离子选择电极—流动注射分析法动力学测定葡萄糖存在下的果糖

本文将离子电极与流动注射分析相结合，利用３０℃下，在强碱性介质中，果糖和葡萄糖与２，４－二硝基酚钠反应速度明显差异，动力学测定了葡萄糖存在下果糖的含量。自制了２，４－二硝基酚电极作为动力学电位测定用的工作电极。本法测定果糖的范围为０．０２～１．００ｍｏｌ／Ｌ，其ＲＳＤ为４．０％～４．９％，ＲＥ为１．０～５．０％；当Ｃ葡／Ｃ果≤３倍时，葡萄糖的干扰不超过５％；本法也曾成功地用于果葡萄浆测定，其ＲＳＤ     

UO2、UC2和UCO分子的结构和热力学性质

用密度泛函B3LYP方法,计算了UO2、UC2和UCO分子的结构和热力学函数,计算了固体U的振动内能Ev、振动和电子熵Sev,以及U在不同气氛（O2、C2、CO）中形成UO2、UC2和UCO晶体的ΔHfΘ、ΔSfΘ和ΔGfΘ.结果表明,UO2晶体最稳定.     

Synthesis, characterization and photodynamic activity of amino-substituted hypocrellin derivatives

Three new hypocrellin derivatives, amino- or amino acid-substituted on the side ring of hypocrellin B (HB), were synthesized by the reactions of HB with 3-methoxypropylamine, 6-aminohexanoic acid and gamma-amino-n-butyric acid, respectively. The structures of these compounds were characterized with proton nuclear magnetic resonance spectra, infrared spectra and mass spectra. The UV-visible absorption spectra, singlet oxygen-generating quantum yield and amphiphilicities of hypocrellin derivatives were measured and compared with HB, the parent compound. These derivatives showed strong absorption in the domain of the phototherapeutic window (600-900 nm) and improved amphiphilicity. HB and the derivatives were preliminarily tested for their photodynamic effects on human oral cavity epithelial carcinoma KB cell line in vitro. Two amino acid-substituted hypocrellins showed phototoxicity to the KB cell line. At an inhibitory dosage of 50% killing only 0.51 mumol L-1 compound 3 (or 0.88 mumol L-1 compound 2) and 0.5 J cm-2 irradiation were required. The hypocrellins exhibited some dark toxicity to the KB cell line. HB and amino acid-substituted hypocrellins showed lower dark toxicity to the KB cell line than amino-substituted hypocrellins in the assessment of cell survival.     

Determinations of combustion and formation enthalpies of C60 and C70

By using a micro-bomb calorimeter, the standard enthalpies of combustion of C₆₀ and C₇₀ have been determined to be - (25 947.1±8.5) and - (29 956.1 ± 8.9) kJ/mol respectively. A g. 1. c. analysis indicated that the amounts of residual organic solvents in the samples were very small, and their effects on the final results were negligible. The energy of combustion ofC60 determined in this work is in agreement in the uncertainty interval with that determined by means of traditional calorimeter using macro amount of sample. The enthalpies of formation of these two substances have been derived. The strain energies in the molecules of C₆₀ and C₇₀ were estimated by a bond energy scheme and by using corannulene as the model compound, the results estimated from different methods are very close. Project supported by the National Natural Science Foundation of China (Grant No. 29473143)     

Diterpene derivative and chromone from Hypericum perforatum

A novel diterpene derivative, 5-methyl-5-(4,8,12-trimethyl-tridecyl)-dihydro-furan-2-one (1) and a new chromone, 5-hydroxy-7-methoxy-3-methyl-chromen-4-one (2), along with a known compound, phytol (3) have been isolated from the aerial parts of Hypericum perforatum. Their structures were established on the basis of spectroscopic analysis and by comparison with published values.     

电极条件对硫酸介质中电解还原提纯镱过程的影响

研究了以钌铱钛合金网和汞分别为阳、阴电极, 在无气氛保护条件下, 采用电解还原方法从铥、镱、镥硫酸盐溶液中分离提纯镱的过程. 讨论了在8 V恒电压时的电极间距、位置, 以及阴、阳极表面积对电解过程中的电流、还原率影响. 优化了电解还原过程, YbSO4产品的纯度稳定达到99.5%以上, 一次收率可达80%;提镱后母液中的铥和镥被富集4倍以上, 其中Lu含量高于50%, 十分有利于后续铥/镥分离.     

Synthesis and Characterization of a Novel Organic/Inorganic Hybrid Based on Octamolybdates and Benzimidazole Molecules [Hbenzimi]4 [(benzimi)2Mo8O26] · 2H2O (benzimi?=?benzimidazole)

A novel organic/inorganic compound [Hbenzimi]₄[(benzimi)₂Mo₈O₂₆] · 2H₂O (1) has been prepared hydrothermally and characterized by elemental analyses, i.r., x.p.s., t.g. and single crystal X-ray diffraction. The single crystal X-ray diffraction analysis reveals that compound (1) consists of the [Mo₈O₂₆]⁴⁻ cluster as the structural motif covalently linked by benzimidazole molecules and protonated benzimidazole molecules as charge compensation cations. It is interesting that the benzimidazole molecules were synthesized from 1,2-phenylenediamine and oxalic acid. The [Mo₈O₂₆]⁴⁻ polyoxoanions and organic ligands in compound (1) interact with each other via extensive hydrogen bonds to form a three-dimensional supramolecular framework.     

D160大孔吸附树脂对染料木黄酮吸附性能的研究

研究了D160大孔吸附树脂对染料木黄酮的吸附性能.结果表明,在pH4.00时,该树脂对染料木黄酮有较好的吸附性能;静态饱和吸附容量为64.5mg/g树脂;用95%乙醇溶液作解吸剂,二次累计解吸率接近100%;表现速率常数k298=1.01×10-4s-1;测得吸附热力学参数分别为:△H=32.2kJ/mol,△S=119J/(mol·K),△G288=-2.03kJ/mol,△G298=-3.22kJ/mol,△G308=4.41kJ/mol.等温吸附服从Freundlich和Langmuir等温吸附规律;研究还表明,提高振荡频率对吸附有利.     

二点滴定法研究

就二点滴定法的原理，方法和应用进行了讨论，导出了二点滴定法计算公式。讨论了滴定剂加入量与测定结果准确度的关系。已用本法对标样样液及试样进行了多次测定，测定结果相对误差及相对标准偏差约０．２％。本法简便，快速，准确，且昨达于任何滴定类型的通用方法。     

Optimized Separation of Nine Xanthones by Microemulsion Electrokinetic Chromatography

A microemulsion electrokinetic chromatography method has been firstly used for the separation of the therapeutically important xanthones from Securidaca inappendiculata. The separation of the nine xanthones was systematically optimized with respect to pH, composition of microemulsion,addition of cyclodextrins, applied voltage and column temperature. Baseline separation was successfully achieved for the nine xanthones, which was also compared with that by micellar electrokinetic chromtography.