sub-group routine analytical chemistry (rac) · products by gas chromatography – reduction in...

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

SSPT2017, Kitzbühel - 171010

Current Objectives




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




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




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





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






RAC Activities - continued

Project 056 – CRM for Nicotine by GC-MS suitable for ISO



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





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)


Cooperation Centre for Scientific Research Relative to Tobacco 9

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



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





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





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





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)





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