As interest in lignocellulosic biomass feedstocks for conversion into transportation fuels grows, the summative compositional analysis of biomass, or plant-derived material, becomes ever more important. The sulfuric acid hydrolysis of biomass has been used to measure lignin and structural carbohydrate content for more than 100 years. Researchers have applied these methods to measure the lignin and structural carbohydrate contents of woody materials, estimate the nutritional value of animal feed, analyze the dietary fiber content of human food, compare potential biofuels feedstocks, and measure the efficiency of biomass-to-biofuels processes. The purpose of this paper is to review the history and lineage of biomass compositional analysis methods based on a sulfuric acid hydrolysis. These methods have become the de facto procedure for biomass compositional analysis. The paper traces changes to the biomass compositional analysis methods through time to the biomass methods currently used at the National Renewable Energy Laboratory (NREL). The current suite of laboratory analytical procedures (LAPs) offered by NREL is described, including an overview of the procedures and methodologies and some common pitfalls. Suggestions are made for continuing improvement to the suite of analyses.

The U.S. Department of Energy (DOE) promotes the production of a range of liquid fuels and fuel blendstocks from lignocellulosic biomass feedstocks by funding fundamental and applied research that advances the state of technology in biomass collection, conversion, and sustainability. As part of its involvement in this program, the National Renewable Energy Laboratory (NREL) investigates the conceptual production economics of these fuels.Between 1999 and 2012, NREL conducted a campaign to quantify the economic implications associated with measured conversion performance for the biochemical production of cellulosic ethanol, with a formal program between 2007-2012 to set cost goals and to benchmark annual performance toward achieving these goals, namely the pilot-scale demonstration by 2012 of biochemical ethanol production at a price competitive with petroleum gasoline based on modeled assumptions for an "n th " plant biorefinery. This goal was successfully achieved through NREL's 2012 pilot plant demonstration runs, representing the culmination of NREL research focused specifically on cellulosic ethanol, and a benchmark for industry to leverage as it commercializes the technology. This important milestone also represented a transition toward a new Program focus on infrastructure-compatible hydrocarbon biofuel pathways, and the establishment of new research directions and cost goals across a number of potential conversion technologies.This report describes in detail one potential conversion process to hydrocarbon products by way of biological conversion of lignocellulosic-derived sugars. The pathway model leverages expertise established over time in core conversion and process integration research at NREL, while adding in new technology areas primarily for hydrocarbon production and associated processing logistics. The overarching process design converts biomass to a hydrocarbon intermediate, represented here as a free fatty acid, using dilute-acid pretreatment, enzymatic saccharification, and bioconversion. Ancillary areas-feed handling, hydrolysate conditioning, product recovery and upgrading (hydrotreating) to a final blendstock material, wastewater treatment, lignin combustion, and utilities-are also included in the design. Detailed material and energy balances and capital and operating costs for this baseline process are also documented.This benchmark case study techno-economic model provides a production cost for a cellulosic renewable diesel blendstock (RDB) that can be used as a baseline to assess its competitiveness and market potential. It can also be used to quantify the economic impact of individual conversion performance targets and prioritize these in terms of their potential to reduce cost. The analysis presented here also includes consideration of the life-cycle implications of the baseline process model, by tracking sustainability metrics for the modeled biorefinery, including greenhouse gas (GHG) emissions, fossil energy demand, and consumptive water use.Building on prior design reports for bioch...

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from the National Renewable Energy Laboratory (NREL) for helpful discussions, comments, and shared insights during the development of this report. We appreciate all of the help from Kathy Cisar for her technical editing and support in publishing this report. Finally, we thank Billie Christen from the NREL for her help in formatting this report and for developing the U.S. bioproduct facilities map.

The most common procedures for characterizing the chemical components of lignocellulosic feedstocks use a two-stage sulfuric acid hydrolysis to fractionate biomass for gravimetric and instrumental analyses. The uncertainty (i.e., dispersion of values from repeated measurement) in the primary data is of general interest to those with technical or financial interests in biomass conversion technology. The composition of a homogenized corn stover feedstock (154 replicate samples in 13 batches, by 7 analysts in 2 laboratories) was measured along with a National Institute of Standards and Technology (NIST) reference sugar cane bagasse, as a control, using this laboratory's suite of laboratory analytical procedures (LAPs). The uncertainty was evaluated by the statistical analysis of these data and is reported as the standard deviation of each component measurement. Censored and uncensored versions of these data sets are reported, as evidence was found for intermittent instrumental and equipment problems. The censored data are believed to represent the “best case” results of these analyses, whereas the uncensored data show how small method changes can strongly affect the uncertainties of these empirical methods. Relative standard deviations (RSD) of 1−3% are reported for glucan, xylan, lignin, extractives, and total component closure with the other minor components showing 4−10% RSD. The standard deviations seen with the corn stover and NIST bagasse materials were similar, which suggests that the uncertainties reported here are due more to the analytical method used than to the specific feedstock type being analyzed.

Corn stover is one of the leading feedstock candidates for commodity-scale biomass-to-ethanol processing. The composition of water-soluble materials in corn stover has been determined with greater than 90% mass closure in four of five representative samples. The mass percentage of water-soluble materials in tested stover samples varied from 14 to 27% on a dry weight basis. Over 30 previously unknown constituents of aqueous extracts were identified and quantified using a variety of chromatographic techniques. Monomeric sugars (primarily glucose and fructose) were found to be the predominant water-soluble components of corn stover, accounting for 30-46% of the dry weight of extractives (4-12% of the dry weight of feedstocks). Additional constituents contributing to the mass balance for extractives included various alditols (3-7%), aliphatic acids (7-21%), inorganic ions (10-18%), oligomeric sugars (4-12%), and a distribution of oligomers tentatively identified as being derived from phenolic glycosides (10-18%).

Pioneer cellulosic biorefi neries across the United States rely on a conventional feedstock supply system based on one-year contracts with local growers, who harvest, locally store, and deliver feedstock in low-density format to the conversion facility. While the conventional system is designed for high biomass yield areas, pilot scale operations have experienced feedstock supply shortages and price volatilities due to reduced harvests and competition from other industries. Regional supply dependency and the inability to actively manage feedstock stability and quality, provide operational risks to the biorefi nery, which translate into higher investment risk. The advanced feedstock supply system based on a network of depots can mitigate many of these risks and enable wider supply system benefi ts. This paper compares the two concepts from a system-level perspective beyond mere logistic costs. It shows that while processing operations at the depot increase feedstock supply costs initially, they enable wider system benefi ts including supply risk reduction (leading to lower interest rates on loans), industry scale-up, conversion yield improvements, and reduced handling equipment and storage costs at the biorefi nery. When translating these benefi ts into cost reductions per liter of gasoline equivalent (LGE), we fi nd that total cost reductions between -$0.46 to -$0.21 per LGE for biochemical and -$0.32 to -$0.12 per LGE for thermochemical conversion pathways are possible. Naturally, these system level benefi ts will differ between individual actors along the feedstock supply chain. Further research is required with respect to depot sizing, location, and ownership structures. Published 2015. This article is a U.S. Government work and is in the public domain in the USA. Biofuels, Bioproducts and Biorefi ning published by Society of Industrial Chemistry and John Wiley & Sons Ltd. Supporting information may be found in the online version of this article.Keywords: biorefi nery; feedstock logistics; depot; bioeconomy; biofuel; advanced feedstock supply system 3 Targets are generally iterated between advancements in feedstock logistics and the development of more robust conversion systems. But it remains unclear if a conventional system will allow for the current goal to be met. Diff erent analyses 4-7 have shown that the conventional system fails to meet this supply cost target outside of highly productive regions and could encounter issues even in highly productive regions in some years due to inclement weather (e.g., drought, fl ood, heavy moisture during harvest, etc.). Th ese supply uncertainties increase risks, which could limit the biorefi nery concept from being broadly implemented.