一种含有亚微米孔洞的新型微孔磷酸盐晶体材料的合成及其生长机理

采用水热法成功地合成了一种含有亚微米级孔洞的微孔磷酸盐晶体材料(记为HAP-TAP),其形貌特征是:六棱柱形的晶体表面分布着大量0.4～0.8μm的亚微米级孔洞,孔洞内长有片层状晶体.在样品晶化的过程中,通过控制合成时间,获得了纯六棱柱形晶体的大单晶(记为HAP).使用扫描电子显微镜(SEM)、粉末X射线衍射(XRD)、红外光谱和电子能谱(EDX)对HAP-TAP独特形貌的形成机理进行了研究和揭示.HAP的单晶XRD数据表明,HAP是一种具有二维空旷骨架结构的新型微孔磷酸铝晶体,其分子式为Al5(OH)2(PO4)7(C2N2H10)3.0.5H2O.EDX分析结果表明,生长于六棱柱形晶体孔洞内的片层状晶体为磷酸钛铝材料.     

三(2-苯并咪唑亚甲基)胺硝酸镍(Ⅱ)配合物的合成及结构

三（２－苯并咪唑亚甲基）胺简称ＮＴＢ与Ｎｉ（Ⅱ）的硝酸盐形成配合物Ｃ２８Ｈ３５Ｎ９Ｏ９Ｓ２Ｎｉ。本文报道其合成，红外光谱及晶体结构。该化合物为三斜晶系，空间Ｐ１↑－，ａ＝９．６５０（３），ｂ＝１２．７１６（２），ｃ＝１４．４３６Ａ，α＝１１．４６（２），β＝９１．６６（３），γ＝９７．５５（２）°，Ｖ＝１７１８（２）Ａ＾３，Ｚ＝２，Ｆ（０００）＝７９３，Ｄｃ＝１．４８ｇ／ｃｍ＾３，Ｍｒ＝７６４．１     

Study on analysis of153Sm-EDTMP stability in vitro and vivo by HPLC

The behavior of¹⁵³Sm-EDTMP in vitro and vivo is analyzed by the size exclusion HPLC. The experimental results show that EDTMP amounts have an obvious effect on the stability in vitro and uptake of¹⁵³Sm-EDTMP in the liver. HPLC analysis of urine sample indicates that¹⁵³Sm-EDTMP es excreted in the original form. The behavior in vivo of¹⁵³Sm-EDTMP containing 4 μg is similar to that of¹⁵³Sm-EDTMP containing 50 μg EDTMP at 1 h post-injection.     

氢化物－气相色谱的元素光度检测器

研究开发的一种新型的元素光度检测器主要用于锗、砷、锡和锑的氢化物气相色谱检测，具有高灵敏，高选择性。它是在普通火焰光度检测器的基础上加装了特制的滤光片改制而成的。对锗、砷、锡和锑的检测限分别为３．０×１０￣（－１１）ｇ、７．０×１０￣（－１１）ｇ、７．０×１０￣（－１０）ｇ和１．１×１０￣（－８）ｇ，相对标准偏差分别为１．８％、２．４％、２．６％和３．０％。     

Synthesis of Obyanamide, a Marine Cytotoxic Cyclic Depsipeptide

Obyanamide 1 is a cyclic depsipeptide that was recently isolated from the marine cyanobacterium Lyngbya confervoides by Moore and co-workers1. This compound displayed a potent inhibitory effect on both KB and LoVo cells in vitro. Several structural analog…     

固载化聚乙二醇三相催化下香豆素的合成

研究了固载化聚乙二醇三相催化下香豆素的合成，探讨了影响反应的主要因素。结果表明，该反应的最佳反应条件为：水杨醛与碳酸钾的摩尔比为 １： ０．７５，反应温度为１７５℃，反应时间为３．５ ｈ，该条件下香豆素的收率为 ６５．７％。     

低温原子化石墨炉原子吸收法测定环境和生物样中的镉

本文描述了以氩/氢混合气体作保护气体,测定环境和生物样品中痕量镉的石墨炉原子吸收法。实验证明,与纯氩气作保护气体相比较用氩/氢混合气体作保护气体,能够降低镉的原子化温度(100℃),并且减少基体物质如MgCl_2和NaClO_4的干扰。这种改善氯化物和高氯酸盐基体干扰的机理,主要是由于氢的存在与基体中的氯形成高离解能的氯化氢,从而避免了通常在镉原子化之前形成易挥发的氯化镉而损失。用本方法测定了七种标准参考物质,结果与标准值一致,证明方法是可靠的。     

中性芳烃稀土有机配合物的合成、结构及性能研究——Ⅲ.RE(C_6H_6)(AlCl_4)_3C_6H_6(RE=La,Nd)的合成及Nd(C_6H_6)(AlCl_4)_3C_6H_6的晶体结构

将加热活化的AlCl_3与三氯化稀土在苯溶液中反应,合成了2个新的轻稀土中性芳烃配合物RE(C_6H_6)(AlCl_4)_3C_6H_6(RE=La或Nd)。并用元素分析和红外光谱对其进行了表征。测定了含Nd配合物的晶体结构。对2个配合物结构的比较表明,中心金属离子对配合物的结构无明显影响,其键参数的差别主要来自“镧系收缩”。     

Comparative X-ray photoelectron spectroscopic study on the desulfurization of thiophene by Raney nickel and rapidly quenched skeletal nickel

The desulfurization of thiophene on Raney Ni and rapidly quenched skeletal Ni (RQ Ni) has been studied in ultrahigh vacuum (UHV) by X-ray photoelectron spectroscopy (XPS). The Raney Ni or RQ Ni can be approximated as a hydrogen-preadsorbed polycrystalline Ni-alumina composite. It is found that thiophene molecularly adsorbs on Raney Ni or RQ Ni at 103 K. At 173 K, thiophene on alumina is desorbed, while thiophene in direct contact with the metallic Ni in Raney Ni undergoes C-S bond scission, leading to carbonaceous species most probably in the metallocycle-like configuration and atomic sulfur. On RQ Ni, the temperature for thiophene dissociation is about 100 K higher than that on Raney Ni. The lower reactivity of RQ Ni toward thiophene is tentatively attributed to lattice expansion of Ni crystallites in RQ Ni due to rapid quenching. The existence of alumina and hydrogen may block the further cracking of the metallocycle-like species on Raney Ni and RQ Ni at higher temperatures, which has been the dominant reaction pathway on Ni single crystals. By 473 K, the C 1s peak has disappeared, leaving nickel sulfide on the surface.