sub-group routine analytical chemistry (rac) · products by gas chromatography – reduction in...
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Kitzbühel, Austria
10 October, 2017
Sub-Group Routine Analytical
Chemistry (RAC)
Coordinator: Linda Crumpler, Cerulean
Secretary: Thomas Schmidt, Borgwaldt-KC
SC Liaison: Karl Wagner, Altria
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.
Production/qualification/testing of new CORESTA Monitor Test Pieces
such as CM8 and CM IP2
Centre de Coopération pour les Recherches Scientifiques Relatives au Tabac
Cooperation Centre for Scientific Research Relative to Tobacco 2 RAC SG Report
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Current Objectives
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Cooperation Centre for Scientific Research Relative to Tobacco 3 RAC SG Report
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New Objectives
With the reorganization of the Smokeless Sub-Group into the
TTPA – Tobacco and tobacco Products and Special Analytes
Sub-Group into SMA – Smoke Analytes Sub-Group, RAC is in
the process of redefining our objectives with more specificity
A small working group has been tasked with identifying these
new and more specific objectives
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 35-45 participants have actively attended
meetings and participated in collaborative studies, with more labs
participating in the studies remotely
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Cooperation Centre for Scientific Research Relative to Tobacco 4 RAC SG Report
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History
Typically 2 meetings per year
May 2017 in Charlottesville, Virginia, USA
October 2017 Kitzbühel, Austria
Participants from tobacco manufacturers, cigarette component
suppliers (e.g. paper and tow), instrument manufacturers, contract and
Government laboratories
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History - continued
Project 051 – Improvement to CRM60 Determination of 1,2-
Propylene Glycol and Glycerol in Tobacco and Tobacco
Products by Gas Chromatography – reduction in extraction
time
Experimental work completed
Technical Report & CRM in progress
Project 054 – CRM Total Sugars in Tobacco by segmented
continuous-flow
Experimental work complete
Technical Report & CRM in progress
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RAC Activities
Project 052-2 – CRM Safer nicotine chemistry by Cont.Flow
Analysis CFA (replacing CRM35) Replaced CRM35 with safer
chemistry
Posted on CORESTA Website April 2017
ISO/TC 126/SC 2 Resolution 86 made in Osaka ISO 15152
Alternative method
Submitted to ISO WG2
Project 054 – CRM for Total Sugars in Tobacco by segmented
continuous-flow
Experimental work complete
Technical Report & CRM in progress
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Cooperation Centre for Scientific Research Relative to Tobacco 7 RAC SG Report
SSPT2017, Kitzbühel - 171010
RAC Activities - continued
Project 056 – CRM for Nicotine by GC-MS suitable for ISO
Experimental work complete
Technical Report & CRM in progress
Project 057 – Revision of CRM62 - Determination of Nicotine in
Tobacco and Tobacco Products by Gas Chromatographic
Analysis
Revisions complete and reviewed by Sub-Group.
Ready for submission to SC/Board
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Cooperation Centre for Scientific Research Relative to Tobacco 8 RAC SG Report
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RAC Activities - continued
Project 103 – 2017 CM8 Collaborative Study for TNCO
Work complete.
Technical Report approved by SC and Board
This year there were 32 participating labs using 45 smoking machines (24 rotary and
21 linear)
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ISO smoking
regime
Year 2008 2010 2011 2011 2012 2013 2014 2014 2016 2017
Test piece CM6 CM6 CM6 CM7 CM7 CM7 CM7 CM8 CM8 CM8
Average
TPM (mg/t.p.) 17.54 17.37 17.43 16.37 16.28 16.16 16.15 17.57 17.33 17.37
WATER (mg/t.p.) 1.87 1.81 1.84 1.78 1.75 1.71 1.71 1.84 1.81 1.82
NICOTINE (mg/t.p.) 1.390 1.366 1.362 1.236 1.221 1.221 1.204 1.650 1.657 1.672
NFDPM (mg/t.p.) 14.28 14.18 14.21 13.34 13.29 13.23 13.25 14.06 13.86 13.95
CO (mg/t.p.) 14.83 14.56 14.42 12.93 12.84 12.76 12.83 13.42 13.24 13.21
PUFF (/t.p.) 9.15 9.09 9.00 8.36 8.36 8.32 8.23 7.70 7.72 7.78
Repeatability (r)
TPM (mg/t.p.) 0.83 0.81 0.94 0.93 0.80 0.85 0.87 1.06 1.05 1.07
WATER (mg/t.p.) 0.43 0.40 0.47 0.41 0.41 0.39 0.36 0.39 0.35 0.40
NICOTINE (mg/t.p.) 0.080 0.074 0.084 0.075 0.066 0.076 0.075 0.119 0.093 0.096
NFDPM (mg/t.p.) 0.71 0.63 0.80 0.77 0.78 0.72 0.72 0.82 0.89 0.89
CO (mg/t.p.) 0.82 0.92 0.95 0.95 0.78 0.75 0.79 1.05 0.79 0.97
PUFF (/t.p.) 0.37 0.39 0.33 0.38 0.34 0.31 0.36 0.30 0.39 0.36
Reproducibility (R)
TPM (mg/t.p.) 1.77 1.54 1.72 1.77 1.67 1.61 1.93 1.89 1.95 1.93
WATER (mg/t.p.) 1.11 1.09 0.98 0.97 1.03 0.98 1.01 1.12 1.08 1.15
NICOTINE (mg/t.p.) 0.131 0.150 0.173 0.150 0.143 0.146 0.155 0.197 0.202 0.254
NFDPM (mg/t.p.) 1.80 1.53 1.92 1.88 1.73 1.85 2.16 1.97 1.91 1.86
CO (mg/t.p.) 1.64 1.96 1.83 1.94 1.75 1.61 1.97 2.02 1.52 1.97
PUFF (/t.p.) 0.88 0.82 0.69 0.86 0.93 0.91 0.82 0.75 0.83 1.00
RAC SG Report
SSPT2017, Kitzbühel - 171010
RAC Activities - continued
Conclusions from CM8 Study
No systematic tendency for the mean values of CM 8
observed between 2014 and 2017
Repeatability and reproducibility figures are quite stable and
comparable to those obtained with the other test pieces,
taking into account the slightly higher mean values of TPM
and nicotine for CM8 than for the previous test pieces
Centre de Coopération pour les Recherches Scientifiques Relatives au Tabac
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SSPT2017, Kitzbühel - 171010
RAC Activities - continued
Project 157 - Summary of CM8 Study data for revision of ISO
10362-1 by TC126-WG17
ISO/TC 126/WG 17 was requested to revise ISO 10362-1 “Cigarettes -
Determination of water in smoke condensates - Gas chromatographic
method” in order to include capillary columns. The WG 17 members agreed
that the capillary column may only be included in the standard if a
collaborative study has shown that the results obtained from a packed
column and a capillary column are comparable.
Therefore CORESTA requested to perform a statistical analysis of the
mean values as well as repeatability and reproducibility data for water
determination results obtained with packed and capillary columns,
respectively.
Statistical analysis complete
Technical Report Pending
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SSPT2017, Kitzbühel - 171010
RAC Activities - continued
Project 105 – LIP Alternate Substrate Study for ISO/TC92-WG15
Behind schedule while we wait for the production of test articles at an
appropriate self-extinction rate
Project 116 – Development of CRM for the determination of the
menthol in mentholated cigarettes and in cut filler of
mentholated cigarettes
Proficiency trial to assess similarities/differences between methodologies -
complete
Refine to a single methodology
Perform collaborative study in 2018
Deliverables are a Technical Report and CRM
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RAC Activities - continued
CM9 Production
CM8 inventory is projected to last for approximately 1 year
JTI Trier kindly offered to produce CM9
Prototypes completed and specification aligned at last Sub-Group meeting
in May
All materials ordered and on site in Trier factory
Production was scheduled for May/June 2017, but canceled due to missing
manufacturing exception from authorities
New schedule for production can be addressed after receiving exception
To keep legal certainty we need to wait for official exception from BVL
(Ministry of Consumer Protection & Food Safety)
Centre de Coopération pour les Recherches Scientifiques Relatives au Tabac
Cooperation Centre for Scientific Research Relative to Tobacco 13 RAC SG Report
SSPT2017, Kitzbühel - 171010
RAC Activities - continued