Crystallographic and electrochemical properties of ball-milled quasicrystalline Ti45Zr35Ni17Cu3 alloy with 20 mass% Ni

Icosahedral quasicrystalline Ti45Zr35Ni17Cu3 alloy powder was ball-milled with 20 mass% Ni, and the effect of the ball-milling time (t) on crystallographic and electrochemical characteristics were investigated. The amounts of icosahedral quasicrystalline and Ni phases decreased when ball-milling time increased from 30 to 180 min. The powder consisted of amorphous and (Ni and Ti) phases after 360 min of ball-milling. The maximum discharge capacity of the powder electrodes first increased from 89 (t = 0 min) to 192 mAh g(-1) (t = 180 min), and then decreased to 138 mAh g(-1) (t = 360 min). The high-rate dischargeability and the discharge capacity after 15 cycles increased with increasing ball-milling time.

Microstructures and tensile properties of Mg-8Gd-0.6Zr-xNd-yY (x+y=3, mass%) alloys

Mg-8Gd-0.6Zr-xNd-yY (mass%) alloys which containing different Nd:Y mass ratio of 3:0, 2:1, 1:2 and 0:3 with a constant x + y = 3 were prepared by metal mould casting method, and the microstructure, aging behaviour and tensile properties have been investigated. The fibrous eutectic areas along the boundaries enlarge clearly in the as-cast alloys containing Y element, and the fine grain boundaries and dispersed precipitation are observed in the aged alloys. The Mg-8Gd-0.6Zr-2Nd-Y alloy exhibits notably age-hardening behaviour and the highest mechanical property. The ultimate tensile strength and yield strength of Mg-8Gd-0.6Zr-2Nd-Y alloy in the peak aged hardness are 293 and 221 MPa at room temperature, 248 and 191 MPa at 230 degrees C. The improvement of age-hardening response and tensile properties is mainly attributed to the quadrate-like stable Mg5RE precipitate, which forms readily and orderly in aged Mg-8Gd-0.6Zr-2Nd-Y alloy.

Structure identification of a prenylflavonol glycoside from Epimedium koreanum by electrospray ionization tandem mass spectrometry

A novel prenylflavonol glycoside, named acetylicariin, has been isolated from the aerial parts of Epimedium koreanum Nakai. The structure has been identified by electrospray ionization multi-stage tandem mass spectrometry (ESI-MSn) and other chemical evidence, which has been elucidated as 8-prenylkaempferol-4'-methoxyl-3-O-alpha-L-rhamnopyranosyl-7-O-beta-D-(2''-O-acetyl)glucopyranoside.

Mass transfer kinetics of yttrium(III) using a constant interfacial cell with laminar flow. Part II. Extraction with Cyanex 272

The yttrium(III) extraction kinetics and mechanism with bis-(2,4,4-trimethyl-pentyl) phosphinic acid (Cyanex 272, HA) dissolved in heptane have been investigated by constant interfacial cell with laminar flow. The data has been analyzed in terms of pseudo-first order constants. Studies on the effects of stirring rate, temperature, acidity in aqueous phase, and extractant concentration on the extraction rate show that the extraction regime is dependent on the extraction conditions. The plot of interfacial area on the rate has shown a linear relationship. This fact together with the strong surface activity of Cyanex 272 at heptane-water interfaces has made the interface the most probable location for the chemical reactions. The forward, reverse rate equations and extraction rate constant for the yttrium extraction with Cyanex 272 have been obtained under the experimental conditions. The rate-determining step has been also predicted from interfacial reaction models. The predictions have been found to be in good agreement with the rate equations obtained from experimental data, confirming the basic assumption that the chemical reaction is located at the liquid-liquid interface.

Mass transfer kinetics of yttriium(III) using a constant interfacial cell with laminar flow. Part I. Extraction with Cyanex 302

The interfacial tension is measured for Cyanex 302 in heptane and adsorption parameters are calculated according to Gibbs equation and Szyskowski isotherm. The results indicate that Cyanex 302 has a high interfacial activity, allowing easy extraction reaction to take place at the liquid-liquid interface. The extraction kinetics of yttrium(III) with Cyanex 302 in heptane are investigated by a constant interfacial cell with laminar flow. The effects of stirring rate, temperature and specific interfacial area on the extraction rate are discussed. The results suggest that the extraction kinetics is a mixed regime with film diffusion and an aqueous one-step chemical reaction proposed to be the rate-controlling step. Assuming the mass transfer process can be formally treated as a pseudo-first-order reversible reaction with respect to the metal cation, the rate equation for the extraction reaction of yttrium(III) with Cyanex 302 at pH <5 is obtained as follows:R-f = 10(-7.85)[Y(OH)(2)(+)]((a))[H(2)A(2)]((o))(1.00)[H+]((a))(-1.00)Diffusion parameters and rate constants are calculated through approximate solutions of the flux equation.

Analysis of norditerpenoid alkaloids extracted from Aconitum sinomantanum Nakai by electrospray ionization tandem mass spectrometry

Electrospray ionization mass spectrometry (ESI-MS) was applied simultaneously in determining norditerpenoid alkaloids from the roots of Aconitum sinomantanum Nakai ( RAS) based on molecular mass information. The tandem mass spectra (ESI-MSn) provided the alkaloidal structural information, through which the existence of these alkaloids was further confirmed. Accordingly, six known norditerpenoid alkaloids were simultaneously determined on the basis of their ESI-MSn spectra. Furthermore, based on the diagnostic fragmentation pathways of alkaloidal MSn, a rapid method for direct detection and characterization of alkaloids from an ethanolic extract of RAS was described.

Detection and characterization of non-covalent complex between lappaconitine and beta-cyclodextrin by electrospray ionization tandem mass spectrometry

The non-covalent complexes between lappaconitine (LA) and beta-cyclodextrin (beta-CD) have been detected and characterized by electrospray ionization combined with ion trap tandem mass spectrometry (ESI-MSn). The experimental results showed that only 1:1 non-covalent complex can be formed in different starting molar ratios of LA to beta-CD. Furthermore, the diagnostic fragmentation of the beta-CD-LA complex, with a significant contribution of covalent fragmentation of LA leaving the N-acetyl anthranoyl (AN) moiety inserted to beta-CD, provided the convincing evidence for the formation of non-covalent complex between LA and beta-CD and the cite of LA molecule included to cavity of beta-CD assigned to AN residue.

Determination of ultra-trace concentrations of elements in high purity tellurium by inductively coupled plasma mass spectrometry after Fe(OH)(3) coprecipitation

In this work, a method was established for the determination of impurities in high purity tellurium by inductively coupled plasma mass spectrometry (ICP-MS) after Fe(OH)(3) coprecipitation. After comparison of coprecipitation ability and separation efficiency between Fe(OH), and Al(OH)(3), Fe(OH)(3) was chosen as the precipitate. A separation factor of 160 for 200 mg tellurium was obtained under conditions of pH 9 and 2 mg of Fe3(+). The 13 elements, such as Bi, Sn, Pb, In, Tl, Cd, Cu, Co, Ni, Zn, Ti, Be and Zr, could be almost completely coprecipitated under these conditions. In addition, Te memory effect imposed on the ICP-MS instrument was assessed, as well as Te matrix effect that caused the low recovery of Ga, As, Sb and V in real sample was discussed. Finally, the method was evaluated through recovery test and was applied to practical sample analysis, with detection limits of most of the elements being below 0.15 mug g(-1) and R.S.D. below or at approximately 10%, which indicated that this method could fully satisfy the requirements for analysis of 99.999% similar to 99.9999% high purity Te.

The relationship between chemical bond properties and Stokes shift of Eu2+ in some silicate host lattices

The covalency of each bond in divalent europium doped hosts CaSiO3, SrSiO3, BaSiO3, Sr2LiSiO4F, Ba5SiO4Cl6 and Ba5SiO4Br6 were calculated by using the complicate crystal chemical bond theory. The relationship between the Stokes shift and the bond properties of Eu2+ in these crystals was discussed. The result demonstrates that, in the isostructural crystals that being doped with Eu2+, there is a more precise connection between the magnitude of Stokes shift and the mean covalency of the dopant site.

Exploring the ester-exchange reactions of diester-diterpenoid alkaloids in the aconite decoction process by electrospray ionization tandem mass spectrometry

The chemical components in the decoctions of Chinese herbal medicines are not always the same as those in the crude herbs because of the insolubility or instability of some compounds. In this work electrospray ionization tandem mass spectrometry was used to explore the ester-exchange reactions for aconitine-type diester-diterpenoid alkaloids occurring during the process of decocting aconite root. The aconitines were screened in a diverse range of samples, including crude aconite, decoction of crude aconite, residues from decoction of crude aconite, prepared aconite, decoction of prepared aconite, decoction of prepared aconite with added palmitic acid, and decoction of a mixture of mesaconitine and hypaconitine standards with liquorice root. It was found that diester-diterpenoid aconitines were converted into lipo-alkaloids as well as monoester alkaloids by the decoction of aconite.

Characterization of aconitine-type alkaloids in the flowers of Aconitum kusnezoffii by electrospray ionization tandem mass spectrometry

The fragmentation mechanism of aconitine-type alkaloids in the flowers of Aconitum kusnezoffii (FAK) was investigated using electrospray ionization tandem mass spectrometry (ESI-MSn) firstly. The analysis of the collision-induced dissociation (CID) spectra of three purified aconitine standards and six previously reported aconitines indicated that the fragmentation of the protonated aconitines at low-energy CID follows a similar pathway. The elimination of a C-8-substituent such as an acetic acid or a fatty acid is the dominant fragmentation mode in MS2. Successive losses of CH3COOH, CH3OH, H2O, BzOH, and CO are the main fragmentation pathways of aconitine-type alkaloids in MS3 spectra. Based on these features, a rapid method for the direct detection and characterization of alkaloids from an ethanolic extract of FAK is described. All the known aconitum alkaloids are detected and a series of lipo-aconitines has been found for the first time in this plant.

Structure identification of five unknown dilipo-alkaloids extracted from processed tuber of Aconitum carmiechaeli by electrospray ionization tandem mass spectrometry

The alkaloids in processed aconite tuber of Aconitum Carmiechaeli were studied, and five novel alkaloids in extract from processed aconite tuber were found. The first step involved the use of electrospray ionization mass spectrometry (ESI-MS), and then multi-stage tandem mass spectrometry (MSn) was used to provide structural information. Based on their MSn spectra, the structures of the five novel compounds were elucidated to be C3,C8-difatty acid esters of mesaconitine, aconitine and 10-hydroxyaconitine.

Mass-transfer kinetics of ytterbium extraction with sec-nonylphenoxy acetic acid

The extraction kinetics of ytterbium with sec-nonylphenoxy acetic acid (CA-100) in heptane have been investigated using a constant interfacial area cell with laminar flow. The influence of stirring speed and temperature on the rate indicated that the extraction rate was controlled by the experiment conditions. The plot of interfacial area on the rate showed a linear relationship. This fact together with the low solubility in water and strong surface activity of CA-100 at heptane-water interfaces made the interface the most probable locale for the chemical reactions. The influences of extractant concentration and hydrogen ion concentration on the extraction rate were investigated, and the forward and reverse rate equations for the ytterbium extraction with CA-100 were also obtained. Based on the experimental data, the apparent forward extraction rate constant was calculated. Interfacial reaction models were proposed that agree well with the rate equations obtained from experimental data.

Studies on the non-covalent complexes between oleanolic acid and cyclodextrins using electrospray ionization tandem mass spectrometry

Non-covalent inclusion complexes formed between an anti-inflammatory drug, oleanolic acid (OA), and alpha-, beta- and gamma-cyclodextrins (CDs) were investigated by means of solubility studies and electrospray ionization tandem mass spectrometry (ESI-MSn). The order of calculated association constants (K-1:1) of complexes between OA and different CDs in solution is in good agreement with the order of their relative peak intensities and the relative CID energies of the complexes under the same ESI-MSn conditions. These results indicate a direct correlation between the behaviors of solution- and gas-phase complexes. ESI-MS can thus be used to evaluate solution-phase non-covalent complexes successfully. The experimental results show that the most stable 1:1 inclusion complexes between three CDs and OA can be formed, but 2:1 CD-OA complexes can be formed with beta- and gamma-CDs. Multi-component complexes of alpha-CD-OA-beta-CD (1:1:1), alpha-CD-OA-gamma-CD (1:1:1) and beta-CD-OA-gamma-CD (1:1:1) were found in equimolar CD mixtures with excess OA. The formation of 2:1 and multi-component 1:1:1 non-covalent CD-OA complexes indicates that beta- and gamma-CD are able to form sandwich-type inclusion non-covalent complexes with OA. The above results can be partly supported by the relative sizes of OA and CD cavities by molecular modeling calculations.

Study on the structure change and oxygen vacation shift for Ce1-xSmxO2-y solid solution

A series of solid electrolytes Ce1-xSmxO2-y (x=0similar to0.6) were prepared by sol-gel method. XRD measurement showed that single-phase solid solution was formed in all investigated ranges at 160 degreesC, which is a significantly lower synthesis temperature compared to traditional solid state reaction. High temperature X-ray, ESR, and Raman scattering were used to characterize the samples. ESR measurement showed that ESR with sample irradiated by high-energy particle is an effective way to study the defect structure. These changes in the Raman spectrum are attributed to O vacancies, which are introduced into the lattice when tetravalent Ce4+ is substituted by trivalent Sm3+.