Analytical tools for evaluating algal biodiesel production collin beal - may 2010
1. Analytical Tools for Evaluating Algal
Biodiesel Production
Beal C.M., Webber M.E., Ruoff R.S.,
Hebner R.E., Romanovicz D., and Connelly R.
ES2010-90277
May 21st, 2010
2. Algal biodiesel production can be
represented in three steps
Beal C.M. et al., “A Framework to Report the Production of Biodiesel from Algae,”
BioEnergy Research, In Review. Colin M Beal
ASME 2010
2 ES2010-90277
May 21, 2010
3. Algal biodiesel production can be
represented in three steps
Three commonly studied pathways are:
1) Transesterification of Algal Lipids
2) Thermochemical Conversion of Algal Biomass
3) Excretion of Oils by Genetically Modified Organisms
Colin M Beal
ASME 2010
3 ES2010-90277
May 21, 2010
4. Transesterification of Algal Lipids
Beal et al., “A Framework to Report the Production of Biodiesel from Algae,” BioEnergy
Research, In Review.
Colin M Beal
ASME 2010
4 ES2010-90277
May 21, 2010
5. The Center for Electromechanics at UT-
Austin has a multi-disciplinary team
I would like to acknowledge:
S. Briggs J. Jones M. Poenie
E. Chen L. Katz M. Randazzo
R. Connelly K. Kinney D. Schmid
J. Choi M. Montoya F. Seibert
M. Fountain B. Morrison J. Van Reet
R. Hebner R. Pearsall M. Werst
I would like to thank OpenAlgae for funding:
Colin M Beal
ASME 2010
5 ES2010-90277
May 21, 2010
6. Algae are grown in flasks,
reactors, tanks, and ponds
UT-CEM, 2009-2010
Colin M Beal
ASME 2010
6 ES2010-90277
May 21, 2010
7. Then, the algae are concentrated by ~100X
Multiple harvesting methods are
being evaluated:
1) Centrifugation
2) pH induced floc/defloc
3) Dissolved Air Flotation
4) Electro-flocculation
5) Filtration
6) Resin collection
7) Electro-wicking
UT-CEM, 2009-2010
Colin M Beal
ASME 2010
7 ES2010-90277
May 21, 2010
8. After harvesting, the cells are compromised
with electromechanical pulsing
• Electromechanical pulsing is a cost
effective technology developed at UT-CEM
UT-CEM, 2010
UT-CEM, 2010
Colin M Beal
ASME 2010
8 ES2010-90277
May 21, 2010
9. After harvesting, the cells are compromised
with electromechanical pulsing
• Electromechanical pulsing is a cost
effective technology developed at UT-CEM
Before After
UT-CEM, 2010
Beal C.M., and Romanovicz D., 2008
Colin M Beal
ASME 2010
9 ES2010-90277
May 21, 2010
10. An enhanced coalescence membrane is
used to extract the algal lipids
UT-CEM 2009, 2010
Colin M Beal
ASME 2010
10 ES2010-90277
May 21, 2010
11. The lipids are then upgraded to fuel
Algal lipids are converted to fatty acid methyl
esters, the primary component in biodiesel, by
transesterification.
Colin M Beal
ASME 2010
11 ES2010-90277
May 21, 2010
12. Evaluating the intermediate products
requires many analytical tools
Colin M Beal
ASME 2010
12 ES2010-90277
May 21, 2010
13. Evaluating the intermediate products
requires many analytical tools
Colin M Beal
ASME 2010
13 ES2010-90277
May 21, 2010
14. Generally, microscopy provides structural
information.
1) Light Microscopy
Colin M Beal
ASME 2010
14 ES2010-90277
May 21, 2010
15. Generally, microscopy provides structural
information.
1) Light Microscopy
Fluorescence microscopy using Nile Red dye
Beal C.M., 2008
Colin M Beal
ASME 2010
15 ES2010-90277
May 21, 2010
16. Generally, microscopy provides structural
information.
1) Light Microscopy
2) Scanning Electron Microscopy
- Useful for evaluating electromechanical lysing
Before
Colin M Beal
ASME 2010
16 Beal C.M. and Romanovicz D., 2008, 2010
ES2010-90277
May 21, 2010
17. Generally, microscopy provides structural
information.
1) Light Microscopy
2) Scanning Electron Microscopy
- Useful for evaluating electromechanical lysing
After
Colin M Beal
ASME 2010
17 Beal C.M. and Romanovicz D., 2008, 2010
ES2010-90277
May 21, 2010
18. Generally, microscopy provides structural
information.
1) Light Microscopy
2) Scanning Electron Microscopy
3) Transmission Electron Microscopy
Control Electrically Pulsed
Control: Compact, well-
LB ordered structures.
chloroplasts
G
LB Pulsed: Disordered,
C initiating apoptosis
CW
CW
Chloroplasts (C), Golgi (G),
Cell walls (CW) , Lipid
Bodies (LB)
Beal C.M. and Romanovicz D., 2008
Colin M Beal
ASME 2010
18 ES2010-90277
May 21, 2010
19. Usually, spectroscopy provides composition
analysis
1) UV-Vis Spectrophotometry
- Measure of chlorophyll absorption (a.u.)
- Absorption corresponds to algal density (g/L)
- Algal productivity calculated from changes in algal density
Grown Mass Productivity
Bidwell 1979
Colin M Beal
ASME 2010
19 ES2010-90277
May 21, 2010
20. Usually, spectroscopy provides composition
analysis
1) UV-Vis Spectrophotometry
2) Raman Spectroscopy
Algal Spectra
(Nitrogen Starved Chlorella and Neochloris)
Huang et al., “Micro-Raman Spectroscopy of Algae: Composition Analysis and
Fluorescence Background Behavior,” Biotechnology and Bioengineering, 2010.
Colin M Beal
ASME 2010
20 ES2010-90277
May 21, 2010
21. Usually, spectroscopy provides composition
analysis
1) UV-Vis Spectrophotometry
2) Raman Spectroscopy
Huang et al., “Micro-Raman Spectroscopy of Algae: Composition Analysis and
Fluorescence Background Behavior,” Biotechnology and Bioengineering, 2010.
Colin M Beal
ASME 2010
21 ES2010-90277
May 21, 2010
22. Usually, spectroscopy provides composition
analysis
1) UV-Vis Spectrophotometry
2) Raman Spectroscopy
3) Infrared Spectroscopy (IR)
IR has been used to:
1) Analyze nutrient status in algae
2) Identify algal species
- Some groups are using it for lipid analysis,
but it requires dry samples.
Colin M Beal
ASME 2010
22 ES2010-90277
May 21, 2010
23. Usually, spectroscopy provides composition
analysis
1) UV-Vis Spectrophotometry
2) Raman Spectroscopy
3) Infrared Spectroscopy (IR)
4) Nuclear Magnetic Resonance Spectroscopy (NMR)
Beal et al., “Lipid Analysis of Neochloris oleoabundans
by Liquid State NMR,” Biotechnology and
Bioengineering, 2010.
Colin M Beal
ASME 2010
23 ES2010-90277
May 21, 2010
24. Chromatography also provides composition
analysis, but requires extraction
1) High Performance (Pressure) Liquid Chromatography (HPLC)
Healthy Starved
Signal Signal
(a.u.) (a.u.)
Time Beal C.M., 2009 Time
Acquired by Poenie M.
(min) (min)
Colin M Beal
ASME 2010
24 ES2010-90277
May 21, 2010
25. Chromatography also provides composition
analysis, but requires extraction
1) High Performance (Pressure) Liquid Chromatography (HPLC)
2) Thin Layer Chromatography (TLC)
Polarity
Connelly R., 2009
Processing Samples Lipid Standards
Colin M Beal
ASME 2010
25 ES2010-90277
May 21, 2010
26. Chromatography also provides composition
analysis, but requires extraction
1) High Performance (Pressure) Liquid Chromatography (HPLC)
2) Thin Layer Chromatography (TLC)
3) Gas Chromatography – Mass Spectrometry (GC-MS)
CB062309b #673-677 RT: 6.85-6.87 AV:5 NL: 4.02E6
T: {0,0} + c EI det=450.00 Full ms [ 50.00-400.00]
55.1
100
67.0
74.0
95
90
83.1
85 87.0
MS fragmentation patter for FAME - Provides
80
75
97.1 molecular
70
98.1
information for
65
60 volatile samples.
Relative Abundance
Relative 55
50
110.1
Abundance 45 - Generally
(a.u.)
40
35
123.1
limited to
30
125.1
264.2 biodiesel, or
25
20
137.1
138.1 180.2
222.2 265.2 FAME derived
15
141.0
152.1
166.1
from algae
10
207.0 221.1
5 193.1 223.2 266.3 296.3
246.2 281.0 297.3
327.0 341.0 355.0 383.0 397.0
0
60 80 100 120 140 160 180 200 220 240 260 280 300 320 340 360 380 400
m/z
m/z
Colin M Beal
ASME 2010
26 ES2010-90277
May 21, 2010
27. Summary: Tricks (or tools) of the trade
Colin M Beal
ASME 2010
27 ES2010-90277
May 21, 2010
28. Questions?
Colin M Beal, MS
Graduate Student
Thermal/Fluids Systems Division
Mechanical Engineering
The University of Texas at Austin
cbeal@mail.utexas.edu
Webber Energy Group
Ruoff Nanoscience and Technology Group
and
The Center for Electromechanics
Colin M Beal
ASME 2010
28 ES2010-90277
May 21, 2010
