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Abstract
A determination method for palladium (Pd) ion in river water has been developed by reversed phase HPLC. The Pd(II) ion was quantitatively extracted into benzene from an acidic solution as 5-methyl-1, 3, 4-thiodiazole-2-thiol (MTT) chelate. The extracted Pd-MTT chelate was then separated on a phenyl ethyl column with an eluent of methanol/water/0.01 mol/L MTT (90:10:0.5, v/v) and detected at 270 nm. The correlation coefficients of the calibration curves obtained with 5 mL Pd standards were more than 0.999 over the range of 10 ng/mL (ppb) to 50 µg/mL (ppm). The detection limit of the Pd ion in 5 mL of water was estimated as 10 ppb by a signal to noise ratio of 3. Relative standard deviations of peak areas (N = 6) for 5, 0.5, and 0.05 ppm Pd standards were 1.5, 1.3, and 0.9%, respectively. The recoveries with a spiked river water sample for 5, 0.5, and 0.05 ppm Pd ion (N = 6) were 99.9 ± 1.0%, 99.5 ± 0.8%, and 94.0 ± 1.1%. Effects of foreign ions on the determination of 0.2 ppm Pd were investigated with 57 metal ions. Almost none of the ions interfered except for Cu(II), Ag(I), Ni(II), Cd(II), Co(II), and Ti(IV) ions.
Notes
a Standard deviation.
b Relative standard deviation.
The relative standard deviations of peak areas for 5, 0.5, and 0.05 ppm Pd standards obtained on other days were less than 2%.
Note: The tolerance limit value of the foreign ion concentration was taken as the value that caused an error of less than 10% in the recovery of Pd(II) ion (0.2 ppm).
When calibration curves were prepared with 4 mL of river water and Pd standards, the recoveries of 0.05 ppm Pd were 100.5 ± 2.1%, and 99.7 ± 1.7% (obtained on other days).