ABSTRACT
Thermal lens detection with a 325.0nm He-Cd excitation laser is used for thermooptical indirect detection in combination with the capillary electrophoretic separation of organic anions. The optimization of indirect thermooptical detection is discussed. With Mordant Yellow 7 (an azo dye) chosen as a probe ion limits of detection for 1-heptane-, 1-pentane-, 1-butane-, 1-propanesulfonic, and acetic acid at a level of nx10(-7)M were achieved with a separation electrolyte containing 50muM of the probe ion and 5mM Tris pH 9.90. A further increase in the detection sensitivity (twofold decrease in the limit of detection ) was obtained with a separation electrolyte containing a volume fraction of 20% acetonitrile.
ABSTRACT
A mode-mismatched parallel dual-beam thermal lens spectrometer with a far-field single-channel detector system was used as a detector in HPLC. An expert estimation of the measurement results was applied to optimize the optical-scheme configuration of the spectrometer to achieve the longest linear calibration range and highest repeatability under chromatographic flow conditions. Chelates with 4-(2-pyridylazo)resorcinol were separated and determined with the limits of detection of n x 10(-8)- n x 10(-7) mol L(-1); the relative standard deviation of measurements was 46%. Xylenol Orange, 4-(2-thiazolylazo)resorcinol, and dithizone were studied as post-column reagents in thermal lens detection in ion chromatography. The limits of detection were n x 10(-8)- n x 10(-7) mol L(-1); the linear calibration ranges were about three orders; the relative standard deviation of measurements was 3-7%. A combined photothermal-refractometric detector for HPLC based on a polarization interferometer is proposed. Metal complexes as 4-(pyridylazo)resorcinol chelates (limits of detection of n x 10(-8)- n x 10(-7) mol L(-1)) and sugars (limits of detection of 10-20 ng L(-1)) were investigated as model substances. Obtained results were compared with results for traditional detectors, which show that photothermal detection has higher sensitivity than photometric and other absorption detectors.
ABSTRACT
Thermal lens spectrometry is used for studying adsorption equilibria in aqueous solutions at the level of nanogram quantities of iron(II) tris-(1,10-phenanthrolinate) as a model system. The kinetics of the sorption of the chelate on silica is studied and adsorption isotherms are built. Thermal lensing is used as a method for direct determination of the chelate concentration adsorbed on a quartz surface. The detected amount is 4.1x10(-15) mol at the area irradiated by the excitation beam. The adsorption of iron(II) tris-(1,10-phenanthrolinate) on laboratory glassware at the nanogram level is characterised by measuring the residual concentration of the sorbate in solution. A procedure for handling and cleaning the laboratory glassware for determining nanogram amounts of iron in aqueous solutions is proposed. The sensitivity of thermal lensing both in measuring adsorption on silica and glass and quartz surfaces is 100-fold higher than diffuse-reflectance measurements under the same conditions.
