アセトアミドオキシムによるニッケルイオンの吸光光度定量
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Acetoamidoxim (AAO) was synthesized from acetonitril and hydroxylamine hydrochloride. Spectrophotometric measurements showed that AAO reacted with nickel(II), iron(III), cobalt(II), chromium (III), copper (II), vanadium (V), manganese (I I), molybdenum (V), aluminum(III), zinc(II), cadmium (II), mercury(II) and lead(II) forming complexes in alkaline solution.<BR>Among these complexes, the AAO-Ni and AAO-Fe complexes had the maximum absorptions in the visible region, which the others had not. The wave lengths of maximum absorption of AAO-Ni and AAO-Fe were in the range of about 615625 nm and 557.5570 nm, and the molar extinction coefficients at the maximum absorption wave lengths were about 4.5 × 10<SUP>3</SUP><I>l</I>/mol·cm and 2.1 × 10<SUP>3</SUP> <I>l</I>/mol·cm, respectively.<BR>AAO-Ni was formed in the pH range of 6.758.8 and full colaration was attained about 5 min after 2 m<I>l</I> of 0.1 % water-methanol mixture was added to the aqueous solutions containing 026 ppm of nickel (II). The presence of ethanol had little effect on the absorption of AAO-Ni. The colaration was highly stable in the presence of air.<BR>Spectrophotometric determination of nickel(II) by using AAO was studied under various conditions. Beer's law was obeyed for 026 ppm of nickel (II), but iron(III), cobalt(II) and CN- ions interfered with the determination.<BR>Cobalt(II) could be removed by the addition of 3-methylglyoxime. Attempts to remove the interference of iron(II) by masking were unsuccessful. Iron (III) and CN- ions should be removed before the determination of nickel(II). When a large quantity of chromium(III) is present, sodium citrate was added to the solution in order to eliminate the interference. The continuous variation method showed that the com-position of AAO-Ni is f {[CH<SUB>3</SUB>(NH<SUB>2</SUB>)CHO]<SUB>3</SUB>Ni}<SUP>-</SUP>. This complex was insoluble in most organic solvents and could not be extracted from the aqueous solution.
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