极谱法测定硫酸稀土复盐母液中的稀土总量

在pH9.0的NH3·H2O-(NH4)2SO4缓冲介质中,RE(Ⅲ)-TP的络合吸附波的波高与RE(Ⅲ)的浓度在0-10μg/mL间成线性。该方法的相对标准偏差2.23%,回收率99.51%-103.38%,用于硫酸稀土复盐母液中微量稀土总量测定,结果满意。     

Solid phase extraction for analysis of biogenic carbonates by electrothermal vaporization inductively coupled plasma mass spectrometry (ETV-ICP-MS): an investigation of rare earth element signatures in otolith microchemistry

Uptake of trace elements into fish otoliths is governed by several factors such as life histories and environment in addition to stock and species differences. In an attempt to elucidate the elemental signatures of rare earth elements (REEs) in otoliths, a solid phase extraction (SPE) protocol was used in combination with electrothermal vaporization (ETV) as a sample introduction procedure for the determinations by inductively coupled plasma quadrupole mass spectrometry (ICP-MS). Effects of various parameters, such as carrier gas flow rate, atomization temperature and chemical modification, were examined for optimization of the conditions by ETV-ICP-MS. Atomization was achieved at 2800 °C. Lower temperatures (i.e. 2600 °C) resulted in severe memory problems due to incomplete atomization. Palladium was used as a chemical modifier. It was found that an increase in Pd concentration up to 0.5 μg in the injection volume (70 μl) led up to four-fold enhancement in the integrated signals. This phenomenon is attributed to the carrier effect of Pd rather than the stabilization since no significant losses were observed for high temperature drying around 700 °C even in the absence of Pd. Preconcentration was performed on-line at pH 5 by using a mini-column of Toyopearl AF-Chelate 650M chelating resin, which also eliminated the calcium matrix of otolith solutions. After preconcentration of 6.4 ml of solution, the concentrate was collected in 0.65 ml of 0.5% (v/v) HNO₃ in autosampler cups, and then analyzed by ETV-ICP-MS. The method was validated with the analysis of a fish otolith certified reference material (CRM) of emperor snapper, and then applied to samples. Results obtained from otoliths of fish captured in the same habitat indicated that otolith rare earth element concentrations are more dependent on environmental conditions of the habitat than on species differences.     

Magnetic behaviour of TbMnFe

Neutron diffraction and M?ssbauer measurements have been carried out on the cubic Laves phase intermetallic TbMnFe. The magnetic moment on the transition metal atom is found to be low, 0.2μ _B, at room temperature. This moment is temperature independent down to 10 K. Magnetic moment on the rare earth atom varies from 2.5μ _B at 296 K to 7.27μ _B at 10 K. M?ssbauer spectra recorded at 298 K and 78 K have magnetic character but there is a large distribution of hyperfine field values. Both these features arise due to magnetic frustration created in the sample due to the competing ferro and antiferromagnetic interactions between the transition metal atoms.     

Solid state phase equilibria in the Gd-Si-B system at 1270 K

Solid state phase equilibria in the ternary Gd-Si-B phase diagram have been proposed at 1270 K using X-ray diffraction, scanning electron microscopy and electron probe microanalysis. Prior to this work, the binary systems Gd-B, Gd-Si and Si-B have also been reinvestigated. The main characteristic of the ternary diagram is the occurrence of two new ternary compounds Gd₅Si₂B₈ and Gd₅Si₃B_0.64. The former crystallizes in tetragonal symmetry, space group P4/mbm with unit cell parameters a=7.2665(3), c=8.2229(7) Å, the second one presents hexagonal symmetry, space group P6₃/mcm with unit cell parameters a=8.5080(4),c=6.4141(2) Å. The X-ray structures of the two structurally related phases Gd₅Si₃B_0.64 and host binary Gd₅Si₃ have been refined from three-dimensional single-crystal intensity data to the final R values of 0.036 (R_w=0.046) and 0.046 (R_w=0.055) for 457 and 401 reflections, respectively with [F>4σ(F)]. Both structures exhibit the Mn₅Si₃-type structure, with in addition for Gd₅Si₃B_0.64 a partial occupancy by boron of the normally vacant interstitial site at the center of the Gd₆ octahedron, which corresponds to the origin of the unit cell. Bonding between the interstitial boron atoms and the gadolinium ones forming the Gd₆B polyhedra is indicated by the decrease in the corresponding Gd-Gd distances and consequently in the unit cell volume. Finally, the Gd-Si-B phase diagram is compared with the previously reported Er-Si-B, at 1070 K.     

Synthesis,characterization, spectroscopy and thermal analysis of rare earth picrate complexes with <Emphasis Type="Italic">L</Emphasis>-lysine

Summary Rare earth picrate (RE) complexes with L-lysine (Lys) were synthesized and characterized. Elemental analysis (CHN), EDTA titrations and thermogravimetry data suggest a general formula RE(pic)₃·2Lys·2H₂O, where RE=La-Lu (without Pm) and Y, pic=picrate). IR spectra suggest that Lys is coordinated to the central ion through the nitrogen of the α-amino group. Parameters obtained from the absorption spectrum of the Nd compound indicated that the metal-ligand bonds are essentially electrostatic. Emission spectrum and biexponential behavior of the luminescence decay of the Eu compound suggest the existence of polymeric species. Thermogravimetric/derivative thermogravimetric (TG/DTG) and differential scanning calorimetry (DSC) curves of all complexes are very similar, with five events. The final products are the corresponding rare earth oxides and their X-ray diffraction patterns are identical to the calcinated oxides.</o:p>     

乙酰丙酮稀土四苯基卟啉配合物的电化学研究

本文指出我国环境保护产业发展中存在的问题，论述了“入关“对我国环境保护产业的影响及应采取的经济和税收政策。     

稀土复合变质对新型铸造热锻模具钢组织与性能的影响

研究了稀土复合变质对新型铸造热锻模具钢（CHD钢）组织与性能的组织。结果表明，稀土复合变质能细化晶粒，并且随着稀土量的增加。细化效果明显；加入适量的稀土复合变质后，夹杂物数量明显减少，夹杂物趋于球化并均匀地分布在钢中，形态和分布得以了改善，向钢中加入稀土进行复合变质，能促进贝氏体、奥氏体和位错亚结构的形成，细化马氏体板条。当残留稀土含量为0.02%时，CHD钢的硬度、强度变化不大，断裂韧性（KIC）和疲劳裂纹扩展门槛值（△Kth）有所提高，冲击韧性、延伸率、断面收缩率提高了近一倍，抗热疲劳性能也最好。     

Ni-SDC固体氧化物燃料电池阳极的合成和性质

采用柠檬酸-硝酸盐溶胶-凝胶低温自蔓延燃烧法制备氧化镍（NiO）粉末和Ce0.8Sm0.2O1.9（SDC）粉末，并将NiO与SDC按不同质量比和不同制备工艺制备了固体氧化物燃料电池（SOFC）的阳极前身。再用自组装的还原装置将其在820℃经2．5h还原后，采用四端子法测量其电导率值。分析了阳极片电导率与阳极片微结构、Ni的质量百分数、混合研磨时间及烧结温度之间的关系。结果显示，阳极片的电导率强烈依赖于镍含量和制备工艺。     

氨基羧酸纤维分离富集-电感耦合等离子体原子发射光谱法测定多种痕量稀土元素

本文制备了氨基羧酸纤维滤纸片作为柱填充物，成功地分离和富集了地化样品中的多种稀土元素。富集后的稀土元素采用电感耦合等离子体原子发射光谱法测定，回收率为90％～109％。本文还对基体干扰及其消除进行了研究。