Deep hydrodesulfurization of diesel oils. Matrix effect in the analysis of low sulfur diesel oils by energy dispersive X-ray fluorescence spectroscopy

Pessayre, Stéphanie; Bacaud, R.; Geantet, Christophe; Vrinat, M.

doi:10.1016/s0016-2361(98)00211-7

Cited by 16 publications

(11 citation statements)

References 1 publication

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“…The determination of the total sulfur content in the processed products was carried out by XRF (Horiba SLFA-1800, Japan). Calibration was performed according to a previously published method . The sulfur content for the hydrotreated derivatives was respectively 9060, 7000, 6000, 4000, 3100, 1700, 970, 610, 290, and 150 ppm.…”

Section: Methodsmentioning

confidence: 99%

Evolution of Sulfur Compounds and Hydrocarbons Classes in Diesel Fuels during Hydrodesulfurization. Combined Use of Thin-Layer Chromatography and GC−Sulfur-Selective Chemiluminescence Detection

Bacaud

Cebolla

Membrado

et al. 2002

Ind. Eng. Chem. Res.

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A straight run gas oil has been hydrotreated with a commercial CoMo/Al2O3 catalyst, under variable conditions of severity, in order to yield processed products containing a variable amount of residual sulfur. These products have been characterized by simulated distillation, gas chromatography with sulfur-selective detection (GC−SCD), and thin-layer chromatography. The sulfur compounds have been grouped into distinct representative families. The rate constants for the reaction of desulfurization of the considered groups and the apparent rate order with respect to some individual sulfur compounds have been determined. The following hydrocarbon groups have been determined in the hydrotreated products by analytical thin-layer chromatography−densitometry: alkanes, cycloalkanes, total aromatics, and polyaromatic compounds (PACs). The straight run gas oil has been submitted to fractionation by preparative thin-layer chromatography, and the resulting fractions of alkanes, cycloalkanes, and aromatics have been characterized by simulated distillation and GC−SCD. It has been observed that the sulfur compounds concentrate in the aromatic fraction. In the hydrotreated samples, the content of total aromatics decreases as sulfur is eliminated. Heavy cycloalkanes and PACs remain constant, while the alkanes content increases. The combined use of TLC and GC−SCD allows one to obtain useful information on the gas oil composition and its behavior in the HDS process.

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Section: Methodsmentioning

confidence: 99%

Evolution of Sulfur Compounds and Hydrocarbons Classes in Diesel Fuels during Hydrodesulfurization. Combined Use of Thin-Layer Chromatography and GC−Sulfur-Selective Chemiluminescence Detection

Bacaud

Cebolla

Membrado

et al. 2002

Ind. Eng. Chem. Res.

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“…Because the analysis relies on the X-ray radiation directly probing the liquid sample, important matrix effects are found since the penetration of the radiation in the internal layers of the sample results in the absorption of both excitation radiation and fluorescence from sulfur, to an extent that depends upon the composition of the matrix [7]. For example, it is known that variations in oxygen content and/or in the C/H mass ratio of the petroleum product under evaluation produce significant variations in the measured values [9]. Therefore, corrections for…”

Section: Introductionmentioning

confidence: 99%

A sustainable and simple energy dispersive X-ray fluorescence method for sulfur determination at trace levels in biodiesel samples via formation of biodiesel spots on a suitable solid support

Marguí

Resano

Queralt

2019

Spectrochimica Acta Part B: Atomic Spectroscopy

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The aim of the present work is the development of a simple, sensitive and sustainable EDXRF method for the determination of trace amounts of sulfur in biodiesel samples. In this method, the deposition of several microliters of sample onto an organic thin layer and the analysis of the resulting adsorbed biodiesel spot by benchtop EDXRF is proposed. A careful study was performed to select the volume and the best solid support to deposit biodiesel samples, including filters made of different materials (glass fiber, Nylon, cellulose, paper) and a commercial disposable absorbent pad (UltraCarry, Rigaku). A critical issue that limits the use of most of these solid supports was the relative high blank signals that hamper the determination of sulfur at trace levels. Finally, it was found that best strategy was the deposition of 50 µL of biodiesel on the UltraCarry sample retainer. Operating conditions for EDXRF measurements were also evaluated to obtain the best instrumental sensitivity for sulfur determination (Excitation: 20 kV, no primary filter, measurement time: 300s). Using the best analytical conditions the quantification limit of the method was 7 mg kg-1 of sulfur. This value is even better than the one reported in the ASTM D4294 method (LOQ: 16.0 mg kg-1) but using a sample amount 100 times smaller. The linearity was confirmed in the range of 10-100 mg kg-1 by analyzing a set of commercial biodiesel standards. Accuracy and precision of the results, evaluated by the analysis of samples prepared with the same matrix as the standards, with levels of 20, 40 and 75 mg kg-1 of sulfur, and processed as unknowns, proved acceptable (Recoveries: 94.3-110.6%, RSD: 10.8-13.6%, n=3) for the intended purpose. Overall, the performance of the method developed is promising and it could be used to determine trace amounts of sulfur in biodiesel samples in a simple, sustainable and cost-effective way. Furthermore, since the original sample is adsorbed onto a solid support, repeat confirmatory analyses on the same specimen, if needed, can be carried out.

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“…Even using matrix-matched reference samples, changes in plasma can occur making direct injection of organic substances prone to some inconveniences for trace S determination [14][15][16]. Alternatively, sulfur determination in crude oil and its fractions has been carried out by X-ray fluorescence (XRF) and also by sample combustion with further titration or infrared detection [17][18][19][20][21]. Despite some automatic sulfur analyzers allow the direct analysis of diesel oil, common procedures for S determination by other techniques involve a previous step of sample preparation [22].…”

Section: Introductionmentioning

confidence: 99%

Feasibility of sulfur determination in diesel oil by inductively coupled plasma optical emission spectrometry after microwave-induced combustion using flame retardant

Cruz

Tirk

Nora

et al. 2015

Fuel

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Deep hydrodesulfurization of diesel oils. Matrix effect in the analysis of low sulfur diesel oils by energy dispersive X-ray fluorescence spectroscopy

Cited by 16 publications

References 1 publication

Evolution of Sulfur Compounds and Hydrocarbons Classes in Diesel Fuels during Hydrodesulfurization. Combined Use of Thin-Layer Chromatography and GC−Sulfur-Selective Chemiluminescence Detection

Evolution of Sulfur Compounds and Hydrocarbons Classes in Diesel Fuels during Hydrodesulfurization. Combined Use of Thin-Layer Chromatography and GC−Sulfur-Selective Chemiluminescence Detection

A sustainable and simple energy dispersive X-ray fluorescence method for sulfur determination at trace levels in biodiesel samples via formation of biodiesel spots on a suitable solid support

Feasibility of sulfur determination in diesel oil by inductively coupled plasma optical emission spectrometry after microwave-induced combustion using flame retardant

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