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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EVAP SG Report

SSPT2019, Hamburg - 191008

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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EVAP SG Report

SSPT2019, Hamburg - 191008

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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EVAP SG Report

SSPT2019, Hamburg - 191008

❖ 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

EVAP SG Report

SSPT2019, Hamburg - 191008

List of Elements

❖ Arsenic (As)

❖ Cadmium (Cd)

❖ Chromium (Cr)

❖ Copper (Cu)

❖ Iron (Fe)

❖ Lead (Pb)

❖ Nickel (Ni)

❖ Silver (Ag)

❖ Tin (Sn)

❖ Zinc (Zn)

7EVAP SG Report

SSPT2019, Hamburg - 191008

EVAP SG Report

SSPT2019, Hamburg - 191008

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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EVAP SG Report

SSPT2019, Hamburg - 191008

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

SSPT2019, Hamburg - 191008

EVAP SG Report

SSPT2019, Hamburg - 191008

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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EVAP SG Report

SSPT2019, Hamburg - 191008

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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EVAP SG Report

SSPT2019, Hamburg - 191008

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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EVAP SG Report

SSPT2019, Hamburg - 191008

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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EVAP SG Report

SSPT2019, Hamburg - 191008

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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EVAP SG Report

SSPT2019, Hamburg - 191008

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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EVAP SG Report

SSPT2019, Hamburg - 191008

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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EVAP SG Report

SSPT2019, Hamburg - 191008

Carbonyl Aerosol

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EVAP SG Report

SSPT2019, Hamburg - 191008

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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EVAP SG Report

SSPT2019, Hamburg - 191008

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

EVAP SG Report

SSPT2019, Hamburg - 191008

EVAP SG Report

SSPT2019, Hamburg - 191008

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

EVAP SG Report

SSPT2019, Hamburg - 191008

EVAP SG Report

SSPT2019, Hamburg - 191008

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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EVAP SG Report

SSPT2019, Hamburg - 191008

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

SSPT2019, Hamburg - 191008

EVAP SG Report

SSPT2019, Hamburg - 191008

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

SSPT2019, Hamburg - 191008

EVAP SG Report

SSPT2019, Hamburg - 191008

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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EVAP SG Report

SSPT2019, Hamburg - 191008

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

EVAP SG Report

SSPT2019, Hamburg - 191008

EVAP SG Report

SSPT2019, Hamburg - 191008

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

EVAP SG Report

SSPT2019, Hamburg - 191008

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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EVAP SG Report

SSPT2019, Hamburg - 191008

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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