An Experimental Study of a Flux Modulated Solid State Metathesis Reaction

A solid state metathesis (SSM) reaction was investigated with respect to the formation of rare‐earth carbodiimides, the role of the co‐produced salt (LiCl), and the eutectic flux medium (LiCl/KCl). A SSM reaction is characterized by an exothermic reaction in which a salt (often LiCl) is coproduced. When the salt melts, it can serve as a useful medium for the crystallization of a desired product. An improved crystal growth can be observed by using an eutectic flux. However, the composition of an eutectic LiCl/KCl flux is altered when LiCl is produced during the reaction. The thermal effects concerning the endothermic melting of the flux and the exothermic ingnition of the SSM reaction may compensate each other, which is not necessarily a drawback for the reaction to proceed.     

Syntheses and structural characterization of New Tl + and K + complexes of 3,5-dinitrobenzoic acid (HDNB), [Tl(μ-DNB)] n and [K(μ-DNB)(μ-HDNB)] n

Two new Tl⁺ and K⁺ complexes of 3,5-dinitrobenzoic acid (HDNB), [Tl(μ-DNB)] _n and [K(μ-DNB)(μ-HDNB)] _n have been synthesized and characterized by elemental analysis, IR, ¹H NMR and ¹³C NMR spectroscopy. Determination of the structure of the [K(μ-DNB)(μ-HDNB)] _n and [Tl(μ-DNB)] _n by X-ray crystallography shows that there are nine coordinate K atoms (KO₉) and eight coordinate Tl atoms (TlO₈). The [Tl(μ-DNB)] _n and [K(μ-DNB)(μ-HDNB)] _n complexes are 2D and 3D coordination polymers, respectively.     

Crystal Structure and Interaction of 6-Amino Coumarin with Nitrite Ion for Its Selective Fluorescence Detection

ABSTRACT

6-Amino coumarin has been established as an efficient nitrite ion selective fluorescent sensor. The developed method shows linearity up to 1.6 × 10^?6 mol L^?1 of nitrite ion concentration. Interference from other common anions is almost negligible. The reagent shows strong binding affinity towards nitrite ion as evident from its binding constant value (5.8 × 10⁴), estimated by Stern-Volmer method. Some real samples were analyzed. Single crystal X-ray structure of the reagent is reported. Preliminary computational studies on the molecular level interaction between the reagent and nitrite ion were performed by density functional theory (DFT, B3LYP) method.     

Radioactive analysis and radiological hazards in different types of Egyptian cement

Studies of the natural γ-emitting radionuclides in different types of cements manufactured by different companies in Egypt (e.g. Iron (HI), Karnak (HK), and Super fine (HSu) products from Helwan Ltd.) have been done to determine their natural levels of radioactivity using a high-purity germanium detector (HPGe). Knowledge of radioactivity present in cement materials enables one to assess any possible radiological risks to human health. The results show that the highest mean values of ²²⁶Ra and ²³²Th activity are 234.01±20.12 and 46.56±4.65 Bq kg^?1, respectively, measured in cement sample ‘Iron’ from Helwan company (HI). The corresponding value of ⁴⁰K is 333.53±26.68 Bq kg^?1 measured in cement sample ‘Karnak’ from Helwan company (HK). For ¹³⁷Cs, this value is 3.27±0.31 Bq kg^?1 measured in cement sample (HI). The average concentrations of measured radionuclides in the different cement samples are 72.21±6.39, 24.98±2.24, 134.49±10.45, and 0.58±0.08 Bq kg^?1 for ²²⁶Ra, ²³²Th, ⁴⁰K, and ¹³⁷Cs, respectively. The measured activity concentrations for these radionuclides were compared with the reported data of other countries. Radium equivalent (Ra_eq) activities and different hazard indices were calculated to assess the radiation hazard. Iron HI cement sample shows a higher Ra_eq activity of 311.91±31.10 Bq kg^?1. Calculations of absorbed doses in nGy h^?1 show that the Iron (HI), Karnak (HK), and Super fine (HSu) products from Helwan company have higher activities than the permissible level (80 nGy h^?1). On the basis of the external hazard index (H _ex), Ra_eq activities, and annual effective dose rates for organs (H _organ), the natural radioactivity of cement samples is not greater than the recommended values in the established standards and hence safe for use in building constructions and therefore for inhabitants.     

依文思蓝-溴酸钾催化体系测定亚硝酸根

本文研究了亚硝酸根的一个新指示反应。在稀磷酸溶液中,依文思蓝-溴酸钾的氧化还原反应受亚硝酸盐催化使依文思蓝褪色。测定灵敏度为7.8×10-11g/mL亚硝酸态氮[当lg（Ao/A）=0.001 b=l cm)。测定范围0—3.5μg NO2/25mL,相对标准偏差1.64%。已用于测定自来水和唾液中的NO2-。     

亚硝酸钠化高铁血红蛋白的拉曼光谱量化检测研究

对亚硝酸钠化的高铁血红蛋白进行了拉曼光谱特性的研究。实验中将正常血红蛋白用亚硝酸钠氧化为高铁血红蛋白,通过测定不同比例高铁血红蛋白/总血红蛋白的拉曼光谱变化研究高铁血红蛋白的拉曼光谱特异性改变,并对不同比例高铁血红蛋白/总血红蛋白在1 586,1 605和1 637 cm-1处的拉曼强度进行线性拟合,以实现其定量检测。结果显示,亚硝酸钠与血红蛋白的摩尔比为3.5∶1时可以获得完全氧化的高铁血红蛋白,其拉曼特征峰在499,1 340,1 562,1 622 cm-1附近;不同比例高铁血红蛋白/总血红蛋白在1 586,1 605和1 637 cm-1处拉曼强度的线性拟合相关系数R2分别为0.972 84,0.997 97和0.991 26,显示出很好的线性关系。研究表明,与正常血红蛋白相比,亚硝酸钠化高铁血红蛋白的拉曼光谱具有特异性改变,其拉曼特征峰的位置和强度随着高铁血红蛋白/总血红蛋白比例的变化而相应发生改变,且比值与拉曼强度存在着线性相关关系,为临床上高铁血红蛋白血症的拉曼光谱检测与量化研究提供了理论基础。     

高碘酸钾催化光度法测定痕量铑

在磷酸和热水浴中 ,Rh( )催化高碘酸钾氧化二甲基黄褪色 ,由此建立了测定铑的新催化光度法。本方法的线性范围为 0— 4 .0 μg/ 2 5 m L,检出限为 4 .71× 10 -10 g/ m L。对 2 .0 μg/ 2 5 m L Rh( )测定的相对标准偏差为 1.4 3% (n=11) ,催化反应的表观活化能为 12 5 .8k J/ mol。此法已用于某些催化剂和冶金产品中痕量铑的测定 ,结果令人满意。     

催化动力学光度法测定痕量钴(Ⅱ)

本法基于钴 (Ⅱ )对高碘酸钾氧化孔雀绿的催化作用 ,提出一种灵敏地测定痕量钴 (Ⅱ )的新方法。该方法线性范围在 0～ 0 8μg·2 5mL- 1 ,检测限为 2 1× 10 - 1 0 g·mL- 1 。测定出反应表现活化能Ea=37 94kJ·mol- 1 。此法用于茶叶、维生素B1 2 中钴的测定 ,结果满意     

钾分子中里德堡态的紫外辐射研究

本文报道了在K-K₂系统中,利用双光子共振激发钾原子8s、6d态,观察到了K₂在(310～365nm)里德堡态的紫外辐射.钾分子里德堡态的布居,受到了多种激发过程影响.文中对其发射和激发过程进行了详细讨论.