An ultrasensitive electrochemical
microelectrode set (μ-ES),
where all three electrodes are made of highly densified carbon nanotube
fiber (HD-CNTf) cross sections (length ∼40 μm), embedded
in an inert polymer matrix, and exposed open-ended CNTs at the interface,
is presented here. Bare open ends of HD-CNTf rods were used as the
working (∼40 μm diameter) and counter (∼94 μm
diameter) electrodes, while the cross section of a ∼94 μm
diameter was electroplated with Ag/AgCl and coated with Nafion to
employ as a quasi-reference electrode. The Ag/AgCl/Nafion-coated HD-CNTf
rod quasi-reference electrode provided a very stable potential comparable
to the commercial porous-junction Ag/AgCl reference electrode. The
HD-CNTf rod μ-ES has been evaluated by electrochemical determination
of biologically important analytes, i.e., dopamine (DA), β-nicotinamide
adenine dinucleotide (NADH), a diuretic drug, i.e., furosemide, and
a heavy metal, i.e., lead ions (Pb2+). Different voltammetric
techniques were employed during the study, i.e., cyclic voltammetry
(CV), square wave voltammetry (SWV), amperometry, and square wave
anodic stripping voltammetry (SWASV). The direct metallic connection
to CNTs gives access to the exceptional properties of highly ordered
open-ended CNTs as electrochemical sensors. The distinct structural
and electronic properties of aligned HD-CNTf rods in the μ-ES
demonstrate fast electron transfer kinetics and offer excellent detection
performance during testing for different analytes with wide linear
ranges, excellent sensitivity, and very low limits of detection.