New methodology for sulfur analysis in geological samples by WD‐XRF spectrometry

Gazulla, M. F.; Gómez, María Pilar Garcés; Orduña, M.; Rodrigo, Marta

doi:10.1002/xrs.1092

Cited by 29 publications

(16 citation statements)

References 20 publications

Supporting

Mentioning

Contrasting

Order By: Relevance

“…Figure illustrates the Kα 1,2 peak shift for mixtures of Freiberg Gneiss and sulphide or sulphate, which is in good accordance to the results of other authors. The mean value of the Kα 1,2 doublet for sulphate mixtures (different sulphates with different mass fractions) is 110.576 ± 0.003° 2θ, respectively 2.3098 keV, and for sulphide mixtures 110.666 ± 0.004° 2θ or 2.3085 keV.…”

Section: Resultsmentioning

confidence: 99%

“…Sulphur is, judged by its average geochemical abundance in the Earth's crust, merely a minor element but nevertheless an inherent constituent in two major mineral groups: sulphides S 2− including sulphosalts and sulphates SO 4 2− . X‐ray fluorescence spectrometry (XRF), among other methods (see and references therein), has been successfully employed for total sulphur analyses of geological samples. However, geochemical investigations often require not only a quantitative analysis of total sulphur but also rather a distinguished determination of the two most important species sulphide and sulphate.…”

Section: Introductionmentioning

confidence: 97%

See 1 more Smart Citation

Quantitative analysis of sulphides and sulphates by WD‐XRF: Capability and constraints

2016

View full text Add to dashboard Cite

In the course of geochemical characterisations, total sulphur analyses are common practice although a differentiated quantification of sulphur species could provide valuable additional information, particularly when samples from unclear or changing redox environments are investigated. Unfortunately, a likewise simple distinct determination of just sulphide and sulphate already requires considerable efforts as sample dissolution or extra equipment. Two comparatively convenient strategies based on extended routine wavelength dispersive X‐ray fluorescence spectrometry measurements were adapted and optimised for a reliable quantitative sulphur speciation whereupon the matrix influence can be neglected. About 100 synthetic samples with different concentration ratios of sulphides and sulphates have been prepared and analysed using a WD‐XRF spectrometer. The first approach to differentiate between oxidation states and their quantification takes advantage of the Kα1,2 doublet shift. Sulphide lines are located at 2309 eV, sulphate lines at 2310 eV, and mixtures can be quantified by a regression curve of fluorescence energy versus sulphide amount. Secondly, the amount of sulphide can be calculated by a regression curve based on the quotient Kβ′/Kβ of the sulphur peak heights or areas. In contrast to sulphides, sulphates show sulphur Kβ′ satellite peaks, and the intensity of S Kβ′ increases with the increasing sulphate content. However, the applicability of this second method is limited by the lower detection limit of sulphide (10 g kg−1 sulphide in the sample) and interferences with lead (Pb Mβ line). Both approaches are validated by an independent method, Electrothermal Vaporisation Inductively Coupled Plasma Optical Emission Spectrometry, and already employed in investigations of ore‐containing mining dumps in Saxony/Germany. Copyright © 2016 John Wiley & Sons, Ltd.

show abstract

Section: Resultsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 97%

Quantitative analysis of sulphides and sulphates by WD‐XRF: Capability and constraints

2016

View full text Add to dashboard Cite

show abstract

“…A z value < 2 was obtained for all analysed materials by both analysers used, so it can be considered that the results obtained are acceptable and the method is accurate. In previous studies, some of these materials were analysed by other techniques such as WD‐XRF, ion chromatography (IC) or infrared (IR) and quadrupole mass spectrometry for evolved gas analysis (EGA) coupled with a thermogravimetric analyser (TGA) (TGA‐EGA) (Gazulla et al. 2009a, b, 2010).…”

Section: Resultsmentioning

confidence: 99%

“…There are various techniques capable of determining C, H, N and S. The elemental analyser (Potts 2003) can be used to measure the four elements, and sulfur can also be determined using an electric furnace coupled to an ion chromatograph (electric furnace‐IC) or by wavelength‐dispersive X‐ray fluorescence (WD‐XRF) spectrometry (Gazulla et al. 2009a, b).…”

mentioning

confidence: 99%

Determination of Carbon, Hydrogen, Nitrogen and Sulfur in Geological Materials Using Elemental Analysers

Gazulla

Rodrigo

Orduña

et al. 2012

Geostandard Geoanalytic Res

View full text Add to dashboard Cite

Registro de acceso restringido Este recurso no está disponible en acceso abierto por política de la editorial. No obstante, se puede acceder al texto completo desde la Universitat Jaume I o si el usuario cuenta con suscripción. Registre d'accés restringit Aquest recurs no està disponible en accés obert per política de l'editorial. No obstant això, es pot accedir al text complet des de la Universitat Jaume I o si l'usuari compta amb subscripció. Restricted access item This item isn't open access because of publisher's policy. The full--text version is only available from Jaume I University or if the user has a running suscription to the publisher's contents.

show abstract

“…Since the WD-XRF analysis is based on a pellet of compressed clay powder, it may therefore suffer from minor element matrix effects as well as orientation effects (e.g. [20] Gazulla et al 2008). The alternative analysis of clay powder in the form of fused disks was not advisable, because the high temperature used in the fusion process may destroy sulphur compounds in the clay, which are of interest here.…”

Section: Source and Composition Of The Raw Clay Used For Brickmakingmentioning

confidence: 99%

Calcium and sulphur distribution in fired clay brick in the presence of a black reduction core using micro X-ray fluorescence mapping

Gredmaier

Banks

Pearce

2011

Construction and Building Materials

View full text Add to dashboard Cite

A new finding of the observation of an elemental gradient or zoning of calcium and sulphur in fired brick bodies is described, that does not appear to have been reported in the literature before. Many raw clays used in brickmaking and pottery contain sulphur and calcium evenly distributed in low amounts in the unfired clay body. However, when the clay body is fired in the kiln at 1050 • C, the elements sulphur and calcium appear to combine to a compound, most probably calcium sulphate. The formation of calcium sulphate, visualised using energy dispersive imaging micro X-ray fluorescence (µ−XRF), only occurs around a so-called reduction core, also known as 'black core', caused by reduced magnetite F e 3 O 4 in the centre of the brick body. The presence of a black reduction core appears to cause the formation of a calcium sulphate layer around the black reduction core. This research contributes to the understanding of phenomena like salt formation, efflorescence and durability in solid clay brick bodies. Large sums are spent on building conservation by national economies and improvement of bricks is of key interest to them.

show abstract

New methodology for sulfur analysis in geological samples by WD‐XRF spectrometry

Cited by 29 publications

References 20 publications

Quantitative analysis of sulphides and sulphates by WD‐XRF: Capability and constraints

Quantitative analysis of sulphides and sulphates by WD‐XRF: Capability and constraints

Determination of Carbon, Hydrogen, Nitrogen and Sulfur in Geological Materials Using Elemental Analysers

Calcium and sulphur distribution in fired clay brick in the presence of a black reduction core using micro X-ray fluorescence mapping

Contact Info

Product

Resources

About