scholarly journals Investigation of per- and polyfluoroalkyl substances (PFAS) in soils and sewage sludges by fluorine K-edge XANES spectroscopy and combustion ion chromatography

2021 ◽  
Author(s):  
Philipp Roesch ◽  
Christian Vogel ◽  
Thomas Huthwelker ◽  
Philipp Wittwer ◽  
Franz-Georg Simon
Keyword(s):  
Ion Chromatography ◽  
Xanes Spectrum ◽  
Direct Analysis ◽  
Xanes Spectroscopy ◽  
Organofluorine Compounds ◽  
Sewage Sludges ◽  
Edge Structure ◽  
Polyfluoroalkyl Substances ◽  
Organic Fluorine ◽  
Inorganic Fluorides

AbstractFor the first time, fluorine K-edge X-ray absorption near-edge structure (XANES) spectroscopy was applied to detect per- and polyfluoroalkyl substances (PFAS) in various soil and sewage sludge samples. The method can be used to determine the speciation of inorganic and organic fluorides, without pre-treatment of solid samples. Therefore, XANES spectra of several inorganic fluorides as well as selected fluorinated organic compounds were recorded. While inorganic fluorides partially exhibit a variety of sharp spectral features in the XANES spectrum, almost all inspected organofluorine compounds show two distinct broad features at 688.5 and 692.0 eV. Moreover, the peak intensity ratio 688.5 eV/692.0 eV in the PFAS XANES spectrum can be inversely correlated to the chain length of the perfluoro sulfonic acid group. The detection of targeted PFAS by bulk-XANES spectroscopy in combination with linear combination fitting in soils and sewage sludges was not applicable due to the low organic fluorine to total fluorine ratio of the samples (0.01–1.84%). Nonetheless, direct analysis of pure PFAS revealed that analysis of organofluorine species might be achieved in higher concentrated samples. Furthermore, quantitative measurements by combustion ion chromatography (CIC) evaluated as sum parameters extractable organically bound fluorine (EOF) and total fluorine (TF) emphasize that besides soils, sewage sludges are a significant source of organic fluorine in agriculture (154–7209 µg/kg).

X-ray absorption near-edge structure (XANES) spectroscopy of fullerenes: inner-shell excitonic effects in fullerenes and the XANES spectrum of a higher fullerene C76

1994 ◽  
Vol 64 (2-3) ◽  
pp. 353-357 ◽  
Author(s):  
Kazuhiko Seki ◽  
Ryuichi Mitsumoto ◽  
Tohru Araki ◽  
Eisuke Ito ◽  
Yukio Ouchi ◽  
...  
Keyword(s):  
Xanes Spectrum ◽  
Xanes Spectroscopy ◽  
Edge Structure ◽  
X Ray ◽  
Excitonic Effects ◽  
X Ray Absorption

XANES of chromium in sludges used as soil ameliorants

2003 ◽  
Vol 81 (2) ◽  
pp. 193-196 ◽  
Author(s):  
R R Martin ◽  
S J Naftel ◽  
T K Sham ◽  
B Hart ◽  
M A Powell
Keyword(s):  
Oxidation State ◽  
Chromium Content ◽  
Xanes Spectroscopy ◽  
Sewage Sludges ◽  
Edge Structure ◽  
Aqua Regia ◽  
X Ray ◽  
X Ray Absorption

Samples of sewage sludges proposed for use as soil ameliorants in an Indo-Canadian project were tested for chromium content. Standard aqua regia extractions found one sludge to have excessive amounts of Cr. X-ray absorption near-edge structure (XANES) spectroscopy, however, indicated that the Cr was present in the relatively benign Cr(III) oxidation state in all the sludge samples.Key words: soil, chromium, synchrotron, XANES.

scholarly journals Bone char effects on soil: sequential fractionations and XANES spectroscopy

SOIL ◽  
2018 ◽  
Vol 4 (1) ◽  
pp. 23-35 ◽  
Author(s):  
Mohsen Morshedizad ◽  
Kerstin Panten ◽  
Wantana Klysubun ◽  
Peter Leinweber
Keyword(s):  
Xanes Spectroscopy ◽  
Bone Char ◽  
Reduced Sulfur Compounds ◽  
Sequential Fractionation ◽  
P Fractionation ◽  
Edge Structure ◽  
Amended Soils ◽  
Soil P ◽  
P Fraction ◽  
Sequential P Fractionation

Abstract. The acceptability of novel bone char fertilizers depends on their P release, but reactions at bone char surfaces and impacts on soil P speciation are insufficiently known. By using sequential fractionation and synchrotron-based X-ray absorption near-edge structure (XANES) spectroscopy we investigated whether and how the chemical composition of bone char particles has been altered in soil and has consequently affected the P speciation of amended soils. Therefore, two different kinds of bone char particles (BC produced by the pyrolysis of degreased animal bone chips at 800 °C and BCplus, a BC enriched with reduced sulfur compounds) were manually separated from the soil at the end of two different experiments: incubation leaching and ryegrass cultivation. Sequential P fractionation of amended soils showed P enrichment in all fractions compared to the control. The most P increase between all treatments significantly occurred in the NaOH–P and resin-P fractions in response to BCplus application in both incubation-leaching and ryegrass cultivation experiments. This increase in the readily available P fraction in BCplus-treated soils was confirmed by linear combination fitting (LCF) analysis on P K-edge XANES spectra of BC particles and amended soils. The proportion of Ca hydroxyapatite decreased, whereas the proportion of CaHPO4 increased in BCplus particles after amended soils had been incubated and leached and cropped by ryegrass. Based on P XANES speciation as determined by LCF analysis, the proportion of inorganic Ca(H2PO4)2 increased in amended soils after BCplus application. These results indicate that soil amendment with BCplus particles leads to elevated P concentration and maintains more soluble P species than BC particles even after 230 days of ryegrass cultivation.

scholarly journals Performance of secondary P-fertilizers in pot experiments analyzed by phosphorus X-ray absorption near-edge structure (XANES) spectroscopy

AMBIO ◽  
2017 ◽  
Vol 47 (S1) ◽  
pp. 62-72 ◽  
Author(s):  
Christian Vogel ◽  
Camille Rivard ◽  
Verena Wilken ◽  
Andreas Muskolus ◽  
Christian Adam
Keyword(s):  
Xanes Spectroscopy ◽  
Edge Structure ◽  
X Ray ◽  
Pot Experiments ◽  
X Ray Absorption ◽  
P Fertilizers

Phosphorus K-edge XANES spectroscopy has probably often underestimated iron oxyhydroxide-bound P in soils

2018 ◽  
Vol 25 (6) ◽  
pp. 1736-1744 ◽  
Author(s):  
Jörg Prietzel ◽  
Wantana Klysubun
Keyword(s):  
Linear Combination ◽  
Xanes Spectroscopy ◽  
Organic P ◽  
Iron Oxyhydroxide ◽  
Edge Structure ◽  
X Ray ◽  
Soil P ◽  
P Sorption ◽  
Fe Oxyhydroxides ◽  
X Ray Absorption

Phosphorus (P) K-edge X-ray absorption near-edge structure (XANES) spectra of orthophosphate (oPO4) bound to soil FeIII minerals (e.g. ferrihydrite, goethite) show a pre-edge signal at 2148–2152 eV. It is unknown whether organic P bound to FeIII oxyhydroxides also show this feature. Otherwise, Fe-bound soil P may be underestimated by P K-edge XANES spectroscopy, because a large portion of Fe oxyhydroxide-bound P in soils is organic P. K-edge XANES spectra were obtained for different organic P compounds present in soils [inositol hexaphosphate (IHP), glucose-6-phosphate (G6P), adenosine triphosphate (ATP)] after sorption to ferrihydrite or goethite and compared with spectra of oPO4 adsorbed to these minerals. P sorption to ferrihydrite increased in the sequence IHP ≪ G6P < oPO4 < ATP. P sorption to goethite increased in the sequence G6P < oPO4 ≪ ATP = IHP. Pre-edge signals in P K-edge XANES spectra of organic P adsorbed to Fe oxyhydroxides were markedly smaller compared with those of oPO4 adsorbed to these minerals and absent for FeIII oxyhydroxide-bound ATP as well as goethite-bound IHP. Linear combination fitting (LCF) performed on spectra of IHP, G6P or ATP adsorbed to ferrihydrite or goethite, using only spectra of FeIII oxyhydroxide-bound oPO4 as reference compounds for Fe-bound P, erroneously assigned >93% (ferrihydrite) or >41% (goethite) of Fe-bound P to non-Fe-bound P species. Inclusion of FeIII oxyhydroxide-bound IHP as reference compounds markedly increased the recovery of oxyhydroxide-bound organic P. Thus, Fe-bound soil P has probably often been underestimated by LCF in soil XANES studies where IHP adsorbed to ferrihydrite and to goethite were not included as reference compounds.

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