摘要
合成了新试剂5 碘[杯(4)芳烃偶氮]氨基喹啉(ICAQ),并研究了该试剂与钯显色反应条件。结果表明,在pH10.2~11.0的Na2CO3 NaHCO3缓冲介质中,在TritonX 100存在下,试剂与钯发生显色反应,生成1∶1稳定络合物。建立了测定钯的光度法新体系,λmax=625nm,ε=1.42×105L·mol-1·cm-1,钯质量浓度在0~0 80μg/mL内符合比尔定律。方法用于钯催化剂中钯的测定,结果与原子吸收法相符,平行6次测定的RSD在2.5%~3.0%。
The new agent of 5-iodo-[calix(4)arene]aminoquinoline(ICAQ) was sythesized. The conditions for color reaction of (ICAQ) with Pd(II) were studied. In the presence of Triton X-100, palladium(Ⅱ) reacted with ICAQ to form a stable complex with n_(ICAQ)∶n_(Pd(Ⅱ))=1∶1 at pH 10.2~11.0 (Na_2CO_3-NaHCO_3 buffer solution). Based on this, a spectrophotometric method for the determination of palladium(Ⅱ) was established. The maximum absorption was at 625 nm with molar absorptivity of 1.42×10~5 L·mol^(-1)·cm^(-1). Beer′s law was obeyed in the rang of 0~0.80 μg/mL for Pd(Ⅱ). The method was applied to the determination of Pd in palladium catalysts. The results were in agreement with those provided by AAS with precision of 2.5% to 3.0% RSD(n=6).
出处
《分析试验室》
CAS
CSCD
北大核心
2004年第6期45-47,共3页
Chinese Journal of Analysis Laboratory
基金
云南省教委自然科学基金资助项目(02ZY001)