REFERENCE MATERIALS FOR MICRO-ANALYTICAL NUCLEAR TECHNIQUES

1992 ◽  
Vol 02 (04) ◽  
pp. 651-664 ◽  
Author(s):  
V. Valkovic ◽  
R. Zeisler ◽  
G. Bernasconi ◽  
P.R. Danesi

Direct application of many existing reference materials in micro-analytical procedures such as energy dispersive x-ray fluorescence (EDXRF), particle induced x-ray emission spectroscopy (PIXE) and ion probe techniques for the determination of trace elements is often impossible or difficult because: 1) other constituents present in large amounts interfere with the determination; 2) trace components are not sufficiently homogeneously distributed in the sample. Therefore specific natural-matrix reference materials containing very low levels of trace elements and having high degree of homogeneity are required for many micro-analytical procedures. In this report, selection of the types of environmental and biological materials which are suitable for micro-analytical techniques will be discussed.

Author(s):  
G. Remond ◽  
R.H. Packwood ◽  
C. Gilles ◽  
S. Chryssoulis

Merits and limitations of layered and ion implanted specimens as possible reference materials to calibrate spatially resolved analytical techniques are discussed and illustrated for the case of gold analysis in minerals by means of x-ray spectrometry with the EPMA. To overcome the random heterogeneities of minerals, thin film deposition and ion implantation may offer an original approach to the manufacture of controlled concentration/ distribution reference materials for quantification of trace elements with the same matrix as the unknown.In order to evaluate the accuracy of data obtained by EPMA we have compared measured and calculated x-ray intensities for homogeneous and heterogeneous specimens. Au Lα and Au Mα x-ray intensities were recorded at various electron beam energies, and hence at various sampling depths, for gold coated and gold implanted specimens. X-ray intensity calculations are based on the use of analytical expressions for both the depth ionization Φ (ρz) and the depth concentration C (ρz) distributions respectively.


2019 ◽  
Author(s):  
Paul Pearce ◽  
Gaurav Assat ◽  
Antonella Iadecola ◽  
François Fauth ◽  
Rémi Dedryvère ◽  
...  

The recent discovery of anionic redox as a means to increase the energy density of transition metal oxide positive electrodes is now a well established approach in the Li-ion battery field. However, the science behind this new phenomenon pertaining to various Li-rich materials is still debated. Thus, it is of paramount importance to develop a robust set of analytical techniques to address this issue. Herein, we use a suite of synchrotron-based X-ray spectroscopies as well as diffraction techniques to thoroughly characterize the different redox processes taking place in a model Li-rich compound, the tridimentional hyperhoneycomb β-Li2IrO3. We clearly establish that the reversible removal of Li+ from this compound is associated to a previously described reductive coupling mechanism and the formation of the M-(O-O) and M-(O-O)* states. We further show that the respective contributions to these states determine the spectroscopic response for both Ir L3-edge X-ray absorption spectroscopy (XAS) and X-ray photoemissions spectroscopy (XPS). Although the high covalency and the robust tridimentional structure of this compound enable a high degree of reversibile delithiation, we found that pushing the limits of this charge compensation mechanism has significant effects on the local as well as average structure, leading to electrochemical instability over cycling and voltage decay. Overall, this work highlights the practical limits to which anionic redox can be exploited and sheds some light on the nature of the oxidized species formed in certain lithium-rich compounds.<br>


2019 ◽  
Author(s):  
Paul Pearce ◽  
Gaurav Assat ◽  
Antonella Iadecola ◽  
François Fauth ◽  
Rémi Dedryvère ◽  
...  

The recent discovery of anionic redox as a means to increase the energy density of transition metal oxide positive electrodes is now a well established approach in the Li-ion battery field. However, the science behind this new phenomenon pertaining to various Li-rich materials is still debated. Thus, it is of paramount importance to develop a robust set of analytical techniques to address this issue. Herein, we use a suite of synchrotron-based X-ray spectroscopies as well as diffraction techniques to thoroughly characterize the different redox processes taking place in a model Li-rich compound, the tridimentional hyperhoneycomb β-Li2IrO3. We clearly establish that the reversible removal of Li+ from this compound is associated to a previously described reductive coupling mechanism and the formation of the M-(O-O) and M-(O-O)* states. We further show that the respective contributions to these states determine the spectroscopic response for both Ir L3-edge X-ray absorption spectroscopy (XAS) and X-ray photoemissions spectroscopy (XPS). Although the high covalency and the robust tridimentional structure of this compound enable a high degree of reversibile delithiation, we found that pushing the limits of this charge compensation mechanism has significant effects on the local as well as average structure, leading to electrochemical instability over cycling and voltage decay. Overall, this work highlights the practical limits to which anionic redox can be exploited and sheds some light on the nature of the oxidized species formed in certain lithium-rich compounds.<br>


2018 ◽  
Author(s):  
Zoltán Kis ◽  
Katalin Gméling ◽  
Tímea Kocsis ◽  
János Osán ◽  
Mihály András Pocsai ◽  
...  

We present precise analysis of major and trace elements of the humic acid. We used three different element analytical techniques in our investigations as prompt-gamma activation analysis (PGAA), neutron activation analysis (NAA) and X-ray fluorescence (XRF) analysis was carried out. We identified 42 elements in our sample.


1992 ◽  
Vol 02 (04) ◽  
pp. 489-491 ◽  
Author(s):  
MOMOKO CHIBA ◽  
VENKATESH G. IYENGAR

Tin (Sn) is one of the causative elements of the environmental pollution. As no certified reference materials for Sn are presently available, existing reference materials were analyzed for Sn by two independent analytical techniques; atomic absorption spectrometry (AAS) and neutron activation analysis (NAA). The results obtained by both methods were in agreement except for mixed diet which contains Sn in the range of 50 μ g/g. Further, tin concentrations in human and animal organs have been examined by AAS. Among organs tested tin concentrations in testes were the highest, 2.08±0.62 μ g/g dry weight (mean ±SD, n=12) in humans, and 1.45±0.55 μ g/g (n=8) in mice.


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