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991.
Magnesium formate dihydrate has been synthesized by the action of formic acid on anhydrous magnesium oxide. This product analysed as Mg(COOH)2 · 2H2O. Its mode of thermal decomposition has been studied by thermal methods of analysis including simultaneous DTA/mass spectrometry. Nitrogen adsorption surface area of the solid products at various stages of its decomposition have been obtained. X-Ray diffraction and scanning electron micrographs have also been used to interpret the results. The decomposition of magnesium formate took place in three stages, which includes a phase change, at 265°C. The endotherm at 430°C changed to an exotherm in the presence of air; it corresponded to the decomposition of a new anhydrous phase of magnesium formate. The effect of the sample holder and changing atmospheres on the DSC analysis has been investigated. A scheme is presented for the thermal decomposition. 相似文献
992.
Santi Tungprapa Tanarinthorn Puangparn Monchawan Weerasombut Ittipol Jangchud Porntiva Fakum Somsak Semongkhol Chidchanok Meechaisue Pitt Supaphol 《Cellulose (London, England)》2007,14(6):563-575
This paper reports an investigation of the effects of solvent system, solution concentration, and applied electrostatic field
strength (EFS) on the morphological appearance and/or size of as-spun cellulose acetate (CA) products. The single-solvent
systems were acetone, chloroform, N,N
-dimethylformamide (DMF), dichloromethane (DCM), methanol (MeOH), formic acid, and pyridine. The mixed-solvent systems were
acetone–DMAc, chloroform–MeOH, and DCM–MeOH. Chloroform, DMF, DCM, MeOH, formic acid, and pyridine were able to dissolve CA,
forming clear solutions (at 5% w/v), but electrospinning of these solutions produced mainly discrete beads. In contrast, electrospinning of the solution of
CA in acetone produced short and beaded fibers. At the same solution concentration of 5% (w/v) electrospinning of the CA solutions was improved by addition of MeOH to either chloroform or DCM. For all the solvent systems
investigated smooth fibers were obtained from 16% (w/v) CA solutions in 1:1, 2:1, and 3:1 (v/v) acetone–DMAc, 14–20% (w/v) CA solutions in 2:1 (v/v) acetone–DMAc, and 8–12% (w/v) CA solutions in 4:1 (v/v) DCM–MeOH. For the as-spun fibers from CA solutions in acetone–DMAc the average diameter ranged between 0.14 and 0.37 μm
whereas for the fibers from solutions in DCM–MeOH it ranged between 0.48 and 1.58 μm. After submersion in distilled water
for 24 h the as-spun CA fibers swelled appreciably (i.e. from 620 to 1110%) but the physical integrity of the fibrous structure
remained intact. 相似文献
993.
T. Datta Samanta S. Laskar D. Nayak S. Lahiri 《Journal of Radioanalytical and Nuclear Chemistry》2007,273(2):323-325
Binding ability of mercury, thallium, lead and bismuth with Erythrina variegata seed protein have been investigated using tracer packet technique. Due to the lack of standard methods, inter-comparisons
have been made among three different approaches, like trichloroacetic acid (TCA) precipitation, isoelectric precipitation
and dialysis of protein after incubation with the metals. Good agreement was observed for all the cases except that of lead. 相似文献
994.
Kobayashi Y Kumar GB Kurachi T Acharya HP Yamazaki T Kitazume T 《The Journal of organic chemistry》2001,66(6):2011-2018
By using the convenient protocol for conversion of 2-substituted furans into 4-oxo-2-alkenoic acids ((i) NBS, (ii) NaClO(2)), macrosphelide B (2) was synthesized from furyl alcohol 5 (>98% ee) and acid 6 (99% ee). The protocol was first applied to the PMB ether of 5 to afford acid 13b. On the other hand, DCC condensation of acid 6 with 5 gave 16 after deprotection of the TBS group. Condensation was again carried out between 13b and 16 to furnish the key ketone 17, which upon reduction with Zn(BH(4))(2) afforded anti alcohol 18 stereoselectively (15:1). After protection/deprotection steps, the furan 18 was converted to seco acid 3 by using the furan oxidation protocol mentioned above, and lactonization of 3 with Cl(3)C(6)H(2)COCl, Et(3)N, and DMAP afforded 22 (MOM ether of 2), which upon deprotection with TFA produced 2. Transformation of 22 to macrosphelide A (1) was then investigated. Although the chelation-controlled reduction of 22 should afford the desired anti alcohol 24, Zn(BH(4))(2) at <-90 degrees C gave a 2 approximately 1:1 mixture of anti/syn alcohols. On the contrary, reduction with NaBH(4) in MeOH at -15 degrees C produced the syn isomer 23 with >10:1 diastereoselectivity. Mitsunobu inversion of the resulting C(14)-hydroxyl group and deprotection of the MOM group with TFA afforded 1. Similarly, reduction of 2 with NaBH(4) afforded the C(14)-epimer of 1 stereoselectively. The observed stereoselectivity in the reductions of 22 and 2 could be explained on the basis of computer-assisted calculation, which showed presence of the low-energy conformers responsible for the stereoselective reduction. In addition, conversion of 2 to 1 was established, for the first time. 相似文献
995.
Gupta D Roitzsch M Lippert B 《Chemistry (Weinheim an der Bergstrasse, Germany)》2005,11(22):6643-6652
Isocytosine (ICH; 1) exists in solution in an equilibrium of tautomers 1a and 1b with the N1 and N3 positions carrying the acidic proton, respectively. In the solid state, both tautomers coexist in a 1:1 ratio. As we show, the N3H tautomer 1b can selectively be crystallized in the presence of the model nucleobase 1-methylcytosine (1-MeC). The complex 1b x (1-MeC)2 x H2O (2) forms pairs through three hydrogen bonds between the components; hydrogen bonds between identical molecules are also formed, leading to an infinite tape structure. On the other hand, the N1H tautomer 1a co-crystallizes with protonated ICH to give [1a x ICH2]NO3 (3), again with three hydrogen bonds between the partners, yet the acidic proton is disordered over the two entities. With M(II)(dien) (M=Pt, Pd; dien=diethylenetriamine) preferential coordination of tautomer 1a through the N3 position is observed. DFT calculations, which were also extended to Pt(II)(tmeda) linkage isomers (tmeda=N,N,N',N'-tetramethylethylenediamine), suggest that intramolecular hydrogen bonding between the ICH tautomers and the co-ligands at M, while adding to the preference for N3 coordination, is not the major determining factor. Rather it is the inherently stronger Pt-N3 bond which favors complexation of 1a. With an excess of M(II)(dien), dinuclear species [M2(dien)2(IC-N1,N3)]3+ (M=Pd(II), 4 and Pt(II), 5) also form and were isolated as their ClO4(-) salts and structurally characterized. In strongly acidic medium 5 is converted to [Pt(dien)(ICH-N1)]2+ (6), that is, to the Pt(II) complex of tautomer 1b. 相似文献
996.
The various thermodynamic parameters for the periodate oxidation of six anilines, viz. aniline, p-chloroaniline, p-ethoxyaniline, o- and p-methoxyanilines and p-methylaniline have been reported and discussed. The validity of the isokinetic relationship and various linear free energy relationships (LFERs) have been tested and discussed. An attempt has been made to correlate these findings with the mechanism operative in these reactions. 相似文献
997.
Oxide ceramic masses react to simple shearing with hardening (peptisation: increase in the shear stress with the shear deformation).
In the present study the correlation between the increase in the shear stress and the porosity, agglomeration processes and
the type of flow are analysed. For this purpose oxide ceramic masses are tested in a shear device especially developed for
pastes and analysed by rheometric experiments, NMR methods and particle size analysis. The results support the hypothesis
that structural changes (hardening, increase in the mean porosity) of the material during the peptisation mainly depend on
the magnitude and not on the kind of the energy input and thus of the type of flow. The fraction of bound (more generally,
the immobilised) water increases with the shear displacement. Also crushing of primary particles could be observed. Both the
crushing of solid particles causing an increased solid surface and the formation of a three-dimensional gel structure are
microscopic effects capable of resulting in the binding or retaining water. On a macroscopic scale these phenomena cause hardening.
Magnetic resonance imaging visualises flow-induced agglomerates, which form owing to the shear flow and increase the porosity
averaged over the whole sample. After the shear experiment rolls of paste can be seen which indicate that the general assumption
of a plane shear flow in the shear device is not warrantable.
Received: 19 July 2001 Accepted: 25 October 2001 相似文献
998.
A method is described to impart flexibility and mechanical strength to conducting polyaniline by polymerizing aniline on fabrics and on cellulose papers. The study indicates that these conducting fabrics offer 16–18 dB of shielding effectiveness for the control of electromagnetic interference (EMI) up to a frequency of 103 MHz. 相似文献
999.
THE PHOTOREACTIVITY OF PYRIMIDINE-PURINE SEQUENCES IN SOME DEOXYDINUCLEOSIDE MONOPHOSPHATES AND ALTERNATING DNA COPOLYMERS 总被引:2,自引:0,他引:2
Abstract— A reversed-phase HPLC system has been developed which separates the common nucleo-bases from the 6-methylimidazo[4,5- b ]pyridin-5-one (6-MIP) produced on acid hydrolysis of a thymine-adenine photoadduct (TA*) that is formed between adjacent thymine and adenine bases in UV-irradiated polydeoxyribonucleotides. By measuring the relative amounts of adenine and 6-MIP in acid hydrolysates, this system has been used to investigate how polynucleotide conformation affects the yield of TA* in poly(dA-dT) irradiated at 254 nm. The photoreactivity of other pyrimidine-purine sequences has been examined with the deoxydinucleoside monophosphates d(TpI) and d(m5 CpA) and with the alternating DNA copolymers poly(dA-dU), poly(dI-dC), poly(dG-dC) and poly(dA-dC).poly(dG-dT). Samples were irradiated at 254 nm in aqueous solution and in ice, and at wavelengths >290 nm with acetone as photosensitizer. A photoproduct resembling TA*, and giving 6-MIP on acid hydrolysis, was isolated from d(TpI) irradiated at 254 nm in solution or in ice; d(m5 CpA) was comparatively unreactive. Acid hydrolysates of the irradiated DNA copolymers were screened by HPLC and by TLC and paper electrophoresis, for the presence of imidazo[4,5- b ]pyridin-5-one, 6-MIP, or other species attributable to specific photoproduct formation. By this criterion, however, none of the copolymers showed evidence of significant photoreactivity in either their single- or double-stranded conformational states. The formation of mixed pyrimidine-purine photoadducts in DNA is therefore probably restricted to T-A doublets. 相似文献
1000.
Equations between the differential order and the maximum of the fractional-order differential for the specified peak signals are developed based on the variation of the maximum of the specified peak signals at different orders. Also, equations between the differential order and the zero-crossing of the fractional-order differential of the specified peak signals are proposed according to the variation of the zero-crossing of the specified peak signals at different orders. Characteristic paramters of the Gaus- sian peak, Lorentzian peak, and Tsallis peak can be estimated using estimator I and estimator II which are obtained by the equations above. As a result, a new method is presented to resolve the overlapped peaks signal. Firstly, a fractional-order differential of the specified peak signals is obtained with the fractional-order differentiation filter. Then, characteristic paramters of the specified peak signals can be extracted using estimator I and estimator II. Finally, the Tsallis peak is used as a model to assign the overlapping peak signals correctly. Experimental results show that the proposed method is efficient and effective for the simulated overlapping peaks and detected overlapping voltammetric peak signals. 相似文献