二乙基三胺五乙酸用于示波极谱络合滴定法的研究

本文对二乙基三胺五乙酸（ＤＴＰＡ）用于示波极谱络合滴定的方法进行了研究，同时测定了多种金属离子和藻酸双酯钠新药，该法快速、准确、终点直观。     

Isothermal Calorimetric Titration of Human Serum Albumin with the Fullerene C60-L-Arginine Adduct

Russian Journal of General Chemistry - The interaction of the fullerene C60-L-arginine adduct with human serum albumin (HSA) has been studied by means of isothermal calorimetric titration at 298.15...     

新方法合成LiFePO4/C

以Fe(NO3)3·9H2O、LiNO3、NH4H2PO4和蔗糖为原料,在超临界CO2流体中反应合成,进而经二次焙烧制得LiFePO4/C。 结果表明,在超临界CO2流体中经50 ℃反应24 h,在350和600 ℃焙烧后制得粒径分布在0.5~1.0 μm的纯LiFePO4/C,该材料作为锂离子电池正极的放电比容量达156.6 mA·h/g,经50次循环后容量几乎没有衰减。     

SynthesisofFullereneC＿（60）DerivativesbyOne－potProcedure

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Synthesis of C60H2 by rhodium-catalyzed hydrogenation of C60.

Reduction of C60 with rhodium(0) on alumina and hydrogen in deuterated benzene (C6D6) at ambient temperature and pressure yields a mixture of hydrogenated compounds; C60H2 has been characterized as the major product in 14% yield based on 1H NMR.     

用电位滴定法测定配合物的组成

本文提出了一种用电位滴定法来测定配合物真正组成的数学模型，只要有两组Ｅ～Ｖ数据即可直接计算出结果，方法简便快速，应用面也较广。     

Synthesis of an Octacyclic C60 Fragment

Fragments of buckminsterfullerene (C₆₀) include the monumental three compounds corannulene, sumanene, and truxene. These three have served as leading molecules in ongoing research for curved, fused, and π-extended polyaromatic materials. Achieving more structural variations that join the ranks of these three archetypes remains challenging. Herein we report synthesis of an octacyclic hydrocarbon that is an unexplored C₆₀-fragment, namely, a 4,11-dihydrodiindeno[7,1,2-ghi:7′,1′,2′-pqr]chrysene (C₂₈H₁₆, which we named Metelykene). The key to success was solution-compatible synthesis in which double pentagonal rings flank hexagonal ones. This solution-phase approach, coupled with the resulting non-planar π-conjugation, is so straightforward that it offers an entry to a derivative such as a cardo aromatic monomer.     

A Convenient Synthesis of Novel Meldrum＇s Acid C60 Fullerene Derivatives

A series of novel Meldrum＇s acid C60 derivatives were prepared in moderate yields from a convenient one-pot reaction of C60, the Meldrum＇s acid derivatives, 12 and 1,8-diazabicyclo-[5,4,0]-undec-7-ene （DBU） in toluene at room temperature under nitrogen atmosphere. All the new compounds were fully characterized by the spectral data and elemental analysis. A carbene intermediate mechanism was proposed for this reaction.     

Synthesis of the C59N+ carbocation. A monomeric azafullerene isoelectronic to C60

A heterofullerene isoelectronic to C60 is reported. The azafullerenium cation C59N+ can be isolated in good yield as a carborane salt via the two-electron oxidation of the C-C bond of (C59N)2 dimer. [C59N][Ag(CB11H6Cl6)2] has been characterized by electronic, IR, Raman, and 13C NMR spectroscopies, MALDI spectrometry, DFT calculations, and X-ray crystallography.     

Synthesis and identification of heterocyclic derivatives of fullerene C60: unexpected reaction of anionic C60 with benzonitrile

During the reaction of reduced C60 with benzyl bromide in benzonitrile, a novel cis-1 C60 adduct, 1,4-dibenzyl-2,3-cyclic phenylimidate C60 (1), was obtained rather than the expected product of 1,4-dibenzyl C60. The structure of compound 1 was analyzed by X-ray single-crystal diffraction, identifying the presence of a five-membered heterocycle at a [5,6] bond of C60. One of the heteroatoms is assigned as a nitrogen atom; however, the identity of the other heteroatom cannot be determined unambiguously by crystallography due to similarity between the nitrogen and oxygen atoms. A related compound (2) bearing the same heterocycle was obtained from anionic C60 benzonitrile solution when no benzyl bromide was added. The structure of compound 2 was determined by NMR, MALDI FT-ICR MS, and UV-vis. Results from MALDI FT-ICR MS for compound 2 show unambiguously that the second heteroatom is an oxygen atom, which is probably from traces of water in the solvent. Control experiments of the reactivity of the neutral, monoanionic, dianionic, and trianionic C60 have shown that the reactive species for the unexpected reaction is the C60 trianion.     

线性滴定的微机绘图-回归处理法

关于线性滴定的理论、方法及特点已有专门文献介绍^[1-4],县体分为图解法和计算法两类.前者直观性强,对所用仪器的精度要求不高,但依靠手工作图,不仅费时费力,而且不免引入主观误差;后者计算繁杂,必须使用高功能电子计算机,本文在图解法基础上引入微机绘图,并自动剔除可疑值,再由微机进行回归处理,直接打印结果.     

Synthesis and characterization of tetrakis-silylated C60 isomers

A photochemical reaction of C(60) with disilane in a 2:3 ratio affords the isomer mixture of the tetrakis-adduct of C(60)((t)BuPh(2)Si)(4) as the major product. The use of a three-stage HPLC separation system isolated three of their isomers. Their structural assignments were based on FAB mass, UV-vis, NMR, and cyclic voltammetry (CV) measurements. The CV analysis showed that the terakis-adduct has lower oxidation and higher reduction potentials than the bis-adduct C(60)((t)BuPh(2)Si)(2) and the parent C(60).     

New Method for Increasing the Accuracy of Back Titration

Titrimetric analysis is an important quantitative analysis method in which the amount of constituent to be determined is calculated from the volumes and concentrations of titrants used in titration procedure.     

Synthesis of water-soluble C60-porphyrin hybrid compounds

Water-soluble C60-porphyrin hybrid molecules were first synthesized toward their pharmaceutical applications.     

豆荚型纳米材料C60@SWNTs的制备和表征

通过气相扩散的方法将C60填入单壁碳纳米管（SWNTs）,制备了豆荚型纳米材料C60@SWNTs,并利用高分辨电子显微镜（HRTEM）和拉曼光谱（Raman spectra）对其进行了表征.结果均证明C60以较高的比例填充入单壁碳纳米管中.HRTEM结果表明,填入单壁碳纳米管的C60之间的距离与面心立方C60晶体中C60之间的距离有细微的差别,说明C60分子与SWNTs间存在弱的范德华相互作用.此外,还观察到在电子束的照射下,C60在SWNT中两两聚合的现象.     

A new surface-enhanced Raman scattering system for C60 fullerene: Silver nano-particles/C60/silver film

Surface-enhanced Raman scattering (SERS) spectrum of very good quality of “silver nano-particles/C60/silver film” system was reported for the first time by using the pyridine as a intermediate to connect and nest the C60 molecules to the gap of silver nano-particles and silver film. Experiment results show that the ternary system of “silver nano-particles/C60/silver film” is very effective and active. Not only was the number of vibrational modes greatly increased, especially some modes that were forbidden in Raman spectrum, but also were the significant Raman bands splitted as well as frequencies up and down shifted, respectively, arising from symmetry lowering and selection rule relaxing of C60 induced by the silver surface. Furthermore, the splitting of the Raman modes is consistent with the calculation based on group theory. The adsorption of C60 molecules is oriented on pentagons of C60 on the silver surface. It is difficult to separate the contributions of the electromagnetic and chemical mechanisms to the great enhancement of the Raman signal. On the one hand, the silver nanoparticles modified on the silver film play an important role in magnifying the surface local electric field near the silver surface through resonant surface plasmon excitation. On the other hand, charge transfer factor may not be neglected.     

酸碱滴定法与碘滴定法测定维生素C

维生素C是一种重要的营养物质和药物,人体如果缺乏维生素将导致多种疾病的发生,严重时将导致坏血病、心脏及脾脏损伤等疾病.测定维生素的方法很多,主要有碘量法[1]、光度法[2]、电化学法[3]、色谱法[4]等.