Development of a discrete flow system using a microsyringe as a cell for the photometric determination of iron

A simple discrete flow system for the photometric determination of iron using a glass syringe as a mixer of a solution and as a sample cell has been developed. The system was assembled from a coupler combining a light source (a light-emitting diode, LED), a glass syringe, a photodiode detector (PD) and two plastic core fiber optics. The reagent and sample solutions were sucked into a syringe, and were then mixed by a reciprocating motion of a plunger, or simply turning the syringe upside down several times, manually. After mixing, the absorbance of the solution was measured in situ. The analytical figures of this system and the mixing method were tested with a methyl orange solution and evaluated through iron(III) determination by a 1,10-phenanthroline method. The proposed system was applied to the determination of iron(III) using 1,10-phenanthroline and thiocyanate as chelating reagents and an off-line concentration method using an activated-carbon column. By this simple system, iron(III) in a river-water certified reference material (CRM), JSAC 0302-3, and river-water samples were successfully determined with a detection limit (3sigma) of 20 microg L(-1).