FTIR Method for E-Cigarette Aerosol Characterization...Primary: Quantify key e-cig aerosol...
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FTIR Method for E-Cigarette Aerosol Characterization September 18-21, 2016 70th TOBACCO SCIENCE RESEARCH CONFERENCE Palm Beach Gardens, Florida USA Falk Radtke Philip Morris International R&D 2016_TSRC62_Radtke.pdf TSRC2016(70) - Document not peer-reviewed
Transcript of FTIR Method for E-Cigarette Aerosol Characterization...Primary: Quantify key e-cig aerosol...
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FTIR Method for E-Cigarette Aerosol CharacterizationSeptember 18-21, 201670th TOBACCO SCIENCE RESEARCH CONFERENCEPalm Beach Gardens, Florida USA
Falk RadtkePhilip Morris International R&D
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Outline
• Introduction
– Background
– Motivation & Target
• Equipment & Method Concept
• Method Verification
– Study design: Quantitative E-cig aerosol analysis
– Results
• Summary
• Outlook
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Background
• Electronic cigarettes (e-cig) are emerging with numerous variations in designs and performance parameters within and across brands
– Disposable or rechargeable, replaceable cartridges
– Tank systems with larger batteries
– Large capacity batteries, integrated circuits allowing heating power and flow adjustment (=> variation of nicotine delivery/puff)
• E-cigarettes emissions needs to be measured
– Existing recommendations as to what needs to be tested (e.g. BSI, AFNOR)
– Various groups working on the topic (e.g. CEN/TC 437/WG 4)
– Carbonyls are known to be emitted by e-cigarettes, in various amounts depending on the design
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Motivation for online e-cig screening method
• Standard chemical characterization is time consuming
– Multiple process steps required (trap aerosol/extract/measure/evaluate)
– Accumulation of 10 to 50 puffs required
• Short product development cycles facilitated by rapid screening tools
– Assess and optimize product performance
– Monitor product quality and reliability
Target
• Primary: Quantify key e-cig aerosol constituents on a puff-by-puff basis
• Secondary: Quantify carbonyls during critical EoB/EoL e-cig operation
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Key E-Cig Aerosol Constituents
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KeyConstituents
Liquid CompositionRange (% w/w)
Boiling Point
Water 6 20 100°C
Nicotine 0.45 7 247°C
Glycerin 20 37.25 290°C
PG 34 65.5 188°C
Flavor* 0 5 -
Menthol* 0 2 212°C*out of scope
Equipment & Method Concept
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Selected FTIR System
• Gasmet™ DX4000 FTIR Gas analyzer
• Gasmet™ Portable sampling system
– Heating controller, heated pump & filter, heated sample lines,calibrator
• PC with CalcmetTM software
Principle of Operation• Michelson Interferometer performs Fourier transformation
on IR beam passing the sample chamber
• Full IR –spectrum measured at high speed (>1 spectrum/s)
• CalcmetTM software calculate factors for ref. spectraof selected gaseous compounds
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Equipment & Method Concept
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Analysis of FTIR SpectraQuantification based on infrared (IR) absorption (wave number 900 cm-1 to 4200cm-1)
1000150020002500300035004000
Sample spectrum
Water 10 vol-% SO2 300 mg/Nm3
CO2 10 vol-%
CO 1000 mg/Nm3
NH3 100 mg/Nm3
HCl 50 mg/Nm3
1000150020002500300035004000
Calculated spectrum
Reference Spectrums (not to same scale)
Analysis:0.881 * Water 10 vol-%1.112 * CO2 10 vol-%0.995 * CO 1000 mg/Nm30.910 * NO 300 mg/Nm3 0.810 * SO2 300 mg/Nm3 0.660 * NH3 100 mg/Nm30.082 * HCl 50 mg/Nm30.210 * Methane 50 mg/Nm3
Methane 50 mg/Nm3NO 300 mg/Nm3
Equipment & Method Concept
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3134.323134.323134.323134.323134.32
3142.043142.043142.043142.043142.04
3149.763149.763149.763149.763149.76
3157.483157.483157.483157.483157.48
3165.23165.23165.23165.23165.2
3172.923172.923172.923172.923172.92
3180.643180.643180.643180.643180.64
3188.363188.363188.363188.363188.36
3196.083196.083196.083196.083196.08
3203.83203.83203.83203.83203.8
3211.523211.523211.523211.523211.52
3219.243219.243219.243219.243219.24
3226.963226.963226.963226.963226.96
3234.683234.683234.683234.683234.68
3242.43242.43242.43242.43242.4
3250.123250.123250.123250.123250.12
3257.843257.843257.843257.843257.84
3265.563265.563265.563265.563265.56
3273.283273.283273.283273.283273.28
32813281328132813281
3288.723288.723288.723288.723288.72
3296.443296.443296.443296.443296.44
3304.163304.163304.163304.163304.16
3311.883311.883311.883311.883311.88
3319.63319.63319.63319.63319.6
3327.323327.323327.323327.323327.32
3335.043335.043335.043335.043335.04
3342.763342.763342.763342.763342.76
3350.483350.483350.483350.483350.48
3358.23358.23358.23358.23358.2
3365.923365.923365.923365.923365.92
3373.643373.643373.643373.643373.64
3381.363381.363381.363381.363381.36
3389.083389.083389.083389.083389.08
3396.83396.83396.83396.83396.8
3404.523404.523404.523404.523404.52
3412.243412.243412.243412.243412.24
3419.963419.963419.963419.963419.96
3427.683427.683427.683427.683427.68
3435.43435.43435.43435.43435.4
3443.123443.123443.123443.123443.12
3450.843450.843450.843450.843450.84
3458.563458.563458.563458.563458.56
3466.283466.283466.283466.283466.28
34743474347434743474
3481.723481.723481.723481.723481.72
3489.443489.443489.443489.443489.44
3497.163497.163497.163497.163497.16
3504.883504.883504.883504.883504.88
3512.63512.63512.63512.63512.6
3520.323520.323520.323520.323520.32
3528.043528.043528.043528.043528.04
3535.763535.763535.763535.763535.76
3543.483543.483543.483543.483543.48
3551.23551.23551.23551.23551.2
3558.923558.923558.923558.923558.92
3566.643566.643566.643566.643566.64
3574.363574.363574.363574.363574.36
3582.083582.083582.083582.083582.08
3589.83589.83589.83589.83589.8
3597.523597.523597.523597.523597.52
3605.243605.243605.243605.243605.24
3612.963612.963612.963612.963612.96
3620.683620.683620.683620.683620.68
3628.43628.43628.43628.43628.4
3636.123636.123636.123636.123636.12
3643.843643.843643.843643.843643.84
3651.563651.563651.563651.563651.56
3659.283659.283659.283659.283659.28
36673667366736673667
3674.723674.723674.723674.723674.72
3682.443682.443682.443682.443682.44
3690.163690.163690.163690.163690.16
3697.883697.883697.883697.883697.88
3705.63705.63705.63705.63705.6
3713.323713.323713.323713.323713.32
3721.043721.043721.043721.043721.04
3728.763728.763728.763728.763728.76
3736.483736.483736.483736.483736.48
3744.23744.23744.23744.23744.2
3751.923751.923751.923751.923751.92
3759.643759.643759.643759.643759.64
3767.363767.363767.363767.363767.36
3775.083775.083775.083775.083775.08
3782.83782.83782.83782.83782.8
3790.523790.523790.523790.523790.52
3798.243798.243798.243798.243798.24
3805.963805.963805.963805.963805.96
3813.683813.683813.683813.683813.68
3821.43821.43821.43821.43821.4
3829.123829.123829.123829.123829.12
3836.843836.843836.843836.843836.84
3844.563844.563844.563844.563844.56
3852.283852.283852.283852.283852.28
38603860386038603860
3867.723867.723867.723867.723867.72
3875.443875.443875.443875.443875.44
3883.163883.163883.163883.163883.16
3890.883890.883890.883890.883890.88
3898.63898.63898.63898.63898.6
3906.323906.323906.323906.323906.32
3914.043914.043914.043914.043914.04
3921.763921.763921.763921.763921.76
3929.483929.483929.483929.483929.48
3937.23937.23937.23937.23937.2
3944.923944.923944.923944.923944.92
3952.643952.643952.643952.643952.64
3960.363960.363960.363960.363960.36
3968.083968.083968.083968.083968.08
3975.83975.83975.83975.83975.8
3983.523983.523983.523983.523983.52
3991.243991.243991.243991.243991.24
3998.963998.963998.963998.963998.96
4006.684006.684006.684006.684006.68
4014.44014.44014.44014.44014.4
4022.124022.124022.124022.124022.12
4029.844029.844029.844029.844029.84
4037.564037.564037.564037.564037.56
4045.284045.284045.284045.284045.28
40534053405340534053
4060.724060.724060.724060.724060.72
4068.444068.444068.444068.444068.44
4076.164076.164076.164076.164076.16
4083.884083.884083.884083.884083.88
4091.64091.64091.64091.64091.6
4099.324099.324099.324099.324099.32
4107.044107.044107.044107.044107.04
4114.764114.764114.764114.764114.76
4122.484122.484122.484122.484122.48
4130.24130.24130.24130.24130.2
4137.924137.924137.924137.924137.92
4145.644145.644145.644145.644145.64
4153.364153.364153.364153.364153.36
4161.084161.084161.084161.084161.08
4168.84168.84168.84168.84168.8
4176.524176.524176.524176.524176.52
4184.244184.244184.244184.244184.24
4191.964191.964191.964191.964191.96
4199.684199.684199.684199.684199.68
4207.44207.44207.44207.44207.4
4215.124215.124215.124215.124215.12
4222.844222.844222.844222.844222.84
4230.564230.564230.564230.564230.56
4238.284238.284238.284238.284238.28
SO2 656 ppm
H2O 8 vol-%
NH3 41 ppm
CO2 14,6 vol-%
C2H4 49 ppm
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0.011903
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Chart2
594.44
'SO2 656 ppm'!#REF!
1
Chart3
594.44
602.16
609.88
617.6
625.32
633.04
640.76
648.48
656.2
663.92
671.64
679.36
687.08
694.8
702.52
710.24
717.96
725.68
733.4
741.12
748.84
756.56
764.28
772
779.72
787.44
795.16
802.88
810.6
818.32
826.04
833.76
841.48
849.2
856.92
864.64
872.36
880.08
887.8
895.52
903.24
910.96
918.68
926.4
934.12
941.84
949.56
957.28
965
972.72
980.44
988.16
995.88
1003.6
1011.32
1019.04
1026.76
1034.48
1042.2
1049.92
1057.64
1065.36
1073.08
1080.8
1088.52
1096.24
1103.96
1111.68
1119.4
1127.12
1134.84
1142.56
1150.28
1158
1165.72
1173.44
1181.16
1188.88
1196.6
1204.32
1212.04
1219.76
1227.48
1235.2
1242.92
1250.64
1258.36
1266.08
1273.8
1281.52
1289.24
1296.96
1304.68
1312.4
1320.12
1327.84
1335.56
1343.28
1351
1358.72
1366.44
1374.16
1381.88
1389.6
1397.32
1405.04
1412.76
1420.48
1428.2
1435.92
1443.64
1451.36
1459.08
1466.8
1474.52
1482.24
1489.96
1497.68
1505.4
1513.12
1520.84
1528.56
1536.28
1544
1551.72
1559.44
1567.16
1574.88
1582.6
1590.32
1598.04
1605.76
1613.48
1621.2
1628.92
1636.64
1644.36
1652.08
1659.8
1667.52
1675.24
1682.96
1690.68
1698.4
1706.12
1713.84
1721.56
1729.28
1737
1744.72
1752.44
1760.16
1767.88
1775.6
1783.32
1791.04
1798.76
1806.48
1814.2
1821.92
1829.64
1837.36
1845.08
1852.8
1860.52
1868.24
1875.96
1883.68
1891.4
1899.12
1906.84
1914.56
1922.28
1930
1937.72
1945.44
1953.16
1960.88
1968.6
1976.32
1984.04
1991.76
1999.48
2007.2
2014.92
2022.64
2030.36
2038.08
2045.8
2053.52
2061.24
2068.96
2076.68
2084.4
2092.12
2099.84
2107.56
2115.28
2123
2130.72
2138.44
2146.16
2153.88
2161.6
2169.32
2177.04
2184.76
2192.48
2200.2
2207.92
2215.64
2223.36
2231.08
2238.8
2246.52
2254.24
2261.96
2269.68
2277.4
2285.12
2292.84
2300.56
2308.28
2316
2323.72
2331.44
2339.16
2346.88
2354.6
2362.32
2370.04
2377.76
2385.48
2393.2
2400.92
2408.64
2416.36
2424.08
2431.8
2439.52
2447.24
2454.96
2462.68
2470.4
2478.12
2485.84
2493.56
2501.28
2509
2516.72
2524.44
2532.16
2539.88
2547.6
2555.32
2563.04
2570.76
2578.48
2586.2
2593.92
2601.64
2609.36
2617.08
2624.8
2632.52
2640.24
2647.96
2655.68
2663.4
2671.12
2678.84
2686.56
2694.28
2702
2709.72
2717.44
2725.16
2732.88
2740.6
2748.32
2756.04
2763.76
2771.48
2779.2
2786.92
2794.64
2802.36
2810.08
2817.8
2825.52
2833.24
2840.96
2848.68
2856.4
2864.12
2871.84
2879.56
2887.28
2895
2902.72
2910.44
2918.16
2925.88
2933.6
2941.32
2949.04
2956.76
2964.48
2972.2
2979.92
2987.64
2995.36
3003.08
3010.8
3018.52
3026.24
3033.96
3041.68
3049.4
3057.12
3064.84
3072.56
3080.28
3088
3095.72
3103.44
3111.16
3118.88
3126.6
3134.32
3142.04
3149.76
3157.48
3165.2
3172.92
3180.64
3188.36
3196.08
3203.8
3211.52
3219.24
3226.96
3234.68
3242.4
3250.12
3257.84
3265.56
3273.28
3281
3288.72
3296.44
3304.16
3311.88
3319.6
3327.32
3335.04
3342.76
3350.48
3358.2
3365.92
3373.64
3381.36
3389.08
3396.8
3404.52
3412.24
3419.96
3427.68
3435.4
3443.12
3450.84
3458.56
3466.28
3474
3481.72
3489.44
3497.16
3504.88
3512.6
3520.32
3528.04
3535.76
3543.48
3551.2
3558.92
3566.64
3574.36
3582.08
3589.8
3597.52
3605.24
3612.96
3620.68
3628.4
3636.12
3643.84
3651.56
3659.28
3667
3674.72
3682.44
3690.16
3697.88
3705.6
3713.32
3721.04
3728.76
3736.48
3744.2
3751.92
3759.64
3767.36
3775.08
3782.8
3790.52
3798.24
3805.96
3813.68
3821.4
3829.12
3836.84
3844.56
3852.28
3860
3867.72
3875.44
3883.16
3890.88
3898.6
3906.32
3914.04
3921.76
3929.48
3937.2
3944.92
3952.64
3960.36
3968.08
3975.8
3983.52
3991.24
3998.96
4006.68
4014.4
4022.12
4029.84
4037.56
4045.28
4053
4060.72
4068.44
4076.16
4083.88
4091.6
4099.32
4107.04
4114.76
4122.48
4130.2
4137.92
4145.64
4153.36
4161.08
4168.8
4176.52
4184.24
4191.96
4199.68
4207.4
4215.12
4222.84
4230.56
4238.28
xxxx
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SO2 656 ppm
SO2 656 ppmH2O 8 vol-%NH3 41 ppmCO2 14,6 vol-%C2H4 49 ppmxxxx594.44
594.44-0.0313640.3347630.0007990.1342220.019632-0.012529602.16
602.160.0175140.3135740.0029490.1249390.0127370.019694609.88
609.880.0310340.341514-0.0008220.138640.007424-0.01265617.6
617.6-0.0154430.309508-0.0042930.122690.017833-0.02683625.32
625.320.0055090.364659-0.0068630.130140.0246820.027617633.04
633.04-0.0073610.361651-0.0062380.138140.0103410.008118640.76
640.760.0344720.3455080.0008090.1445610.01010.023252648.48
648.480.021670.294354-0.0008440.1397990-0.008558656.2
656.20.0039130.298014-0.0089090.104620.0073820.006434663.92
663.92-0.0091430.3301470.0031930.1387980.002406-0.013095671.64
671.6400.329405-0.0007640.132985-0.007299-0.006531679.36
679.360.0432990.356683-0.0007780.1631810.012517-0.019305687.08
687.08-0.020640.34197200.1432510.0072990.013502694.8
694.80.0184830.369469-0.0022520.1509520.0050210.041813702.52
702.520.0037120.366236-0.0049820.161242-0.0023290.028453710.24
710.240.0207290.3547930.0055320.144860.0074670.048433717.96
717.960.0265590.3060670.0069350.1438620.0194130.029188725.68
725.68-0.0019090.3220.0043430.1290010.0172260.022163733.4
733.4-0.0037770.328816-0.0039230.1650960.0184830.058901741.12
741.12-0.0365750.332877-0.0061820.1417090.0158770.050378748.84
748.840.0434660.373256-0.0051480.166094-0.002380.061091756.56
756.560.003650.3662770.0059090.1574490.0022440.139945764.28
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