Cloud point extraction procedure for flame atomic absorption spectrometric determination of lead(II) in sediment and water samples

The conditions for cloud point extraction of lead(II) from aqueous solutions were investigated and optimized. The procedure is based on the separation of Pb(II) – brillant cresyl blue (BCB) complexes into the micellar media by adding the surfactant Triton X-114. After phase separation, the surfactant-rich phase was dissolved with 1 mol L⁻¹ HNO₃ in ethanol and diluted with 1 mol L⁻¹ HNO₃ solution before lead was determined by flame atomic absorption spectrometry. Optimization of the pH, ligand and surfactant quantities, incubation time, temperature, viscosity, sample volume, and interfering ions was performed. The effects of the matrix ions were also examined. The detection limits for three times the standard deviations of the blank for lead were 7.5 μg L⁻¹ for water samples and 0.33 μg g⁻¹ for sediment samples. The validity of cloud point extraction was checked by employing certified reference samples of Lake Sediment IAEA-SL-1 and Sewage Sludge BCR-CRM 144R. The procedure was applied to natural waters and sediment samples with satisfactory results (recoveries >95%, relative standard deviations <6.4%).     

Localized defects in classical one-dimensional models

Several aspects of localized defects in the Frenkel-Kontorova, classicalXY chain and analogous models with a finite range of interactions are discussed from a general point of view. Precise definitions are given for defect phase shifts (charges) and for creation, pinning, and interaction energies. Corresponding definitions are also provided for interfaces (localized regions separating two phases). For the nearest-neighbor Frenkel-Kontorova model, the various defect energies are related to areas enclosed by contours joining heteroclinic points of the area-preserving map generated by the conditions of mechanical equilibrium.     

CYCIAE型回旋加速器负离子剥离引出的光学行为研究

为了CYCIAE型回旋加速器的剥离靶轴线及旋转角的概念设计,必须对负离子剥离后的光学特性进行研究,基于根据CYCIAE型回旋加速器剥离引出特点编制的程序CYCRS,计算了CYCIAE30加速器不同能量束流引出剥离点的位置,并与实际位置进行比较,证明计算所用的理论及方法是正确的,同时,考察了剥离后的束流空间运动的光学特性.在此基础上,确定了CYCIAE70回旋加速器能量为35—70MeV的束流引出剥离点位置.     

速调管输出间隙能量转换过程的二维数值分析模型

本文提出了分析速调管束波互作用能量转换的二维模型和假设，详细描述了在能量转换过程中的电子运动方程，并指出了能量转换的二维数值分析可能会对速调管基础理论的发展有所贡献的方面。     

高功率激光反射镜的几个关键技术

 分析了制作高功率连续激光反射镜材料的热性能、缺陷及其加工工艺, 提出了制作高功率激光反射镜应考虑的几个关键问题: 反射镜材料的综合热性能比值S, 材料的微观结构、缺陷的大小和晶向的选择, 以及加工工艺的设计。并介绍了实验结果。     

HPLC-determination of nifedipine in plasma on normal phase

Summary For the determination of nifedipine in plasma a sensitive and selective method is required. The use of on-line pre-column enrichment, followed by reversed phase separation and UV-detection at 350 nm proved to be too susceptible. Therefore, detection was carried out after a post-column on-line reduction and photoreaction step using a fluorescence detector. Although this method proved to be extremely sensitive (limit of detection 0.1 ng/ml plasma) and selective, a number of problems cropped up caused by the reduction agent which finally prevented the procedure being used in routine analysis. As a consequence, the following method was developed. After liquid-liquid extraction of nifedipine a 1/3 of the extract was chromatographed on a normal phase (diOH) system and detected at 235 nm, because detection at 350 nm was not sensitive enough. This method has a limit of detection of 1 ng nifedipine/ml plasma and the calibration curve is linear up to 320 ng/ml. The recovery lies around 82% and the standard deviation for the range 6–320 ng/ml is less than 5%. So far about 2000 plasma samples have been analysed by this method.     

Defect structure and migration in Fe3O4

We present the results of a computer simulation study of the defect formation and migration energies in Fe₃O₄. Calculated Frenkel and Schottky energies are found to be similar in magnitude and both are considerably reduced by screening due to electron redistribution around the charged-defect species. The calculations also suggest that cation diffusion is mainly effected by a colinear interstitialcy mechanism at low P_o2 and by a simple octahedral vacancy mechanism at higher P_o2.     

The effect of oxygen exposure on pentacene electronic structure

We use ultraviolet photoelectron spectroscopy to investigate the effect of oxygen and air exposure on the electronic structure of pentacene single crystals and thin films. It is found that O₂ and water do not react noticeably with pentacene, whereas singlet oxygen/ozone readily oxidize the organic compound. Also, we obtain no evidence for considerable p-type doping of pentacene by O₂ at low pressure. However, oxygen exposure lowers the hole injection barrier at the interface between Au and pentacene by 0.25 eV, presumably due to a modification of the Au surface properties.     

Determination of nonsteroidal antiinflammatory drugs in water samples using liquid chromatography coupled with diode-array detector and mass spectrometry

An analytical method for the determination of trace levels of six different nonsteroidal antiinflammatory drugs (NSAIDs) in water samples has been developed and validated. Environmentally relevant pharmaceuticals were chosen according to human consumption in Poland. Final analysis of the target compounds was performed by RP LC-diode-array detection-MS, whereas sample preparation included an SPE step. For this SPE step, a number of packing materials, such as LiChrolut RP-18, calixarene, Strata-X, BAKERBOND Narc-2, BAKERBOND Polar Plus, BAKERBOND styrene divinylbenzene-1, and Discovery DSC-18, were used, and their respective advantages and disadvantages in this study were discussed. The RP-18 phase was found to be the most retentive for all analytes. The detection limits for compounds in surface waters were varied from 0.005 for diflunisal to 0.095 microg/L for ibuprofen. The average recoveries of NSAIDs from the surface water samples ranged from 80 up to 103%. RSD value is relatively low (from 4% for fenoprofen up to 8% for ibuprofen). The performance of the method was tested with several environmental water samples.     

Manifestation of a Photorefractive Effect in the Raman Scattering Spectra of Lithium Niobate Crystals of Variable Composition

Using the Raman scattering spectra, we investigated the ordering of the structural units in the cation sublattice and the photorefractive properties of lithium niobate single crystals of variable composition, i.e., nominally pure ones with different Li/Nb ratios and those doped with the nonphotorefractive cations Mg²⁺, Gd³⁺, and Y³⁺. It is shown that at low concentrations of Mg²⁺, Gd³⁺, and Y³⁺ the magnitude of the photorefractive effect is substantially determined by the ordering of the structural units of the cation sublattice. It has been found for the first time that the intensity of the line corresponding to the bridge valence vibrations of oxygen atoms in the octahedrons of NbO₆ is sensitive to the dipole ordering of the cation sublattice of the crystal. __________ Translated from Zhurnal Prikladnoi Spektroskopii, Vol. 72, No. 5, pp. 611–614, September–October, 2005.