手控注射式钛酸锶钡多孔球富集器分离富集-火焰原子吸收法测定水中铅和镉  

Determination of Lead and Cadmium in Water by Flame Atomic Absorption Spectrometry after Separation/Pre-concentration with Manual-Controlled Injection Porous Nano-Barium-Strontium Titanate Microspheres Separator

作　　者：张东[1] 李楠 高頔[1] 

机构地区：[1]沈阳理工大学环境与化学工程学院,沈阳110168 [2]辽宁省朝阳市环境监测站,朝阳122000

出　　处：《分析化学》2009年第8期1188-1192,共5页Chinese Journal of Analytical Chemistry

摘　　要：以D311树脂为模板,采用溶胶-凝胶法制备了纳米钛酸锶钡多孔球,用X射线衍射仪(XRD)、扫描电子显微镜(SEM)和傅立叶变换红外光谱仪(FTIR)进行了表征。考察了Pd2+和Cd2+的吸附和解脱条件。将微球装柱,制成注射式富集器,研究了此富集器对水中痕量Pd2+和Cd2+的富集性能。结果表明:此法合成的多孔球,由钙钛矿结构的纳米钛酸锶钡组成,晶体平均粒径为21nm,球体表面布满了不规则的纳米孔洞。当pH4～7时,此多孔球对水中的Pd2+和Cd2+具有很强的吸附能力,静态吸附容量分别为61.9和14.8mg/g。由多孔球装柱制成的手控注射式富集器,可成功实现对水中Pd2+和Cd2+的同时吸附。用2mol/LHNO3洗脱后,火焰原子吸收测定。建立了手控注射式纳米钛酸锶钡富集器分离富集、FAAS法测定水中痕量Pd2+和Cd2+的新方法。此方法对Pd2+和Cd2+的检出限分别为0.099和0.0034μg/L。用于水样中痕量Pd2+和Cd2+的富集和原子吸收测定,回收率分别为97.8%～106.5%和93.0%～100.7%。Using D311 resin as template, porous nano-bariumstrontium titanate microspheres（PBST） were prepared by the sol-gel method, and characterized by XRD, SEM and FTIR. Applied to the adsorption for lead and cadmium in water, the conditions of adsorption and elution were studied. Using micro-column packed with PBST, joining with injector, a new manual-controlled injection separator was prepared. The enrichment capability of the manual-controlled injection PBST separator for lead and cadmium was investigated. The results showed that the microspheres were porous, perovskite nano-barium-strontium titanate,and the average particle diameter of crystalloid was 21 nm. The lead ion and cadmium ion could be quantitatively retained at a pH value range from 4 to 7. The adsorption capacities of PBST for lead and cadmium were 61.9 mg/g and 14.8 mg/g, respectively. And 2 mol/L HNO3 was sufficient for complete elution. The manual-controlled injection PBST separator could be used to concentrate for lead and cadmium together. A new method for the determination of trace lead and cadmium in water based on manual-controlled injection separator preeoncentration and FAAS determination was established. The detection limits were 0. 099 μg/L for lead and 0. 0034 μg/L for cadmium. The method has been applied to the determination of trace lead ion and cadmium ion in water samples. The recoveries were 97.8% - 106.5% and 93.0% - 100.7% respectively.

关 键 词：纳米钛酸锶钡 多孔球 富集 铅 镉 火焰原子吸收光谱 

分 类 号：X832[环境科学与工程—环境工程]