Determination of the boiling point distribution of sulfur compounds in light cycle oil using GC with a flame photometric detector and pyrolyzer

A method has been developed to determine the boiling point distribution of sulfur compounds in light cycle oils (LCO'S). The method chosen for this analysis was GC with a flame photometric detector (FPD) and pyrolyzer. Tests were carried out to evaluate the recovery efficiency, repeatability, and accuracy of the method. Repeatabilities within 2% were obtained. The recovery of benzothiophenes and dibenzothiophenes was close to 100%; this was important because these are the major sulfur components in LCO's. No hydrocarbon or solvent interferences were observed with the use of the pyrolyzer, even for a 95% solvent level. Comparison with results from other techniques showed that the method accurately determined the levels of sulfur compounds in the LCO boiling point range.     

Resolution of binary mixtures of cephalothin and clavulanic acid by using first derivative spectrophotometry

First-derivative spectrophotometric method with a “zero-crossing” technique of measurement has been used for the quantification of two-components mixtures of cephalothin and clavulanic acid. As the absorption bands of these drugs overlap, both direct and derivative spectrophotometric methods have been investigated and evaluated by a rigorous statistical analysis of the experimental data. The first-derivative spectrophotometric method was found to be more accurate, direct and reproducible. Beer's law was valid over the concentration range 2.0–28.0 mg/l for both compounds. The detection limits of cephalothin and clavulanic acid, at a 0.05 level of significance, were calculated to be 0.13 and 0.15 mg/l. The method was applied for determining these antibiotics in mixtures, some of them containing inject-able dosage forms of cephalothin, and so to determine both compounds in saline and glucosed physiological sera.