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制备了附载有五硫代-15-冠-5(PT15C5)的反相微孔树脂固相萃取柱,并研究了其对钯的固相萃取,含钯样品以0.1mol/L的盐酸介质过柱,样品溶液中的钯可定量吸附在小柱上,富集完后用0.5mol/L的硫脲洗脱小柱上富集的钯,可实现钯的高倍数富集和干扰离子的分离。洗脱液中的钯可用火焰原子吸收光谱法测定,钯浓度在0.1—3.0μg/mL内与吸光度成良好的线性关系;方法用于环境水样中钯的实际测定,相对标准偏差在3.2%—4.1%之间,加标回收率在87.8%—104.7%之间,结果令人满意。
A reversed-phase microporous resin SPE column with pentathio-15-crown-5 (PT15C5) was prepared and its solid-phase extraction on palladium was studied. The palladium-containing sample was treated with 0.1mol / L hydrochloric acid Column, the sample solution of palladium can be quantitatively adsorbed on a small column, after enrichment with 0.5mol / L of thiourea to elute the small column of palladium, palladium can achieve high-fold enrichment and interference ion separation . The palladium in the eluent was determined by flame atomic absorption spectrometry. The concentration of palladium in the range of 0.1-3.0μg / mL was in good linear relationship with the absorbance. The method was applied to the determination of palladium in environmental water samples with the relative standard deviation of 3.2% -4.1%. The recoveries of spiked samples ranged from 87.8% to 104.7% with satisfactory results.