电感耦合等离子体原子发射光谱法测定钯炭中钯

将样品置于马弗炉中,从室温升温至700 ℃后灼烧30 min分解活性炭,残渣用1 mL水合肼还原后、使用15 mL盐酸和5 mL硝酸溶解,待测溶液加入钇做内标,选择Pd 340.458 nm作为分析线,优化仪器测定条件,建立了电感耦合等离子体原子发射光谱法(ICP-AES)测定钯炭中钯的方法。结果表明,钯炭样品中微量共存元素对钯测定无影响。钯的质量浓度在50.00~300.00 mg/L范围内与其发射强度呈线性,相关系数r=0.999 99,方法中钯的检出限为0.015 mg/L。使用方法测定钯炭样品中钯,结果的相对标准偏差(RSD,n =11)小于1%。测定结果与丁二肟析出-EDTA络合滴定法测定结果相吻合。

Determination of palladium in palladium-carbon by inductively coupled plasma atomic emission spectrometry

The sample was put in muffle furnace. After increasing the temperature to 700 ℃, the sample was burned for 30 min to decompose the activated carbon. The residue was reduced with 1 mL of hydrazine hydrate followed by dissolution with 15 mL of hydrochloric acid and 5 mL of nitric acid. Yttrium was added into testing solution as internal standard. Pd 340.458 nm was selected as the analytical line. The instrumental conditions were optimized. The determination method of palladium in palladium-carbon by inductively coupled plasma atomic emission spectrometry (ICP-AES) was established. The results showed that the trace coexisting elements in palladium-carbon sample had no influence on the determination of palladium. The mass concentration of palladium in range of 50.00-300.00 mg/L was linear to the emission intensity with correlation coefficient of r=0.999 99. The detection limit of palladium in this method was 0.015 mg/L. The proposed method was applied to the determination of palladium in palladium-carbon sample. The relative standard deviations (RSD, n=11) were less than 1%. The found results were consistent with those obtained by dimethylglyoxime precipitation - EDTA complexometric titration method.