Experimental investigation of the difference in B-term dominated band broadening between fully porous and porous-shell particles for liquid chromatography using the Effective Medium Theory

The difference in B-term diffusion between fully porous and porous-shell particles is investigated using the physically sound diffusion equations originating from the Effective Medium Theory (EMT). Experimental data of the B-term diffusion obtained via peak parking measurements on six different commercial particle types have been analyzed (3 porous and 3 non porous). All particles were investigated using the same experimental design and test analytes, over a very broad range of retention factor values. First, the B-term reducing effect of the solid core (inducing an additional obstruction compared to fully porous particles) has been quantified using the Hashin-Shtrikman expression, showing that the presence of a solid core can account for a reduction of about 11% when the core diameter makes up 63% of the total particle diameter (Halo and Poroshell-particles) and a reduction of 16% when the core diameter makes up 73% (Kinetex). Remaining differences can be attributed to differences in the microscopic structure of the meso-porous material (meso-pore diameter, internal porosity or relative void volume). The much lower B-term diffusion of Halo and Kinetex particles compared to the fully porous Acquity particles (some 20-40% difference, of which about 10-15% can be attributed to the presence of the solid core) can hence largely be attributed to the much smaller internal porosity and the smaller pore size of the meso-porous material making up the shell of these particles.     

用峰鉴别技术反相高效液相色谱法测定火锅汤料中微量吗啡

本文报道了以峰鉴别技术为定性依据的测定火锅汤料中微量吗啡的反相高效液相色谱法。本法采用改良的Ｓｔａｓ－ｏｔｔｏ法分离提取复杂样品中的微量吗啡。由于采用峰鉴别技术，增加了定性参数，大大提高了定性方法的准确性。本法简便、快速。最低检出浓度为０．０４ｍｇ／Ｌ。在数十例样品分析中，与其它仪器分析结果比照，非常符合。     

溶剂蒸气对聚对苯二甲酸乙二酯作用的差示扫描量热研究

用差示扫描量热(DSC)研究了几种有机溶剂蒸气对聚对苯二甲酸乙二酯(PET)的作用,表明可分为反应性的和非反应性的两种。同时,对于非反应性的作用,依冷结晶峰面积的变化,又可分为三种类型:冷结晶峰面积不变,经诱导期后下降,无诱导期而迅速下降。双冷结晶峰现象在一些非反应性溶剂处理过的PET试样的DSC曲线也观察到。     

STUDY ON THE SEQUENCE STRUCTURE OF SBR BY 13C—NMR METHOD Ⅰ. ASSIGNMENT FOR UNSATURAT CARBONS SPECTRA*

The sequence structures of emulsion-processed SBR and solution-processed (by lithium catalyst) SBR were investigated by ~(13)C-NMR spectroscopy. Seventeen peaks within unsaturated carbon region were recorded under the adopted experimental conditions. Assignments for these peaks were made by empirical-parameter-evaluation method.     

Peak Points for Pseudoconvex Domains: A Survey

This paper surveys results concerning peak points for pseudoconvex domains. It includes results of Laszlo that have not been published elsewhere.      

Probability of failure of the watershed algorithm for peak detection in comprehensive two-dimensional chromatography

The watershed algorithm is the most common method used for peak detection and integration in two-dimensional chromatography. However, the retention time variability in the second dimension may render the algorithm to fail. A study calculating the probabilities of failure of the watershed algorithm was performed. The main objective was to calculate the maximum second-dimension retention time variability, Δ²t_R,crit, above which the algorithm fails. Several models to calculate Δ²t_R,crit were developed and evaluated: (a) exact model; (b) simplified model and (c) simple-modified model. Model (c) gave the best performance and allowed to deduce an analytical expression for the probability of failure of the watershed algorithm as a function of experimental Δ²t_R, modulation time and peak width in the first and second dimensions. It could be demonstrated that the probability of failure of the watershed algorithm under normal conditions in GC × GC is around 15–20%. Small changes of Δ²t_R, modulation time and/or peak width in the first and second dimension could induce subtle changes in the probability of failure of the watershed algorithm. Theoretical equations were verified with experimental results from a diesel sample injected in GC × GC and were found to be in good agreement with the experiments.     

Nondestructive evaluation for remanent life of modified 9Cr-1Mo steel by reversible magnetic permeability

We present a magnetic and nondestructive method to evaluate the remanent life of modified 9Cr-1Mo steel by measuring the reversible magnetic permeability. Specimens with ten different kinds of aging periods were prepared using an isothermal heat treatment at 690 °C. The Larson-Miller parameter (LMP) was calculated and the peak interval of reversible magnetic permeability (PIRMP) was measured using the surface type probe. PIRMP was inversely proportional to LMP. We can evaluate the remanent life of modified 9Cr-1Mo steel using the relationship between PIRMP and LMP. Also, we present the possibility that the tensile strength and yield strength measured by destructive methods could be estimated by PIRMP measured nondestructively.     

Effects of first dimension eluent composition in two-dimensional liquid chromatography

Comprehensive two-dimensional liquid chromatography (LC×LC) has received a great deal of attention during the past few years because of its extraordinary resolving power. The biggest advantage of this technique is that very high peak capacities can be generated in a relatively short time. Numerous approaches to maximize the peak capacity in LC×LC have been employed. In this work we investigate the impact of the first dimension mobile phase on selectivity. LC×LC has several potential advantages over one-dimensional LC (1DLC) in that unconventional solvents, at least in reversed-phase LC, can be used. For example, solvents which strongly adsorb in the UV in the first dimension are not problematic in LC×LC. This so because the UV detector is placed after the second dimensional column, as pulses of the first dimension eluent arrive at the second dimensional column, they elute well before the solutes of interest and therefore do not interfere at all with detection of solute peaks. So far, the most widely used solvents in reversed-phase 1DLC are methanol and acetonitrile. However, the "UV advantage" of 2DLC allows us to employ UV active solvents, such as acetone. We compare their differential selectivities to that of acetonitrile for the separation of 23 indole acetic acids of interest in plant biology. We also apply them to the separation of a maize seed extract, a very complex sample. In both sample sets, mobile phase composition can be an important parameter to increase the orthogonality of the two dimensions and thus, to increase the effective peak capacity of LC×LC.