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Accession number 2050 Lorillard Research Center Greensboro The Spray Addition of Menthol Onto a Newport Tobacco Blend Using a Propylene Glycol Carrier - Production Test 1 Submitted by: W.E. Crouse Report number: B-439/84-1 Date: 4/6/84 Summary or Abstract: Previous pilot plant studies had indicated that menthol could be successfully applied onto a Newport tobacco blend using a reduced quantity of propylene glycol relative to the ethyl alcohol carrier. The work was continued by the preparation of an experimental Newport sample in the Greensboro menthol spray room in cooperation with the Industrial Engineering and Product Development groups. The theoretical menthol concentration of the experimental sample was reduced to a level of 0.28 percent so as to compensate for the enhanced menthol amplitude imparted by the propylene glycol carrier. A control production sample was prepared at a 0.35 percent menthol level. Eighty-five millimeter filtered cigarettes were made, packed and organoleptically evaluated. The process and organoleptic results in addition to specific recommendations are discussed. 2 /Jw Co W : Xc: J.H. Bell M.W. Connelly B.J. M.F. Pember Reich w V O A.B. Hudson J.H. Smith O T.D. Jessup A. Sallez 00 S.B. McGee H.J. Minnemeyer F.J. C.L. Schultz Tucker N S9. Barnes Library D. E. Fernald

Table 4 Organoleptic Evaluation of Control and Experimental Newport Cigarettes Sample No. Description % Menthol Impact Taste Amp. 0. Acc. M. Amplitude 1036 Control 0.344 10.0 10.0 10.0 10.0 1037 PG-Sample 0.259 10.5 10.5 9.8 10.7

Table 3 Menthol Analyses of Menthol-Propylene Glycol Samples Cut Tobacco Tub # Sample #1 (%) Sample #2 M Avg. (%) 5 0.276 0.261 0.268 6 0.262 0.266 0.264 7 0.274 0.267 0.270 8 0.237 0.232 0.234 Cartons Code # Sample #1 M Sample #2 (%) Avg. ($) 1036 (Control 0.341 0.347 0.344 1037 (Experimental) .0.256 0.262 0.259

Reference 1. W.E. Crouse, "The Spray Addition of Menthol Onto a Newport Tobacco Blend Using Propylene Glycol and a Propylene Glycol Water Carrier System-II", Lorillard Research Report 7, Accession Number 1991, September 29, 1983.

2 Organoleptic Evaluation The results of the organoleptic evaluations are presented in Table 4. The data indicated that the propylene glycol applied sample at a reduced leaf menthol concentration of 0.259 percent exhibited significantly greater menthol amplitude than the control sample at a 0.344 percent menthol content: A puff-by- puff profile (Figure 1) for both samples did not indicate an increase in menthol delivery that could be attributed to the propylene glycol carrier. The overall delivery rate of the propylene glycol applied sample was virtually identical to the control run. Presently, headspace and other studies are being conducted in order to determine the effect of the solvent carriers on menthol volatility. An assessment of the data by Mr. Howard Smith revealed that the taste properties of the control and experimental cigarettes are identical with exception of the menthol amplitude value. It was suggested that the leaf menthol content be further reduced in order to bring the menthol amplitude in line with the production control. Summary / Recommendations The in-plant spray addition of a reduced volume of propylene glycol containing a reduced concentration of menthol onto a continuous flow of Newport blend was achieved at the desired target concentration. Filtered 85 mm cigarettes were made, packed and organoleptically evaluated by Product Development. The results indicated the experimental cigarettes exhibited significantly greater menthol amplitude even though the leaf menthol concentration was twenty-five percent lower than production control cigarettes. A puff-by-puff profile of each sample did not reveal the propylene glycol carrier to accentuate mainstream delivery of smoke menthol. To date, the mechanism of enhanced menthol amplitude remains unknown. If leaf menthol concentrations could be reduced from 0.35 percent to 0.23 percent without compromising menthol or taste amplitude, an annual savings of $170,000 could be realized on the Newport proper line alone. The cost estimates are presented in Table 5 and may be somewhat conservative since the price of natural menthol has been escalating due to the Chinese situation and the unavailability of synthetic menthol. Another one time $250,000 savings could be realized by not explosion proofing the Greensboro spray system. If our remaining menthol lines are included, the net annual savings could probably exceed $250,000. It is recommended that a meeting be scheduled with Industrial Engineering and Product Development so as to discuss these current findings. An additional set of pilot plant experiments should be planned in order to "bracket" the menthol levels. Once an organoleptically acceptable lower menthol limit has been obtained, a continuous manufacturing run should be made and the product organoleptically evaluated versus a production control.

Table 2 Experimental Menthol Carrier Formulation For Plant Run of Newport Tobacco For 6000 Pound Lot of Blend Theoretical: 0.28% Menthol Propylene Glycol: 3.4 gallons Menthol: 16.8 lbs. menthol x 453.6 grams = 7620.5 grams lb. Density of Menthol: 0.890 7620.5 g 0.890 g/mL g/tal x 1000 mL/liter = 8.56 liters menthol 3.785 liters 8.56 liters gallon 3.78 liters/gallon = 2.23 gallons menthol Propylene Glycol 3.4 gallons x 3.785 liters/gallon = 12.87 liters 12,870 mL x 1.036 g/mL _ 29.39 lbs. propylene glycol 453.6 g/lb. = Total Theoretical Spray Volume = 2.23 gallons menthol + 3.40 gallons propylene glycol = 5.63 gallons/6000 lb. blend Specific Gravity Results: Theoretical: 2.95 lbs. menthol/gallon solution (for 0.28% Found : 2.88 lbs. menthol/gallon solution application rate)

11/30/83 SBM - KRC PROPYLENE GLYCOL AS MENTHOL CARRIER TENTATIVE PLAN Prepare 10-12 gals.~of test solution per R&D Specs. Use high shear mixer if necessary. Check test solution for menthol content and specific gravity. Determine pump settings for test solution. Re-check test solution for menthol content and specific gravity. Prepare new test solution and check menthol content and specific gravity if necessary. Re-check pump rate at calibrated setting for test solution. Sample test (n = 10) before process for % P. Glycol. Spray NEWPORT blend using test solution at .28% menthol target: 30-minute run (approx. 3,000 lbs. blend). Record lbs./# containers of blend dumped. Record run time and all system settings. Record amount test solution sprayed. Sample (n = 20) off process for % menthol. Sample test (n = 20) after approx. 1 day for % menthol. Sample test (n = 10) after approx. 1 day for % P. G. & H20. Make/pack 85 mm& 100 mm test NEWPORT for evaluation. Sample test (n = 20) after approx. 5 days for % menthol. Sample test (n = 20) after approx. 15 days for % menthol. Spray NEWPORT blend using alcohol control solution at .35% menthol target: Regular production run. Record all system settings. Record amount solution sprayed. Sample control (n = 20) after approx. 1 day for % menthol. Sample control (n = 10) after approx. 1 day for % P. G. & H20. Make/pack 85 mm & 100 mm control NEWPORT for evaluation.

Table 5 Calculations of Potential Cost Savings Based Upon 1984 Cost Figures* 1984 Projection for Menthol Usage: (Total) 185,000 lbs. x $15.50/lb. = $2,867,500 Assume.a 50/50 mix with synthetic menthol: (a)$ 9.00/lb. Avg: $12.00/lbs. Newport Line: 11,829,000 lbs. blend x 0.35 percent menthol = 41,404.5 lbs. menthol Proper (b) 41,405 lbs. x $12.00/lb. = $496,818.00 Assume a leaf menthol reduction to 0.23% menthol using propylene glycol carrier: 11,829,000 lbs. x 0.23% menthol level = 27',207 lbs. menthol 27,207 lbs. x $12.00/lb. = $326,484 Net Savings $496,818.00 - at 0.35% application level - 326,484.00 - at 0.23% application level $170,334.00 (a) Presently unavailable * As supplied by E.W. O'Neill and L.B. Tanner (b) Does not include Newport Lights

Introduction In the previous report, a reduced, cost effective volume of propylene glycol was successful as a menthol carrier for a Newport blend (1). Organoleptic evaluations indicated the system to be superior to the ethanol applied control sample. The perceived menthol amplitude enhancement of the propylene glycol applied cigarettes was conjectured to be a result of increased leaf penetration by the menthol. A puff-by-puff menthol profile indicated that propylene glycol enhanced menthol delivery by approximately ten percent. Based upon these data, the next phase of the project was to spray a large batch of tobacco blend with the experimental carrier system on a continuous basis. A joint meeting was held with selected individuals from the Industrial Engineering, Product Development and Research staff. It was decided that a three thousand pound batch of Newport blend would be treated in the Greensboro facility with the experimental carrier system at a target menthol concentration of 0.28 percent. It was hoped that a reduction in the menthol concentration of the experimental sample would yield a menthol amplitude comparable to that imparted by an 0.35 percent menthol control sample. Once the Newport blend had been sprayed, Product Development would be responsible for making, packing and organoleptically evaluating the product. Sample Preparation A tentative plan for treating the samples was developed by Sam McGee and Kenny R. Carper of the Industrial Engineering group. The scheme is listed in Table 1. The propylene glycol-menthol solution was prepared by the author in the pilot plant as per Table 2 and was submitted to Quality Assurance for specific gravity and menthol analyses prior to use. The data indicated the solution met specifications for a 0.28 percent menthol application rate onto the blend. The solution was stored in a stainless steel container and forwarded to Mr. Kenny Carper. The solution was used to calibrate the pumps and determine flow rates in the spray system. All specific inquiries regarding pump flow rates, calibration settings and application details should be forwarded to S.B. McGee and K.R. Carper of the Industrial Engineering department. Representative samples of treated cut tobacco for experimental and control runs were forwarded to Quality Assurance for menthol analyses. The menthol analyses of cut tobacco and packaged cigarettes are given in Table 3. Based upon the data, it is quite apparent that the target values were obtained. This confirmed the assumption that menthol can be successfully applied with a significantly reduced volume of carrier. Selected saratoga bins of tobacco were used to make the experimental cigarettes. Newport blend was sprayed with a production ethanolic menthol solution at a menthol concentration of 0.35 percent in order to prepare control cigarettes. After making and packing, the sample cigarettes were aged for approxi- mately four weeks in the Research Center's conditioning room prior to organoleptic evaluation.

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