Determination of trace amounts of bromide by flow injection/stopped-flow detection technique using kinetic-spectrophotometric method

A simple, sensitive and selective method for the determination of bromide in seawater by using a flow injection/stopped-flow detection technique was examined. The detection system was developed for a new kinetic-spectrophotometric determination of bromide in the presence of chloride matrix without any extraction and/or separation. The detection was based on the kinetic effect of bromide on the oxidation of methylene blue (MB) with hydrogen peroxide in a strongly acidic solution. Large amounts of chloride could enhance the sensitivity of the method as an activator. The decolorisation of the blue color of MB was used for the spectrophotometric determination of bromide at 746 nm. A stopped-flow approach was used to improve the sensitivity of the measurement and provide good linearity of the calibration over the range of 0-3.2 p,g ml(-1) of bromide. The relative standard deviation was 0.74% for the determination of 2.4 jig ml(-1) bromide (n=5). The detection limit (3 sigma) was 0.1 mu g ml(-1) with a sampling frequency of 12 h(-1). The influence of potential interfering ions was studied. The proposed method was applied to the determination of bromide in seawater samples and provided satisfactory results. </p

A membraneless gas diffusion unit: Design and its application to determination of ethanol in liquors by spectrophotometric flow injection

This work presents new design of a gas diffusion unit, called 'membraneless gas diffusion (MGD) unit', which, unlike a conventional gas diffusion (GD) unit, allows selective detection of volatile compounds to be made without the need of a hydrophobic membrane. A flow injection method was developed employing the MGD unit to determine ethanol in alcoholic drinks based on the reduction of dichromate by ethanol vapor. Results clearly demonstrated that the MGD unit was suitable for determination of ethanol in beer, wine and distilled liquors. Detection limit (3S/N) of MGD unit was lower than the GD unit (GD: 0.68%, v/v; MGD: 0.27%, v/v). The MGD design makes the system more sensitive as mass transfer is more efficient than that of GD and thus, MGD can perfectly replace membrane-based designs

Enantiomeric separation of some common controlled stimulants by capillary electrophoresis with contactless conductivity detection

CE methods with capacitively coupled contactless conductivity detection (C4D) were developed for the enantiomeric separation of the following stimulants: amphetamine (AP), methamphetamine (MA), ephedrine (EP), pseudoephedrine (PE), norephedrine (NE) and norpseudoephedrine (NPE). Acetic acid (pH 2.5 and 2.8) was found to be the optimal background electrolyte for the CE-C4D system. The chiral selectors, carboxymethyl-beta-cyclodextrin (CMBCD), heptakis(2,6-di-O-methyl)-beta-cyclodextrin (DMBCD) and chiral crown ether (+)-(18-crown-6)-2,3,11,12-tetracarboxylic acid (18C6H4), were investigated for their enantioseparation properties in the BGE. The use of either a single or a combination of two chiral selectors was chosen to obtain optimal condition of enantiomeric selectivity. Enantiomeric separation of AP and MA was achieved using the single chiral selector CMBCD and (hydroxypropyl)methyl cellulose (HPMC) as the modifier. A combination of the two chiral selectors, CMBCD and DMBCD and HPMC as the modifier, was required for enantiomeric separation of EP and PE. In addition, a combination of DMBCD and 18C6H4 was successfully applied for the enantiomeric separation of NE and NPE. The detection limits of the enantiomers were found to be in the range of 2.35.7 mu mol/L. Good precisions of migration time and peak area were obtained. The developed CE-C4D method was successfully applied to urine samples of athletes for the identification of enantiomers of the detected stimulants