Bio-Oil Analysis Laboratory Procedures

NREL develops laboratory analytical procedures (LAPs) for the analysis of raw and upgraded pyrolysis bio-oils. These standard procedures have been validated and allow for reliable bio-oil analysis.

Procedures

Corrosivity Screening of Pyrolysis Bio-Oils by Short-Term Alloy Exposures
This method allows for rapid screening of a bio-oil’s corrosivity without the need for complex equipment and long-term exposures. A robust and repeatable method for assessing the corrosivity of bio-oils is necessary to remove materials degradation as an obstacle to research, upgrading, use, and storage of bio-oils.

Elemental Analysis of Bio-Oils by Inductively Coupled Plasma Optical Emission Spectroscopy (ICP-OES)
This procedure covers the preparation and analysis of fast pyrolysis and catalytic fast pyrolysis bio-oils. It includes two methods for quantification of inorganic elements by inductively coupled plasma optical emission spectroscopy (ICP-OES). Procedure A uses microwave-assisted digestion with concentrated nitric acid, and Procedure B is an organic ICP-OES method using a diglyme solvent.

Determination of Phenolic Groups in Bio-Oils Using Revised Folin-Ciocalteu Methods: Single Cuvette and Plate Reader
This procedure covers the determination of phenolic compounds in fast pyrolysis oils. It includes two methods: the first allows for shorter analysis time at increased reaction temperature, while the second employs a longer analysis time but at room temperature. Additionally, the method presents the use of both a single cuvette and a plate reader.

Determination of Biogenic Content by ¹⁴C in Fuels Using Liquid Scintillation Analysis
This procedure covers the determination of the biogenic content (quantified via percent ¹⁴C) in biogenic gasoline, jet fuel, and diesel range hydrocarbons prepared from distillation of hydrotreated pyrolysis oils and blended with fossil derived hydrocarbons (e.g., fossil diesel, gasoline, jet, or toluene).

Determination of Carbon Functional Groups in Pyrolysis Bio-Oils Using ¹³C NMR
This procedure quantifies different carbons in the different functional groups in pyrolysis bio-oils, including carboxyl groups; aromatic C-O, C-C, and C-H bonds; six different carbons in levoglucosan; aliphatic C-O and C-C bonds; methoxyl groups; and two different methyl groups.

Determination of Water Content in Bio-Oils by Volumetric Karl Fischer Titration
This method analyzes the concentration of water in fast pyrolysis oil, catalytic fast pyrolysis oil, and aqueous phases isolated from these products. Other products can be measured using this technique if water concentration is within the approximate range of 0.1 to 100 wt%.

Determination of Carbon, Hydrogen, Nitrogen, and Oxygen in Bio-Oils
This procedure uses combustion analysis to determine the weight percent of carbon, hydrogen, and nitrogen in fast pyrolysis oil (FP), catalytic fast pyrolysis oil (CFP), distillate range hydrotreated oil products, and aqueous phases isolated from FP and CFP oils.

Accelerated Aging of Fast Pyrolysis Bio-Oil Using Carbonyl Titration
Bio-oils change both physically and chemically during storage. This procedure accelerates the aging of fast pyrolysis bio-oils and can be used to gauge how a sample has changed, or will change, with varying times of storage at room temperature.

Determination of Carbonyls in Pyrolysis Bio-Oils by Potentiometric Titration: Faix Method
This procedure uses potentiometric titration to quantify carbonyl functional groups in raw pyrolysis bio-oils. Carbonyl groups are characterized as the sum of aldehydes and ketones.

Acid Number Determination of Pyrolysis Bio-Oils Using Potentiometric Titration
This procedure measures the acidic content of bio-oils using potentiometric titration. Acid content is characterized through both the carboxylic acid number (CAN) and the total acid number (TAN).

Determination of Hydroxyl Groups in Pyrolysis Bio-Oils Using ³¹P NMR
This procedure uses phosphorus-31 nuclear magnetic resonance (³¹P NMR) to quantify three different hydroxyl groups (-OH) in pyrolysis bio-oil: aliphatic-OH, phenolic-OH, and carboxylic-OH.

Quantification of Semi-Volatile Oxygenated Components of Pyrolysis Bio-Oil by Gas Chromatography/Mass Spectrometry (GC/MS)
This procedure quantifies semi-volatile oxygenated compounds present in raw bio-oils produced from fast pyrolysis of lignocellulosic feedstocks.

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