E-Vapour (EVAP) Sub-Group 2019 Report - CORESTA · 2019. 11. 3. · EVAP SG Report SSPT2019,...
Transcript of E-Vapour (EVAP) Sub-Group 2019 Report - CORESTA · 2019. 11. 3. · EVAP SG Report SSPT2019,...
Hamburg, Germany
October 8, 2019
E-Vapour (EVAP) Sub-Group
2019 Report
EVAP SG Report
SSPT2019, Hamburg - 191008
E-Vapour Products SG Membership
❖ SG Coordinator
o Charles Garner - RAI Service Company
❖ SG Secretary
o Gene Gillman – Enthalpy Analytical
❖ SG membership
o ≈ 50 people US, EU, Asia
o E-Vapour Product Companies, Suppliers, Contract Labs, Regulatory
Agencies, Academia, Others, …...
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E-Vapour Product Sub Group
Scope:
1)To identify areas of scientific research and conduct studies that will
characterize liquids, e-vapour product emissions, and device
properties and performance
2)To develop and publish methods and guides
3)To organize and conduct periodic proficiency/collaborative studies
of identified constituents in liquids and/or e-vapour product aerosol
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Accomplishments
Guide No. 26 - Technical Guide for Designing E-Vapour Product
Stability Studies
Published on the CORESTA website September 2019
Guide No. 25 - Technical Guide for Aerosol Collection and
Considerations when Testing E-Vapour Product Technologies
Published on the CORESTA website May 2019
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❖ Active NWIPs
E-Vapour Sub Group
ProjectNo. Activity Leader Time
127 Carbonyls in aerosol Gillman Ongoing
088 Comparison of Puffing Parameters – Peer-Reviewed
Publication
Gupta Under SG
review
184 Metals Proficiency Study Wagstaff/Joza/
Gillman
Report with
SG
210 LOD/LOQ values for the determination of metals in
aerosol
Cook Ongoing
231 Aerosol Collaborative Study Reference Device Weidman Ongoing
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Metals CRM and Proficiency Study
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List of Elements
❖ Arsenic (As)
❖ Cadmium (Cd)
❖ Chromium (Cr)
❖ Copper (Cu)
❖ Iron (Fe)
❖ Lead (Pb)
❖ Nickel (Ni)
❖ Silver (Ag)
❖ Tin (Sn)
❖ Zinc (Zn)
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EVAP SG Report
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Metals in e-liquid
Study Coordinator - Pete Joza
Statistical Analysis - Wendy Wagstaff
Method Selection –In house ICP-MS method
➢Phase I – e-Liquids only
⚫ Study Closed September 2018
⚫ Data verified by participants November-January
⚫ Draft report sent to SG for review April 2019
⚫ Comments received from the SG and revised report sent to the group in
September 2019
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Metals in e-liquid-Next Steps
Next Steps
✓ Draft technical guide on analysis of metals in liquid samples
✓ Draft CRM based on dilution method
✓ Distribute to SG for review on August 2019
⚫ Comments received on draft, under revision
⚫ Technical report to SC by December 2019
⚫ Plan collaborative study with draft CRM method 2019/2020
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Carbonyl Method
Aerosol
EVAP SG Report
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EVAP SG Report
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Carbonyls in Aerosol
Study Coordinator - Gene Gillman (Enthalpy)
Statistical Analysis - Mike Morton (Altria)
Method Selection - HPLC with DNPH
Phase I – Liquid (Completed), Technical report published
Phase II – Emissions (Small Group Study 2018)
✓Spiked liquid transfer study with four SG members
✓Device and liquid selection
Phase III – Collaborative study
✓ In house spiked liquids and standardized device
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Carbonyl Aerosol
Method Selection: HPLC with DNPH
Study Protocol
➢ Harmonized Device: Aspire Tank and Evolv DNA power supply
➢ Compounds included: formaldehyde and acetaldehyde
➢ Three e-liquids, unflavored, tobacco and menthol
➢ Samples fortified at three levels (0, 15, 25 and 35 mg/ml) immediately before
analysis
➢ Aerosol samples collected using 55/3/30 CORESTA CRM 81puffing
➢ Collected ~300mg of aerosol per liquid and spiking level, in triplicate
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Carbonyl Aerosol
Why use fortified e-liquids?
➢ We expected the native production of formaldehyde and acetaldehyde
to be both low and variable in the un-spiked aerosol, based on pre-
study work.
➢ Formaldehyde and acetaldehyde added to e-liquids will transfer into
the aerosol, based on pre-study work.
➢ Adding a known amount of formaldehyde and acetaldehyde to the
native amount produced by each device should improve the
consistency of measurements and correct for device to device
differences
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Carbonyl Aerosol
0.00
2.00
4.00
6.00
8.00
10.00
12.00
14.00
1 2 3 4 7 9 10
mg/p
uff
Lab #
Aerosol Massunspiked liquid
Data for the unflavored e-liquid
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Carbonyl Aerosol
0.0
2.0
4.0
6.0
8.0
10.0
12.0
14.0
16.0
18.0
1 2 3 4 7 9 10
mg/g
ram
Lab #
Formaldehyeunspiked liquid
Data for the unflavored e-liquid
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Carbonyl Aerosol
0.0
1.0
2.0
3.0
4.0
5.0
6.0
1 2 3 4 7 9 10
mg/g
ram
Lab #
Acetaldehydeunspiked liquid
Data for the unflavored e-liquid
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Carbonyl Aerosol
✓ Each lab reported aerosol mass, formaldehyde and
acetaldehyde
✓ Aerosol formaldehyde and acetaldehyde results reported in
mg/gram of aerosol.
✓ Formaldehyde showed a linear increase in all labs.
✓ Acetaldehyde showed linear response, except for lab 4. Some
labs reported low values for the stock spiking solution.
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Carbonyl Aerosol
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Carbonyl Aerosol
Average transfer from the liquid to the aerosol for formaldehyde and
acetaldehyde was ~65%
Several labs reported issues with the acetaldehyde standard (low) and either
corrected or used an alternate source. Not all labs verified the spiking
solutions.
Spike Amount Lab 1 Lab 2 Lab 3 Lab 4 Lab 7 Lab 9 Lab 10µg/gram % Transfer % Transfer % Transfer % Transfer % Transfer % Transfer % Transfer
15 55.9 66.3 75.0 67.6 52.5 57.9 68.2
25 59.6 54.7 61.2 144.1 42.2 49.0 72.6
35 56.0 54.2 60.3 97.6 46.5 52.8 72.9
15 33.9 49.4 104.7 37.3 38.6 77.6 62.2
25 39.4 44.8 96.4 238.2 26.7 54.6 65.4
35 30.2 39.7 94.3 141.1 34.4 67.9 70.4
Formaldehyde
Acetaldehyde
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Carbonyl Aerosol
Next Steps:
✓Study remains open to allow submission of additional data sets
✓Prepare draft Technical report for review by the SG.
✓Publish Technical report on the CORESTA website.
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Technical Guide on Designing Stability Studies
Completed
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EVAP SG Report
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Guide on Stability Studies
❖ Stability indicating compounds
➢ Formal stability studies outside of scope of group
➢ Draft guide circulated to the SG in March 2018. Revised draft
circulated to the SG in October 2018, Final draft to SG March 2019
➢ Published on CORESTA Website September 2019
➢ Leader Gary Dull (RJR)
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Primary Constituents in Aerosol
Reference Device Study
Approved NWIP
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EVAP SG Report
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Reference Devices
❖ E-vapour emission method requires suitable generation devices
o References devices are needed for future collaborative studies
o SG has identified a suitable tank based product from the carbonyl studies
o Primary constituents collaborative study under away to add reference device r
and R data to CRM 84
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Reference Device
Study Coordinator - Randy Weidman (RJR)
Statistical Analysis - Mike Morton (Altria)
Method Selection – CRM 81 and CRM 84
Study Protocol
➢ Harmonized Device: Aspire Tank and Evolv DNA power supply
➢ Compounds included: nicotine, propylene glycol, glycerin @ water
➢ Three e-liquids, unflavored, tobacco and menthol
➢ Study extended to allow maximum participation from SG
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Metals LOD/LOQ
Approved NWIP
EVAP SG Report
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EVAP SG Report
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Approved NWIP
❖ Metals LOD/LOQ
➢ Filter pad based trapping systems contain some analytes of interest.
➢ Other trapping system may also contain some analytes of interest.
➢ Reported values are impacted by trapping system
⚫ Recommend best practice for determining method LOD/LOQ values
⚫ Recommend best practice to handle contribution from trapping system
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ISO TC 126 SC3 WG3
Update
EVAP SG Report
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EVAP SG Report
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TC 126 SC3 WG3 Update
❖ 3 year track
➢ June 2022 ISO publication due date
❖ Four approved NWIPS
➢ Convener: Liliana Chaves
ISO/NP Title Leader
24197 Analytical method to measure mass of e- liquids vaporized Marie Fetter
24199 Analytical method to measure nicotine of e-vapor products emissionsXiaoyu Wang and Jacques
Cinquin
24211 Analytical method to measure carbonyls of vapor products emissions John Miller
24198 Analytical method to measure metals of e- vapor product emissions Peter Joza
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Relevant Work from CORESTA
ISO/NP Ttile EVAP SG Work Item
24197Analytical method to measure mass of e- liquids
vaporizedCRM-84
24199Analytical method to measure nicotine of e-vapor
products emissionsCRM-84
24211Analytical method to measure carbonyls of vapor
products emissionsCurrent Collaborative Study
24198Analytical method to measure metals of e- vapor
product emissionsDraft CRM for Metals analysis in e-liquids
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Nicotine Degradants in smokeless and
e-liquids: Proficiency Study
Possible NWIP
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EVAP SG Report
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Nicotine Degradants
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❖ Joint Study with TTPA and EVAP –NWIP required
❖ Proficiency Study: laboratories use their in-house methods
❖ Samples: 8 total➢ 4 e-liquids
➢ 4 tobacco free, tobacco derived nicotine products (TDN)
➢ samples will not be branded and may be subjected to accelerated aging
to ensure measurable levels
❖ Report z-scores and method synopses
❖ Timeline:➢ Ship samples week of January 8th 2020
➢ Laboratories immediately conduct analyses or freeze samples
➢ Data due February 28, 2020
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Nicotine Degradants
❖ Compounds of interest
➢ nicotine-N-oxides (cis and trans; CAS #491-26-9),
➢ cotinine (CAS #486-56-6)
➢ nornicotine (CAS #5746-86-1)
➢ anatabine (CAS #2743-90-0)
➢ myosmine (CAS #532-12-7)
➢ anabasine (CAS #13078-04-1)
➢ β-nicotyrine (CAS #487-19-4)
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Two year plan for the group
❖ Carbonyls in aerosol technical report – In process
❖ Carbonyls aerosol draft CRM – In process
❖ Reference device collaborative studies – In process
❖ Metals collaborative study with draft CRM (CRM drafted)
❖ Organic acids – methods review (Planning stage)
❖ Flavors (Planning stage)
❖ Nicotine degs by LC-MS/MS (TTPA joint study) – In process
❖ TSNAs
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