Analysis of anions by solid-state spot-tests

Trituration and capillary solid-state spot-tests for 25 anions with a number of organic and inorganic reagents have been examined. A comparative study of the corresponding reactions in solution has also been made. Incorporation of a glass-wool plug in the capillary improves the selectivity. Schemes are presented for possible use of the technique.     

Enzyme production and profile by Aspergillus niger during solid substrate fermentation using palm kernel cake as substrate

The oil palm sector is one of the major plantation industries in Malaysia. Palm kernel cake is a byproduct of extracted palm kernel oil. Mostly palm kernel cake is wasted or is mixed with other nutrients and used as animal feed, especially for ruminant animals. Recently, palm kernel cake has been identified as an important ingredient for the formulation of animal feed, and it is also exported especially to Europe, South Korea, and Japan. It can barely be consumed by nonruminant (monogastric) animals owing to the high percentages of hemicellulose and cellulose contents. Palm kernel cake must undergo suitable pretreatment in order to decrease the percentage of hemicellulose and cellulose. One of the methods employed in this study is fermentation with microorganisms, particularly fungi, to partially degrade the hemicellulose and cellulose content. This work focused on the production of enzymes by Aspergillus niger and profiling using palm kernel cake as carbon source.     

Construction of solid-liquid phase diagrams in ternary systems by titration calorimetry

Titration calorimetry was used to construct the solid-liquid equilibrium line in ternary systems containing the solute and an aqueous mixed solvent by measuring the heat of dissolution of the solid solute during successive additions of the liquid solvent. The plot of cumulated heats versus the mole ratio, n_solvent/n_solute, yields two (almost) linear increases of different slopes. These two lines represent successively the enthalpy of dissolution then the enthalpy of dilution of the medium; their intersection gives the solubility and the enthalpy of dissolution of the solute. Phase diagrams have been established over the whole concentration range for o-anisaldehyde, 1,3,5-trimethoxybenzene and vanillin, in water + methanol, +ethanol, or +n-propanol at 303, 313 and 318 K.     

A facile synthesis of new 3-(2-benzimidazolyl)-2-alkyl-4-(3H)-quinazolinones under microwave irradiation

Preparation of 2-amino-N-(1-H-benzimidazol-2-yl)benzamide and a variety of new 3-(2-benzimidazolyl)-2-alkyl-4-(3H)-quinazolinones using isatoic anhydride, 2-aminobenzimidazole and orthoesters under microwave irradiation are described.     

A Method for the Acetylation of Alcohols Catalyzed by Heteropolyoxometallates

Summary. Esterifications of acetic acid with some linear, secondary, tertiary, and benzylic alcohols mediated by catalytic amounts of Keggin, Wells–Dawson, and Preyssler type heteropolyacids were carried out under reflux at mild reaction conditions with good to excellent yields. Among the examined catalysts, H₃PW₁₂O₄₀ and H₁₄NaP₅W₃₀O₁₁₀ revealed better results than other heteropolyacids. This work was performed with the aim of simplifying the esterification process by omitting any solvents and mineral acid catalysts. Easy work-up, low cost, and acidic waste reduction, which are all important features from the environmental and economical points of view, are distinct aspects of this protocol. Heteropolyacid catalysts could be separated after a simple work-up and reused for several times.     

Water as an Efficient Solvent for Oxygenation Transformations with 34% Hydrogen Peroxide Catalyzed by some Heteropolyoxometalates

Summary. A highly efficient, selective, fast, and cheap protocol is developed for oxidation of aromatic amines and alcohols utilizing 34% hydrogen peroxide in water catalyzed by some W- and Mo-based heteropolyoxometalates. Findings showed that dodecatungstophosphoric acid, H₃PW₁₂O₄₀, was the most efficient catalyst in the examined oxidation reactions. This methodology may prove to be a valuable alternative for eco-friendly green oxidation. Inherent simplicity, easy work up, and using regenerable catalysts were other key aspects of this oxidation protocol.     

Headspace solvent microextraction of trihalomethane compounds into a single drop

Headspace solvent microextraction (HSME) into a single drop is developed for the determination of six trihalomethanes, CH2Cl2, CHCl3, C4H9Cl, CCl4, C2HCl3, and C2Cl4, in aqueous solution. A drop of benzyl alcohol containing bromoform, as an internal standard, is used for extraction. The analytes are extracted by suspending a 3-microL drop directly from the needle of a microsyringe. The needle passes through the septum of a vessel, and the needle tip appears above the surface of the solution. After the prescribed extraction time, the drop is drawn back into the syringe. The syringe is then removed, and its content is injected directly into a gas chromatography column for analysis. The main parameters affecting the HSME process, such as stirring speed, microdrop volume, sample solution temperature, microsyringe needle temperature, sample volume, solution pH, extracting solvent, and ionic strength of the solution, are studied. Also, the linear range and precision of the method are examined.     

Solvation numbers and hydration constant for thorium(IV) in ethanol-water medium

The solvation number and hydration constant of Th⁴⁺ in ethanol-water medium were determined at 25°C using UV-spectral and electrochemical measurements. A solvate formation equilibrium is demonstrated and characterized. Three molecules of ethanol (S) can bond to the metal cation with strengths comparable to that for H₂O to form ThS₃(H₂O) ₃ ⁴⁺ Formation of thorium monochelate with lawsone (2-hydroxy-1,4-naphthoquinone) eliminates bonding with alcohol molecules. The dissociation constant of the chelating agent_sK_a and the formation contant of the monochelated metal ion_sK _f ^* that are essentially independent of the solution composition are evaluated. Hydration titrations involving thorium-lawsone monochelate are performed and the data obtained from the changes of pH with solvent composition are analyzed. The solution independent constant,_sK _f ^* for thorium-lawsone complex formation in mixed aqueous ethanol is given by $$log_s K_f * = vpK_a + log_s K_h - log[LH] - vpH + 3logv$$ where vpK_a is the dissociation constant of the chelating agent LH in the solvent system of ν volume fraction of water and_sK_h is the solution-independent hydration constant of thorium (IV) in the solvent system. Log-values for the constants_sK_h,_sK _f ^* and_sK _a ^* are found to be 7.8±0.02, 11.38±0.04 and ?0.753, respectively.     

以金属硫酸氢盐为催化剂在无溶剂条件下高效合成3,4-二氢嘧啶-2(1H)-酮

以金属硫酸氢盐M(HSO4)n(Ca(HSO4)2,Zn(HSO4)2和过硫酸氢钾制剂oxone○R)为催化剂催化醛、1,3-二羰基化合物和尿素进行缩合反应,在90℃及无溶剂的条件下高收率、一锅法合成了3,4-二氢嘧啶-2(1H)-酮.     

SnCl4 and SbCl5 promoted aromatization of enamines

Aromatic amines have been synthesized efficiently from enamines using SnCl₄ and SbCl₅ in CH₂Cl₂ at room temperature.