High resolution FT-ICR mass spectral analysis of bio-oil and residual water soluble organics produced by hydrothermal liquefaction of the marine microalga Nannochloropsis salina

Sudasinghe, Nilusha; Dungan, Barry; Lammers, Peter J.; Albrecht, Karl; Elliott, D.C.; Hallen, Richard T.; Schaub, Tanner

doi:10.1016/j.fuel.2013.11.019

Cited by 160 publications

(106 citation statements)

References 51 publications

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“…3 presented that the major components of aqueous fraction were N&O-heterocyclic compounds, which was different from those of bio-crude oil. Sudasinghe et al [32] carried out a detailed compositional characterization of a bio-crude oil and aqueous by-product from hydrothermal liquefaction of Nannochloropsis saline by direct infusion Fourier Transform Ion Cyclotron Resonance Mass Spectrometry (FT-ICR MS) and reported similar results to those obtained in the present study. Saturated & unsaturated hydrocarbons were barely found due to the low solubility in water molecules.…”

Section: Characterization Of Aqueous Fractionsupporting

confidence: 85%

An investigation of reaction pathways of hydrothermal liquefaction using Chlorella pyrenoidosa and Spirulina platensis

Gai

Zhang

Chen

et al. 2015

Energy Conversion and Management

248

109

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a b s t r a c tLow-lipid microalgae can be successfully converted to bio-crude oil in a hydrothermal liquefaction (HTL) environment. This study examined the behavior of hydrothermal liquefaction of two low-lipid content microalgae in subcritical water between 200°C and 320°C at 20°C intervals. Under these conditions, the chemical composition and functional groups for the bio-crude oil and aqueous fraction were analyzed. Results indicated that reaction temperature greatly affected the distribution of chemical composition and functional groups of HTL bio-crude oil and aqueous fraction. The bio-crude oil with a higher percentage of aliphatic functional groups was obtained at higher reaction temperatures (280-320°C). Besides, the aqueous fraction recovered under the same operating conditions had a lower concentration of nitrogenous organic compounds (NOCs) with two or more methyl groups. The general reaction network for HTL of low-lipid microalgae was proposed. The specific reaction pathways for microalgae substrates were analyzed in terms of lipid, protein and non-fibrous carbohydrate based on the spectral analysis.

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Section: Characterization Of Aqueous Fractionsupporting

confidence: 85%

An investigation of reaction pathways of hydrothermal liquefaction using Chlorella pyrenoidosa and Spirulina platensis

Gai

Zhang

Chen

et al. 2015

Energy Conversion and Management

248

109

View full text Add to dashboard Cite

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“…ESI MS n measurements for structure elucidation were not available for these ions due to the high complexity of the sample. The observed compounds likely correspond to long-chain diamines, alkyl-substituted imidazoles (DBE=3), or alkylated pyrazines (DBE=4) as reported for N. salina HTL oil in previous work [18].…”

Section: Class Analysissupporting

confidence: 67%

“…Therefore, even if a high oil yield is obtained from low-lipid microalgae at higher processing temperature, elevated nitrogen and oxygen content will require upgrading for the removal of polar molecules. Among upgrading methods, hydrotreatment is a promising technique for the treatment of these oils, and the efficiency of the process highly depends on the chemical nature of the oil [18,30]. The detailed compositional description of the high-temperature HTL oil shown here will benefit to devise efficient upgrading strategies to produce a high-quality liquid fuel from HTL of microalgae.…”

Section: Resultsmentioning

confidence: 99%

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Temperature-Dependent Lipid Conversion and Nonlipid Composition of Microalgal Hydrothermal Liquefaction Oils Monitored by Fourier Transform Ion Cyclotron Resonance Mass Spectrometry

et al. 2015

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We illustrate a detailed compositional characterization of hydrothermal liquefaction (HTL) oils derived from two biochemically distinct microalgae, Nannochloropsis gaditana and Chlorella sp. (DOE 1412), for a range of reaction temperature as observed by high-resolution electrospray ionization Fourier transform ion cyclotron resonance mass spectrometry (ESI FT-ICR MS). The unique capability to unequivocally derive molecular formulae directly from FT-ICR MS-measured mass-to-charge ratio (for several thousand compounds in each oil) shows that lipids are completely reacted/converted for any reaction temperature above 200°C and reveals the formation of nonlipid reaction products with increasing temperature. Specifically, lipid-rich oil is obtained at low reaction temperature (<225°C) for both microalgal strains. For positive ion mode, the major lipid components in Chlorella sp. and N. gaditana HTL oils are betaine lipids and acylglycerols, respectively. Acidic species in the HTL oils (observed by negative ion mode) are dominated by free fatty acids (FFA) regardless of reaction temperature. HTL oils obtained at higher temperatures (≥225°C) are composed of a variety of basic nitrogen-and oxygen-containing compounds that originate from protein and carbohydrate degradation at elevated temperature. Similar structural features are observed for the abundant nitrogen heterocyclics between the two strains with slightly lower carbon number for Chlorella sp., overall.

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“…For ESI(+), the predominant classes were of the general formula N x O y (x=1-3 and y=0-3), the most abundant of which was the N 2 class. Pyridine (N) and imidazole and pyrazine derivatives (N 2 ) are common constituents of the basic fractions of organic matter [24]. That is, the assigned classes always contained a N atom, which facilitates protonation.…”

Section: Discussionmentioning

confidence: 99%

Comprehensive Characterization of Second-Generation Biofuel from Invasive Freshwater Plants by FT-ICR MS

Santos

Silva

et al. 2015

Bioenerg. Res.

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Ultra-high resolution and mass accuracy Fourier transform-ion cyclotron resonance mass spectrometry (FT-ICR MS) with an electrospray ionization source (ESI) was applied to characterize the bio-oils that were obtained using a micropyrolysis process of alternative biomasses from Eichornia crassipes (water hyacinth), Eichornia azurea, and Nymphaea ssp. The methods that have been developed for petroleomic analyses using FT-ICR MS data from crude oils and derivatives have been successfully employed herein to process such data for bio-oils, which are known as secondgeneration liquid biofuels. Class distributions and DBE versus carbon number plots (DBE×Cn) were, therefore, obtained. The class distribution for the oil obtained from water hyacinth was similar to those of classical bio-oils and appeared to be applicable as a fingerprint for bio-oils in general. The N 2 and O 2 classes obtained via ESI(+) and the O 2 and O 3 classes obtained via ESI(−) were the major classes detected in the bio-oil samples. In the DBE x Cn plot of the ESI(−)-FT-ICR MS data, the distribution of saturated and unsaturated fatty acids could be visualized, and characteristic profiles were determined for each bio-oil. It is, therefore, demonstrated that the FT-ICR MS methodology that is commonly applied to petroleomic studies can also be applied to biofuel characterization in a comprehensive Bbio-oilomics^approach.

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High resolution FT-ICR mass spectral analysis of bio-oil and residual water soluble organics produced by hydrothermal liquefaction of the marine microalga Nannochloropsis salina

Cited by 160 publications

References 51 publications

An investigation of reaction pathways of hydrothermal liquefaction using Chlorella pyrenoidosa and Spirulina platensis

An investigation of reaction pathways of hydrothermal liquefaction using Chlorella pyrenoidosa and Spirulina platensis

Temperature-Dependent Lipid Conversion and Nonlipid Composition of Microalgal Hydrothermal Liquefaction Oils Monitored by Fourier Transform Ion Cyclotron Resonance Mass Spectrometry

Comprehensive Characterization of Second-Generation Biofuel from Invasive Freshwater Plants by FT-ICR MS

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