环境样品中痕量邻苯二甲酸酯的分离与测定

本文研究了以小粒径（１０－４０μ）硅胶柱色谱分离富集、反相高效相色谱分析测定大气颗粒物、土主植物样品中痕量邻苯二甲酸酯的方法，方法操作简单，回收率高，空白值低，利用该方法分析了部分环境样品中邻苯二甲酯酯含量。     

群青颜料呈色机理的电子顺磁共振研究

研究了阿富汗青金石矿石、敦煌石窟青金石颜料、合成群青的呈色机理。实验表明三者均有ｇ＝２．０２９峰，前两者多一个ｇ＝２．０４７峰，４００℃时，ｇ＝２．０４７峰变平，６００℃时消失。ｇ＝２．０２９峰随温度升高而增强，８００℃时增强放慢，颜色也随温度变深。在Ｍ０Ｏ３／ＳｉＯ２和Ｍ０Ｏ３／Ａｌ２Ｏ３表面上，Ｓ２＾－的ＥＰＲ有ｇ１＝２．０４７，ｇ２＝２．２０８，ｇ３＝１．９９８三个分量。因此，群青、青金石和     

Development of an alcohol optode membrane based on fluorescence enhancement of fluorescein derivatives

A new type of optode membrane for the determination of alcohols, such as methanol, ethanol, propan-1-ol and propan-2-ol etc, is presented that can be exploited in optical and fibre-optic sensors. It is based on the use of a new lipophilic fluorescent reagent, namely fluorescein octadecyl ester (FODE), which is immobilized in a plasticized PVC membrane. The response mechanism relies on the fact that FODE can reversibly recognize alcohol molecules due to the hydrogen bonding formation between FODE and alcohol molecules. The analytical information in this membrane is the enhancement of the relative fluorescence intensity measured at 527 nm (463 nm, excitation). Under the optimum condition, the membrane has a wide measuring range for alcohol samples. The membrane has been applied to determine the concentration of ethanol in alcoholic drinks with satisfactory results.     

含铈类水滑石的制备及其衍生物催化研究

采用共沉淀水热法制备了镍铝铈三元复合层状氢氧化物.详细探讨了合成体系pH值、Ce/Al比及陈化条件对合成产物物相的影响;通过XRD,ICP,TG-DTA手段研究了合成物物相、组成及热行为.考察了以合成物为前驱体经焙烧后转化为镍铝铈复合金属氧化物在催化消除NO反应中的应用.实验结果表明,合成镍铝铈三元复合层状氢氧化物的适宜条件是:M2 /M3 =2,Ce/Al=0.07～0.75,pH=5.5～6.9,水热处理条件为110℃,5 h;在pH=5.5～6.9条件下,合成原料配比不同,产物物相相同,但组成不同;合成物热稳定性较差,在T=100～400℃之间,层间吸附水及层间平衡阴离子NO3-脱去,转化为复合氧化物,将此氧化物应用于NO消除反应中,表现出高的低温活性,400℃进行反应,NO转化率达95%,N2选择性几乎100%.     

Methodology for the preparation of C1-monoalkylated 1,2-dihydro[C70)] derivatives: formation of the "other" regioisomer

Deprotonation of 1,2-C(70)H(2) with TBAOH, followed by alkylation with methyl bromoacetate, results in formation of a C1-monoalkylated 1,2-dihydro-C(70) derivative. The position of the alkyl group (C1) was established by NMR spectroscopy and comparison with literature spectra of C2-monoalkylated analogs. Presumably, C1-alkylation is the major process due to selective deprotonation of 1,2-C(70)H(2) at C1. Substitution of benzyl bromide for methyl bromoacetate results in rapid dialkylation, unless the amount of base is carefully controlled, in which case C1-monobenzylation is the major process. This methodology for alkylation at C1 is complimentary to methods for the C2-monoalkylation of C(70) with Zn and methyl bromoacetate.     

Pyranoxanthones from Calophyllum Inophyllum

Phytochemical investigation of the stem bark of Calophyllum inophyllum resulted in the isolation of a new dipyrenoxanthone, calophinone ( 1 ), together with four related xanthones ( 2–5 ). Identification of the isolated compounds was achieved through intensive studies of their spectral data, especially 2D NMR.     

Synthesis and in vivo study of metallofullerene based MRI contrast agent

Gd@C₈₂(OH)₄₀ has been developed as a new generation of MRI contrast agent. But recently, it was found that Gd@C₈₂(OH) _x with a larger number of OH (x>36) would lead to cage break and hence, release of highly toxic Gd ions. We synthesized the more stable Gd@C₈₂(OH) _x with less OH-number, Gd@C₈₂(OH)₁₆, and studied its proton relaxivity and MRI images. The results indicate that Gd@C₈₂(OH)₁₆ also gives high proton relaxivity, even higher than that of (NMG)₂-Gd-DTPA. The bio-distribution indicated that Gd@C₈₂(OH)₁₆ tends to be entrapped in the liver and kidney and remained in tissue for about 2 hours. The results suggest that the more stable metallofullerene derivative Gd@C₈₂(OH)₁₆ can be the potential candidate of the new MRI contrast agent.     

杂原子Pb同晶取代Si－ZSM－12中的部分Si及其鉴定

杂原子Ｐｂ同晶取代Ｓｉ－ＺＳＭ－１２中的部分Ｓｉ及其鉴定赵修松，王清遐，李宏愿（中国科学院大连化学物理研究所，大连１１６０２３）关键词Ｐｈ－ＺＳＭ－１２，合成，表征ＺＳＭ－１２属丝光沸石类，具有一维线性非交叉孔道（０．５７×０．６１ｎｍ）［１，２］，...     

Yb:GdVO4晶体的缺陷研究

Yb：GdVO4晶体是一种很好的激光材料，但缺陷会对晶体的激光性能产生严重影响，开展对该晶体的缺陷研究有助于提高晶体质量。采用提拉法生长了面25mm×20mm，掺杂浓度为2％的Yb：GdVO4晶体；分析了晶体的结构及其对晶体解理性的影响；采用化学腐蚀法，以盐酸、氢氟酸为腐蚀剂，对晶体的主要晶面进行了化学腐蚀实验，通过其腐蚀坑形貌对晶体中的位错和晶界进行了研究；对晶体进行了高分辨X衍射实验，结果表明晶体中存在镶嵌块结构；开裂及散射颗粒也为晶体中较常见缺陷。分析了缺陷的成因并提出了预防措施。