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61.
A new capillary electrophoresis procedure based on micellar electrokinetic capillary chromatography for the separation of humic acids (HAs) isolated from Antarctica soil was developed. The HAs were separated and characterized using a background electrolyte containing 0.09 M borate+0.09 M Tris+0.001 M EDTA (BTE) of pH 8.3, modified with alpha-, beta-, or gamma-cyclodextrins (CDs) and sodium dodecyl sulfate. It was found that from alkaline solution of HAs in the presence of CDs, the HAs are not completely precipitated with a strong acid and a certain part (some fractions) remains soluble. Mass spectrometry shows that HAs contain 15-25 simple low-Mr compounds and several families of compounds with similar structure (m/z approximately 800-1200). Comparison of HA analysis from Antarctica soil with those of soil HAs from the American continent show a high similarity between the samples and confirm several identical compounds and some with very similar structural units. 相似文献
62.
Polysulfonyl Amines. LXXII. Triphenylcarbenium and Triphenylphosphonium Di(fluorosulfonyl)amides: Two Crystal Structures with Ordered (FSO2)2N? Sites Treatment of HN(SO2F)2 in CH2Cl2 with Ph3P, Ph3PO or collidine (=B) affords the compounds Ph3PH⊕[(FSO2)2N]? ( 3 ), Ph3PO · HN(SO2F)2, and BH⊕[(FSO2)2N]? ( 7 ). The carbenium salt Ph3C⊕[(FSO2)2N]? ( 5 ), obtained by metathesis of Ph3CBr with [(C6H6)AgN(SO2F)2] in CH2Cl2, crystallizes from chloroform/petroleum ether as a monosolvate Ph3C⊕[(FSO2)2N]? · CHCl3 ( 6 ). In presence of a sterically hindered base, viz. collidine, 5 is a suitable reagent for the tritylation of molecules containing weakly activated H atoms (e. g.: MeCN → Ph3CCH2CN, acetone → tritylacetone; co-product: 7 ). The crystal structures of the ionic solids 3 (monoclinic, space group P21/n) and 6 (monoclinic, P21/c) were determined by X-ray diffraction at ?130°C; the structure refinements were not impaired by the notorious tendency of the (FSO2)2N moiety towards crystallographic disorder. As in the known structure of the tetraphenylarsonium salt, the anion of 3 and 6 adopts a staggered conformation of approximately C2 symmetry (averages of all values: S? N? S 121.4°, N? S 156.2, S? O 141.6, S? F 156.6 pm). The crystal packing of 6 displays a three-centre C? H(…?O)2 hydrogen bond between the CHCl3 molecule and two oxygen atoms of a single anion, resulting in a six-membered ring [R12(6) pattern; H …? O 234 and 262 pm]. The crystal of 3 contains one-dimensional arrays of alternating cations and anions connected by a three-centre P? H(…?O)2 bond [C(6) pattern; H …? O 237 and 254 pm]. The Ph3C⊕ cation of 6 is propeller-shaped, with three coplanar central bonds (mean C? C 144.5 pm) and interplanar angles of 52.7, 56.4 and 60.1° between the phenyl groups. 相似文献
63.
64.
Dietger Leyendecker Dagmar Leyendecker F. P. Schmitz E. Klesper 《Journal of separation science》1987,10(3):141-144
The dependence of the selectivity α and the effective plate number, N, on temperature and pressure is shown in three-dimensional diagrams. The specific system studied was pentane as the mobile phase, unmodified silica as the stationary phase, and a set of four polycyclic hydrocarbons as the test mixture. Temperature and pressure ranges were from 25 to 300°C and from 30 to 75 bar, respectively. The plots for α and N are found to resemble those for capacity ratio, k′, and resolution, R, studied earlier with the same system [1]. A distinct maximum is observed for N in the supercritical region, as found earlier for k′ and R. This applies also to α for the homologous substrate pair naphthalene/anthracene, while the resemblance for α is less pronounced for the pair anthracene/pyrene. 相似文献
65.
Bernhard Wielage Siegfried Steinhäuser Dagmar Dietrich Thomas Lampke Gudrun Fritsche 《Mikrochimica acta》2006,156(1-2):83-87
Zinc and zinc calcium phosphate coatings on steel were formed by dipping in commercial baths. A surface activation with titanium
phosphate influences not only the film morphology but also the composition of the conversion films. Qualitative phase analysis
of the polycrystalline deposits reveals a typical phosphophyllite crystal growth apart from hopeite and scholzite respectively.
The growth rate depends on the free surface of the steel; the contact area to the solution controls the rate of iron pickling. 相似文献
66.
Jiří Plíšek Lenka Kujovská Krčmová Jana Aufartová Tanausú V. Morales Sarah M. Esponda Roman Oros Eva Kasalová Jose J. Santana‐Rodriguez Luboš Sobotka Petr Solich Dagmar Solichová 《Journal of separation science》2013,36(23):3702-3708
Biomarkers, 25‐hydroxyvitamin D3 and 25‐hydroxyvitamin D2, are important indicators of the vitamin D general status and are monitored in several pathophysiological disorders, such as osteoporosis, diabetes, heart disease, etc. A novel ultra‐HPLC with MS/MS methodology for the analysis of 25‐hydroxyvitamin D derivatives coupled with a very simple and highly rapid sample preparation step was developed. Analytical parameters obtained showed linearity (R2) above 0.999 for both vitamins with accuracies between 95.8 and 102%. The LODs were as low as 0.22 and 0.67 nmol/L for 25‐hydroxyvitamin D3 and 25‐hydroxyvitamin D2, respectively. Intra‐assay precision (%RSD) was lower than 4.5%, and inter‐assay precision (%RSD) was lower than 6.5%. The feasibility of the developed methodology to be applied in clinical routine analysis has been proved by its application in blood samples from non‐agenarian patients, patients with familial hypercholesterolemia and patients suffering from age‐related macular degeneration. 相似文献
67.
68.
69.
Salis A Pinna MC Bilanicová D Monduzzi M Lo Nostro P Ninham BW 《The journal of physical chemistry. B》2006,110(6):2949-2956
The effect of electrolytes on pH measurements via glass electrodes is explored with solutions buffered at pH 7 (phosphate and cacodylate). Salt and buffer concentrations are varied. Direct and reverse Hofmeister effects are observed. The phenomena are significant for salt concentrations above 0.1 M and for buffer concentrations below 20 mM. Changes in measured pH show up most strongly with anions. They can be related to the usual physicochemical parameters (anion molar volumes, molar refractivity, and surface tensions) that are characteristic of Hofmeister series. They correlate strongly with anionic excess polarizabilities; this suggests the involvement of non-electrostatic, or dispersion, forces acting on ions. These forces contribute to ionic adsorption at the glass electrode surface, and to the liquid junction potential. 相似文献
70.
Dagmar C. Kapeller 《Tetrahedron》2010,66(3):591-598
The synthesis and testing of configurational stability of chirally monodeuterated PMB- and THP-substituted oxymethyllithiums are described. Macroscopically they are configurationally stable up to −35 °C, the limit of their chemical stability, and microscopically even up to 0 °C. Furthermore, THP-protected oxy-[D1]methyllithium has been applied in the formal synthesis of (6R)-[6-D1]-d-glucose (four steps, 40% yield), an example of its use as a homochiral hydroxymethyl synthon. 相似文献