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Thelma_.q. Heatwole A:,.Tamol :a~~~~~~DENTIA July 7, 1967 ~;~ec.t: Reuiew of Controlled Profile_Cigaret (Delayed Dilution) I have hypothesized that the smoker would be satisfied by a cigaret that delivers early normal full-bodied puffs in the first part of a cigaret; thereafter the cigaret would become air diluted, reducing TPM and*nicotine delivery during the second portion of the cigaret. The metkod of accomplishing this delayed dilution would be to cover air dilution holes in the filter with a film that would degrade and open the holes after being contacted by smoke constituents (primarily water) during the early normal puffs. Invention I consider°`4e point of invention to be degradation of the film covering the dilution holes by smoke constituents (primarily water), automatically in a controlled manner after a portion of the cigaret has been smoked in a normal fashion, i.e., TPM, RTD, etc. Results to Date 1. Filter dilution at or near last puffs has been reproducibly demon- strated using several water soluble films of varying melting points in several filter configurations. 2. Dilution at middle puffs has been recorded but cannot be repro- duced for reasons unknown at this time. . Closing of some partially opened water soluble films beginning at early puffs has been demonstrated, indicating that smoke constituents (probably water) can affect films in the filter_at earlier puffs. -4. Degradation of film material in the filter cannot be attributed to the temperature alone based on projected filter temperatureswhen film A degradation takes place. Materials that melt at much highertempera- ' Ntures than can ever be achieved in the filter have opened dilution .holes. One experiment sub,jecting film in filters to high-.temperatures alone for a much longer period of time than in an actual cigaret did fax~ot open, From these results, coupled"with temperature gradients lished in the literature,' we can only conclude that smoke constitu- ,,,are responsible for film degradation. The high`melting or heat ng temperatures of some successful films further reinforce this usion. The following areas have been investi gated and you will probably want to modify the original disclosure to include some of them.

Page 2 Mrs. Thelma C. Heatwole July 7, 1967 Demonstrations Made in the Following Areas (data sheets attached) Films with Bubble Coated Reactive Stressed I~tono Films Filler Films Films Films . PV alcohol 2. Polybond 4. Radel (starch ether) (polyethylene Polycryl (filler) oxide) 3. PV alcohol Alundum (filler) 5. Polybond 7. Quick-Sol-P. (CO2 release) (modified 6. Radel Radel) CO2 release (thick film (S-P configu- 0.3 mil ration, bubble heat sealed) coated) 8. Quick-So1-P. (laminated b roll coater}y A. Bubble Coated Films We have found that many thin water soluble films are instantaneously soluble when placed on a water surface. However, when these same mater- ials are used to fill the small air dilution holes at thinner minimum thickness dimensions. (10-15 microns) small atomized particles of water contacting these films do not break them. The particles remain on the surface of the film with some local dissolution taking place but not causing the film to rupture. Surface phenomena appear to come into play. Films that have a bubble coated porous structure (a patented process - ref. your file) are desirable because they are wetted by these same atomized particles. The bubble structure has been observed to break down but films do not rupture because of this wetting action alone, again due to surface effects. B. Reactive Films An approach to make the water soluble film more degradable when contacted by smoke moisture has been to incorporate reactive components into the films that react with water. One attempt has been to add citric acid and sodium bicarbonate to the film via a suitable solvent system. The reaction would generate CO2 which should help in film degradation. An extension of the reactive film approach would be to add reactants Some reactive films have been made in bubble coated form, but no advan- tage, such as degradation at earlier puffs, has been achieved. However, this approach has not been exhausted and might prove fruitful at a later C,fl date. Ga 'XIq such as an acid and a base which would form water. A Al

Page 3 Mrs. Thelma C. Heatwole July 7, 1967 C. Stressed Films We have investigated the possibility of increasing degradability of films by using an oriented or stressed film to close dilution holes. Quick-Sol-P (Polymer Films, Inc.) is a Radel film that has been cast at approximately 2.1 mils, then pulled down to a 0.3 mil thickness introducing a permanent orientation in the machine direction. This type of film breaks when hit by water droplets. When loosely laminated in the filter)cigarets also degraded at or near last puffs. The same film has been machine laminated itito holes, also exhibiting degradation at last puffs. During solvent system bubble coating investigations, some films have been cast that exhibit a granular structure that appears to be a stressed film. Water droplets easily broke the film. When coated in holes, however, the granular structure was not as apparent and no increase in film degradation was noted. Mr. Jenkins has suggested the possibility of an irradiated water soluble film that would be under stress. His search of the litera- ture did not produce a candidate to be investigated; however, this possibility exists. Another type of film that remains to be investigated is a stressed bubble coated film. This could possibly be accomplished by bubble coating a stretchable carrier (i.e., creped or clupaked paper), then pulling out a percentage of built-in stretch, thus stressing the bubble coating. The basic film carrier that has been used is the Ecusta mechanically perforated tipping paper or plug wrap used in standard air diluted cigaret filters. In addition, inherently porous tissue papers have been investigated as this type of paper has many more and smaller holes compared to the plug wrap. A paper of this type has a potential of more uniform air dilution. . Filter Configuration Several types of filter configurations were initially investigated, such as CA covered by a coated plug wrap. Most of the films, however, have been investigated in a plug-space-plug configuration. The only requirement on filter configuration is that the smoke constituents must come in contact with the film. The one that affords the more intimate and longer length of contact time is probably most desirable. CD

Page 4 Mrs. Thelma C. Heatwole July 7, 1967 Summary I feel we have demonstrated invention by causing films to degrade via water in the smoke stream. Other smoke constituents may aid in degrada- tion but are unknown. Reproducible demonstrations have been made only at last puffs from 15-20mm before the film. Although the effect of "hot water" cannot be ruled out as aiding degradation, I feel we have shown that tempera- ture alone is not responsible as films of high melting point (i.e., starches) have opened. Another argument that can be made for films being affected by smoke constituents is our early non-reproducible success at early puffs and also more recent demonstrations of films with initial dilution closing starting at early puffs. This latter effect is probably due to film swelling caused by water. If the examples I have noted and arguments presented are not sufficient, I feel we can design experiments to produce more definitive data to further substantiate effects on water soluble films of smoke stream constituents (water), especially by comparing them directly to non- soluble materials of approximately the same melting point. In addition, the original disclosure should be updated to include bubble coated, reactive and stressed films along with all possible filter configurations and carriers, such as porous tissue type papers. /cb cc: R. B. Seligman R. G. N. E. Thomson Inskeep Attachments

DATA SHEI;T #1 Mono Films Material Configuration -plug-space-plug PVA - polyvinyl alcohol supplier - Gohsenol - Osaka, Japan 6% GM-14 (PVA - 150t softens to heat seal (plug wrap removed) 5mm 65mm ref. Elvanol Polyvinyl alcohol - DuPont Co. A 47499-2N Development Notebook #3620, page 17 mm Puff No. RTD % Dilu tion Initial 5.1 3 1 6.2 3 2 6.2 3 3 6.2 3 4 6.2 3 5 6.2 3 6 6.0 3 7 6.0 3 8 5.0 3 9 5.0 3 10 5.0 20 Definition of last puffs: 90mm I 6 5mm ~ ---~ I~---- 2 Omm --4 < I 5mm1 61mm Last puff - begins approx. 6mm from tipping paper ends approx. lmm from tipping paper Next to last puff - begins approx. llmm from tipping paper ends approx. 6mm from tipping paper

DATA SHEET #2 Films with Filler Material 20% polybond*(Polymer Industries Inc.) 10% polycryl (Polymer Industries Inc.) (*Polybond - starch ether Amylose - decomposes approx. 150°C ref. A.E. Staley Mfg. Co. Market Development Div. Bulletin No. 101) Configuration - plug-space-plug paper - tipping, 6 line CA tow, 4.0/49,000 I Development Notebook #3620, page 77 65mm film in holes-- Puff No. RTD % Dilution Initial 4.5 0 1 5.5 6 2 5.5 5 3 5.5 6 4 5.5 6 5 5.0 7 6 - 7 7 5.5 7 8 4.8 7 9 5.0 11+ 10 - 23

DATA SHEET #3 Films with Filler Patent Example Material 400 mis H20 16 gins GM 14L (PVA) 60 gms Alum. 320 abrasive Configuration - plug-space-plug 65mm 5mm r~ 7mm r e ! oc kLiT Film 3595-69-1 Development Notebook #3595, page 69 '1 page 82 Puff No. % Dilution Ini.tial 7.6 3 1 8,8 3 2 9.2 3 3 9.4 4 4 8.7 4 5 8.8 4 6 8.6 3 7 8.1 3 8 7.4 3 9 8.3 7 10 7.4 30

DATA SHEET #4 Bubble Coated Aqueous P-55 pl, Material Radel*5 gms (Union Carbide) H20 100 gms Kerosene 100 gms (*Radel - 65-75°C softening point Configuration coated plug wrap paper TOD 2496 - 450D Development Notebook #3858, page 24 ref. Union Carbide Chemicals F-40246-C) Puff No; RTD % Dilution Initial 3.4 26 1 4.1 30 2 4.1 30 3 . 4.2 30 4 4.0 28 5 4.0 30 -6 4.4 28 7 4.1 26 8 4.4 26 9 3.7 28 10 2.0 64 11 2.0 66

DATA SHEET #5 Reactive Films Material 12.5% Polybond 50% reactive 37.5 g Polybond (dried from H20 (sample film infrared dried) Configuration - plug-space-plug paper - 13 line tipping 5mm ~ 65mm ~ 7mm ~ °-7;- {holes filled with fi m) solution 43.4 (dried film) 18 75 g citric acid 21 7 . . 30.00 g NaTHCO3 . 56.4 213.75 g Dmf Development Notebook #3748, page 31 11 it if n 91 Puff Not. .~. RTD % Dilution Initial 4.5 24 1 5.0 24.5 2 5.0 27 3 5.0 27 4 5.0 26 5 5.0 26 6 5.0 26 7 5.0 26 8 5.0 25 9 5.0 25 10 5.0 40 11 5.0 55 13mm

DATA SHEET #6 Reactive Film - Radel Material Ethylene dichloride 400 gms Citric acid 40 gms Sodium bicarbonate 64 gms Radel 40 gms "varsol 120 Sms Film processed through Mantor (Film E) Bubble Coated Configuration - space-plug 9 line tipping paper paper tube mm -=W 65mm 4, 20mm film in holes smalPCA Gaulin homogenizer filter Development Notebook #3748, page 77 Puff No. RTD % Dilution Initial 3.4 0 1 4.0 0 2 4.0 1 3 4.0 1 4 4.0 1 5 4.0 1 6 4.0 1 7 4.0 1 8 4.0 1 9 4.0 15 10 4.0 32