IMPERIAL TOBACCO PRODULTS DIVISION Of tMASCO LIMITED OUARTERLY RESEARCH REPORT OF RESEARCH DEPARTMENT Orroher 1)"embpr, 1970 ent OCT I.. 11.0%. r'1971 ................ '7i A ..-tj le job BATCo document for Province of British Columbia 12 April 1999 PA- R. It D. E. LIBRARY B.A,T. CO. LTD. SOUTHAMPTON ry oft % C-C2 L@L Issue I Date received:-a=@::@, Reader Page Initials Date CRJ TIJT TIMURY TO: R 6. 7- -71 Oil, jo ip Z::b BATCo document for Province of British Columbia 12 April 1999 R. & D. B. LIBRARY B.A.T. CO. LTD. S2U "PTON Journal: -T Pi-.*ALrV S Issue: Date reCeiV9Q;.-=-,-1 tL--c. 7c Reader i Page Initials Date PI ET 4-- -.fall 16 2h. %D BATCo document for Province of British Columbia 12 April 1999 R. & D. E. LIBRARY B.A.T. CO. LTD. SOUTHAMPTON Jt%vual: -T P r. A X a 3 C'm Issue: CL Ij 54 A V IC 9t RF- PC, r Date received: 19 -7a Reader Page Initials Date -Lea.-- . ............................... 74 1-T 7VM 14-7-71 SIL @-21 -IL,, 71 7- 7) VI-7 IL - C) NJ N) Xb- BATCo document for Province of British Columbia 12 April 1999 COPY NO. IMPERIAL TOBACCO PRODUCTS DIVISION OF IMASCO LIMITED RESEARCH LABORATORY IPa- Aest;r-.h & MONTREAL wl-@- I 0 M A-Y 1 9 7 I . ...........................-k QUARTERLY RESEARCH REPORT OF RESEARCH DEPARTMENT October - December, 1970 ......... Edited By: Dr. T. A. Smith Issued by: Dr. T. A. Smith Date Issued: February 22, 1971 DISTRIBUTION Copy No. 1 Library 19 Dr. F. Haslam 2 Library 20 Dr. F. Raslam 3 Mr. KIM. Cibb 21 Dr. I.W. Hughes 4 Mr. C. Warren 22 Dr. R. A. Sanford 5 Mr. L.A. Ricard 23 Dr. R. A. Sanford 6 Mr. R. S. Wade 24 Manager, R & D.D., Australia 7 Dr. T.A. Smith 25 Manager, R & D.D., Australia 8 Mr. S.M. Candlish 26 Dr. M. H. Billmoria 9 Mr. D.E. Schroeder 27 Mr. E. R. Freiesleben 10 Mr. R. L. Rice 28 Mrs. J. Johnson 11 Dr. M.A. Nisbet 29 Mr. R.S. Perrier 12 Dr. G. W. Boswall 30 Kr. M.P. Scherbak 13 Dr. S.J. Green 31 Mr. A. F. El Naggar t4 Dr. S.J. Croon 32 Mrs. M.T. Schiff 15 Dr. S.J. Green 33 Miss R. R. Smith 16 Dr. S.J. Green 34 Mr. B.J. Stirling 17 Dr. S.J. Croon 35 Mr. W.A. Gray IS Dr. D. G. Felton 36 Manufacturing Dept. 37 Engineering Dept. "N. @Jn BATCo document for Province of British Columbia 12 April 1999 T 6126 Determination of Tar Producing Properties of Tobacco in Granular Form Objective: To develop methodology that will permit the evaluation of yields of tar. nicotine and other products of combustion using very small tobacco samples, of potentially great value in many work areas. To show that tar yields from granulated tobacco can be used to predict deliveries from tobacco In cut form, studies are being made of: (1) the effect of method of sample preparation on particle size and size distribution. (2) the effect of particle size and size distribution on tar yields. (3) the relation between tar yields from cut and granular forms. The granular tobacco is supported in a cigarette tube by a small filter plug.- and in smoked in a vertical position. In preparation of the 'cigarette' containing granulated tobacco. the selected particle size must not give such a high pressure drop that the tar yield in too low to be measured. The particle size giving favourable pressure drop characteristics must also be representative of the total sample. Tobacco strips were equilibrated at two RH conditions. namely 60% and about 40% RH. They were ground in a Wiley mill through e'-t-; a 3mm screen, and separated into three sieve fractions: 12 on 20, 20 on 40 and 40 an 60 mash. The effect of particle size k1j on pressure drop-length relationships was determined using the tobacco ground at 60% RH. The 40 an 60 mash fraction gave an unacceptable pressure drop, but those of 12 on 20, 20 an 40 and 12 on 40 were suitable. The following table illustrates the findings for flue-cured grade CFL. Pressure Drop (in. W.G. ) at Different Lengths for Flue-cured Grade CYL Fraction 30 = 1 60 mm 90 M 12 on 20 mash 1.5 3.0 4.4 12 on 40 2.7 5.5 8.0 20 on 40 3.4 6.7 10.1 40 on 60 8.0 15.5 - Xlb. C) PO 11@1- %O BATCo document for Province of British Columbia 12 April 1999 2 The combined fraction, 12 on 40 mash, is the most attractive since, in addition to having acceptable pressure drop characteristics, it represents 66 to $22 of the initial weight of the tobacco after grinding at 6OZ RH. for a number of flue-cured grades representative of the different portions of the plant. Comparison of the Z retained an 40 mesh for samples ground at the two RH conditions is shown below: X of Particle Size Graator then 40 Mesh Grade Ground at Ground at about 40% RH 60% RH R 65.2 81.3 FS-2 63.1 65.9 CFL 62.2 71.9 A,F-2 68.7 82.3 G-2 65.6 79.8 D-2 60.5 74.2 M 62.7 82.3 BF-2 65.8 81.3 Coefficients of filtration, impedance and retention have been calculated using the Fordyce method for 12 on 20 and 12 on 40 mesh fractions and for cut tobacco, and the results are currently being analyzed. (RSP. RLR). T 6351 Comparison of TPM Yields from Old Port Cigarillas Obi active: To determine the reasons for the very large differences observed in puff numbers and tar yields between Old Port tipped and plain and eigarillos. By sucking cigars with and without the wrapper, as was described in the previous quarterly report, the Ultra A wrapper was shown to be responsible for increasing the tar yield of the cigar two fold over the basic tar yield of the cigar without the wrapper. During the past quarter, additional work has beta carried out to confirm the above findings and to determine the effects of other parameters on tar yields. This work has NJ BATCo document for Province of British Columbia 12 April 1999 3 been discontinued as It would appear that the tar yields of the ci&arillos vary very appreciably from sample to sample. Consideration is being given to the design of a sampling scheme that will give a reliable estimate of the variability in tar yields of 0. P. cigarillos and the reasons for this variability, I.e., wrapper, binder, filler. etc. Comparison of data originating from Montreal and from Lancaster, ?&., indicate a much lower car yield from the U. S. product. A collaborative experiment has been set up between Lancaster and 4ontreal to determine if the differences are real, and if so, to determine the cause. The collaboration also provides an opportunity to compare the methodology of the two laboratories. (R. L. R.) T 6530 Evaluation of PCL Produced from Different Tobaccos Objective: To find the effects of tobacco reconstitution principally on the subjective properties, but also an the biological activity (by the hyperplasia test) and chemical composition of the smoke. Two leaf grades in both leaf and sheet form were compared. The AJ100 process was employed for making the sheets so that the comparison between leaf and sheet would not be complicated by chemical differences. A. Flue cured grade D C. Flue cured grade D CRS, 3:1 ratio, VS, 3:1 ratio, cased with glycerol processed into PCL at a level equivalent by the Ailoo process. to that In C & D. B. Flue cured grade R D. Flue cured grade R CRS, 3:1 ratio, VS, 3:1 ratio, cased with glycerol processed into PCL at a level equivalent by the AJ100 process. to C & D. The smoke chemistry of these samples was described in the previous quarterly, and the results of the hyperplasia tests and subjective comparisons are al-rized below. The test materials at a 10OZ level in plain and cigarettes, were used in the h"erplasia tests. The results indicate that the AJ100 process does not reduce the specific biological activity of the condensate as judged by the hyperplasia test. However, the condensate from samples A and C has a lower activity than NJ that from B and D. C;O BATCo document for Province of BritiSh Columbia 12 April 1999 4 Filter tipped cigarettes were used in the subjective evaluation, employing the test materials at a 50% level. Comparison of A to C and of 5 to D suggested that the AJ process may increase the irritation of the smoke. However, this result can be considered to be inconclusive as no differences in irritation were perceived in comparisons between A and 3 and between B and C. This project is of considerable importance in relation to future work an sheet. It is recommended that new samples be manufactured and that the subjective tests be repeated. MR) T 6533 A Comparison of Reconstituted Tobaccos Made by Five Processes Objective: To compare sheet and smoke properties. smoke composition and subjective smoking characteristics of reconstituted tobaccos made by different processes, as a basis for future sheet work. Reconstituted tobaccos were made from common starting materials, by the following five processes; (a) Regular PCL process (b) Schweitzer paper process (c) Rapaport (Gerlach) process (d) AJ100 process (e) MK II (Brown & Williamson) process The sample of paper reconstituted tobacco sade for us by Peter J. Schweitzer (U.S.) weakened the value of the results, since It had a high nitrate content which could not have been derived from the starting materials supplied. The sugar and nicotine contents of this sample were lower than those of regular PCL, suggesting either only partial add-back of tobacco extract or the use of foreign materials during its preparation. However, the differences between the five processes were such that the sheets could not be expected to have identical chemical composition. The five sheets varied considerably in apparent surface area per gram (62 to 148 cm2/gram) and thickness (0.09 to 0.21 mm). but not in "apparent volume". Comparison of the properties of cigarettes containing 100% sheet was made difficult because the cigarettes had neither a common weight, pressure drop or firmness due to manufacturing problem probably stemming from the physical properties or moisture retention of the sheets. The calculated weight of the cigarettes for a common firmness varied in the range 1080 to 1280 mg, with the MK 11 sheet having the poorest filling properties. Calculated cigarette pressure drops for a common weight of 1200 mg varied from 7.4 inches for the Rapaport sample to 0.8 inches for that from the NX It process. apparently more through the influence of apparent surface area than apparent volume. The wide variations in weight and pressure drop of the cigarette BATCo document for Province of British Columbia 12 April 1999 5 samples containing 1002 sheet had a considerable effect on their smoulder rates and puff numbers, making smoke deliveries per puff the best basis for comparing the smoke composition. Caution Is required in extrapolating data obtained with 100% sheet cigarettes to blends containing only a portion of sheet. The properties and composition of the smoke from the 10OX sheet cigarettes were examined extensively. to serve as' reference points for future sheet work. Previous biological tests have suggested that Rapaport (Gerlach) reconstituted tobacco may give smoke with a specific activity that is lower than that from regular FCL. This is supported by many results of the present study. Thus the Rapaport sample gave smoke condensate containing the lowest 2 nitromethane fraction, the lowest yield of bento(a)pyrans, the lowest specific DCIP- reducing and ascorbate-oxidising activities, the lowest fluorescence and the lowest % total neutrals fraction. The smoke from the Schweitzer sample had a higher % nitromethane fraction than that from regular PCL, but in the other proper- ties listed above, the two smokes were very similar. In future sheet development work, It is important to confirm and account for the lower activity of sheet made by the relatively simple Rapaport process. The carbon monoxide content and the CO/CO2 ratio of the smoke, indicators of the degree of combustion, were very similar for the five samples, with Rapaport giving the highest CO level. Nitric oxide deliveries reflected the nitrate content of the sheets. The significance of relative deliveries of other vapour phase components from the five samples was difficult to assess. The Schweitzer sample gave highest yields per puff of acetaldehyde, formaldehyde and acrolein, with the AJ100 sample giving the least aldehydes. Regular PCL gave the highest deliveries of HCN, H2S, isoprene and methyl chloride. The delivery ratio of dry particulate matter to nicotine was high for all samples (between 29 and 45, with Rapaport giving the highest), but the different cigarette weights, pressure drops, and hence tobacco filtrations would affect the values. The transfer of nicotine from the Rapaport sample was lower than that from regular PCL or Schweitzer samples. The Rapaport sample also gave an exceptionally low phenol delivery. C=) BATCo document for Province of British Columbia 12 April 1999 6 Samples of Matinee, Player's Filter and du Maurler cigarettes, made from blends containing different levels of regular PCL, Schweitzer and Rapaport sheets, were prepared for subjective smoking tests. In making blends containing 50% sheet, the normal blend for a brand was not diluted with the sheet; indeed it replaced all the CRS and some of the low-tar yielding strips, in attempts to provide an acceptable smoke. The smoking tests, on samples containing about 50% of the sheets, indicated that the blends containing Rapaport sheet gave the least acceptable smoke. At the normal level of 7.72 in Player's Filter and Matinee cigarettes, differences were not apparent in the Player's series, with Schweitzer appearing to be the most acceptable in the Matinee blend. The value of results for the Schweitzer sample is reduced by its high nitrate content. Because of the nature of the substitution by the sheet samples in the Matinee and Player's Filter blends, one can expect marked differences in cigarette and smoke properties between the cigarette samples containing 7.7% sheet and those containing nearly 50% sheet; in fact observed differences at 50% included reduced, pressure drop and puff number in nearly all cases, and increased TPH yield, except for the samples containing Schweitzer sheet. The nicotine yield was decreased by the blend changes in the Player's Filter series. The foregoing study will form in part a basis for future sheet studies, In which the objectives will be to identify those physical and/or chemical factors of sheet which control the yield and specific biological activity of smoke tar, so as to develop new products with reduced tar yields and biological activity, while maintaining the satisfaction of the smoke. (MHB, ERF, RLR, MPS, MTS, RRS, TAS) T 6953 Determination of Sulahur and Chlorin@ Compounds in Smoke and Tobacco Objective: To provide a reliable method of measurement of the total sulphur content of smoke, since many of the sulphur compounds have a profound influence an smoke taste. The versatility of the Wickbold Apparatus, used to achieve the objective, has been described in I.T.P. Research Laboratory Report Number 116, and at the Tobacco Chemist's Research Conference in Montreal. In preparation for the r-i BATCo document for Province of British Columbia 12 April 1999 7 Conference paper, the distribution of sulphur and chlorine between the particulate and vapour phases of =wke was studied for Player's Mild flue-cured cigarettes. The particulate matter was trapped an a Cambridge filter, and the vapaur phase in a cooled glass spiral trap. The deliveries and 2 distributions are shown below. Smoke Found (UX/ciXt) 2 Distribution Component Particulate Va ur Particulate Vapour Phase Phase Phase Phase Sulphur 105 72 59.3 40.7 Chlorine 89 132 40.3 59.7 The H2S content of the vapour phase of these cigarettes was 35 US/cigarette. Thus this represents about 502 of the total sulphur content of the vapour phase. About 2OZ of the sulphur of the particulate phase Is estimated to be H2S- All determinations are averages of at least four determinations. The results for chlorine contrast sharply with that found as methyl chloride in the vapour phase by gas chromatography (T7175). The reason for the disagreement will be identified (ERF) . T 6961 Camver Test Obiactive: To become familiar with this well-established test, which has been used to distinguish between smoke from different tobacco types, since it may be helpful In studies of reconstituted tobacco. An apparatus has been constructed, similar to that of C. W. Ayers (R & DE Report No. R.D. 611-R). for measurement of the time and amount of smoke required, under controlled conditions, to block a Cambridge filter pad such that it attains a given pressure drop. The results are believed to relate to the viscosity of the condensate, which in turn may be controlled by chemical or other physical properties. Player's Mild flue-cured cigarettes, selected at 1045 15 mg and 2.9 + 0.1 inches P.D.) blocked the filter in 267 + 12 seconds during a trial involving 10 determinations, with 3 cigarettes per test. (M. P. S.) T 7084 Smoke Condensate fraction Ratios as a Guide to the Biological Activity and Taste of Smoke Objectives: (1) To establish in this Laboratory the C@h method for determination of the Lokstedt nitromethane fraction of smoke condensate, considered by BAT Hamburg rQ BATCo document for Province of British Columbia 12 April 1999 8 to correlate with specific biological activity as determined by the sebaceous gland test. (2) To quantify specific fractions of smoke condensate (total neutral*, total acids, total bases and subtractions) according to the Stedman scheme, and to use the relative amounts of these fractions to identify smokes with different levels of taste. (a) Lokstedt Nitrocethane fraction: the reproducibility of the method was determined for individual samples of 50 cigarettes, and by bulking smoke condensate and taking aliquots equivalent to 50 cigarettes for sample. The nitrowthane fraction was isolated by the procedure described in RAT Hamburg Progress Report April/June 1969. Individual Smoking Sample Condensate Nitromethane it 9 2 1 1.4074 0.1069 7.6 2 1.4180 0.1065 7.5 3 1.3992 0.1078 7.7 4 1.4253 0.1030 7.2 5 1.4393 0.1037 7.2 6 1.4694 0.1200 9.2 1.4263 0.1080 7.57 C.V.2 1.61 5.22 4.49 Bulk Condensate Solution Sample Condensate NitrometKane 9 x 2 1 1.4187 0.1056 7.4 2 1.3965 0.1081 7.7 3 1.4333 0.1104 7.7 4 1.3903 0.1125 8.1 1.4097 0.1092 7.7 C.V.2 1.22 2.35 3.22 C) 111-j NJ BATCo document for Province of British Columbia 12 April '1999 9 The coefficient of variation for nitromethane fraction in smoke condensate for individual smoking and bulk solution was thus found to be 4.5 and 3. ZZ respectively. (b) Stedman Fractionation: To avoid unreasonable variation in the weight of the water soluble acidic and basic fractions and to improve the reproducibility of results for other fractions, a method of weighing by difference was Implemented. For example. an ether solution of smoke condensate of known weight was extracted with sodium hydroxide solution, the ether fraction was reduced to dryness and the weight was determined. The difference between the original weight and the weight after extraction represented the weight of the acidic fraction in the condensate. In a similar way the weight of other fractions was obtained. The results for smoke condensates from 100 standard flue-cured cigarettes are shown below: New Method Stedman Method 9 9 starting weight of condensate 2.8156 3.1886 Total weight of all fractions 2.7305 3.8491 The new method gave a better correlation between original weight of smoke condensate and the total weight of fractions after separation. (MIPS) T 7175 Analysis of Smoke Vacour Phase by Gas Chroustograohy Objective: To facilitate the combined analysis of some important components of smoke vapour phase related to irritation, and hence reduce the time and cost of such determinations. If successful, this provides means of studying the effects of additives an smoke vapour phase by radioactive tracer techniques. Such additives could be burn retardants, sucker control chemicals. etc. (a) In the analysis, a constant vacuum. single port smoking machine Is used, Instead of the BAT bellovs engine, and the smoke vapour phase Ls collected in a plastic bag. TPM and nicotine deliveries of standard cigarettes, as smoked by the two machines, were compared using Cambridge filters. In addition, tests were made to see whether use of the plastic bag distorts the puff profile causing changes in deliveries of particulate matter. The deliveries of TPM and nicotine are shown below, with each result being the average of 10 determinations, using 2 cigarettes per set. Xhl C) BATCo document for Province of British Columbia 12 April 1999 10 TP.4 Nicotine Puff Mt/clit Mthiat No. Single Fort Machine with plastic bag 36.1 1.75 9.3 without plastic bag 37.2 1.80 9.0 Bellows Machine 36.3 1.76 8.5 Statistical analysis showed no significant difference between the use of the two smoking machines for TPH and nicotine deliveries and the insertion of a plastic bag did not influence the yields, although a difference in puff numbers was observed. (M. P. S.) (b) Further attempts have been made to improve the chromatographic separation of smoke vapour phase components. A 12' x 1/8" column with Chromosorb 102 (made as suggested in R & DE Laboratory Report No. L 330-F) generally matched the peak resolution obtained with the previously used Poropak Q column, and gave improved resolution for the low boiling smoke components. The new Chromosorb 102 column will be used in future studies. Machyl chloride has been separated and identified in the chromatogram; results of its quantitative determination presently conflict with chlorine deliveries measured by the Wickbold technique (T 6953), and the reason for the dilemma Is being sought. (M?S). T 7703 Effect of Tobacco Smoke and Smoke Comoonents on Mammalian Call Fraction Enzymes Obiective: To find a short-term bioassay for smoke based on possible effects of tobacco smoke and its components on parts of calls In which reside the enz7mes responsible for energy production and drug metabolism. I.e. enzymes controlling oxidations. The studies of smoke's redox properties (T 6256) have stemmd from this project. Inhibition of Cytochrome Oxidase The Inhibition of cytochrone oxidase (terminal oxidase in the mitochondrial electron transport system) Is being studied to see if we can differentiate between tobacco smoke conden- sates obtained by smoking flue-cured, yeast-treated flue- cured and two air-cured tobaccos (cigar and Burley types). Vapour phase and TPM's from all these types inhibit this enzyme. (M.H.B.) T 6256 Studies of the Redox Proverties of Smoke Objective: To identify smoke with low biological activity %D BATCo document for Province of British Columbia 12 April 1999 and to correlate redox properties with bioassays performed elsewhere an animals. Yeast Fermented Flue-Cured Tobacco Since the redox activity of smoke from flue-cured tobacco was found to be higher than that from air-cured types (cigar and burley types), It was felt that the higher level of sugars in the flue-cured tobaccos could explain the larger amount of redox substances in the smoke. To test this, most of the sugars in a sample of flue-cured tobacco was remmed by yeast fermentation. Both the untreated and yeast-treated flue-cured tobaccos were then dried, powdered and smoked in cigarette tubes. The TPM's obtained were examined both for DCIP-reducing and ascorbate-oxidising activities and the results obtained are presented in the following table. From the results it will be seen that although there is a distinct drop in the redox activities, it did not parallel the removal of sugar, but the activities do approach those obtained for air-cured tobaccos with respect to DCIP reduction. It should be pointed out that the TPM values from yeast-treated flue-cured tobaccos are distinctly higher than those from the untreated flue-cured tobacco. Similar results appear to have been obtained at Southampton, (R 6 D.E. Report No. R.D. 309-R), when the higher tar delivery was attributed to lower filtration (due to lower pressure drop) in cigarettes made from yeast-treated tobacco. At the present time it is difficult to account for the higher tar values. Wt. of TPM Sugar content DCIP reduction Ascorbate Tobacco (mg) from Specific activity oxidation 5 cigarettes units per mg. TP4 UM oxygen Reducing Total uptake per min. per ag, TP.4 Flue-cured 101.4 23.2 23.8 7.17 0.81 control Yeast-treated 196.7 4.9 5.0 5.34 0.73 24 hours Yeast-treated 179.1 3.4 3.9 4.64 0.68 96 hours I I I I I Measurements have also been mAde of the reducing properties of smoke from reconstituted tobaccos made by five processes (T 6533). The specific activities of both DCIF reduction and ascorbata oxidation were Lower for the smoke from all C=) the sheet samples than for that from normal flue-cured rQ 4@1- PO r_j BATCo document for Province of British Columbia 12 April 1999 12 cigarettes. with the Rapaport sample having the lowest activities. (MM3) T 7652 Effect of Smoke on Hemoslobin Obiective: To develop a bicassay for smoke based on penetration of erythrocytes and reduction of hemoglobin by smoke. Work has continued on the action of cigarette smoke (TPM) on blood cells and hemoglobin (Hb). The work has been car-.4.ed out mainly in two directions: 1. incubation of hemolysate (i.e. HB) with smoke solution. 2. incubation of whole red blood cells with smoke solution. 1. Known volumes of hemolysate (of about 0.03H Hb conc.) were incubated at 370C with varying concentrations of smoke solution (5 cigs. in 10 or 20 ml buffer) and the spectral changes at wavelengths 540 and 580 mu noted. Increasing concentrations of smoke caused a gradual diminution of the 580 mu peak with time. By measuring the differences between absorption maxima at 540 and 590 mu (i.e. A 540-580) a quantitative relationship could be established between smoke concentration and reaction race. Attempts have been made to find out the mechanism(s) of action involved in the breakdown of Ub by aqueous smoke solution. Hemolysate (of about 0.15 M HO was Incubated with phenylhydrazine (0.001 N) 'and spectral changes at the two absorption maxim again noted. The phenylhydrazine- treated Hb reaction differed from that of the smoke-treated Rb as evidenced by the difference in spectra of the end points of both reactions. This would indicate that the mechanism of action of smoke and phenylhydrazint may not be the same. However, in both cases one reaction product seems to be formed since the lines in the spectrum pass through isobestic points. With sodium borohydride the spectral changes differ markedly from those of smoke and phenylhydrazine reaction (see diagram). 2. Attempts have been made to produce Heinz bodies by incubating freshly washed red blood calls with smoke solution. These attempts have been complicated by the fact that washing the calls with isotonic saline SeeM3 somehow to increase the fragility of the cells. Alternative methods are currently being sought to wash, stain and fix the smoke-treated cells. U.J.) NJ P.) N-) BATCo document for Province of British Columbia 12 April 1999 L J COM, arlson Am Letween (A)5mAe - Olt (B) @ken Urazine- anJ CC) NQ-@Orok JrJe rJc Herno9ialo-ln PL.,,),Ib Nd LrAydri-6 - @.W - , yd tr*dfC4 PQ I.C NJ 00 BATCO document for Province of British Columbia 12 April 1999 T 6900 Determination of Sweeteners in Plastic Cigar Tips Objective: 1. To support the Company's patents governing the use of sweeteners in plastic cigar tips, which are being challenged by the Simon Cigar Company. The support is provided by Identifying and measuring the sweeteners, and in finding their mode of application. 2. To apply the same analytical techniques to some problems in the consistency of our ova supplies. Tips from Portins (Simon) and Old Part tipped cigarillos were exhaustively extracted in whole form with m*thanol, to determine the amount of sweetener on their surface. The tips were then pulversed, and reextracted exhaustively to determine the amount of sweetener within the tips. Large differences were found between the amounts of sugar and sodium saccharin which the Simon Cigar Company claimed to use (6.7 and 7.7 mg/tip respectively) and the amounts found (0.3 and 1.2 mg/tip respectively). possibly due to several factors: 1. an overestimation by Simon of the additives left on the tips after coating, based on the amount used by the process: 2. a process variation caused by the nature of the dipping process; 3. analytical error. Two methods have been used for saccharin determination, 1. direct spectrophotometric measurement at 254 mg. 2. the calorimetric method of S. Di Pasquale et Al. (Annals of the Faculty of Economics and Commerce, University of Messina. 6. (3), 1%8). Although neither are fully satisfactory, results obtained are in reasonable agreement. Although a coating technique is used for the Porting tips, only about 74% of the saccharin is 'available' an the surface, some having migrated into the plastic probably through the solvent action of the cellulose gum used in applying the coating. The saccharin in the Old Port tips is applied in the mold, and of the 3.9Z found in the whole tips, only 0.17% is 'available' on the surface (i.e. only 4% of the total saccharin). Wide variations in the level of saccharin in the Old Part tips were observed. The tests also showed that the tips contained residues other Chan the added sweetener e.g., possibly slip agents. antioxidants. (ERF) BATCo document for Province of British Columbia 12 April 1999 15 During the quarter, throe papers were presented at the 24th Tobacco Chemist's Research Conference In Montreal. These were: 1. Filling capacity as a function of the bulking volume and the capacity of the tobacco to resist compression, by R. L. Rice. 2. Determination of sulphur and chlorine In tobacco and tobacco smoke using the Wickbold apparatus, by E. R. rreiesleben and T.A. Smith. 3. Effect of tobacco smoke condensate on reduction- oxidation compounds with particular reference to ascorbate oxidation, by M. H. Bi limoria and M.A. Nisbet. Three papers have been published: 1. The calorimetric determination of glycerol in tobacco, by M.A.-Nisbet and Mrs. S. Schmeller, in 'Tobacco', October 9, 1970, page 29. 2. A weight loss technique for determining rate of static burn, by R. L. Rice, also In 'Tobacco', December 11, 1970, page 47. 3. A calorimetric method for the determination of nitric oxide in cigarette smoke, by M.P. Scherbak and T. A. Smith, in 'Anakyst', volume 95, page 964 (1970). The following reports were issued: R. L. Report No. 128: Differentiation of tobacco smoke condensates on the basis of reducing properties. by M. R. Bilimoria and M.A. Nisbet. R. L. Reports No. 129 and 130; Summary reports of 24th Tobacco Chemist's Research Conference, Section A. edited by T.A. Smith. Jbb CD BATCo document for Province of British Columbia 12 April 1999 402421931