Single-run capillary electrophoretic determination of inorganic nitrogen species in rainwater.

A capillary electrophoretic (CE) method for the simultaneous determination of nitrate, nitrite, and ammonium ions has been developed. Direct (NO3-, NO2-) and indirect (NH4+) UV detection at 214 nm in conjunction with electromigration sampling from both ends of the capillary was used. The optimized separations were carried out in 10 mmol/L imidazole sulfate, 2 mmol/L 18-crown-6, and 0.02 mmol/L tetradecyltrimethylammonium hydroxide electrolyte (pH 4.0). The method permits excellent separation of three nitrogen species in only 4 min. A 1 x 10(-4) mol/L KBr solution was used as an internal standard to limit possible electrokinetic injection biases. Experimental results showed that the use of an anionic internal standard for cationic analytes and vice versa gives only slightly better precision than analysis with no internal standard. Using Br- internal standard for NO3- and NO2- ions and K+ for NH4+, peak area RSD values decrease significantly. The proposed system was applied to the speciation of inorganic nitrogen ions in rainwater samples. The recovery tests established for external calibration and standard addition techniques using one or two internal standards were within the range 100 +/- 10%. The CE results agree with those obtained by spectrophotometric methods.

Capillary electrophoretic determination of thiosulfate and its oxidation products.

Capillary electrophoresis (CE) was developed for the rapid and simple determination of thiosulfate and its oxidation products such as common polythionates, sulfite and sulfate. Direct and indirect UV detection techniques were investigated. The optimized separations of UV absorbing S2O3(2-), S4O6(2-), S5O6(2-) and S6O6(2-) anions were carried out in 5 mmol l(-1) (NH4)2SO4, 5 mmol l(-1) KH2PO4 electrolyte at pH 5.0, with direct UV detection at 214 nm. All analytes were well resolved in less than 4 min. Analysis of S2O3(2-), S4O6(2-), SO4(2-) and SO3(2-) ions can be performed in 5 mmol l(-1) H2CrO4, 1 mmol l(-1) hexamethonium hydroxide electrolyte neutralized with triethanolamine to pH 8.0, using indirect UV detection at 254 nm. However, the detection sensitivity for tetrathionate was poor. Other polythionates can not be detected at all because of their high absorbance even at 254 nm. The developed CE method was applied for the monitoring of sulfur species in spent fixing solutions during the electrolytic oxidation.

Rapid analysis of cation constituents of urine by capillary electrophoresis.

Capillary electrophoresis was applied for the simultaneous determination of K(+), NH(4)(+), Na(+), Ca(2+) and Mg(2+) cations in urine. The separations were carried out in electrolyte containing 7. 5 mmol/l copper(II) acetate, 15 mmol/l ethylenediamine and 2 mmol/l triethanolamine at pH 8.0, with indirect UV detection at 230 nm. All cations were well separated in less than 4 min. The results obtained by this method were comparable with ion chromatography. The proposed system is simple, rapid and does not require any preliminary treatment of the urine samples except diluting.

On-line preconcentration and determination of chromium(VI) in waters by high-performance liquid chromatography using precolumn complexation with 1,5-diphenylcarbazide.

A method for on-line chromatographic preconcentration and determination of chromium(VI) traces has been developed. Chromate was preconcentrated on a C18 column (50 x 6 mm I.D.) after complexation with diphenylcarbazide (DPC). Following the preconcentration step, analysis of the sample was performed using a C18 column (100 x 6 mm I.D.) with an eluent containing 6.10(-3) mol/l sulphuric acid and 20% (v/v) acetonitrile. Direct spectrophotometric detection at 546 nm was used. Experimental parameters such as mobile phase pH, DPC concentration, preconcentration flow-rate, sample volume were optimized for preconcentration and detection of Cr(VI)-DPC complex. Under the optimum conditions, most metal ions [Cr(III), Fe(III), Cu(II), Hg(II), Mo(VI), V(V)] and inorganic anions did not interfere. A detection limit of 0.02 ng/ml Cr(VI) can be attained when a sample volume of 100 ml is used. The technique has been applied successfully to the determination of Cr(VI) traces in drinking, surface and groundwater samples and the recoveries of added chromium were in the range 94-104%.

Simultaneous determination of inorganic anions and cations in waters by capillary electrophoresis.

The applicability of a recently proposed capillary electrophoresis technique based on the electromigrative sample introduction from both ends of the capillary was further investigated for the simultaneous determination of inorganic anions and cations in real water samples. The optimized separations were carried out in 5.0 mmol l-1 copper(II)-ethylenediaminehydroxide and 2.0 mmol l-1 triethanolamine electrolyte neutralized with chromic acid to pH 8.0, using indirect UV detection at 254 nm. Nine inorganic ions (Cl-, NO3-, SO4(2-), HCO3-, K+, NH4+, Na+, Ca2+ and Mg2+) were well separated in less than 5 min. The analytical performance of the method is discussed in terms of migration time, peak area and corrected peak area repeatability, linearity of response and detection limits. To evaluate this system, the determination of anions and cations was examined for mineral water, tap water and river water samples using Li+ as the internal standard. The comparison of the results with ion chromatography and conventional capillary electrophoresis is presented.