• Rapid Biomass Analysis
    Using NIR


Celignis has developed unique proprietary models that allow the lignocellulosic composition of biomass samples to be predicted from their near infrared (NIR) spectra. This service is offered in Analysis Package P11 (NIR Prediction Package). That Package provides the following advantages over the standard wet-chemical methods for analysis:

  - Rapid Analysis:

  We typically provide data within one day of receipt of the samples.

- Lower Cost:

  The NIR method involves less laboratory work than the wet-chemical analytical methods which allows us to provide the service at a lower cost.

 
  • Effective Sample Screening:

      As a result of the increased speed and reduced cost of analysis the NIR method allows a far greater number of samples to be analysed than would otherwise be possible with standard methods. This means that you can screen more samples in order to find those that are most appropriate for your desired end-use.


  • Request a QuoteNIR Analysis



    Analytes Determined

    We have developed NIR models for a range of compositional parameters of importance for the production of advanced biofuels. These parameters are listed below, click on an entry to see statistics concerning the accuracy of the NIR model in predicting that constituent.
    These models have been developed based on wet-chemical data obtained from biomass samples that have had their ethanol-soluble extractives removed and then been put through an acid-hydrolysis process to determine their sugars and lignin composition.

    Suitable Feedstocks for NIR Analysis

    The data and spectra of thousands of samples have been used to construct our NIR models. Listed below are just some of the biomass types that have been used to build these models. By covering such a wide variety of biomass feedstocks, and with numerous samples collected for each feedstock (covering different conditions such as: plant variety, time of year, productivity, and region/environment), our models are highly robust and able to predict the composition of any lignocellulosic sample.

    Confidence in Our Analysis

    We use formulae to estimate the Deviation in Prediction for the compositonal values that our NIR models predict. This deviation represents a form of a confidence interval with regards to the prediction. For example, a deviation of 1% in a predicted Klason lignin content of 15% suggests that the real Klason lignin content of the sample is likely to be in the range of 14-16%. Approximately 95% of the samples in our independent prediction set had actual compositional values, determined by wet-chemistry, that were within the range of the NIR predicted value +/- 2 times the Deviation in Prediction.

    At Celignis, we pride ourselves on the accuracy and precision of our analysis. Customer satisfaction is of paramount importance. For our NIR Analysis Package, if we find that the deviation in prediction is relatively high (defined as a value over 3% for the total lignocellulosic sugars content) then we will undertake the chemical analysis of that sample at no extra charge and provide you with all of the data that we obtain in this analysis. This chemical analysis will cover the analysis packages that we used to develop our NIR models: P3 - Ash Content, P4 - Ethanol Extractives, and P9 - Lignocellulosic Sugars and Lignin.

    Request a QuoteNIR Analysis



    Publications on NIR Analysis 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.

    Wnetrzak, R., Hayes, D. J. M., Jensen, L. S., Leahy, J. J., Kwapinski, W. (2015) Determination of the higher heating value of pig manure, Waste and Biomass Valorization 6(3): 327-333

    Link

    The ability of using novel method of near infrared (NIR) spectra to predict the composition and higher heating value (HHV) of dry pig manure was examined. Number of pig manure solid fractions variously pre-treated samples were collected in Denmark, from different pig slurry treatment plants (using mechanical or chemical-mechanical separation) and then analysed for their energy values. These values were determined by conventional method using bomb calorimetry and also calculated based on ultimate analysis. NIR spectra method was successfully applied and reasonable R2 values were obtained for the independent prediction set for nitrogen, ash, and the HHV. NIR also showed ability for predicting which type of treatment plants the samples came from. In addition, new empirical equations, based on ultimate analyses of pig manure solids used for prediction of the HHV was established.

    Hayes, D. J. M., Hayes, M. H. B., Leahy, J. J. (2015) Analysis of the lignocellulosic components of peat samples with development of near infrared spectroscopy models for rapid quantitative predictions, Fuel 150: 261-268

    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), moisture, and ash were obtained for 53 peat samples. These included samples with high, medium, and low degrees of humification. Klason lignin was the main constituent and was greatest in the samples classified as being highly humified, with structural sugars the lowest in this class. The total sugars contents of all samples were considered to be insufficient to allow for their use in biorefining hydrolysis processes for the production of chemicals and biofuels. NIR models were developed for spectral datasets obtained from the samples in their unprocessed (wet), dry and unground, and dry and ground states. Typically the most accurate models were based on the spectra of dry and ground samples. However the NIR models for the wet samples still offered reasonable predictive capabilities. All models were suitable at least for sample screening, with the models for total sugars, glucose, xylose, galactose, and moisture suitable for quantitative analyses.

    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.

    Hayes, D. J. M. (2011) Analysis of Lignocellulosic Feedstocks for Biorefineries with a Focus on The Development of Near Infrared Spectroscopy as a Primary Analytical Tool, PhD Thesis832 pages (over 2 volumes)

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    The processing of lignocellulosic materials in modern biorefineries will allow for the production of transport fuels and platform chemicals that could replace petroleum-derived products. However, there is a critical lack of relevant detailed compositional information regarding feedstocks relevant to Ireland and Irish conditions. This research has involved the collection, preparation, and the analysis, with a high level of precision and accuracy, of a large number of biomass samples from the waste and agricultural sectors. Not all of the waste materials analysed are considered suitable for biorefining; for example the total sugar contents of spent mushroom composts are too low. However, the waste paper/cardboard that is currently exported from Ireland has a chemical composition that could result in high biorefinery yields and so could make a significant contribution to Irelandís biofuel demands.

    Miscanthus was focussed on as a major agricultural feedstock. A large number of plants have been sampled over the course of the harvest window (October to April) from several sites. These have been separated into their anatomical fractions and analysed. This has allowed observations to be made regarding the compositional trends observed within plants, between plants, and between harvest dates. Projections are made regarding the extents to which potential chemical yields may vary. For the DIBANET hydrolysis process that is being developed at the University of Limerick, per hectare yields of levulinic acid from Miscanthus could be 20% greater when harvested early compared with a late harvest.

    The wet-chemical analysis of biomass is time-consuming. Near infrared spectroscopy (NIRS) has been developed as a rapid primary analytical tool with separate quantitative models developed for the important constituents of Miscanthus, peat, and (Australian) sugarcane bagasse. The work has demonstrated that accurate models are possible, not only for dry homogenous samples, but also for wet heterogeneous samples. For glucose (cellulose) the root mean square error of prediction (RMSEP) for wet samples is 1.24% and the R2 for the validation set ( ) is 0.931. High accuracies are even possible for minor analytes; e.g. for the rhamnose content of wet Miscanthus samples the RMSEP is 0.03% and the is 0.845. Accurate models have also been developed for pre-treated Miscanthus samples and are discussed. In addition, qualitative models have been developed. These allow for samples to be discriminated for on the basis of plant fraction, plant variety (giganteus/non-giganteus), harvest-period (early/late), and stand-age (one-year/older).

    Quantitative NIRS models have also been developed for peat, although the heterogeneity of this feedstock means that the accuracies tend to be lower than for Miscanthus. The development of models for sugarcane bagasse has been hindered, in some cases, by the limited chemical variability between the samples in the calibration set. Good models are possible for the glucose and total sugars content, but the accuracy of other models is poorer. NIRS spectra of Brazilian bagasse samples have been projected onto these models, and onto those developed for Miscanthus, and the Miscanthus models appear to provide a better fit than the Australian bagasse models.



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