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5th International Symposium on Energy from Biomass and Waste Venice, Italy Nov 17-20 2014

“Use of Near Infrared Spectroscopy for the Rapid Low-Cost Analysis of a Wide Variety of L ignocellulosic Feedstocks ”. 5th International Symposium on Energy from Biomass and Waste Venice, Italy Nov 17-20 2014 Dr. Daniel Hayes dan@celignis.com www.celignis.com.

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5th International Symposium on Energy from Biomass and Waste Venice, Italy Nov 17-20 2014

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  1. “Use of Near Infrared Spectroscopy for the Rapid Low-Cost Analysis of a Wide Variety of Lignocellulosic Feedstocks” 5th International Symposium on Energy from Biomass and Waste Venice, Italy Nov 17-20 2014 Dr. Daniel Hayes dan@celignis.com www.celignis.com

  2. www.carbolea.ul.ie“Oil from Carbohydrates” “One-day analysis of biomass” www.celignis.com

  3. Carbolea Research Group • Focused on the non-biological methods for obtaining value from biomass. Biochar and Soils Rapid Biomass Analysis Heterogeneous Catalysis Pyrolysis + Gasification Bio-Oil Upgrading Chemical Conversion “One-day analysis of biomass” www.celignis.com

  4. DIBANET…Chemical hydrolysis for biofuel and platform chemical production www.dibanet.org

  5. Important Chemical Properties • Hydrolysis process (e.g. enzymatic hydrolysis). • C6 Sugars: Glucose, Galactose, Mannose • C5 Sugars: Arabinose, Xylose • Lignin content (acid soluble and insoluble) • Extractives • Ash. • Thermal (e.g. combustion) and thermochemical (e.g. pyrolysis and gasification). • Elemental analysis (C, H, N, O, S) • Heating value • Ash • Anions and cations. “One-day analysis of biomass” www.celignis.com

  6. Time for Conventional Analysis Wet Chopped Sample Sample as Collected Dry Sample Air Drying ~ 3+ days Chop sample ~ 10 mins Milling + sieving ~ 1 hour Extractives-free sample Hydrolysis and hydrolysate analysis ~ 3 days Extractives Removal ~ 3 days Completed Lignocellulosic Analysis ~ 10 days !!!! Dry Sample of Appropriate Particle Size “One-day analysis of biomass” www.celignis.com

  7. Interaction of NIR Light with Biomass Specular Reflectance Diffuse Reflectance Absorption Transmittance Refraction Scattering “One-day analysis of biomass” www.celignis.com

  8. NIR Analysis • FOSS XDS Monochromator. • 400-2500nm (visible and NIR). • Moving sample transport for inhomogeneous/wet samples. “One-day analysis of biomass” www.celignis.com

  9. Sample Preparation Process Sample Collected Dry & Ground Wet & Unground Dry & Unground “One-day analysis of biomass” www.celignis.com

  10. Scans of One Sample “One-day analysis of biomass” www.celignis.com

  11. Development of NIR Models (1) • Target: Predict composition using NIR spectra. • Consider a spectrum as a vector with a dimension equal to the number of variables (wavelengths). • xi = (A400 A400.5 A401 …. A2499.5 A2500) • 4200 datapoints • A matrix can be built from the spectra of all samples in the model • X = A1,400 A1,400.5 A1,401 …. A1,2499.5 A1,2500 A2,400 A2,400.5 A2,401 …. A2,2499.5 A2,2500 … An,400 An,400.5 An,401 …. An,2499.5 An,2500 “One-day analysis of biomass” www.celignis.com

  12. Development of NIR Models (2) • Celignis models are based on Partial Least Squares (PLS1) regression that determines latent variables that consider the variation in X, Y (compositional data) and correlation between X and Y. • Reduces dimensionality of data (e.g. 4200 variables reduced to 7factors). • The loadings for each factor describe its relation to the manifest variables (which ones are important). • Each sample will have a score for each factor, describing its location on the new coordinate axes of the reduced dimension subspace. • Models are built on a set of samples (calibration set) and then tested on an independent set of samples (validation set). “One-day analysis of biomass” www.celignis.com

  13. 13 Constituents Predicted

  14. Types of Samples Included “One-day analysis of biomass” www.celignis.com

  15. Important Regression Statistics • R2 for the validation set. • RMSEP. • RER (range error ratio) = Range/SEP. • RER > 15 model is good for quantification. • RER 10-15, screening control. • RER 5-10, rough sample screening. “One-day analysis of biomass” www.celignis.com

  16. Results for Prediction Set “One-day analysis of biomass” www.celignis.com

  17. Regression Plot – Total Sugars “One-day analysis of biomass” www.celignis.com

  18. Regression Plot – Klason Lignin “One-day analysis of biomass” www.celignis.com

  19. Results for Prediction Set “One-day analysis of biomass” www.celignis.com

  20. Results for Prediction Set “One-day analysis of biomass” www.celignis.com

  21. Feedstock-Specific Models “One-day analysis of biomass” www.celignis.com

  22. Miscanthus Models • Approx. 115 Miscanthus plants sampled. • These plants were separated according to the fractions, resulting in a total of around 700 samples. • “I” = Internodes • “N” = Nodes (each plant also sampled by the metre). • “K” = Live leaves (>60% green by visual inspection) • “M” = Live Sheaths • “F” = Dead leaves (<60% green by visual inspection) • “H” = Dead sheaths • “FL” = Flowers • “WP” = Whole plant (sometimes separate metre sections are collected) • All samples analysed via NIRS, selected samples via processed to DS/DF state and analysed via wet-chemical methods. “One-day analysis of biomass” www.celignis.com

  23. Models for Miscanthus Klason Lignin Glucan Xylan “One-day analysis of biomass” www.celignis.com

  24. Models for Miscanthus “One-day analysis of biomass” www.celignis.com

  25. Time for Conventional Analysis Wet Chopped Sample Sample as Collected Dry Sample Air Drying ~ 3+ days Chop sample ~ 10 mins Milling + sieving ~ 1 hour Extractives-free sample Hydrolysis and hydrolysate analysis ~ 3 days Extractives Removal ~ 3 days Completed Lignocellulosic Analysis ~ 10 days !!!! Dry Sample of Appropriate Particle Size “One-day analysis of biomass” www.celignis.com

  26. Discriminant Analysis • Plant fraction: Stem section vs. leaf section. • Plant fraction (detailed): internode; node; live leaf blade; dead leaf blade; dead leaf sheath. • Harvest period: Early (Oct-Dec) vs. Late (Mar-Apr). • Stand age: 1 year vs. over one year. • Variety: Miscanthus x giganteus vs. other varieties “One-day analysis of biomass” www.celignis.com

  27. Waste Papers/Cardboards “One-day analysis of biomass” www.celignis.com

  28. Results for Prediction Set “One-day analysis of biomass” www.celignis.com

  29. Celignis Analytical • Launched July 2014. • Based on personal experience 10 yrs. • Work on NIR models ~ 20 person-years. • Provision of characterisation services for biomass (lignocellulosic and thermal properties). • NIR data provided within 24 hoursof receiving a sample. “One-day analysis of biomass” www.celignis.com

  30. Remove Risk from NIR Analysis… • NIR analysis carried out without payment. • Figures for Deviation in Prediction for the Total Sugars and KL contents provided for free. • Can then decide whether to pay for NIR data, wet-chemical analysis, or nothing! • All operations carried out online with interactive database… “One-day analysis of biomass” www.celignis.com

  31. “One-day analysis of biomass” www.celignis.com

  32. Future Plans • Further improve models with more samples. • Develop a local calibration algorithm do develop unique models for each sample to be predicted (only select relevant samples for calibration set). • Develop models for thermochemical properties (C/H/N/S, heating value, volatile matter, fixed carbon etc.) using existing sample database (1,700 samples) and new samples. • Open to collaboration in future Horizon 2020/JTI research projects for models for new feedstocks or analytes. “One-day analysis of biomass” www.celignis.com

  33. Acknowledgements • This work was part funded by: • DIBANET project, funded by the European Community’s Seventh Framework Programme (FP7/2007–2013), grant agreement #227248-2. • Irish Department of Agriculture Fisheries and Food • Irish EPA. • Irish Research Council for Science Engineering and Technology (IRCSET). • Enterprise Ireland. • Limerick Local Enterprise Office. • Assistance provided by colleagues at University of Limerick and Carbolea. “One-day analysis of biomass” www.celignis.com

  34. Website: www.celignis.com “One-day analysis of biomass” www.celignis.com

  35. Thank You! www.celignis.com dan@celignis.com (353) 89 455 5582

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