Venkateswarlu G, Sahayam A C, Chaurasia S C, Mukherjee T
National Centre for Compositional Characterisation of Materials, B.A.R.C., E.C.I.L. (P.O.), Hyderabad, India.
Talanta. 2006 Jan 15;68(3):748-52. doi: 10.1016/j.talanta.2005.05.022. Epub 2005 Jul 5.
A method has been developed for the separation and determination of a set of 11 impurities from chromium matrices using oxalate form of Amberlite IRA 93. Due to slower kinetics of formation of the anionic complex, Cr(III) passed in the effluent while impurities forming strong complexes rapidly are retained on the exchanger. The adsorption of impurities of interest is found to be uniform in pH range 2-6. The adsorbed impurities are eluted with 2 mol l(-1) HNO(3) and determined by inductively coupled plasma-optical emission spectrometer (ICP-OES). The percentage recoveries of Al, Bi, Cd, Co, Cu, Fe, Mn, Ni, Pb, Ga and Zn are in the range 88-101% and separation of matrix is >99.9%. The method has been applied for the analysis of two samples namely CrCl(3).6H(2)O and Cr. The R.S.D. of the method is 5-6% at >10 microg g(-1) level and approximately 15% at <1 microg g(-1) level. The process blank values are in the range sub-microg g(-1) and detection limits are in ng g(-1) range.
已开发出一种方法，用于使用Amberlite IRA 93草酸盐形式从铬基质中分离和测定一组11种杂质。由于阴离子络合物形成的动力学较慢，Cr(III)进入流出物中，而迅速形成强络合物的杂质则保留在交换剂上。发现感兴趣的杂质在pH值2 - 6范围内的吸附是均匀的。吸附的杂质用2 mol l(-1) HNO(3)洗脱，并用电感耦合等离子体发射光谱仪(ICP - OES)测定。Al、Bi、Cd、Co、Cu、Fe、Mn、Ni、Pb、Ga和Zn的回收率在88 - 101%范围内，基质的分离率>99.9%。该方法已应用于两个样品即CrCl(3).6H(2)O和Cr的分析。该方法在>10 microg g(-1)水平时的相对标准偏差为5 - 6%，在<1 microg g(-1)水平时约为15%。方法空白值在亚微克g(-1)范围内，检测限在纳克g(-1)范围内。
