Routine Analytical Chemistry Sub-Group Report Berlin 2016

Transcription

1 Routine Analytical Chemistry Sub-Group Report Berlin 2016 Coordinator: Linda Crumpler, Cerulean Secretary: Colin Sinclair: JTI UK (until April 2016) Thomas Schmidt, Borgwaldt-KC

2 1. To develop CORESTA Recommended Methods as requested by the Scientific Commission. 2. To maintain existing CORESTA Recommended Methods (CRMs) pertinent to analytical test methods related to tobacco, smoke, and cigarette components. 3. To check on an annual basis the CORESTA monitor test piece by conducting collaborative experiments. Objectives Production/qualification/testing of new CORESTA Monitor Test Pieces such as CM8 and CM IP2 2

3 The Routine Analytical Chemistry Sub-Group (RAC) is the second longest standing Sub- Group actively contributing to the work of CORESTA having been established in 1985 Currently the sub-group sits under the Product Technology umbrella however, because the group s remit covers test methods related to tobacco, smoke, and cigarette components we have over the years also existed as part of the Smoke Science Study Group Membership has grown tremendously over the years In 1999 around 25 participants was typical In recent years typically between participants have actively attended meetings or participated in collaborative studies, with more labs participating in the studies remotely Typically 2 meetings per year April 2015 in Lausanne, Switzerland October 2016 Berlin, Germany History Participants from tobacco manufacturers, cigarette component suppliers (e.g. paper and tow), instrument manufacturers, contract and Government laboratories 3

4 Recommended Methods N 5 Determination of Carbon Monoxide in the Mainstream Smoke of Cigarettes by Non-Dispersive Infrared Analysis (second edition) Sep N 7 Determination of Nicotine in the Mainstream Smoke of Cigarettes by Gas Chromatographic Analysis (second edition) Aug N 8 Determination of Water in the Mainstream Smoke of Cigarettes by Gas Chromatographic Analysis (second edition) Aug N 21 Atmosphere for Conditioning and Testing Tobacco and Tobacco Products (second edition) Aug N 22 Routine Analytical Cigarette-Smoking Machine: Specifications, Definitions and Standard Conditions (second edition) Aug N 23 Determination of Total and Nicotine-Free Dry Particulate Matter using a Routine Analytical Cigarette-Smoking Machine; Determination of Total Particulate Matter and Preparation for Water and Nicotine Measurements (second edition) Aug

5 Recommended Methods cont. N 24 Cigarettes - Sampling (second edition) Aug N 25 Ambient Air-Flow Around Cigarettes in Routine Analytical Smoking Machines: Control and Monitoring Aug N 35 Determination of Total Alkaloids (as Nicotine) in Tobacco by Continuous Flow Analysis (second edition) Aug N 36 Determination of Nitrate in Tobacco and Smokeless Tobacco Products by Reduction to Nitrite and Continuous Flow Analysis (third edition) Aug N 37 Determination of Reducing Substances in Tobacco by Continuous Flow Analysis (second edition) Aug N 38 Determination of Reducing Carbohydrates in Tobacco by Continuous Flow Analysis (second edition) Aug N 39 Determination of the Purity of Nicotine and Nicotine Salts by Gravimetric Analysis - Tungstosilicic Acid Method Nov

6 Recommended Methods cont. N 56 Determination of Water in Tobacco and Tobacco Products by Karl Fischer Method (second edition) May 2011 N 57 Determination of Water in Tobacco and Tobacco Products by Gas Chromatographic Analysis Dec N 60 Determination of 1,2-Propylene Glycol and Glycerol in Tobacco and Tobacco Products by Gas Chromatography (second edition) May 2011 N 61 Determination of 1,2-Propylene Glycol, Glycerol and Sorbitol in Tobacco and Tobacco Products by High Performance Liquid Chromatography (HPLC) (second edition) May 2011 N 62 Determination of Nicotine in Tobacco and Tobacco Products by Gas Chromatographic Analysis Feb N 73 Determination of Ammonia in Tobacco by Ion Chromatographic Analysis May

7 RAC Method Directly to ISO ISO 13110:2012 Cigarettes -- Determination of menthol in smoke condensates -- Gas-chromatographic method 7

8 RAC Method Maintenance Also as time marches on so does technology advancement, thus objective 2 requiring the maintenance and updating of analytical test methods related to tobacco, smoke, and cigarette components. As new instrumentation and techniques (e.g. introduction of capillary columns versus packed columns) become available to increase the robustness of analytical methods and/or to improve the limits of detection and quantification, the RAC has a responsibility to revisit methods previously developed for updating 8

9 Annual Testing of the CORESTA Monitor Test Piece The 3 rd objective of the RAC is stated To check on an annual basis the CORESTA monitor test piece by conducting collaborative experiments This is in fact a bit of a misstatement as the RAC is also responsible for the production of suitable monitor test pieces for the parameters Conditioned weight TPM Puff Count Nicotine Water NFDPM CO A few years ago the RAC was also charged with the production of the first CORESTA LIP Monitor Test Piece for Ignition Propensity Testing CM IP2 released for sale in

10 CM8 Production and Testing To date the RAC has produced 8 CORESTA Monitor Test Pieces for TNCO and 1 for Ignition Propensity Testing Both ISO and Canadian Intense Smoking Regimes have been included since 2009 (except for 2014/2015) for laboratory accreditation purposes 2016 Collaborative study on CM8 completed in spring 2016 Technical Report sent to the secretariat for distribution to the SC. The values obtained for CM8 are comparable to those obtained for CM7 and 2015 CM8 values in terms of repeatability and reproducibility 10

11 CORESTA Monitor Test Piece for all Machine Types CM CM CM7 2014/2015 CM7 2014/2015 CM CM8 Average Level Puff Number TPM Water Nicotine NFDPM CO Cond. Cigt Wt Repeatability [r] Puff Number TPM Water Nicotine NFDPM CO Cond. Cigt Wt Reproducibility [R] Puff Number TPM Water Nicotine NFDPM CO Cond. Cigt Wt

12 Documents Produced for the Production and Usage of Monitor Test Pieces Technical Guide No. 8: CORESTA MONITOR TEST PIECE PRODUCTION AND EVALUATION REQUIREMENTS (April 2009) Basis for ISO 16055:2012 Tobacco and tobacco products - Monitor test piece - Requirements and application CM8 - Use and Conditions (June 2015) CM IP 2 - Use and Conditions (April 2015) 12

13 Current RAC Activities Investigation of a GC-MS method for the determination of Nicotine Included various tobacco types and smokeless CRP s Study complete and technical report circulated to group for review and comment before submission to the SC Development of a CRM tor the Determination of Total Sugars in Tobacco Study completed and technical report circulated to group for review and comment before submission to the SC CRM to be written 13

14 Current RAC Activities Development of a CRM for Safer chemistry with regard to Total Nicotine Alkaloids by Segmented- Continuous Flow Analysis Study completed and results shared with Sug-group Technical Report circulated to the SC and Board Will be proposed to ISO as a replacement for ISO 15152: 2003, Determination of Total Alkaloids (as Nicotine) in Tobacco by Continuous Flow Analysis Improvement to CRM60 - Determination of 1,2-Propylene Glycol and Glycerol in Tobacco and Tobacco Products by Gas Chromatography (third edition) Study completed and results reviewed by the group at October 7 th meeting Technical Report and revised CRM to be written and submitted to the SC 14

15 Current RAC Activities Update to CRM62 - Determination of Nicotine in Tobacco and Tobacco Products by Gas Chromatographic Analysis Clean up method to separate the CDC MTBE extraction method from the Hexane extraction method and update chromatography conditions, i.e. columns NWIP 116 CRM for Determination of Menthol in Cigarettes and Cut Filler Approved by SC Work commencing 2017 Collaborative Study on CM8 Protocol to be distributed by end of November Testing Jan Feb 2017 Data submitted by mid-feb for statistical analysis 2017 Collaborative study on CMIP2 for ignition propensity 15

16 Future RAC Activities Production of CM9 5 million test pieces produced of CM8 and we have exhausted about half of that Our experience has been that it takes about 2 years from identifying a need and having the new monitor tested and approved for sale That means we need to identify a willing manufacturer and start the process NOW! NWIP 106 Approved by SC, to assess and compare different substrates for LIP/FSC testing Next meeting will be in Charlottesville, Virginia, week of May 1, 2017 at the kind invitation of Altria Client Services 16

17 Thank You To all the RAC members who have prepared and shipped samples and participated in our collaborative studies. And a very special thank you to the statisticians who help to analyze our data and give it context. 17