A new approach for fluorine determination by solid sampling graphite furnace molecular absorption spectrometry

This work deals with the determination of fluorine by solid sampling graphite furnace molecular absorption spectrometry. The molecular absorbance of aluminum monofluoride (AlF), which is produced in the vapor phase in the presence of Al³⁺, is measured at 227.5 nm, a non-resonant platinum line. A conventional graphite furnace program has been used with pyrolysis and vaporization temperatures of 800 and 2300 °C, respectively. Solutions of Ba²⁺ and Al³⁺ have been used to avoid fluorine losses during the pyrolysis stage and to produce AlF in the vaporization stage, respectively. Certified coal and alumina samples were analyzed using aqueous standards for calibration. The agreement between the found concentration and the certified value, or the value obtained by another method ranged from 92 to 105%, with a relative standard deviation less than 8.5%. The limit of detection and the characteristic mass was 0.17 μg g^− 1 and 205 pg, respectively.     

Physico-Chemistry of the Limestone Sulphation Process

Aspects of the mechanism of the overall reaction between CaCO₃/CaO and SO₂/SO₃ under oxidizing conditions are discussed. The limestone and lime sulphation processes were carried out in a thermobalance under conditions relevant to atmospheric fluidized bed combustion. Sulphated samples, prepared in the form of cross-section particles, were examined in a scanning electron microscope by energy-dispersive X-ray and back-scattered electron imaging. Photomicrographs are presented. The reaction proceeded from the outer surface of the particles and along the pores. Surface textural changes during the reaction were considered. The layer of products was identified as controlling both the rate and extent of limestone/lime sulphation. In the products, two sulphur-bearing solids (CaSO₄ and CaS) were identified. The presence of CaS, which may cause difficulties in practice, is attributed to CaSO₃ disproportionation. This revised version was published online in August 2006 with corrections to the Cover Date.     

Determination of manganese in brain samples by slurry sampling graphite furnace atomic absorption spectrometry

A simple procedure for the determination of manganese in different sections of human brain samples by graphite furnace atomic absorption spectrometry has been developed. Brain sections included cerebellum, hypothalamus, frontal cortex, vermix and encephalic trunk. Two sample preparation procedures were evaluated, namely, slurry sampling and microwave-assisted acid digestion. Brain slurries (2% w/v) could be prepared in distilled, de-ionized water, with good stability for up to 30 min. Brain samples were also digested in a domestic microwave oven using 5 ml of concentrated HNO₃. A mixed palladium+magnesium nitrate chemical modifier was used for thermal stabilization of the analyte in the electrothermal atomizer up to pyrolysis temperatures of 1300 °C, irrespective of the matrix. Quantitation of manganese was conducted in both cases by means of aqueous standards calibration. The detection limits were 0.3 and 0.4 ng ml⁻¹ for the slurry and the digested samples, respectively. The accuracy of the procedure was checked by comparing the results obtained in the analysis of slurries and digested brain samples, and by analysis of the NIST Bovine Liver standard reference material (SRM 1577a). The ease of slurry preparation, together with the conventional set of analytical and instrumental conditions selected for the determination of manganese make such methodology suitable for routine clinical applications.     

Characteristics of vinyl iodide microwave plasma etching of GaAs/AlGaAs and InP/InGaAs heterostructures

Vinyl iodide (C₂H₃I) microwave discharges with additions of H₂ and Ar are found to provide faster etch rates than conventional CH₄/H₂/Ar discharges for InP, InGaAs, GaAs, and AlGaAs. This is a result of the relatively high volatilities of indium, gallium, and aluminum iodide species. The etched features are smooth and anisotropic over a wide range of do self-biases (–150 to –350 V), process pressures (1–20mTorr), and microwave powers (150–500 W). The polymer that forms on the mask during the plasma exposure can be readily removed in O₂ discharges. Electron spectroscopy for chemical analysis (ESCA) showed that the etched surfaces are slightly deficient in the group V elements under most conditions, but changes to the optical properties of the semiconductors are minimal. No defects are visible by transmission electron microscopy (TEM) in GaAs or InP samples etched at dc biases –250 V.     

Cavitands bearing four fluorophores

The synthesis of novel cavitands containing four fluorophores [tert-butoxycarbonyl protected 2,2′-bis(furyl)benzidine (t-BOC FurylBz) or 5,5′-bis(4-aminophenyl)-2,2′-bifuryl (t-BOC PFDA)] and ionophoric functional groups on the upper rim is reported. The cavitands bearing the four fluorophores emit blue light photoluminescence. In particular, the cavitand containing PFDA moieties exhibits a high photoluminescence quantum yield.     

微波聚合制备单分散、超细聚甲基丙烯酸甲酯微球

在微波辐照下,通过甲基丙烯酸甲酯(MMA)的无乳化剂乳液聚合,制备出粒径单分散、超细聚甲基丙烯酸甲酯(PMMA)微球。微波显著缩短聚合诱导期,加快聚合反应,其部分原因是微波加快引发剂过硫酸钾(KPS)的分解。实验证明微波辐照下KPS的表观分解活化能(ED)由128.3kJ/mol降低到106.0kJ/mol。单体浓度是影响PMMA乳液粒子尺寸的主要因素,在[MMA]小于0.3mol/L时,平均粒径随单体浓度提高而线形增加;[MMA]为0.3～1.0mol/L时,平均粒径稳定在约200nm;之后随单体浓度进一步增加,乳液稳定性变差。引发剂浓度增加对平均粒径影响较小,但增大引发剂浓度可显著降低粒径分散度。选取[MMA]为0.23～0.3mol/L、[KPS]为3×10-3～6×10-3mol/L可以得到粒径200nm的单分散微球。以丙酮/水(体积比1/3)为反应介质,可制备出数均粒径45nm的PMMA纳米粒子。在体系中加入3.5×10-3mol/L的Cu2+,可制备出数均粒径67nm、单分散的PMMA纳米粒子。     

A novel hyperbranched polyester acrylate used for microfabrications

A novel hyperbranched polyester acrylate (HPEA) was synthesized based upon ethylenediamine tetraacetic acid as a “core” molecule, 5‐hydroxyisophthalic acid as an AB₂ monomer, and 2‐hydroxyethyl acrylate as an endcapping reagent. The obtained oligomer has an unsaturation concentration of 4.10 mmol_C?C g^?1 measured by nuclear magnetic resonance and a wide molecular weight distribution of 1.64 measured by gel permeation chromatography. The two‐photon absorption (TPA) photopolymerization of HPEA under the exposure of a Ti : sapphire femtosecond laser with a wavelength of 800 nm was investigated through laser exposure dose‐dependant spatial resolutions of its resins. The TPA photopolymerization thresholds at the range 1.6–4.3 × 10⁷ mJ cm^?2, and exposure dose windows at the range 3.4–4.3 for three formulations were determined. A spatial resolution of 0.85 μm was obtained through the TPA photopolymerization of the formulation containing 1 wt% photoinitiator and 0.3 wt% photoinhibitor. A diffraction grating and real three‐dimensional coupled gear wheel created by TPA photopolymerization were described to demonstrate the unique capability of HPEA in microfabrications. Copyright © 2004 John Wiley & Sons, Ltd.     

Synthesis, Structures, and Thermal Expansion of the La2W2−xMoxO9 Series

The La₂W_2−xMo_xO₉ series has been synthesized by the ceramic method. An alternative synthesis using microwave radiation is also reported. La₂W₂O₉ has two polymorphs and the low-temperature phase (α) transforms to the high-temperature form (β) at 1077°C. The influence of the W/Mo substitution in this phase transition has been investigated by DTA. The β structure for x≥0.7 compositions can be prepared as single phase at any cooling rate. The β phase for 0.3≤x≤0.7 compounds can be prepared as single phase by quenching, whereas a mixture of α and β phases is obtained by slow cooling. The W/Mo ratio in both coexisting phases is different with the β-phase having a higher Mo content. The x=0.1 and 0.2 compounds have been prepared as mixtures of phases. The room temperature structure of β-La₂W_1.7Mo_0.3O₉ has been analyzed by the Rietveld method in P2₁3 space group. The final R-factors were R_WP=9.0% and R_F=5.6% with a structure similar to that of β-La₂Mo₂O₉. Finally, the thermal expansion of both types of structures has been determined from a thermodiffractometric study. The thermal expansion coefficients were 2.9×10⁻⁶ and 9.7×10⁻⁶°C⁻¹ for α-La₂W₂O₉ and β-La₂W_1.2Mo_0.8O₉, respectively.     

双（1,2—丙二胺）合铜的TCNQ盐的合成与光谱研究

合成了导电性ＴＣＮＱ盐Ｃｕ（ｐｎ）２（ＴＣＮＱ）ｎ（ｎ＝２和３，ｐｎ＝１，２－丙二胺，ＴＣＮＱ＝７，７，８，８－四氰基对苯二醌二甲烷）。红外光谱、电子光谱和Ｘ－光电子能谱研究表明ＴＣＮＱ盐中存在ＴＣＮＱ°和ＴＣＮＱ－，ＴＣＮＱ°与ＴＣＮＱ－之间发生了部分电子转移，致使铜呈混合价态。它们的粉末室温电导率为１．１×１０－５～２．４×１０－６ｏｈｍ－１ｃｍ－１。     

Direct and simultaneous voltammetric analysis of heavy metals in tap water samples at Assiut city: an approach to improve the analysis time for nickel and cobalt determination at mercury film electrode

Tap water samples (Assiut city, lie in the middle north of upper Egypt, approx. 370 km from Cairo, January-March, 2002) were taken from the eight sampling sites of different locations at Assiut city. The samples are analyzed to determine the total content of cadmium, copper, lead and zinc by differential pulse anodic stripping voltammetry (DPASV) while nickel and cobalt are determined by a new simple differential pulse adsorptive stripping voltammetry (DPAdSV), using dimethylglyoxime (DMG) as the complexing agent. This method uses sodium sulfite as the supporting electrolyte, which facilitates the removal of oxygen interference without the traditional necessity of purging with inert gas. The effect of various parameters was studied using DPASV (for Cd, Pb, Cu and Zn) and AdSV (for Ni and Co) methods. Subsequently, under the so found experimental conditions, the stability of calibration curves and the detection limits (μg/l) have been determined. The data achieved (for all metals utility) are comparable to those measured by the graphite furnace atomic absorption spectrophotometric (GF-AAS) method. The effects of the interferences between these metal ions have been investigated. Moreover, the effect of storage was discussed and the obtained results were compared favorably with standard official methods. Statistical analysis of the database exhibits applicability and the accuracy of the techniques. The results obtained from the two techniques (Voltammetry and GF-AAS) are in very good agreements in the most tap water samples.