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\5g-1, and the recoveries are from 78%-105%.     

ICP-MS的仪器参数对稀土元素离子信号强度的影响

研究了电感耦合等离子体质谱法（ICP－MS）的仪器主要参数（射频功率、雾化气流量、离子透镜电压）对15种稀土元素的离子、氧化物离子、氢氧化物离子和氢化物离子信号强度及各多原子离子产率的影响,并对各稀土元素多原子离子产率与各稀土元素性质的关系进行了探讨．研究结果有助于在测定单一高纯稀土中的其他稀土杂质时,选择仪器参数．     

以二-(2-乙基己基)磷酸酯(P_(204))/四氢呋喃/硝酸/多聚乙醛为展开剂薄层色谱法分离铕、钆、铽、镝、钬、铒等元素

本文应用二-(2-乙基己基)磷酸酯(P_(204))/四氢呋喃/硝酸/多聚乙醛[12∶60∶14∶140(v/v)]作为展开剂,对分离镧系元素进行了研究。在这个条件下,可将镧系元素中的铕、钆、铽、镝、钬和铒等元素分离,并获得较为满意的效果。同时本文对将条件试验和计算机优选法相结合方面做了一些尝试。     

以二-(2-乙基己基)磷酸酯(P_(204))/四氢呋喃/硝酸/多聚乙醛为展开剂薄层色谱法分离铕、钆、铽、镝、钬、铒等元素

本文应用二-(2-乙基己基)磷酸酯(P_(204))/四氢呋喃/硝酸/多聚乙醛[12∶60∶14∶140(v/v)]作为展开剂,对分离镧系元素进行了研究。在这个条件下,可将镧系元素中的铕、钆、铽、镝、钬和铒等元素分离,并获得较为满意的效果。同时本文对将条件试验和计算机优选法相结合方面做了一些尝试。     

微量元素对高纯铝箔立方织构的影响

采用晶体取向分布函数(ODF)研究和分析了在高纯铝中分别加入不同含量的微量稀土或铍对成品高纯铝箔立方织构的影响．研究结果表明添加微量稀土和铍,能改变高纯铝箔变形织构组分含量,单独加稀土时,形变织构变化不大;在单独加铍时,其S取向{123}<634>和Cu取向{112}<111>变化较大,随铍含量增加,其S取向密度f(g)减少,Bs{110}<112>取向密度增加．再结晶退火后,随稀土加入量增加,立方织构{100}<001>取向密度增加,R织构{124}<211>取向密度减少;铍添加较少时能增加成品箔材中立方织构{100}<001>强度,但随铍含量增加,立方织构含量急剧减少,R织构强度相应增加．稀土和铍在铝中溶解度都极小,与铁等微量杂质元素可能形成化合物析出后,能净化基体,减小铁对形成立方织构的阻碍作用,促进再结晶立方取向核心的形成与长大,增加立方织构比例．     

<Emphasis Type="Italic">In-situ</Emphasis> trace element analyses of zircons from Dabieshan Huangzhen eclogite: Trace element characteristics of eclogite-facies metamorphic zircon

The internal structures of zircons in eclogite from Huangzhen have been studied by cathodoluminescence (CL) microscopy. Two growth stages were distinguished: protolith magmatic cores and metamorphic overgrowth rims. These different domains were analyzed for trace elements using LAM-ICP-MS. The protolith and the overgrowth zircons have different trace elements characteristics. The trace element contents of protolith zircons are high and very variable. The overgrowth zircons show a typical trace element feature of equilibrium with garnet, e.g. low contents of HREE (132.2–197.6 μg/g) and small differential degree of HREE ((Yb/Gd)_CN=8.6–11.9). The contents of Nb, Ta and the ratio of Nb/Ta are lower in the metamorphic domains (0.5–1.4 μg/g, 0.7–1.5 μg/g, 0.3–1.3, respectively) than in the protolith domains (3.8–19.7 μg/g, 2.7–12.1 μg/g, 1.0–4.6, respectively). This is the first time to give the evidence that the metamorphic zircon equilibrates with the rutile, which formed during the peak metamorphic stage. The REEs and other trace elements data demonstrate that the metamorphic zircons overgrow in the eclogite-facies conditions. The trace element composition of zircon can therefore give new ways to constrain their formation conditions.     

In situ simultaneous determination of trace elements, U-Pb and Lu-Hf isotopes in zircon and baddeleyite

This paper describes a combined method of simultaneously measuring U-Pb and Lu-Hf isotopes as well as trace elements in Phalaborwa baddeleyite and 91500, GJ-1, TEMORA-1 and SK10-2 zircons by means of Neptune MC-ICPMS and Agilent Q-ICPMS connected to a 193 nm excimer laser ablation system. Material ablated by laser was carried in different proportions into Q-ICPMS for U-Pb isotopic and trace elemental and MC-ICPMS for Lu-Hf isotopic compositions. Experiments indicate that different proportions of ablated material for the Q-ICPMS and MC-ICPMS （6：4, 5：5 and 4：6 respectively） do not show any bias for the zircon/baddeleyite U-Pb age, Lu-Hf isotope and trace elemental compositions within analytical errors. Using 40-60 μm spot size, the obtained U-Pb ages of Phalaborwa baddeleyite, 91500, GJ-1, TEMORA and SK10-2 zircons are 2065±15 （2σ, n=20）, 1063±6 （2σ, n=-19）, 613±6 （2σ, n=20）, 416±5 （2σ, n=20） and 32.6±0.5 （2σ, n=20） Ma, respectively. The ^176Hf/^177Hf ratios are 0.281231±24 （2SD, n=20）, 0.282310±35 （2SD, n=19）, 0.282028±34 （2SD, n=20）, 0.282687±34 （2SD, n=20） and 0.282752±53 （2SD, n=20）, respectively. The obtained trace elemental compositions are identical to the reference values. Therefore, this kind of technique makes it possible to simultaneously obtain the U-Pb age, Lu-Hf isotopes and trace elemental compositions of zircon and baddeleyite, which could be an important tool in solving problems in earth sciences.     

中子活化法研究叶绿体中的稀土元素

用中子活化分析测定了油菜叶绿体中的稀土元素含量。结果表明叶绿体中含有微量稀土,其含量相当于每个稀土原子对应约2000个叶绿素分子,低于Fe, Mn, Cu等必需元素。     

薄层色谱法分离、测定稀土元素——I.展开剂的选择(2)四氢呋喃/磷酸三辛酯/硝酸/乙醚

用硅胶H/羧甲基纤维素/硝酸铵作载体,用磷酸三辛酯/四氢呋喃/硝酸/乙醚(3:18:2:18)作展开剂,镧、铈、镨、钕、钐之间能相互分离;轻稀土和钇能能完全分离;在轻重混合稀土中能单独分离镧、铈、镨、钬、钪。本方法能用于分离、测定独居石中的稀土元素。     

Determination of rare earth elements in plant protoplasts by MAA

A preliminary study on the speciation of rare earth elements in plant cells has been carried out by molecular activation analysis (MAA). Mesophyll protoplasts ofBrassica napus were isolated by enzymatic digestion. After being washed with isosmotic solution containing EDTA for several times, the protoplasts were purified by gradient centrifugation. Then the concentration of rare earth elements (REEs) in the protoplasts was determined by neutron activation analysis. The result shows that REEs can enter the cells of the plant.     

The environmental index of the rare earth elements in conodonts: Evidence from the Ordovician conodonts of the Huanghuachang Section,Yichang area

High-resolution microanalysis was performed on conodonts collected from the Huanghuachang section in the Yichang area using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). This region is regarded as a standard section for the division and correlation of the Ordovician system in southern China. The results show that the values of (La/Yb)N and (La/Sm)N decrease, while the values of δCe increase as seawater deepens and energy decreases. As the sedimentary environment changes from shallow-water carbonate platform to platform margin to open continental shelf to shelf basin, rare earth element distribution curves gradually transform from a right inclined pattern to a flat pattern to a left inclined pattern and a hat-shaped pattern. The present work proves that the values and distributive patterns of rare earth elements in conodonts correspond with the sedimentary environment, and therefore provide reliable evidence for the application of rare earth element concentrations of biogenic phosphates such as conodonts for palaeoenvironmental reconstructions.     

微波消解-ICP-MS法测定青海和西藏产区冬虫夏草中的35种元素

为了测定青海和西藏产区的17批冬虫夏草中的35种元素(其中16种为稀土元素)的含量,并进行初步产地鉴别分析,运用微波消解-ICP-MS法测定了3批玉树、4批那曲和10批果洛产区的虫草样本,并对3个产区的测定结果进行聚类分析。结果表明,不同产区的虫草药材各种元素含量差别较大,本文对其中4种有害元素Cd,Pb,As,Cu推荐了限量标准;聚类分析结果表明,玉树和果洛产区聚类较近、差异性较小;那曲产区聚类较远,相对差异性较大。该方法快捷、准确、可行性强,为不同产地冬虫夏草药材的质控和用药安全指导提供了理论依据。     

手性稀土配合物在不对称催化应用中的研究进展

近年来随着光学纯化合物需求的不断增大,不对称催化逐渐成为科学研究的前沿领域之一.稀土元素则是由周期表中ⅢB族Sc、Y和镧系元素(La~Lu)的17种元素组成.相比其他过渡金属与各类配体轨道间的作用,稀土金属有其独特之处,因此,近年来手性稀土配合物在不对称催化领域的应用,也逐渐引起人们的重视.根据各类手性配体中所含配位原子的不同,对手性稀土配合物的类型及相关的不对称催化反应作简要综述.     

稀土元素和巴比妥酸配合物的研究

在无水甲醇中，由氧化稀土和巴比妥酸（Ｂａｒｂｉｔｕｒｉｃａｃｉｄ）合成了６种稀土元素和巴比妥酸的配合物．通过元素分析、红外光谱、热谱分析、核磁共振和Ｘ射线粉末衍射等方法，确定了这些配合物的组成为ＬｎＢ３·４Ｈ２Ｏ（Ｌｎ＝Ｌａ、Ｎｄ、Ｅｕ、Ｇｄ、Ｔｂ、Ｄｙ．Ｂ＝巴比妥酸的－价负离子），并对成键情况作了讨论．     

Size distributions of major elements in residual ash particles from coal combustion

Combustion experiments for three coals of different ranks were conducted in an electrically-heated drop tube furnace. The size distributions of major elements in the residual ash particles (>0.4μm) such as Al, Si, S, P, Na, Mg, K, Ca and Fe were investigated. The experimental results showed that the concentrations of Al and Si in the residual ash particles decreased with decreasing particle size, while the concentrations of S and P increased with decreasing particle size. No consistent size distributions were obtained for Na, Mg, K, Ca and Fe. The established deposition model accounting for trace element distributions was demonstrated to be applicable to some major elements as well. The modeling results indicated that the size distributions of the refractory elements, Al and Si, were mainly influenced by the deposition of vaporized elements on particle surfaces. A dominant fraction of S and P vaporized during coal combustion. Their size distributions were determined by surface condensation, reaction or adsorption. The partitioning mechanisms of Na, Mg, K, Ca and Fe were more complex. Supported by the National Natural Science Foundation of China (Grant Nos. 50706013, 50721005 & 50720145604)     

Study of spectrophotometric method for determination of trace copper after the separation and enrichment with solid phase extractant-microcrystalline phenolphthalein

A new method of using phenolphthalein loaded with 1-(2-pyridylazo)-2-naphthol (PAN) as solid phase extractant to separate and enrich trace copper in diverse water samples has been developed. The ef- fects of different parameters, such as the amounts of PAN and phenolphthalein, stirring time, various salts and metal ions on the enrichment yield of Cu(II) have been investigated to select the experimental conditions. Under the optimum conditions, Cu(II) can be totally adsorbed on the surface of microcrys- talline phenolphthalein. By controlling appropriate acidity (pH=1.0), Cu(II) is completely separated from Cd(II), Pb(II), Mn(II), Co(II), Fe(III), Ni(II), Al(III), Zn(II) and Hg(II) in the solution. The possible reaction mechanism of the enrichment of copper is discussed in detail in this paper. The detection limit of this proposed method is found to be 0.03 μg·L-1 with the enrichment factor of 200. The recovery is in a range of 96.8%―105%. The standard deviation is less than 2.5%. The proposed method has been successfully applied to the determination of trace copper in different water samples with satisfactory results.     

阿克提什坎金矿床稀土元素研究

系统地研究了新疆阿尔泰诺尔特地区阿克提什坎金矿床的稀土元素组成特征及热液中稀土元素的配分模型 ,并应用 Grant等位线方法讨论了热液蚀变作用过程中稀土元素的行为。认为在热液蚀变作用过程中 ,稀土元素保持惰性 ,成矿热液与岩浆热液有关 ,赋矿围岩及矿区花岗岩提供了成矿物质。     

高纯Sc2O3中杂质稀土元素的电感耦合等离子体发射光谱测定法

本文提出了用电感耦合等离子体发射光谱测定高纯Ｓｃ２Ｏ３中的杂质稀土元素的方法，文章讨论了光谱干扰的基体干扰，报道了一些灵敏线的谱图，拟定出适合工厂日常分析的标准加入分析方法，获得了较好的分析结果。     

Direct determination of trace silicon in lanthanum oxide by using a selective volatility and slurry sampling-FETV-ICP-AES

A new method for determination of trace sillicon in high purity lanthanum oxide by using electrothermal vaporization (ETV)-ICP-AES with polytetrafluoroethylene (PTFE) slurry as a fluorinating reagent has been proposed. Under the optimized experimental conditions, the fluorination reactions of analyte (Si) and matrix(La) with PTFE in the graphite furnace took place at high temperature, and the fractional volatilily between Si and La was observed. Based on this principle the matrix interference could be eliminated. The detection limit of Si was 4.0μg·L⁻¹, and the RSD was 3.4%(C=0.2mg·L⁻¹,n=10). The procedure proposed has been applied successfully to determine trace Si in La₂O₃ without any chemical pre-treatment. Supported by the National Natural Science Foundation of China Qin Yongchao: born in Dec. 1953, ph. D., Assciate Professor     

Effects of rare earth elements on the microstructureand properties of magnesium alloy AZ91D

The effects of rare earth elements on the microstructure and properties of magnesium alloy AZ91D alloy were studied. The different proportion of rare earth elements was added to the AZ91D and the tensile tests were carried out at different temperatures. The experimental results show that at room temperature or at 120℃ the AZ91D's strength decrease with the increasing amount of the rare earth elements. However, the ductility is improved. The influence of 0.14%Sb (mass fraction) on the AZ91D's strength is like that of rare earth elements (0.2%-0.4%) (mass fraction). Microstructure graphs demonstrate that appropriate amount of rare earth elements (0.1%-0.2%) can fine AZ91D's grain and improve its ductility.