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Accession number 773 LarliAord L ~'cooarch Canfaa° Graenshcgv'o APPLICATION OF FREE NICOTINE TO CIGARETTE TOBACCO AND THE-DELIVERY OF THAT NICOTINE IN THE CIGARETTE SMOKE Submitted by: T. M. Larson and J. P. Morgan Report number: Qate: 6/8/76 5utnmary or Abstract: Nicotine was applied as free nicotine and nicotine tartrate to different tobaccos for the purpose of increasing the nicotine to tar ratio in the cigarette smoke. Leaf analyses showed that the added nicotine remained on the tobaccos for up to a five week period. Smoke analys¢s and puff by puff smoke analyses showed that the nicotine was delivered in the smoke in the same manner as naturally occurring nicotine in regular production cigarettes. Random taste paneling implied that only a small addition of free nicotine was needed to provide the impact of a higher nicotine cigarette. TML&JPM:lmh Xc: Dr. F. J. Schultz Ms. M. S. Ireland Dr. H. J. Minnemeyer Mr. C. L. Tucker Library

r Part I. Application of Free Nicotine to Cigarette Tobacco : Free nicotine (Eastman Practical Grade) or.nicotine tartrate was sprayed on cut cigarette tobaccos three different ways to determine if the spray solvent played a role in enabling the free nicotine to remain on the tobacco. Nicotine was sprayed onto each of three 100 gram batches of our Kent Golden Light blend. Thirty milliliters of solvent and 5 ml of nicotine were sprayed each time using water and free nicotine, ethanol and free nicotine,and water with nicotine tartrate. After spraying, approximately half of each 100 gram batch was divided into two equal portions. One portion was dried in air under a fume hood, and the other portion was dried in an oven at 105°C for 2 1/2 hours. A sample of each portion was submitted to the leaf lab for nicotine analysis immediately after drying. A second sample of each portion was resubmitted to the leaf lab after one week in the conditioning room. The results of these analyses are given in Table 1. . Nicotine was applied to the same Kent Golden Light blend by spraying with a nicotine-freon-11 solution. A time study over a five week period was done, to test the stability of nicotine applied in this manner. The results are given in Table 2. Nicotine was also sprayed onto one grade of flue-cured tobacco (VEE-71-4) and to puffed tobacco using freon as the spray solvent. Leaf analysis data for nicotine is given in Table 3. Interpretations - Table 1. Data in Table 1 show that significant losses of nicotine due to drying do not take place. Differences that are apparent may be due to different moisture levels of samples. It appears that once nicotine is applied to tobacco it is not easily driven off by heat. Those samples on which water solutions were sprayed, had moisture levels of 30%, yet the oven drying did not remove significant levels of nicotine. Interpretations - Table 2. Data in Table 2 shows that nicotine applied to cigarette tobacco remains on the'tobacco over long periods of time. No significant decrease in nicotine over a five week span was observed. Interpretations - Table 3. Data in Table 3 shows that nicotine can be applied to puffed ~ tobacco or flue-cured tobacco and that no significant losses of nicotine occur from that tobacco over a five week period of time.

2 Conclusion Free nicotine can be sprayed onto tobacco using a variety of solvents ( Water, freon, ethanol.) Nicdtine tartrate can'be sprayed on using water. Drying does not cause significant losses of nicotine and the nicotine will remain-on the tobacco for at least five weeks. Part II. Delivery of Added Free Nicotine on Tobacco to the Smoke Various publications in the literature report that the nicotine delivery from cigarettes smoked in the standard manner (one 35 ml, 2 second puff every 60 seconds) is 12-18%. From our experiments we have determined that free nicotine added to tobacco is delivered in the smoke similarly to nicotine naturally occurring in tobacco. Experimental One grade of flue-cured tobacco (VEE-71-4) was cut and made into 85 mm straight cigarettes. These cigarettes were submitted to the smoking lab for standard analysis (Table 4). From the average weight per cigarette, the % nicotine in the tohacco, the butt length and the milligrams of nicotine delivered per cigarette the % delivery was calculated.(Table 5). The same grade of tobacco was sprayed with a nicotine solution in Freon 11, made into 85 mm straight cigarettes and submitted for smoke analysis. The percent delivery on these cigarettes was calculated, as well as for production Old Gold Straights. (See Table 5 ) A puff by puff analysis of three different 85 mm straight cigarettes identified as KGLN-38, VEE-71-4N, and production Old Gold Straights was done to see if added nicotine was delivered in an unusual manner. Sample KGLN-38 was a blend similar to ' Kent Golden Light except that all flue-cured tobacco and regular puffed tobacco was replaced with nicotine treated puffed tobacco (3.2% nicotine) so that the final blend contained 38% treated puffed tobacco. This gave an overall 3.3% nicotine level to the blend. The VEE-71-4N was the same tobacco described in Table 3. The puff by puff profiles of each of the 85 mm straights are given in Figure 1. Interpretations - Nicotine Delivery in the Smoke Table 5 lists the nicotine delivery of the three types of cigarettes smoked (Figuring that 73% of the tobacco in each cigarette was smoked). The two cigarettes with added nicotine delivered 9-10% of the total nicotine, while the "natural" nicotine cigarettes delivered 11-12% of the total nicotine. The difference may be within experimental error.

Puff by Puff Analyses The puff by puff analyses (profiles) show that added nicotine is delivered in a manner similar to natural nicotine in tobacco; that is, the nicotine delivery increases with each puff. Conclusion Added nicotine is delivered in the smoke at the same rate or close to the same rate as natural nicotine in tobacco. The puff by puff profiles show that this delivery is spread out over the entire smoking of the cigarette and the nicotine is not delivered at a higher rate on the first few puffs. Comments Most of the nicotine treated samples made into cigarettes were so strong when smoked that they were very unpleasant to most smokers who tried them. This was puzzling, because based on our calculations, these cigarettes would not have delivered an extraordinary amount of nicotine. One particular sample of cigarettes made with the KGLN-38 blend in Kent Golden Light paper with Kent Golden Light filters should have delivered less than 1.0 milligrams of nicotine per cigarette, yet they were far stronger than even an Old Gold Straight. We submitted a few of these cigarettes to.the smoking lab and the average nicotine delivery was 0.8 mg/cig. This indicated that a small amount of free nicotine added to the tobacco at a level low enough not to significantly change'the T & N numbers did provide the impact of a'regular higher nicotine cigarette. This may be what R. J. Reynolds is doing with Vantage. Summary Free nicotine can be successfully applied to cigarette tobacco at levels up to 5% by weight simply by spraying in a convenient solvent. The nicotine treated tobacco can undergo drying at - 105°C for 2 1/2 hrs. and periods of storage for at least 5 weeks without significant loss of applied nicotine. No evidence of nicotine decomposition on the tobacco was seen. The added nicotine was delivered in the smoke at levels comparable to naturally occurring nicotine and the puff by puff profiles indicated normal delivery patterns for added nicotine. Also, it appeared that the added free nicotine, even when delivered at low levels, provided the impact of a high delivery cigarette. Suggestions for further work O 1. Determine what level of added free nicotine is necessary W to provide a "popular" impact. a M 2. Investigate ways of applying nicotine and/or nicotine saltv to R.L. ~A"

3. Investigate a nicotine addition at different locations in current production process, i.e., recasing, top flavor, R.L. puffing process.

Table 1 - Effect of Drying on Nicotine Level of Nicotine Treated Tobacco . Sample N0. 1 2 3 4 5 6 7 Nicotine Level ($) 5/25/76 1.63 5.08 4.84 5.12 5.01 4.40 4.59 Nicotine Level (%) 6/2/76 1.77 4.76 4.76 4.80 4.97 4.68 4.85 Sample Identification #1 - Control - Kent Golden Light Blend #2 - KGL Blend, Nicotine sprayed with water, dried at 105°C for 2 1/2 hours #3 - KGL Blend, Nicotine sprayed with water, air dried #4 - KGL Blend, Nicotine for 2 1/2 hours. #5 #6 sprayed with ethanol, dried at 105°C KGL Blend, Nicotine sprayed with ethanol, air dried KGL Blend, Nicotine tartrate sprayed with water, dried at 105°C for 2 1/2 hours. . #7 - KGL Blend, Nicotine tartrate sprayed with water, air dried.

Table 2 Kent Golden Light Tobacco + 2% Nicotine with Freon 11 Date Nicotine Added: Analysis Dates 4/12/76 • Control Sample 4/12/76 1;67% 3.35% 4/19/76 1.72 3.45 4/26/76 1.60 3.31 5/3/76 1.60 3.29. 5/10/76 1.55 3.22 5/17/76 1.62 3.29

Table 3 VEE-1971-4 Tobacco + 5% Free Nicotine with Freon 11 Date Sample Sprayed . 5-10-76 Analysis Dates Sample (% Nicotine) 5-10-76 5.40 5-17-76 5.44 5-24-76 5.40 Puffed Tobacco + 5% Free Nicotine Date Sample Sprayed . 5-12-76 Analysis Dates Sample (% Nicotine) 5-12-76 3.20 5-19-76 3.40 5-26-76 3.10

Table 4 Smoke Analyses: Control VEE-1971-4 Sample VEE 1971-4N* KGLN-38* Weight (gms/cig.) 1.094 1.106 ' 0.962 Pressure Drop mm water/cig.) 92 93 . 118 Dry Particulate. Matter (mg/cig.) 21.4 23.0 17.3 Nicotine (mg/cig.) 1.31 4.29 2.00 Corrected Particulate 20.1 18.7 15.3 Matter (mg/cig.) Puff Count 8.7 9.5 7.4 % Nicotine on Tobacco (From Leaf Analysis) 1.42 5.4 3.3 *Nicotine sprayed on with Freon 11

. Table 5 72.94% Tobacco Smoked ' Nicotine Delivery VEE-1971-4 11.6% VEE-1971-4N 9.8% , KGLN-38 8.6% Old Gold Straight 10.6% Table 6 Puff by Puff Analyses: Milligrams nicotine per puff Number of Puffs VEE-1971-4 KGLN-38 Old Gold Straight 1 0.485 mgs/puff 0.183 0.094 2 0.514 0.203 0.103 3 0.571 0.222 0.118 4 0.615 0.269 0.125 5 0.685 0.298 0.130 6 0.572 0.337 0.148