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极谱测定微量钯见报道。我们用α-呋嘀甲酰二肟-NH_3·H_2O-NH_4Cl体系测微量钯,并研究极谱波性质,认为是络合吸附波。但用微分脉冲极谱测定,需扣除空白和除氧。使方法简便,用单扫描示波极谱对该体系作试验,钯在-0.70伏(对饱和甘汞电极)有一导数极谱波,测定下限为0.03μg·ml~(-1)。为改进灵敏度,体系中加氯化十四烷基苄基二甲基铵、溴化十六烷基三甲基铵(CTMAB)、溴化十六烷基吡啶、氯化四甲基铵、聚乙烯醇、十二烷基磺酸钠等表面活性剂,结果CTMAB效果最佳。适量加入可增加峰电流30～40%,测定低至0.005μg·ml~(-1)的钯,波形稳定,不必扣空白和除氧。底液中加酒石酸钾钠使大多数干扰离子允许共存量显著增加。方法可测钯氧化铝催化剂中钯含量,回收率达92～108%。
Polarographic determination of trace palladium reported. We measured the trace palladium with α-fumaryl dioxime -NH_3 · H_2O-NH_4Cl system and studied the polarographic wave properties, which is considered to be a complex adsorption wave. However, with differential pulse polarography, to be deducted blank and oxygen. The method was simple and simple. The system was tested by single-sweep oscillopolarography. The derivative of Pd was -0.70V (for saturated calomel electrode) and the lower limit of determination was 0.03μg · ml ~ (-1). In order to improve the sensitivity, tetradecylbenzyldimethylammonium chloride, cetyltrimethylammonium bromide (CTMAB), cetylpyridinium bromide, tetramethylammonium chloride, poly Vinyl alcohol, sodium dodecyl sulfate and other surfactants, the results CTMAB best. The amount of added can increase the peak current 30 ~ 40%, measured as low as 0.005μg · ml ~ (-1) of palladium, stable waveform, without deduction blank and deoxygenation. Potassium sodium tartrate in the base fluid allows most interfering ions to allow a significant increase in coexistence. The method can be used to measure the content of palladium in palladium-aluminum oxide catalyst, and the recovery rate reaches 92-108%.