A study on the simultaneous determination of Ni(II) and Co(II) dimethylglyoximates (Ni-DMG and Co-DMG) through adsorptive cathodic stripping voltammetry at an in situ bismuth-modified gold electrode (Bi-AuE) is reported. The key operational parameters, such as Bi(III) concentration, accumulation potential and accumulation time were optimized and the morphology of the Bi-microcrystals deposited on the Au-electrode was studied. The BiAuE allowed convenient analysis of trace concentrations of solely Ni(II) or of Ni(II) and Co(II) together, with cathodic stripping voltammograms characterized by well-separated stripping peaks. The calculated limit of detection (LOD) was 40 ng L À1 for Ni(II) alone, whereas the LOD was 98 ng L À1 for Ni(II) and 58 ng L À1 for Co(II), when both metal ions were measured together. The optimized method was finally applied to the analysis of certified spring water (NIST1640a) and of natural water sampled in the Lagoon of Venice. The results obtained with the BiAuE were in satisfactory agreement with the certified values and with those provided by complementary techniques, i.e., ICP-OES and ICP-MS.
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Macroporous bismuth film screen‐printed carbon electrode (mpBiF‐SPCE) was used for simultaneous measurement of Ni(II) and Co(II) at their trace concentration level by means of adsorptive cathodic stripping voltammetry with dimethylglyoxime as a complexing agent. The mpBiF‐SPCE was prepared on a screen printed carbon electrode by colloidal crystal templating using aqueous suspension of polystyrene microspheres which were self‐assembled onto the electrode by slow evaporation of solvent. Following the electrochemical deposition of bismuth film, the microspheres were dissolved with toluene providing the macroporous bismuth film structure. The mpBiF‐SPCE offered good electroanalytical performance with estimated limits of detection of 27 and 94 ng L−1 for Ni(II) and Co(II), respectively, in combination with an accumulation time of 180 s, and relative standard deviations of 3.3 % for Ni(II) and 5.2 % for Co(II). The effect of potentially interfering ions and the surface‐active compounds was also investigated. Both Ni(II) and Co(II) were assayed in the sample of sewer water with satisfactory recovery.
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