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111.
Ethylene diamine (EDA)/salt solvent systems can dissolve cellulose without any pretreatment. A comparison of the electrical
conductivity of different salts in EDA was made at 25 °C, and conductivity decreased in the order of KSCN>KI>NaSCN at the
same molar concentration. Among the salts tested, potassium thiocyanate (KSCN) was capable of dissolving both high molecular
weight (DP>1000) and low molecular weight (DP = 210) cellulose, and this was confirmed by polarized light microscopy. 39K and 14N NMR experiments were conducted at 70 °C as a function of cellobiose concentration with EDA/KSCN as the solvent. The results
showed that the K+ ion interacts with cellobiose more than the SCN− ion does. Recovered cellulose was studied by infrared spectroscopy (FTIR) and wide angle X-ray diffraction (WAXD). Changes
in the FTIR absorption bands at 1,430 and 1,317 cm−1 were associated with a change in the conformation of the C-6CH2OH group. The changes in positions and/or intensities of absorption bands at 2,900, 1,163, and 8,97cm−1 were related to the breaking of hydrogen bonds in cellulose. X-ray diffraction studies revealed that cellulose, recovered
by precipitating cellulose solutions with water, underwent a polymorphic transformation from cellulose I to cellulose II. 相似文献
112.
E. Yu. Nesterova M. V. Voevudsky A. V. Samukha R. I. Zubatyuk O. V. Shishkin 《Chemistry of Heterocyclic Compounds》2005,41(12):1511-1520
Acylation of 3-ethoxycarbonyl-2,6-dimethyl-5-pyridinecarboxylic acid hydrazide and 2,6-dimethyl-3,5-pyridinedicarboxylic acid
dihydrazide using aromatic acid chlorides gave the corresponding N-aroyl hydrazides. It was found that the hydrazinolysis
of 3-ethoxycarbonyl-2,6-dimethyl-5-pyridinedicarboxylic acid N-aroyl hydrazides occurred not at the ester group but as a rehydrazinolysis
reaction at the dihydrazide fragment.
__________
Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 12, pp. 1834–1845, December, 2005. 相似文献
113.
Naumov P. Jordanovska V. Boyanov B. Jovanovski G. 《Journal of Thermal Analysis and Calorimetry》2001,66(2):469-477
The complexes [M(HIm)4(H2O)2](sac)2 (M=Co, Ni) and [Cd(HIm)2(sac)2]2 with saccharin (sac) and imidazole (HIm) were synthesized and their thermal (TG, DTG and DTA) behaviour in the interval from
room temperature up to 1000°C in a static air atmosphere was investigated. Irrespectively of whether the deprotonated saccharinato
residues are present as ligands or ions or both as ligands and ions, the anhydrous complexes regularly decompose in two stages.
The thermal data of 16 saccharinato complexes (including the title compounds) were correlated with the respective structural
data. The general thermal stability order of the saccharinato complexes can be represented as: Pb(II)<Zn(II)<Co(II)Ni(II)<Cd(II)
(the stability of the Cu saccharinates depends on the particular compound) and is dictated by
several structural factors, e.g. metal ionic radii, participation of the water in the coordination sphere of the metal and
other structural characteristics.
This revised version was published online in August 2006 with corrections to the Cover Date. 相似文献
114.
Convenient synthesis of 7-aryl-3,4,5,6-tetrahydro-2H-pyrido[4,5-b]- and [2,3-b]-1,5-oxazocine-6-ones
Shigeki Seto 《Tetrahedron letters》2004,45(46):8475-8478
A convenient and diversity-oriented method for synthesis of the novel 7-aryl-3,4,5,6-tetrahydro-2H-pyrido[4,5-b]-1,5-oxazocine-6-one skeleton 1 and the very rarely described 7-aryl-3,4,5,6-tetrahydro-2H-pyrido[2,3-b]-1,5-oxazocine-6-one skeleton 2, featuring cyclization using nucleophilic aromatic substitution (SNAr) and Suzuki coupling, is described. 相似文献
115.
Summary An on-line combination of liquid chromatography, gas chromatography and mass spectrometry has been realized by coupling a quadrupole mass spectrometer to an LC-GC apparatus. Liquid chromatography was used for sample pretreatment of oil samples of different origin. The appropriate LC fraction, containing polycyclic aromatic hydrocarbons, was transferred to the gas chromatograph using a loop-type interface. After solvent evaporation through the solvent vapour exit and subsequent GC separation, the compounds were introduced into the mass spectrometer for detection and identification. The GC column was connected to a short piece of deactivated fused silica that protruded into the ion source. The total analytical set-up allowed the direct analysis of oil samples after dilution in n-pentane without any sample clean-up. Detection limits are about 40 pg in the full scan mode and about 1 pg with selective ion monitoring, i.e. 20 ppb and 0.5 ppb respectively. 相似文献
116.
Summary A pure silica gel (Pia Seed 5S-60-SIL), synthesized by the hydrolysis of pure tetraethoxysilane [Si(OCH2CH3)4], was applied as a cation-exchange stationary phase in ion chromatography with indirect photometric detection for common
mono-and divalent cations (Li+, Na+, NH4
+, K+, Mg2+, and Ca2+) using various protonated aromatic monoamines (tyramine [4-(2-aminethyl) phenol], benzylamine, phenylethylamine, 2-methylpyridine
and 2,6-dimethylpyridine) as eluet ions. When using 0.75 mM tyramine-0.25 mM oxalic acid-1.5 mM 18-crown-6 (1,4,7,10,13,16-hexaoxacyclooctadecane)
at pH 5.0 as the eluent, excellent simultaneous separation and highly sensitive detection at 275 nm for these mono-and divalent
cations were achieved on the Pia Seed 5S-60-SIL column (150×4.6 mm I.D.) in 20 min. 相似文献
117.
The kinetics of mesophase formation of a lyotropic aromatic polyamide from isotropic state has been studied by means of depolarized light intensity. Avrami type analysis of the data gives an exponent close to 1, which suggests the nucleation followed by one-dimensional growth. No influence of blending flexible chain from nylon 6 to the aromatic polyamide on the kinetics of mesophase formation was observed. 相似文献
118.
119.
Summary A method has been developed for the determination of trace levels of 32 pesticides, 19 explosives and 16 polycyclic aromatic
hydrocarbons (PAH) in water in three individual steps. Solid-phase enrichment (SPE) is coupled to high-performance liquid
chromatography (HPLC) with a fully automated system. The organic pollutants are enriched on reusable cartridges packed with
adsorbent materials: pesticides and explosives on a mixed bed of divinylbenzene-ethylvinylbenzene copolymers (LiChrolut EN?) and perfluorinated polyethylene (PolyF?), and polycyclic aromatic hydrocarbons on C18-modified silica (Zorbax? ODS1). Thermally assisted desorption (TAD) has been shown to increase the recovery of analytes significantly. As all enriched
analytes are transferred to the detector, only fifty millilitres of sample is needed for each single on-line analysis, compared
with at least a litre for conventional methods. The separation of the enriched organic analytes is performed on specialized
HPLC columns based on reversed-phase materials. The limits of detection of the system employed were found to be below 100
ng L−1. Use of fluorescence detection for the polycyclic aromatic hydrocarbons resulted in limits of detection in the upper pg L−1 range. Thek values, number of theoretical plates, the recovery rates and the limits of detection of this method for fast screening of
organic pollutants from three fifty-millilitre aqueous samples are described.
Presented at the 21st ISC held in Stuttgart, Germany, 15th–20th September, 1996 相似文献
120.
Equimolar mixtures of aromatic aldehydes with thioglycolic acid and thiosemicarbazide in H2SO4 transform into 2-amino-5-aryl-5H-thiazolo[4,3-b]-1,3,4-thiadiazoles.Translated fromIzvestiya Akademioi Nauk. Seriya Khimicheskaya, No. 3, pp. 763–764, March, 1996. 相似文献