Use of a Tensammetric Wave for the End-Point Detection in Chelatometry

Abstract

A new method for the end-point detection in complexometric titration using a tensammetric wave of organic reagents such as oxine and alizarin complexone (ALC) was studied. The tensammetric wave of these reagents disappears by their chelate formation and reappears by the liberation of free indicator during the exchange reaction between indicator chelate and EDTA. This mechanism is utilized for the end-point detection in complexometric titration of metals. Since the sensitivity of tensammetric wave is extremely high, very sharp end-point can be obtained for the titration of metals even in the concentration of 10^?5M.     

Effect of solvent on the construction of Co(II) coordination polymers containing a semi-rigid bis(benzimidazole) derivative: syntheses,structures, and properties

Two Co(II) coordination polymers, [CoL(npa)]·2H₂O (1) and [CoL(Hnpa)₂] (2) (L = 1,4-bis(5,6-dimethylbenzimidazole-1-yl)benzene, H₂npa = 5-nitroisophthalic acid), have been synthesized in different solvent systems and characterized by Infrared (IR) spectroscopy, elemental analysis, and powder and single crystal X-ray diffraction. Compound 1 was synthesized under solvothermal conditions with DMF as solvent and had a pair of L ligands adopting a μ₂-bridging mode and connecting two Co²⁺ cations to generate a 26-membered Co₂L₂ loop. The npa^2? link adjacent Co₂L₂ loops via a bis(monodentate) bridging mode to create a 1-D channel-like chain structure. Compound 2 was obtained under hydrothermal conditions, and the carboxylate of the monodeprotonated Hnpa^? adopt a μ₁-η^0?:?η¹ coordination to connect adjacent Co²⁺ cations into a 2-D polymeric layer. The μ₂-bridging L ligands connect adjacent 2-D [Co(Hnpa)]_n polymeric layers into a 3-D NaCl-like framework. The Co²⁺ cations and the L ligands in compounds 1 and 2 exhibit different coordination geometries and conformations. Effects of solvents on the construction of Co(II) coordination polymers were investigated. In addition, the electrochemical behavior of carbon paste electrodes containing 1 and 2 and the thermal stabilities of 1 and 2 were investigated.     

ICP－AES法测定钨合金中镍、钴、铁、锰时酸度的影响

本文研究了用电感耦合等离子体发射光谱技术测定钨合金中镍、钴、铁、锰含量的方法及酸度对测量结果的影响。用氢氟酸及硝酸处理试样，并加入适量盐酸。实验研究了测量值随氯离子浓度增大而下降的变化曲线，找出了测量不同元素的最佳测定条件，测量结果同标准值比较，误差较小。     

双齿配体—1,2—C_6H_4SX(X=O,S)的钴化合物~1H NMR研究

以~1H NMR谱学和磁化率对一些含邻苯二硫酚或巯基苯酚配体的钴化合物的磁性作了研究,并讨论了它们的电子结构。     

First-principles study of antiferromagnetic cobalt spinels

We report a comparative study of the electronic structure and magnetic properties of two cobalt compounds Co₃O₄ and Co₃S₄, through first-principles Hubbard-U calculations. Our results indicate that Co₃O₄ and Co₃S₄ have similarities in crystal structure (normal spinel), magnetic order (antiferromagnetism), Co spin configuration (high spin Co²⁺ and low spin Co³⁺), and comparable band-gap energy. However, the U-dependence on electronic structure in two materials are different from each other. With a change in the applied U values, the band dispersion and the type of band gap are significantly changed in Co₃O₄, while the band-gap energy only is affected in Co₃S₄.     

Structural studies on banana oil,isoamyl acetate,by means of microwave spectroscopy and quantum chemical calculations

The rotational spectrum of isoamyl acetate, H₃C–COO–(CH₂)₂–CH(CH₃)₂, has been recorded and assigned using a molecular beam Fourier transform microwave (MB-FTMW) spectrometer in the frequency range of 3–26.5?GHz. One conformer has been observed. By comparing the spectroscopic data with the quantum chemical data, it was found that the conformer observed does not have C_s symmetry. The rotational and centrifugal distortion constants were determined. The barrier to internal rotation of the acetate methyl group was found to be 93.98?cm^?1. Due to the high number of the conformers, a systematic nomenclature will be presented.     

Preparation and Flammability of a Flame-Retardant Poly(Butyl Acrylate-Vinyl Acetate) System Based on Gemin-Surfactant Modified Montmorillonite and Ammonium Polyphosphate

Gemin-surfactant modified montmorillonite (G-MMT) was successfully prepared by an ion exchange reaction and characterized via Fourier-transform infrared spectroscopy (FTIR) and X-ray diffraction (XRD). The P(BA-VAc)/G-MMT emulsion was prepared via an in-situ polymerization method using potassium persulfate (K₂S₂O₈, KPS) as an initiator. Ammonium polyphosphate (APP) was introduced for obtaining P(BA-VAc)/APP/G-MMT flame-retardant latex with a constant total content of 15 wt% of APP and G-MMT in P(BA-VAc). The flame retardancy and thermal behavior of the latex films were investigated by limiting oxygen index (LOI), vertical burning test (UL-94) and thermal gravimetric analysis (TG/DTA). Compared with the P(BA-VAc)/APP composite, the LOI value of P(BA-VAc)/APP/G-MMT containing 0.5 wt% G-MMT at the same total additive loading increased to 29.1 from 20.0 and its UL-94 increased from no rating to V-0. Thermal gravimetric (TG) data showed that the amount of residues increased significantly with the loading of G-MMT. In addition, the LOI values increased with the increase in char residues. The morphology and microstructure of the residues generated during LOI testing were investigated by scanning electron microscopy (SEM). The outer surfaces of P(BA-VAc)/APP/G-MMT charred layers were more continuous and compact than those of P(BA-VAc)/APP.     

The Determination of Lactate or Acetate in Intravenous Infusions and Haemodialys1S Solutions by 1H NMR Spectroscopy

A ¹H NMR spectroscopic determination for acetate and lactate in intravenous and haemodialysis solutions is reported. The methyl resonances of acetate and lactate were chosen for integration using N-methylurea and sodium acetate, respectively, as internal standards. The results obtained indicate that the quantitative measurements are reproducible. The method provides also a specific identification of the analytes.     

Atmospheric oxidation chemistry of 1–methoxy 2–propyl acetate initiated by OH radicals: kinetics and mechanisms

Kinetics and mechanism of the gas-phase reaction of CH₃C(O)OCH(CH₃)CH₂OCH₃ (MPA) with OH radicals in the presence of O₂ and NO have been investigated theoretically by performing a high and reliable level of theory, viz., CCSD(T)/6-311?+?G(d,p)//BH&HLYP/6-311++G(d,p)?+?0.9335×ZPE. The calculations predict that the H-abstraction from the ?CH₂?O? position of MPA is the most facile channel, which leads to the formation of the corresponding alkoxy radicals CH₃C(O)OCH(CH₃)C(O ?)HOCH₃ under atmospheric conditions. This activated radicals CH₃C(O)OCH(CH₃)C(O ?)HOCH₃ will undergo further rearrangement, fragmentation and oxidative reactions and predominantly leads to the formation of various products (methyl formate HC(O)OCH₃ and acetic anhydride CH₃C(O)OC(O)CH₃). In the presence of water, acetic anhydride can convert into acetic acid CH₃C(O)OH via the hydrolysis reaction. The calculated total rate constants over the temperature range 263–372?K are used to derive a negative activation energy (E_a= ?5.88 kJ/mol) and an pre-exponential factor (A?=?1.78×10^?12 cm³ molecule^?1 s^?1). The obtained Arrhenius parameters presented here are in strong agreement with the experimental values. Moreover, the temperature dependence of the total rate constant over a temperature range of 263?1000?K can be described by k?=?5.60 × 10^?14×(T/298?K)^3.4×exp(1725.7?K/T) cm³ molecule^?1 s^?1.     

Cu/HMOR催化二甲醚羰基化合成乙酸甲酯: 催化剂制备方法的影响 (cited: 2)

采用氨蒸发法、尿素水解法、离子交换法及浸渍法制备HMOR负载的Cu催化剂, 考察其催化二甲醚(DME)羰基化合成乙酸甲酯(MA)性能. 结果表明离子交换法制得Cu/HMOR催化剂在Cu的金属中心和酸性分子筛载体的共同作用下具有较好催化反应活性. 在210 oC、1.5 MPa、空速4883 h^-1,DME转化率为95.3%,MA选择性为94.9%. 对催化剂进行N2物理吸附、X射线衍射、NH₃程序升温脱附和CO程序升温脱附等表征发现,离子交换法制得Cu/HMOR催化剂具有较高比表面、大量弱酸及一定中强酸、适中的CO吸附强度,提高了CO插入DME羰基化反应活性.