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Accession No. 81-192 Copy No. Issued To: PHILIP MORRIS U.S.A. Research Center I: r i: A; I ~ L I l This report contains information which is CONFIDENTIAL to the business of the Company. The information must be carefully handled and not divulged to outside sources without express authorization. This report is signed out to you! individually. It is not transferable and must not be reproduced. Please return it to the Research Center Records Facility when it is not longer useful. CONFIDENTIAL MONTHLY PROGRESS REPORTS Period Covered July 1 - 31, 1981 Date Issued: August 15, 1981

DISTRIBUTION El E C c [ U c Dr. R. Seligman Mr. F. Resnik Mr. T. Goodale/Mr. W'. McDowell Dr. M. Hausermann. Dr. W. Farone Dr. W. Gannon Mr. L. Meyer Dr. T. Osdene Mr. R. Thomson Mr. P. Eichorn Dr. D. Lowitz Dr. M. Bourlas Mr. K. Burns Mr. H. Daniel Mr. F. Daylor Mr. P. Gauvin Dr. A. Kassman Mr. B. Kosakowski' Mr. W. Kuhn Mr. W. Mutter Mr. J. Osmalov Dr. E. Sanders Mr. F. Watson Dr. J. Whi dby Mr. J. Wickham Dr. W. Dunn Dr. R. Fagan Dr. R. Ikeda Mr. R. Carpenter Mr. W. Claflin Mr. 0. Clark Mr. R. Jenkins Mr. A. Kallianos Mr. A. Lilly Dr. A. Manzelli Mr. H. Merritt Mr. R. Bass Mr. R. Comes Dr. M. Counts Mr. R. E. Davis Dr. R. Dwyer Dr. W. Edwards Dr. R. Ferguson Dr. W. Geiszler Mr. G. Gellatly Ms. B. Goodman Mr. H. Grubbs Mr. W. Harvey Mr. W. Houck Dr. Y. Houminer Mr. G. iCeritsis Dr. R. Kornfeld Mr. C. Kounnas Mr. H. Lanzillotti Mr. B. LaRoy Dr. C. Levy Dr. B. Losee Dr. V. Malik Dr. Peter Martin Ms. L. McCray Mr. W. Nichols Dr. R. Pages Mr. A. Robinson Mr. M. Rosenberg Dr. J. Seeman Mr. J. Sherwood Mr. H. Spielberg Mr. J. Swain. Mr. R. Tamol Dr. D. Teng Ms. P. Thomas Mr. R. Uhl- Mr. F. Utsch Mr. D. Watson Mr. R. Heretick Mr. A. Pasquine Mr. T. Newman Mr. Art Palmer Ms. S. Hutcheson Dr. L. Sykes Dr. T. Laszlo Dr. H. Gaisch Dr. A. Wol f Central File (2)

CHARGE NUMBER: Various DATE: August 12, 1981 PROGRAM TITLE: Analytical Research WRITTEN BY: G. Vilcins, G. H. Bokelman, R. H. Cox, R. E. Davis, W. R. Harvey, J. 0. Lephardt and D. C. Watson r 1'. E C I :. C L Ii I. TOBACCO ANALYSIS A. The f easibility of an N02 process monitor has been demonstrated by pumping a sample of SEL and using an on-line dilution rather than filtration prior to analysis by the AutoAnalyzer. Steady state is obtained in about 1.5 minutes and holds for the same sample for at least 2 hours. The procedure is linear from 50 to 2.50 ppm nitrite nitrogen and recovery of nitrite added to SEL is quantitative. The next logical step would be to position this monitor by a large fermentor in the Pilot Plant to detect changes in N02 concentration. B. Two separate precision studies for the enzymatic starch determination procedure were performed using f ield-grown, green Coker 319 bright tobacco obtained from the V.P.I. & S.U. agricultural experiment station in Blackstone, Virginia. The following conclusions have emexged from these studies: 1) Starch can be determined on green tobacco samples in the fresh, freeze-dried or oven-dried forms with similar results. 2) Green tobacco must be prepared quickly after harvesting for determination of starch (in whatever form) since even storage at 50C for 2 days results in the loss of >50% of the initial starch content. C. Data collection was initiated on a series of samples subjected to WET expansion before and after cylinder treatment and before and after high moisture bulking. The objective of' this study is to attempt to differentiate puffing effects from stiffening effects during expansion. II. SMORE ANALYSIS The apparatus for making puff-by-puff tar by fluorescence determination was improved by installation of a new trap and circulation pump which was set at two speeds. This resulted in a more accurate control of puff volume and a faster equilibrium after the puff. Carry-over was reduced to indetectability. III. EVOLVED GAS ANALYSIS A. The original N02/N03 cellulose study has been expanded to include a comparison of both sodium and potassium salts. Samples of cellulose were prepared with the following salt additions: 2% KC1, 2% RN02, 2% KN03i 4% (27 KNO3 + 2% NaN03). These will be examined in addition to the original NaNO2 & NaN03 treated samples. Analyses are now in progress.

Analytical Research 2 August 12, 1981 B. A study was initiated to examine the facility of a sweep procedure using a nitrogen carrier containing water and ammonia to sweep nicotine from tobacco with minimal secondary alterations. If successful, the approach may enable selective removal of labeled nicotine from labeled plants grown in the greenhouse, while leaving the remaining tobacco little altered'and usable for other purposes. IV. FLAVOR ANALYSIS To insure column stability for analyses being developed for the new Flavor Center lab, approximately 100 compounds were chromatographed on a bonded SE-54 capillary column. This column is intended to replace the CW-20M column which, although the column of choice, has had problems in production and is often not available. The bonded SE-54 column should show a high degree.of stability and therefore be an ideal type for use in a QA environment. V. CHEMOMETRICS Data from 31 peaks in the gas phase prof iles of cigarettes of cased and uncased versions of 100% bright, burley, oriental, and of 2 blends were subjected to Factor Analysis routines. Excellent tobacco type groupings and indications of differentiating cased versus uncased versions were observed on plotting the various factors against each other. The data validity were conf irmed upon subjecting a second set of 30 of the gc peaks to Factor Analysis. Although the grouping positions were different, these data also gave good sample type discrimination. VI. NMR J. Wooten and R.- Cox visited Bruker Scientific and Nicolet Magnetics for demonstrations of their 360 MHz NMR spectrometers. As a part of these demonstrations, 'H"spectra were obtained on the seven, pyrrolidine-ring methyl substituted nicotines and some fluorine substituted ethyl analogs of nicotine. These spectra are presently being analyzed for chemical shifts and coupling constants which will be used to establish the influence of substitutions on the conformation of the pyrrolidine ring. This information will be used in structure- activity correlations of nicotine derivatives. Work is continuing on the determination of barriers to rotation of nicotine derivatives and the structure determination of labdane derivatives. Enantiomeric purity of several nicotines was determined using chiral shift reagents.

CHARGE NUMBER: 0108 PROGRAM TITLE: Mechanism for Smoke Formation PERIOD COVERED: July 1-31, 1981 PROJECT LEADER: R. A. Kornfeld DATE OF REPORT: August 10, 1981 Vi r. r. Research has begun into the transfer of tetramethylpyrazine (TMP) from filler to filter in unsmoked cigarettes. Sets of filtered cigarette~ containing 100, 300, and 500 ppm TMP were stored at room temperature, -25 C, and -85°C. While only preliminary results are available, there are indications that transfer of TMP is occurring rapidly at room temperature. Essentially no transfer occurs at the two lower temperatures. These studies will be completed this month. The transfer of TMP to filters during smoking will also be investigated'.''2 GC/MS analyses of several alkylated nicotines confirmed their structural assignments. Samples included 2-methyl~, 4-methyl, 4,6-d~imethyl, 6-ethyl, and 6-isopropyl nicotine derivatives. Additionally,products from the following reaction were determined via GC/MS: t-bu00H FeSOa H2SOa CH3CHO r. The major compound in the reaction mixture was unreacted nicotine. Minor amounts of 6-methyinicotine, 4-methylnicotine, and 6-acetylnicotine (the expected product) were also found.2'3 Problems with chromatographic reproducibility have hampered the quantitation of the major peaks in the pyrolysis of 7564-115 cooked flavor's non-dialyzable portion. Chromatographic modifications are being made to improve both retention time and quantitative reproducibility.3s'' References: 1. L. Brown 2. C. Connolly 3. J. Naworal 4. J, Kang f-c ~;~.Z ~ .;t ~ IG

CHARGE NUMBER: 0307 PROJECT TITLE: Cigarette and Tobacco Measurement Methods PROJECT LEADER: C. L. Irving PERDOD COVERED: July, 1981 DATE OF REPORT: August 7, 1981 1. Moisture Measurement Data analysis was completed on sampl,es of Marlboro tobacco with and without menthol and Merit tobacco with and without WS. All four samples were tested in the L-Band automatic microwave moisture meter at seven moisture levels and five weight levels. The analysis showed that different equations are required for predicting OV for Marlboro with and without menthol. In addition, separate equations are also required to predict GC water content for Marlboro with and without menthol. The analysis of the Merit data showed that a single equation can be used to predict OV for Merit with and without WS and that one equation can be used to predict GC water for Merit with and without WS. In all cases except for Merit with WS the variation of the microwave test was found to be greater than the variation of the standard OV test. A comparison of values calculated with this data and the equation developed in October, 1980, showed an average difference of 0.27% OV. This is in good agreement with the resulits shown by the Marlboro monitor. The comparison also showedthat the sensitivity of the microwave instrument has not changed and that only an intercept shift has occurred. As previous experiments have shown, statistical analysis of this data confirmed that Marlboro and Merit filler could be combined for prediction of OV or GC water. An experiment was completed to determine the possibility of using the automatic microwave moisture meter to predict OV for Burley tobacco with 0TM at high OV levels. Analysis of this data is under way. An experiment is also in progress to determine the effect of PG and glycerin on, microwave attenuation. II. Measurements Development Further testing of the RoTap sieve tester and analysis of the data showed that the unit does separate tobacco particles by size but not con- sistently enough to be useful. For example, using data from five runs of Marlboro tobacco to develop a particle size prediction equation showed that at a 95% confidence level only the 6 and 20 mesh screens could be shown different from one another out of a stack of 6, 8, 10, 14, 20 and 28 mesh screens. (The particle length on a 6 mesh screen was approximately 40 mm and on 20 mesh approximately 8 mm.) Testing also showed the Zeiss video- plan and Hamamatsu image analyser to work well and to be very reproducible compared to the sample to sample variation of the tobacco. Analysis of data

C. L. Irving Mo. Progress Rpt. (July, 1981) Pa ge 2 August 7, 1981 r I I f. f, C from these experiments also showed that the average particle length on a given screen is much too long to have passed the screen above, probably due to tipping of the tobacco particle. Testing is now in progress with tobacco conditioned to very high moistures in an effort to make the particles pliable enough to prevent tipping. A PM sieve tester is expected to be received by August 15 so that a similar analysis of particle size separation consistency can be made. A set of perforated plates are being ordered for the Kason sieve tester that is due to arrive by September 30. Tobacco friability is currently being evaluated using a ball mill with both high and low density ba1J s and various sample loadings and running times. Standard sieve analysis of the tobacco generated from the ball mill testing is under way. Analysis of this data is expected to provide information about the amount of energy required to degrade tobacco to the desired level. Several ideas for designs of friability testers are also being evaluated. III. Cigarette Circumference The electronics that go with the dynamic circumference gauge were modified to allow zero output at target circumference and a direct readout of deviation from target circumference. The first test since the modifications resulted in accuracy of ± 0.10 mm circumference at a 95% confidence level, but the deviation shown by the meter was approximately 19% low. Additional testing is planned after a gain adjustment is made. L

CHARGE NUMBER: 1005 PROJECT TITLE: Improved' Semiworks Operations PROJECT LEADER: J. F. Sherwood PERIOD COVERED: July, 1981 DATE OF REPORT: August 11, 1981 I. Primary Processing A. Addition of Lamina Scrap to Filler At the request of the Tobacco Utilization group, a test was run to determine the effects on blend characteristics of adding bright (BTBL) and burley (BUBL) lamina scraps from the Stemmery to cut filler. This technique would allow Stemmery by-products.to be directly used in blends instead of being converted'into a sheet product. The following three sizes of BTBL and'BUBL were used: - 5 mesh + 16 mesh, - 6 mesh + 16 mesh,, and - 8 mesh + 16 mesh. The different sizes of BTBL and BUBL were evaluated in Marlboro blends at twice the total utilization levels of bright and burley scrap, 1.1 and 1.3% in the total blend, respectively. The results showed no significant differences in CV between the three blends containing the lamina scrap and a control Marlboro blend to which no scrap was added. Sieve data showed the blend containing the 5 mesh scrap to average 5-8% higher in longs than the control and the two test blends containing the 6 and 8 mesh scrap. Visual inspection of the longs fractions of the blend's showed the 5 mesh blend to contain distinctly larger pieces of lamina than the control or the other two test blends. Smoking analyses on cigarettes made from these blends showed no significant differences among the different cigarettes. It was therefore recommended that a limited run be made in Manufacturing to confirm these results. B. The Effect of Lamina Size on Filler Size Another test was run at the request of the Tobacco Utilization group to determine the effect of lamina size on final filler size. In this ex- periment, five different sizes of bright strip (over 2" x 2", over 1" x 1", over 3/4° x 3/4", over 31" x;j", and over h° x 4") were obtained from the Stemmery and added to Marlboro strip blends at a 50% level. Sieve analyses of the cut filler samples showed that the addition of the largest two strip sizes to the Marlboro strip blend resulted in a slight increase of 1-3% in filler longs over a control Marlboro blend. Addition of the three smallest strip sizes to the Marlboro blend caused the % longs level to decrease. Thus, only strip remaining on a 1" x I"'or larger screen appears to increase filler % longs. C. WS Application In support of the Northwind test market production run, cleanup procedures were provided to the production personnel at the 20th Street facility. Swab samples taken from equipment and surrounding areas at 20th

J. F. Sherwood Mo. Progress'Rpt. (July, 1981) Page 2 August 11, 1981 Street after the test market run showed the cleanup procedures to be effective and'indicated no contamination problems with the WS. II. New Semiworks Startup and debugging of the Primary Pilot P1'ant equi!pment in the new R&D Semiworks was initiated, with checkout of the electrical and instrument systems in the control room being nearly complete. After the control room is operational, checkout of the process equipment and field instrumentation will begin. Processing of blends is expected to begin i'~n October. Installation of the flooring in the Make/Pack area is in progress and is scheduled for completion in the next two weeks. Delivery of rebuilt equipment from the York facility will then begin. ~ J. F. Sherwood JFS/jn