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采用新型二苯碳酰二肼修饰的介孔硅分离富集同时测定环境样品中痕量 Cd(II)和 Cu(II)。

Simultaneous separation and determination of trace amounts of Cd(II) and Cu(II) in environmental samples using novel diphenylcarbazide modified nanoporous silica.

机构信息

Department of Chemistry, Shahid Beheshti University, G.C., Tehran 1983963113, Iran. b

出版信息

Talanta. 2012 Jan 30;89:455-61. doi: 10.1016/j.talanta.2011.12.062. Epub 2011 Dec 28.

Abstract

A novel sorbent for simultaneous separation of cadmium and copper was prepared by functionalizing SBA-15 nanoporous silica with diphenylcarbazide. A solid-phase extraction method using the above sorbent has been developed to separate and concentrate trace amount of cadmium and copper ions from environmental samples by flame atomic absorption spectrophotometry measurements. The optimum experimental conditions such as pH, flow rates, type and the smallest amount of eluent for elution of cadmium and copper ions, break through volume and effect of coexisting ions on the separation and determination of cadmium and copper ions were evaluated. The extraction efficiency for cadmium and copper ions were greater than 98% and limit of detection (LOD) was 0.15 and 0.45 ng mL(-1) for cadmium and copper, respectively. The preconcentration factor was 294 and 291 for cadmium and copper, respectively, and the relative standard deviation (RSD) of the method was <4% for 10 separate column experiments for the determination of 5.0 μg cadmium and copper ions. The adsorption capacity of the nanoporous silica was 198 mg g(-1) for cadmium and 105 mg g(-1) for copper on functionalized SBA-15 nanoporous silica. Validation of the outlined method was performed by analyzing certified reference materials (Soil (NCS DC 73323) and ore polymetallic gold Zidarovo-PMZrZ (206 BG 326)). The practical applicability of the developed sorbent was examined using real samples such as sea water, fish and sediment samples.

摘要

一种新型的用于同时分离镉和铜的吸附剂是通过在 SBA-15 介孔硅上功能化二苯卡巴肼制备的。通过火焰原子吸收分光光度法测量,已经开发了一种使用上述吸附剂的固相萃取方法,用于从环境样品中分离和浓缩痕量的镉和铜离子。评价了最佳实验条件,如 pH 值、流速、洗脱镉和铜离子的洗脱液类型和最小量、穿透体积以及共存离子对镉和铜离子分离和测定的影响。镉和铜离子的萃取效率均大于 98%,镉和铜的检出限(LOD)分别为 0.15 和 0.45ng/mL。镉和铜的预浓集因子分别为 294 和 291,对于 5.0μg 镉和铜离子的 10 次单独柱实验,方法的相对标准偏差(RSD)均小于 4%。在功能化 SBA-15 介孔硅上,纳米孔硅对镉的吸附容量为 198mg/g,对铜的吸附容量为 105mg/g。通过分析认证参考物质(土壤(NCS DC 73323)和矿石多金属金 Zidarovo-PMZrZ(206 BG 326))验证了所提出方法的验证。通过使用海水、鱼类和沉积物等实际样品检验了开发的吸附剂的实际适用性。

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