Am. Bond et al., COMPARISON OF THE GOLD REDUCTION AND STRIPPING PROCESSES AT PLATINUM,RHODIUM, IRIDIUM, GOLD AND GLASSY-CARBON MICRO-DISK AND MACRODISK ELECTRODES, Analyst, 122(10), 1997, pp. 1147-1152
The gold Au-III + 3e(-) --> Au-0 reduction and Au-0 --> Au-III + 3e(-)
oxidation stripping processes in dilute aqua regia electrolyte (0.1 M
HCl + 0.32 M HNO3) were examined at platinum, rhodium, iridium, gold
and glassy carbon disk electrodes, After ascertaining that the preferr
ed material was platinum, the effect of electrode size was evaluated b
y using nine different platinum disk electrodes having diameters rangi
ng from 2 to 2000 mu m. The optimum analytical response was obtained w
ith a 50 mu m diameter platinum disk electrode, With this electrode di
ameter, a sharp symmetrical gold stripping peak was obtained and the d
eposition process occurred predominantly under conditions of radial di
ffusion so that stirring of the solution was not required. In contrast
, larger sized platinum electrodes produced a broader, asymmetric stri
pping response for the gold oxidation peak, whereas electrodes of smal
ler diameter provided poorer signal-to-noise ratios. The limit of dete
ction and limit of quantification were calculated to be 4.4 x 10(-7) M
(86 ppb) and 13.1 x 10(-7) M (258 ppb), respectively, at the 50 mu m
diameter platinum disk electrode under conditions of linear sweep stri
pping voltammetry at a scan rate of 200 mV s(-1) and a 140 s depositio
n time. The optimum electrode gave a very well defined gold oxidation
signal with negligible background current when applied to the determin
ation of gold in a gold ore sample.