Differential pulse anodic stripping voltammetric determination of traces of copper with a tobramycin-Nafion modified electrode.
A Nafion-modified glassy carbon electrode incorporated with tobramycin for the voltammetric stripping determination of Cu2+ has been explored. The electrode was fabricated by tobramycin containing Nafion on the glassy carbon electrode surface. The modified electrode exhibited a significantly increased sensitivity and selectivity for Cu2+ compared with a bare glassy carbon electrode and the Nafion modified electrode. Cu2+ was accumulated in HAc-NaAc buffer (pH 4.6) at a potential of -0.6 V (vs. SCE) for 300 s and then determined by differential pulse anodic stripping voltammetry. The effects of various parameters, such as the mass of Nafion, the concentration of tobramycin, the pH of the medium, the accumulation potential, the accumulation time and the scan rate, were investigated. Under the optimum conditions, a linear calibration graph was obtained in the concentration range of 1.0 x 10(-9) to 5.0 x 10(-7) mol l(-1) with a correlation coefficient of 0.9971. The relative standard deviations for eight successive determinations were 4.3 and 2.9% for 1.0 x 10(-8) and 2.0 x 10(-7) mol l(-1) Cu2+, respectively. The detection limit (three times signal to noise) was 5.0 x 10(-10) mol l(-1). A study of interfering substances was also performed, and the method was applied to the direct determination of copper in water samples, and also in analytical reagent-grade salts with satisfactory results.
Electrochemical detection of copper(II) at a gold electrode modified with a self-assembled monolayer of penicillamine
A penicillamine (PCA) self-assembled monolayer (SAM) was prepared on a gold electrode. It has been found that the modified electrode exhibited a selective response to copper ions. As demonstrated by cyclic voltammetric experiments, the SAM-based electrode showed an attractive ability to preconcentrate efficiently traces of copper(II) from solutions. Under optimum conditions, the anodic peak current was proportional to the concentration of Cu(II) in the range from 8.0 × 10−7 to 1.0 × 10−4 M with a detection limit of 4.0 × 10−7 M. Moreover, this modified gold electrode is also characterized by excellent repeatability, showing a relative standard deviation of 3.2% for nine successive measurements of 1.0 × 10−5 M Cu(II). The PCA/Au SAM gold electrode was used for the determination of Cu(II) in a tap water sample and the results showed a good agreement with the data obtained by atomic emission spectrometry.
Submicron polymer structures with X-ray lithography and hot embossing
This article describes the process chain for replication of submicron structures with varying aspect ratios (AR) up to 6 in polymethylmethacrylate (PMMA) by hot embossing to show the capability of the entire LIGA process to fabricate structures with these dimensions. Therefore a 4.7 μm thick layer of MicroChem 950k PMMA A11 resist was spin-coated on a 2.3 μm Ti/TiOx membrane. It was patterned with X-ray lithography at the electron storage ring ANKA (2.5 GeV and λc ≈ 0.4 nm) at a dose of 4 kJ/cm3 using a Si3N4 membrane mask with 2 μm thick gold-absorbers. The samples were developed in GG/BDG and resulted in AR of 6–14. Subsequent nickel plating at 52°C resulted in a 200 μm thick nickel tool of 100 mm diameter, which was used to replicate slit-nozzles and columns in PMMA. Closely packed submicron cavities with AR 6 in the nickel shim were filled to 60% during hot embossing.