散射背景下激光热透镜光谱分析法测定人体血清中锌量

建立了散射背景下测定人体血清中Zn^2＋含量的激光热透镜光谱分析方法。比较了蛋白质微粒散射对于分光光度法和激光热透镜光谱分析法测定的影响。结果表明，激光热透镜光谱分析方法能够避免溶液中存留蛋白质微粒散射的影响。Zn^2＋量在0～1．6μg/mL范围内呈线性关系（r=0．9986），检出限为1ng/mL。应用于人体血清中Zn^2＋含量的测定，与原子吸收法测定结果基本一致。     

纳米PbSnO3的制备及其燃烧催化性能的研究

Nanocomposite PbSnO₃was synthesized by coprecipitation method , and its phase evolution process was investigated. The particle size, crystal form, and phase of samples were determined with XRD, TEM and EDS. The catalytic actiyity of sample on the thermal decomposition of RDX was investigated by DSC. The results show that nanocomposite PbSnO₃with the diameter of 9 nm can be obtained by calcining at 600 ℃ for 2 h, which crystal is cubic (pyrochlore type). The catalytic actiyity of nanocomposite PbSnO₃on the thermal decomposition of RDX is much higher than that of normal PbSnO₃. The nanocomposite PbSnO₃can decrease the peak temperature of thermal decomposition of RDX from 240.1 ℃ to 236.5 ℃, and the decomposition enthalpy ΔH of RDX increases 722 J·g^-1 （about 70%）.     

Characterisation of the comonomer composition and distribution of copolymers using chemometric techniques

Chemometric techniques have been applied to FTIR and DSC data to correlate polymer composition. Since structural differences in the polymers with only hydrocarbon structure, often cause subtle changes in spectra, the ability of chemometric techniques is required to discern these differences. FTIR spectra and thermal fractionation using DSC were measured for 28 types of polyethylenes (PE) varying in chain branching type, content and distribution. Unsupervised clustering methods such as principal component analysis (PCA) and supervised discriminant analysis were used to classify the PEs according to their structural class. The DSC data was the more successful in both classifying PEs according to their class. This revised version was published online in July 2006 with corrections to the Cover Date.     

Thermal Stability Of Folic Acid in the solid-state

This study attempts to identify the degradative process which folic acid undergoes in the solid-state under thermal stress. In order to facilitate the process, the various pieces of the chemical structure, namely, p-amino benzoic acid, pterin and glutamic acid as both its d- and l-isomers were investigated as separate entities. These structured solid-state pieces were then compared to the composite solid state folic acid degradative curves in order to identify the peaks seen and provide direction for the interpolation of the degradative mechanism. It was observed that none of the structural pieces could be superimposed as assumed earlier and hence an attempt was made to identify the decomposition products using various analytical techniques such as infrared spectroscopy, mass spectroscopy and X-ray diffraction which suggested that the glutamic acid fragment is lost first as evidenced by acid loss and amide enhancement in the IR spectra. The vitamin was ultimately degrading to carbon fragments and that further identification was not necessary. This revised version was published online in August 2006 with corrections to the Cover Date.     

Transition metal(II) ions with dinegative tetradentate schiff base

Some new coordination polymers of Mn(II), Co(II), Ni(II), Cu(II), Zn(II) and Cd(II), obtained from the interaction of metal acetate with dipotassium salt of N,N’-di(carboxyethylidene)terephthalaldehydediimine (K₂SB) are described. The products, which have been characterized by elemental analyses, magnetic measurements, thermogravimetric analyses, electronic and infrared spectral studies, have composition, [M(SB)(H₂O)₂]_n. These colored coordination polymers are non-hygroscopic and quite stable at room temperature. On the basis of analytical data and IR studies, a 1:1 metal to ligand stoichiometry has been suggested to these coordination polymers. The IR studies have also revealed that ligands are coordinated to metal ion through carboxy oxygen and azomethine nitrogen. All the studies suggested tetradentate nature of the ligand with octahedral symmetry of the coordination polymers. All the coordination polymers are insoluble in acetone, ethanol, chloroform, methanol, benzene, DMF and DMSO. The thermal decomposition of the coordination polymers is studied and indicates that not only the coordinated water is lost but also that the decomposition of the ligand from the coordination polymers is necessary to interpret the successive mass loss.     

Memory effects in isothermal crystallization II. Isotactic polypropylene

The effects of temperature and duration of melting on the rate of isothermal crystallization of isotactic polypropylene were investigated by differential scanning calorimetry (DSC). Crystallization rates were found to decrease with increasing melt temperature and melting time. The results were discussed in the framework of the theoretical model of transient isothermal crystallization developed by the present authors [1]. The results suggest gradual destruction of predetermined nuclei with activation energyE _a=89±7 kJ/mole as a main mechanism of the observed effects.This work and Part I of this research [1] have been supported in part by Research Grant Number PB 1291/52/93/04 from State Committee for Scientific Research (KBN), Poland, and by 40% MURST founds, Italy.     

XPS,AFM, ATR and TPD evidence for terraced,dihydrogen terminated, 1×1 (100) silicon

Heating (100) silicon at high temperature (say, higher than 850 °C) in H₂, cooling to 670–700 °C in the same ambient, and quenching to room temperature in N₂ results in environmentally robust, terraced 1 × 1 (100) SiH₂. Evidence for this conclusion is based on angle‐resolved x‐ray photoelectron spectroscopy, atomic force microscopy, infrared absorption spectroscopy in the attenuated total reflection mode, thermal programmed desorption, and reflection high‐energy electron diffraction. Copyright © 2005 John Wiley & Sons, Ltd.     

Synthesis, Characterization and Thermal Decomposition Mechanism of Cetyltrimethyl Ammonium Tetrathiotungstate

The synthesis, characterization and thermal decomposition mechanism of cetyltrimethyl ammonium tetrathiotungstate （CTriMATT） were studied herein. The as-synthesized CTriMATT was characterized by Elemental analysis, X-ray diffraction （XRD）, Fourier transform infrared （FT-IR）, Ultraviolet visible （UV-Vis） spectra. The results showed that the as-synthesized CTriMATT had high purity and good crystallinity. The introduction of alkyl groups induced a shift of the stretching vibration band of W-S bond to lower wavenumber, while it had no influence on the position of WS4^2-. Thermogravimetric analysis （TG）, differential thermal analysis （DTA） and in situ XRD characterizations revealed that CTriMATT began to decompose at 423 K in nitrogen and was converted to WS2 eventually. In addition, the decomposition product of CTriMATT at 673 K in nitrogen was characterized by N2 adsorption （BET） and scanning electron microscopy （SEM）. The results demonstrated that WS2 with higher specific surface area, and pore volume could be obtained from the thermal decomposition of CTriMATT in nitrogen.     

聚氯乙烯接枝丙烯酸稀土的研究

将无机稀土有机化后与聚氯乙烯(PVC)进行接枝共聚。探讨了氧化稀土与丙烯酸反应、PVC接枝丙烯酸稀土的原理和方法，并通过红外光谱、扫描电镜对接枝共聚物进行定性表征，用微量热天平对接枝共聚物的热性能进行测定。实验结果表明，经丙烯酸稀土接枝共聚后的PVC，其耐热分解性能和韧性有了明显的提高。     

A comparative study on the thermal decomposition of some transition metal carboxylates

Thermal decomposition of transition metal malonates, MCH₂C₂O₄?xH₂O and transition metal succinates, M(CH₂)₂C₂O₄?xH₂O (M=Mn, Fe, Co, Ni, Cu, Zn) has been studied employing TG, DTG, DTA, XRD, SEM, IR and Mössbauer spectroscopic techniques. After dehydration, the anhydrous metal malonates and succinates decompose directly to their respective metal oxides in the temperature ranges 310–400 and 400–525°C, respectively. The oxides obtained have been found to be nanosized. The thermal stability of succinates have been found to be higher than that of the respective malonates.