Water content of pyrolysis oil: Comparison between Karl Fischer titration, GC/MS-corrected azeotropic distillation and 1H NMR spectroscopy

Smets, Koen; Adriaensens, Peter; Vandewijngaarden, Jens; Stals, Mark; Cornelissen, Tom; Schreurs, Sonja; Carleer, Robert; Yperman, Jan

doi:10.1016/j.jaap.2010.10.010

Cited by 35 publications

(21 citation statements)

References 13 publications

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“…A series of works has either directly addressed the issue of water determination in pyrolytic oils (or just oils) by the Karl-Fischer titration, or has included it in studies of other phenomenon [25][26][27][28][29][30][31]. Choi et al [25] determined a wide spectrum of properties of red oak-derived pyrolytic oil and the water content was determined by Karl-Fischer titration.…”

Section: The Water Content Determinationmentioning

confidence: 99%

“…Meesuk et al [29] examined the effect of temperature on product yields and the composition of rice husk pyrolytic bio-oil and the water content in bio-oil was determined by Karl-Fischer titration. Smets et al [30] dealt with comparison between the Karl Fischer titration, GC/MS-corrected azeotropic distillation and 1H NMR spectroscopy. All three methods had comparable results and were free of interferences, only for samples with a very high water content (> 50 wt%), the spectroscopy gave an underestimation in comparison with the titration and the distillation.…”

Section: The Water Content Determinationmentioning

confidence: 99%

“…For the water content determination, it is possible to use the azeotropic distillation. This method is used for various types of samples (herbs, spices and petroleum products), but sometimes it is not recommended to use the azeotropic distillation, for pyrolytic oils due to the interference of water soluble volatile organic compounds [30].…”

Section: The Water Content Determinationmentioning

confidence: 99%

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Determination of Water Content in Pyrolytic Tars Using Coulometric Karl-Fisher Titration

Jílková¹,

Hlinčík²,

Ciahotný³

2017

Acta Polytech

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Abstract. The liquid organic fraction of pyrolytic tar has a high energy value which makes possible its utilization as an energy source. However, before utilization, it is crucial to remove water from the liquid fraction. The presence of water reduces the energy value of pyrolytic tars. Water separation from the organic tar fraction is a complex process, since an emulsion can be readily formed. Therefore, after phase separation, it is important to know the residual water content in the organic phase and whether it is necessary to further dry it.The results presented in this manuscript focus on a water determination in liquid products from coal and biomass pyrolysis by a coulometric Karl-Fischer titration. The Coulometric Karl-Fischer titration is often used for a water content determination in gaseous, liquid and solid samples. However, to date, this titration method has not been used for a water determination in tars. A new water determination method, which has been tested on different types of tar, has been developed.The Coulometric Karl-Fischer titration is suitable for tar samples with a water content not greater than 5 wt%. The obtained experimental results indicate that the new introduced method can be used with a very good repeatability for a water content determination in tars.

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Section: The Water Content Determinationmentioning

confidence: 99%

Section: The Water Content Determinationmentioning

confidence: 99%

Section: The Water Content Determinationmentioning

confidence: 99%

See 1 more Smart Citation

Determination of Water Content in Pyrolytic Tars Using Coulometric Karl-Fisher Titration

Jílková¹,

Hlinčík²,

Ciahotný³

2017

Acta Polytech

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“…9). Pyrolysis bio-oils, whether derived via thermal or catalytic routes, all contain significant water (spanning 10-60 wt% 42 ), and hence water tolerance is a key requirement for any practical bio-oil upgrading catalyst, and hence we conducted a spiking experiment in which a 40 mol% relative to benzyl alcohol was deliberately introduced to the reaction media at the start of reaction. 17 This is also a reflection of the aromatic alcohols being better nucleophiles than phenol, and that lower boiling point of methanol leads to lower reaction temperatures at ambient pressure.…”

Section: Acetic Acid Esterificationmentioning

confidence: 99%

Mesoporous sulfonic acid silicas for pyrolysis bio-oil upgrading via acetic acid esterification

et al. 2016

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Propylsulfonic acid derivatised SBA-15 catalysts have been prepared by post modification of SBA-15 with mercaptopropyltrimethoxysilane (MPTS) for the upgrading of a model pyrolysis bio-oil via acetic acid esterification with benzyl alcohol in toluene. Acetic acid conversion and the rate of benzyl acetate production was proportional to the PrSO 3 H surface coverage, reaching a maximum for a saturation adlayer. Turnover frequencies for esterification increase with sulfonic acid surface density, suggesting a cooperative effect of adjacent PrSO 3 H groups. Maximal acetic acid conversion was attained under acid-rich conditions with aromatic alcohols, outperforming Amberlyst or USY zeolites, with additional excellent water tolerance.

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“…Recently, nuclear magnetic resonance (NMR) spectroscopy has been used to determine the water content of pyrolysis oil. Smets et al (2011) and David et al (2012) used 1 H NMR and 31 P NMR, respectively, in their studies to determine the water content of pyrolysis oil. However, these methods are only effective for pyrolysis oil with water contents of less than 50 wt%.…”

Section: Introductionmentioning

confidence: 99%

Novel Method for the Determination of Water Content and Higher Heating Value of Pyrolysis Oil

et al. 2015

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a This research provides a novel approach for the determination of water content and higher heating value of pyrolysis oil. Pyrolysis oil from Napier grass was used in this study. Water content was determined with pH adjustment using a Karl Fischer titration unit. An equation for actual water in the oil was developed and used, and the results were compared with the traditional Karl Fischer method. The oil was found to have between 42 and 64% moisture under the same pyrolysis condition depending on the properties of the Napier grass prior to the pyrolysis. The higher heating value of the pyrolysis oil was determined using an oildiesel mixture, and 20 to 25 wt% of the oil in the mixture gave optimum and stable results. A new model was developed for evaluation of higher heating value of dry pyrolysis oil. The dry oil has higher heating values in the range between 19 and 26 MJ/kg. The developed protocols and equations may serve as a reliable alternative means for establishing the actual water content and the higher heating value of pyrolysis oil.

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Water content of pyrolysis oil: Comparison between Karl Fischer titration, GC/MS-corrected azeotropic distillation and 1H NMR spectroscopy

Cited by 35 publications

References 13 publications

Determination of Water Content in Pyrolytic Tars Using Coulometric Karl-Fisher Titration

Determination of Water Content in Pyrolytic Tars Using Coulometric Karl-Fisher Titration

Mesoporous sulfonic acid silicas for pyrolysis bio-oil upgrading via acetic acid esterification

Novel Method for the Determination of Water Content and Higher Heating Value of Pyrolysis Oil

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