Jamali Mohammad Reza, Assadi Yaghoub, Shemirani Farzaneh, Salavati-Niasari Masoud
School of Chemistry, University College of Science, University of Tehran, Tehran, Iran.
Talanta. 2007 Mar 15;71(4):1524-9. doi: 10.1016/j.talanta.2006.07.034. Epub 2006 Aug 22.
A new and efficient method was described for an easy synthesis of functionalized mesoporous silica (MCM-41) using thiophene-2-carbaldehyde. This new chemically bonded analytical reagent was used as an effective sorbent for the solid phase extraction of palladium(II) ion from aqueous solutions. Conditions for effective adsorption of trace levels of palladium concentration were optimized with respect to different experimental parameters in batch process. Thiourea solution could efficiently elute adsorbed palladium(II) ion from the surface of the sorbent which then was determined by inductively coupled plasma atomic emission spectrometer (ICP-AES). Common coexisting ions did not interfere with the separation and determination. The preconcentration factor was 100 (1ml elution volume) for a 100ml sample volume. The limit of detection of the proposed method is 0.2ngml(-1). The maximum sorption capacity of sorbent under optimum conditions has been found to be 5mg of palladium per gram of sorbent. The relative standard deviation under optimum conditions was 3.2% (n=10). Accuracy and application of the method was estimated by using test samples of natural and synthetic water spiked with different amounts of palladium(II) ion.
描述了一种使用噻吩 - 2 - 甲醛简便合成功能化介孔二氧化硅(MCM - 41)的新型高效方法。这种新型化学键合分析试剂被用作从水溶液中固相萃取钯(II)离子的有效吸附剂。在分批过程中,针对不同实验参数对痕量钯浓度的有效吸附条件进行了优化。硫脲溶液可有效地从吸附剂表面洗脱吸附的钯(II)离子,然后通过电感耦合等离子体原子发射光谱仪(ICP - AES)进行测定。常见共存离子不干扰分离和测定。对于100ml样品体积,预富集因子为100(洗脱体积为1ml)。该方法的检测限为0.2ngml⁻¹。已发现吸附剂在最佳条件下的最大吸附容量为每克吸附剂5mg钯。最佳条件下的相对标准偏差为3.2%(n = 10)。通过使用添加不同量钯(II)离子的天然水和合成水测试样品评估了该方法的准确性和应用。