几种常见水果的微量元素分析

运用原子吸收分光光度法测定了几种常见水果中部分微量元素含量。其中榴莲的Mg、Zn、Cu、K含量位于四种水果之首。美国提子中Ca含量最高，芒果中Fe含量最高。以上差别具有统计学意义。六种元素的回收率为90％-106．5％。连续6次测定样品，变异系数(CV)为0．96％。     

测接触角法确定偶联剂的最佳用量

偶联剂是一类能在无机填料和聚合物基材之间形成“分子桥”、改善两者之间相容性或提高两者之间相互作用能力的化合物。将经偶联剂改性的无机填料填充到聚合物中可以制得成本低、性能好的复合材料。由于偶联剂用量多少将对复合材料的性能产生较大影响,因此建立一种准确、简便地确定偶联剂最佳用量的方法有着十分重要的理论和实际应用意义。     

Investigation of gas chromatographic interaction mechanism on permethylated cyclodextrins by molecular modelling

Summary The capillary gas chromatographic retention behavior of -pinene and tricyclene has been investigated on stationary phases of different polarities. On all but one of the columns employed, tricyclene eluted before -pinene; only permethylated -cyclodextrins dissolved in moderately polar polisiloxanes gave a reversed elution order. The intermolecular interactions which caused the unexpected retention behavior were investigated in detail, applying methods of computer simulation. To achieve this, we have developed a calculation algorithm on the basis of molecular mechanical optimizations and programmed it in a macro. This makes it possible to systematically investigate a given configuration space in which all the possible interactions can take place. It was shown that permethylated -cyclodextrin as host molecule for both guest molecules offers an optimum cavity size. As a result the number of energetically favorable contacts between host and guest molecules as well as the strength of the interactions in this stationary phase were larger. As a consequence the elution order, normally only influenced by the vapor pressure of the compounds at a given temperature, was changed. Nonspecific interactions played an especially important role for these kinds of substances.     

Fermi and Coulomb correlations in the 21 S state of the helium isoelectronic sequence

The Fermi and Coulomb holes of the 2¹ S state of the helium isoelectronic sequence are investigated. Several interesting differences between the results obtained and those which might be expected on the basis of the corresponding 2³ S state are pointed out and discussed.     

Some Conversions of Thiazoline Carboxylic Acid Esters

We have carried out solvolysis of the previously described ethyl esters of 3-methyl(aryl)-4-methyl-2-thioxothiazoline-5-carboxylic acids, leading to the corresponding acids without breaking down the heterocycle. We synthesized a series of novel esters from the latter by treatment with dimethyl sulfate or reactive halides. Of these, only in the case of the ethyl ester of 3,4-dimethyl-2-thioxothiazoline-5-carboxylic acid did we obtain the hydrazinolysis product (the hydrazide), from which we synthesized novel hydrazones by treatment with aldehydes and ketones.     

Supercritical fluid chromatography of industrial paraffins and waxes

Summary The application of capillary SFC for SIMDIST investigations of paraffins and waxes is reported. Pressure, density and temperature of the mobile phase are optimized to obtain high chromatographic resolution of complex mixtures of industrial products. Isothermal linear pressure programming and asymptotic pressure and density programming are used in the range from 15 to 35 MPa in the isothermic mode above 100°C. SFC chromatograms of natural and synthetic paraffins, microcrystalline wax and candle wax are compared. The retention behaviour of paraffin mixtures and waxes has been investigated on methyl/phenyl and biphenyl capillary columns. The polarity of the stationary phases influences the absolute retention time more than it influences the chromatographic resolution.     

Photochemical properties and structures ofN-amino andN-azomethine derivatives of 2,4,6-triphenylpyridinium perchlorates

The molecular structures of the initial compounds and the products of photocyclization involving amino and azomethine groups in perchlorates ofN-amino (1) andN-azomethine (2) derivatives of 2,4,6-triphenylpyridinium cations were studied. Cations1 and2 have an essentially non-coplanar arrangement of the -Ph rings, and the product of photocyclization of2, cation3, is characterized by a flattened structure. It was found that the orientation of the lone electron pair of the N atom with respect to one of the planes of the -Ph rings in molecule1 is more favorable for monocyclization involving the amino group. The structure of molecule2 allows two routes of the photoreaction,viz., O N proton transfer and monocyclization with an -Ph ring. However, the structural features of molecule2 are more favorable for photocyclization.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 2, pp. 296–301, February, 1995.     

A study of the oxidation of vegetable oils by inverse gas chromatography

Summary Inverse gas chromatography is shown to be suitable for the study of the oxidation of vegetable oils. With air as carrier gas characteristic plots of retention index versus time are obtained for hydroxylic test solutes that are consistent with the oxidation behaviour of vegetable oils. Shifts of retention are found to be accompanied by changes of column efficiency due to the oxidative crosslinking of polyunsaturated vegetable oils. The technique also leads to useful information concerning the oxidation of antioxidant inhibited systems. Presented at the 15th International Symposium on Chromatography, Nürnberg, October 1984     

Diagnostic and therapy-control of inborn metabolic disorders by high-performance liquid chromatography: 2,8-dihydroxyadeninuria,xanthinuria

Summary 2,8-Dihydroxyadeninuria and xanthinuria are inborn enzyme disorders which must be under lifelong therapeutic control. Quantitative determination of 2,8-DHA and xanthine using reversed phase HPLC was performed. A new application for the separation of purines shortens analysis-time. Examples of the determination of 2,8-DHA and xanthine before and under certain therapies are shown. Long term monitoring of the patients offers the possibility of a reliable prophylaxis against stone recurrence.     

Structural and magnetic investigations of the mixed-valence Fe(II,III) two-dimensional layer complex, [Fe2(II) Fe2(III)(HCOO)10(C6H7N)6]n.

The structure of the complex, [Fe2(II)Fe2(III)(HCOO)10(C6H7N6)n, (1) exhibits a neutral two-dimensional layer network of alternating iron(II) and iron(III) ions, bridged equatorially by formate groups. All iron atoms are octahedrally coordinated, with iron(III) coordinating axially to one gamma-picoline and one formate group, while the iron(II) centers interact axially with two gamma-picoline groups, above and below the layer plane. The complex crystallizes in the triclinic space group P1 at all studied temperatures [at 120 K, the cell dimensions are: a = 10.228(1), b = 12.071(1), c = 12.072(1) A, alpha = 89.801(2), beta = 71.149(2), gamma = 73.371(2) degrees]. An intralayer antiferromagnetic exchange interaction of J = -2.8 cm(-1) between iron(II) and iron(III) was observed in the magnetic studies. Decreasing the temperature to close to 20 K causes a magnetic-ordering phenomenon to occur and a low-temperature phase with a long-range antiferromagnetic spin orientation appears. The magnetic phase transition was confirmed by M?ssbauer spectroscopic studies at temperatures above and below the critical temperature. Structural information of 1 from synchrotron X-ray diffraction data collected at room temperature and 16 K suggests that the antiferromagnetic ordering is caused by an enhanced pi-pi interaction between chi-picoline groups from adjacent layers.