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991.
The influence of a water vapor admixture in helium, nitrogen, and carbon dioxide on capacity coefficients of C3−C5 alcohols and pyridine during chromatography process in capillary columns with polar (PEG-20M) and nonpolar (SE-30) stationary
phases was studied. The introduction of a water admixture into the carrier gas, increases the capacity coefficient of polar
organic compounds on the capillary column with PEG-20M and has almost no effect on this value in the case of SE-30. The change
in retention of polar organic compounds on the capillary column with the PEG-20M polar phase occurs due to a change in the
properties of the stationary phase when it adsorbs water from the mobile phase.
Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 11, pp. 2258–2261, November, 1998. 相似文献
992.
993.
Transparent glasses of various compositions in the system (100−x)Li2B4O7−x(SrO-Bi2O3-Nb2O5) (where x=10, 20, 30, 40, 50 and 60, in molar ratio) were fabricated via splat quenching technique. The glassy nature of the as-quenched samples was established by differential thermal analyses. X-ray powder diffraction (XRD) and transmission electron microscopic studies confirmed the amorphous nature of the as-quenched and crystallinity in the heat-treated samples. Fluorite phase formation prior to the perovskite SrBi2Nb2O9 phase was analyzed by both the XRD and high-resolution transmission electron microscopy. Dielectric and the optical properties (transmission, optical band gap and Urbach energy) of these samples have been found to be compositional dependent. Refractive index was measured and compared with the values predicted by Wemple-Didomemenico and Gladstone-Dale relations. The glass nanocomposites comprising nanometer-sized crystallites of fluorite phase were found to be nonlinear optic active. 相似文献
994.
《Journal of separation science》2003,26(8):686-692
Two capillary columns for reversed phase (RP) capillary liquid chromatography (CLC), viz. Nucleosil 100‐5 C18 and LiChrosorb RP‐select B, were characterized by the Walters test, i.e. the chromatographic test proposed for RP stationary phases. Hydrophobicity indices were determined not only in acetonitrile/water mobile phase, as proposed in the test, but they were also measured in buffered systems. This approach was used to quantify the influence of mobile phase composition on the modification of the surface of the stationary phases. In the next step, small basic compounds differing in their hydrophobicity and basicity were selected and their retention on the stationary phases in mobile phases of the same composition as used for column testing was examined. Furthermore, the retention of newly synthesized drugs, chemotherapeutics derived from thioacridine and pyridoquinoline, differing in their structures, basicity, and hydrophobicity, was also studied. The composition of the mobile phases had to be shifted to higher contents of organic modifiers – acetonitrile or methanol – in order to elute these hydrophobic compounds from the columns. The question we wanted to answer was: How is the method for testing of reversed phases related to retention, separation efficiency, and peak symmetry of various analytes? 相似文献
995.
The solid phase extraction as a solvent-free method for the analysis of oil and grease in waters was studied. The use of
a PTFE surface as a solid phase allows the retention of the volatile fraction of oil and grease, and further analysis of carbon–hydrogen
bonds using infrared spectroscopy can be done on the surface.
Various oils and grease samples were tested: n-hexadecane, n-tetradecane, n-nonadecane, n-docosane, isooctane, diesel oil
and gasoline. Temperatures from 25° to 90 °C and a range of heating times were checked for extraction.
Precision tests showed relative standard deviation values of around 10% in several samples of the same concentration. Calibration
lines of n-hexadecane showed high correlation coefficients from 0.9 to 30 mg/l. Recoveries for the various oils using different
calibration lines showed values from 90 to 110%.
The method described here is fast and clean, and allows reproducible measurements of oil and grease in water that do not require
the use of a solvent.
Received March 1, 2001; accepted August 15, 2001; published online July 15, 2002 相似文献
996.
Wojakowska A. Krzyżak E. Wojakowski A. 《Journal of Thermal Analysis and Calorimetry》2001,65(2):491-495
The phase diagram for the RbBr–CuBr system has been determined. In the system two intermediate compounds are formed: RbCu2Br3, melting congruently at 537 K and Rb3CuBr4, melting incongruently at 544 K. The coordinates of the two eutectic points are: 501 K, 54 mole% CuBr and 522 K, 74 mole%
CuBr.
This revised version was published online in July 2006 with corrections to the Cover Date. 相似文献
997.
998.
An aniline-based polymer was electrochemically prepared and applied as a new fiber coating for solid phase microextraction (SPME) of some priority phenols from water samples. The polyaniline (PANI) film was directly electrodeposited on the platinum wire surface in sulfuric acid solution using cyclic voltammetry (CV) technique. The efficiency of new coating was investigated using a laboratory-made SPME device and gas chromatography with flame ionization detection for the extraction of some phenols from the headspace of aqueous samples. The scanning electron microscopy (SEM) images showed the homogeneity and the porous surface structure of the film. The results obtained proved the ability of this polymer as a suitable SPME fiber coating for trapping the selected phenols. Influential parameters affecting the extraction process were optimized and an extraction time of 50 min at 50 °C gave maximum efficiency, when the aqueous sample was saturated with NaCl and adjusted at pH 2. This new coating can be prepared easily in a reproducible manner and it is rather inexpensive and stable against most of organic solvents. The PANI thickness can be precisely controlled by the number of CV cycles. At the optimum conditions, the R.S.D. for a double distilled water spiked with phenol and chlorophenols at ppb level were 4.8-17% (n = 3) and detection limits for the studied compounds were between 0.69 and 3.7 ng ml−1, except for phenol and 4-chlorophenol. The optimized method was successfully applied to some real-life water samples. 相似文献
999.
Hiroshi Tanaka Tsuyoshi Hasegawa Narumi Kita Hiroko Nakahara Takahiro Shibata Sho Oe Makoto Ojika Koji Uchida Takashi Takahashi 《化学:亚洲杂志》2006,1(5):669-677
An efficient solution‐phase synthesis of rac‐15‐deoxy‐Δ12,14‐PGJ2 (15dPGJ2) derivatives that contain variable α and ω chains based on a polymer‐assisted strategy and their neurite‐outgrowth‐promoting activity are described. The strategy for the synthesis of PGJ2 derivatives involves the use of a vinyl iodide bearing cyclopentenone as a key intermediate, which undergoes Suzuki–Miyaura coupling and subsequent Lewis acid catalyzed aldol condensation for incorporation of the ω and α chains, respectively. For easy access to the PGJ2 derivatives, a polymer‐supported catalyst and scavengers were adapted for use in these four diverse steps, in which workup and purification can be performed by simple filtration of the solid‐supported reagents. By using this methodology, we succeeded in the synthesis of 16 PGJ2 derivatives with four alkyl boranes and four aldehydes. The neurite‐outgrowth‐promoting activity of the 16 synthetic compounds in PC12 cells revealed that the side‐chains play a major role in modulating their biological activity. The carboxylic acid on the α chain improved the biological activity, although it was not absolutely required. Furthermore, a PGJ2 derivative with a phenyl moiety on the ω chain was found to exhibit an activity comparable to that of natural 15dPGJ2. 相似文献
1000.
Andrés G. León Ana I. Olives M. Antonia Martín Benito del Castillo 《Journal of inclusion phenomena and macrocyclic chemistry》2007,57(1-4):577-583
The use of cyclodextrins (CDs) in HPLC as mobile phase additives provides a flexible alternative for the separation of chemically
related compounds because these separations can be performed on conventional columns and are economically advantageous over
the use of chiral stationary phases. The present paper describes the influence of the presence of β-cyclodextrin (β-CD) and
2-hydroxypropyl-β-cyclodextrin (HPβ-CD) on the separation of the β-carboline alkaloids norharmane, harmane and harmine. The
nature of the stationary phase (reverse phases C1 and C18) affects the chromatographic separations and also the stability of the inclusion complexes that are developed. The changes
in the proportion of the organic solvents at constant concentration of CDs (3 mM for β-CD and 15 mM for HPβ-CD) modify the
retention factors (k′) for all alkaloids studied. The nature of the organic solvent in the mobile phase also changes the chromatographic parameters.
The logarithm of the capacity factor (k′) is linearly increased with the proportion of water in the hydro-organic mobile phase (ethanolic or methanolic) but the
slopes obtained vary depending on the CD added to the mobile phase. The role of competitive equilibria, i.e., chromatographic
distribution and inclusion complexes formation is discussed.
This paper was presented at XIIIth International Cyclodextrin Symposium. Torino, Italy, May, 14–17, 2006 相似文献