Two-dimensional separations and behaviour of alkaloids of various polarities on unmodified silica gel in polar and very polar neutral or acidic mobile phases

Summary New separation procedures for alkaloids of similar polarity and structure or of very different polarity and structure, based upon two-dimensional thin-layer chromatography on unmodified silica gel under mild conditions are described. Separation factors and separation mechanisms based on the structure of the bases and mobile phase composition are discussed for some examples of very efficient procedures.Proportions in solvent mixtures are v/v except where otherwise indicated.     

Effect of Hydration–Dehydration Processes on the Structure and Porosity of Detemplated Silica Fibers

A study was carried out on the conditions of template removal (calcination or extraction by solvents) and hydration–dehydration processes on the hexagonal structure and porosity of detemplated fibers. The hydration–dehydration cycle leads to a decrease in fiber porosity, especially in fiber detemplation by extraction with surfactant solvents such as ethanol and acetic acid.     

An application of factorial design to the development of fused silica capillary columns

Stationary phase crosslinking conditions for fused silica capillary columns were optimized with the use of a factorial design experiment. This experimental strategy was chosen because it provided for the determination of two-factor interactions. A predictive model was developed for the desired chromatographic performance parameters as a function of the variables of the crosslinking reaction. Confirmatory experiments proved the usefulness of the mathematical model which resulted in the production of capillary columns of superior performance with significant improvements in reproducibility.     

Preparation of octadecyl modified column gels using heat-treated silicas and their retention behaviour in high-performance liquid chromatography

Summary The effect of silanol groups on three types of octadecylmodified column gels using heat-treated silicas by calcination has been studied by high-performance liquid chromatography. After heat-treating at 180°C, 500°C and 950°C, the silicas treated with octadecyldimethylchlorosilane were used for the measurement of physical and chemical analysis. From elemental carbon analysis data, the reactive silanol group concentrations, _OH(s), were determined to be 2.0 in the 180°C treated silica, 2.1 in the 500°C treated silica and 1.6 in the 950°C treated silica, respectively (original silica: mean pore diameter 116 Å, specific surface area 298 m²/g, pore volume 1.22 ml/g, particle size 5.0 m). The separation factors, , of pyridine versus phenol were measured to be 0.79 on 180°C treated silica, 0.91 on 500°C treated silica and 1.98 on 950°C treated silica, using acetonitrile-water mixtures as the eluent. And then, on the basis of the physico-chemical and chromatographic data, the three types of octadecyl modified column gels using heat-treated silicas by calcination have been compared.     

Characterization of plant oils on a monolithic silica column by high-performance liquid chromatography-atmospheric pressure chemical lonization-mass spectrometry

Summary Five plant oils (peanut, pumpkin seed, sesame seed, soybean, and wheat germ) have been analyzed by high-performance liquid chromatography-atmospheric pressure chemical ionization-mass spectrometry (HPLC-APCI-MS). Gradient elution was performed with acetone-acetonitrile mobile phases on a short monolithic silica column (SilicaROD, RP-18e, 50 mm×4.6 mm). Identification of plant oil triacylglycerols (TAG) was based on the pseudomolecular ion [M+H]⁺ and the diacylglycerol [M−RCO₂]⁺ fragments. Positional isomers of triacylglycerols were identified from the relative intensities of the [M-RCO₂]⁺ fragments. Principal-component analysis, used to find similarities and differences between the different oils, indicated that the different plant oils could be clearly differentiated according to their triacylglycerol composition. Presented at Balaton Symposium '01 on High-Performance Separation Methods, Siófok, Hungary, September 2–4, 2001     

On the determination of polarity parameters of silica by means of solvatochromic probe dyes

Empirical solvent parameters of silica surfaces are determined by means of solvatochromic dyes, e.g., Cu(tmen) (acac)⁺ ClO ₄ ^– /B(C₆H₅) ₄ ^– , Fe(phen)₂(CN)₂, and Michlers Ketone dissolved in 1,2-dichloroethane or cyclohexane. The values obtained by UV/VIS-measurements are compared with both the polarity scales of Kamlet and Taft and with Gutmann's donor and acceptor numbers. Kamlet and Taft's -parameter (the hydrogen-bond donation capacity of a solvent) is determined independently by means of salicylideneaniline. The ^* of silica is determined using 5-N,N-dimethylamino-5-nitro-2,2-bithiophene and the complex of tetracyanoethylene with Michlers Ketone, respectively. Further on the reliabilities of the obtained Kamlet-Taft parameters , , and ^* are checked by comparism with experimental and calculated values of theE _T(30)-parameter of silica by means of multi-parameter regression analysis. The surface properties of silica are influenced mainly by HBD-properties (75%) and dipolarity/polarizability ^* (20%), but hardly by the HBA-properties (<5%). UV/VIS-measurements were carried out in a special equipment with glass fiber optics, A drawing of the apparatus is given.     

Formation of the surface charge on silica in mixed solvents

At sufficiently high concentrations of methanol and of alkali salts in aqueous silica dispersions, the negative -potentials of the particles are decreased. This effect is more pronounced with lithium than with other alkali cations, and it is independent on the anion. The NMR spectra indicate lithium adsorption on silica from mixed solvents, but not in the absence of alcohol.Supported by a contract with the XMX Corporation, Burlington, Massachusetts, USA     

悬砂稠化剂流变特性研究

研制出一种具有三维网络状结构的悬砂稠化剂，该稠化剂具有极强的悬砂能力，能与山砂以任意的配比形成复合浆体，并将山砂和水固结在一起而不脱水，极大地提高了砂浆防灭火效果；此外使砂不易堵管，大大地降低砂子对管道的磨损，并有利于管道长距离输送．并对悬砂稠化剂流变特性进行了研究，得到该稠化剂是具有剪切稀化特性的假塑性非牛顿流体；当悬砂稠化剂浓度为0．4％时，溶液具有最佳的流体力学特性；同时悬砂稠化剂的粘度与Ca^2＋离子浓度、Na^＋离子浓度、pH值、温度以及存放时间等因素密切相关．最后，用悬砂稠化剂进行了悬浮山砂的实验，制备出具有优良防灭火性能的稠化砂浆．图7，参8。     

The age of formation of the mirabilite and sand wedges in the Hexi Corridor and their paleoclimatic interpretation

The Hexi Corridor is located at the transition zone of the Asian summer monsoon and westerly airflow, and lies in an important position in terms of its ecological fragility and climatic sensitivity. During a recent field expedition to this region, we found a sedimentary mirabilite layer in a number of localities including Suwushan, Yanchi, Baitujing, Yanchi Gaotai, Huahai, Yumen, Halanuo扙r, and Dunhuang (Fig. 1), which have the potential to provide important information about environmenta…     

Contributions of different land cover types in Otindag Sandy Land and Bashang area of Hebei Province to the material source of sand stormy weather in Beijing

Different land cover types in Otindag Sandy Land and Bashang area of Hebei Province are linked to a material source of sand stormy weather in Beijing based on results of field vegetation and soil survey and laboratory works. Results of grain size analysis show that dust release potential in per unit area of moving sandy land is small,while lowland meadow and meadow steppe in stony hills have high potential of releasing dusts in per unit area during sand stormy weather occurrence. Further considering the effects of vegetation, it is inferred that the moving sandy land served as a material source of past dust storm and the possibility of dust release in per unit area is low in current time.Typical steppe in stony hills is undergoing desertification and its dust release possibility in per unit area is high. Farmland has strong potential of release dusts when they are ploughed in spring, but a large amount of therophytes grow and thus prevent dusts from release when cultivation was terminated.Potentials of dust release in per unit area in fixed sand dunes,stony mountain meadow steppe and low land meadow are lowdue to high cover of perennials. Sand dune reactivation and desiccation of lakes and lowlands under estimated future climatic change will make them serve as a future material source of sand stormy weather.