 10,2 - 10,8 0,98 0,036 10 0,95 - 1,01 B25 21,6 8,6 0,30 10 8,4 - 8,8 0,87 0,028 10 0,85 - 0,89 B50 54,0 4,6 0,33 10 4,4 - 4,8 0,49 0,036 10 0,46 - 0,52 B85 82,6 0,8 0,15 10 0,7 -. 0,9 0,08 0,018 10 0,07 - 0,09 C.L. = Confidence Level ~~z89pgzoz

FILTER-NIC©TINE(ting/cig) / VENTILATION X of human smoked cigarettes 1.5 1.4 1.3 ZI 0.6 ~ 0.5 0.4 0.3 0.2 0.1 0.0 , y, ;.y 'UYiF'HIL1P MQRRIS ULTRA L IGH±S ventiiation 0 20 40 60 80 100 VEN?ILATION 7G O PMU y=1.049-0.0066x 0lSz&svRzoz

EILTER-NIOOTINE(mg/ci9) / VENTILATION 76 0 ~ •.,,.. of human smoked wiqarettea 20 T ' ' 80 100 40 60 yE_ NTILATION % 0 BAR y=1.365-0.0059x 83z9gtszoz

TAR (mg/cig.) / VENTILATION X ACCORDING NEN 3382 12 11 10 9 8 a ~ ~ a ~ 6 ~ 0 13 BAR y=1 1.006-0.121 x r #, ,..,.. - F 20 real I ventilation 40 T 60 real T ventilation T- 80 100 VENTILATION R 0 PIAl1 y=8.456-0.0929x ~SCsA~ V ts4~~ ~'t ~:~

SMOKE-NICOTINE(mg/Cig.) / VENTILATION 7. ACCORDING TO NEN 3382 1.2 +, 1.1 1.0 0.9 u 0 8 \ . a E W z O .6 - U z I 0.5 - W Y 0 0.4 -~ ~ 0.3 0.2 0.1 0.0 ,w ;,* real SN real _1 SN --f 0 20 40 reali ventilation 1 60 real iventilation T-T--- T - 1 80 100 VENTILATION 7L p BAR y=1.062-0.011 x O PMU y= 0.565-0.0058x a~zss~szo~

Appendix I 6204 Taunusslein 4 (Neuhol) Telefon (06128) 744-0 Telex 4-182756-bios d -28- Gesamt-Strom A Strangteil' der Zigarette Strang-Strom , ~ ventilations- Strom B.M~t: Vors. MW. Dr. W. Frws-Mm.§IWMC O/rNLLb W. Sch"0440r - GeschY1NOMnm. Or. R. Fes.n1us. L Fre..n1Ys -/M811]A 94b4 SGMwaWac/l. -~~-~+.nry 2Y YYMOs2r1GkM.OMOAM - OYCr1 ~fLWswNN - Y/1OMM.GMNITIVYnO. ~e.On.nikUtuq. V.nA.MYflpurq.unw.r Atl.a. und GuNM1.n•.o.rN tl.renu~w..~.....~'~ Lnu maGnc. unu ..,,~~ ,~, 8101oglsatie ~~S~~~u~ Laboratoi~en GmbH', Fresenius Schernatische Darstellung d'er Glasbirne fur PPA-MeBanordnung Filterende d'er Zigarette N - 79 -

PHILIP MORRIS HOLLaNID 8t: Appendix II GASCHROMrATOGRAPHI!C DETERMINATION OF WATER AND NICOTINE Water determination Conditions : injection temperature 220 °C oven temperature 180 °C TCD temperature 220 °C Colom : Porapack Q 80 - 100 mesh 6' * 1/8" s.s. Carrier gas : Helium 30 ml/min. Inte#na1 standard : Ethanol 0,5 mg/ml Extraction solvent : Isopropanol Nicotine determination Conditions : injection temperature 220 °C oven temperature 180: °C FID temperature 250 °C Colom : 7% carbowax 20 m & 2% KOH & 3% PMPE 80 - 100 mesh 4' * 1/8" s.s. Carrijr gas : Nitrogen 30 ml/mim. Internal! standard': Heptadecaan 0,2 mg/ml Extraction solvent : Isopropanol'