Abstract: | The electroanalytical detection of trace mercury(II) at gold ultra‐microelectrode arrays is reported. The arrays consist of 256 gold microelectrodes of 5 μm in diameter in cubic arrangements which are separated from their nearest neighbor by 100 μm. The array was utilized in nitric acid using linear sweep voltammetry where a linear response from mercury additions over the range 10 μg L?1?200 μg L?1 (10?8?10?6 M) was observed with a sensitivity and detection limit of 0.11 nC/μg L?1 and 3.2 μg L?1 (16 nM) respectively from using a deposition time of 30 s at ?0.2 V (vs. SCE). This methodology was explored in 0.1 and 1 M chloride media over the mercury range 10 μg L?1?200 μg L?1 (5×10?8?10?6 M) where similar sensitivities of 0.087 nC/μg L?1 and 0.078 nC/μg L?1 were observed with an identical detection limit. The protocol is demonstrated to be useful for the determination of mercury for analysis of environmental water samples. |