• Analytes Determined at Celignis
    Extractives (Ethanol-Soluble)

The Ethanol-Soluble Extractives content is the proportion of the biomass that is lost as a result of extraction with 95% ethanol.

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Analysis Packages for Extractives (Ethanol-Soluble)

The Celignis Analysis Package(s) that determine this constituent are listed below:

Analytical Procedure for Extractives (Ethanol-Soluble)


☑ Step 1: Removal of Ethanol-Soluble Extractives

The steps involved in the removal of 95% ethanol-soluble extractives from samples are listed below:

1. The moisture content of the sample is determined, in duplicate.

2. Two 11 ml capacity DIONEX ASE (Accelerated Solvent Extraction) cells are filled with recorded weights of the sample.

3. The following DIONEX ASE 200 Method is then used on each cell:

   Pressure:   1500 psi
   Temperature:   100 celcius
   Preheat Time:   0 mins
   Heat Time:   5 mins
   Static Time:   7 mins
   Flush Volume:   150%
   Purge Time:   150 s
   Static Cycles:   3
   Solvent:   95% Ethanol


4. A box, of known weight, is taken and the remaining biomass from the extraction cell transferred to it. This is repeated for the other cell.

5. After 2 days each box is weighed again and the moisture content of a subsample of the extracted biomass determined (in duplicate).

6. The weight of extractives is determined as the mass loss in the biomass sample due to extraction in the ASE-200 (corrected for moisture).

Equipment Used for Extractives (Ethanol-Soluble) Analysis



NIR Spectrophotometers

We have several FOSS XDS NIR devices. These have solid content modules, that can allow for samples of a heterogenous particle to be analysed, and liquid modules that allow liquids to be analysed via transmittance spectroscopy.



Solvent Extractor

Dionex ASE-200 devices are used to determine the extractives (water-soluble, ethanol-soluble) contents of biomass samples.

NIR Model

Ethanol-Soluble Extractives Global 1
Min. Value (%)0.00
Max. Value (%)33.24
Calibration Samples472
Validation Samples163
R2 (Validation)0.8822
RMSEP (%)1.7248
Bias (%)-0.0803
SEP (%)1.7283
RPD2.8274
RER18.7991

Publications on Extractives (Ethanol-Soluble) By The Celignis Team

Hayes, D. J. M., Hayes, M. H. B., Leahy, J. J. (2017) Use of Near Infrared Spectroscopy for the Rapid Low-Cost Analysis of Waste Papers and Cardboards, Faraday Discussions 202: 465-482

Link

Analytical data and quantitative near infrared (NIR) spectroscopy models for various lignocellulosic components (including Klason lignin and the constituent sugars glucose, xylose, mannose, arabinose, galactose, and rhamnose), ash, and ethanol-soluble extractives, were obtained for 53 samples of paper and cardboard. These samples were mostly the type of materials typically found in domestic wastes (e.g. newspapers, printing paper, glossy papers, food packaging). A number of the samples (48) were obtained by separating a sample, after milling, into two particle size fractions. It was found that the fractions containing the smaller particles typically had higher ash and Klason lignin contents and lower glucose and xylose contents that the larger particle size fractions. Nevertheless, all of the sample types had attractive total sugars contents (>50%) indicating that these could be suitable feedstocks for the production of biofuels and chemicals in hydrolysis-based biorefining technologies. NIR models of a high predictive accuracy (R2 of > 0.9 for the independent validation set) were obtained for total sugars, glucose, xylose, Klason lignin, and ash and with values for the Root Mean Square Error of Prediction (RMSEP) of 2.36%, 2.64%, 0.56%, 1.98%, and 4.87%, respectively. Good NIR models (R2 of > 0.8) were also obtained for mannose, arabinose, and galactose. These results suggest that NIR is a suitable method for the rapid, low-cost, analysis of the major lignocellulosic components of waste paper/cardboard samples.

Hayes, D. J. M. (2013) Mass and Compositional Changes, Relevant to Biorefining, in Miscanthus x giganteus Plants over the Harvest Window, Bioresource Technology 142: 591-602

Link

Miscanthus plants were sampled from several plantations in Ireland over the harvest window (October-April). These were separated into their anatomical components and the loss of leaves monitored. Three distinct phases were apparent: there was minimal loss in the "Early" (October to early December) and "Late" (March and April) phases, and rapid leaf loss in the interim period. Samples were analysed for constituents relevant to biorefining. Changes in whole-plant composition included increases in glucose and Klason lignin contents and decreases in ash and arabinose contents. These changes arose mostly from the loss of leaves, but there were some changes over time within the harvestable plant components. Although leaves yield less biofuel than stems, the added biomass provided by an early harvest (31.9-38.4%) meant that per hectare biofuel yields were significantly greater (up to 29.3%) than in a late harvest. These yields greatly exceed those from first generation feedstocks.

Hayes, D. J. M. (2012) Development of near infrared spectroscopy models for the quantitative prediction of the lignocellulosic components of wet Miscanthus samples, Bioresource Technology 119: 393-405

Link

Miscanthus samples were scanned over the visible and near infrared wavelengths at several stages of processing (wet-chopped, air-dried, dried and ground, and dried and sieved). Models were developed to predict lignocellulosic and elemental constituents based on these spectra. The dry and sieved scans gave the most accurate models; however the wet-chopped models for glucose, xylose, and Klason lignin provided excellent accuracies with root mean square error of predictions of 1.27%, 0.54%, and 0.93%, respectively. These models can be suitable for most applications. The wet models for arabinose, Klason lignin, acid soluble lignin, ash, extractives, rhamnose, acid insoluble residue, and nitrogen tended to have lower R(2) values (0.80+) for the validation sets and the wet models for galactose, mannose, and acid insoluble ash were less accurate, only having value for rough sample screening. This research shows the potential for online analysis at biorefineries for the major lignocellulosic constituents of interest.

Additional Material

Click here to read more about our methods for analysing extractives.

We can determine the Extractives (Ethanol-Soluble) content of biomass, click here to learn more about our various biomass analysis methods.



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