WIV R % 0 CRIUZE 13 APRC;1988 R.J.Reydolp Tobacco o!i!l (919) 777-5000 S.Em by: ..................... ...... April 7, 1988 Nip: FntJJ 9n I TO: CORESTA ETS Collaborative Study Participants I have been informed that you wish to participate ~n the CORESTA ETS Collaborative Study program that was discussed at our ,7anuary meeting in London. The analytical methodologies for nicotine, respirable suspended particles (RSP), and ultraviolet particulate matter (UV-PX) to be collaboratively studied are those contained in the R. T. Reynolds Tobacco Company documents titled "Pi7ocedure for Determination of Nicotine collected in in- door Environments" (for nicotine)., and "A Method for Estimating the Contribution of Environmental Tobacco Smoke to Respirable Suspended Particles" (for RSP and UV-PM) . Copies of these protocols were distributed in London; however, please inform me immediately if you do not have them. The three methods require the following instrumentation: Nicotine., gas chromatograph with capillary column capability and nitrogen-selective detector (UPD) . RSP: electronic "microgram" balance with 1 microgram readability. UV-PM. HPLC injector, pump, and ultraviolet detector set at 325 nm. "Semi-microgram" (10 microgram readability) balances and standard spectrophotoisters do not possess adequate sensitivity for these methods and should not be used. I The collaborative study will be conducted in three phases: 1) material acquisition, instrument set-up, and method familiarization. 2) Analysis of spiked samples for -~erification of method implementation.. 3) Analysis of collaborative study samples. Each participant should be engaged in Phase, I at this time. Phase 2 is currently in progress in several laboratories and will continue until all participants can successfully meet the evalua- tion criteria proposed for this study (enclosed on a separate sheet). Phase 3 will consist of additional spiked samples in ad- dition to ETS samples generated in our environmental chamber. During Phase 2, each participant' will be informed of the expected concentration at the time they receive spiked samples. However, during Phase 3, all samples will be analyzed without any prior Ln co U4 BATCo document for Legal Services: Health Canada 19 October 1999 knowledge of expected concentration. It is expected that you will communicate your results from Phase 2 to me as the study proceeds. All results from Phase 3 will be reported to me for compiling and statistical evaluation. A standardized format for reporting Phase 3 results will be sent to you with the samples. Please be aware that Phase 2 of this study will take a mini- mum of several months to complete due to unavoidable shipping delays that will occur with several overseas participants and unexpected analytical difficulties that always arise. It is un- likely that Phase 3 of the study will be scheduled to begin before mid-,Tuly. I will keep everyone informed as things progress. Enclosed with this letter are descriptions of consumable supplies that each participant should obtain, procedures for preparing spiked samples, and a current list of acknowledged participants. As stated previously, . shipping/cqX1respondpn9&- delays -with overseas participants could be severe. Therefore; 1, urge each participant to confirm in writing their willingness to par- ticipate in the analyses indicated and their complete, correct address for receipt of both samples and correspondence (if different). Also, please provide me with information on the fastest method of communicating with you (telephone, telefac- simile [preferred], or telex) and any suggestions for rapid ship- ping (Federal Express or other overnight air mail company). My address for both samples and correspondence is: Dr. Michael W. Ogden R. J; Reynolds Tobacco Co. Research and Development BGTC 611-13/102E Winston-Salem, KC 27102 USA Office telephone: 919/741-5787 Secretary's telephone: 919/741-5366 Talefacsimile number: 919/741-4682 Spiked nicotine and UV-PM samples can be prepared and shipped to you for analysis at any. time. However, to prepare spiked samples for RSP, I must receive pre%,--.,* ghed.f ilters from you in advance. Please advise me when your 'laboratory is ready. With sufficient preparation, I feel we can have a successful collaborative study effort in our first'attempt. If you have any questions regarding the analytical protocols or the collaborative study sequence, please do not hesitate to contact me. sincerely, k MJchael W. Ogden, Ph.D. Research Chemist Enclosures 00 BATCo document for Legal Services : Health Canada 19 October 1999 COLLABORATIVE STUDY EVALUATION CRITERIA i Data from this collaborative study will be evaluated by a 2-way analysis of variance (ANOVA) as described in "Statistical Manual of the Association of Official Analytical Chemists", W. ZT. Youden and E. H. Stainer, 1975. Comparability will be successfully demonstrated-if the between-laboratory variance ratio and the -laboratory-sample interaction variance ratio are both judged insignificant at the 951 confidence level. Nicotine For spiked nicotine samples,'accuracy should be within 15% of the true values. For spiked particulate matter samples, accuracy for gravimetric determinations (RSP) up to 20 micrograms should be within 50% of the true values and at levels greater than 20 micrograms should be within 20% of true values. For UV-Px determinations at all levels, the accuracy should be within 15% of the true values. _;~b C) 011 00 Qn BATCo document for Legal Services : Health Canada 19 October 1999 CONSUMABLE SUPPLIES TO BE OBTAINED BY EACH PARTICIPANT Nicotine PrQtocol XAD-4 resin tubes - Catalog no. 226-30-11-04 (with foam spacers) or Catalog no. 226-30-11-04-GWS (with glass wool spacers) ob- tained from SKC, Inc. (worldwide distributor information enclosed). As stated in the method, tubes with glass wool spacers are preferred; however, these tubes'are currently a cus- tom item made for RJR by SKC in Appomattox, Virginia, and are not available from European distributors. As a result, the stock tubes with foam spacers are recommended for this study. Each participant should obtain enough tubes to practice spiking, extraction, and desorption efficiency determination for Phase 1. All spiked tubes sent to participants (Phase 2) and all tubes used for the collaborative study (Phase 3) will be provided by RJR to ensure the same lot number from the supplier. RSP/UV-PM Protocol Filter cassette assembly - Catalog no. M00003700 and Fluaropore membrane filter - Catalog no. FALP 03700 obtained from Millipore Corp. (worldwide distributor information enclosed). Filter cassette gasket - Part code no. 0301139-A31 ("Handle, Gasket", 48 per package) obtained from SlQan Valve Co., 10500 Seymour Avenue, Franklin Park, Illinois, 60131, USA. (NOTE: These gaskets are used instead of the support pads supplied with the Fluoropore filters. A tighter seal is obtained, thus preventing air leaks around the filter during sampling.) Each participant should obtain enough complete filter assemblies to practice spiking, weighing, and extraction for Phase 1. Fil- ters to be spiked for Phase 2 and filters to be used for Phase 3 must be supplied by-each participant. For both Phases 2 and 3, pads must be weighed in the participants laboratory, sealed in the cassette holders, and shipped to RJR for spiking/sample collection. The entire cassette will be returned to the originating participant for analysis. For Phase 2, 12-16 filters should be shipped for each trial. For Phase 3, 20 complete as- semblies will be required. As the turn-around time for cassette assemblies shipped overseas will probably be several weeks, I suggest you obtain at least 50 assemblies to begin with. one Fluoropore membrane filter and one gasket are enclosed for your reference. (-n ON -(.n CD (31*1 BATCo document for Legal Services : Health Canada 19 October 1999 SPIXING PROCEDURES FOR PREPARING PRACTICE/QUALITY CONTROL SAMPLES Nicotine Prepare several solutions of known nicotine concentration in ethyl acetate modified with triethylamine and inject no more than 3 microliters into the resin bad inside the XAD-4 sample tube. More than 3 uL has a tendency to locally saturate the resin al- lowing solution to contact the glass tube walls resulting in low bias. If desired, the tubes can be air dried for several minutes with a low flow (0.2 - 0.5 L/min) of clean,' compressed air. RSP/UV-PH Accurately weigh 0.010 q of 2,21,4,41-Tatrahydroxybenzaphanone (THBP, the surrogate U`V-PX standard) and 0.100 g of Carbowax 1000 (polyethylene glycol, average mol. wt. 1000) into a 10-mL volumetric flask, dilute to volume with HPLC-grade methanol, and shake to mix. Each microliter of this solution contains the equivalent of I ug UV-PM and-11 ug of RSP. Typically, 1-10 uL are then injected onto a preweighed Fluoropore filter'inside the cassette holder. This pad must be air dried prior to analysis and this is accomplished by drawing air (with a personal sampling pump at 1-2 L/min for several minutes) first through a Cambridge filter pad and then through the Fluoropore pad. I J.>. CD Ln Co BATCo document for Legal Services : Health Canada 19 October 1999 LIST OF PARTICIPANTS CORESTA ETS COLLABORATIVE STUDY. (AS OF 4-07-88) Company Contact Person Analyses ---------------------------------------------------------------------- BAT (U.K. & Export) LTD R. R. Baker Nicotine, RSP, UV`-PM Brown & Willia-mon J. F. Nall Nicotine, RSP, UV-PH Imperial Tobacco LTD C. A. Hill Nicotine Japan Tobacco Inc. Y. Ishizu Nicotine, UV`-PX Philip Morris Europe ZT. J. Piade Nicotine, RSP, UV-PM R. J. Reynolds Tobacco USA M. W. Ogden Nicotine, RSP, UV-PM H.F. Ph.F. Reemtma GmbH X. Ball ? Rothmans Int. Services LTD E. D. John Nicotine Verband der Cigarettenindustrie G. Scherer (.n Co CD BATCo document for Legal Services: Health Canada 19 October 1999 SKC World-Wide Service SKC Is a dedicated Inter- national company with For locations not serviced by a world-wide distribution. local distributor, SKC We have technically 7 International Sales are handled by: qualified distributors GUILD CORPORATION that can assist you with f (An SKC Affilialed Company) your air sampling and 1 384 Thomas-Venetia -Road equipment needs rA)n- Eighty Four, PA 15330 I n tact the distribu~;r in USA the location neares you. TEL: (412) 941-9754 TLX-. 510-697-3140 K~' K-;-:AUTHORIZED, DISTRIBUTORS. ARGENTINA CANADA (Western) ICELAND PORTUGAL 0 Aislair S.R.L. Flock Brothers Plastionnun HF Soboequip Lao. Concepcion Arenall 4232 7720 69th Street P.O. Box 176 Ouinta Da Piedade (1427) Buenas Aires Edmonton, Alberta T613 2,17 230 Koftvik Lots 12. 10 Tat 8S4-8926 Tel: (403) 4364414 Tel: 354-2-6616 2625 Provoa Do Santa Iria Tlx: 52 'nx: 037-3426 TIx: 2307 Tel: (01) 259 4462 TIx: 43926 AUSTRALIA CHILE IRELAND Air-Met Scientific Quantum Scientific SINGAPORE P ' 0. Box 93 Alslar do Chile Ltda. 113 Clonrosse Drive Sciencescan Cons. & Serv. Pte. Ltd. Doncaster ran Miguel Clare 1467 Santiago do ChIle Malahide Road 168A/B & 170A Block I -Vaoria'3109 Tel: 223-8358 Dublin 13 Kallang Avenue Industrial Centre Tel: (03) 419 8042 Tel: Dublin 470186 Kallang Avenue Tic 10717605 DENMARK Singapore 1233 Mikrofab Aarhus AIS ITALY Tok 2912351 AUSTRIA Axel Kiera Val 34 TCR Tecora S.R.L. Tlx: RS 28501 Please contact SKC. Ud., U.I-L OK-8270 Hdiberg Val San Luca. 10 BELGIUM Teh (06) 29 61 11 20122 Milano SPAIN Tlx: 68720 Tel: (02) 83-99-168 Sodift S.A. Delta International SM. Tlx: 3IR09 Caramuel 38 Posthus 438 FINLAND MALAYSIA 28011 Madrid 1400 OK Bussunt Oy Chroma-Lab A13 Juru-Aubcoil San. t5rid. Tel: Madrid 463 77 62 Holland 01100 Ostersundom 5D-8 Jalan Tapah The 48595 Tel: 02159-33055 Tel: (90) 8777013 OIIJajan Goh Hock Huat SWEDEN TIx: 73250 (ATTN. REF 520) Tlx: 121394 (Alm, CHROMTEL) 41400 Kelang, Solarigor I Scantac: Laboratorioutrustning A13 BRAZIL Tel: 03-326534 Box 238 Ric Lab Pmductos W.GERMANY 71x: 39572 S-433 24 Partille a Equipamentes Please contact SKC. Ltd., U.K. par2 Laboratodos Ltda. NETHERLANDS Tel: 031-44 71 80 Rua 29 do Julho. 14243onsucesso GREECE Deha International B.V. TIx, 21412 21040 Ric Do Janeiro Purcon Ltd. Postbus 438 SWITZERLAND Tel: 2704899 116 Vas Soflas Aves 1400 OK Bussufn Or, Jacques Bourgeois Ing. EPFL TIx., 02123872 115 28 Athens Tel. 02159-4.WSS En Cumon - B.P. No. 39 Tel: 779=1 lk 7793W The 73=5 (Attn: REF 520) Ch-1603 Grandvaux CANADA TIx: 218429 NEW ZEALAND Tel-, (021) 99 19 08 Safety Supply Canada Ltd. TIX: 25 516 90 West Beaver Crosk Road HONG KONG Northrop Insitruments. Flichmand HUI (ramnlo) SoUth Ea3t Chemicals & InSt. Ltd. & Systems Ltd. TAIWAN (R.O.C.) Ontario. Canada L46 IE7 Victoria Centre, 41F 459 Khyber Pass Road Kohan Instruments Co. Ltd. Tel: (416) =-4111 No. 4. IS Walson Road Private Sag. Newmarket P.O. Box 99-25 TLY-1 069"829 Causeway Bay Auckland 7F-5. 191 Fu-1-1sing, North Road Tel: 5-717201-6 To[: 545-065 Taipei (10441) CANAOA (Eastern) Tlx: 83661 Tlx: 21570 Tel: (02) 717-2003.4 Our-Pro Liao NORWAY UNITED KINGDOM 3070 Boul. de Rome Teknolab AIS SKC. Ltd. Brossard. Quebec J4Y IV9 P.O. Box 131 Unit 2 Tel* (514) 445-2356 Tlx: 05-268765 N-I"l Drdbak Stone Lane Industrial Estate Tel. 02/93 24 34 Wimbome, Dorsal BH21 IND 71x: 72727 England Tel: (0202) 841116 -9~k W4014fis ~ yeftntaftWOV Iii thrftqhW to waft& Tlx: 41589 but evireney auctmiene &w vn~si ziwvprV casts can enm uw hnd to" 78 ance's yaw beaten. co %~Cl BATCo document for Legal Services : Health Canada 19 October 1999 Index and Ordering. Information Pago Pogo Page Adapter KiL Detector Tubes 36 Film Solution ~ -25 Sample Sags 34-36 Air Flow Motors Filters & Accessories 27-29 Sample Tubes Air Sampling Guide 47-77' Gas Monitoring Badges 42-45 Sampling Related Equipment. Badges 42-44 GC Syringes 9 Air Flow Motors 40-41 Bags. Sample & Aere$=03 34,35 High Volume Air Sample Pump 37 Sealing Bonds 29 Battery Chargers, Pumps 10.14,23 Holders, Tube - Low Flow Pump 14 SOrbent Air Sample Tubes 34 Books 7 Holders. Tube - Universal Pump 22 Sorberit Sample Tubes Calibrators 24-26 Impactors 30-31 Sampling Accessories 7-8 Cascade Impactor 31 Impingors & Accessories 32-33 Sorbent Sample Tubes Cassettes. Filters 28 Liquid Badges 44 Analysis Accessories 9 Color Badges 46 Long Durttion Color Detector Tubes 10-11 Stopwatch, Digital 24-25 Color Detector Tubes 10-11, 311-39 Low Flow Pump 1243 Syringm GC 9 Compulef-Controlled Pump 16-17 Mercury Badges 45 Tandem Tube Holder 10 Cowls 26 Organic Vapor Badges 42-45 Trap. Impingef 32-33 Cyclones 29 Parallel Impactor ............ 30 Trap Sorbent 32-33 Detector Pump )(It 10.39 Phosgene Badges ::: 45 Trap Tube 10 DetectorTubes. Grab Sample 3849 Pneumatic Test 10 23 Tubing. Rubber 8.29 Detector Tubo% Long Duration.: 10-11 Pump Accessories 22-23 Tubing. Teflon 36 Developing Vibrator g Pump. Computer-Controlled 16-17 Tubing. Tygon 29 Drying Tubes a Pump. High Volume 37 UnKlersw PUMPS ......... 16-21 Element% Fixed & Variable Row 22 Pump, Low Flaw 12-13 Vial Racks 9 Pumps. Universal 16-21 Vials 9.32 SKC restem Ow rilpret to rno* avinote wencaa it~ nom ea any produM &w46 10 0 IFIN niUbdr. *Ac*m W 08@WL SKC done no anuffm any UDW &" am of ine of am of W" Prom W. As Patent rights nor the M;Ift of athers. T&PROMPT:St~VldE Orcier froni ihe source in your 43rea FOR ORDERING FOR TECHNICAL ASSISTANCE To piece an order, or forprice and avalWility informadon, ca/1 Our staff of Industdal Hygienists, Chemical Engineers and the SKCftadon or alsVibutorin your area for prompt service. Product Specialists will be happy to answer your questions on applications, procedures and SKC products. Call the SKC location in your area for prompt assistance. SKC. INC. SKC WEST 334 Vafty Vle- Read P.O. Box AIM Eighty Four. PA IS330-%14 Fudanon. CA 9293"133 T41100horm 14110 941.9mi T81M)h1XW 1714) 222-27W T.Nm 510497-33- SAN FRAHCMCO AREA Otgaidt, PA.- " 732-6472 Tokohomir IMM 22&4103 M PA' 1800) 242-1279 ALASX4 A HAINAN Teleekaftec. (734) 29ZQM SKC GULF COAST P. These Stat" Otter. ov Mtho'n 011,09 WA. OR. i1% UT. MV. AZ Ho%tslM TX 77095-SW Tewpnonat 78 70160whe (70) W94NO Ckateide Tit 414M 225-1W9 In TX- (140% ZZZ-7534 H LOUISIANA Aoooraanci~ VA 145n-2016 1758 Souww court 352-7149 Baton RaVe, LA 70511) T.1.1111-W. ", 2".. SKC AUTHORIZED DISTRIBUTORS ARGUS SUPPLY COMPANY MCP AMALYnCAL ORR SAFETY EQUIPMENT CO. P.O. am "o P.O. Box 304 P.O. Boa is'= MI ASM Newark. OE 19715 Loymille. XY 402yd (313) 7?649M VJ02) 3M74OO (= 77"797 SwvcinF 56--g: DoL~ ETA ASSOCUITES No. jentey Kw--Y P.O. am 13 Eauten P nsyn am Noratern 411inoet Honafdio.L KIA 02325 wash"Pon, D.C. (NO (6171 5VA544 OCCUPAT10MAL HEALTH ASSOMATES SCIENTIFIC INDUSTRIES SA-V P.O. SM 2117411 =7 Sk"011 A~ SL LCIML MO $3146 souide". co 8= Maine (800) ZIM9557 0= 443-7097 Ma"40%mits S----T. Ne~ KORIPO" An- Warld Wyaw 4~:b vennom ONAI'dom THOMAS SCIENTIFIC C=) souuwm Wk" P 0. am Smcftloowo. NJ -8005 79 C:) BATCo document for Legal Services : Health Canada 19 October 1999 ~tR z R 27-`, M, 7'. :4- ~~;s , " z'~* , --*,-~ V; RQ~ Zt as. CORPORATE OFFICES Belgium and Luxemburg Singapore M1111pore Corporailon Millipore Benelux SA-N.V. Millipore, Interlech, Inc. Ashby Road Hellotropes Avenue 1111030 Brussels c/o Waters Associates Pty. Ltd. Bedford. Massachusetts 01730. U.SA Tel. (02) 215.81LIS, Telex 22798 milben brub 187 Goldhill Shopping Centm Thomson Road 113Q Singapore Tel. Toll Free (800) 225-1380 BrAa In Massachusetts 1-(617) Z7S4= Millipore Industda e Cornercio Ltda. Tel. 251-Ml. Telex 36 031 watemrs Telex 92-34S7. TWX 71 ON126-1938 Caixa Postal 190M CFP 01000, Sao Paulo South Africa Tel. (011) 881.72.2ZTelex (11) 2507a mily br Millipore South Africa (Ply) Ltd. WESTERN DISTRIBUTION CENTER Canada 6 Kramer RoacL Kramerviile 2146 M90pare Corporation Millipore Ud. Transvaal 448 Granview Dr. 3688 Nashua Dri,.* Tel. SM-SOSO/3, Telex 4-2SIS7 South San Francisco. California 94080 Mississauga, Ontario L4V 1M5 Millipore South Africa (Ply) Ltd. Tel. Toll Free (800~ 227-0234 Tel. Toll Frw. (800) 268-4581 P.O. Box 1561. Bellville 7530 In California (800) 632-2708 In Toronto Area: 1-(416) 678-2161. Cape Province Alaska & Hawaii (415) 252-9= Telex 696 8513 Tel. 95-126liZ Telex 57-20 990 Telex33-1437 - Denmark Spain . DOMESTIC SUBSIDIARIES . Millipore AS Millipore lberica S-k Continental Water Systems Sygstubben I Z 295D Vedbaek Explanada 5. Madrid 3 El Paso, Texas Tel. (02) 89.3CLS5 Tel. 233.50.50. Telex 23 545 milli e Waters Associates Finland Millipore lberica S.A- Milford. Massachusetts Millipore OY Deu y Mata 104, Sa Iona 29 Puolikuu 3.02210 Espoo 21 Tel. 259.1&65 EUROPEAN HEADQUARTERS., Tel. (GQ 8&01.77. Telex 122 123 mipor sf Sweden France Millipore AS 43 Avenue de l'Europe Technical Assistance. Box 233. 42 123 V. Frolunda 78140 VeliZy. France Millipore SA Tel. 031/28.911601. Telex 21064 milipor s Tel. 3-946-97-49, Telex 698371 43. Avenue de rEuropm 73140 Vellizy M1111pore AS MANUFACTURING FACILITIES: Tel. (3) 94&97.4% Telex 698 371 euromil Pyramidvagen 9A. 17136 Solna Bedford. MA. U.S.A. Order Semce: Tel. 0&730.55.40 Cidra. PR. U.S.A. Millipore SA. Switzerland El Paso. TX. U.SJL Zone Industrielle. 67120 Molsheirn Millipore AG Jaffrey, NH, U.SA Tel. (88) 38 53 33 Telex 8W 457 F Schaffhauserstrasse 146 Milford, MA, U.S.A. Holland 8302 Klaten (Zurich) Taunton. MA. U.S.A. Millipore Nederland Tel. (01) 8141 3631M, Telex 56 067 milag ch Madrid, SPAIN Arnbachtstraat 6b. 3732 CN 09 Silt I.I.K. and Ireland Molsheirn. FRANCE Tel. (030) 75.47.44, Telex 70 212 miltb nI Millipore (U.K.) Limited Sao Paulo, BRAZIL Italy 11-15 Peterborough Road Millipore S.p.A. Harrow. Middlesex HA1 ZYH SUBSIDIARIES Viale delle Regioni 26-2& 20090 Segrate MI Tel. (01) 664 54 9% Telex 24 191 milpor g Tel. 2-21.30LB41/5. Telex 312 264 Milsipa I West Germany Argentina "Ilipore S.PA M1111pore GmbH Millipore Argentina &k Montevideo 49E Piso 9.1019 Buenos Alms Via Livorno 63. W162 Roma RM SlemensstrAsse 2M 607a Neu-Isenburg Tel. 40-4017/18.49-3643. Telex 21528 Tel. 06/4ZSZGI - 4Z53.75 Tel. 0 61 OZ128 94, Telex 417 668 mil d In - . jaw In all ot1w countrim, Austral Millipore Ply. Ud. Nihon Millipore Ud 16111111pore Intertech. Inc. 5. Lyon Park Road, P.O. Box 303 4-1S, I-Chome. Shiroganedai P.O. Box. 256 MInato-Ku. Tokyo 108 Bedford, Massachusetts 01730, U.SA North Ryft N.S.W. 2113 Tel. Inwats: (OW) 222-111 Tel. (03) 443-4514, Telex 24 948 milipor Tel. (617) 275-9200. Telex 92-3457 In Sydney area: (a2) 887-122Z Telex 26 M Mexico Austria Millipore S.A. do C.V. Waters Ge3. m.b.1-L Avenida Ingenieros Militam 85 I I Mexico 11230 D.F. Schonbachstrasse 13.1130 Wien Tel. (0222) SZ01.76. Telex 131464 wavie Tel. 576-96BIL Telex 1777 442 misa me Norway Millipore AS CD R 5- -N- Enebakkveien 135, Oslo 6 Cat. No. MC579 Printed in U.SA TeL (02) 67.SZ53 2182 Copyright61982 Millipore Corp, Seciford. MA 01730 un oi ON RY'- ow J-1 BATCo document for Legal Services : Health Canada 19 October 1999 R.J.Reynolds Tobacco Company Whs',.:)r.-S_=1ei-., N.C. 27102 IN nno February 23, 1989 To: Participants in the CORESTA. ETS Collaborative Study Program Dr. Gerhard Scherer - VdC Dr. Ed John -,Rothmans Dr. J.J. Piade - PH Europe Dr- Yoshiaki Ishizu - JT1 Dr. Dave Colby - B&W Dr. Chris Proctor - BAT I am delighted to report that the sample generation phase of our col- laborative study program has proceeded precisely on schedule. ETS was genera- ted and samples were collected in our environmental chamber February 14-16. The remaining days were necessary to prepare spiked samples, generate data reporting 'sheets for each laboratory, and to label and sort samples for ship- ment. As a result, samples were dispatched via air mail to you today. Enclosed in each package is an additional copy of this complete memorandum. In an attempt to ensure the utmost consistency among laboratories and thus ensure the utmost reliability of our collaborative tests, I ask each of you to carefully read and abide by the enclosed instructions in addition to the list of "Instructions to Collaborators" published by The Association of Official Analytical Clir6mists (AOAC) which I have also enclosed. Irk an effort to avoid confusion, I have, grouped specific instructions by method with some redundancy occurring. Also enclosed, please find a copy of the criteria which I have set for the evaluation of analytical results. While they may seem conservative in some respects, I assure you that we will need an extra effort from everyone involved to successfully meet them. Please convey this sentiment to your analytical personnel. In addition, I would like to emphasize that this ETS collaborative study program was designed and is being implemented as a study of three analytical methods being employed and not of the individual laboratories' performance. As a result, any biases observed in the results reflect differences in materials, instrumentation, and interpretation of the written protocols and not the capabilities of the individual analysts. It is still my hope that all samples can be analyzed and data reported to me by March 31. This will ensure that I have ample time to collate the data, perform the necessary statistical analyses, and generate a report prior to the June Task Force meeting in Madrid. As I mentioned previously, I foresee the successful outcome of our efforts leading to publication. In anticipation of that, I ask each of you to provide me with a list of the names (please include middle name or initial) of analysts from your laboratory who are participating in this study. U11 %-0 r%,) BATCo document for Legal Services : Health Canada 19 October 1999 Finally, I wish to express my sincere thanks to each of you for all of your careful preparation put forth regarding this collaborative study program. Fith the quality of work demonstrated thus far, I have no doubt that the out- come of our efforts will be most gratifying and somethimg of which we are all very proud. Good luck! Sincerely, Michael W. Ogden, Ph.D. Senior R&D Chemist xc: Dr. C. Green I 0, CD CN Un "0 BATCo document for Legal Services : Health Canada 19 October 1999 Instructions to Collaborators 1. Read the method carefully-, if you have any questions, check them with the Associate Referee before you begin the collaborative determination. 2. Make at least one practice run, if enough sam- 5-1e has been provided, or on your own sam- ples, to familiarize yourself with the method so that you can avoid errors in manipulations. 3. Make the determination as soon as possible ifier receiving the samples, since delay may cause the samples to deteriorate. Store the samples according to the Associate Referee's instructions. 4. When you make the collaborative determina- ,tion, FOLLOW THE METHOD EXACTLY IN 6VERY DETAIL. DO NOT INSERT MINOR MODIFICATIONS, even though they may be in common use in your laboratory. You will des- troy the value of the collaborative study if you depart from 'the instructions given in the method- If for any reason you are unable to fol- low the method to the letter, report the devia- tions to the Associate Referee. S. Report all your results, unless the Associate Referee has specifically instructed you other- wise. Do not take the "best two out of three" values; do not report averages unless you were asked to do so in addition to single results. 6. Make only the number of determinations requested by the Associate Referee (more or less data often complicate the statistical analysis). 7. Write a full report of your collaborative work, including all the data you obtained, and send it to the Associate Referee as soon as possi- ble. Include any comments, suggestions, criti- cisms, or description of difficulties that you feel are important. If you tried out a modification of the method, report your findings to the Associate Referee but submit these data in a separate report. Un ON V1 __0 .P-- BATCo document for Legal Services : Health Canada 19 October 1999 INSTRUCTIONS Nicotine Analyze each sample only one (1) time. If poor chromatography of a given sample results in a questionable determination you may repeat the analysis only until a valid chromatogram is obtained. 2. Report results onlyfrom a second degree polynomial calibration curve (both for desorption efficiency and analysis of samples). 3. Enclose a plot and the equation of your calibration curve when you report results. 4. Fill in all information on the enclosed three (3) sheets and return to me as soon as possible. Observe the convention used in the example on each sheet regarding reporting of significant figures. In general, report at least one (1) figure in excess of what is normally considered significant. 5. Save all original data (chromatograms, calculations, etc,) in case any questions arise regarding a particular sample. RSP 1. Weigh each filter pad five (5) times. 2. Fill in all information on the enclosed (1) sheet and return to me as soon as possible. Observe the convention used in the fxample regarding report- ing of significant figures. U_V_ 1. Analyze each sample only two (2) times. If poor chromatography of a given sample results in a questionable determination you may repeat the analysis only until two (2) valid chromatograms are obtained. 2. Fill in all information on the enclosed (1) sheet and return to me as soon as possible. Observe the convention used in the example regarding report- ing of significant figures. j~;b CD BATCo document for Legal Services : Health Canada 19 October 1999 COLLABORATIVE STUDY EVAIWIQN CRITER Data from this collaborative study will be evaluated by a 2-way analysis of variance (ANOVA) as described in "Statistical Manual of the Association of Of- ficial Analytical Chemists", 9. J. Youden and E. H. Steiner, 1975. Com- parability will be successfully demonstrated if the between- laboratory variance ratio and the laboratory- sample interaction variance ratio are both judged insignificant at the 950 confidence level. In addition, repeatability and reproducibility coefficients of variation will be calculated for each level of each analyta and overall repeatability and reproducibility will be calculated for each method. Regarding accuracy. the following guidelines have been set: Nicotine For spiked nicotine samples, accuracy should be within 15% of the true value at all levels. Particulate Matter For spiked particulate matter samples, accuracy for gravimetric determinations up to 20 micrograms should be within 50% of the true values and at levels greater than 20 micrograns should be within 20% of true values. For UV-PK determinations at all levels, the accuracy should be within 15% of the true values. I 0. .r-l CD Lfi Un %.0 C71% BATCo document for Legal Services : Health Canada 19 October 1999 to 0 0 CL CORESTA/ETS COLLABORATIVE STUDY -3 NICOTINE ANALYTICAL RESULTS (D 13-A.T. (U-K. and EXPORT) LIMITED r+ 0 PRIMARY PR I MARY PRIMARY NIC/GUIN PRIMARY 8ACK*UP BACK-UP BACK-UP wIC/GUtN BACK-UP TOTAL 70TAL NICOTINE NICOTINE QUINOLINE PEAK NICOTINE RICOTI14E NICOTINE QUINDLINE PEAK NICOTINE NICOTINE NICOTINE Q RET. T114E PEAK PEAK AREA WEIGHT RET. TIME PEA% PEAK AREA WEIGHT WEIGHT DESORPTION (microgram) SAMPLE ID (minutes) AREA AREA RATIO (micrograms) (minutes) AREA AREA RATIO (micrograms) (microgrou) EFFICIENCY (D.E. CORRECTED) "a ===--v ... Mm 2 ....... z.aw a 11 z = i (0 1 ....... w = w =__Q =_ 532- 1.99 3,t;y 0.~j (D t41A N.D 2 00 0 0 N _J~ 0 0 15)3)8~ - r4 .1D t~, 3t+ 0 0 _a i 3 A-2; -4,99 T W2 ";7?- 0. 01 0' 4 *~_~ 14 ~. 1,91 _0 (D 0 0 .6 1,4.3) il!, A_ - "D 3d. 0 ___0 0 UJA N-3~ ~,j 0 0 0 7 5.40 '.*3 3C 1613 a --- - OL 14 in 0 (D 9 57.31 3. 0g: 121ao 5' 91 - 0,03 0 0 10 0. O!g 3, ojq_ 11 15*.!9 0 1.;~ 0, 175 C) . 5 6 _-p C01) 0 0 NIft r4 :p It, py- 0 0 1-4 -2-91, 0 0 13 5-13 0-4-3 .44-1 10.1~!70 0-p- -Q 22- 14 X, ~ ur 0 NI , 0 .4 r4 0 0 0 1 12 0 - 1~:E D gq- 0.00 0.1 1!4 0 91) )7/3/8 16 0.~ja 0-S __0 0,184= - CL 17 -LYA - 0 0. 2) N.D 0 0 _wA ?4.D 3,vil- 0 0 0 - -1 15 =-32- 0.4k 2-atp O-If"2_0 0-f-3 .2-GR 0 19 "D C)o 40 0 0 r4-r2- -1.03 0 40 20 -:> - 37- 0 ~ 1-7 _).S(p ~ 0 1 I(As 0 .." a.* * ............... a EXAMPLE 1.52 rqL 12.82 220.53 0.0581 0.158 N/A N.D. 221.68 0 0 0.156 100% 0.158 0 ....... a we a ... ... ===.== = va mat Cr NOTE.' Please rtPQrt microgram nicotine to 3 decimal Places and 11/4 area ratios to at least 4 decimal places. (D (0 i I CID 6'q9 S I 10 I .0.** *® * ...... ........... . . ew.:- CORESTAIETS COLLABORATIVE STUDY *.:::: NICOTINE ANALYTICAL RESULTS ...... CALIBRATiom DATA TRUE wIC/QUtN NICOTINE NICOTINE NICOTINE QUINOLINE PEAK WEIGHT RET. TIME PEAK PEAK AREA SAMPLE ID (micrograms) (minutes) AREA AREA RATIO a . a . . ...... . . CALIBRATION STU 1 Q-0730) .42- 0.1-2, ~t:g~m .2. -01,?!; CALIBRATICN STU 1, 5. it 0,1013 -q,2~ 0.01 CALIBRATION STD 1 T-46 0 1 13L~ *tlis, a '0Z*- AV ERAGE ------------------------------------------------------------------ 0. fxi I CALIBRATION STO 2 f -,522- o -7j,5 CALIBRATION STD 2 04,41 14- :z3 C7 0. 0562. CALIBRATION STD 2 4 5- 3i,- AVERAGE 0. 0!;~50, CALIBRATION S70 3 'j, ~.R ^ - ;7,*- Q 4142.0 CALIBRATION STO 3 O,S,--I. 0 fli-a CALIBRATION STO 3 o -jtk2 AVER~GE ------------------------------------------------------------------ 0 - 1144 CALIBRATION STD 4 0. 1. 07 1 3-1 CALIBRATION STO 4 0 51~ 0 - 2-93 CALIBRATION STO 4 LgUL 1,~ 1 0.113 AVERAGE -------------------------- ---------------------------------------- 0, V11-i CALIBRATION STO 5 CALIBRATION SID 5 CALIBRATION STO 5 Z AVERAGE ---------------------------------------------------------- 0-55 EXAMPLE 0.0519 3.52 4.16 220.62 0.0189 NOTE: Please report microgrand nicotine and 11/0 area ratios to at least 4 declowil places. 0- -tC;?-.2,3,D€ -x-) 4 0-.11 lut '2 ŒDQ 0 CD (-n BATCo document for Legal Services : Health Canada 19 October 1999 .............. . . . . . . . . . . . . . . . . . . . . . CORESTA/ETS COLLABORATIVE STUDY NICOTINE ANALYTICAL RESULTS CALIBRATION DATA TRUE HICIQUIN NICOTINE NICOTINE NICOTINE OUIROLINE PEAK WEIGHT RET. TIME PEAK PEAK AREA SAMPLE ID (jaicrograms) (minutes) AREA AREA RATIO CALIBRATION SID 1 u.". C'~).C) CALIBRATION SID I S. :I, 1 0 .3,% 0. 01 CALIBRATION STO 1 .5-31 a.:. -2.'2 0, C-1 AVERAGE ------------------------------------------------------------------ 0 - C ir CALIBRATION SID 2 L, CALIBRATION STO 2 ~- > ( -'~Ci A CALIBRATION SID 2 6 S;3 0.(1:4 .2-10js? a 1. 216 LO AVERAGE 0. cf.~5 CALIBRATION SID 3 o - Wc~ ~i. -.~l 0 -St, 1 0- 1 U-4` CALIBRATION SID 3 0-ki,10) 3-3s 0 - CALIBRATION SID 3 -4,~3 ~ - 1 Cc7 0 - IQ AVWrZ ------------------------------------------------------------------- 0 - I 'i CALIBRATION SID 4 ;Z ~Llq 0. 3-~s CAL13RATION SID 4 0 - zQ, (-)-; CALIBRATION SID 4 AVERAGE ------------------------------------------------------------------ '7 CALIBRATION SID 5 -'~tL94 I - CALIBRATION STD 5 2 -7:i:; CALIBRATION SID 5 t7, (c%!,. oSL-a AVERAGE ---------------------------------------------------------- 7-: . . . . . . = . EXAMPLE 0.0519 3.52 4.16 220.62 0.0189 NOTE, Please report micrograms nicotine ard 9/0 are s..ratios to at Least 4 dacfzaL places. -D~jt, : I C'~- MC1JLL1 V~gO~ ~40T.", . '. -0.01 ak ( 17 -+ (L L,~ I dy = - 0. 002-1-t-~ -1- 3.25 75 oc T o 0 ,~./ V/ Z-37.3 :P-0 .2 1&1~ 1. Wei C-9 11 3,133 . .1 -/ 4S , 3-~, I 5*t.6z -^ 1~41C ,If - tj I' ok 1. 1%0 BATCo document for Legal Services : Health Canada 19 October 1999 31 ............ . . * * ....... COREST"ETS COLLABORATIVE STUDY ....... NICOTINE ANALYTICAL RESULTS CALIBRATION DATA . . . . . . . . . . . . TRUE NICIQUIX NICOTINE NICOTINE NICOTINE QUINOLINE PEAK WEIGHT RET. TIME PEAK PEAK AREA SAMPLE 10 (micrograms) (minutes) AREA AREA RATIO *Mau . . . . . . CALIBRATION STO 1 0. on 4~ - ;k~, 0 o? 1 3. Z 1~ '~a 0. C-~ I a.o~c CALIBRATION STO I - %. CALIBRATION STD I '. - ?-,-4 0.127 3-90~ o-o,213 AVERAGE C. 0i2c) CALIBRATION SID 2 17 57 10 CALIBRA710M SID 2 F 7-7-7- L-L-Cffio CALIBRATION STD 2 0 - 1'4--' 0 -C6 I AVERAGE ---------------- 2L CALIBRATION STO 3 C - IL4-; CALIBRATION STO 3 n 7 CALIBRATION STO 3 G AVERAGE ---------------------------------------------- * ----------------- - 0. 1 L", CALIBRATION STO 1. CALIBRATION SID 4 o CALIBRATION STO 4 T) - -.I. A AVERAGE ................................................................... CALIBRATION STO 5 - i- if:zeo '5 1 - Ct.'r-t I o.t.L0) CALIBRATION STD 5 S-3 1. 17- L.- ~'; i 0 - 972 CALIBRATION STD 5 1.7-13 !2 .5 1., Lb AVERAGE ------ ------------------------- * ---------------------------------- ............. EXAMPLE 0.0519 3.52 4.16 220.62 NOTE., Ptease report micrograms nicotine and 9/0 arjw ratios to at Least 4 decimal places. 0 q~Avua, tyi2- T D '5, ~3 2, 43 1. 3~0 1. 4:77 3 ~; -32- 1.13S .1 2,073 .1-S113 2.,;17- 1 - GeV I. 4-~94- c), c) i -2>-L ~74- 3:, 1 0 0/~ ON 01, 0 058q- 4 _4-) - (0.0 3-S~g BATCo document for Legal Services : Health Canada 19 October 1999 I DIRC) ... ...... ................... CORESTA TS CMLABORATIVE STUDY NICOTINE AMALYTICAL RESULTS lb****** DESORPTION EFFICIENCY DETERMINATION * BLANK TRUE VIC/QUIN CORRECTED NICOTINE NICOTINE NICOTINE QUINOLINE PEAK NICOTINE NICOTINE DESORPTION WEIGHT AZT. TIME PEAK PEAK AREA WEIGHT WEIGHT EFFICIENCY SAMPLE ID (microgram) (mirutes) AREA AREA RATIO (microgram) (microgrants) M 4 . . --- - - -e . . . ..... . . 2*22=3.8 CALIBRATION SID 1 0. 101.~ '5- 0. 07f 1.911? 0.05-7/ CALIBRATION STO 1 3 IN AVERAGE ........................................................ .. CALIBRATION $TO 2 0.901 5-34 01/cg 605 CALIBRATION STD 2 '5 - 2-44- 0. 104? AVERAGE 7 CALIBRATION STo 3 0-S19 L -4T 1. -0. CALIBRATION STO 3 Z -L-a' 0. L';ro'l 0 AVERAGE -01=1-- CALI:RATIOR M 4 /a,./- i~- 0-430 1. qO& CALL RATION STO 4 Jul~- g;, ~- 1, (!10 0. Ar? AVERAGE 0-305 CALIBRATION STD 5 -2.07 -!LA4- 0, rsov 1.311 0. C- t,:~.G CALIBRATION STO 5 AVERAGE . - ............... D.E. I (LOU) 0.0914- 0-0 -2--shQ 0,0a6a 0 D-E. I (LOW) 0 - 01 0 - 11-~ 1 D.E. I (LOW) D.E. I (LOW) D.E. I (LOW) AVERAGE .................................................................. D.E. 2 CHIw t 0. 129 5-al 043 01 0.0,75 0 D.E. 2 CHID) 0. -f (7kj- D.E. 2 (MID) D.E. 2 CHID) D.E. 2 (MID) AVERAGE o D.E. 3 (HIGH) 5- ;3 0.119f 0-93Y- 1 0-1416-1 0,(W~ q D.E. 3 (HIGH) i -I A& j a -- U? U- I 177L;~- 0 4-71i I: 0.1. 3 (HIGH) c-l-Aa ):IE: 3 (HIGH) 0 3 (HIGH) AVERAGE .................................................................. D.E. BLANK 0 Pi - 0,~56 D.E. BLANK Pj A 1-j -1> D.E. BLANK t r4 - D al A K ..: :'LANK AA. RAGE = ............. EXAMPLE 0.156 3.52 12.63 215.93 0.0585 0.159 0.154 ga.7% ...... . ............ NOTE: Ptesse report aticrograms, nicotine to 3 decimal pieces and NIQ area ratios to at Least 4 decimal places. 12 r - 1- 2 c2k, Mu tbNC,-,CJ- 2t R ~ (OD, 0 tlicm.Srz t-rr. 1~t ) - 0 - 0 1? 3 4(-3-403 X ~~-O) + (0 - OgL~4 x ~ C:) 1"31 &f~- ~~ o,%3 6a4i sexch,~v jtx~yerc.~ - &,3 ,.0 ' * ) S,,jVjj ,Saj . (_n -141C - ..- C7% * I -C) ON lAscal E% ~ XA~ htba- W"w Out BATCo document for Legal Services: Health Canada 19 October 1999 I D~- pl~zt 1~31) S CO WETS COLLASCRATIV; ;TUDT ::::::: 91=INE ANALYTICAL RESULTS DESORPTION EFFICZENCY DETERMINATION . I BLANK TRUE NICIOUIR CORRECTED NICOTINE NICOTINE NICOTINE QUINOLINE PEAK HIC07INE MICOTI14E DESORPTION WEIGHT RET. TIME PEAK PEAK AREA WEIGHT WEIGHT EFFICIENCr SAMPLE ID (micrograms) Coinutes) AREA AREA RAT 10 (micrograms) (microgra.ats) M CALIBRATION SID 1 0-1,04+. CALIBRATION SID I o'l asi AVERAGE ------------------------------------------------------------------ CALI:RAIION SIC 2 1 19? 0-2 Lp. W~_ CALI RATION STO 2 1 . 9 -10 G - (-- 0 ). - g.oq AVERAGE -------------------------------------------- ..... 0. VS CALIBRATION $TO 3 5-1c, 0.710 6-3177- 0,(-A;,) CALIBRATION $TO 3 AVERAGE ------------------------------- : -------------------------- CALIBRATION STO 1. 6-15W4 0. 2-7 it CALIBRATION STO 4 5"'41 t. 71612 0. 7:t?o 0 AVERAGE -------------------------------------------- 7:7= CALIBRATION $10 5 .2.07 '7. 0 -7 - CALIBRATION STO S -ILL.2ALL I - I '1 2 - 2."A AVERAGE D.E. I (LOU) D.E. I CLOW) D.E. I CLOW) 5-30 01 61~ 010915 D.E. I (LOW) -.11 U- 0 0.044 6-42 0 go, 'TT- D.E. I (LOW) 5'. A f 0 - 0 Fab 0. 01 cll~- AVERAGE ------------------------------------------------------------------ D.E. 2 CHID) D.E. 2 (MID) D.E. 2 (MID) D.E. 2 (HID) 5-30 0-1<~3 A - 7-lu- 0.11.1 0 - .1-17- 9,7.9 D.E. 2 (MID) 5". -31 4- 5~0 0,0170 ~ 0. f-+O 0. 1z P-4'i AVERAGE .................................................................. D.E. 3 (RICH) D.E. 3 (HIGH) D.E. 3 (HIGH) D.E. 3 (NIGH) - E. 3 (HIGH) 6-wsl DAVERAGE ------------------------------------------------------------------ D.E. BLANC D.E. BLANK D:E: :LARK E D LANK 40. D.E. BLANK S',.3*)- C" ~170 -23 - 0 U- -1 0, . 0. n :3 0,0213 AVERAGE .................................................................. EXAMPLE 0.156 3.52 12.63 215.93 0.0585 0.159 0.154 98.7% NOTE: Pfease report micrograms nicotine to 3 decimal places arxi M/0 area ratios to at least 4 decimal places. 0 2 = (00. C) 9. ki- tr,~" ,- 0.01 '41C.0-r'-fc- -fr- 30+ (3-63~5y, Zaho)+ (O.:~3'74~ Lyl -ii5/ froa DAD Z.,Gk sac+~V4 xyiy"W f4Det'- W~t 1'1P6A%3 ".Vv2a solve-C(PsW C711 A-ev'trik Z-T~. XACD'L~ 3LaA ;r"-" -ev- 'V~'e '-n . 1-~L f"-41" ~~ BATCo document for Legal Services : Health Canada 19 October 1999 CL C EStA IS COL OR COLLABORATIVE S;UD *:::::: C EstA/ 1 RSP AMALYTICAL RESULIS .... O.A.T..(U.K..…nd EXPORT).%.IHIIED * 0 CD lot 2rid 3rd 4th 5th AVERAGE lot 2nd 3rd 4th 5th AVERAGE TARE UT. TARE UT. TARE UT. TARE UT. TARE UT. TARE UT. FINAL UT. FINAL WT. FINAL WT. FINAL WT. FINAL UT. FINAL UT. DIFFERENCE CD SAMPLE 10 (mg) (ma) (re) (M) (mg) Caitilorams) (ou) iCQ) , coq) (mg) (ma) imlitigrau) (mlcrograms) X v ne 9 o une*® ...... V.Oucunez c a un ........... BAT 1 ~5; - 0-4,se - b - &Qe -O-u… -0-4-15 -0-4360 ~ - 0 - wn - 0 -#4!~ -O-kv -0.4-31 -0-tt7~p 3. BAT 2 -~.O IL i 9 -Q-Oti~ -0.012 -0-cit> -0.012, -C).Qoo)O -0.01;k -0-01-% -0,012 -0-012 -c>.011 c>l;l 114- (0 AI 3 -0.0;ts -0-0>9 -0.p -o-015 -0.01 -0-0236 -0.Q,2~ -0.0 -… CD 2~Œ -C.Oa -0.0 :1. LF. BAT 4 Q. lj!k 0. lie 0. 44- 0. ttJ- P. fl%…. 0-111+2- -0. lb2- lgp®x 0. j(q~ 0. if.% .2. 16-L 0. ~6 4-8-0 2 BAT 5 0. tt>f. - lot‚- 0.104- 0 - %ci+ Q. i CL$- O~ 1 cq-c> -:Lcz -a I oc>. G D 2t>… ID 01-…0g 0 augo 0 -&~t 0.,ac>44. ci BAT 6 ~%k&% 0 0.,A4~% 0-14-3 0-3qq- 0.~lq‡ 0. jq6 0 - M54.>. S'il.% CD BAT -Q.Dal -0,231 -0-2.3L2. -0-1>8 -0.13ap -0.1 -0-12-413 %o(a - 4 0 BAT a C.':-rzo O-Z30 O-S30 ojao 0 -3 %QQ 0.382- 0.3t;t 0.19-% 0 -3Q,~G Z54. (- BAT 9 0. c>61 -0-9foo O-0W o. o.o(,oj+, c>.c>(oo 0-061 *,D[Rl 0,0(.10 c>.(. BAT 10 0- P711- -0. PYI 0-l"52. 0. #92- 0 - 0 - V*) Z2, C.;10>8 0, 2a2j 0 t a.04 0. 2 v;. 0,;k,>e 0. DLO(P2 1 ~j. G CD BAT 11 0 - -kf11~ p. es;2 0 asq 0-22Q “ -.1® .2tzua- 0,-290 0 0.189 0-mi 0.;Lgœl 0 , Dsq 0 0-8 RAT 12 - 0 -4,ai -0040-1 - 0 - t4->l - 0 - 1,c 11 -0-4ai - ~3 --vai - -®+10 - 4-1.1- -0.4al? -0,8 BAT 13 Oas~;' 0. 2:Œ<¯ 0 Oa5e 0 zs>-Q .0,2,S3 0 - 'jj~!2 0 .34p) 0 - L'œs 0-151 J'z 12- 9L. 2- A T 14 -O->09 -101 -0.;kol -0. 2¯01 -0. 2-p q 0. 1 *> -0,111 -0-IA -0. 13A -D, I%D -0.137 ;ri. f, C) :Ai 15 -0. -O*15(o - 0 - L4-SG - 0. tms -0-le -0-®~ - 0 .3 €,+ -0-3 -0,3 101 - Li. Cu BAT 16 077 -0.07 -o.‚~L; -0. -0-07-4 -0. oc:>C) -o.of,,o -O-gbo -C>.Om - 0. oir - O.C>5q 1-; o BAT 17 -0-'3!3-f -0-3 -O,3-Z?l -D~ -0.3ag -0., Q: 0) ~a4- -O.-ai!k -O-31~r -0.3)e 'J.0 Q DAI 18 LH.2- -0-Lill --0-4-12- -0-4-143- -0-44 -0. tg 1 IR -0,40 -0.4o2- -0-4vy- -0-4c -O-Li-o2- -0.4 8.6 DAI 19 o~IUQ 0.140 -0-140 0, P%q 0~ 13!œ p.1326 0 - 14-!j: 0. 1 W--j 0-146 0. I%elL o - itpr 5. & BAT 20 0 - 12A(> 0. r,(,% 0-OLI 0.0&? 0.0(03 O.C>,qro 0.0qa G>,aq 0. c>99 0 '099 0. Q2&0 30-0 Co m ® m m = . ...... EXAMPLE 25.128 25 129 25.129 25.131 25.130 25.1294 25.164 25.159 25.163 25.162 25.159 25.1614 32.0 0 ........ -*7 00-8e* '®' ' ' ' - -* """' ® "' "® - non 80, 0 ";;,.®,Ptease Io lemore docimt'ptoce thon t¯he®2bƒtonce'wiit'ruad ; P* PO Cr CD Co CORESTAMTS COLLABORATIVE SIUDY. UV-PM ANALYTICAL RESULTS B.A.T. CU.K. wid MUD L1141TED .UV-pM. TRUE jqJV-pMw &UV-PHM AVERAGE THBP EQUIVALENT TURP PEAK PEAK w-PM" ECUIVALENT WEIGHT WEIGHT AREA AREA PEAK WEIGHT (micrograms) SAkPLE 10 - Cug/4mL) Cist REP) (2rd REP) AREA (micrograms) (THOP EQ. x 81 .............. CALIBRATION STD 1 0 C~LL- 3-29 A64- 34/6-5 0 - :A62 5-30 CALIBRATION STD 2 xg 6-9r- /0-51 CALIBRATION SID 3 3~2 J5", 3-7- CALIBRATION STO 4 3.2-0 1 6177~ IG3S i 624 ~S- M - - -0 CALIBRATION STD 5 6-4-0 a I -;Cl~ 11947 (01 6013s- CAL18RATION STD 6 9.60 -+,B:z:5 9.1411 7S.2.9- CALIBRATION $TO 7 1,0 - 0c) a.2,13 1G. 139- 1,2~a SAT I 106 9,9 9+-5, 0,;L3~L- I-9to BAT 2 --------------- 77-- !)0 8,3,:!!r 01.Zt 0 1./09 SAT 3 --------------- 91 t 07, 0 C), 2S-f, a,o SAT 4 --------------- -2&LpG -~7 02-F 4-0- SAT 5 --------------- /&5a /&act IWO.< -,Z~G - 10 BAT 6 --------------- 86.5, 77-*- - R19-5 1 ~25!;k /-3, BAT 7 --------------- (Oc~.%R G 0) 3-6 (,?30-< 13, L-tO 4 00) BAT 6 --------------- S-15~0 . ~323 -0 1. C4-11 /3, SAT 9 --------------- 7A :57 0-iML- 1"3 BAT 10 --------------- S15-7 54- 1 092- 8 - SAT 11 --------------- I I ~; 9 2~ -3.2s-o Z-00 BAT 12 )193 )-74 0 0. 40 Z, 3-22-' SAT 13 --------------- I -f 0) 7- M:0- 3. M za 144- BAT 14 ---- ---------- a4,9 S ag-" ;291-2-0 5. U4& 6k, &AT is --------------- 70R,+- -Z-0o3 70ZF:?. ra. 8 fio-0)0 BAT 16 MO:)- ;Z-78 al?0-0 0-GI,5- 419Z BAT 17 --------------- 4-2 4- 4-1!~ - BAT la --------------- 5,:9" B1 . -6q-0 0. (M. SAT 19 115 , 8(0 too-!r a -:42 1 - ~M/- SAT 20 --------------- +Of 4-4-3 :T~c -u's-r4- 6 122 EXA14PLE 3847 3885 3866.0 4.530 36.24 0. OLt(IZ6 + 0. 00 1% 16 A' Do/. BATCo document for Legal Services : Health Canada 19 October 1999 Our Ref: CJP/MM/46M 28th April, 1989 Dr. M.W. Ogden, R.J. Reynolds Tobacco Company, Winston-Salem, N.C., 27102, U.S.A. Dear Mike, I am happy to enclose the BAT data from the CORESTA ETS collaborative study. Because of the use of certain analytical equipment in our laboratory, there is some deviation from the specified protocol. Hence, I also enclose my analyst's (Mike Bevan) comments on the way in Which the study was performed in Southampton. If you require anymore information, please call me. Otherwise, J look forward to seeing you in Madrid. Best regards. Yours sincerely, C.J. Proctor -C-…- CD E Cr% c::) (il BATCo document for Legal Services : Health Canada 19 October 1999 M, 0-yro-wkl"' ., to.-. -Colt ? LIP ~4 CCA ID JUQ CIV . C-0 LUC 4~- ? L~ & C-L t- ~ S, 0 1 cFTS Up- ? -7 4Y CD ~i-t.!CV-4-- UI ON BATCo document for Legal Services: Health Canada 19 October 1999 09/08/19M 15:2B RJR R&D 9J9 741 4682 P.01 "YELEFACSIAILE YEASSAISSICS 0 Q&DSciendc infomaLicxi Services Library ~n MJ P-SeymMs Tobw n bowman Cray Technic* Center DATE: 9 PRioury: 0: DIZ. /~OcM-71,' T FROM: NOTES: PAGES FOLLOW FRom(919) 741-4682 PLEASE AOMWLEDGE RECEIPT YOU! *-4 BATCo document for Legal Services : Health Canada 19 October 1999 09/0e/iSGS 15.29 R_TR R&D 919 741 4682P.e2 R.J.Reynotda Tobacco Company Wirston-Salem, N. C. 27102 September a, 1988 Dr. Chris Proctor BAT R&D Southampton Fax no.: 44-703780332 Dear Chris: Thank, you for your letter of August 23 in which you reported RSF and UV-PM results from the recent spiking experiment. I apologize for my delay in getting back to you; I've been out of the lab for several days and an now playing "catch up". I need one point of clarification on your results. You state that the UV-PM data have been blank corrected (avg. blank = 0.03 ug) but for the RSP I am not quite sure whether it was corrected or not. I assume it was not and therefore, I calculated the average blank (-1.4 ug) and applied it to each of your results (e.g., BAT #3.- reported value 9.5 ug; corrected value 10.9 ug). If you had already applied the blank correction, please let me know. You mentioned some concern over the quality of the RSP results. Strangely enough, I disagree with your conclusion. With the exception of BAT f16 (474 error), all of the results you reported fall within the range of acceptable measurements (within 30t for values <.,20 ug and within 20% for values > 20 ug) . Your effort in this first trial run is better than many laboratories can demonstrate after several years of experiencel As far as suggestions for improvement, barring mechanical malfunctioning of the balance or the balance being located in an extremely "active" area, I have only two. Static electricity and humidity control are the only factors normally encountered which will cause trouble. Static elimination is by far the most dif- ficult to accomplish and, of course;*is potentially the most dis- astrous. Enclosed is a copy of a letter sent to 7.,T. Piade describing the unit we use. Regarding humidity control, we condition all filters for 24 hr in a small humidity chamber (ca. 50* RK, described in the written protocol) prior to obtaining the tare weight and again prior to obtaining the final weight. Significant drift is a problem if the filter is left out in the room for too long during the weighing replications. For this reason, the filters should be removed from the humidity chamber one at a time and weighed as C) quickly as possible. This involves placing the filter under the ionizing unit for ca. 1 =in, placing the filter on the balance pan, taking the first reading after the pan becomes stable, im- mediately removing the filter after the reading and replacing un- der the ionizing unit while re-zeroing the balance, and repeating (4 times). .90 BATCo document for Legal Services: Health Canada 19 October 1999 09/08/19E38 15:29 R-IR R&D 919 741 4SE32 P.03 R.J.Reynolds TobacCo Company Meisltcn-Saalern. N C. 27102 (9',Oj -177-5G00 16N ma, .7une 27, 1988 Dr. t7ean-i.Tacques Piade' Philip Morris Europe 2003 Neuchatel Switzerland Fax # 38-312476 Dear J-J: Attached is information on the static inhibitors we use in the RSP determinations with tle microbalance. We obtain these items from Baxter Scientific Products. I contacted tha World Trade Office of the company (telephone no. 312-291-4100) and received the following tame and address of the Baxter representa- tive in Switzerland; Ms. Verina Glatz Baxter Industriestr 31 8305 Dietlikon Switzerland telephone no.: 1 833 3360 The instructions wit-'h this unit recommend replacement at 6-month. intervals; however, we replace them at 3-month intervals. If you require further assistance from me in obtaining these units, please write or call. Zt was good to see you in London.Take care. ^,Personal regards, Michael W. Ogden, Ph.D. Research Chemist (k.4 E CREVO a-70-k , I&. : -4t go 19.5 k-6 . -.2 * : a V Vt '. M Is jj I e I _~:& . W 40 - W i:s : CD -a "Mg-jed -7 .1 a : ir ; . E '*'r Z . rZ CD M r -2 = C-M-114#11 !"ci. "MAV5 e .1I='=Hj iN LrI U2 ON BATCo document for Legal Services: Health Canada 19 October 1999 09/08/1988 1530 RJR R&D 919 741 4682 P.04 As far as I can tell, your lab is ready for Phase 3 of the collaborative study. Unfortunately, several of the other labs are no so.fortunate. In the meantime, if you desire additional practice in the RSP and UV-PM determinations, feel free to send another set of pre-weighed filters. Practice is the key to con- sistent results with the RSP yrocedure. Let me know if I can be of any additional assistance. With all beat regards, ~~ael W. Ogden t. -pi. C) c-n 01,11 cy\ i CITAL P. 04 CD BATCo document for Legal Services : Health Canada 19 October 1999 BAT (U.K. and Export) Limited RESEARCH.& DEVELOPMENT CENTRE Regent's Park Road Southampton S09 IPE England Telephone: Southampton 40703) 782111 Telex: 477269 Fax: 780332 Rat.' CJP/MM/46M 23rd August, 1988 Dr. M. Ogden, R.J. Reynolds, Winston-Salem. Dear Mike, Re: Coresta Co-operative Study on ETS I enclose the following data regarding the spiked filter samples. Gravimetric weight No) UV-RSP (ug) Sample Code Observed Expected Observed Expected BAT 1 -0.2 Blank 0.1 Blank 2 -4.6 Blank 0.04 Blank 3 9.5 15.02 1.03 1.03 4 -2.1 Blank 0.34 Blank 5 9.1 15.02 1.17 1.03 6 1.2 Blank 0.36 Blank 7 14.6 15.02 1.04 1.03 8 44.1 45-06 3.00 3.09 9 95.5 90.12 5.93 6.18 10 124.7 120.16 8.08 8.24 11 95.3 90.12 6.15 6.18 12 50.3 45.06 3.11 3.09 13 26.3 30.04 2.03 2.06 14 47.0 '45.06 ~3.01 3.09 15 119.5 120.16 8.10 8.24 is 42.7 30.04 2.09 2.06 Blank 1 0.07 Blank 2 0.11 UV-RSP data is corrected for an average blank of 0.08 Vg (BAT 4 and 6 looked odd and so two additional blanks from the same batch of filters were run). We feel pretty happy about this analysis. The gravirrietric analysis, however, is obviously giving us more of a problem, particularly at low weights. We have noticed some drift in the balance. Moreover, although we condition filters for 24 hours prior to weighing, I think we may also be seeing some humidity effects (lab RH has been running around 271/o recently). C:) (JI C7% CN A Member of the B.A.T industries Group Regd. Office: P.O. Box 492 westminster House, 7 Mllbank. London Swi P 3jE. incorporated in London No 2-29762 BATCo document for Legal Services : Health Canada 19 October 1999 A~y advice you might have, Mike, would be gratefully received. Best regards. U. Proctor 0 I Jz~- (D (-n C7% BATCo document for Legal Services : Health Canada 19 October 1999 BAX (VIC and Export) Limited RESEARCH & DEVELOPMENT CENTRE Regent's Park Road Southampton $09 1PE England Telephone: Southampton (07031782111 Telex: 477269 Fax. 780332 Our ref: CJP/JP/46M 9 August 1988 Dr. M. Ogden, R.J. Reynolds, Winston-Salem, U.S.A. Dear Mike, CORESTA ETS CO-OPERATIVE STUDY At long last, I enclose our data from the spiked DAO-4 tubes. No results from blanks are enclosed, as these were used in some in-house validation studies. All data is from front section only. Both 073 and 074 were run for back-up secHon, but no nicotine was found on either. Apologies again for the delay. I B --A, T Best regards, Yours sincerely, 140. . ' C.J. PROCTOR (Dr.) Encs. C;\ A Mernberof the B.A.T Industries Croup G\ Regd. Office: P.O. Box 482 Westminster House. 7 Millbank, London SW1 P 3JE. Incorporated in London No. 239762 (J4 BATCo document for Legal Services : Health Canada 19 October 1999 Nicotine (pg) as per RJR method RJR Code No. 'Spiked'Amount Sample Amount % Recovery 065 1.93 1.66 86 066 0.64 0.62 97 40. 068 0.19. 0.187 98 069 0.38 0.345 91 071 0.19 0.171 90 072 0.38 0-37 97 073 3.86 3.28 85 074 3.86 3.77 98 075 1.28 1.135 89 076 1-28 1.14 89 078 0.64 0.546 85 080 1.93 1.74 90 -t~b CD BATCo document for Legal Services : Health Canada 19 October 1999 C 0 0 CP% Cn BATCo document for Legal Services: Health Canada 19 October 1999 - I OCIVBER 1987. BAT (UK&E)'STANDMO 14ETMDS. MM DEIERœ=ICN CF NICO= IN AfflIENT AIR. SUMARY. A measured volume of aar is passed through an adsorbent trap omtaining Tenax TA. The quantity of collected nicotine is determined by thermal desorption of this trap followed by capillary gas chromatography with mass selective detection. The base peak of the nicotine mass spectrum, m/z 84, is used for quantitation of the sample. APPARATUS. Perkin-Elmer stainless steel thermal desorpticn tube parked with 0.4 g Te-nax TA. MDA Ac=ibaler Model 808 pump and calibration kit. Pexkin-Elmer ATD-50 automated thermial desorption device coupled Pexkin-a-lmear Sigma 3 gas atograph linked to Ifewlett-Pack-ard Mdel. 5970 mass seleqtive detector. SBP-5, 30 meter 0.25um, capillary gas chromatographic column. REAGENTS. Nicotine (G.P.R.), minim3n purity 98% as determined by CC assa-y. Propan-2-ol (G.P.R.) Tenax TA 35-60 Mesh, manufactured by Chrampack. LFI cr, ON BATCo document for Legal Services: Health Canada 19 October 1999 SAFETY PRB=MNS. Care mist be taken when weighing out pure nicotine. Disposable gloves and eye protection Mist always be wom. MMUM I 1. Collection of the ambient air sample. 1.1 Preparation of adsor bent tubes. Adscm:bent tubes should be packed with conditioned Tenax using the Perkin-FJnw packing rig. Appr=nately 0.4g Tenax should be used in each tube, and every attempt should be mde to rake all tubes to a similar pressure drop. Before any tube is used to collect a sample, it should be rLm through the analytical procedure to ensure no background. If peaks are detected, then the tube should be repacked with freshly c=ditioned Mn=. 1.2 Calibratim of the pump. The MDA Accuhaler 808 is a low flow, fixed volume pump. Flow is determined by use of a critical flow orifice nozzle. The pumrk a2.lcws calculation of the total volume passed regardless of the flow restriction, var:Lat2.cns that will occur between sampling tubes. Calibration of the volume per stroke should be no at least cnce each week using the MDA, calibration kit. This simply involves scapling frcm a fixed volume sampling bag; the pump will stop wtuan there is no , , air to sanple, and since each stroke is indicated on a reter on the instrunent, it is easy to calculate the volume rer stroke. 0 1.3 Acquirincj a sauple. The adsorbent tubes a transported to the sampling s1te with both ends sealed with caps. At the site the tube is unsealed and one end connected to the pump by a short length of inert tub=g. The minber of strokes of the pump are recorded, and at the end of sampling the tube is resealed. If the sample is not to be analysed inmediately an return to the laboratory, the tubes should be stored under ze-fridgerated conditions. Samples should be analysed within 2 weeks of acquisition. t:b 0 01% BATCo document for Legal Services : Health Canada 19 October 1999 2. Analvsis of the samole. - 2. 1. Setting-up the analytical system. The ATD-50 Thermal desorption device should be set in Mode 2 with the following conditions ; Primary desorption time 15 minutes Primary desorption tenperature 150 C Split ratio 25:1 Box temperature 150 C Cold trap low temperatLire -30 C Cold trap desorption teaperature 220 C The cold trap contains approximately 10 mg Tenax TA. The SPB-5 capillary column is fed through a a heated transfer line maintained at 150 C in czder that the head of the column is positioned directly in front of the exit of the cold trap. Splitting of the f1w of Helium carrier- gas also takes place at this position. The column is r4=kLUy run at 140 C, under which conditions nicotine will have a retention time of the order of 8 minutes using a head Pressure bf 10 psi. After nicotine elution the column should be temperature ramped to 220 C in Order to clear any other collected a311POUMdS. The mass spectrometer is set in total ion mod with a multiplier setting of 2000 volts. A solvent delay of 4 minutes must be used whP-n running standards. 2.2. Calibration of the analytical systr=m. A series Of standards Of nicotine in propan-2-ol should be node fresh -in cOnCientrations relevant to the environment sampled and the volume Of air e-xMnined. Typically, a series of standards around the I ng Per mic=olitre cmumntxaticn are appropriate. Standards are intrcdUCed bY injection of 2ul Onto a clean sampling tube followed by the M=al analytical Procedure- Each standard will result in a response factor for the M/z 84 ion. This response factor should be cmsistmt across the range of standards analysed. -r-lb CD CN BATGo document for Legal Services: Health Canada 19 October 1999 2.3 Analysis of the sample. Each sample tube is heated at 150 C for 15 minutes with a flow of helium gas purgial the released =npounds onto the cold trap. This is the primary desorpticn. After 15 minutes, primary desorpticn is ccaplete and the cold trap is rapidly heated fran -30 C to 220 C lectranically (secondary desorption). - Mis, in effect, injects the sanple onto the ch=matographic column. The mass spectrcmeter output is a total ion signal against retention tke. Cnce the scan is omplete, the peak corzesponding to nicotine -is identified th=gh its mass spectrum. This mass spectrum must be checked against those acquired when analysing the standards to ensure that the m/z 84/133/162 ratios -are consistent. This then eliminates the possibility of high ocncentrations distorting the mass spectrum. The signal due only to the m/z 84 ion is then extracted and integrated. F= this the concentration of nicotine in the sample may be calculated frarL the response factor acquired frarL standards. Niootine level in sample (ng) = m/z 84 ion count for sample / PF where IW, the resPonse factor = m/z 84 ion count for standard amount of nicotine injFc~ (ng) The concentration of nicatine in ambient air is then Nicotine (ug/m3) = nicotine level in samDle (ng) x 1000 volume of air sampled Uitres) .Pb C711 cr% BATCo document for Legal Services : Health Canada 19 October 1999 October 1987. BAT(UK&E) STANDARD ME'=DS. UE DETEF142MMCN CF CARBON VZNCKIDE IN AMBIENT AIR BY MEANS OF PCRIAELE INSTRUENTATION. SUMMARY. Cazboa manmr-ule ray be measured in low ooncentratisms in ambiemt air by usuq a portable General Electric CO mcnitor. The device operates by drawriM the air through a filter before introducincj it to a electrocbemical, sensor. APPARATUS. General Eleclaic direct reading CO detector, Model 15ECS3CO3. General El ctric support console, Model 1-'MS2006. REAGMM. Gas standards contaiLing zero, 2ppm, 10 ppu and 50 pom carbcn monoxide. SAFETY PIMCA=CNS. Carbon monoxide is toxic! All gases should be vented into an exhaust system; particular care should be taken with the disposal of the standard gases. -t-Ii. CD C7% C> r\j CD BATCo document for Legal Services : Health Canada 19 October 1999 A PROCEDUFOE. I. Description of the monitor. This moni-tor contains a small pump that draws ambient aix through a filter that is designed to remove organics that can give responses on the sensor. Mis filter must be replaced regularly.. Me sensor itself is an electronically biased solid polyrer electrolyte fuel cell sensor. 2. Calibration of the monitor. It is essential that the monitor is calibrated each day using a range Of low :entration. carbon mor=xide samples. Standards may be antroduced. by filling 2 litre inert evacuated bags with each standard (zero, 2ppm, 10ppn and 50Mn) and in turn connecting the bags to the inlet of the monitor. Low concentration standards ray be produced using gas blending techniques if not commercially available. Instrument response is manuaLly adjusted. 3. Analysis with the =)nitor. The instrument gives a direct indication of the CD concentration, which may be rec=ded manually, or a signal way be taken into a portable signal recorder. The support console allows aquisiticn. of time weighted data. C:) VI BATCo document for Legal Services : Health Canada 19 October 1999 1 . F j ou&.®¯ a 09-XLOMU- ~@ October 1987 BAT (UK AND E) METHOD FOR PARTICULATE MATTER IN ENVIRONMENTAL TOBACCO SMOKE SUMMARY The standard instrument used in BAT R and D Environmental Tobacco Smoke (ETS) studies is the T.S.I. Model 5000 Automatic Respirable Aerosol Mass Monitor - "PIEZOBALANCE". The device is a stand-alone instrument capable of measuring and recording concentrations of respirable smoke, fumes, dusts and other aerosols in the 0.01 - 10 pm size'and 0.005 10 mg m-3 concentration ranges. A wide range of applications is possible due to the piezo-sensing technique used and flexibility of the internal microprocessor based electronic control. The instrument is thus-suited to the measurement of the aerosol mass concentration of environmental tobacco smoke on a continuous basis. PRINCIPLE OF OPERATION'(based an T.S.I. manual for the instrumentl (1) An internal vacuum pump draws aerosol into the Model 5000 at the rate of I L/min (liter per minute). Particles larger than 3.5 PM. deposit on the impactor; particles smaller than 3.5 pm pass through the impactor to the precipitator. In the precipitator, the particles are charged and deposited on the piezoelectric microbalance sensor, which is a quartz crystal oscillating at its natural frequency (Figure 1). BATCo document for Legal Services: Health Canada 19 October 1999 -2- As particles collect on the sensor, its oscillating frequency decreases by an amount proportional to-the mass of the particles. The frequency change is detected periodically by a counter and the reading is evaluated by the processor. When the measurement Is complete, the frequency change is used to calculate concentration, mg m-3, and displayed. (2) The Impactor As the aerosol stream is drawn into the impactor chamber, its velocity is accelerated by passage through a small diameter nozzle. This aerosol jet is directed at the face of the impactor head - the impaction surface. As soon as the aerosol jet enters the impactor chamber it begins to turn to follow the path into the precipitator. Large particles, due to their greater inertia, maintain their trajectories and strike the impaction surface, where they are captured by stopcock grease. Smaller particles, with less inertia, follow the flow and miss the impaction surface. Ideally, the impactor collects all particles larger than its aerodynamic cut-off diameter, 3.5 Um for the Model 5000, and passes all smaller particles, Due to the impj~rfect velocity profile at the nozzle and other fluid mechanics considerations, however, the cut-off size is not so sharp. Th. e impaction surface of the Model 5000 is surrounded by a..'lip" that is intended to reduce blow-off and thus sharpen the effective cut-off size. The metal tube connecting the impactor and the precipitator is used to reduce electrostatic charging and particle attraction and to stabilise the aerosol temperature as recommended by Daley (1). Ln N) (A BATCo document for Legal Services : Health Canada 19 October 1999 il -3- (3) Th6'Pr6cioitat6r The precipitator block of the Model 5000 is constructed of Teflon, an electrical insulator which is inert to most chemicals found in ambient air - motor car exhaust, for example. The size and shape of the precipitator chamber is designed to optimise the collection efficiency of the sensor. Because the sensitivity of the piezoelectric microbalance d6pends inversely on the crystal electrode area, the chamber has as small a diameter as possible. The depth of the chamber (precipitator needle point to sensor plane distance) is large enough to allow time for particles to become charged and precipitate, but small enough to maintain a stable corona current with reasonable voltages. Experimental results for collection efficiency agree well with detailed cilibrations based on electrostatic charging and precipitating theory. Since the precipitating chamber is made of Teflon, its inner surface carries a high surface charge with the.'same polarity as the particles, making deposition on the chamber walls negligible. The high-voltage power supplied to the precipitator needle 'operates at constant corona current assuring constant particle collection efficiency. The combination of flowing air and the electric field generated by the precipitator needle carries the particles to the electrode surface of the piezoelectric- crystal. The high adhesive force between the particles and the surface causes the particles to stick firmly to the surface. (4) The Piezoelectric Microbalance When a quartz crystal or other piezoelectric material is placed in an electric field, the crystal becomes mechanically stressed. Conversely, if a piezoelectric material becomes mechanically stressed, electric charges of like polarity appear on certain 4= surfaces of the material. ON cr% r%j BATCo document for Legal Services : Health Canada 19 October 1999 -4- Wh.en.a piezoelectric material is made a part of an electrical driving circuit, the. piezoelectric material vibrates with a precise natural frequency, depending on the orientation of the cut of the crystal with respect to the axis of the raw crystal and on the thickness and density cW the crystal. For a given cut, the natural frequency of the crystal depends on the mass of material that sticks to its surface. The addition of mass to the surface of a given crystal causes the natural frequency to decrease in direct proportion to this added mass. This is similar to the decrease in frequency of a vibrating mechanical spring-mass system when more mass is added to the system. The piezoelectric crystal sensor used in the Model 5000 is an AT- cut quartz crystal. AT-cut quartz crystals vibrate in the thickness- shear mode. In the fundamental thickness-shear mode, the vibrating node is a plane passing through the centre of the crystal between the flat surfaces of the p7ate-like crystal. No node exists on the surface where particles are weighed. Only the portion of the crystal between the electrodes vibrates. The sensor, therefore, detects only those particles that stick to the electrode surface. Particles sticking to the surface of the quartz outside the electrode area have a negligible effect on the,vibrating portion of the crystal and are not detected. A given mass of particles sticking to the electrode of a given crystal will cause- a downward shift in natural vibrational frequency. The simplified relationship between added mass and natural frequency for AT-cut quartz crystal is; Af (2.27 fO2/A) AM where: Af change In naturall frequency, Hz fo = natural vibrational frequency of the crystal, MHz A = electrode area of crystal, cm2 CD aM = mass added to electrode area, ug ; (31% (-n BATCo document for Legal Services : Health Canada 19 October 1999 -5- It the frequency shift, Af, Is sufficiently small in comparison to the natural frequency (typically Af is- less than 0.02% of fo), then af is a linear function of the added mass AM, given by Equation 1. The crystal sensor used in the Model 5000 has a nominal frequency of 5 MHz with 0.635 cm'aiameter electrodes. The theoretical sensitivity S - f/AM of this sensor is: S ='180 Hz/ug Since the frequency shift of 1 Hz can easily be measured with the frequency counter in the 5000, a mass as low as approximately 0.005 jig can be detected; The sensor frequency is effectively reduced to a more convenient range, 1-3 kHz, by electrically mixing the sensor frequency against a ieference crystal having a resonant frequency 1-3 kHz higher than the sensor frequency. The resulting mixed frequency is equal to the difference between reference crystal and senior crystal frequencies. The mass concentration is then calculated as: C Af/AtSQ (3) where: C aerosol mass concentration- mg/m3 Af mixed' crystal frequency over time At At sample time. seconds Q volumetric air sampling rate, m3/sec S mass sensitivity of-the crystal sensor, Hz/pg For the sensor described by Equation 2 with an aerosol flow rate of 1 L/min: C = 333 Af/At CD BATCo document for Legal Services : Health Canada 19 October 1999 Figure 2 shows the electronic b . lock diagram for both the prima" and reference crystals which are driven by separate electronic circuits. The frequen~ signals from the two driving circuits enter a frequency mixer that electrically subtracts the two frequency signals, resulting in a "beat" frequency. The beat frequency is'the output frequency signal of the piezoelectric microbalance. This signal is then processed by'the electronic microcomputer. The microcomputer processes the frequency, time of day and sample time as well as controlling the cleaning operations. Typical operation of the Model 6000 is such that environmental smoke is sampled over a 30- second interval. (6) Data Output The T.S.I. Model 5000 provides two independent methods of obtaining data output. The first is a self-contained printer mechanism that gives a paper copy of the various parameters, namely. 1. Current day and month 2. Time in 24-hour format 3. Concentration (mg m-3) I 0 4. Average doncentrati on (mg m-3) I 5. Average change in sensor frequency 6. Start frequency (Hz) 7. Frequency change over sample period A typical printout is giYen in Figure 3. The second method of data output consists of a range of analogue signal outputs for the various parameters listed above, together 6 with data-valid and cleaning-cycle signals. The output signal U1 BATCo document for Legal Services : Health Canada 19 October 1999 -7- wtll be the output associated with a manually selected parameter available from a key-pad fixed on the front of the instrument casing. These signals are interfaced, in the case of the BAT R and D instrument, to a Biodata amplifier/signal conditioner/ interface and finally ~id to a Sirius microcomputer, acting as a data logger/formatter. (7) Calibration Comparisons between the T.S.I. model 5000 results and other methods of measuring particle concentrations should be carried out as a means of cross-checking particle concentration. The primary check should be on a gravimetric basis. As a secondary check, a U.V. spectrometry method may be employed. EaCh method involves drawing environmental air through a Cambridge filter pad, at a known flow rate for a known period of time. Work at R and D has shown that both methods give similar 'results for PMWNF estimation. The T.S.I. Model 5000 is not normally calibrated on a regular basis, since the change in crystal frequency is proportional to the amount of material deposited over the sampling time. Hence any uncleaned deposit on the crystal which causes a lowering of the natural (clean) frequency is used..as a reference point for the next sampling period. (8) Portability The T.S.I. Model 5000 is not designed to be a portable unit for use in field experiments. Its size and weight dictate that it should be employed as a free-standing unit in a laboratory or similar environment. C:) r1j I co BATCo document for Legal Services : Health Canada 19 October 1999 However, a very similar, albeit much less sophisticated, unit is available for "external" use - the Model 3500 (Figure 4). It must be stated, however, that this model must be cleaned manually and does not have as wide a range of facilities as the Model 500n. The principle of operaffon is identical to that of the larger instrument, and gives similar results when appropriate comparative tests are made. REFERENCES 1. Daley, P.S. The use of piezo electric crystals in the determination of particle mass concentrations in air. Ph.D.,Thesis: University of Florida, Gainsville, Florida-9 U.S.A. (1974). No t on original: DISTRIBUTION Dr. R.R. Baker Dr. C.J. Proctor Mr. P.D. Case Mr. N.D. Warren File 46M NDW/JP/46M 14th October 1987 I CIS i r~j 1 1*-0 BATCo document for Legal Services: Health Canada 19 October 1999 0 0 CL 0 0 FIG 1. (D PRINCIPAL OPERATING COMPONENTS OF TSI MODEL 5000 'PIEZO BALANCE' PRECIPITATOR cf) IMPACTOR X Corona precipitation regi ion 0 ........... .............. . ..... ....... :11 ................ CL . - .*. " -* : -. -:.: ........... ........ .. . VACUUM Impaction F PUMP surface Cr Sensing crystal u to to I O'Ms 1 lot 0 0 0 0 FIG 2 Q 0 ELECTRONIC BLOCK DIAGRAM HIGH VOLTAGE (D POWER SUPPLY, PRECIPITATOR Di'GITAL NEEDLE DISPLAY CORONA 0SCIIJ- X CURRENT CONTROL LATOR 0 SENSING U Bo- *dRYSTAL UIXER PRINTER PROSSER 1. TOR (o Ei: 1 2 ; GEL HH PC 4HREEECE PREC 0 REFERENCE is a an 0 CRYSTAL u u L 'ROSSER 4 0 7 a9 cic CD N-a. 1 10 ff KEYBOARD I ov FIG 3. TYPICAL PRINTOUT OF RESULTS FROM TS1 5000 ^0 11 1645 0 .1131) 1) 0 (1 "30 2`3 09 00 IS C.0 I 1 1642'. 0 .08-3 1) .45-':-- 008 a 223 16 00 15 , 3 2318 CIO 19 20 11 1639 0 .105 0 .464 - 0 0 20 11 IJK2.6. 0 .111 0 .473n 008-5 2, P14 Mao " 7 P 0 1 E. CO I I 163a 0 . 088 0 .46:2 a 0 0 21) 11 16-1:110 0. ILI -5 0 .4922 008,31 2-3127 r1c, 19 25 E 0 11 16, 0 . 1' #8 0 .502 0 091) .2322 V C, 0- 20 11 16.'--'4 0 .122 0 -.5 12 a 0 0 92 232'a 00 22 20 If 1621 0 . 10 5 0 . 5-23 a 0 0 9 4 2 32 -' 0 0 19 `4 0 C, 20 If 1618. 0 .1615 0 .553-55 - 0 096 21-FE 20 11 1615 0 .144'0 .546 , - 0098 2:32:1? 6026 r- 20 11 1612 0 . 155 0 .552, 1- 0100 233, 1 D 0 i2 8 20 11 160 9 0.183 0,102 233-31 0033 0.211 0 fe,2 0105 L.33-2 0038 20 11 1603 0.222 0 .596 0107 2341 0040 20 11 1600 0 .2722- 0.6080 0109 234 1 0045 20 11 1557, 0 .322, 0 .62- 1 - 0111 2.",37 1." 0 58 20 11 1554 0.35.5 0 .6,22'. 0113 233,53 0064 20 11 1551 0.45.5 0 .642 - 0115 2382 0082 20 11 1 -548 0.566 0 .6Fr a 8117 2`1 , , 369 L) 10 DA 1111 TI CONC M., C AV--,r SMI., --F M9/M3 M,1413 H Z 1-14. HZ- 20 If 1545 0 .661 0 .653 - 0 117 2389 01111, 20 11 1""42 0 .79.4 0 .6-53 - 0 117 2417 0143 20 If 153,9 1.027 0 .6477- 0 110, 2*.3?'--,1 0185 20 11 1536- - 1 .233 0 .62e. - 0 113 2369 0231 0 1 20 11 153.3 1.483 0.596- 0107 2397 026" 21) 11 1530 1.838 0.549, 0099 2-394 0':40 0.4.75a 0085 V, 0 45 4 20 11 1527 20 11 152-4 2.688 0 .354 - 0 0 63, 2.3,032 0484 20 11 152. 1 1.361 0 .209 - 0037 2365 0245 20 11 1518 0.977 0 . 1232- - 0023 Z-3353i 0 176 20 If 1515 0.072 0.0711, 0013 2349 0013 20 If 15120.083 0.071n 0 0 1 .3) 2-355 0016 . CD Ln ON cr% L-4 r,j BATCo document for Legal Services : Health Canada 19 October 1999 FIG 4. EXTERNAL COMPARISON OF TSI MODELS 5000 AND 3500 . " I= iff. HEIGHT: 771 mm WIDTH : 432 mm DEPTH : 380 mm WEIGHT: 48 kg MODEL 5000 .HEIGHT: 170 mm WIDTH 311 mm DEPTH 130 mm WEIGHT: 4.5 kg MODEL 3500 Jib, Cl) (Ln (7% BATCo document for Legal Services : Health Canada 19 October 1999 1. MER IN fihdil wn~R of i I top** filtv to 1.0 MI Podcti-N16 3. .5pi~E wit~ 9~1 i0tuRdl stp~pd solutioh 1-tPidCoRtmol ip 61. 1. Md ~. 15 1 fltac. 5. 1dP ~idlsj pldc~ ip U11trdsoRic Nb dt 317 fop] Mih. 6. Eid opdt~ to 6pjuss, N61i N2 P'Uppi 1. ~~j JNflj pjlnib~, IN)I-EIR A S~di~ to mix. 8. Hodt dt 1A for ] mip, 1. Pd,hsfor to dutomplop Vidl, ipjnt opto E wit~ cibcp ~ F19 op E [SA d~tpctioi. -ex. CD Ln ON ON L14 4bb BATCo document for Legal Services : Health Canada 19 October 1999 GAS EMOMTOGRPHIC COUTIONS DPILLMY COLR-l me 0.53 tml i. d. fused silica coated with-0.05 PM film of U n , " '1-2 pl for FIB, M pl for MS dete" flon -, okolum MORIMPH PAWTERS. Initidl oven temp. 100"C oven temp. program rate = 1060in Final oven temp. 300% I [run tile = 20 tin) FID telp. = 350% MS Nnsfor lipie temp@ = 310 ac Drrictf)r gas = He @ 0.5 psig (7 MI/min 100%] UNTITATION., internal standard method 5-point calibration curve (0.5 - 50 ng/pl solanesol) -- line8p regression CD 01% C.4 V1 BATCo document for Legal Services : Health Canada 19 October 1999 WAII-6 Visit BAT (U.K. and Export) Limited rogramme RESEARCH & DEVELOPPAENT CENTRE,. RRB/PMW/57 Drs C. Green, D.W. Eaker & M.W. Ogden (R.J. Reynolds Tobacco,ComRany, U.S.A.)- Tfiesda-y 19th January 1988 0942 R&D transport fr6m -Central Station - 1000-1015 Introduction to the R&D Centre' `Dr.' R.R.- taker. 1015-1145 Review of ETS Work Mr. P.D. Case (Lynwood Room) br-. C.J. Proctor Dr. D.P. Robinson Mr. N.D. Warren 1145-1245 Laboratory visits: Sidestream analysis Environmental rooms 1245-1400 LUNCH in the'Visitors' Dining Room Dr. R.R. Baker (10) Dr. R. Binns Mr. P.D. Case Dr. C.J. Proctor I Dr. D. P. Robinson Mr. N.D. Warren Mr. R.P. Ferris 1 1400-1500 _--Discussion of specific Mr. P.D. Case -1'echnical areas Dr. C.J. Proctor (M.W. Ogden and D.W. Eaker) Dr. D.P. Robinson Mr. N.D. Warren Y>z~-'~iscussion of future ETS work, Dr. R.R. Baker CORESTA, etc. (C. Green) 1500-1600 NC Talk by Dr. Green: URRENTSTATUS OF ETS RESEARCH" (Sheridan Room) 1620 Depart R&D 1638 Depart Southampton Central 1748 Arrive Waterloo, London Distribution: CD Those involved Reception Gardner Merchant File-57 0N ON Q-j 0\ BATCo document for Legal Services : Health Canada 19 October 1999 7 R.J.Reynolds Tobacco Company wiiistw-Saiein, N.C. 27102 (919)'777-'jr)00 Charles R. Green 12 Principal Scientist InUj 9n Research and Developrnent January 25, 1988 Dr. Richard R. Baker BAT (UK&E) Limited R&D Centre Regents Park Road Southampton S09 1PE UNITED KINGDOM Dear Richard, On behalf of Mike Ogden, Dave Eaker and myself, I thank you for the hospitality extended to us by yourself and your colleagues during our visit to Southampton and later in London. we were voiry impressed with the SS and ETS research conducted in your laboratories. I personally feel that the BAT sidestream methodology will form the basis of the standard CORESTA method. From my perspective, the task force meeting was a success and actually accomplished more than I expected. Hopefully, the work can proceed without too many delays. We look forward to further cooperative and collaborative studies. Again, thanks for an informative and hospitable visit. Please call or write if you have any questions. Sincerely, u4L- Charles R . Green, Ph.D. GROUP R & D CENTRE I Revd: 3 FEB 1988 I- . .................................... .. ............ ......... .... ............ ... ... .................................... 2b. - 1 CD BATCo document for Legal Services : Health Canada 19 October 1999 Imperial Tobacco Limited /Limit6e 13 3810, rue St-Antoirte Street Montrial. P.Q. M4C 05 (514] 932-6161 P.O. Sox 6500 C.P. Mantrdal.?.Q. H3C3LB December 14, 1988 CablvMle 7elimp* Telex/TMex 055-60673 Fax (514) 939-0432 Dr. C. Proctor B.A.T. (U.K. Fc Export) Ltd. Research & Development Centre Regent's Park Road Southampton, S09 1PE England. Dear Chris, i have finally managed to decipher my notes on the papers fr= the TCRC concerning ETS. There is perhaps not as much detail as I remembered but then TCRC's are notorious for a lot of talk and not so much information. However you are welcome to what little wisd=. I can share. if Nigel or Nike have any problems with the method I faxed to you please give me a ring, If I can't answer the question straightaway, I'm sure I can dig it out. Please pass on my thanks to both Nigel and Mike for showing me about the lab an Thursday. It was much appreciated. Thank you also for your time it was a pity we didn't have a longer session. Best wishes for Christmas and the New.Year. Regards, .P…. CD 01% CD BATCo document for Legal Services : Health Canada 19 October 1999 - .-1 SUIMRY OF PAPERS CONCZRNTNG ETS MEASUREIUMS PRESENTED AT THE 42nd TCRC #46 M6 1-.40 COLLœCnONOPCA"ONYLCC?NIPCMDSINFWIItON?dENrALTOBACM SMOKEUSIN02.4-DINMOPHENYLHYDRA7JNECOATEDSIUCAW-PAK CARTRIDGES. %rScis rr r ~ Del -m RJ. Reyr" Toba= Cc4 Winum-Satem NC 27102 afaldr…ydesand = hu eximd for qidu mm dur- A mrch ci the Umm= av&MUe un d— me*M indintu:hc … bu b= Uud exumgrwcty Siam the 19W ibr "Ysis o(cutot*l emqmxulds> …im mcmdy, it bu =vMeqmdm in ficid smplint mono= esp=-n Flowevw. v®Y ƒcdc dm cW=dy c…iu M ebe :r= .- in cnvuomnmm This &bu= cUm =y bc due oe " lack. midi row. of a =4 &rmmedmd ub-yi compouade in dm awmunn®L A ma"d bas b= devck*M fir COUOCMM afcarbm avag" dlia Sqb.Pak - ~ - ', Ce& Tbe prcffli- or pmdumm usicg wbotics wM bc de=ibe& Cutmyl cf -V®~s -e-Y, -q- ytoxqo-A wotclxmmcuoy gi congoup… &nd a&pL&tim to mu C-f-b… mm cdkctcd by dmwing ak *acuth … 2,4 -DNPH cowed cutridge wi& U 1 5 imrm, ShydrumdenvafimmelusadudaimlyzedbyHPLJCwichrV'd.".ie-l~6 - Ibs cuLW las b= " lu gcx= qundUmin and quoamivc dm foe thr Kcnwc4 uden= Ut4Fcigv=r~ - wdl as =v" -,km brin& in ancavmrmx"chwiber. la adƒdoc4 dm mriJtsof > 0 ErS &W sudŒ- in resuwam ud affim wW be pmmted. 0 1 - Study Objectives: 1) establish benchmark for actual levels in ETS of formaldehyde, acrolein, acetone and acetaldehyde. 2) provide an objective basis for subjective comparisons i.e. irritation (?) 3) compare actual and regulatory le'Vels as given by NIOSH, OSHA and literature TLVIs. Method uses 2,4 DNPH derivatization. of HPLC UV detection at 365 nm. HPLC: 2 C113 columns in series Mobile Phase : acatonitrile/E.0 Elution Time : 45 minutes Gradient Flow Method appears to be a "miniaturization" of a standard carbonyl determination method. ITL method is a further modification of the standard method using & isocratic made and methanol/water as the mobile phase. Details are attached. .Z:…. L'hi BATCo document for Legal Services : Health Canada 19 October 1999 - Tested the method i. a. the collection cartridges for breakthrough in the environmental chamber - 2 sets in series. No breakthrough. - Presented typical results fromi an office study.- n Acetone Formaldehyde Acetaldehyde (pg/m) Non-smoker W :F9. 10 25.30 43.77 Smoker a 74.45 31.51 71.75 Photocopy Room 5 64.21 23.48 94.74 Outside at night 3 36.75 9.19 19.23 - No measurable acrolein. - No zero levels. Restaurant study showed expected increases at "Happy Hour"; no zero levels; and no increase in acrolein or formaldehyde levels over time. Comments: Typical RJR paper: clear, concise and relatively low keyed. So overwhelming amount of detail and precisely timed to avoid a large number of questions. No future work outside of simply monitoring levels was described e.g. subjective comparisons. However the assumption must be made that this will be one of their next steps also assum' ng that their ETS work will continue after new management comes in. 0 CD Ln 0% -t-IM CD BATCo document for Legal Services : Health Canada 19 October 1,999 - 3 - #47 447 2zW EVALUATMN OF NIC0nNE PASSIVE SAIaILM DEVICE FOR ESTIMAING - EXPOSURE M ENVIRONMENTALTORACCO SMOKE ch"i- IE2=10 Guy & Oldsker HL and Red C_ Comad. Jr, IL L Rerwids Tobamo C. Winsum-S&Iew. NC 27102 Nicotine is used by some mck-chn as a nowforeawimweend wbww MWM (EM because U u; tutiquemMindisamajarconstiumstafEM Ab byi:oUocdmoaXAD-4.msinioa,-pHnga6c-Wby gap--W pimp to dnrw air am 0 dhe I I b= The msjor disadvantge .(= g rysems is the weight of the: -.i sod bwomm Fusm Wpe samplers 4a sat re*Am pumps ardbommeswdif 410 am have this disadysmgL Elmizatmemw zi~s Agency (EPA) hu UndroaJopmeesafadad-ficed pwroe SIOR simmly for dig pwi)id expasuzz c(bdivicktals RavrPow wtvam Tat 2' ==ad passive s was pecked with XAD-4 resia and evalumW a a passive for Riciscim The Bow me 0 die was evalusted in an awimamcasal zhandw under amdZims sod desenrAned us be 71 Mgfid& Ibil 'a in apeet== *M the shearackally kuWWv&hPr_ The resula at the avaktatim ofs w-Aw atfactors potentially EN i gibe-lismMy 0(passive iM*A&RgssmpGngr=wd, dwing expoom and swage bility. In A"xim zesubs an p a aircads Cabins - Device is a series of plates and screens with XAD-4 resin in the center Dimensions: 5-6 cm diameier 2-3 c* thick - Flow rate actu ally 62.6 ml/min. - Principle of operation is based on Fick's Law X DA x C x t H = Wt. absorbed t = time D - diffusion cceff. A at cross-sectional area L - length of channels Passive sampler has a much larger coefficient of variation than an active sampler; 27.1 vs 2.69 The only coament arising from this was - therefore you need a larger number of samples when using the passive sampler(!) U-1 C7% BATCo document for Legal Services : Health Canada 19 October 1999 - 4 - Tested the passive sampler for various factors as follows. TEST LEVEL CONCLUSION 1) Orientation to flow: horizontal 0.88 + 0.32 no difference vertical 0.92 7 0.28 2) Exposure Stability : a samples for 2.a9 + 0.38 6.6 hrs.ETS no difference 8 samples for 2.92 + 0.58 6.6 hrs. ETS + 4 hrs. clean air 3) Sampling Capacity 8 samplesl 1.54 + 0.24 m= 3 hrs. 7.84 + 0.92 8 samplesl 6.30 + 0.68 no loss of capacity 6 hrs. on repeated exposure a samples first at 3 hrs. 8.24 + 0.71 followed by another 6 hrs. 4) Storage Stability : In . m. analysis 2.54 + 0.24 no difference between 14 days at RT 2.98 + 0.43 immediate & freezer , 14 days in 1.ar. :; 0.31 analysis'. freezer Higher level for RT due to nicotine absorption on the stainless steel screens & subsequent desorption. Modifying analysis to include analysis of screens in order to account for nicotine absorbed there. Typical results from aircraft study., Nicotine Level big/m:2) n max. min. S.D. Non-smoking 14 6.8 17.1 <1.8 5.2 Smoking 17 25 55.4 5.3 15.3 Ln r\j BATCo document for Legal Services : Health Canada 19 October 1999 - S - Comments: Probably has its place in ETS studies perhaps surreptitious ones but the C.V. is of same concern as is the limited (to date) determination of different ccr;K=dn - nicotine only; organic solvents may not be relevant. Also an imagined scenario comes to mind - a subject strewn with passive samplers (somewhat reminiscent of a Christmas tree) in order to monitor levels of different compounds. 0 0 -$t:- CD Ln CYN BATCo document for Legal Services : Health Canada 19 October 1999 - 6 - #48 Mg 2-M COU.EMON AM AMALYSLS OFSOLANESOLAS,% TRAM OF ENVIRONNtEMAkLTOBACCOSMOXF-NfichmdW.OrdmtndKadnnmC. Maielo. &J. RerxMs Tobacco Co- Winum-Satc…¯. NC 27102 U-ffled a C-45 isope=W …l=W. bu been idendfied as ihe major ==inwm et the ~"M phase o(rwimmmtd ut¯=mwke zero". air wt—ch miies M the col Ft fa= Ming pemad s=p—ng pim" wM be deso*e& Aficr RSP is dc=wined ;==Mun an Md dw mmc! is "ymd by tu chmemmography wM exm%Ddy 9w, thui-rdm wide-bm caoigny "mm 1 . ' witheidxrNmagxuzm*mormmsp=l ' 1 (SCU=d im Me&) detuxio& T%‹s mffl"be wu m1une m au =vumcm=at chambe wider coevoUed c"—m cfoembusdoc (candl= cd Mm, MW cigammsX vm—la—m I&M uumu*Dir, and mfacive bucidby. %WM —xb= dwicisacidcwp=2-3%byw‚ghtofRSPiotwabdouETS fmm=mwrcwcipmm Ccmxtumdy. doe soiwmsoMP wetsk mdo can bc und co, *ppomoa cool RSP into EU cd me-ETS comalutior& Tbca=zw miummi au idcil W= ot rM parfiWIM m= in Wcor oev—~zL 0 Same paper as presented in London in June. "9 3--.00 SMOES ONTHIE SOURCE AMRMONMENTOFVOLAIILE ORCIAMC 24DOOR - AIR CONTAMANM DUETO(UGAREMSMDKF-CeeilFfErtrsud Mkkad R. Gumiii. AzWy—W Chaniwy DwW=. Oak Mge Nid" Labcxmy. 09 Ridr- TN 37831 Da=…udm of *u pordoc of bxlooe aw ceaunun= contribLned by mba= combus" is … cmw=gFcubl=L A immberof methodt —r…u"g tneasww= ci carbort moe=…dc and bM bam cmpkrje& Cub= mon=kb stdtm Imm contribuom by Cam swams. bu bMe appƒ=nmcfodm guphucconsdmem bas bM inv=uple D" eico,3pmm tu Cb=--02>~ie amalyuz vme pesfamnd en ampki takea of expui = (sidcwum IR4F cilpnu =%cW in a SW rocm) for oemparison with samptes u&m Imoe tu" mvvommnm cw4mmnmz or -cd comme= in duemmtt®tal "Usph" -- comli-A mlurn to the C&Q&" gts pbau Œ commncom lhesc facon ®M dm a‡piwd il… Othe or-irmomm based on ft I tonomawm'L &M m, p-zylents in esavuomemm of ‚ mskk=. ftsmumu. vd bowrmg &Dey vme 5& 43. and 4M 9129. and 49%4 and M 42. nid 1%. rutpectivdy. Pytmie indkaoed 6L 45. vd 455n IM 32. and QS, wd X 3& and IS, rcspecuvdy. Isobwymmuft indkucd 7S.53~ juwi ¯%, M 47. and 319k; Aitlm*theyi"wilhamaiWeu ' ' vnmcmnnxiybigb 0 br dm rcsuu= sUrdospbem &… ether appuconnma wem, mm numunaWa di= vaim obuined bued Abstract says it all. Used a triple sorbent trap: tenax + carbon + ? Thermal desorption/GC to analyse Basically a lousy paper - conclusions did not fit data and only summary 41- conclusion give was vinylpyridine & picolene correlate best with ETS VOC's, C) This paper as some relation to the EPA team study but the,connection was unclear. VI CN O's -9:A. 4z:b- BATCo document for Legal Services : Health Canada 19 October 1999 7 -rcpl C_ M 3M PMULTS PROU A MRVEYOP EN'MOE4MENTALTOBACCO SMOKE CM) IN PMAURANTS. f~nm,qp Nt Sue Imlao& lemiter ~& Jobuon, Richud K S&;~JT i~ey%:hia 5. %Idn…nt Lmllwd Restimb Cenur. 420 G 1 EngE* C d– g.®rmd by ibe fonawmt aheriw Division olmiturmi —m fond style ruetor= st rm foeL An=-= Slyir- ethnk etr- an QPCMY adopted ni policy, 2nd Unir®M di3cilm‚oc, of rescurau thmth= ft M. waccoueeedfor-ppmxkm Yeu bowwu itbancy-offlod ?WM~c mambtsy=m or PASS. Tbe umpURS pwqn woec cockscd in wh…: appears to bc sa ongnary kxftg Mcf‡= W-C-…dm ps dmampaphy and, I, - S speci& dc=cimL UV-PM wu n-ffl by lhe acalym of medmx…uc easc‚ess of ft RSP flu-don. Mm concoencens ne akadm M ud UV-PU wm U 64. $ad X 1 nW. MsPecrivdy. The in= CO cmmmd= wu 7-7 ppo. EUW=d ®Pou= ; Œ ¯ fta me" ai adne Vmi UV-PM rendu conne woeaOO49aridO.0014cit~ g equW&Imt pcr bour. n3pecd-ly, based open a 1986 seles %ocigtord 0 '‚quivalent ci gum" deUycring U mg micadu &rA 12M ost ®W'~ 1 1 Sampling: 42 restaurants over I month with seating capacity > 50 American 19 Fast Food 5 Ethnic 5 Sandwich 4 Pizza 5 Seafood 3 Steakhouse I - Random seating by hostess or geometric center of room. - Pass briefcase on a cbLir. - Noted the smoking behaviour of 4>ccupants (# of cigts.) the occupancy density the dimensions & ventilation (ACH etc.) characteristics. 2.5 pm cut off for RSP's. Results are log-normal distribution therefore used the geometric mean: Level (W) Rancre N = 36 out of the 42 Nicotine 5.3 1.6-3.47 VV_PM 26.1 7-172 RS? 64 16-255 co 2.7 ppm 0.9-6.3 Significant correlations (Pearson Ist order regression) between cigarette density and # cigts./hr. nicotine concentration un Cr" BATCO document for Legal Services : Health Canada 19 October 1999 - S - Further Correlations: M P n Nicotine and UV-PK 0.3849 0.013 33 cigt. rate density 0.4814 9.001 36 CO O.S835 <0.001 35 UV-PM and RSP 0.6019 <0.001 33 Ciqt. Densit and CO 0.2892 0.046 35 No correlation between nicotine concentrations and RSP, therefore concluded that there are alternative sources for RSP. Combined Office and Restaurant Stuj: Level (Ig/m3) Rance n Offices Nicotine 4.4 0.1- 69.7 151 UV-pM 33.7 12.3-447.9 161 RSP 123.5 15.7-623.2 131 Restaurants Nicotine 4.7 0.8- 34.7 160 UV-pM 41.3 12.6-258.6 169 RSP 99.2 15.4-853.3 170 Used typical assumptions: UV-PM = FTC tar - Breathing rate 12 1/min. SWAT equivalent cigt. - 12.08 mg tar Concluded the following: Office nicotine exposure: 0.0049 cigt/equiv/hr. (0.0009-0.02) 204 hours Office UV-PK exposure 0.0014 (0.0006-0.07) 720 hours Summarized as follows: 1) Nicotine is the best indicator of ETS. 2) RSP is not suitable as an indicator. 3) PASS system is satisfactory. 4) Smoking behaviour is equivalent across all samples. 5) Office and restaurants are not equal with respect to ETS. 6) Exposures are low. -c~;- CD BATCo document for Legal Services : Health Canada 19 October 1999 - 9 - Comments: Once again a typical RJR paper, although this time given by a Lorillard person No surprising results, in fact rather obvious ones in term of the Correlations. The Ottawa study conducted by RJR was included in these results but the RSP and perhaps the UV-PM (if they did it) were ina~curate in the Ottawa study and were never reported. This is reflected in the different samples sizes (151 ve 161 va 131). However, if 161 is thq total sample size including Ottawa where 30 offices were studied thee would appea to have also been a problem with nicotine, assuming the same offices weA excluded from RSP as from nicotine. 0- CD BATCo document for Legal Services : Health Canada 19 October 1999 - 10 - ~ #51 M 3.40 RMULTSFROMSURVEYOFMfVMONMENrALTOBA=SMOKEIN PASSENGERCABINSOFB747AIRCRAFr.€oUL2,Qld—ctUMcl-®i-W. SancUL ud Red W. C®ai& Ir- Rcm=b … Deve4me=. Bowmu Gmy Tu*r" Ceim. RJ. Rcyn" Tob…= Ciimpany. Winmn-Sab= NC 27 10Z Rob= A. Fcn=. John 0. L-phucit. P. Gleu B…M Jmoy Ly=-Hm. and Mihoe L Purith, Reseamb A DcwJ‡ - 14 Philip Merr;3 USA. P. 0. Box 2658X Rmhmm& VA 23261 Nfusum=nu wut mode tis pasunM u)iv® ofBocing 747 litCr…ft ce Iboe Gights cmm=g New Yeut. Tokyo. and =4Kcng in ordff to estimate du expouxes ofpaumt= in wkkbodied a—cmft toenvimwxr.W uneloc mm lutd W wen ta effeclivem scpcpwa es … Mc= tmduciagrmunM eitpommtDEM Pocmbic…rsmspbng vme -Ployed to i[= tmerated smVla for -. . % s conmtm&m W si paffigkz (RSP). and uwww" pardculm muter(UV-PNL a meam PMviding an umxr es—mm of *c RSPwasdem--v...--y. V-Mwu bycmozctiagibecogemdRSP—m-,f---,Imdmez=g 'dl in abs®ba-~s*dm 325nia Meta cois=mlmas ofnwouar- RSP, ud Urvpm in nuo- Moel'; . wem 2X I& ad 12 "JW. tespec:dwcllr coerespor®Eng cwmustiom in swaking secdous wffl 13& 41. ud 34 n1W. respccdveiy. RSP wd UV-PU oDcccmmom %we tucntwiy equivakat SufLidcWy sipiUm cW&eom wert dwm bmwm cixcc=Mm --md in ma- mmkingumisimking the snmpdoein Md-ins ~Z tDETS. C€CWIMM based upoe nicad &W UV-goewcm Io* sa boe ov~g and sincking r-n=L 1 . two 0 *ace om*n et mapim… ku thm %hm usucia" Wgh amm smobas. Smoking Non-Smoking Sampling: 2 samples 5 to 6 hrs. each First Class 1 1 Business 2 2 Economy 2 2 - Collected all ci9t. butts Nicotine RSP UV-PM (SE & range/pg/=3) Results: Non-Smoking 2.0 (0.2-10.4) 11(2-82) 6(2-25) Smoking 9.1 (1.3-35.8) "30(2-140) 19(2-85) - Levels In non-smokinq indicate some smokers in ncn-smoking - Significant difference in smoking vs non-smoking~p < 0.0203. No difference between smoking section of different classes p > 0.1073 No difference between seating position within non-smoking p> C.S031. Assuming SWAN = 0.82 mg nicotine and a breathing rate of M l/minute Cigarette equivalents in smoking - 0.0053/hr. = 32 round trips non-smoking - 0.001/hr. Ul ON co BATCo document for Legal Services : Health Canada 19 October 1999 - il - Number of cigarettes per passenger per hour: Now York - Tokyo 0.28 Tokyo - Hong Kong 0.25 half of the level being used in Hong Kong - Tokyo 0.37 current estimation models. Tokyo - New York 0.25 Comments: A very public awareness oriented paper i.e. slick, conclusive, readily understood. Would make great headlines. No argument with methods, results or conclusions but the questions removin - how effective is the information? can its effectiveness be measured? Is it short or long torm? My answers would be most effective if at all as long term; influencing consumers - a slow process that requires repetition. Political climate in the U.S.A. might be more amenable to influence of this type than in Canada where the legislature as well as the Mealth & Welfare arms of the government are militantly anti-smoking. ~11 2~)_ I CMcB/kb cc: T.A. Smith A. Porter P.J. Du= S.R. Massey C. McBride Central File -t" (31\ BATCo document for Legal Services : Health Canada 19 October 1999 BAX (UJK. and Export) Limited RESEARCH & DEVELOPMENT CENTRE Regent's Park Road Southampton S09 1PE England Telephone: Southampton (0703) 782111 Telex: 477269 Fax: 700332 Our Ref: CJP/MM/46M P -0 28th April, 1989 Dr. M.W. Ogden, R.J. Reynolds Tobacco Company, Winston-Salem, N.C., 27102, U.S-A. Dear Mike, I am happy to enclose the BAT data from the CORESTA ETS collaborative study. Because of the use of certain analytical equipment in our laboratory, there is some deviation from the specified protocol. Hence, I also enclose my analyst's (Mike Bevan) comments on the way in which the study was performed in Southampton. If you require any more information, please call me. Otherwise, I look forward to seeing you in Madrid. Best regards. Yours sincerely, G.J. Proctor C-% C"N A Member of the B.A.T Industries C(oup Un Regd. Office: P.O. Box 492 Westminster House. 7 Millbank. London SW1P 3)E. incorporated in London No 139762 CD BATCo document for Legal Services : Health Canada 19 October 1999 CJPIMW46M 2-8th April, 1989 .1 Comments on the Analysis of Nicotine Nicotine analysis was carried out on three consecutive days as manual injection of calibration stds. and samples could only be achieved during normal working hours, hence the three separate calibration data sheets. The high column pressure required to obtained the approximate 5:1 split ratio occasionally caused back flushing of sample within the syringe when the needle entered the septum. The variability observed in peak area values within replicate injections during calibration did not affect the NICIQUIN peak area ratios to any appreciable extent however. When determining desorption efficiencies, twenty XAD-4 tubes, Lot No. 485, were broken open on 15/3189. In this procedure, three sets of live tubes were doped with nicotine, corresponding to the three low calibration stds., injected directly onto the front section of resin contained within each tube, i.e. 10 0 secondary std. injected onto front section of first set of five tubes, 20 W for second set and 50 ~d for third set of five tubes. No nicotine was added to the fourth set of five tubes required as blanks. All tubes were capped and stored in the same manner as actual samples, i.e. storage of labelled XAD-4 tubes in freezer until analysis. Nicotine determination began on the front sections of the spiked tubes approximately one month later (13t"9). It became apparent after analysing the first two samples of set D.E. 1 (low) that some-nicotine injected onto the resin could have passed to the wall of the glass tube or the back section of resin or both. A decision was made to extract both front and back sections together, which saved time whemmanually injecting, and also to wash the inner wail of -the empty glass tube with modified solvenL A larger volume of solvent was required to accommodate the amounts of resin and glass wool now present in each sample vial. From thp initial 75% recovery the desorption efficiencies increased to between 90% and 99%. A replacement NPD bead was used for the second batch of desorption efficiency determinations (19/4189). A more consistent set of data was obtained and I would strongly recommend the use of this set when correcting Total Nicotine Weights.' A12gar2tus: Perkin Elmer Model Sigma 2000 gas chromatography, equipped with NPD, and Sigma 15 data console. Column: 25 m x 0.32 I.D. WCOT fused silica capillary with 1.18 prn film DB-5 (CP-Sil-8-CB) from Chrompack. Uri 01\ ON Ln BATCo document for Legal Services Health Canada 19 October 1999 G.C. Conditions 1. Helium Carrier Flow: approx. 3 3 min.4 (0.32 mm ID) 2. Detector Flows: (a) Hydrogen 2 cm3 min.-' (b) Air 160 =3 min.` 3. Detector Temperature: 3001C 4. NPD Bead Current: 10 pico amps (low setting) 5. Injector Temperature: 250'G 6. Injection: -3 Id manual(split ratio -5:1) 7.- Initial Oven Temp: 150'C, hold 0 min. 8. Program Rate: S'C min.-to 180*C GG run time 6 min., NPD equilbration time = 2.5 min. TotalRunTime: 10-12min. Retention times under the above conditions are approximately: Quinoline - 4.00 min.; Nicotine - 5.30 min. Measurement of peak areas: Sigma 15 data console. Comments on UV-RSP Anglygis With the LC system currently in use, a certain degree of drift is apparent during each run. The 'Input Level' parameter, which is continuously monitored throughout each run does fluctuate and although slight, it will affect the integrated peak area values obtained from the lower standards more so than for the higher standards. lnordertobe6onfident of the mean values for the calibration standards and samples alike, it is normally necessary to average the data from five replicate injections as opposed to the one or t~o specified in the collaborative procedure. Apparatus: Liquid Chromatography System Comprises: Waters Associates EguiRment: (a) Model 6000A Solvent Delivery System (b) Lambda-Max Model 481 LC Spectrophotometer (c) Model 730 Data Module (d) 0.009 in ID Stainless Steel Tubing (-10 ft length) Ln ri BATCo document for Legal Services : Health Canada 19 October 1999 LC C-ond&-ns- 1. 1 LC Pump Flow: = 0.4 cm*3 min.' 2. Injection Volume: = 50 pI (MANUALLY) 3. Run Time: = 2 minutes 4. Wavelength Setting (UV detector) = 325 nm -0.55 minutes (UV-PM) Retention Time 5. Mobile Phase purged with Helium continuously. Peak areas measured electronically with Model 730 Data Module. 0 Is -z~ƒ CD C71, ~_n LM BATCo document for Legal Services : Health Canada 19 October 1999 0 0 CL . . t -A ; S 0 COR SIA/ETS COLI GOIATIV TUDY 0 NICOTINE ANALYTICAL RESULTS B.A.T. CU.K. and EXPORT) LIMITED r+ PRIMARY PRIMARY PRIMARY WIC/QUIN PR I MARY BACX-UP, :ACK,UP BACK*UP NICIOUIN BACK-UP TOTAL 70TAL NICOTINE NICOTINE QUINOLINE PEAK NICOTINE HICOIIN IC071HE QUINCLIME PEAK NICOTINE NICOTINE NICOTINE r PET. TIME PEAK PEAK AREA WEIGHT RET. TIME PEAK PEAK AREA WEIGHT WEIGHT DESORPTION (micrograms) CD SAMPLE 10 (minutes) AREA AREA RATIO (micrograms) (mirutes) AREA AREA RATIO (micrograms) (micrograms) EFFICIENCY (D.E. CORRECTED) 8.82 ................ a ......... :U. 1.99 .3~.t;* D.;gSj t'l-b $-. U CA 2 N v-0 a. 1>0 'n r' .1) 3+ 0 CD )5)3189 ik 9 0 - 3 ~~ -A -9R jjka2~ "'.41 0.05. 5.2~j O.C)l _0,o(4 .,q aj 0 4 tj,"b OIL 0 0 0 .3> 0 5 .2-90 0 am! 0 0 6 0 41A o3> 3.20 0 7 S-4-1 1-*3 .2 - 2 9 0. S,126 MIA N'D. :5.sl 0 0 1 riL 0 1. 1:, G 9 31 3.05, R.-Xo i,m(. (1-. ?,73 S,A( 0103 '15.Na 0. oc-S 3, 5jq_ .4t -40-f- 10 G - Z~ -1,13 0.1?5 0- SL9 t4ja " 3,P-2 0 CD NIA rc..p ~F- VV- 0 0 ~;."M 1-4 N qa a .4K X 0 0 13 t~"Al (-4-3 - % 0,1770 0,7580 M J2 g7 ..x7- 0 0 0 - SR r~l D ;LIT o .'r - 0 0 C) ::~ - 42 -1 -wr 0 - -0 - 17/3/8 is =2- _0114- -?-a+- 0-(41~A 0.15 r4,p 2.qz 0 0 0.1,9 16 5,--4; 0-%f3 .2.8-3 v-16q6 r4ZL- -,I.> 0 0 0. 11) 17 ___ " .1> 0 CL is 5,327 2-:40 a_-2_>L 0. tj ~A r4 ,~ -3 alif, Q 0 0 'R.at~ 0.162.0 rjj? .2. Go 0 0 19 0 .D --A. C>O 0 0 r4cb. A.03 0 40 20 5. 32= ox.?~ _.p.96 0.05') 0,19's t4b_- 3. 0;t Q ............. ........... z x.x9z&8 0 EXAMPLE 3.52 12.82 220.53 0.0581 0.158 H/A N.D. 221.68 0 0 0.158 100% 0.154 0 ... a ...... ....... ........... V.- ........ f-P 0 NOTEt Please report micrograms nicotine to 3 decimal places and U/0 area ratios to at least 4 decimal places. Cr to i I V9999110V I ...... . * . CORESTA/ETS COLLABORATIVE STUDY NICOTINE ANALYTICAL RESULTS CALIBRATION DATA ............. ~ 9) (.% ) TRUE MtC/QUIM NICOTINE NICOTINE NICOTINE QUIROLIUE PEAK WEIGHT RET. TIME PEAK PEAK AREA SAMPLE 10 (micrograms) Dairlutes) AREA AREA, RATIO CALIBRATION SID I ' 0- 09 34* 0 - 1"x CALIBRA710H SID 1 5. 3 1 0.10S. -q , 1)" 0 0-:L CALIBRATION SID 1 548 ( 11.3* 4!72.5- C c2~t'4- AVERAGE ------------------------------------------------------------------ 0-ax9l CALIBRATION SID 2 C2 0. CALIBRATION SID 2 '5 -'~ 7 T. 7 T 2 -IC. ~ G '120 3,9"' CALIBRATION SID 2 5--34 Q.^ NZ I -'~ L-M I AVERAGE ------------------------------------------------------------------ 0.0 CALIBRATION SID 3 0 .(4,ZV CALIBRATION STD 3 's. ts. F-57T T Tf~; 0 CALIBRATION SID 3 5 ;0 =.!Z A-744- 0 - W2 AVERj%GE ---------------------- Z -------------------------------------------- CALIBRATION SID 4 0. 0 CALIBRATION SID 4 C).=' 3~ 0.2M CALIBRATION SID 4 5.3-- /. ou 7 1, a- I 0.2-S AVERAGE ------------------------------------------------------------------- 0. CALIBRAT113H SID 5 0. CALIBRATION SID 5 1. =FL-F "2,77V 0 - .q-, 0 CALIBRATION SID 5 is fo:5, 2. 321q- o.5#43 AVERAGE --------------------------------------------------------- - --- - 0 -'55 70 EXAMPLE 0.0519 3.52 4.16 220.62 0.0189 MOTE., Please report micrograms nicotine &M NJO arts ratios to at least 4 decimal placas. 0, 0044 0,,~l 32 r wt C% (-n U-1 BATCo document for Legal Services : Health Canada 19 October 1999 > 0. 0 0 0 0 C M CO) i CD BAT REGRESSION EQUATION (NICOTINF-) i CD i 0.40- CDF CL C). 2 0 - 0.00 0.50 1.00 l.bo 2. C) 0 WEIGHT ( ug 9599stiov I ..... * * ..... ** . . . . . . * . . *.*".* . . W. ...... * COMMETS COLLABORATIVE STUDI .* ....... NICOTINE ANALYTICAL RESULTS ....... CALIBRATIOM DATA ****et* TRUE XIC/QUIH NICOTINE NICOTINE NICOTINE QUIROLIKE PEAK WEIGHT AZT. TIME PEAK PEAK AREA SAMPLE 10 (microgram) (minutes) AREA AREA RATIO CALIBRATION STO I !:%Z 4-2(0 CALIBRATION STO 1 0 . 1 c4j- 0.0", CALIBRATION BID I 2=9 Lt Q~ 0 AVERAGE 0 - C CALIBRATION STO 2 L12ii 0 -).Lr." ?I - (- k--Qf!~-q CALIBRATION STO 2 i & . ~<:; 0. o CALIBRATION STO 2 - " ~ < ~ ]" f-~ - AVERAGE --------------------------------- ; o. C?-~5 1 CALIBRATION STO 3 0 .4 U'Y" 0 - S-L" I ~! .01 , (I. I UJ11-% CALIBRATION STO 3 0- - CALIBRATION STV 3 - 5133 0 - wi3 C"11) 0 - ILI AVERAGE ------------------------------------------------------------------ 0. f 14-2 CAL182ATIOU STO 4 "1 -T; 0 L- - 3. X-3 CALIBRATION $71) 4 CALIBRATION STO 4 t AVERAGE ------------------------------------------------- ---------------- V. CALIBRATION STD 5 CALIBRATION STD 5 CALIBRATION STD 5 f"aL; - AVERAGE -------------------------- - ------------------------------ 0 -------- C, -,S(-r EXAMPLE 0.0519 3.52 Z.16 220.62 0-0189 .Vsxze~.* NOTE: Piense report micrograms nicotine and V/Q area. ratios to at teast 4 decimat ptaces. L ke ivitLo't 1. + 3.Z.137~ -x T 100/. 3,133 j L- ~L Kt ot. ~- 4 - C / !;- 3 " wic "r. rL I j f 24 4~2 F .1 r4 IA P-,., 7. V1 01% E3ATCo document for Legal Services : Health Canada 19 October 1999 49 0 CL 17 ca BAT REGRESSION EQUATION NICC)TINE CM~ 1.2- CD 0 lb CL lb -A 0.4- co - 0 0 cr 0,0 1 1 1 1 1 2 WEIGHT ( ug PS99stiop . . . . . . . . . . CORESTA/ETS COLLABORATIVE STUCT NICOTINE ANALYTICAL RESULTS ....... CALIBRATION DATA -)C -9 TRUE RIC/QUIN NICOTINE NICOTINE NICOTINE QUINOLINE PEAK WE I ONT RET. T114E PEAK PEAK AREA SWLE 10 (micrograms) Cminutes) AREA AREA RATIO CALIBRATION STU I kl CIZ? I CALIBRATION STU 1 CALIBRATION STU I I r,,7 3--goa 0-028 AVERAGE ------------------------------------------------------------------ (I CALIBRATION STU 2 -"2- 0. 1 1z ;z,17S O.N. 10 CALIBRATION STU 2 -:~I. 3. 17" 0 . ~06JQ (0 CALIBRATION STU 2 -.E3 I AVERAGE ------------------------------------------------------------------ D -.QkQ0 CALIBRATION STU 3 CALIBRATION STU 3 f - 2,2- 0 CALIBRATION STU 3 ~01 12 91 ~Z? 0 AVERAGE ------------------------------------------------------------------ 0. 1 LLIL CALIBRATION STU 4 Ll .---I rl -C- LA CALIBRATION STU 4 %) - CALIBRATION STU 4 1 - F)5~ L) - 413 AVERAGE ------------------------ r ------------------------------------------ 0 CALIBRATION STU 5 CALIBRATION STU 5 7. 75 CALIBRATION STO 5 AVERAGE ---------------------------------------------------------- -------- EXAMPLE 0.0519 3.SZ 4.16 220.62 0.0189 NOTE: PLease report micrograTs nicotine and X/0 are* ratios to at teast A decimat ptaces. LD tvte AVULJ, (06 C41, '5'33 2 - CC-3 1.39-- 1. 1+-7-13 1?- 2, 13S" 2.03 I-su-3) 1 4-M,57- c). c) 31 ~7 -f- Lt- '6 (JI too/" ej a, * ) 'Y~ - O~ - Un x .. 0 BATCo, document for Legal Services : Health Canada 19 October 1999 0 0 CL CD I A 00 (D BAT REGRESSION EQUATION NICOTINE 1,2- Or CL to 0.4- 0 0 0.01 cr i 2 3 4 WEIGHT ug 0999511op I I D1- AT-,iLt 1~3~ CDRESTA/ETS COLLABORATIVE S1Wy NICOTINE ANALYTICAL RESULTS DESORPTION.EFFICIENCY DETERMINATION . . BLANC TRUE RIC/QUIN CORRECTED NICOTINE NICOTINE NICOTINE QUINCLINE PEAK NICOTINE NICOTINE DESORPTION WEIGHT RET. TIME PEAK PEAK AREA WEIGHT WEIGHT EFFICIENCY SAMPLE ID (microgram) (minutes) AREA AREA RATIO (micrograms) (microgram) M CALIBRATION SID 1 0 -Ickl- 5- -AP CALIBRATION M 3 -6 - 0 7,71 11- - -+q 0 2-t AVERAGE ------------------------------------------------------------------ CALIBRATION SID 2 2--212-2- % - 2.,q 0. 14-.Uvq 0.01~1 CALIBRATION SID 2 G.(,)02- AVERAGE 0,05 CALIBRATION SID 3 0-518 5-7cl 0.-4161 z'; Sl 26 0 0 1,41', CALIBRATION SID 3 0 4-,(,A)(.1 AVERAGE --------------------------------------------- -------------- 0 If= CALIBRATION STU 4 1-01~ !;.I-?- I - -K-7,7-- 6,1btt 0. 2--f CALIBRATION SID 4 1- ft*4 RAZ3-10c AVERAGE 0 - U~ CALIBRATION $TO 5 .0-4 *9 CALIBRATION M 5 -.5 ;5 AVERAGE --------------------------------------------- ------------- D.E. 1 (LOW) D.E. 1 (LOW) D.E. I (LOW) 0 - 00N. -5 -30 0-fep 0 3. (66 o;~-97 0.1.).t 010 D.E. I (LOW) 5; - U) 0.11 Gf it 0 0. "g.?- D.E. 1 CLOW) 5'. -'-~ I :? .6to f.,2- AVERAGE ------------------------------------------------------------------ D.E. 2 CHID) D.E. 2 (HID) D.C. 2 (MID) O-C M-3 1 3 0. D.E. 2 (HID) 5-3.) 0. 1,; 2- 11-7.9 D.E. 2 (MID) 0 - 5:60 O'C'510 AVERAGE- --- -, -------------------------------------------------- D.E. 3 (HIGH) D.E. 3 (HIGH) D.E. 3 (HIGH) D.E. 3 (HIGH) 0 jo. 1,1!~ f 0-443%1 D.E. 3 (HIGH) L, 6'5 0 - I L7 A 0144~4& 0-*151 'f&,0 AVERAGE-1 -------- *011-1 -------------------------------------- D.i. BLANK D.E. BLANK D.E. BLANX D.E. BLANK .3. D.E. BLANK 0. 0-;,6 ein AVERAGE 0 0 EXAMPLE 0.156 3.52 12.63 215.93 0 .0585 0.159 0.1% ".7% NOTE: Piesse report microgram nicotine to 3 decimal places and X/O area ratios to at teast 4 decimal places. 100.0 9. .0.., 0) 41- 0 - 0 1-3 0 + 63 - ~10 Y, ~~C~ + 0 :~yn x CD s,. Ivex (p as~4 P-Ji5/ Frat' owD eyk-cte~ fucwfv W~g XA-0-4~ 36,4L re,,oe a. ---O~ CIN BATCo document for Legal Services : Health Canada 19 October 1999 . I ~~ Ay~j I D(~C) . . COLLABORATIVE STUDY CGv2jcorINE ANALYTICAL RESULTS DESORPTION EFFICIENCY DETERMINATION LA IX TRUE NICIGUIN JREICTED NICOTINE NICOTINE NICOTINE QUINOLINE PEAC NICOTINE NICOTINE DESORPT9011 WEIGHT RIET, TIME PEAK PEAK AREA WEIGHT WEIGHT EFFICIENCY SAMPLE 10 CmIcrograw) Cminutes) AREA AREA RATIO Cmicrograms) Colcrograms) (2) . . . . --X CALIBRATION SID 1 0. Ica 0.0-41 1. 91 & 0-2qall CALIBRATION Vo 1 0. 0C?.L L~a~: a,, -,D)7 Iiia_ ;73? AVERAGE . CALIBRATION $To 2 O ;LO! 5~34 ~L- 10-17 1. ow, o W CAL19RATION SID 2 0- /,2 ef AVERAGE .................................................................. 11 CALIBRATION SID 3 S-42-- CALIBRATION $To 3 17-2).3 1 - -1-4440 0. L701 AVERAGE ---------------------------------------------------- ------------- CALIBRATION SID 4 C7 0.141, CALIBRATION SID 4 L240 0,'ko AVERAGE ------------------------------ . . 0, 3050 CALIBRATION $10 5 0. silov 0, t- 1;:L CALIBRATION SID 5 o - AVERAGE & ----------------------------------------------- D E I CLOW) t 0-o9q- 5-. 32~- 0 - om< 0, 0'r-'62 0, 6"Pr t Ia's t 2-13w - D:E: I (LOW) 0. 0?-!37- 01,17511 0-00-0 D.E. I CLOW7 0. E. 1 CLOW) D.E. 1 CLOW) AVERAGE ---------------- - ------------- ----------- D.E. 2 CHID) t 0. N9 S7 al 0,063 0, LIJa 0. C-f-5 0 -x~q - . IA4-4 1 * D.E. 2 CHID)t I - S 117;- O-OSI 0-16ki- D.E. 2 ("to) D.E. 2 CHID) D.E. 2 CHID) AVERAGE .................................................................. 0' E: 3 CHIGIQ+ 0 * it -k*l 5. .2 3 0-1191 A, Ly- - - 04filL r),U&L - 179.1 . E 3 C" IGIII j 1-1 0,1&41 1-1,T) 0 It :V1 D.E. 3 CHIGH) t 0 1 1 7tk 1 0.11%4. D.E. 3 (HIGH) D.E. 3 CHIGH) AVERAGE .......................................................... D.E. BLANK 4( 0 k pj.to . 0.(,56 D.E. BLANK 0- 1 A --t~ . t> D.E. BLANK t -jj-*- r4 -V I. f -Nf;, C.E. BLANK D.E AVE~AIGEAKI ............. .............. EXAMPLE 0.156 3.52 12.63 215.93 0.0585 0.159 0.154 98.7% NOTE: Ptoase report micrograms nicotine to 3 dectmai pieces and N/O area ratios to at Least A. decimal, pieces. V = c2 "-1 04w ta)-o7. t-1LCVT,.S6 t~S-t. -0 -OV93 +~Z 4cG xi~q-L--O) +(0-C)gLPG x C) o-nJ 6"i sedc;rUr ic c,,3 U-1 s.-tv&,e maj 01% z -C) cn~ %A"P-~ tuj:4. ~vc.Skg~ Ot N.) BATCo document for Legal Services : Health Canada 19 October 1999 CL ** * * . 6 i 0 RSP AMALYTItAt RESULIS fu.x. end MORT) L11411ED loi Znd 3rd 4th $th AVERAGE lot ?nd 3rd 41b Sth AVERAGE 1 TARE Ur. TARE UT. TARE UT. TARE UT. TARE Wy. TARE WY, FINAL UT. FINAL Wy- FINAL UT. FINAL UT. FINAt UT. FINAL UT. DIFFERENCE m s¯N`LE (mg) cing) (MI 11 f gram) tam) (mg) (Mo) (mg) (log) traititurau) (elcruoror3) lm ue ........... ............. x ft.scuse-e. m.t.ze ... ® Bu ¯ BAT 1 -2.Ll 35 -0-4~-sE - 0 -O-t…‡ -0-435 -(.t&UO 0 - W33 - 0 - 113 -0,411 -O.tt3,o -o'ti SI& BAT 2 -0-010) -9.011) -1>0101 -0-21 -0.013 =-, - 0, Vf~L I& BAT 3 -O-fL;13 P;L 1~ - 0, 0.> 029b 0. P~1~ -0.0,2S -0.0 -0, - 0. 0~s BAT 4 -a. lick 0. lie ej4~ 0. Il%)- ilu- -0-19+-2- 0 - ib2. 0. l tp2. 0 - 1 f..>- 0. ti,% t f.-I BAT 5 0.10+ atipy- 0,104. 0- BAT 6 0. --4t‚®4 Q~,3…i3 0 - 'X 4-'A 0-3q-3 0. 1>."-kett‚ a Ci 7, O"Sq4. 0.'~qIz c¯ a.," L- P - mmi -M - -x BAT ? -.9_-jzm -C>-Xlj -9,23) - - (X L%< - 0-Wo -0~ 12p- -0.12JO -0-1 -0.1ffl 10(a - !t BAT a 0- >-zo D-7.3c> 0 - mQ -110 C>- jao 0 "1 mX3, 0. u% 0-387- L>'®M>,It't ZW 0.3~R3 0 - lq2.G U'… - (, RAT 9 0.061 0. v (-,,0 0,0W D-2~# 0 -0&0 0.0&.Y, o.oti“ o.o(.1 c>.O(.1 0.06-L- CP,2(al 0.0!Wto 04 CD BAT le 0 - 1,->j 1 0. Š‡~j 0 !>Z 0. j9j= 0-od~)7- 0 - 1 Ce 3et 0~;XD9 0 - xDt. - 0. 2 of* C> - xQe 0. X0 (,,œ ~ 144 lu it a. mf2 a. -œLZRL 0 laŒ 0 181 0-199 -0-lŠl -O.W 1 -0-4DI ~-3 -o -4> 1 -0.!—a2. -O.WLIS BAT 13 0,…!~€ œ4 4L 0_1~r…-D .0.&Sƒ 0-2,50 0-3e D.JS-A O-ls j *g - 2. IIAI 14 -01.401 -O.zc;,q -0.2.09 -0.2iig ~=C>,2A?.20 -0,1%fo -0,11*7 -0,8 -0.138 zi - La BAT 15 -0.4-S6 -O-esu -C~4-5;SR -2,3, tout e -0.,3e -O..;t -0-3 RAT 16 -0-077 -0. -O,c>'?66 -0,0~ -tl-oLc) -0,05 - 0,05q BAT il -0-337-f -0-31 -0-33-7 2ffl i-2r -0.&144. 931 - 0 BAT la -O.L"2- -0-491 -0-412- -0-44 -0-4119 -D,4D -0-44 -0.y. -0.4 8.6 lu BAT 19 0~l4<) 0.140 0-140 0 - '?2!j 0,112 0-1:~96 0,j~K 0, 1 kt 1,t 0. j~2! 0 - l~jm 0. S. Co BAT 20 0 - CG9 0 0.01-8 0-C&R O-C&S O.&L-80 O,Gqrp 0~œAR ... = * ........ ==mg 0 EXAMPLE 25.128 25.129 25.129 25.131 25.130 Z5.1294 25.164 25.159 25.163 25.16e 25.159 25.1614 32.0 ............. lu ...... ...... 0 NOTE: Ptease report average weights and the final dIfference to t mre cleCtoal place thon the balance witt rend. Cr CD œ999S [ 1 op 11,-~ CORESWETS COLLABORATIVE TUDY UV-PM ANALYTICAL RESULTS B.A.T. (U.X. and EXPORT) LIMITED -UV-PM- TRUE I-IN-PH-9 IUV-PM" AVERAGE THOP EQUIVALENT ?HOP PEAK PEAK "UV-PM1 EQUIVALENT WIGHT WIGHT AREA AREA PEAK IJEIGNT Cmicrograms) SAMPLE 10 cug/440 (1st REP) (2nd REP) AREA (microgramis) tTRBP Ea. x 81 CALIBRATION SID 1 0 5.211 346-5 0 , '7.2 5-80 CALIBRATION STD 2 1.22 1-314- /0-51 CALIBRATJON STO 3 !)2 1. 42)S-L 1 )9'. 3-;L- CALIBRATION STO 4 -) 0 61 -3L IGIS i&U-0 3-22(cl