Skip to main content
SpringerLink
Log in

A Novel Method for Monitoring the Transesterification Reaction of Oil in Biodiesel Production by Estimation of Glycerol

  • Original Paper
  • Published:
Journal of the American Oil Chemists' Society

An Erratum to this article was published on 28 April 2010

Abstract

A quantitative method is reported for the estimation of glycerol during transesterification of oil to form biodiesel. The reagent used to derivatize glycerol was 9,9-dimethoxyfluorene. Glycerol is estimated by both UV–visible spectrophotometric and high performance liquid chromatography methods. Using the former method, detection limits of 0.05% w/w of glycerol in biodiesel was established. Validation of the developed method was done using the Greenhill method for determination of free glycerol formed during the transesterification reaction.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Log in via an institution

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Institutional subscriptions

Scheme 1
Scheme 2
Scheme 3
Scheme 4
Fig. 1
Fig. 2
Fig. 3
Fig. 4
Fig. 5

Similar content being viewed by others

Abbreviations

ASTM:

American Society for Testing and Materials

ATR-FTIR:

Attenuated total reflectance-Fourier transform infrared

CCDC:

Cambridge Crystallographic Data Collection

CE:

Capillary electrophoresis

FAME:

Fatty acid methyl esters

FID:

Flame ionization detection

HPLC:

High performance liquid chromatography

HTGC:

High temperature capillary gas chromatography

NIR:

Near infrared spectroscopy

PTSA:

p-Toluenesulfonic acid

SEC:

Size exclusion chromatography

TG:

Triglycerides

TLC:

Thin layer chromatography

mp.:

Melting point

NMR:

Nuclear magnetic resonance

HRMS:

High resolution mass spectra

RT:

Retention time

References

  1. Murugesan A, Umarani C, Chinnusamy TR, Krishnan M, Subramanian R, Neduzchezhain N (2009) Production and analysis of bio-diesel from non-edible oils. Renew Sustain Energy Rev 13:825–834

    Article  CAS  Google Scholar 

  2. Ma F, Hanna MA (1999) Biodiesel production: a review. Bioresour Technol 70:1–15

    Article  CAS  Google Scholar 

  3. Suppes GJ, Bockwinkel K, Lucas S, Botts JB, Mason MH, Heppert JA (2001) Calcium carbonate catalyzed alcoholysis of fats and oils. J Am Oil Chem Soc 78:139–145

    Article  CAS  Google Scholar 

  4. Basu HN, Norris ME (1996) Process for production of esters for use as a diesel fuel substitute using a non-alkaline catalyst. US Patent 5,525,126

  5. Karmee SK, Chadha A (2005) Preparation of biodiesel from crude oil of Pongamia pinnata. Bioresour Technol 96:1425–1429

    Article  CAS  Google Scholar 

  6. Hsu AF, Jones KC, Foglia TA, Marmer WN (2002) Immobilized lipase-catalysed production of alkyl esters of restaurant grease as biodiesel. Biotechnol Appl Biochem 36:181–186

    Article  CAS  Google Scholar 

  7. Knothe G (2006) Analyzing biodiesel: standards and other methods. J Am Oil Chem Soc 83:823–833

    Article  CAS  Google Scholar 

  8. Monteiro MR, Ambrozin ARP, Liao LM, Ferreira AG (2008) Critical review on analytical methods for biodiesel characterization. Talanta 77:593–605

    Article  CAS  Google Scholar 

  9. Mittelbach M (1996) Diesel fuel derived from vegetable oils, VI: specifications and quality control of biodiesel. Bioresour Technol 56:7–11

    Article  CAS  Google Scholar 

  10. Freedman B, Pryde EH, Kwolek WF (1984) Thin layer chromatography/flame ionization analysis of transesterified vegetable oils. J Am Oil Chem Soc 61:1215–1220

    Article  CAS  Google Scholar 

  11. Cvengros J, Cvengrosova Z, Hoka C (2002) Conversion of acyl glycerols to methyl esters by TLC method. Petrol Coal 44:67

    CAS  Google Scholar 

  12. Bansal K, McCrady J, Hansen A, Bhalerao K (2008) Thin layer chromatography and image analysis to detect glycerol in biodiesel. Fuel 87:3369–3372

    Article  CAS  Google Scholar 

  13. Freedman B, Kwolek WF, Pryde EH (1986) Quantitation in the analysis of transesterified soybean oil by capillary gas chromatography. J Am Oil Chem Soc 63:1370–1375

    Article  CAS  Google Scholar 

  14. Plank C, Lorbeer E (1995) Simultaneous determination of glycerol, and mono-, di-, and triglycerides in vegetable oil methyl esters by capillary gas chromatography. J Chromatogr A 697:461–468

    Article  CAS  Google Scholar 

  15. Holaapek MP, Jandera P, Fischer J, Prok B (1999) Analytical monitoring of the production of biodiesel by high-liquid chromatography with various detection methods. J Chromatogr A 858:13–31

    Article  Google Scholar 

  16. Hajek M, Skopal F, Machek J (2006) Determination of free glycerol in biodiesel. Eur J Lipid Sci Technol 108:666–669

    Article  CAS  Google Scholar 

  17. Foglia TA, Jones KC, Nunez A, Phillips JG, Mittelbach M (2004) Comparison of chromatographic methods for the determination of bound glycerol in biodiesel. Chromatographia 60:305–311

    Article  CAS  Google Scholar 

  18. Gelbard G, Bres O, Vargas RM, Vielfaure F, Schuchardt UF (1995) 1H nuclear magnetic resonance determination of the yield of the transesterification of rapeseed oil with methanol. J Am Oil Chem Soc 72:1239–1241

    Article  CAS  Google Scholar 

  19. Dimmig T, Radig W, Knoll C, Dittmar T (1999) 13C-NMR Spektroskopie zur Bestimmung von Umsatz und Reaktionskinetik der Umesterung von Triglyceriden zu Methylestern [13C NMR spectroscopic determination of the conversion and reaction kinetics of transesterification of triglycerols to methyl esters]. Chem Tech (Leipzig) 51:326–329

    CAS  Google Scholar 

  20. Arzamendi G, Arguinarena E, Campo I, Gandia LM (2006) Monitoring of biodiesel production: simultaneous analysis of the transesterification products using size-exclusion chromatography. Chem Eng J 122:31–40

    Article  CAS  Google Scholar 

  21. Bondioli P, Della Bella L (2005) An alternative spectrophotometric method for the determination of free glycerol in biodiesel. Eur J Lipid Sci Technol 107:153–157

    Article  CAS  Google Scholar 

  22. Filho LCG, Micke GA (2007) Development and validation of a fast method for determination of free glycerol in biodiesel by capillary electrophoresis. J Chromatogr A 1154:477–480

    Article  Google Scholar 

  23. Greenhill S (2004) Method for determination of free and combined glycerin in biodiesel. US Patent WO 2004/059315

  24. Karmee SK, Chandna D, Ravi R, Chadha A (2006) Study of the kinetics of base catalyzed transesterification of triglycerides from Pongamia oil. J Am Oil Chem Soc 83:873–877

    Article  CAS  Google Scholar 

  25. Karmee SK, Mahesh P, Ravi R, Chadha A (2004) Study of the kinetics of base catalyzed transesterification of monoglycerides from Pongamia oil. J Am Oil Chem Soc 81:425–430

    Article  CAS  Google Scholar 

  26. Bakthavachalam V, Lin L-G, Cherian XM, Czarnik AW (1987) Synthesis, stereochemistry, intramolecular cyclization, and rates of hydrolysis of adenosine 2′, 3′-acetals. Carbohydr Res 170:124–135

    Article  CAS  Google Scholar 

  27. Cherian XM, Arman SAV, Czarnik AW (1990) Models for nucleoside glycosylase enzymes: evidence that the hydrolysis of β-d-ribofuranosides requires a backside preassociation nucleophile. J Am Chem Soc 112:4490–4498

    Article  CAS  Google Scholar 

  28. Thurkauf A, Mattson MV, Richardson S, Mirsadeghi S, Ornstein PL, Harrison EA Jr, Rice KC, Jacobson AE, Monnt JA (1992) Analogues of the dioxolanes dexoxadrol and etoxadrol as potential phencyclidine-like agents: synthesis and structure-activity relationships. J Med Chem 35:1323–1328

    Article  CAS  Google Scholar 

  29. Tartaglia S, Padula D, Scafato P, Chiummiento L, Rosini C (2008) A chemical/computational approach to the determination of absolute configuration of flexible and transparent molecules: aliphatic diols as a case study. J Org Chem 73:4865–4873

    Article  CAS  Google Scholar 

  30. Neises B, Steglich W (1978) Simple method for the esterification of carboxylic acids. Angew Chem Int Ed 17:522–524

    Article  Google Scholar 

  31. Zhou H, Lu H, Liang B (2006) Solubility of multicomponent systems in the biodiesel production by transesterification of Jatropha Curcas L. oil with methanol. J Chem Eng Data 51:1130–1135

    Article  CAS  Google Scholar 

  32. Sundharapandian S (2007) Performance and emission analysis of biodiesel operated CI engine. J Eng Comput Archit 1:1–22

    Google Scholar 

  33. Kaul S, Saxena RC, Kumar A, Negi MS, Bhatnagar AK, Goyal HB, Gupta AK (2007) Fuel Process Technol 88:303–307

    Article  CAS  Google Scholar 

Download references

Acknowledgments

Funding from the Department of Science and Technology (DST), Government of India is gratefully acknowledged. The authors thank the Sophisticated Analytical Instrumentation Facility (SAIF), Indian Institute of Technology Madras and Dr. Babu Varghese for the X-ray data collection. The authors also acknowledge valuable suggestions received during the drafting stage from Professor R. Ravi and G. Ravikumar.

Author information

Authors and Affiliations

  1. Laboratory of Bioorganic Chemistry, Department of Biotechnology, Indian Institute of Technology Madras, Chennai, 600 036, India

    Sabbasani Rajasekhara Reddy, Devamani Titu & Anju Chadha

  2. National Center for Catalysis Research, Indian Institute of Technology Madras, Chennai, 600036, India

    Anju Chadha

Authors
  1. Sabbasani Rajasekhara Reddy
    View author publications

    You can also search for this author in PubMed Google Scholar

  2. Devamani Titu
    View author publications

    You can also search for this author in PubMed Google Scholar

  3. Anju Chadha
    View author publications

    You can also search for this author in PubMed Google Scholar

Corresponding author

Correspondence to Anju Chadha.

Additional information

An erratum to this article can be found at http://dx.doi.org/10.1007/s11746-010-1570-5

About this article

Cite this article

Reddy, S.R., Titu, D. & Chadha, A. A Novel Method for Monitoring the Transesterification Reaction of Oil in Biodiesel Production by Estimation of Glycerol. J Am Oil Chem Soc 87, 747–754 (2010). https://doi.org/10.1007/s11746-010-1549-2

Download citation

  • Received:

  • Revised:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s11746-010-1549-2

Keywords

Search

Navigation