电感耦合等离子体原子发射光谱法测定载钯树脂中钯的前处理方法考察

采用电感耦合等离子体原子发射光谱法(ICP-AES)测定载钯树脂中的钯,对比了灰化法、硝酸-高氯酸法和微波消解法3种前处理方法,考察了称样量、消解加酸量、处理时间和灰化温度等对测定的影响,优化了最佳试验条件,讨论了共存离子的干扰.结果表明,钯质量浓度在0~50 mg/L范围内与强度线性关系良好,线性相关系数为0.999 5,灰化法、硝酸-高氯酸法和微波消解法3种方法的检出限分别为0.002 8、0.005 4、0.002 3 mg/L,相对标准偏差(n=11)分别0.69%、0.63%、0.42%,加标回收率分别为98%~100%、98%~101%、100%~104%.采用3种方法对实际样品进行测定,发现微波消解法处理时间最短,样品处理最完全,检测值最平行.用试验方法与原子吸收光谱法测定同一个载钯树脂,两者测定结果基本相符.

Pretreatment Method Inspection of Palladium Loaded Resins in Determination of Palladium by Inductively Coupled Plasma Atomic Emission Spectrometry

Palladium in palladium loaded resin was determined by inductively coupled plasma atomic emission spectrometry (ICP-AES) after the palladium loaded resins were pretreated by the ashing method, nitric acid-perchloric acid method or microwave digestion method. Three pretreatment methods were compared. The effect of sample weighing, acid amount, handling time and ashing temperature were investigated to obtain optimal experimental conditions. The interference of coexisting ions was discussed. It was found that palladium concentration in the range of 0~50 mg/L exhibited a good linearity to intensity. The linear correlation coefficient was 0.999 5. Detection limits of these three method were 0.002 8 mg/L, 0.005 4 mg/L and 0.002 3 mg/L, respectively. The relative standard deviation (RSD, n=11) were 0.69%, 0.63% and 0.42%, respectively. The recoveries were 98%~100%, 98%~101% and 100%~104%, respectively. The three methods were applied to the determination of real samples. It is found that when using the microwave digestion method the treatment time is the shortest, the sample processing is most complete and the determined values was most parallel. When both the experimental method and the atomic absorption spectrometry were applied to the same palladium loaded resin the results basically accordant with eachother.