Tobacco Documents Online

CONFIDENTIAL PROJECT IVUMBER : 2501 PROJECT TITLE : Smoke Chemistry PROJECT LEADER : R. A. Comes PERIOD COVERED : May, 1991 I. SIDESTREAM SMOKE CHAMBER A. Objective: Operate an environmentally controlled chamber to measure selected components of sidestream smoke. B. Results: Normal thirty cigarette chamber runs and five cigarette aerosol runs have been compl'eted on the cigarettes in the sidestn;am analytical-subjective series. The run data is cwrently being tablulated and a report will be written. The hardware for the chamber modifications has been fabricated and will be installed when static smoke nms are completed. These static experiments are currently in progress. A new chamber smoking procedure had to be devised to conduct these experiments since the Borgwaldt smoker is designed to only operate under puffing conditions. The gc procedure in use for the analysis of nicotine requires a run time of thirty five minutes. This is quite long considering the number of nicotine samples analyzed for a set of chamber runs. Modi~fications to the procedure have now reduced that time to approximately ten minutes per gc run. Studies were conducted to insure that no loss of precision or accuracy was involved with this procedural change. Personnel of CAD are in process of optimizing several RS/1 procedures to reduce the manual effort required in generating reports, calculating results and file management of chamber data base files. These changes should be implemented within this next reporting period. Initial studies have begun directed at the incorporation of a procedure for the analysis of acrolein into the chamber analytical procedures. Acrolein is rarely seen using the current DNPH SepPak trapping procedure. Tests have shown that acrolein (as the DNPH derivative) placed on a clean SepPak cartridge or on one impregnated with acidified DNPH solution is recovered when flushed with acetonitn7e in the manner described in the standard chamber procedure. This indicates that acrolein is not being collected during smoke runs. A bubbler procedure will be investigated. Procedures for the collection of sidestream particulate during normal chamber runs in sufficient quantity for separation and further analysis are being investigated. An impaction trapping system incorporating the small vials used for neutron activation analysis work is being studied with some initial success obvious. C. Plans: Chamber runs will continue as required. Work will continue on chamber modifications to allow for the sidestream analytical-subjective study. A procedure for the analysis of acrolein will continue to be investigated. Procedures for collection of sid'estream TPM during normal chamber operation will continue. C91-02637

2501-2 H. SIDESTREAM SMOKE A. Objective: Conduct studies on sidestreant smoke including: development of methods for collection and analysis of sidestream semivolatiles and gas phase; visibility determinations; analysis of selected materials relating to sidestream odor and irritation; development of proprietary products. B. Results: Optimization of the operation of the headspace-gc-ms system continues. Successful automation of the method was accomplished during this period. Previously, it was possible to make only one desorption-gc-ms run at a time due to built in constraints imposed by the total system. Following the successful automation, multiple runs were made to simultaneously study several method variables. Information was gathered on nm-to-run variability, breakthrough of the sample components during collection onto the air tube adsorbent, comparison of Tenax -Carbopack traps with Carbopack only traps, comparison of runs with different desorb times and comparison of runs with different purge times. This work continues and results will be detailed at a later date. Work has been completed on the method to account for the smoke escaping from~ the ventilation holes of cigarettes. A prototype apparatus was designed that seems to be effective in accounting for all of the escaping smoke. Requested cigarette models were evaluated and the data reported in memo format. A video of the smokings was also supplied. This work has stopped at this time. C. Plans: The O.l: H.P. system will continue to be vigorously studied to determine its overall utility as a new instrument for conducting sidestream chamber analytical studies, particularly as they may relate to the new sidestream analytical-subjective work. CORESTA smokings will continue as required. IIL MISCELLANEOUS 1. Infrared camera - New software for analyzing the IR camera images has been received. The image processor computer used with the IR camera is experiencing disk problems so the new software has not been loaded. A request to repair the computer has been submitted. 2. Neutron radiography - The buildup of condensibles during smoking has been measured in the cigarettes from the sidestream analytical-subjective series (X8Ta1WG - WK) and in banded cigarettes from Project Tomorrow under both static and puffing conditions. Data analysis is in progress.. Requested modifications to the smoking machine are in progress that will allow the taking of one puff followed by the remainder of the smoking under smolder conditions. A manually operated solenoid' has been placed in the line from the smoking machine to the cigarette. The operator can turn the solenoid on to take one puff and then turn it off. The smoking machine will continue to take puffs, keeping data collection properly timed, but no air will be drawn through the cigarette. 2

2501-3 A second request was to investigate a change in the method of data reporting from a "change in density-thickness (mg/cm~" to a percent mass loss value. One method attempted was to calculate the scattering cross section of tobacco from the elemental composition of the tobacco. This effort is continuing. A second was to devise a calibration method using tobacco. Cigarettes were cut into sections with several different lengths. The sections were weighed, measured for size so the tobacco density could be calculated and placed in the neutron beam head on. Thus, the attenuation of the neutron beam could be measured as a function of the amount of tobacco it passed througlL This provides a calibration curve relating the change in the neutron beam intensity with the actual amount of tobacco present. From this work came the suggestion by a Physical Research Division co-investigator to look at the sum of the density-thiclaRess changes for all twenty of the measurement zones in the experiments. This gave a density-thickness change curve that was linear with time for a smoldering cigarette and is the curve shape obtained when the mass loss of a smoldering cigarette is measured using a balance. Initial data comparisons have given quite good agreement and these studies will continue. The major valiue to this technique is that it can be used to measure mass loss for puffed cigarettes which cannot be done using the balance technique. 3. Pyrolysis gclms analyses were conducted in support of the menthol release and potential new product materials programs. Memos were issued, in support of these studies. 4. Assistance was provided to personnel of the BCR division in the attempted gc/ms analysis of N-methylputrescine and related products. Additional support will be provided when instrumental probl'ems are resolved. 3