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首页> 外文期刊>The journal of physical chemistry, A. Molecules, spectroscopy, kinetics, environment, & general theory >Sulfur Speciation in Biochars by Very High Resolution Benchtop K alpha X-ray Emission Spectroscopy
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Sulfur Speciation in Biochars by Very High Resolution Benchtop K alpha X-ray Emission Spectroscopy

机译：通过非常高分辨率的BENCHTOP KαX射线发射光谱法在Biochars中的硫形态

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摘要

The analytical chemistry of sulfur-containing materials poses substantial technical challenges, especially due to the limitations of S-33 NMR and the time-intensive preparations required for wet-chemistry analyses. A number of prior studies have found that synchrotron-based X-ray absorption near edge structure (XANES) measurements can give detailed speciation of sulfur chemistry in such cases. However, due to the obvious access limitations, synchrotron XANES of sulfur cannot be part of routine analytical practice across the chemical sciences community. Here, in a study of the sulfur chemistry in biochars, we compare and contrast the chemical inferences available from synchrotron XANES with that given by benchtop, extremely high resolution wavelength-dispersive X-ray fluorescence (WD-XRF) spectroscopy, also often called X-ray emission spectroscopy (XES). While the XANES spectra have higher total information content, often giving differentiation between different moieties having the same oxidation state, the lower sensitivity of the S K alpha XES to coordination and local structure provides pragmatic benefit for the more limited goal of quantifying the S oxidation state distribution. Within that constrained metric, we find good agreement between the two methods. As the sulfur concentrations were as low as 150 ppm, these measurements provide proof-of-principle for characterization of the sulfur chemistry of biochars and potential applications to other areas such as soils, batteries, catalysts, and fossil fuels and their combustion products.
机译：含硫材料的分析化学构成了实质性的技术挑战，特别是由于S-33 NMR的局限性以及湿化学分析所需的时间 - 密集型制剂。许多事先研究发现，在边缘结构（XANES）测量附近的基于同步的X射线吸收可以在这种情况下给出硫化学的详细描述。然而，由于可用的访问局限性，硫磺的同步Xanes不能成为化学科学界的常规分析实践的一部分。在这里，在生物触发器中的硫化学研究中，我们将从Synchrotron Xanes提供的化学推迟与由Benchtop提供的Synchrotron Xanes进行比较，非常高分辨率波长分散性X射线荧光（WD-XRF）光谱，也经常被称为x - 射线发射光谱（XES）。虽然XANES光谱具有更高的总信息含量，通常在具有相同氧化状态的不同部分之间的分化，但SKαxes与协调和局部结构的较低灵敏度为量化S氧化状态分布的更有限的目标提供了务实的益处。在该受约束的公制中，我们在两种方法之间找到了良好的一致性。随着硫浓度低至150ppm，这些测量提供了原则上，用于表征生物脉内的硫化学和潜在应用，如土壤，电池，催化剂和化石燃料等地区及其燃烧产物。

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