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CONFIDENTIAL Copie QUANTITATIVE EVALUATION OF CIGARETTE SIDESTREAM SMOKE COMPONENTS UNDER CONTROLLED EXPERIMENTAL CONDITIONS Interim Report No. 1 Installation and testing of experimental room and analytical instruments. Determination of carbon monoxide, nitrogen oxides, ammonia, hydrogen cyanide and nicotine. PME/R&D Neuchatel January 23, 1984

TABLE OF CONTENTS Cl OBJECTIVE GENERAL EXPERIMENTAL APPROACH EXPERIMENTAL EQUIPMENT Page 1 2 4 - Experimental Room 4 - Smoking Machine 4 - Analytical Instrumentation 5 - Experimental Equipment for Single Cigarette Experiments 6 EXPERIMENTAL CIGARETTES 7 EXPERIMENTAL METHODS 8 - Smoking Conditions 8 - Testing of Experimental Room 8 Mixing of Air 8 Airtightness 9 Humidity and Temperature 9 - Determination of Carbon Monoxide 9 - Determination of Oxides of Nitrogen 10 - Determination of Total Ammonia 10 - Determination of Nicotine 11 - Determination of ydrogen Cyanide I2 - Single Cigarette Determinations 12 EXPERIMENTAL RESULTS AND COMMENTS 14 - Carbon Monoxide 14 - Oxides of Nitrogen 14 - Total Ammonia 15 - Nicotine 15 - Hydrogen Cyanide 16 SUMMARY OF RESULTS 17 FUTURE PROGRAMME 18

Page REFERENCES APPENDIX 1 APPENDIX 2 APPENDIX 3 19

QUANTITATIVE EVALUATION OF CIGARETTE SIDESTREAM SMOKE COMPONENTS UNDER CONTROLLED EXPERIMENTAL CONDITIONS by Blake-C. and Piad6-J.J. Interim Report No. 1 OBJECTIVE Cigarette smokers and non-smokers may be exposed to various levels of tobacco smoke in indoor environments depending on the rate of smoking, the cigarette type, the size of the room, etc. Data available in the literature for sidestream smoke levels are often not comparable (1). Results were obtained under different and sometimes unrealistic experimental conditions. To gain a comprehensive knowledge of sidestream smoke levels and a more thorough understanding of tobacco smoke behaviour in indoor environments carefully controlled experiments have to be performed. The objective of this study is to experimentally determine the concentration of several components of cigarette sidestream smoke in ambient air as a function of time and of the number of cigarettes smoked. The experiments have to be performed in an experimental room under controlled experimental conditions. The components to be evaluated are CO, NO, NO , NH , HCN, nicotine, N-nitrosamines, tobacco specific 2N-nitiosamines, organic acids, phenols, formaldehyde, acetaldehyde and particle mass. In addition the particle number and the particle size distribution should be investigated. In the first part of the programme reported here the experimental set-up was installed and tested and the following compounds investigated : carbon monoxide (CO), nitrogen oxides (NO, NO2), ammonia (NH3), hydrogen cyanide (HCN) and nicotine. The work was carried out under VDC contract (VDC project No. 9/82) in the period between February and December 1983.

2 GENERAL EXPERIMENTAL APPROACH Experimental procedures in this study were designed with the intention of generating and analyzing cigarette sidestream smoke under controlled conditions. The initial experiments were concerned with the installation and testing of the experimental room. It was designed to be airtight, to have inert inside surfaces and to allow for effective air mixing. The room was equipped with a 30-port smoking machine fitted with an automatic feeder, an automatic butt extractor, an automatic lighter, and with a remote controlled manual overriding facility. The room was fully equipped for sampling at different positions within the room, with automatic 14-channel sampling systems located outside of the room with feedback flow controls and timers for sample collection. Air samples were returned to the room after passing through the analytical equipments. The mainstream smoke was totally directed out of the experimental room. In the second phase of the project the concentrations of selected components of sidestream smoke were determined and their change with time was monitored. Cigarette were smoked under standard smoking conditions (35 ml puff, 2 sec. duration, 1 min. intervals) at 60 % relative humidity and 22°C. The atmosphere in the experimental room was thoroughly mixed immediately after the extraction of the last butt. One minute later sampling was started. Throughout the study carbon monoxide was used as an internal standard to compensate for losses by diffusion out of the room during sampling periods exceeding 4 hours. The concentration of certain sidestream smoke components e.g. nitrogen oxides or nicotine changes rapidly with time. In such cases efforts were made to reduce to a minimum the sampling period for these compounds. Two approaches were considered for data reporting : - The actual concentrations as measured after a defined time are tabulated so that experimental data for various smoke components can be correlated. Calculations were made in order to derive values less dependent upon sampling time, aging of smoke, room volume, air mixing period, number of cigarettes smoked, etc. In this approach the decay of the component concentration was recorded and fitted to an equation allowing extrapolation to a chosen reference point i.e. to "zero" time. The middle of the smoking period was considered to be an acceptable approximation for this point.

- 3 - The "zero" time concentrations were measured after smoking various numbers of cigarettes (5 to 60). They were plotted against the number of cigarettes smoked to check for any deviation from proportionality and to obtain the averaged contribution per cigarette to the concentration value. This allowed the calculation of a yield per cigarette. The final step of the study was to compare the calculated experimental room yield per cigarette with the yield per cigarette determined by single cigarette bench-scale sidestream smoke analysis. For this purpose single cigarette experiments were performed for CO, NO, NO2, NH3, HCN and nicotine.

EXPERIMENTAL EQUIPMENT Experimental Room A cold storage room (Frigorex Type KZ 80) was purchased from Frigorex AG/Luzern and modified to be used as an experimental room. It had external dimensions of 2.98 x 2.67 x 2.72 m and internal dimensiops of 2.83 x 2.54 x 2.53 m. The volume of the room was 18.2 m . The room was internally covered with stainless steel. It was insulated with polyurethane foam (6 cm thick) and covered externally with galvanized steel plates. A door was f itted to gain entry into the room with a viewing hatch to visually monitor the smoking process. The room was equipped with lighting, electrical power points and two 21 cm-diameter ventilation ports. One port was connected to an air extraction system for removing smoke, while fresh air could be drawn through the other port. Two 1 1/2" stainless-steel pipes were extended through the wall into the room. One pipe was connected to the smoking machine. The other pipe carried the stainless steel tubings (5.3 mm i.d.) for sample drawing and the connection to the probe for humidity and temperature monitoring. A stainless-steel stand was installed towards the middle of the room to which were attached sampling traps and a camera for monitoring the smoking process from the instrument room. For diagram of the experimental set-up, see Figure 1 and photographs 1 and 2. After experiments, walls, ceiling and floor were washed with aqueous isopropanol solution (50 %) to remove deposits. A second wash with water removed the residual isopropanol. The room was dried by forced ventilation before starting a new experiment. Duration of cleaning cycle approx. 2 hours. Smoking Machine A modified 30-port Battelle smoking machine was installed in the middle of the room on an adjustable table at 68 cm hight. The puff profile was checked to be essentially square. The case of the smoking machine and the table were made of stainless- steel. The smoking machine was equipped to provide automatic feeding and lighting of cigarettes and extraction of butts shorter than a given length. A remote control from outside the room allowed one to override these automatic functions. A 1 1/2" stainless-steel pipe connected directly to the smoking machine carried all the cables and tubes associated with the machine to an external control panel.

5 The mainstream smoke was directed out of the experimental room through the same pipe. The mainstream smoke was filtered through a 15 cm-diameter Cambridge filter before entering the diaphragm pump. This filter size allowed at least 60 cigarettes to be smoked without any change in puff volume. Cigarettes were lit by means of a hydrogen flame which was ignited by a spark from a platinum wire. The flame was left burning for as short a time as possible. Extracted butts fell into a water-filled container which was sealed by an automatically actuated lid. Ashes were constantly brushed into the same container. The arrangement is shown in photograph 3. Analytical Instrumentation Relative humidity (RH %) and temperature (T°C) were monitored with a Humilab 20 meter (Lee Dickens Ltd.) fitted with a sintered bronze-protected probe. The probe was placed inside the experimental room. Carbon monoxide was monitored by a microprocessor driven linearized non-dispersive IR (NDIR) monitor Model CO-1OM (Environnement S.A.). An internal pump gave a measured flow rate of 2 1/minute. The air in the experimental room was sampled by means of 5.3 mm i.d. stainless-steel tubing connected to the CO analyzer and returned to the room.* A Wilks Miran 80 Infrared (IR) single beam analyzer fitted with a 20 m pathlength cell was tested for carbon monoxide monitoring. Air samples were pumped by a Wilks "ambient air pump" operating at 2 1/minute through a silica gel cartridge of 18 cm length and 5 cm i.d.* A CSI Model 1600 Chemiluminescence NO Analyzer was used to determine NO and NO . Air was sampled Yby means of 5.3 mm i.d. stainless-steel tubing. After analysis the exhaust gas passed through a charcoal cartridge, which removed residual ozone, before being returned to the experimental room.* * Instruments were calibrated with standard gas mixtures in nitrogen obtained from Carbagas. For CO the concentrations used were 9.9, 25.2, 50.2, 96.4 and 200 ppm (+/- 3$ relative). For NO, concentrations of 2 and 5 ppm (+/- 3% relative) were requested. The cylinders were changed every 2 months. During this period no drop in NO concentration was noted, even for the lower concentration.

6 A 10-channel data-logger system HP Model 3056 DL (including an HP 85B micro-computer) was used to collect, handle and print automatically data from the various instruments (CO, NO, NO2, RH, T). The air samplers used throughout the study were Digitel D 75 fourteen-channel samplers (Wisag AG/ZUrich) with timer and flow control facilities. Experimental Equipment for Single Cigarette Experiments FTR-Huguenin piston single-port smoking machine. Siemens NDIR CO Analyzer, Model Ultramat, 0-10 %. Leybold Heraeus NDIR CO Analyzer, Model Binos 1, 0-5 %. Thermo Electron Analyzer. Corp. Series 14 Chemiluminescence NO/NO2 Thermo Electron Analyzer. Corp. Model 10 Chemiluminescence NO/NO2 Pear shaped 1-litre glass smoking chamber with cambridge filter holder, 9.2 cm 0, cigarette holder with rubber sleeve, air diffuser and opening for lighting and extinguishing the cigarettes. The experimental apparatus used for the single cigarette analysis is depicted in Figure 2.

7 EXPERIMENTAL CIGARETTES Two types of experimental German blend filter cigarettes (blend composition : ca. 50 % Virginia, 20 % Burley, 20 % Orient and 5-7 % reconstituted tobacco) coded C20 and C50 and supplied by the VDC were used for the experiments. The cigarettes were stored in a freezer at -40°C. Before use the cigarettes were placed in open packs in a room of contrglled humidity (58 $+/- 3$) and temperature (220 C +/- 2 C) for at least 72 hours. Cigarette specifications, tobacco values and mainstream smoke values are given in Table 1.