Ultrasonic extraction and separation of anthraquinones from Rheum palmatum L

The ultrasonic nebulization extraction (UNE) was developed and applied to extract anthraquinones (emodin, aloe-emodin and rhein) from Rheum palmatum L. Several parameters of UNE, including type of extraction solvent, concentration of extraction solvent, volume of extraction solvent, extraction time and ultrasonic power, were studied and the optimized parameters were selected. The operation conditions of micellar electrokinetic capillary chromatography (MEKC) were also studied. Under the selected conditions, contents of emodin, aloe-emodin and rhein obtained from different cultivated areas of R. palmatum L. were 1.08–2.04 mg/g, 0.65–1.16 mg/g and 0.70–2.90 mg/g, respectively. The relative standard deviations (RSDs) for emodin, aloe-emodin and rhein were 1.3–2.4%, 1.9–4.7% and 1.3–3.9%, respectively. Compared with maceration extraction (ME), reflux extraction (RE), stirring extraction (SE) and ultrasonic extraction (UE), the proposed method was more efficient, faster and easier to be operated and lower equipment costs and lower extraction temperature were required. The results indicated that UNE was a good alternative method for extracting anthraquinones from R. palmatum L. Compared with traditional extractions, the proposed extraction has a potential in on-line sampling, especially when the gas is used as the carrier of sample.     

Molecular diversity of volatile compounds in rare willow (<Emphasis Type="BoldItalic">Salix</Emphasis> spp.) honeydew honey: identification of chemical biomarkers

Salix spp. honeydew honey volatiles were analyzed for the first time by headspace solid-phase microextraction (HS-SPME) and ultrasonic solvent extraction (USE) followed by gas chromatography and mass spectrometry (GC, GC-MS). The use of HS-SPME and USE had advantageous results over the use of one single technique, as it provided different complementary chromatographic profiles for a comprehensive screening of the honeydew volatile composition. The volatiles with different functionality, molecular weight, and polarity were extracted and identified. High percentages of benzoic acid, phenylacetic acid, 2-hydroxybenzoic acid, 4-hydroxyphenylacetic acid with minor percentages of 4-methoxybenzoic acid, 4-hydroxyphenylethanol, and 4-hydroxybenzoic acid from USE extracts can be emphasized as volatile biomarkers of this honeydew that probably originated from Salix spp., as well as methyl salicylate identified only by HS-SPME. The application of heat treatment at 80 °C for 2 h did not change significantly the volatile composition of this honeydew.     

The oxidation of fullerene [C70] with various oxidants by ultrasonication

The reaction of C₇₀ by ultrasonication with various oxidants such as 3-chloroperoxy benzoic acid (Fluka 99%), 4-methyl morpholine N-oxide (Aldrich 97%), chromium (VI) oxide (Aldrich 99.9%), and oxone^® monopersulfate compound, at room temperature causes the oxidation of fullerene [C₇₀(O)_n] (n=1–2 or n=1). The FAB-MS, UV–visible, FT-IR spectra, and HPLC analysis confirmed that products of fullerene oxidation are [C₇₀(O)_n] (n=1–2 or n=1).     

Optimization of ultrasound-assisted extraction of anthocyanins in red raspberries and identification of anthocyanins in extract using high-performance liquid chromatography-mass spectrometry

Anthocyanins (Acys) are naturally occurring compounds that impart color to fruit, vegetables and plants. The extraction of Acys from red raspberry (Rubus idaeus L. var. Heritage) by ultrasound-assisted process (UAP) was studied. A central composite rotate design (CCRD) was used to obtain the optimal conditions of ultrasound-assisted extraction (UAE), and the effects of operating conditions, such as the ratio of solvents to materials, ultrasonic power and extraction time, on the extraction yield of Acys were studied through response surface methodology (RSM). The optimized conditions of UAE were as follows: ratio of solvents to materials was 4:1 (ml/g), extraction time was 200 s, and ultrasonic power was 400 W. Under these conditions 34.5 mg of Acys from 100 g of fresh fruits (T_Acy, expressed as cyanidin-3-glucoside), approximately 78.13% of the total red pigments, could be obtained by UAE. The Acys compositions of extracts were identified by high-performance liquid chromatography–mass spectrometry (HPLC–MS), 12 kinds of Acys had been detected and eight kinds of Acys were characterized. Result indicated that cyanidin-3-sophoroside, cyanidin-3-(2^G-glucosylrutinoside), cyanidin-3-sambubioside, cyanidin-3-rutinoside, cyanidin-3-xylosylrutinoside, cyanidin-3-(2^G-glucosylrutinoside), and cyanidin-3-rutinoside were main components in extracts. In addition, in comparison with the conventional solvent extraction, UAE is more efficient and rapid to extract Acys from red raspberry, due to the strong disruption of fruit tissue structure under ultrasonic acoustic cavitation, which had been observed with the scanning electron microscopy (SEM). However, the Acys compositions in extracts by both methods were similar, which were investigated using HPLC profile.     

Study of effects of Mn in CdS nanocrystals

Mn²⁺-doped CdS nanocrystals have been synthesized by adopting an aqueous solution precipitation method. These nanocrystals have been studied using X-ray diffraction (XRD), X-ray fluorescence (XRF), optical absorbance, photoluminescence (PL), DC electrical conductivity measurements and positron annihilation lifetime spectroscopy (PALS). The system has been found to be in the hexagonal phase. PL spectra have been studied on most prominent exciton peaks within the wavelength range (586–731 nm). The emission intensity is found to increase on increasing Mn²⁺ ion concentration (0–5%). Electrical conductivity lies within 0.819×10⁻⁶ to 1.69×10⁻⁶ Ω⁻¹ m⁻¹ and the system shows power law dependence for n=3–3.77. The Cd vacancies concentration has been found to decrease on increasing Mn%.     

Improved synthesis of chalconoid-like compounds under ultrasound irradiation

Claisen–Schmidt condensation of various substituted acetophenones with cinnamaldehyde catalyzed by KF–Al₂O₃ results chalconoid-like compounds, (2E,4E)-1,5-diarylpenta-2,4-dien-1-ones, in 67–92% yields in 5–60 min under ultrasound irradiation.     

Low-temperature specific heat of Ni–Mn–Ga ferromagnetic shape memory alloys

Results of the low-temperature specific heat measurements (2–80 K) for one austenitic and three martensitic Ni–Mn–Ga ferromagnetic alloys are presented. The alloy compositions are chosen to comprise a wide span of valence electron concentrations e/a=7.3–7.78. Debye temperature (261–345 K) is found to be an increasing function of e/a while the experimental values of the Sommerfeld coefficient (2.9–3.4 mJ/mol K²) appear to be increasing in the martensitic region only. Observation of those trends rekindles the discussion about the role of vibrational and electronic contributions to the lattice instability and transformation mechanism of studied alloys.     

Magnetic anisotropy induced in Nd16Fe76B8 by Hf additions

Remanence, coercivity and maximum energy product (BH)_max of Nd₁₆Fe_76−xHf_xB₈ (x=0, 0.1, 0.2) magnets processed under different hydrogenation-disproportionation-desorption-recombination (HDDR) conditions, were studied. Vibrating sample magnetometry results showed that Hf-doped materials develop an important degree of anisotropy, especially for the case of solid-HDDR treatments at 800°C and 850°C, with the largest effect at 850°C. Maximum values of remanence and coercivity were observed for Hf-added samples S-HD at 850°C, and 900°C, respectively. The highest (BH)_max value was also observed in S-HD 900°C Hf-added samples. These results are discussed in terms of the expected microstructure of the intermediate HD and final HDDR processed powders.     

The contribution of 2N photon absorption in C(γ,2N) reactions for Eγ = 150–400 MeV

The ¹²C(γ,pn) and ¹²C(γ,pp) reactions have been studied using tagged photons of energy E_γ = 150–400 MeV. Recoil momentum distributions are compared to the results of Monte Carlo calculations based on a two-nucleon photon absorption model and two different phase space models. The ¹²C(γ,pn) data at low missing energy are consistent with absorption on 1p² and 1s1p nucleon pairs.     

Observation of unrecoverable domains in two-dimensional-arrayed Pr0.5Ca0.5MnO3−y junctions

Two-dimensional-arrayed 14×14 sandwich-type junctions of Au–Pr_1−xCa_xMnO_3−y (PCMO, x=0.5)–SrRuO₃ were fabricated on SrTiO₃ (0 0 1) substrates. The resistivity–voltage (ρ–V) characteristics of each junction was measured by a two-probe method. The junctions that return to the insulating state after removing the voltage (recoverable) and the ones that remain metallic (unrecoverable) were found to co-exist in one PCMO film. The variation in the lattice constant of the PCMO film, rather than the variation of the composition, is thought to be related to the separation of recoverable–unrecoverable domains. Among several samples with a PCMO layer fabricated under various conditions, the junctions with thin PCMO layers deposited at low temperature showed a pronounced hysteresis in their ρ–V characteristics. The clear hysteresis and good crystallinity of PCMO films were correlated.     

Effect of oxide thickness on the capacitance and conductance characteristics of MOS structures

In this work, the investigation of the interface states density and series resistance from capacitance–voltage (C–V) and conductance–voltage (G–V) characteristics in Au/SnO₂/n-Si (MOS) structures prepared at various SnO₂ layer thicknesses by spray deposition technique have been reported. It is fabricated five samples depending on deposition time. The thicknesses of SnO₂ films obtained from the measurement of the oxide capacitance in the strong accumulation region for MOS Schottky diodes are 37, 79, 274, 401, and 446 Å, for D1, D2, D3, D4, and D5 samples, respectively. The C–V and G–V measurements of Au/SnO₂/n-Si MOS structures are performed in the voltage range from −6 to +10 V and the frequency range from 500 Hz to 10 MHz at room temperature. It is observed that peaks in the forward C–V characteristics appeared because of the series resistance. It has been seen that the value of the series resistance R_s of samples D1 (47 Ω), D2 (64 Ω), D3 (98 Ω), D4 (151 Ω), and D5 (163 Ω) increases with increasing the oxide layer thickness. The interface state density D_it ranges from 2.40×10¹³ cm⁻² eV⁻¹ for D1 sample to 2.73×10¹² cm⁻² eV⁻¹ for D5 sample and increases with increasing the oxide layer thickness.     

Strong charge carrier effect on the magnetic coupling of La-doped CaMnO3

The exchange interactions in polycrystalline samples of Ca_1−xLa_xMnO₃ (0.00x0.05) are studied by means of Raman scattering and electron paramagnetic resonance. Dramatic reductions in the spin-phonon interactions and magnetic correlations are observed for La doping levels as small as 2–3%. These results show that the charge carriers play an important role in the overall exchange coupling in the electron-doped manganites, even at very low doping levels.     

Determination and analysis of the dispersive optical constants of the 5,5′,6,6′-tetraphenyl-2,2′-bi([1,3]dithiolo[4,5-b][1,4]dithiinylidene)–DDQ complex thin film

The synthesis and optical properties of the 5,5′,6,6′-tetraphenyl-2,2′-bi([1,3]dithiolo [4,5-b] [1,4]dithiinylidene)–2,3-dichloro-5,6-dicyano-p-benzoquinone (DDQ) complex thin film were investigated by the optical characterization. The optical constants such as refractive index, extinction coefficient and absorption coefficient were determined using the transmittance T(λ) and reflectance R(λ) spectra and the refractive index dispersion was analyzed using single oscillator of Wemple–Didomenico model. The single oscillator energy E₀ and the dispersion energy E_d were calculated. The effect of temperature on refractive dispersion and optical band gap E_g is also discussed. As a result, the annealing temperatures have an important effect on refractive index of thin film.     

Coexisting antiferromagnetism and ferromagnetism in mechanically alloyed Fe-rich Fe–Ni alloys: implications regarding the Fe–Ni phase diagram below 400°C

Fe–Ni alloys below the Invar region with compositions Fe_100−xNi_x (x=21, 24, and 27 at%) were prepared by high-energy ball milling technique (mechanical alloying). The as-milled samples, characterized by X-ray diffraction and Mössbauer spectroscopy, contain a mixture of (BCC) and γ (FCC) phases, whereas the samples annealed at 650°C for 0.5 h show a single γ (FCC) phase displaying a single line Mössbauer spectrum at room temperature (RT). At low temperature, the Mössbauer spectra of annealed Fe₇₆Ni₂₄ and Fe₇₃Ni₂₇ alloys show the existence of a magnetically split pattern together with a broad singlet, which are ascribed to a high-moment ferromagnetic Ni-rich phase and a low-moment Fe-rich phase, respectively. The Fe-rich phase in annealed Fe₇₆Ni₂₄ alloy, which is paramagnetic at RT, undergoes antiferromagnetic ordering at 40 K, estimated from the dramatic line broadening of its spectrum, giving rise to a small hyperfine field (e.g. 2 T at 6 K). The coexistence of these phases is attributed to phase segregation occurring in these alloys as a result of enhanced atomic diffusion. The stability of these alloys towards martensitic (FCC→BCC) transformation at low temperatures is discussed in connection with the Fe–Ni phase diagram below 400°C.     

Atmospheric neutrinos: LMA oscillations, Ue3 induced interference and CP-violation

We consider oscillations of the low energy (sub-GeV sample) atmospheric neutrinos in the three neutrino context. We present the semi-analytic study of the neutrino evolution and calculate characteristics of the e-like events (total number, energy spectra and zenith angle distributions) in the presence of oscillations. At low energies there are three different contributions to the number of events: the LMA contribution (from ν_e-oscillations driven by the solar oscillation parameters), the U_e3-contribution proportional to s₁₃², and the U_e3-induced interference of the two amplitudes driven by the solar oscillation parameters. The interference term is sensitive to the CP-violation phase. We describe in details properties of these contributions. We find that the LMA, the interference and U_e3 contributions can reach 5–6%, 2–3% and 1–2% correspondingly. An existence of the significant (>3–5%) excess of the e-like events in the sub-GeV sample and the absence of the excess in the multi-GeV range testifies for deviation of the 2–3 mixing from maximum. We consider a possibility to measure the deviation as well as the CP-violation phase in future atmospheric neutrino studies.     

Influence of N2:(N2 + Ar) flow ratio and substrate temperature on the properties of zirconium nitride films prepared by reactive dc magnetron sputtering

Preferred crystal orientation and low electrical resistivity are required for ZrN_x films applied in electronic devices. In this paper, effects of N₂:(N₂+Ar) flow ratio (F(N₂)) and substrate temperature on the properties of the films deposited on glass substrate by reactive dc sputtering are investigated. In a wide range of F(N₂) (4–24%), the films show fcc NaCl structure. While for F(N₂) in the ranges of 5–12, 12–24 and >24%, the films show (1 1 1)/(2 0 0), (1 1 1) only and amorphous structures, respectively. The electrical resistivity increases with F(N₂) from 5 to 24%, and can be controlled to some extent by changing the substrate temperature.     

Characterization of metal/GaN Schottky interfaces based on I–V–T characteristics

Interface properties of metal/n- and p-GaN Schottky diodes are studied by I–V–T and C–V–T measurements, and simulation of their characteristics. On the basis of the previously proposed “surface patch” model, the gross behavior of I–V–T characteristics, which includes Richardson plots together with temperature dependence of the effective Schottky barrier heights (SBHs) and n-values, can be well reproduced. Furthermore, the dependence of the true SBH on the metal work function was also deduced from high-temperature I–V curves, giving S-values of 0.28 and 0.20 for n- and p-GaN samples, respectively, and the interface Fermi level tends to be pinned at a characteristic energy of about two-third of the bandgap.     

Ionic conduction in dilute pseudo-binary systems CuBr–Cu2Se

Ionic conductivity, σ_i, of dilute pseudobinary alloys (CuBr)_1−x(Cu₂Se)_x (x≤0.1) in their γ-phase has been measured by an ac method. The increase of the ionic conductivity propertional to x has been observed, which is attributed to interstitial ions brought by Cu₂Se dissolved in CuBr. It is found that the temperature dependence of mobility of interstitial ions, μ, evaluated by the relation Δσ_i/x=kμ (k is a constant) is bent at the temperature corresponding to the extrinsic–intrinsic transition of the based material CuBr.     

Very strong interlayer exchange coupling in epitaxial Fe/Fe1−xSix/Fe trilayers (x=0.4–1.0)

Fe/Fe_1−xSi_x/Fe (x=0.4–1.0) wedge-type epitaxial trilayers with improved homogeneity are grown by co-evaporation from two electron-beam sources. The coupling strengths of the bilinear (J₁) and biquadratic (J₂) coupling terms are derived from Brillouin light scattering (BLS) spectra and longitudinal MOKE hysteresis loops. The total coupling strength J=J₁+J₂ increases dramatically with increasing x and reaches values in excess of 6 mJ/m².     

Simultaneous extraction of phenolic compounds of citrus peel extracts: effect of ultrasound

Ultrasound-assisted extraction (UAE) has been widely applied in the extraction of a variety of biologically active compounds including phenolic compounds. However, there is an insufficiency of information on simultaneous extraction of these compounds in this area. In the present study, seven phenolic compounds of two families including cinnamic acids (caffeic, p-coumaric, ferulic, sinapic acid), and benzoic acids (protocatechuic, p-hydroxybenzoic, vanillic acid) from citrus (Citrus unshiuMarc) peels were evaluated by UAE. The effects of ultrasonic variables including extraction time, temperature, and ultrasonic power on the yields of seven phenolic acids was investigated. Results showed that the yields of phenolic compounds increased with both ultrasonic time and temperature increased, whereas the opposite occurred with increasing time at higher temperature to some certain. In the case of 40 degrees C, the decrease in the yields of some phenolic compounds was observed with increased time, whereas those of other compounds did not significantly declined. Ultrasonic power has a positive effect on the yields of phenolic acids under study. Among all ultrasound variables, temperature is the most sensitive on stability of phenolic compounds. Moreover, when phenolic compounds from citrus peel extracts were subjected to ultrasound process, the benzoic acids were more stable than the cinnamic acids. Meanwhile, the optimal ultrasound condition was different one compound from another. These were partly attributed to both the differently chemical structures of phenolic acids and the combination effects of ultrasonic variables.