Soylak Mustafa, Yilmaz Erkan, Ghaedi Mehrorang, Montazerozohori Mortaza, Sheibani Marjan
University of Erciyes, Chemistry Department, 38039 Kayseri, Turkey.
J AOAC Int. 2012 Nov-Dec;95(6):1797-802. doi: 10.5740/jaoacint.10-370.
A cloud point extraction procedure for the preconcentration of Pb2+ in various samples following complexation with 2,2'-(1E,1'E)-1,1'-(2,2'-azanediylbis(ethane-2,1-diyl)bis(azan-1-yl-1-ylidene)) bis(ethan-1-yl-1-ylidene)diphenol in Triton X-114 after centrifugation is reported. A 0.5 mL portion of methanol acidified with 1.0 M HNO3 was added to the surfactant-rich phase prior to analysis by flame atomic absorption spectrometry. The influence of analytical parameters--including pH, concentrations of ligand, Triton X-114, and HNO3, bath temperature, heating time, and centrifugation rate and time--were optimized, and the effect of the matrix ions on the recovery of Pb2+ was investigated. An LOD of 1.9 ng/mL along with a preconcentration factor of 50 with RSD of 1.0% for Pb2+ were achieved. The proposed procedure was applied to the analysis of various real samples.
报道了一种浊点萃取方法，用于在离心后，使各种样品中的Pb2+与2,2'-(1E,1'E)-1,1'-(2,2'-氮杂二基双(乙烷-2,1-二基)双(氮杂-1-基-1-亚基))双(乙烷-1-基-1-亚基)二酚在Triton X-114中络合后进行预富集。在通过火焰原子吸收光谱法分析之前，向富含表面活性剂的相中加入0.5 mL用1.0 M HNO3酸化的甲醇。优化了包括pH、配体浓度、Triton X-114浓度、HNO3浓度、浴温、加热时间以及离心速率和时间在内的分析参数，并研究了基体离子对Pb2+回收率的影响。实现了Pb2+的1.9 ng/mL的检出限以及50的预富集因子，相对标准偏差为1.0%。所提出的方法应用于各种实际样品的分析。
