Application of diaza-18-crown-6-capped beta-cyclodextrin bonded silica particles as chiral stationary phases for ultrahigh pressure capillary liquid chromatography

Two bonded chiral stationary phases (CSPs), 8-aminoquinoline-2-ylmethyl- and 8-aminoquinoline-7-ylmethyl-diaza-18-crown-6-capped [3-(2-O-beta-cyclodextrin)-2-hydroxypropoxy]propylsilyl silica particles (non-porous, 1.5 microm), have been prepared and evaluated using capillary liquid chromatography at high pressures (> or = 8000 p.s.i.). High column efficiency (up to 400 000 plates m(-1)) was achieved for chiral separations. These CSPs with two recognition sites, i.e. substituted-diaza-18-crown-6 and beta-cyclodextrin combined with high chromatographic efficiency provide good resolution of a variety of enantiomers and positional isomers in relatively short times under reversed-phase conditions. After inclusion of a Ni (II) ion from the mobile phase, the positively charged crown ether-capped beta-cyclodextrin facilitates specific static, dipolar, and host-guest complexation interactions with solutes.     

氢谱在甾醇类化合物定量和纯度分析中的应用

用^1HNMR谱可定量确定繁茂膜海绵(Hymeniacidon perleve)中分离得到的结构类似的甾醇类化合物的含量，这种方法是对鉴定分析组成复杂而性质很相近的天然甾醇化合物的新思路。     

用共振电离飞行时间质谱仪分析土壤中超痕量气态金

采用激光共振电离飞行时间质谱技术（简称ＲＩＳ－ＴＯＦ技术）对土壤中超痕量气态金的含量进行了分析研究。ＲＩＳ－ＴＯＦ谱仪具有极高的灵敏度和很强的选择性，避免了对样品的预富集过程。本文给出了该谱仪对金元素的检测限和６５个土壤中气态金样品的分析结果，以及用中子活化法随机抽样检查的结果。     

精制煤液化中油加氢裂化制取喷气燃料的研究

在实验室固定床反应装置上,选用Mo-Ni-P/Si-Al工业催化剂,对精煤液化中油进行了加氢裂化制取喷气燃料的实验。考察了反应温度、空速对芳烃加氢转化及产品馏分分布的影响。通过加氢裂化,降低了油品芳烃含量,提高了喷气燃料馏分的收率。在总压为15MPa,反应温度为350—360℃,空速为0.8—1.0h~(-1)条件下,获得了芳烃含量低于10w%的低结晶点的优质喷气燃料产品。并对煤液化中油制取的喷气燃料的组成和性质进行了分析和评价。     

七-O-乙酰基-β-乳糖异硫氰酸酯的合成、表征及电化学研究

本文合成了并培养出了七-O-乙酰基—β—乳糖异硫氰酸酯的单晶，用X射线衍射分析了其晶体结构。结果表明，晶体为正交晶系，P2₁2₁2₁空间群，a＝1．23282(7)，b＝1．80012(10)，c＝1.85230(10) nm，α＝β＝γ＝90°，V＝4．1107(4) nm³，Z＝4。电化学实验观测到单链DNA和双链DNA对该化合物的峰电流均有明显降低作用，表明化合物与DNA发生了静电作用。     

流动注射化学发光法测定甲氨蝶呤

研究了甲醛增强高锰酸钾与甲氨蝶呤的化学发光反应，由此建立了一种测定甲氨蝶呤的流动性注射化学发光分析法，方法的检出限为３．４×１０＾－９ｇ／ｍＬ，相对标准偏差为１．１％（２．０×１０＾－６ｇ／ｍＬ甲氨蝶呤，ｎ＝１１）线性范围为１．０×１０＾－８～１．０×１０＾－５ｇ／ｍＬ。该法已用于甲氨蝶呤针剂及片剂中甲氨蝶呤含量的测定。     

LaPO4纳米微粒的制备及表征

Surface-modified LaPO4 nanoparticales were synthesized in the mixture solvent of water-ethanol with the surface modification age of dialkylphosphate. The conditions of synthesis and characterization were discussed. The results indicated that nanoparticle core of LaPO4 and surface-modified layer were formed. The surface-modified nanoparticles of LaPO4 can be dispersed in organic solvent and has better lubricating properties.     

Synthesis,characterization, and theoretical studies of group 4 amido hydrotris(pyrazolyl)borate complexes

Titanium and zirconium amido complexes containing a hydrotris(pyrazolyl)borate (Tp) or hydrotris(3,5-dimethylpyrazolyl)borate (Tp*) ligand TpM(NMe(2))(3) (M = Ti, 1; M = Zr, 2) and Tp*M(NMe(2))(3) (M = Ti, 3; M = Zr, 4) were prepared by the reactions of M(NMe(2))(3)Cl (M = Ti, Zr) with sodium hydridotris(pyrazol-1-yl)borate and potassium hydridotris(3,5-dimethylpyrazol-1-yl)borate, respectively. The structures of 1, 2, and 4.CH(2)Cl(2) were determined by X-ray diffraction and show octahedral coordination geometry around the metal centers. Density functional theory calculations at the B3PW91 level were performed to understand the orientations and the rotational behavior of amido ligands in these metal complexes.     

繁峙煤镜质组的生烃特征与热解产物生成动力学研究

本文利用付立叶红外光谱（ＦＴＩＲ），热解气相色谱（Ｐｙ－ＧＣ）及热解气相色谱质谱（Ｐｙ－ＧＣ－ＭＳ）联用技术等分析手段，探讨了我国山西繁峙煤镜质组的生烃特征，鉴定了如气体烃、正构脂肪烃、苯酚、单环芳烃以及甲氧基酚类等热解产物６７种化合物。用相继等温热解法一级反应动力学模型，求取了热解产物如气体组分（Ｃ１￣Ｃ６）、轻烃（Ｃ７￣Ｃ１４）、重烃（Ｃ１５￣Ｃ３０）、正构脂肪烃（ｎＣｉ）、烷基芳烃、苯酚等的     

The determination of calcium in yttrium oxide by alpha-particle activation analysis

The determination of calcium in yttrium oxide through the⁴⁰Ca(α, p)⁴³Sc reaction was studied, using a post-irradiation radiochemical separation procedure. The half-life of⁴³Sc was determined to be 3.87 hr. The chemical recovery was about 70%. The detection limit was about 10 ppb, for a 30 min irradiation at an alpha-particle beam current of 1 μA (E_α=13.4 MeV) and γ−γ coincidence counting (background counts being<1, cpm), with counting starting at 4 hours after the end of irradiation. Four samples of a batch of yttrium oxide (A.R.) were analyzed, and found to contain 13.9±1.0 ppm of calcium.