A novel azocalix[4]arene, 5,17-bis (quinolyl-8-azo)-25,26,27,28 -tetrahydro
xycalix [4] arene 1, was prepared by linking 8-aminoquinoline to calix[4]ar
ene through a diazo-coupling reaction. Based on it, a simple, sensitive and
selective spectrophotometric method was developed for the determination of
Ni2+. In basic media, Ni2+ formed a 1:1 complex with 1. Beer's law was obe
yed in the range 1.7 x 10(-7)-5.1 x 10(-6) mol l(-1) of Ni2+. The apparent
molar absorptivity (epsilon) of 1-Ni2+ complex was 1.28 x 10(5) 1mol(-1) cm
(-1) at 580 nm, and the detection limit was 1.4 x 10(-7) mol l(-1) (S/N = 3
). The relative standard deviation for measurement of 8.5 x 10(-7) mol l(-1
) Ni2+ was 2.7% (n = 10). The proposed method was applied to the determinat
ion of trace amount of Ni2+ in certified samples with satisfactory results.
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