Pulse EPR Methods for Studying Chemical and Biological Samples Containing Transition Metals

This review discusses the application of pulse EPR to the characterization of disordered systems, with an emphasis on samples containing transition metals. Electron nuclear double‐resonance (ENDOR), electron‐spin‐echo envelope‐modulation (ESEEM), and double electron–electron resonance (DEER) methodologies are outlined. The theory of field modulation is outlined, and its application is illustrated with DEER experiments. The simulation of powder spectra in EPR is discussed, and strategies for optimization are given. The implementation of this armory of techniques is demonstrated on a rich variety of chemical systems: several porphyrin derivatives that are found in proteins and used as model systems, otherwise highly reactive aminyl radicals stabilized with electron‐rich transition metals, and nitroxide–copper–nitroxide clusters. These examples show that multi‐frequency continuous‐wave (CW) and pulse EPR provides detailed information about disordered systems.     

Clay Supported Bis-(trimethylsilyl)-chromate: An Efficient Reagent for Oxidative Deoximation

Summary.  A convenient method for the direct conversion of oximes to carbonyl compounds upon treatment with clay supported BTSC under classical heating as well as microwave irradiation in a solvent-free system is described.     

An experimental investigation of polyacrylamide and sulfonated polyacrylamides based gels crosslinked with cr(III)-acetate for water shutoff in fractured oil reservoirs

Abstract

Water injection as one of the most efficient and worldwide extensively employed approach in homogenous oil reservoirs suffers from early water breakthrough time as well as low oil sweep efficiency values in fractured oil reservoirs. This study investigates the potential application of Cr(III)-acetate based gel polymer system in a typical water injection process using one fractured micromodel. For this purpose, three sulfonated polyacrylamides, different in solfunation degree, and one hydrolyzed polyacrylamide were studied regarding gelation time, gel strength and stability to find the optimized conditions in terms of polymer type and concentration, and polymer/Cr(III)-acetate ratio, which were subsequently used for one dynamic test. Results illustrated the optimized conditions as AN 105 polymer with concentration of 5000?ppm and polymer/Cr(III) ratio of 5. Moreover, results showed that implementing such gel system yields an increased oil recovery value of 24.46% OOIP at 1.55 PV and delays the breakthrough time from 0.47 PV to 0.51 PV.     

Expanded capsules with reversibly added spacers

Glycolurils insert as spacer elements in a capsule to create a new space with enhanced dimensions.     

A rapid derivative spectrophotometric method for simultaneous determination of naphazoline and antazoline in eye drops

A zero-crossing first-derivative spectrophotometric method is applied for the simultaneous determination of naphazoline hydrochloride and antazoline phosphate in eye drops. The measurements were carried out at wavelengths of 225 and 252 nm for naphazoline hydrochloride and antazoline phosphate, respectively. The method was found to be linear (r2>0.999) in the range of 0.2-1 microg/ml for naphazoline hydrochloride in the presence of 5 microg/ml antazoline phosphate at 225 nm. The same linear correlation (r2>0.999) was obtained in the range of 1-10 microg/ml of antazoline phosphate in the presence of 0.5 microg/ml of naphazoline hydrochloride at 252 nm. The limit of determination was 0.2 microg/ml and 1 microg/ml for naphazoline hydrochloride and antazoline phosphate, respectively. The method was successfully used for simultaneous analysis of naphazoline hydrochloride and antazoline phosphate in eye drops without any interference from excipients and prior separation before analysis.     

Validated HPLC method for determination of carboxylic acid metabolite of clopidogrel in human plasma and its application to a pharmacokinetic study

A new, simple, and reproducible method for determination of carboxylic acid metabolite of clopidogrel in human plasma has been developed. After liquid-liquid extraction in acidic medium with chloroform, samples were quantified on a Nova-pak C(8), 5 microm column using a mixture of 30 mM K(2)HPO(4)-THF-acetonitrile (pH = 3, 79:2:19, v/v/v) as mobile phase with UV detection at 220 nm. The flow rate was set at 0.9 mL/min. Ticlopidine was used as internal standard and the total run time of analysis was about 12 min. The method was linear over the range of 0.2-10 microg/mL of clopidogrel metabolite in plasma (r(2) > 0.999). The within-day and between-day precision values were in the range 1.0-4.8%. The limit of quantification of the method was 0.2 microg/mL. The method was successfully used to study the pharmacokinetics of clopidogrel in healthy volunteers.     

Silica-bonded N-propyl sulfamic acid as an efficient catalyst for the formylation and acetylation of alcohols and amines under heterogeneous conditions

A simple and efficient procedure for the preparation of silica-bonded N-propyl sulfamic acid (SBNPSA) by the reaction of 3-aminopropylsilica (1) and chlorosulfonic acid in chloroform is described. This solid acid is employed as a new catalyst for the formylation of alcohols and amines with ethyl formate under mild and heterogeneous conditions at room temperature with good to excellent yields. Also, SBNPSA catalyzed acetylation of various alcohols and amines with acetic anhydride at room temperature.     

Silica-bonded S-sulfonic acid a recyclable catalyst for the synthesis of coumarins

Silica-bonded S-sulfonic acid(SBSSA) was prepared by the reaction of 3-mercaptopropylsilica(MPS) and chlorosulfonic acid in chloroform.This solid acid has been employed as a recyclable catalyst for the synthesis of coumarins from phenols andβ-ketoesters at 80℃under solvent-free conditions.