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Benchtop methods for measuring the fraction of free liquid of biomass slurries

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Abstract

The free-liquid fraction of slurries is strongly correlated with other slurry properties, especially the rheological and transport properties. Measuring free-liquid fraction can be problematic with lignocellulosic materials, and many studies to-date have instead used the total mass-fraction of liquid as a surrogate measure. This study presents two bench-scale methods for determining the free-liquid content of lignocellulosic biomass slurries. One is based on centrifuge-filtration of biomass for increasing time intervals until an asymptote is observed. The other uses solute exclusion methods and includes a proper accounting for unavoidable adsorption of the tracer solute molecules on the biomass solids. Overall, we found both methods gave reasonable results for washed pretreated corn stover. Among our controls, the centrifuge dewatering method tends to enable better results for large, rigid particles, and can give unrealistic results for small, compressible particles. This tendency is also reflected in the results for different pretreated corn stover slurries, where the quality of the results varied with the particle size distribution of the slurries. The solute exclusion method gives physically realistic results for all of our control materials and for washed pretreated materials, but produced physically unrealistic results for one unwashed pretreated corn stover sample. Further, we show that blue dextran interacts chemically with lignocellulosic material via adsorption and suspected degradation reactions.

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Abbreviations

a :

Empirical Langmuir fitting parameter (–)

c :

Concentration of tracer in free liquid (mg/mL)

k :

Empirical asymptotic fit parameter (–)

m a :

Mass of tracer adsorbed to substrate (mg)

m r :

Mass of liquid removed during centrifuge filtration (g)

m T :

Total mass of sample (g)

m T,avg :

Average total mass of samples (g)

m tr :

Mass of tracer molecule added to the sample (mg)

m u :

Mass of tracer molecule in the sample that is unadsorbed (mg)

m x :

Adsorption capacity of the substrate (mg)

t :

Centrifugation time (min)

V add :

Volume addition to sample from tracer solution (mL)

V l,f :

Volume of free liquid in the sample (mL)

V l,i :

Volume of liquid included within the particles (mL)

V p :

Volume of particles in the sample (mL)

w f :

Mass fraction of free liquid in the sample (–)

w r :

Mass fraction of liquid removed from the sample via centrifuge filtration (–)

w s :

Mass fraction of insoluble solids in the sample (–)

\(\epsilon_l\) :

Volume fraction of particle consisting of liquid (–)

\(\epsilon_s\) :

Volume fraction of particle consisting of solids (–)

ρ l :

Density of liquid in the slurry (g/mL)

ρ p :

Calculated density of the particles within the slurry (g/mL)

ρ s :

Calculated intrinsic density of the solids (g/mL)

ρ T :

Bulk density of the slurry (g/mL)

ϕ f :

Volume fraction of the slurry consisting of free liquid (–)

ϕ p :

Volume fraction of the slurry consisting of particles, including the liquid included within (–)

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Acknowledgments

This work was funded by the U.S. Department of Energy under Contract No. DE-AC36-08-GO28308 with the National Renewable Energy Laboratory through the BioEnergy Technologies Office.

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Correspondence to James J. Lischeske.

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Lischeske, J.J., Nelson, R.S. & Stickel, J.J. Benchtop methods for measuring the fraction of free liquid of biomass slurries. Cellulose 21, 2261–2269 (2014). https://doi.org/10.1007/s10570-014-0185-7

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  • DOI: https://doi.org/10.1007/s10570-014-0185-7

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