银－2－羧基－4－溴苯基重氮氨基偶氮苯－Triton X－100－SDS显色体系的研究及应用

新三氮烯类试剂之一，２－羧基－４－溴苯基重氮氨基偶氮苯，在ｐＨ１１．０的Ｎａ_２Ｂ_４Ｏ_７－ＮａＯＨ缓冲介质中，有非离子表面活性剂ＴｒｉｔｏｎＸ－１００及阴离子表面活性剂ＳＤＳ的共同存在下，可与Ａｇ（Ⅰ）生成稳定的２∶１红色配合物，红色配合物的λ_（ｍａｘ）＝５４０ｎｍ，表观摩尔吸光系数ε_（５４０）＝１．１０×１０￣５Ｌ·ｍｏｌ￣（－１）·ｃｍ￣（－１）。Ａｇ量在０－１０μｇ／２５ｍＬ符合比尔定律。方法用于工业废水中痕量Ａｇ的测定，结果满意。     

Ultrasonic and infrared study of molecular interactions in ternary mixtures of 1-naphthol and 2-naphthol with 2-propanone in benzene

The measurements of ultrasonic velocity and density were made for the ternary mixtures of l-naphthol/2-naphthol with 2-propanone in benzene at 20, 30 and 40°C in the mole fraction range of 0.00 to 0.05. Adiabatic compressibility and intermolecular free length have been evaluated using ultrasonic velocity data. The non-linear variation of ultrasonic velocity and allied parameters with mole fraction indicates solute-solute interactions through hydrogen bonding between unlike molecules. Results of ultrasonic velocity and density measurements are further supported by FT-IR spectra. The change in transmittance as well as the shift in the frequency of the representative peak of the OH stretching in FT-IR spectra give inferences about the complex formation.     

新试剂2-(3-羧基-2,4,5-三氮唑偶氮)-5-二甲氨基苯磺酸与钯显色反应的研究及应用

本文合成了水溶性新型显色剂 2 - (3-羧基 - 2 ,4 ,5 -三氮唑偶氮 ) - 5 -二甲氨基苯磺酸 (CTZAMBS) ,并研究了其与钯的显色反应。结果表明 ,在 p H=1.5 8邻苯二甲酸氢钾缓冲液中 ,试剂与钯形成 2∶ 1蓝色络合物 ,λmax为 5 78.6nm,钯含量在 0— 2 .0 μg·m L-1范围内符合比耳定律 ,表观摩尔吸光系数为 3.19× 10 4 L·mol-1· cm-1,选择性好。本方法可直接测定钯催化剂中的微量钯 ,操作简便 ,结果令人满意     

Influence of the structural nonrigidity of nitrobenzene, 1-nitrosonaphthalene,and 1-nitroso-2-naphthol molecules on the absorption spectra

Nitrosobenzene, 1-nitrosonaphthalene, and 1-nitroso-2-naphthol molecules are investigated by experimental and quantum-chemical methods. For all molecules, the optimized structure is established and analyzed by the molecular dynamics method. For nitrobenzene and 1-nitrosonaphthalene, 10 geometrical structures with different angles of nitrosogroup rotation are investigated together with the energy, oscillator force, and nature of the electronic states. The 1-nitroso-2-naphthol absorption spectrum is interpreted. The dipole moments of molecules are estimated. Possible interaction centers of molecules with a protonodonor solvent are determined.     

5-羧基-3-氨基-1,2,4-三氮唑芳香醛席夫碱的合成与表征

利用氨基胍碳酸氢盐与草酸反应合成5-羧基-3-氨基-1,2,4-三氮唑,然后用5-羧基-3-氨基-1,2,4-三氮唑与芳香醛反应,合成了2种5-羧基-3-氨基-1,2,4-三氮唑芳香醛席夫碱,通过元素分析,红外光谱和紫外光谱对产物的结构进行了表征.     

Thermodynamic Analysis and Crystallographic Properties of MFe2O4, MCr2O4 and MAl2O4 (M = Fe,Ni, Zn) Formed on Structural Materials in Pressurized Water Reactor Primary Circuit under Zinc and Zinc-aluminum Water Chemistry

Zinc injection technology (zinc water chemistry, ZWC) was widely applied in pressurized water reactor (PWR) primary circuits to reduce radiation buildup and improve corrosion resistance of structural materials. The simultaneous injection of zinc-aluminium (ZAWC) is a novel implement created to replace part of Zn²⁺ by Al³⁺. It was reported ZAWC can improve further corrosion resistance of carbon steels and stainless steels. However, ZAWC sometimes showed even negative effects on Nickel-alloys. In this study, mechanism of formation of oxide film on metals was investigated. The reactions of Fe²⁺ Ni²⁺ in oxide films replaced by Zn²⁺, or Fe³⁺ replaced by Al³⁺ in ZAWC were analysed. The thermodynamic data and solubility of mixed oxides (ZnFe₂O₄, ZnCr₂O₄, and ZnAl₂O₄), the products of replace reactions, were calculated. According to the Gibbs free energy difference between products and reactants, ΔGθ(T) values of the formation reaction of ZnFe₂O₄, ZnCr₂O₄, and ZnAl₂O₄ are extremely negative. Solubility of ZnAl₂O₄ is the lowest among mixed oxide products, which implies the oxide film composites of ZnAl₂O₄ may show a lower corrosion rate. In addition, the preferential formation of NiAl₂O₄ on Ni-based-alloy, under ZAWC, was discussed based on crystallographic properties of spinel, which was considered as the cause of negative effects of ZAWC on corrosion resistance of Nickel-alloys. This research provides an analytical basis for the study of thermodynamic stability of oxide films under different chemical chemistry and a theoretical basis for improving corrosion resistance of different metals and optimizing the chemical conditions of PWR primary circuit.     

Structural and dielectric properties of Pb(Li1/4Dy1/4W1/2)O3

The polycrystalline samples of Pb(Li_1/4Dy_1/4W_1/2)O₃ have been synthesized by high-temperature solid-state reaction techniques. Room temperature X-ray diffraction (XRD) studies of the compound provided preliminary structural data, and hence formation of a single phase desired material was confirmed. Detailed studies of dielectric constant (ε) and loss (tanδ) as a function of frequency (100 Hz to 10 kHz) at room temperature (298 K) and also as a function of temperature (liquid nitrogen to 403 K) at 10 kHz suggest that the compound undergoes a ferroelectric phase transition of diffuse type.     

Synthesis,Structural and Magnetic Resonance Studies of YxEr2-xCu2O5 Compounds

Polycrystalline samples of Y_xEr_2—xCu₂O₅ compound, where x = 2.0, 1.75, 1.5, 1.25. 1.0,0.75.0.25, and 0.0, have been synthesized by the solid state reaction technique. The XRD measurements have shown that the obtained samples were single-phase and belong to the orthorhombic space group Pna2₁. The measured lattice constants of Y_xEr_2-xCu₂O₅ compounds scaled linearly with the itrium index x. The TGA/DSC measurements allowed to establish the temperature range of stability for the samples and enabled the observation of their decomposition. EPR studies at room temperature showed that the integral intensity of the resonance line decreases nonlinearly with the increasing erbium content and that the Er₂Cu₂O₅ compound is EPR inactive. A broad copper EPR line has been analyzed in order to establish the contributions of different spin—spin relaxation mechanism. The observed resonance linewidth has been explained by the action of the dipole—dipole, anisotropic exchange, and Dzialoshinky—Moriya (DM) interactions.     

1-亚硝基-2-萘酚为配合剂流动注射固相富集原子吸收光谱法测定铜和钴

本文研究了用１－亚硝基－２－萘酚为配合剂，Ｃ１８键合硅胶为固相富集材料，流动注射在线固相萃取预富集火焰原子吸收测定痕量和钴的方法。该方法自动化程度高，选择性强，方法的采样速度达９０ｈ＾－１时，铜和钴的订九分别达２０倍和１８倍，检出限分别达１．８μｇ／Ｌ和３μｇ／Ｌ。用这一方法来测定生物样品淡菜、钢样ＮＢＳ－３６４和ＮＢＳ－３６２等标准样品，结果与标准值相符。     

Synthesis and Structural Characterization of a New Phase of GaAsO 4

A new polymorph of GaAsO 4 has been synthesised at high pressure and temperature (60 kbar and 1273 K). Samples were characterised by powder X-ray diffraction, scanning electron microscopy and EDAX spectroscopy. This material shows an hexagonal symmetry with cell parameters, a =8.1931(4) Å and c =4.3744(2) Å; particles are of hexagonal shape with a narrow size distribution around 2-3 w m and composition close to the Ga:As atomic ratio=1:1. This new high pressure phase of GaAsO 4 represents a new transition path for the ABO 4 compounds.     

Effect of Synthesis Conditions on the Structural,Photocatalic, and Self-Cleaning Properties of TiO2 Nanoparticles

Physics of the Solid State - TiO2 nanoparticles were synthesized via the hydrothermal method. As-synthesized TiO2 properties were characterized by XRD, EDX, FESEM, FTIR, and UV-Vis spectroscopy....     

Ultrasound-promoted synthesis of 1-amidoalkyl-2-naphthols via a three-component condensation of 2-naphthol, ureas/amides, and aldehydes, catalyzed by sulfamic acid under ambient conditions

A three-component one-pot condensation of 2-naphthol, ureas/amides and aldehydes catalyzed by sulfamic acid, under ultrasound irradiation and ambient conditions gives 1-amidoalkyl-2-naphthols in excellent yield and in short time.     

4(5)-氰基咪唑的合成与表征

以D-果糖为初始原料,经环合、氧化,再加入盐酸羟胺作为氰基化试剂一步法制得4(5)-氰基咪唑.利用1H NMR、13C NMR等手段对各步所得产物的结构进行了表征,结果表明产物为4(5)-氰基咪唑.以D-果糖计,3步反应的总收率为33.5％.     

Synthesis, structure, and dielectric properties of KH2PO4 fractal aggregates

Macroscopic fractal aggregates of KH₂PH₄ (KDP) measuring up to 500 μm have been obtained. The fractal structure forms as a result of the precipitation of KDP particles from a supersaturated aqueous solution in the presence of a temperature gradient followed by a diffusioncontrolled mechanism of aggregation. The electron-microscopic analysis performed has shown that the fractals are formed predominantly from crystallites of the tetragonal modification measuring ∼1 μm. The dielectric constant (ɛ) of fractal KH₂PO₄ has been measured in the temperature range 80–300 K. A characteristic anomaly has been discovered on the ɛ(T) curve in the vicinity of 122 K, which attests to a ferroelectric phase transition. The absolute value of ɛ is significantly smaller than the components ɛ ₁₁ and ɛ ₃₃ for KH₂PO₄. Fiz. Tverd. Tela (St. Petersburg) 41, 2059–2061 (November 1999)     

LiMn2−xTixO4 spinel-type compounds (x ≤ 1): Structural,electrical and magnetic properties

LiMn_2−xTi_xO₄ compounds with 0 ≤ x ≤ 1 were prepared by solid state reaction and Pechini technique. Powder X-ray diffraction showed that all samples crystallize with the spinel crystal structure (S.G. Fd3¯m). The cubic unit-cell parameter increases with the Ti content. The influence of the Ti content and cationic distribution on the magnetic properties of the compounds was studied by measuring the temperature and magnetic field dependences of the magnetization: substitution by non-magnetic d⁰ Ti⁴⁺ ions appeared to weaken the magnetic interactions between the manganese ions. The electrical properties of LiMnTiO₄ were studied by AC impedance spectroscopy and DC polarisation measurements, which revealed the electronic character of the conduction process.     

1，1－二氯双硅烷热分解的理论研究

用ＭＮＤＯ方法研究了１，１－二氯双硅烷的热分解反应，得到了两条反应途径及其过渡态，证明了１，１－二氯双硅烷的热分解是通过１，２－氢迁移和２，１－氢迁移实现的。     

1-[2-(2,4-二氯苯基)-4-烷基-1,3-二氧戊环-2-基甲基]-1H-1,2,4-三唑的NMR研究

测定了戊环唑（1）、甲环唑（2）、丙环唑（3）的NMR谱,对其一般特征进行 了对比与讨论,用¹³C-¹H COSY、¹³C-¹H COLOC、DQF-COSY、DEPT等技术对它们的¹H、¹³C NMR谱峰进行了全归属,并应用¹H-¹H NOESY谱研究其立体结构.
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