微分脉冲溶出伏安法同时测定食品中的锌铁锰

在1％乙二胺-0．1mol／L酒石酸钠-pH11．82 Britton—Robinson缓冲溶液体系中用微分脉冲溶出伏安法同时测定锌、铁、锰三种微量元素。它们的峰电位分别为-1184，-1392和-1456mV(vs．Ag/AgCl)；线性范围分别为：0.001—0.015，0．005—0．05和0．04—0．7μg／mL，最低检出浓度分别为0．0007，0．0014和0．0193μg／mL。本法操作简便、准确、灵敏度较高，用于食品中这三种元素的分析，结果令人满意。     

Low-threshold, high-efficiency, high-repetition-rate optical parametric generator based on periodically poled LiNbO3

We report a high-repetition-rate optical parametric generator (OPG) with a periodically poled lithium niobate (PPLN) crystal pumped by an acousto-optically Q-switched CW-diode-end-pumped Nd:YVO_4 laser. For the maximum 1064nm pump power of 970mW, the maximum conversion efficiency is 32.9% under the conditions of 250℃, 1064nm pulse repetition rate of 22.6kHz and pulse width of 12ns, and the PPLN OPG threshold in the collinear case is less than 23.7μJ. The output power increases with the increase of the crystal temperature. The 1485－1553nm signal wave and 3383－3754nm idler wave are obtained by changing the temperature and the angle of the PPLN crystal.     

Inorganic Sol-Gel Preparation of Medium Sized Microparticles of Li2TiO3 from TiCl4 as Tritium Breeding Material for Fusion Reactors

Microspheres of Li₂TiO₃ were fabricated by a classical, inorganic sol-gel process from commercially available TiCl₄. Elaborated process consists of the following main steps: (1) dissolving of TiCl₄ in concentrated aqueous HCl and addition of LiOH; (2) formation of sol emulsion in 2-ethylhexanol-1 containing the surfactant SPAN-80 (EH); (3) gelation of emulsion drops by extraction of water with partially dehydrated EH; (4) impregnation of gel to Li:Ti molar ratio MR = 2; (5) thermal treatment at 1200°C in order to receive chloride free product. This temperature can be significantly lowered (to 750°C) by dechlorination starting solution TiCl₄ by chemical treatment of the with nitric acid to form of nitrate-stabilized titania sols. Tritium release from sol-gel made Li₂TiO₃ microspheres were found very close to that observed for other traditional materials, however for the first sample process starts slightly earlier.     

若干具有[(PO4)2Mo5O15]簇骼的化合物的光谱研究

本文对所合成的具有 [(PO4 ) 2 Mo5O1 5]簇骼的 3种新颖的有机 磷钼酸盐簇合物(NH3CH2 CH2 NH3) 2 5[(PO4 ) (HPO4 )Mo5O1 5]·7 5H2 O (Ⅰ ) ,(H3NCH2 CH2 NH3) 3·[(PO4 ) 2 Mo5O1 5]·3H2 O (Ⅱ )和(H3NCH2 CH2 NH3) 2 ·[Cu(en) ][(PO4 ) 2 Mo5O1 5]·5H2 O (Ⅲ )用FTIR ,NIR Raman ,紫外 可见漫反射光谱 (UV VisDRS)和荧光光谱等研究手段 ,对其进行光谱研究 ,探讨其结构和性能的关系。在这些化合物中 ,化合物Ⅰ和Ⅱ具有孤立的 [(PO4 ) 2 Mo5O1 5]簇骼基元 ,而化合物Ⅲ的 [(PO4 ) 2 Mo5O1 5]簇骼基元是由 [Cuen]基团桥联成链 ;磷钼酸盐的特征振动频率和这些化合物的结构相关 ;UV VisDRS显示 ,在 2 0 0和 2 6 0nm左右有两个杂多化合物的特征吸收谱带 ;化合物的稳态荧光光谱中 ,观察到以 2 4 0nm激发 ,在大约 4 0 0nm附近出现的由金属氧簇Oμ→Mo跃迁激发所引起的较强的发射峰 ,在化合物 (Ⅲ )中 ,还观察到通过 [Cuen]的荷移跃迁的以 5 70nm激发所产生的 6 0 4nm的发射峰。     

Structures and syntheses of layered and framework amine-bearing uranyl phosphate and uranyl arsenates

Two hydrated uranyl arsenates and a uranyl phosphate were synthesized by hydrothermal methods in the presence of amine structure-directing agents and their structures determined: (N₂C₆H₁₄)[(UO₂)(AsO₄)]₂(H₂O)₃, DabcoUAs, {NH(C₂H₅)₃}[(UO₂)₂(AsO₄)(AsO₃OH)], TriethUAs, and (N₂C₄H₁₂)(UO₂)[(UO₂)(PO₄)]₄(H₂O)₂, PiperUP. Intensity data were collected at room temperature using MoKα X-radiation and a CCD-based area detector. The crystal structures were refined by full-matrix least-squares techniques on the basis of F² to agreement indices (DabcoUAs, TriethUAs, PiperUP) wR₂=5.6%, 8.3%, 7.2% for all data, and R₁=2.9%, 3.3%, 4.0%, calculated for 1777, 5822, 9119 unique observed reflections (|F_o|?4σ_F), respectively. DabcoUAs is monoclinic, space group C2/m, Z=2, a=18.581(1), b=7.1897(4), c=7.1909(4) Å, β=102.886(1)°, V=936.43(9) Å³, D_calc=3.50 g/cm³. TriethUAs is monoclinic, space group P2₁/n, Z=4, a=9.6359(4), b=18.4678(7), c=10.0708(4) Å, β=92.282(1)°, V=1790.7(1) Å³, D_calc=3.41 g/cm³. PiperUP is monoclinic, space group Pn, Z=2, a=9.3278(4), b=15.5529(7), c=9.6474(5) Å, β=93.266(1)°, V=1397.3(1) Å³, D_calc=4.41 g/cm³. The structure of DabcoUAs contains the autunite-type sheet formed by the sharing of vertices between uranyl square bipyramids and arsenate tetrahedra. The triethylenediammonium cations are located in the interlayer along with two H₂O groups and are disordered. Both TriethUAs and PiperUP contain sheets formed of uranyl pentagonal bipyramids and tetrahedra (arsenate and phosphate, respectively) with the uranophane sheet-anion topology. In TriethUAs, triethlyammonium cations are located in the interlayer. In PiperUP, the sheets are connected by a uranyl pentagonal bipyramid that shares corners with phosphate tetrahedra of adjacent sheets, resulting in a framework with piperazinium cations and H₂O groups in the cavities of the structure.     

Magnetic properties of lanthanum orthoferrite fine powders prepared by different chemical routes

Fine powders of lanthanum iron oxide, LaFeO₃, have been prepared by solid state reaction as well as sol-gel synthesis and nebulized spray pyrolysis. Structures, morphologies and magnetic susceptibility measurements of these powders have been examined. The powders prepared by all the three low-temperature routes contain nearly spherical particles with an average diameter of 40 nm. These samples show a lower Neel temperature than the powder prepared by solid state reaction besides showing much lower magnetic susceptibility at low temperatures. Dedicated to Professor C N R Rao on his 70th birthday     

磷酸三丁酯从硝酸介质中萃取铀（Ⅵ）的动力学研究

用上升单液滴法和恒界面池法研究了磷酸三丁酯-环己烷从硝酸介质中萃取铀(Ⅵ)的动力学。萃取过程为扩散控制,得到了在扩散控制下影响萃取速率的一些规律。     

水浸对含钕熔铁氨合成催化剂的影响

已有熔铁氨合成催化剂中添加稀土的报道.我们通过添加稀土得到了几种活性较高的催化剂,经进一步改进制备工艺(水浸处理后),活性又有所提高.本文利用XRD和AES等,对经水浸前后的含稀土催化剂的结构进行了测试,探讨了水浸后活性提高的原因.     

三硼酸锂晶体的生长形态

用自由生长系统研究了三硼酸锂ＬｉＢ_３Ｏ_５（ＬＢＯ）晶体的实际生长形态。实验表明，它的各晶面簇的重要性的顺序为：｛１１０｝＞｛０１１｝＞｛２０１｝＞｛１１１｝。讨论了ＬＢＯ晶体的生长习性与内部结构之间的关系并应用负离子配位多面体理论模型解释了ＬＢＯ晶体的生长形态。