Mass spectrometric analysis of free fatty acids in infant milk powders by frozen pretreatment coupled with isotope‐labeling derivatization

In combination with frozen pretreatment and carboxyl group derivatization, a novel workflow was developed for the determination of free fatty acids in milk powder. The workflow showed a significantly enhanced performance for comprehensive free fatty acid analysis owing to a highly efficient frozen extraction method. In addition, the advantages of the workflow also involved high sensitivity and great tolerance to a complex matrix. Characteristic fragment ions of derivatization reagents also provide clear evidence for the qualitative analysis of free fatty acids. Fourteen types of free fatty acids in a number of domestic and overseas infant milk powders have been successfully detected. The content of free fatty acids in the different samples was different, which probably indicates the diverse quality of infant milk powder. The workflow is expected to be a pragmatic tool for the analysis of free fatty acids in intricate matrices.     

Yield criterion and elasto-plastic damage constitutive model for frozen sandy soil

A series of triaxial compression tests was carried out on a frozen sandy soil under confining pressures of 0–18 MPa at −6 °C. The experimental results indicate that, the strength of frozen sandy soil increases versus the increase in the confining pressures when σ₃ ? 3 MPa, but decreases when σ₃ > 3 MPa. This phenomenon is called the strengthening and weakening effects of confining pressures. A yield function, considering both effects, is proposed using the experimental method according to Drucker’s postulate, and the mathematical expression of the hardening parameter, which can describe the softening and hardening phenomenon, is provided. An elasto-plastic constitutive model for frozen sandy soil is developed. Based on the continuum damage theory, the cross anisotropic damage variables are deduced and their change regularities are investigated. Then the elasto-plastic damage constitutive model is proposed by introducing damage variables into elasto-plastic constitutive model. The validity of the model is verified by comparing its modeling results with experimental results obtained from triaxial tests. It is found that, this model can predict the deformation regularity of frozen soil exactly. It can simulate the stress–strain process under high confining pressures when pressure melting phenomena appear especially well.     

A combined temperature-dependent electron and single-crystal X-ray diffraction study of the fresnoite compound Rb2VV2O8

High-purity Rb₂V₃O₈ has been grown and temperature-dependent electron and single-crystal X-ray diffraction used to carefully investigate its fresnoite-type reciprocal lattice. In contrast to other recently investigated representatives of the fresnoite family of compounds, Rb₂V₃O₈ is not incommensurately modulated with an incommensurate basal plane primary modulation wave vector given by q∼0.3 〈110〉^*. A careful low-temperature electron diffraction study has, however, revealed the existence of weak incommensurate satellite reflections characterized by the primitive primary modulation wave vector q₁∼0.16c^*. The reciprocal space positioning of these incommensurate satellite reflections, the overall (3+1)-d superspace group symmetry, as well as the shapes of the refined displacement ellipsoids determined from single-crystal XRD refinement, are all consistent with their arising from a distinct type of condensed rigid unit modes (RUMs) of distortion of the Rb₂V₃O₈ parent structure.     

Electrochemical redox reactions studied in frozen tetrabutylammonium halide hydrates

The electrochemical redox reactions: Fe(CN)₆ ⁴⁻−e⁻↔ Fe(CN)₆ ³⁻, Ru(NH₃)₆ ³⁺+e⁻↔ Ru (NH₃)₆ ²⁺ and Fc(CH₂OH)₂−e⁻↔ Fc(CH₂OH)₂ ⁺ (Fc–ferrocene) were investigated in tetrabutylammonium halide hydrates at temperatures below and above the electrolyte melting point. They were studied by cyclic voltammetry, potential step chronoamperometry and impedance spectroscopy. Freezing of the electrolyte affects both the shape and position of the cyclic voltammogram on the potential scale. Also the shapes of the current-time relationship and the impedance spectra change at temperatures below the melting point. It has been proposed that this behaviour is caused by slow transport of the reactant and the heterogeneous nature of the electrolyte. The activation energies of reactant transport are about four times larger in frozen electrolytes than those in liquid. It has been concluded that reactant transport is restricted to the intergrain space of the electrolyte. Received: 16 December 1997 / Accepted: 10 February 1998     

胃肠道正常组织与相应肿瘤组织结构的FTIR光谱研究

本文用傅里叶变换红外显微光谱对一系列胃肠道（食道、胃、结肠）肿瘤组织和相应正常组织的冰冻切片进行了研究。结果显示，所有肿瘤组织的光谱基本一致。而正常组织的光谱按１４００－９５０ｃｍ＾－１区域的特点可分为三类。对光谱中蛋白质酰胺Ｉ带曲线拟合的结果表明，正常组织和肿瘤组织中蛋白质的二级结构有着很大的差别。     

Strength criterion and elastoplastic constitutive model of frozen silt in generalized plastic mechanics

Triaxial compressive tests of frozen silt were carried out under confining pressures from 0.0 to 14.0 MPa at the temperatures of −2, −4 and −6 °C. A strength criterion based upon experimental results is presented by the combination of extended Lade–Duncan strength function f_π(θ) in π-plane and f_p–q(p) in p–q-plane. In order to describe the deformation characteristic of frozen silt, an elastoplastic constitutive model in generalized plastic mechanics has been proposed for the nonlinear behavior of frozen silt, such as the pressure melting and crushing phenomena, strain softening/hardening characteristics and dilatation, etc., by employing an elliptical yield surface, together with a non-associated flow rule for the compressive mechanism, and two parabolic yield surfaces, together with non-associated flow rules for the shear mechanism. The validity of the model is verified by comparing its modeling results with the results of triaxial compressive tests. It is found that the stress–strain curves predicted by this model agree well with the corresponding experimental results both under low and high confining pressures.     

Stability Analysis of a Porous Layer Heated from Below and Subjected to Low Frequency Vibration: Frozen Time Analysis

We investigate the convection amplitude in an infinite porous layer subjected to a vibration body force that is collinear with the gravitational acceleration and heated from below. The analysis focuses on the specific case of low frequency vibration where the frozen time approximation is used. The results reveal that for moderate Vadasz numbers, increasing the magnitude of the acceleration stabilizes the convection. The results of the large Vadasz number analysis reveals that the acceleration plays a passive role in the stability of convection and the classical stability criteria for Rayleigh–Benard convection applies.     

A general theory for the Frozen Waves and their realization through finite apertures

In this paper, we present a generalization of the so-called Frozen Waves, which are new solutions to Maxwell’s equations having the important characteristic of remaining static in space and keeping any previously chosen arbitrary longitudinal field pattern. In the pioneering work, these waves were introduced as a discrete superposition of zero-order Bessel beams. As a fact, here we will represent these waves as a continuous superposition of Bessel beams leading to a simpler and more compact mathematical formalism, which allows us to derive certain inequalities that restrict the physical properties of the Frozen Waves, such as their attainable longitudinal resolution. Besides this, we will discuss losses compensation in a lossy medium and, finally, their practical realization through finite apertures.     

Frozen water phase method for logD measurement using a 96-well plate

In this study, a frozen water phase method for log D measurement using a 96-well plate was developed. In the case of log D measurement of compounds, the problem of octanol contamination often occurs; in lipophilic compounds, the concentration of the octanol phase is much higher than that of the water phase. When the water phase is separated from the octanol phase, a small amount of octanol phase contamination could strongly influence the concentration of the water phase. To avoid this problem, the frozen water phase method was developed. The water phase was frozen in liquid nitrogen and then the unfrozen octanol phase was removed. To remove the portion of the octanol remaining on the frozen water phase, the surface of the frozen water phase was washed with octanol and water/ethanol (50/50, v/v). The validity of the method was confirmed by results of commercially available drugs at the log D range from 0 to 4. Further, it was found that this method had the ability to evaluate the pH-log D profile of compounds in the range from pH 2 to pH 12. As a result, we developed the convenient and accurate method that is effective in preventing contamination with a wide dynamic range.