Suvardhan K, Rekha D, Kumar K Suresh, Prasad P Reddy, Kumar J Dilip, Jayaraj B, Chiranjeevi P
Environmental Monitoring Laboratory, Department of Chemistry, SV University, AP, India.
J Hazard Mater. 2007 Jun 1;144(1-2):126-31. doi: 10.1016/j.jhazmat.2006.10.001. Epub 2006 Oct 10.
Cloud-point extraction was applied as a preconcentration of nickel after formation of complex with newly synthesized N-quino[8,7-b]azin-5-yl-2,3,5,6,8,9,11,12octahydrobenzo[b][1,4,7,10,13]pentaoxacyclopentadecin-15-yl-methanimine, and later determined by flame atomic absorption spectrometry (FAAS) using octyl phenoxy polyethoxy ethanol (Triton X-114) as surfactant. Nickel was complexed with N-quino[8,7-b]azin-5-yl-2,3,5,6,8,9,11,12octahydrobenzo[b][1,4,7,10,13]pentaoxacyclopentadecin-15-yl-methanimine in an aqueous phase and was kept for 15 min in a thermo-stated bath at 40 degrees C. Separation of the two phases was accomplished by centrifugation for 15 min at 4000 rpm. The chemical variables affecting the cloud-point extraction were evaluated, optimized and successfully applied to the nickel determination in various water samples. Under the optimized conditions, the preconcentration system of 100 ml sample permitted an enhancement factor of 50-fold. The detailed study of various interferences made the method more selective. The detection limits obtained under optimal condition was 0.042 ngml(-1). The extraction efficiency was investigated at different nickel concentrations (20-80 ngml(-1)) and good recoveries (99.05-99.93%) were obtained using present method. The proposed method has been applied successfully for the determination of nickel in various water samples and compared with reported method in terms of Student's t-test and variance ratio f-test which indicate the significance of present method over reported and spectrophotometric methods at 95% confidence level.
浊点萃取用于在新合成的N-喹啉并[8,7-b]嗪-5-基-2,3,5,6,8,9,11,12-八氢苯并[b][1,4,7,10,13]五氧杂环十五碳-15-基亚甲胺形成络合物后对镍进行预富集,随后通过火焰原子吸收光谱法(FAAS)使用辛基苯氧基聚乙氧基乙醇(吐温X-114)作为表面活性剂进行测定。镍在水相中与N-喹啉并[8,7-b]嗪-5-基-2,3,5,6,8,9,11,12-八氢苯并[b][1,4,7,10,13]五氧杂环十五碳-15-基亚甲胺形成络合物,并在40℃的恒温浴中保持15分钟。通过在4000转/分钟下离心15分钟实现两相分离。对影响浊点萃取的化学变量进行了评估、优化,并成功应用于各种水样中镍的测定。在优化条件下,100毫升样品的预富集系统的富集因子为50倍。对各种干扰的详细研究使该方法更具选择性。在最佳条件下获得的检测限为0.042纳克/毫升(-1)。在不同镍浓度(20 - 80纳克/毫升(-1))下研究了萃取效率,使用本方法获得了良好的回收率(99.05 - 99.93%)。所提出的方法已成功应用于各种水样中镍的测定,并与报道的方法进行了学生t检验和方差比f检验比较,结果表明在95%置信水平下本方法相对于报道方法和分光光度法具有显著性。