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Xc: H. J. Minnemeyer R. R. J. W. W. M. Slaven Hurst Johnson y0ak'-fed MEMORANDUM August 4, 1982 TO: M. S. Ireland FROM: M. A. Sudholt SUBJECT: Cigarette with Increased Impact and Nicotine to Tar Ratios The migration of nicotine from tobacco to acid treated paper has been done routinely by mixing paper and cut tobacco in covered jars and heating to 45°C. Currently, the same system is being used to study the migration of nicotine from tobacco to acidic ion exchange resin and cellulose acetate filters. The migration to cellulose acetate filters was done by heating rods and Golden Light blend plus 5% by wt K CO for 24 hours in a closed jar at 45°C. The procedure was repeatea and the jar was heated for a week. The treated filters were then attached with tape with no air dilution, to 100 Golden Light tobacco rods. As shown in the smoke data in Table 1, the nicotine to tar ratio was increased by about 5% for both the 24 hour and 1 week study. The difference in the control and treated samples was very small. The one week sample and its control were compared organoleptic- ally by a member of the taste panel. The results are shown in Table 1. The approach did not appear to be useful for increasing nicotine to tar ratios. Migration to sulfLhc acid and carboxylic acid polystyrene divinylbenzene ion+exchange resin was attempted. The resin was converted to the H form and then allowed to be in contact with Golden Light blend in a covered jar at 45°C. The resin was put in a cellulose acetate filter and the filter was attached with tape to a 100 mm Golden Light tobacco rod. There was no air dilution. The initial data collected is shown on Table 2. The resin was not weighed, however a 3/8" 1 x 5/16" d cavity was filled in each cigarette. A 33% increase and a 7% increase in nicotine to tar ratio's was observed. The work was repeated with an exact amount of resin, 100 mg, in each cavity. The cellulose acetate plugs were loosened and moved and placed up against the resin in the cavity. The results are shown in Table 3. Although the change in the ratio of nicotine to tar was small in the Amberlite IRC-50 cigarette, an increase in impact was detected. O Organoleptic results were very promising. The sulfonic acid group resins did not give increases in nicotine to tar ratios in W the second run which was contrary to previous results. The work N was repeated again with the use of burley strip in place of ~ Golden light blend ~ ~

in the migration step. The results are shown in Table 4. Little or no increase in the nicotine to tar ratio was seen. The initial experiment was repeated using 5% K CO - Golden Light Blend and similar cigarette construction. 2No3increases were seen in nicotine to tar ratios at shown in Table 6. Either the initial data showing nicotine to tar ratio increases were artifacts or the cigarette cavity construction may not be providing good mixing of resin and smoke. Alternative ways of getting nicotine on t~e ion exchange resins were also investigated. Contacting the, H form resin in a batch process with watdr extracts of golden light blend, flue cured TPP scrubber water, and burley TPP scrubber water did not give increased nicotine to tar ratios as shown in Table 4 and 5. Although the results from attempts to migrate nicotine to ion exchange resins and then elute nicotine from the resin in a cigarette filter have been negative, the general approach still seems promising: The organoleptic results indicated increases in impact from resin,treated in the standard oven migration experi- _ ment. A British patent reported a cigarette filter containing nicotine spray-dried in gum acacia giving nicotine transfer of , 0.77 mg into the mainstream from the filter (1). Future studies may include the following: 1. Investigation of the migration of nicotine from tobacco to other materials for use in filters, such as a cellulose phosphate ion exchange material or ground dried tobacco stems. 2. Investigation of the transfer of nicotine from an ion exchange resin to smoke aerosol using resin which contains nicotine absorbed from the burley dryer stack effluent. 3. Adding a diluent such as pumice to the treated ion exchange resin to promote better mixing of smoke and resin in the ~ cavity filter. 4. Determine if the impact is increased in these migrated resin cigarettes even though the nicotine to tar ratio did not change. * References: 1. Bolt, Anthony John Nelson; Chard Brian Chester, BRIT. UK Pat. Appl. GB 2064 296, June 17, 1981. /lp:2 2

Table 1. Results of smoke data on cigarettes prepared from 100 mm Golden Light tobacco rods and cellulose acetate filters treated by standard oven migration for 24 hours and one week. 24 hr Control 24 hr 1 week Sample Control 1 week Sample Weight 1.157 1.157 1.176 1.183 Pressure Drop 129.7 127.5 135.3 139.3 Dry Part Mat 16.0 16.3 14.9 15.8 Nicotine 1.09 1.17 1.06 1.19 Corrected Part Mat 14.9 15.1 13.8 14.6 Carbon Monoxide 19.0 19.6 20.1 20.1 Puff Count 7.8 7.5 7.9 8.1 Nicotine/Dry Part Mat 0.0681 0.0718 0.07114 0.0753 5.4% inc. 6% inc. Impact 10 10 Taste Amplitude 10 11 Overall Acceptability 10 9 Comments sample has a musty, earthy note 3

Table 2. Preliminary Smoke data (1 pad per sample) on cavi~y cellulose acetate filters filled with ion exchange resin (H ) which was prepared using the standard oven migration procedure. 50-100 Mesh Dowex 50W-X4 20-50 Mesh 20-50 Mesh Amberlite IR-120 Amberlite IRC-50 (SO3H) Control Sample (SO3H) Control Sample (CO3H) Control 5ample Weight 1.112 1.198 1.141 1.170 1.173 1.203 Pressure Drop 112.4 133.6 110.2 114.8 112.4 116.4 Dry Part Mat 26.3 17.6 21.8 18.9 17.6 18.3 Nicotine 1.40 1.24 1.39 1.30 1.25 1.28 Corrected Part Mat 24.9 16.3 20.4 17.6 16.3 17.1 Carbon Monoxide 18.7 15.8 17.9 16.4 18.7 18.8 Puff Count 7.8 8.1 7.5 7.3 7.3 7.3 Nicotine/Dry Part Mat 0.053 0.0705 0.0638 0.0688 0.0710 0.0699 33% inc. 7% inc. 4

Table 3. Smoke data (3 pads per sample) on cavity celluloTe acetate filters containing 100 mg of ion exchange resin (H ) which was prepared using the standard oven migration procedure. 50-100 Mesh Dowex 50W-X4 20-50 Mesh 20-50 Mesh Amberlite IR-120 Amberlite IRC-50 (SO3H) Control Sample (SO3H) Control Sample (CO3H) Control Sample Weight 1.300 1.265 1.290 1.271 1.265 1.257 Pressure Drop 139.1 137.7 126.1 122.9 124.8 119.8 Dry Part Mat 17.3 17.2 17.0 17.0 17.3 17.0 Nicotine 1.17 1.19 1.21 1.20 1.13 1.20 Corrected Part Mat 16.1 16.0 15.8 15.7 16.2 15.8 Carbon Monoxide 17.6 18.2 17.1 17.2 16.8 17.0 Puff Count 7.8 7.4 7.5 7.2 7.1 7.2 Nicotine/Dry Part Mat 0.0676 0.0692 0.0711 0.0711 0.0653 0.0705 , 8% inc. Impact 10 11 Taste Amplitude 10 10 Overall Acceptability 10 9.5 Comments sample has a sl bitter taste which could be masked by flavors- 11 may be conservative for impact. 5

Table 4. Smoke data (3 pads per sample) on cavity cellulose acetate filter filled with treated ion exchange resin-no air dilution. Sulfonic Acid IR-120 20-50 Mesh Flue Cured Burley Cptrol H form Migration burley strip Scrubber H2 0 Scrubber H2 O Weight 1.205 1.200 1.192 ~1.218 8 Pressure Drop 123.5 128.5 126.8 139.9 Dry Part Mat 17.5 17.2 16.7 17.3 Nicotine 1.15 1.17 1.11 1.19 Corrected Part Mat 16.4 16.0 15.6 16.1 Carbon Monoxide 18.4 18.5 17.5 19.5 Puff Count 7.3 7.3 7.2 7.3 Nicotine/DPM 0.0657 0.0680 0.0665 0.0688 6

Table 4 (cont) Sulfonic Acid Dowex 50W-X4 50-100 mesh C?ntrol Migration H form burley strip Flue Cured Scrubber HmO Burley Scrubber Hm0 Weight 1.183 1.188 1.205 1.189 Pressure Drop 127.5 132.1 171.6 167.3 Dry Part Mat 16.6 16.8 16.2 17.1 Nicotine 1.11 1.15 1.06 1.17 Corrected Part Mat 15.5 15.7 14.7 16.0 Carbon Monoxide 17.6 18.6 18.3 18.1 Puff Count 7.4 7.4 7.1 7.2 Nicotine/Dry Part Mat 0.0669 0.0684 0.0654 0.0684 7

Table 4 (cont) Carboxylic Acid IRC-50 20-50 mesh Weight Pressure Drop Dry Part Mat Nicotine Corrected Part Mat Carbon Monoxide Flue Cured Burley C~ntrol Migration Scrubber Scrubber H form burley strip E220 H~0 1.213 1.194 1.199 1.200 130.9 122.7 129.2 127.1 19.7 17.8 19.0 17.3 1.29 1.24 1.24 1.19 18.4 16.6 17.7 16.1 20.0 18.5 20.5 18.7 Puff Count 8.1 7.9 Nicotine/DPM 0.0655 0.0697 6% inc. 7.5 7.5 0.0653 0.0688 8

Table 5. Smoke Data (3 pads per sample) on cavity cellulose acetate filters filled with ion exchange resin (H ) treated with water extract of Golden Light blend. 50-100 Mesh Dewex 50W-X4 20-50 Mesh 20-50 Mesh Amberlite IR-120 Amberlite IRC-50 (SO3H) Control Sample (SO3H) Control Sample (CO3H) Control Sample Weight 1.300 1.271 1.290 1.209 1.265 1.276 Pressure Drop 139.1 149.9 126.1 126.7 124.8 124.9 Dry Part Mat 17.3 17.5 17.0 16.8 17.3 17.9 Nicotine 1.17 1.11 1.21 1.19 1.13 1.19 Corrected Part Mat 16.1 16.4 15.8 15.6 16.2 16.5 Carbon Monoxide 17.6 18.2 17.1 16.8 16.8 17.0 Puff Count 7.8 7.2 7.5 7.4 7.1 7.6 Nicotine/Dry Part Mat 0.0676 0.0634 0.0712 0.0708 .0653 0.0665 9

Table 6. Results from repeat of procedures used to make cigarettes smoked in Table 2. (3 pads per sample) Resins were in migration jar at 45°C for 1 week with 5% by wt. K2C03 - Golden Light blend. 50-100 Mesh Dowex 50W-X4 (SO3H) Control Sample 20-50 Mesh Amberlite IR-120 (SO3H) Control Sample 20-50 Mesh Amberlite IRC-50 Contro103HSam le Weight 1.258 1.292 1.307 1.275 1.271 1.356 Pressure Drop 118.0 113.2 113.0 117.3 115.4 114.1 Dry Part Mat 19.5 17.8 18.4 19.3 19.4 17.9 Nicotine 1.31 1.19 1.24 1.27 1.31 1.24 Corrected Part Mat 18.2 16.6 17.1 18.0 18.4 16.7 Carbon Monoxide 21.2 19.4 19.9 20.3 21.1 18.6 Puff Count 7.8 7.3 7.7 7.2 7.7 7.5 Nicotine/Dry Part Mat 0.0669 0.0669 0.0674 0.0658 0.0675 0.0693 10