Characterization of organic sulfur functional groups in coal by means of temperature programmed reduction

Majchrowicz, Bernard B.; Yperman, Jan; Reggers, Guy; François, J; Gelan, Jan; Martens, Henri; Mullens, J.; Poucke, L. C. Van

doi:10.1016/0378-3820(87)90058-0

Cited by 21 publications

(7 citation statements)

References 6 publications

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“…Temperature-Programmed Reduction Procedure. The concept of the TPR setup has been described in previous papers (3,4). An amount of the sample according to its sulfur content was mixed with a reducing solvent mixture (2) in a modified quartz glass reaction vessel (Figure 2).…”

Section: Sectionmentioning

confidence: 99%

“…Hitherto, there has been no convenient method available for determining the functional group distribution of organic sulfur in coal (1). Recently, an interesting approach to the characterization of organic sulfur has been developed, namely the temperature-programmed reduction (TPR) of coal (2)(3)(4). Nonisothermal heating of a coal or other sulfur-containing compounds with a fixed programming rate in a reducing atmosphere results in a maximum evolution of H2S at discrete temperatures.…”

Section: Introductionmentioning

confidence: 99%

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Automated potentiometric determination of sulfur functional groups in fossil fuels

Majchrowicz¹,

Yperman²,

Mullens³

et al. 1991

Anal. Chem.

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A fully extended description is given of an automated setup to monltor H,S continuously in a sensltlve, qualitative, and quantltatlve way. H,S Is led by a stream of N, Into an alkallne solution and is contlnuousty determlned as S2-by a potentiometric detectlon system. The H,S detection system has been applied to the temperature-programmed reduction (TPR) of fossil fuel samples. The TPR procedure conslsts of the nonIsothermal heating of a sample in a reducing atmosphere, In order to liberate the different sulfur functional groups as H,S at dlscrete temperature ranges.

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Section: Sectionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Automated potentiometric determination of sulfur functional groups in fossil fuels

Majchrowicz¹,

Yperman²,

Mullens³

et al. 1991

Anal. Chem.

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“…Temperature-programmed reduction (TPR) is based on the principle that different organic sulfur forms present in fossil fuels have different characteristic reduction temperatures at which they will be converted to H 2 S under a hydrogen atmosphere. Initial studies − yielded poor sulfur balances, with virtually all the thiophenic sulfur remaining in the char due to the low hydrogen pressures used. Additionally, little account was taken of the reduction of pyrite to pyrrhotite and retrogressive reactions including the conversion of sulfides into thiophenes.…”

Section: Introductionmentioning

confidence: 99%

Speciation of the Organic Sulfur Forms in a Recent Sediment and Type I and II-S Kerogens by High-Pressure Temperature-Programmed Reduction

Brown¹,

Sirkecioglu²,

Snape³

et al. 1997

Energy Fuels

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Temperature-programmed reduction (TPR) with a well-swept fixed-bed reactor operating at 15 MPa of hydrogen pressure has facilitated the speciation of the organic sulfur forms in coals and petroleum source rocks through complete hydrodesulfurization with typically 75−80% of the sulfur being released as hydrogen sulfide with the remaining 20−25% occurring as primarily thiophenic compounds in the oils obtained in high yield. In this study, the technique has been applied to kerogens isolated from a series of unconsolidated Peru margin sediments, and for comparison, to type I and II-S kerogens (Göynük oil shale and Monterey Fm, respectively) from immature organic-rich rocks. Visual resolution in the hydrogen sulfide TPR evolution profiles has been achieved between mono- and di/polysulfidic forms with the latter being reduced below 250 °C. Indeed, di/polysulfides account for high proportions of the reduced sulfur in surficial sediment samples collected from close to the top of the sediment. In contrast, monosulfides are the dominant sulfur form in the sample analyzed from deeper in the Peru margin sediment where thiophenes account for up to ca. 35% of the organic sulfur. This distribution is remarkably similar to those found for both the type I and II-S kerogens investigated, indicating that the major changes in organic sulfur forms occur during the early stages of diagenesis.

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“…Organic sulfur in coal includes a series of sulfur-containing organic sulfur groups, such as thiols (R-SH, Ar-SH), thioethers (R-S-R', R-S-Ar), thiophene, sulphoxides, ethersulfone, Sulfone and thiophenelikes, etc. [3,4] Howerver, there is little reports of organic sulfur in detail existing forms, one reason is that, as a part of coal structure, organic sulfur exists as a netlike structure and heterocyclic rings which are dissoluble and very difficult to remove from coal; the other reason is that acute removal way will change the forms and structure of coal [5] . In this study, components of NW coal were separated by isopycnic density gradient centrifugation (IDGC) (ZnCl 2 was used as density fluid), and then sulfur forms of the separated components were analyzed.…”

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confidence: 99%

Study on Forms of Sulfur in NW Coal and Behavior of Desulfurization

Wang

Ren

et al. 2008

2008 2nd International Conference on Bioinformatics and Biomedical Engineering

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macerals of NW coal were separated by isopycnic density gradient centrifugation (IDGC) (ZnCl 2 was used as density fluid) and each macerals were undertaken forms of sulfur. Sulfur was removed by peroxyacetic acid-oxidation under ultrasonic and microwave radiation. Transformations of organic sulfur forms were expressed by XPS spectra. The results showed that forms of organic sulfur were enriched in different macerals, thiophenes in vitrinite and thioethers, thiols in exinite. Desulfurization rate of NW raw coal was up to 38.1% with peroxyacetic acid under ultrasonic and microwave radiation. From easy to difficult, the order of desulfurization of each macerals was the same as mineral and inertinite inertinite exinite vitrinite, the most high desulfurization rate of macerals was 53.1%.

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Characterization of organic sulfur functional groups in coal by means of temperature programmed reduction

Cited by 21 publications

References 6 publications

Automated potentiometric determination of sulfur functional groups in fossil fuels

Automated potentiometric determination of sulfur functional groups in fossil fuels

Speciation of the Organic Sulfur Forms in a Recent Sediment and Type I and II-S Kerogens by High-Pressure Temperature-Programmed Reduction

Study on Forms of Sulfur in NW Coal and Behavior of Desulfurization

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