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81.
Syed Laik Ali 《Analytical and bioanalytical chemistry》1973,262(4):278-282
The different aspects of Vitamin D3 determination and the data reported in the literature are discussed. The spectrophotometric determination of Vitamin D3 in cod-liver oil is carried out after the alkaline saponification, extraction of unsaponified parts, precipitation of accompanying sterols and the column- and thin-layer chromatographic purification and separation of vitamin D3 on 40 cm plates from other vitamins. The dyestuff α-naphtholbenzein is suited well as standard substance for the better location and identification of vitamin D3 zone on the thin-layer plate. The results obtained from the chemical method were checked through the simultaneous biological determination. 相似文献
82.
A novel 3D polymeric heteropolynuclear sodium(I) lead(II) complex containing different ligands, [NaPb(ClO4)(en)(NO2)2] was synthesized and characterized by elemental analysis and IR, and 1H‐, 13C‐, and 207Pb‐NMR spectroscopy. The single‐crystal X‐ray data of [NaPb(ClO4)(en)(NO2)2]n established that the complex is a three‐dimensional polymer, [(en)Pb(μ3‐ONO)2Na(μ3‐ONO)2Na(μ‐O2ClO2)Na]n. The Pb and Na atoms have four‐ and eight‐coordinate geometry, respectively. The lone pair of electrons at the PbII atom is ‘stereochemically active’. 相似文献
83.
Brahim Lakhrissi Mohamed Massoui El Mokhtar Essassi Vincent Lequart Nicolas Joly Patrick Martin Grard Goethals 《Journal of heterocyclic chemistry》2004,41(6):1011-1014
Reaction of 1,5‐benzodiazepin‐2,4‐dione with 3‐O‐substituted‐5,6‐anhydro‐1,2‐isopropylidene‐α‐D‐glucofuranose gave the unexpected N,N'‐di‐glucofuranosyl benzimidazol‐2‐one by a novel rearrangement and ring closure reaction. A mechanism is proposed. 相似文献
84.
Enhancing the enzymatic hydrolysis of cellulosic materials using simultaneous ball milling 总被引:1,自引:0,他引:1
Mais Ursula Esteghlalian Ali R. Saddler John N. Mansfield Shawn D. 《Applied biochemistry and biotechnology》2002,98(1-9):815-832
One of the limiting factors restricting the effective and efficient bioconversion of softwood-derived lignocellulosic residues
is the recalcitrance of the substrate following pretreatment. Consequently, the ensuing enzymatic process requires relatively
high enzyme loadings to produce monomeric carbohydrates that are readily fermentable by ethanologenic microorganisms. In an
attempt to circumvent the need for larger enzyme loadings, a simultaneous physical and enzymatic hydrolysis treatment was
evaluated. A ball-mill reactor was used as the digestion vessel, and the extent and rate of hydrolysis were monitored. Concurrently,
enzyme adsorption profiles and the rate of conversion during the course of hydrolysis were monitored. α-Cellulose, employed
as a model substrate, and SO2-impregnated steam-exploded Douglas-fir wood chips were assessed as the cellulosic substrates. The softwood-derived substrate
was further posttreated with water and hot alkaline hydrogen peroxide to remove >90% of the original lignin. Experiments at
different reaction conditions were evaluated, including substrate concentration, enzyme loading, reaction volumes, and number
of ball beads employed during mechanical milling. It was apparent that the best conditions for the enzymatic hydrolysis of
α-cellulose were attained using a higher number of beads, while the presence of air-liquid interface did not seem to affect
the rate of saccharification. Similarly, when employing the lignocellulosic substrate, up to 100% hydrolysis could be achieved
with a minimum enzyme loading (10 filter paper units/g of cellulose), at lower substrate concentrations and with a greater
number of reaction beads during milling. It was apparent that the combined strategy of simultaneous ball milling and enzymatic
hydrolysis could improve the rate of saccharification and/or reduce the enzyme loading required to attain total hydrolysis
of the carbohydrate moieties. 相似文献
85.
Bakhsh M. Majid R. El-Awady Abbas A. Khalifa Mohamed A. 《Transition Metal Chemistry》2000,25(1):52-59
Kinetic studies of ligand substitutions of the six-coordinated RuII pseudo-macrocyclic complex [Ru(CHDH)2- (PPh3)2] (CHDH=cyclohexanedione-dioximato) have been spectrophotometrically investigated in a variety of solvents and at 70, 80, 85 and 90°C. The reactions studied are of the form:[(PPh3)Ru(CHDH)2(PPh3)] + L =[(PPh3)Ru(CHDH)2L] + PPH3
where L is imidazole, pyridine, piperidine or thiophene or a solvent molecule (PhCl, PhMe, MeCN, DMSO or DMF). The solvolysis reactions with chlorobenzene and toluene proceed to an equilibrium position favoring the bis-triphenylphosphine complex. All other reactions proceed to completion. From a mechanistic point of view the reactions were found to proceed through the formation of a five coordinate intermediate that possesses little or no discriminating ability towards the incoming nucleophiles. The rate data were thus interpreted in terms of a dissociative (D) or dissociative interchange (Id) mechanism. Activation parameters H and S are reported. Preliminary studies on the solvatochromic behavior of [Ru(CHDH)2(PPh3)2] and the corresponding mixed complexes are discussed. 相似文献
86.
R. Abu-Eittah Maher M. Hamed A. A. Mohamed 《International journal of quantum chemistry》1991,39(2):211-226
The electronic absorption spectra of 2-, 3-, and 4-vinylpyridines and 1,2-(2,3-dipyridyl), 1,2-(2,4-dipyridyl), 1,2-(3,4-dipyridyl), and 1,2-(4,4-dipyridyl) ethylenes have been investigated in polar and nonpolar solvents. A correlation has been made between the geometry of the molecule and the observed spectrum. Molecular orbital calculations have been carried out using the INDO/S? CI procedure and a limited geometry optimization. The solvent effect at the MO level has been calculated. MO calculations predicted the existence of nπ* transitions that were not observed experimentally. The wave functions of the different CI states were calculated. The experimental transition energy as well as oscillator strength corresponded satisfactorily with the calculated ones. The observed transitions were assigned according to the results of MO calculations. 相似文献
87.
Combination of an ultrasonic nebulizer and plasma excitation sources for spectrochemical analysis offers desirable features of low detection limits, high sample throughput, wide dynamic range of operation, acceptable precision and accuracy, and simultaneous quantitative analytical capabilities. Moreover, the ultrasonic nebulizer does not require sample preconcentration. Recently we have developed a three-phase plasma arc (TPPA) for atomic emission spectrochemical analysis. In the present work, to increase the analytical utility of the three-phase plasma system, an ultrasonic nebulizer was used for sample introduction. The effects of the argon gas flow rate, current, excitation temperature have been studied. The analytical calibration curves are obtained for Ca, Cr, Fe, Mg and Mn, and detection limits have been calculated. The present technique is used to determine the concentration of the elements Ca, Cr, Fe, Mg and Mn in airborne samples. 相似文献
88.
The conversion of amorphous tricalcium phosphate with different hydration ratio into apatite in water at 25 °C has been studied by microcalorimetry and several physical-chemical methods. The hydrolytic transformation was dominated by two strong exothermic events. A fast, relatively weak, wetting process and a very slow but strong heat release assigned to a slow internal rehydration and the crystallization of the amorphous phase into an apatite. The exothermic phenomenon related to the rehydration exceeded the crystalline transformation enthalpy. Rehydration occurred before the conversion of the amorphous phase into apatite and determined the advancement of the hydrolytic reaction. The apatitic phases formed evolved slightly with time after their formation. The crystallinity increased whereas the amount of HPO42− ion decreased. These data allow a better understanding of the behavior of biomaterials involving amorphous phases such as hydroxyapatite plasma-sprayed coatings. 相似文献
89.
Two new coordination polymers of PbII complexes with bridging 4,4′‐[(1E)‐ethane‐1,2‐diyl]bis[pyridine] (ebp), thiocyanato, and acetato ligands, [Pb(μ‐SCN)2(μ‐ebp)1.5]n ( 1 ) and {[Pb(μ‐OAc)(μ‐ebp)](ClO4)}n ( 2 ), were synthesized and characterized by elemental analysis, FT‐IR, 1H‐ and 13C‐NMR, thermal analysis, and single‐crystal X‐ray diffraction. In 1 , the Pb2+ ions are doubly bridged by both the ebp and the SCN− ligands into a two‐dimensional polymeric network. The seven‐coordinate geometry around the Pb2+ ion in 1 is a distorted monocapped trigonal prism, in which the Pb2+ ions have a less‐common holodirected geometry. In 2 , the Pb2+ ions are bridged by AcO− ligands forming linear chains, which are also further bridged by the neutral ebp ligands into a two‐dimensional polymeric framework. The Pb2+ ions have a five‐coordinate geometry with two N‐atoms from two ebp ligands and three O‐atoms of AcO−. Although ClO acts as a counter‐ion, it also makes weak interactions with the Pb2+ center. The arrangement of the ligands in 2 exhibits hemidirected geometry, and the coordination gap around the Pb2+ ion is possibly occupied by a configurationally active lone pair of electrons. 相似文献
90.
Mohamed S. A. El‐Gaby Ahmed M. Sh El‐Sharief Ahmed A. Atalla Abu‐Bakr A. A. M. El‐Adasy 《中国化学会会志》2004,51(2):327-333
The novel cyanothioformamides 2a‐d were prepared by treatment of isothiocyanatosulfonamides 1a‐d with potassium cyanide at room temperature. Cyclocondensation of compounds 2b,c with phenyl isocyanate as electrophile furnished the corresponding imidazolidines 3a,b . The reactivity of compound 3a towards some nitrogen nucleophiles was investigated. Thus, the thiosemicarbazone 4 and imidazo[4,5‐b]quinoxaline 6 were synthesized by condensation of compound 3a with thiosemicarbazide and o‐phenylenediamine, respectively. Treatment of 3a with hydrochloric acid afforded compound 7 . Our investigation was extended to include the reactivity of cyanothioformamide 2 towards o‐aminophenol, anthranilic acid, and o‐phenylenediamine and yielded the corresponding heterocycles 9 , 11 and 13 derivatives, respectively. Structures of the synthesized compounds were established by their elemental analysis and spectral data. 相似文献