Eliminating the Need for Standards and Calibration in GC/FID Analysis of Hydrocarbons and Oxygenates
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1 Eliminating the Need for Standards and Calibration in GC/FID Analysis of Hydrocarbons and Oxygenates 20 October 2015 Andrew J. Jones, Ph.D. Co-founder
2 Methanol to Dimethyl Ether H + CH 3 OH CH 3 OCH 3 + H 2 O 433 K 2
3 Methanol to Dimethyl Ether H + CH 3 OH CH 3 OCH 3 + H 2 O 433 K MFI (Si/Al = 44) r ~ [CH 3 OH] 0 r ~ [CH 3 OH] 433 K Jones et al., J Catal., 312 (2014) 58 3
4 Methanol to Dimethyl Ether H + CH 3 OH CH 3 OCH 3 + H 2 O 433 K MFI (Si/Al = 44) CH 3 OH r ~ [CH 3 OH] 0 r ~ [CH 3 OH] 433 K CH 3 OCH 3 Jones et al., J Catal., 312 (2014) 58 4
5 Methanol to Gasoline (MTG/MTH/MTO) CH 3 OH H + Hydrocarbons >550 K Oxygenates Gasoline 5
6 Methanol to Gasoline (MTG/MTH/MTO) CH 3 OH H + Hydrocarbons >550 K Oxygenates Gasoline Too many compounds to calibrate accurately and regularly Time consuming analysis Degradation of standards Invisible compounds 6 Michele Sarazen in the Iglesia Group at Berkeley
7 Methanol to Gasoline (MTG/MTH/MTO) CH 3 OH H + Hydrocarbons >550 K Oxygenates DME Gasoline C1-C3 C2-C4 C4-C5 C5-C6 C7 C8 Too many compounds to calibrate accurately and regularly Time consuming analysis Degradation of standards Invisible compounds 7 Michele Sarazen in the Iglesia Group at Berkeley
8 Why calibrate? 8
9 Why calibrate? Flame ionization detector (FID) CHO V e - air H 2 sample Holm, T., J. Chromatogr. A, 842 (1999) 221 9
10 Why calibrate? Flame ionization detector (FID) FID Detection Sensitivity (per carbon) CHO V e - air H sample Dietz, W. A., J. Gas Chromatogr., 5 (1967) 68 Holm, T., J. Chromatogr. A, 842 (1999)
11 Why calibrate? Reactive Chromatography Any Molecule FID Detection Sensitivity (per carbon) Catalytic Reactor xch 4 FID
12 Eliminate calibrations and detect more Reactive Chromatography Any Molecule FID Detection Sensitivity (per carbon) Catalytic Reactor xch 4 FID Maduskar, S., et al., Lab Chip, 15 (2015) 440 Watanabe, T., et al., Talanta, 72 (2007)
13 Eliminate calibrations and detect more Reactive Chromatography Any Molecule FID Detection Sensitivity (per carbon) xch 4 FID
14 Chemically convert molecules to CH 4 during GC analysis CH 3 OH H + Hydrocarbons >550 K Oxygenates DME Gasoline C1-C3 C2-C4 C4-C5 C5-C6 C7 C8 Too many compounds to calibrate accurately and regularly Time consuming analysis Degradation of standards Invisible compounds 14 Michele Sarazen in the Iglesia Group at Berkeley
15 Chemically convert molecules to CH 4 during GC analysis CH 3 OH H + Hydrocarbons >550 K Oxygenates DME Gasoline C1-C3 C2-C4 C4-C5 C5-C6 C7 C8 Too many compounds to calibrate accurately and regularly Time consuming analysis Degradation of standards Invisible compounds 15 Michele Sarazen in the Iglesia Group at Berkeley
16 Chemically convert molecules to CH 4 during GC analysis CH 3 OH H + Hydrocarbons >550 K Oxygenates Gasoline C1-C3 CH 4 /CO CO 2 Formaldehyde C 2 H 4 /C 2 H 6 Too many compounds to calibrate accurately and regularly Time consuming analysis Degradation of standards Invisible compounds Michele Sarazen in the Iglesia Group at Berkeley 16
17 What this means for your chemical analysis 17
18 What this means for your chemical analysis Peak Compound 1 ethanol 2 1,2-dichloroethane 3 aniline 4 2-chlorophenol 5 1-octanol 6 2-nonanone 7 2-dodecanol 8 methyl laurate 9 n-heptadecane 10 n-nonadecane Polar-Iso Test Mix 18
19 What this means for your chemical analysis Standard FID Peak Compound 1 ethanol 2 1,2-dichloroethane 3 aniline 4 2-chlorophenol 5 1-octanol 6 2-nonanone 7 2-dodecanol 8 methyl laurate 9 n-heptadecane 10 n-nonadecane Polar-Iso Test Mix
20 What this means for your chemical analysis Standard FID Peak Compound 1 ethanol 2 1,2-dichloroethane 3 aniline 4 2-chlorophenol 5 1-octanol 6 2-nonanone 7 2-dodecanol 8 methyl laurate 9 n-heptadecane 10 n-nonadecane Polar-Iso Test Mix
21 What this means for your chemical analysis Standard FID Polar-Iso Test Mix Peak Compound Area Concentration 1 ethanol ? 2 1,2-dichloroethane ? 3 aniline 233? 4 2-chlorophenol 158.5? 5 1-octanol 216.9? 6 2-nonanone 218.5? 7 2-dodecanol 231.7? 8 methyl laurate 207.8? 9 n-heptadecane 266.8? 10 n-nonadecane 259.6?
22 Compound Response (area/µmol C) What this means for your chemical analysis 40 Standard Calibration Curve Standard FID y = 1.45x R² = EtOH Response (area/µmol C) 22
23 Compound Response (area/µmol C) What this means for your chemical analysis Standard Calibration Curve 1 2 Standard FID EtOH Response (area/µmol C) 23
24 Compound Response (area/µmol C) What this means for your chemical analysis Standard Calibration Curve 1 2 Standard FID Unknown EtOH Response (area/µmol C) 24
25 Compound Response (area/µmol C) Measurement Error What this means for chemical analysis 40 Standard Calibration Curve 7% Standard FID 35 6% 30 5% 25 4% Unknown 3% 2% 5 1% EtOH Response (area/µmol C) 0% Peak Number 25
26 Measurement Error What this means for chemical analysis Catalytic Conversion to CH 4 7% FID signal with reaction 6% 5% 4% 3% 2% 1% 0% Peak Number 26
27 Measurement Error What this means for chemical analysis Catalytic Conversion to CH 4 7% FID signal with reaction 6% 5% 4% 3% No calibration necessary 2% 1% mol C = Area Area std mol Cstd 0% Peak Number 27
28 Measurement Error What this means for chemical analysis FID signal with reaction Catalytic Conversion to CH 4 7% 6% 5% 4% Average Error FID: 4% With Reaction: 2% 3% No calibration necessary 2% 1% mol C = Area Area std mol Cstd 0% Peak Number 28
29 What is the Polyarc reactor? 29
30 What is the Polyarc reactor? 30
31 What is the Polyarc reactor? 31
32 What is the Polyarc reactor? 32
33 Works on all GC-compatible hydrocarbons C5-C18 n-alkanes C5 C18 Spanjers, C. et al., Application Note, 2015, University of Minnesota, Twin Cities 33
34 Works on all GC-compatible hydrocarbons C5-C18 n-alkanes C5 C18 Spanjers, C. et al., Application Note, 2015, University of Minnesota, Twin Cities 34
35 Works on all GC-compatible hydrocarbons Spanjers, C. et al., Application Note, 2015, University of Minnesota, Twin Cities 35
36 Works on all GC-compatible hydrocarbons Spanjers, C. et al., Application Note, 2015, University of Minnesota, Twin Cities 36
37 Works on all GC-compatible hydrocarbons C1-C6 n-alkanes C 6 H 14 C 5 H 12 C 2 H 6 C 3 H 8 C 4 H 10 CH 4 37
38 Works on all GC-compatible hydrocarbons C1-C6 n-alkanes Response Factors C 6 H 14 C 5 H 12 RF (mol C) = 1.01 ± 0.01 C 2 H 6 C 3 H 8 C 4 H 10 CH 4 38
39 Designed for heteroatoms 39
40 Designed for heteroatoms Food/Flavors/Fragrances Carbohydrates Commodity Chemicals Pharmaceuticals Cosmetics 40
41 Response Factor Specially engineered long-life cartridge 1.2 EtOH/n-heptane ROH RCl RC(O)OH RNH 3 RN: ROH Low priced replacement cartridges $ Injections 41
42 Response Factor Specially engineered long-life cartridge No performance degradation with over 5000 injections 1.2 EtOH/n-heptane ROH RCl RC(O)OH RNH 3 RN: ROH Injections 42
43 Response Factor Specially engineered long-life cartridge No performance degradation with over 5000 injections 1.2 EtOH/n-heptane ROH RCl RC(O)OH RNH 3 RN: ROH Low priced replacement cartridges $ Injections 43
44 Conclusions Chemical conversion to CH 4 eliminates the need for standard calibrations in quantification Full conversion and high accuracy for a variety of heteroatoms (O, N, S, Cl, Si and more) Negligible impact on separation performance Long lifetime Available Now! Only at ARC: activatedresearch.com 44
45 Questions? See us at Booth #346 and vote for us in the New Product Showcase Andrew Jones Brad Cleveland Kim Herzog 45
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