Structural variation of solid core and thickness of porous shell of 1.7 μm core-shell silica particles on chromatographic performance: narrow bore columns

Chromatographic and mass transfer kinetic properties of three narrow bore columns (2.1 × 50 mm) packed with new core–shell 1.7 μm EIROSHELL™-C₁₈ (EiS-C₁₈) particles have been studied. The particles in each column varied in the solid-core to shell particle size ratio (ρ), of 0.59, 0.71 and 0.82, with a porous silica shell thickness of 350, 250 and 150 nm respectively. Scanning and transmission electron microscopy (SEM and TEM), Coulter counter analysis, gas pycnometry, nitrogen sorption analysis and inverse size exclusion chromatography (ISEC) elucidated the physical properties of these materials. The porosity measurement of the packed HILIC and C₁₈ modified phases provided the means to estimate the phase ratios of the three different shell columns (EiS-150-C₁₈, EiS-250-C₁₈ and EiS-350-C₁₈). The dependence of the chromatographic performance to the volume fraction of the porous shell was observed for all three columns. The naphtho[2,3-a]pyrene retention factor of k′ ∼ 10 on the three EiS-C_18s employed to obtain the height equivalents to theoretical plates (HETPs) data were achieved by varying the mobile phase compositions and applying the Wilke and Chang relationship to obtain a parallel reduced linear velocity. The Knox fit model gave the coefficient of the reduce HETPs for the three EiS-C_18s. The reduced plate height minimum h_min = 1.9 was achieved for the EiS-150-C₁₈ column, and generated an efficiency of over 350,000 N/m and h_min = 2.5 equivalent to an efficiency of 200,000 N/m for the EiS-350-C₁₈ column. The efficiency loss of the EiS-C18 column emanating from the system extra-column volume was discussed with respect to the porous shell thickness.     

Dependence of fluorescence properties on substitution of BaF2 for BaO in barium gallo-germanate glass

3.5 mol%, 6.5 mol%, 9.5 mol%, and 12.5 mol% BaF₂ were gradually substituted for BaO in 0.3 mol% Tm₂O₃ doped 12.5 BaO-12.5 Ga₂O₃-75 GeO₂ (BGG) glasses to study the effect of the substitution on the OH⁻ elimination and emission properties. The FTIR spectral demonstrated that the substitution effectively eliminated OH⁻ groups and 9.5 mol% BaF₂ was enough for the OH⁻ elimination. The J-O parameters of all the samples were calculated according to J-O theory. The calculation showed that the Ω₂ parameter decreased monotonically with BaF₂ content increasing, while Ω₄ and Ω₆ did not change much. The radiative lifetime increased while BaF₂ content increased as well. The emission cross section of ³F₄ → ³H₆ transition was calculated by the F-L formula. However, it decreased with the gradual BaF₂ addition.

Research Highlights

? OH⁻ groups were eliminated by the substitution of BaF₂ for BaO in (BGG) glass. ? The optimal substitution level of BaF₂ was 9.5 mol% for OH⁻ elimination. ? The Ω₂ parameter decreased monotonically by the elimination. ? The emission cross section of ³F₄ → ³H₆ transition was decreased by the substitution.     

影响阻尼牛顿法收敛性的两个重要参数

对阻尼牛顿算法作了适当的改进,证明了新算法的收敛性.基于新算法,运用计算机代数系统Matlab,研究了迭代次数k,参数对(μ,λ)与初值x0三者间的依赖关系,研究了病态问题在新算法下趋于稳定的渐变(瞬变)过程.数值结果表明:(1)阻尼牛顿迭代中,参数对(μ,λ)与迭代次数k间存在特有的非线性关系;(2)适当的参数对(μ,λ)与阻尼因子α的共同作用能够在迭代中大幅度地降低病态问题的Jacobi阵的条件数,使病态问题逐渐趋于稳定,从而改变原问题的收敛性与收敛速度.     

New Analysis of the ν3 fundamental band of HDCO: Positions and intensities

Using high-resolution Fourier transform spectra of mono deuterated formaldehyde (HDCO) recorded in the 5.8-μm spectral range at Giessen (Germany), we carried out an extensive analysis of the strong ν₃ fundamental band (carbonyl stretching mode) at 1724.2676 cm⁻¹, starting from results of a previous analysis [J.W.C. Johns, A.R.W. McKellar, J. Mol. Spectrosc. 64 (1977) 327-339]. For this hybrid band (with both A- and B-type transitions) the analysis was pursued up to high rotational quantum numbers. In this way, it was possible to evidence a resonance which perturbs the ν₃ lines for high K_a values which is due to the existence of the 2ν₅ and ν₅ + ν₆ dark bands in the same spectral region. In addition a local resonance is perturbing the 3¹ levels in  = 8 which is due to a crossing with the 4¹ energy levels in K_a = 11. The model used to calculate the energy levels accounts for the observed A- type, B- type C-type Coriolis (and/or) Fermi resonances which couple the 3¹ and the 5¹6¹, 5², and 4¹ energy levels. However the 4¹ state is also involved in strong vibration-rotation interactions coupling the {5¹,6¹,4¹} system of resonation states of HDCO [A. Perrin, J.M. Flaud, L. Margulès, J. Demaison, H. Mäder, S. Wörmke, J. Mol. Spectrosc. 216 (2002) 214-224]. Therefore the final energy levels calculation was performed for the {5¹,6¹,4¹,3¹,5²,5¹6¹} resonating states and in this way it was possible to reproduce the observed line positions, within their experimental uncertainties. The present work also led to the determination of the intensity ratio of the B- to A-type components of the ν₃ band I_A/I_B ∼24 band from spectral fittings performed in several parts of the observed spectrum. Finally, using the 5.8 μm band intensity available in the literature we generated, for the first time, a list of line parameters (positions and intensities) for the 5.8 μm region of HDCO.     

Rapid high performance liquid chromatography method development with high prediction accuracy,using 5 cm long narrow bore columns packed with sub-2 μm particles and Design Space computer modeling

Many different strategies of reversed phase high performance liquid chromatographic (RP-HPLC) method development are used today. This paper describes a strategy for the systematic development of ultrahigh-pressure liquid chromatographic (UHPLC or UPLC) methods using 5 cm × 2.1 mm columns packed with sub-2 μm particles and computer simulation (DryLab^® package). Data for the accuracy of computer modeling in the Design Space under ultrahigh-pressure conditions are reported. An acceptable accuracy for these predictions of the computer models is presented. This work illustrates a method development strategy, focusing on time reduction up to a factor 3–5, compared to the conventional HPLC method development and exhibits parts of the Design Space elaboration as requested by the FDA and ICH Q8R1. Furthermore this paper demonstrates the accuracy of retention time prediction at elevated pressure (enhanced flow-rate) and shows that the computer-assisted simulation can be applied with sufficient precision for UHPLC applications (p > 400 bar). Examples of fast and effective method development in pharmaceutical analysis, both for gradient and isocratic separations are presented.     

半群中的(λ,μ)-模糊理想(英文)

在半群中给出了(λ,μ)-模糊子半群和各种(λ,μ)-模糊理想的概念,讨讹了它们的一些性质,并给出了各种(λ,μ)-模糊理想的充分必要条件.     

Incorporation of DNA/PEI polyplexes into gelatin/chitosan hydrogel scaffolds: a μ-DSC study

Polyplexes between a double-stranded Salmon DNA and hyperbranched poly(ethyleneimine) (PEI) as well as a maltosylated PEI-Mal were incorporated into a gelatin/chitosan hydrogel scaffold. Calorimetric experiments of the polyplexes show a decrease of the melting temperature in presence of PEI and a peak splitting in presence of PEI-Mal, which can be interpreted to a partial compaction of the DNA strands in presence of PEI-Mal. When the polyplexes are incorporated into a gelatin/chitosan scaffold in the swollen state, the DNA melting peaks at 90 and 93 °C, respectively, indicate in both cases the release of the DNA at the surface of the hydrogel scaffold in a more compact form. Specific interactions between the PEI-Mal shell and gelatin are responsible for the tuning of the release properties in presence of the maltose units in the hyperbranched PEI.     

联系数在梯形模糊数多属性决策中的应用

属性权重和属性值都是梯形模糊数的多属性决策问题是一种带有不确定性的决策,需要作不确定性分析后才能得出结论.为此把梯形模糊数表示的属性值和属性权重先用其特征函数"均值+偏差"联系数(特征联系数)表示,再利用联系数运算法则作"加权求和"运算,不仅获得与其它决策方法相同的结果,而且借助联系数中i的不同取值考察决策对象的排序变化,方法简便易行,且具有较强适用性.     

Counter-examples of regularity behavior for σ-evolution equations

In this paper, we mainly discuss the infinite loss of regularity and μ-loss for a σ-evolution type model with oscillating in time coefficients. On the one hand, an explicit counter-example has been constructed in the frequency space to show the precise infinite loss of regularity. On the other hand, due to the finite propagation speed property for σ∈(0,1], we construct the counter-example of a sequence of solutions in R by applying state of art techniques.