Recent Development of the XANES Spectral Analysis Methods for the Structure Characterization of Metal Complexes in Solution

Kurisaki, Tsutomu; Matsuo, Shuji; Tóth, I.; Wakita, Hisanobu

doi:10.2116/analsci.24.1385

Cited by 7 publications

(6 citation statements)

References 34 publications

Supporting

Mentioning

Contrasting

Order By: Relevance

“…The lack of reliable information on X-ray attenuation and absorption coefficients revealed by several studies (Grodstein, 1957;Cooper, 1965) led to various experimental efforts towards accurate absorption measurements and theoretical tabulations of X-ray mass attenuation coefficients (Hubbell, 1969;Bearden, 1966;Kopfmann & Huber, 1968;McMaster et al, 1969;Kessler Jr et al, 1982;de Meulenaer & Tompa, 1965;Deslattes, 1969). The availability of advanced X-ray sources and development of improved theories have enhanced the development of experimental methodologies (Diaz-Moreno, 2012;Prešeren et al, 2001;Kurisaki et al, 2008;Chantler, 2009) particularly for structural analyses of materials using different sample types. Several particularly insightful and accurate X-ray absorption studies have been verified by developments in theory and by comparison of experimental results (Deslattes, 1959;Hughes et al, 1968;Gerward et al, 1979;Rao et al, 1981;Nathuram et al, 1988), claiming accuracy of around 1%, usually for ideal systems such as elemental metals or monoatomic solids.…”

Section: Accuracymentioning

confidence: 99%

See 1 more Smart Citation

High-accuracy X-ray absorption spectra from mMsolutions of nickel (II) complexes with multiple solutions using transmission XAS

Chantler

Islam

Best

et al. 2015

J Synchrotron Radiat

View full text Add to dashboard Cite

A new approach is introduced for determining X-ray absorption spectroscopy (XAS) spectra on absolute and relative scales using multiple solutions with different concentrations by the characterization and correction of experimental systematics. This hybrid technique is a development of standard X-ray absorption fine structure (XAFS) along the lines of the high-accuracy X-ray extended range technique (XERT) but with applicability to solutions, dilute systems and cold cell environments. This methodology has been applied to determining absolute XAS of bis(N-n-propyl-salicylaldiminato) nickel(II) and bis(N-i-propyl-salicylaldiminato) nickel(II) complexes with square planar and tetrahedral structures in 15 mM and 1.5 mM dilute solutions. It is demonstrated that transmission XAS from dilute systems can provide excellent X-ray absorption near-edge structure (XANES) and XAFS spectra, and that transmission measurements can provide accurate measurement of subtle differences including coordination geometries. For the first time, (transmission) XAS of the isomers have been determined from low-concentration solutions on an absolute scale with a 1-5% accuracy, and with relative precision of 0.1% to 0.2% in the active XANES and XAFS regions after inclusion of systematic corrections.

show abstract

Section: Accuracymentioning

confidence: 99%

“…Solvent properties also affect the reactivity of metal complexes and their stability in solution. Characterization of solvent effects is important to quantify structural analysis of metal complexes in solution (Kurisaki et al, 2008).…”

Section: Accuracymentioning

confidence: 99%

High-accuracy X-ray absorption spectra from mMsolutions of nickel (II) complexes with multiple solutions using transmission XAS

Chantler

Islam

Best

et al. 2015

J Synchrotron Radiat

View full text Add to dashboard Cite

show abstract

“…The XAFS analysis provides useful information for the local structure of the element. 11 By using XAFS analysis, the oxidation state of Cr is determined nondestructively. This method was applied for the determination of hexavalent Cr ratio in industrial products during this study.…”

Section: Introductionmentioning

confidence: 99%

Application of X-ray Absorption Fine Structure Method for the Quantitative Analysis of Hexavalent Chromium in Chromate Conversion Coating and Plastic

et al. 2014

View full text Add to dashboard Cite

The X-ray absorption fine structure method was applied for the quantitative analysis of hexavalent Cr in electronic products. The pre-edge peak intensity of the Cr K-edge increased according to the hexavalent Cr amount, and the hexavalent Cr ratio was calculated quantitatively by using the intensity. By combining with inductively coupled plasma atomic emission spectroscopy measurement results that gave the total Cr amount, the absolute amount of hexavalent Cr in chromate conversion coating and plastic samples could be evaluated. The results obtained by this method were in good agreement with those obtained by the chemical analysis method. This method can be successfully applied for the determination of hexavalent Cr amount in electronic products such as chromate conversion coating and plastic.

show abstract

“…With the increasing oxidation state of the absorbing atom, the absorption edge shifts to higher energies, which allows determination of the valence of the atom. 1,5 The XAS spectra can be obtained quickly using a chargecoupled device (CCD) detector. Thus, an in-situ study of the structure of the material used as catalyst can be easily carried out while the reaction is in progress.…”

Section: Introductionmentioning

confidence: 99%

In-situ Monitoring of the Structure of a Goethite-Based Catalyst during Methane Oxidation by X-Ray Absorption Near-Edge Structure (XANES) Spectroscopy Assisted by Chemometric Methods

et al. 2011

View full text Add to dashboard Cite

A goethite-based catalyst was evaluated using in-situ X-ray absorption near-edge structure (XANES) spectroscopy during methane oxidation under increasing reaction temperature. Determination of rank by median absolute deviation (DRMAD), evolving factor analysis (EFA), and multivariate curve resolution (MCR) were used to detect the species present in the catalyst during the reaction and determine their concentration profiles and their pure spectra. The reactants and reaction products were monitored on-line by mass spectrometer. The goethite-based catalyst was active for methane oxidation, with CO(2) and H(2)O as the main products. DRMAD and EFA were useful to determine the number of chemical species present in the catalyst structure during reactions. The catalyst presented phase transition during the reaction from goethite to maghemite according to XANES spectra determined by MCR. On the other hand, it was verified that the catalyst presented phase transition from goethite to wüstite in the process in the absence of the oxidant (O(2)).

show abstract

Recent Development of the XANES Spectral Analysis Methods for the Structure Characterization of Metal Complexes in Solution

Cited by 7 publications

References 34 publications

High-accuracy X-ray absorption spectra from mMsolutions of nickel (II) complexes with multiple solutions using transmission XAS

High-accuracy X-ray absorption spectra from mMsolutions of nickel (II) complexes with multiple solutions using transmission XAS

Application of X-ray Absorption Fine Structure Method for the Quantitative Analysis of Hexavalent Chromium in Chromate Conversion Coating and Plastic

In-situ Monitoring of the Structure of a Goethite-Based Catalyst during Methane Oxidation by X-Ray Absorption Near-Edge Structure (XANES) Spectroscopy Assisted by Chemometric Methods

Contact Info

Product

Resources

About