Quo Vadis total reflection X-ray fluorescence?

The multielement trace analytical method ‘total reflection X-ray fluorescence’ (TXRF) has become a successfully established method in the semiconductor industry, particularly, in the ultra trace element analysis of silicon wafer surfaces. TXRF applications can fulfill general industrial requirements on daily routine of monitoring wafer cleanliness up to 300 mm diameter under cleanroom conditions. Nowadays, TXRF and hyphenated TXRF methods such as ‘vapor phase decomposition (VPD)-TXRF’, i.e. TXRF with a preceding surface and acid digestion and preconcentration procedure, are automated routine techniques (‘wafer surface preparation system’, WSPS). A linear range from 10⁸ to 10¹⁴ [atoms/cm²] for some elements is regularly controlled. Instrument uptime is higher than 90%. The method is not tedious and can automatically be operated for 24 h/7 days. Elements such as S, Cl, K, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Br, Sn, Sb, Ba and Pb are included in the software for standard peak search. The detection limits of recovered elements are between 1×10¹¹ and 1×10⁷ [atoms/cm²] depending upon X-ray excitation energy and the element of interest. For the determination of low Z elements, i.e. Na, Al and Mg, TXRF has also been extended but its implementation for routine analysis needs further research. At present, VPD-TXRF determination of light elements is viable in a range of 10⁹ [atoms/cm²]. Novel detectors such as silicon drift detectors (SDD) with an active area of 5 mm², 10 mm² or 20 mm², respectively, and multi-array detectors forming up to 70 mm² are commercially available. The first SDD with 100 mm² (!) area and integrated backside FET is working under laboratory conditions. Applications of and comparison with ICP-MS, HR-ICP-MS and SR-TXRF, an extension of TXRF capabilities with an extremely powerful energy source, are also reported.     

生地当归药队煎剂的表面增强拉曼散射光谱

为揭示单味煎剂与方剂间的关系,分别测试分析了生地当归药队、单味药生地和单味药当归煎剂的表面增强拉曼散射(surface-enhanced Raman scattering, SERS)光谱,并对其进行谱峰归属。本文主要针对存在于三种煎剂中的17个拉曼信号(538,622,732,761,835,876,959,1 145,1 245,1 276,1 326,1 402, 1 456,1 470,1 518,1 546和1 605 cm-1)进行讨论。生地当归药队煎剂SERS光谱在538,732,761,835,876,959,1 145,1 245,1 276,1 326,1 402,1 456,1 470,1 518和1 605 cm-1处,出现15个明显的拉曼信号;生地煎剂SERS光谱在538,761,835,876,959,1 145,1 245,1 276,1 326,1 402,1 470,1 518和1 546 cm-1处,出现13个明显的拉曼信号;当归煎剂SERS光谱在538,622,732,761,835,876,959,1 245,1 326和1 402 cm-1处,出现10个明显的拉曼信号。生地当归药队煎剂SERS光谱保留了和未观察到生地和当归单味煎剂的某些拉曼峰,且产生了生地和当归单味煎剂中所没有的拉曼信号(1 456和1 605 cm-1),即产生新药物成分。生地当归药队煎剂所包含的药物成分并非是生地和当归单味药物煎剂所含药物成分的简单相加。结果表明,SERS光谱可能为方剂研究提供一种高灵敏度、快速准确和操作简单的检测方法。     

Application of generalized diagonal dominance in wireless sensor network optimization problems

The recent application of the diagonal dominance in the development of the optimization algorithms in the wireless sensor networks design, has been done by Yuan and Yu (2006) [14], extended in Yu et al. (2006) [9], and surveyed in Machado and Tekinay [11]. In this paper, we will use the concept of generalized diagonal dominance, to improve the obtained results regarding the power control game, in three directions. We also discuss the applicability of such improvements.     

Low-energy EDX – A novel approach to study stress corrosion cracking in SUS304 stainless steel via scanning electron microscopy

Intergranular stress corrosion cracking (IGSCC) in type SUS304 stainless steels, tested under pressurized water reactor (PWR) primary water conditions, has been characterized with unprecedented spatial resolution using scanning electron microscopy (SEM) and novel low-energy (∼3 kV) energy dispersive X-ray spectroscopy (EDX). An advancement of the large area silicon drift detector (SDD) has enhanced its sensitivity for X-rays in the low-energy part of the atomic spectrum. Therefore, it was possible to operate the SEM at lower accelerating voltages in order to reduce the interaction volume of the beam with the material and achieve higher spatial resolution and better signal-to-noise ratio. In addition to studying the oxide chemistry at the surface of intergranular stress corrosion cracks, the technique has proven capable of resolving Ni enrichment ahead of some crack tips. Active cracks could be distinguished from inactive ones due to the presence of oxides in the open crack and Ni-rich regions ahead of the crack tip. Furthermore, it has been established that SCC features can be better resolved with low-energy (3 kV) than high-energy (12 kV) EDX. The low effort in sample preparation, execution and data analysis makes SEM the ideal tool for initial characterization and selection of the most important SCC features such as dominant cracks and interesting crack tips, later to be studied by transmission electron microscopy (TEM) and atom probe tomography (APT).     

Synthesis,enzymes inhibitory properties and characterization of 2- (bis (4-aminophenyl) methyl) butan-1-ol compound: Quantum simulations,and in-silico molecular docking studies

In this study to be presented, the BAPMB molecule was synthesized and structurally characterized. All calculations were applied using the detailed DFT/B3LYP method with 6-311G (d, p) and SDD depended on the stable phase geometry of the molecule. Also, various HOMO-LUMO energy gaps, inter-orbital intramolecular interactions of the natural bond, and electro-static surface mapping actions were also realized. The molecule was characterized by NMR spectroscopic analysis. Besides, LC/MS data were acquired. In this analysis, fragment ions (m/z 168.9) of BAPMB were obtained as 137.8, 179.9, 198, 201.5, and 228.0 approximately. Also, molecular docking was performed while examining the exact binding site and binding mechanism of the ligand on the protein. In the study, glide scores in binding affinity with BAPMB – AChE, BAPMB – BChE, and BAPMB – GST, respectively; It was found to be −7.228 ​cal/mol, −7.205 ​cal/mol, −6.07 ​cal/mol and BAPMB - AChE was found to be more effective with receptor binding score. BAPMB was analyzed for its inhibition features counter AChE, BChE, and GST enzymes that exhibit effective inhibition. AChE, BChE, GST enzymes were powerfully inhibited by BAPMB. BChE showed excellent activity, particularly in comparison to standard tacrine. Eventually, AIM analysis was performed to search intermolecular interactions in the BAPMB compound.     

Evolution of Electron Velocity Distribution during ECRH and Heating Effect Analysis

1 Electron velocity distributions and energy deposition of ECW Two set of soft X-ray spectra detection system consist of high performance sillicon drift detectors （SDD） , high speed A/D transform and processing software, software pulse height analyzer （SPHA）. They are installed at mid plane （ r=0 ） and undermid plane （ r=-16.4 cm ） of HL-2A tokamak respectively to measure the time evolution of soft X-ray spectra. According to spectrum, the thermal electron and superthermal electron temperatures are derived. Because of the ratio of peak counts to background counts is very high （p/b 〉1 400-3000 ） ,     

Improvements of portable energy dispersive X-ray fluorescence instrument: Resolution with Silicon Drift Detector,measurements stability using pyroelectric sources,and adaptation for space use

An energy dispersive X-ray fluorescence instrument has been developed to be used for space exploration. In particular, the electronic readout has been redesigned to withstand the radiation environment of space and improve the energy resolution down to 121.17 eV using an Silicon Drift Detector (SDD). Besides, the instrument uses pyroelectric sources as excitation sources. We include a renormalization to reduce measurement fluctuation from 25.2% to 3.7%. A peak search algorithm has been implemented based on calibration to improve accuracy and reduce possible aging drift effects.     

Recent advances in sample preparation techniques and methods of sulfonamides detection – A review

Sulfonamides (SAs) have been the most widely used antimicrobial drugs for more than 70 years, and their residues in foodstuffs and environmental samples pose serious health hazards. For this reason, sensitive and specific methods for the quantification of these compounds in numerous matrices have been developed. This review intends to provide an updated overview of the recent trends over the past five years in sample preparation techniques and methods for detecting SAs. Examples of the sample preparation techniques, including liquid–liquid and solid-phase extraction, dispersive liquid–liquid microextraction and QuEChERS, are given. Different methods of detecting the SAs present in food and feed and in environmental, pharmaceutical and biological samples are discussed.     

HL-2A装置SDD软X射线能谱测量结果

Measurements of soft X-ray spectra during Electron Cyclotron Resonance Heating (ECRH) has been achieved on HL-2A tokamak using two independent silicon drift detector (SDD) systems. Electron temperatures are derived from the measured soft X-ray energy spectra. A comparison indicates that the results measured by SDD are consistent with ECE measurements. Experimental results of soft X-ray spectra measure- ment using SDD show that the increment of electron temperature is larger at z=0 than that at z = 16.4cm chord, so, we can conclude that the energy of ECW is deposited dominantly in the core of plasma and electron temperature profile become peaked during on-axis ECRH (B_T=2.4T). The statistic survey of ECRH discharges (2.41T ≤B_T≤2.43T,1.5×10¹⁹m^-3≤n_e≤2.5≤10¹⁹m^-3,300kW≤ECRH power≤600kW) shows that plasma electron temperature rises obviously during on-axis ECRH, especially, in the core of plasma (z=0). It has been observed that the on-axis ECRH can make electron temperature increase up to 30%～80% at z=0 chord and 15%～55% at z=-16.4cm chord.     

Experimental and theoretical studies on inversion dynamics of dichloro(l-difluoromethionine-N,S)platinum(II) and dichloro(l-trifluoromethionine-N,S)platinum(II) complexes

Fluorinated analogues of methionine such as l-S-(difluoromethyl)homocysteine (l-difluoromethionine; DFM) and l-S-(trifluoromethyl)homocysteine (l-trifluoromethionine; TFM) have been demonstrated to be interesting analogues for incorporation into peptides and proteins. The presence of the fluorine nucleus adjacent to the sulfur atom in the side chain not only serves to alter the nucleophilicity and electron density of the sulfur atom but it can function as an important NMR spectroscopic (¹⁹F) probe. Additional information on the properties of these fluorinated amino acid analogues was obtained by studying their interactions with dipotassium tetrachloroplatinate (K₂PtCl₄). The resulting complexes, dichloro(l-difluoromethionine-N,S)platinum(II) and dichloro(l-trifluoromethionine-N,S)platinum(II) were investigated with respect to their sulfur inversion rates utilizing dynamic NMR methods. Inversion barriers for the DFM- and TFM-platinum complexes were experimentally determined to be 16.4 ± 0.2 and 18 ± 1 kcal/mol, respectively. Density functional calculations at the B3LYP/SDD level were also performed to model the structures and energies of the ground and transition states for these complexes.