悬浮体制样氟化辅助ETV-ICP-AES直接测定中药绞股蓝中微量元素

报道了以聚四氟乙烯悬浮体（PTFE）为化学改进剂,采用电热蒸发电感耦合等离子体原子发射光谱法（ETV－ICP－AES）直接分析中药绞股蓝中微量元素Cu、Mn、Cr、Fe、Zn。考察了影响分析信号的主要因素。本法用于实际样品分析,结果满意。     

Synthesis of lanthanum oxide nanosheets by a green carbonation process

Two-dimensional metal oxide nanostructures, such as nanoplates, nanowalls, and nanosheets, have received further attentions in recent years, due to their outstanding properties resulted from the small thickness and quantum size effects. In this work, lanthanum oxide nanosheets with the thickness of 56 nm had been suc-cessfully prepared by an originally simple method of car- bon dioxide carbonation; the preparation process was green without using surfactants and detergent. The X-ray dif-fraction, transmission electron microscopy, and scanning electron microscopy were used to characterize the pro-ducts. Thermogravimetric-differential thermal analysis and FT-IR were introduced to prove that the lanthanum oxide precursor with lamellar morphology was La2（CO3）3.3H20. The carbon dioxide carbonation method would provide significant benefits containing mild reaction conditions, high efficiency, low cost, and easy to realize large-scale production.     

ICP-AES测定稀土尾矿中的镧铈锶钡

采用电感耦合等离子体原子发射光谱(ICP-AES)法对稀土尾矿中的La、Ce、Sr、Ba元素进行了测定。研究了ICP-AES的操作条件并确定了适宜的实验条件,研究了酸度的影响以及谱线干扰的消除。样品平行测定的相对标准偏差小于1.6%,回收率在97.6%~103.3%之间,实现了稀土尾矿中镧、铈、锶、钡的快速、准确测定。     

Simultaneous determination of trace rare earth elements and other elements in high purity terbium oxide (Tb4O7) by ICP-AES after HPLC separation using P507 resin

This article describes a new method for the simultaneous determination of trace rare earth elements (REEs) and non rare earth elements (NREEs) in high purity terbium oxide by ICP-AES after HPLC separation using P507 resin. The chromatographic separation of the analytes from the matrix using dilute nitric acid as mobile phase was studied. The experimental results showed that a favorable separation of trace metals (Cu and Gd) from the matrix (Tb) can easily be achieved by elution with dilute nitric acid within 25 min. The proposed method was applied to the determination of trace metals (Ca, Cu, Mg, Mn, Ni, Si, La, Ce, Pr, Nd, Sm, Eu and Gd) in high purity terbium oxide. The detection limits (DLs) for the analytes ranged from 0.4–4.0 μg· g⁻¹, and the recoveries are from 78%–105%. Foundation item: Supported by the National Science Foundation of China (No. 20007010108) and Wuhan Municipal Science & Technology Commission (No. 995004080) Biography, Wanjau Ruth (1961-), female, Ph. D. candidate, Kenyatta University, Kenya, research direction: determination of trace elements.     

Determination of trace heavy metals in milk using an ionic liquid and bismuth oxide nanoparticles modified carbon paste electrode

A novel carbon composite electrode modified with bismuth oxide nanoparticles and the ionic liquid n-octylpyridinium hexafluorophosphate was fabricated and used to simultaneously determine cadmium and lead levels using square wave anodic stripping voltammetry.This electrode combines the unique advantages of nanomaterials and ionic liquid with the low cost and easy fabrication of the carbon composite electrode.Compared with the traditional binder based composite electrode,our electrode exhibited well-defined and separate stripping voltammetric peaks for cadmium and lead.Furthermore,the antifouling capacity of the bismuth film electrode was significantly improved by the ionic liquid.Under optimized conditions,the linear range of the composite electrode was from 3.0 to 30.0 μg L-1 for both metal ions with a detection limit of 0.15 μg L-1 for cadmium and 0.21 μg L-1 for lead.Trial milk sample analyses showed that the modified electrode was sensitive,reliable and effective for the determination of trace heavy metals,holding great promise for routine analysis applications.     

2,4-二羟基苯乙酮缩三羟基甲基氨基甲烷的合成及其在稀土矿样中铽的痕量荧光分析中的应用

合成了一种新的席夫碱配体2,4-二羟基苯乙酮缩三羟基甲基氨基甲烷.该配体与铽(Ⅲ)的配合物的荧光强度在磷酸钠或六次甲基四胺的存在下可增强18或26倍.有机溶剂CH3CN,DMF,丙酮,THF,DMSO,CH3OH,C2H5OH的添加可使其荧光强度进一步增加3～19倍.其中,用CH3CN作溶剂时荧光增加倍数最大,Tb-HL-HMTM体系荧光最强.pH=6.0时,激发和发射波长分别是355和545 nm.在理想情况下,荧光强度与Tb3+离子浓度成正比.对于HL-Na3PO4-CH3CN体系,线性范围2.3×10-10～5.8×10-5 mol/L,检测限2.0×10-10 mol/L,对于HL-HMTM-CH3CN体系,线性范围9.8×10-11～7.2×10-5 mol/L,检测限9.0×10-11 mol/L.基于此对Tb3+进行定量测定,该分析方法简单、快速、灵敏、干扰小.同时对荧光增强的机理进行了分析和讨论.