Simultaneous determination of C1−C8 n-alkyl acetates and corresponding mono-, di- and trichloroacetates on glass capillary columns with programmed temperature rise

Summary Gas chromatography of mixtures of aliphaticn-alkyl acetates (CH₃–COOR), chloroacetates (CHCl₂–COOR), dichloroacetates (CHCl₂–COOR) and trichloroacetates (CCl₃–COOR), where the alcohol chain length (R) varied between 1 and 8, has been studied on SE-30, Carbowax 20M and OV-351 glass capillary columns with programmed temperatures from 50°C at 2, 4, 6, 8 and 10°C/min. Compounds in the homologous series are eluted in the direct order from methyl ton-octyl acetate. The isomeric chloro esters are eluted on SE-30 according to their boiling points in the order: mono-, di- and trichloro isomer, whereas on polar columns di- and trichloro esters are eluted in the reverse order. The complete separation of all 32 individual components from the mixture could not be reached by any single column, the best separation occurred on SE-30. The mixture can, however, be separated by using columns with polar and non-polar stationary phases. The relative retention times for the compounds are given and the retention order discussed.     

Free release static coating of glass capillary columns; Static coating at elevated pressure — Theoretical considerations and practice

Summary Static coating of glass capillary columns has hitherto solely been carried out by evaporation of the stationary phase solvents under vacuum conditions. However, since a solvent vapour pressure higher than the external pressure is the only requirement for the vapour to flow out of the column, evacuation should not be necessary. Several important factors in the static coating procedure, such as mass (solvent vapour) — and heat transfer, heat of vaporisation of the solvent and viscosity of the stationary phase solution at elevated temperature and outlet pressure are discussed, principally to rationalise an improved static coating procedure. The alternative, so-called free-release static coating procedure, was evaluated practically by coating several columns with OV-101 and SE-30. Coating speed was found to be rapid and relatively constant whereas coating efficiency was between 80 and 100%.     

The melt elastic behavior of polypropylene/glass bead composites in capillary flow

The melt extrudate swell and entry pressure losses are important characteristics of elastic properties during die extrusion of polymeric fluids. They are usually expressed with die-swell ratio (B) and entry pressure drop (ΔP_o). In the present paper, the die-swell behavior and entrance pressure drop of a polypropylene (PP) filled with A-glass beads were investigated by using a Rosand capillary rheometer to identify the effects of the filler contents and extrusion rate on the elastic behavior of the sample melts. The experiments were carried out under the conditions with an apparent shear rate range of 50–10⁴ s⁻¹ and a temperature of 190 °C. The results showed that B increased nonlinearly with increasing shear rate at the wall (γ_w), and increased linearly with the increase of shear stress at the wall (τ_w). With the increase of the volume fraction of the fillers B decreased nonlinearly. Similarly, the entry pressure drop increased linearly with the increase of τ_w, whereas the influence of the filler concentration on ΔP_o was insignificant in this case. Furthermore, B increased as a linear function of ΔP_o, and extension stress (σ_e) increased nonlinearly with increasing γ_w.     

Differential 3ω calorimeter

We have developed a new dynamic calorimeter using the differential 3ω detection method. The differential 3ω calorimeter is capable of measuring dynamic heat capacity of liquid samples. The new calorimeter consists of a Wheatstone bridge made of two identical heater/sensors, and is based on the sensitive null detection method. The balancing is done automatically at all frequencies and is independent of temperature; once a sample is placed on one heater/sensor, a third harmonic signal is produced due to the difference in the two arms of the bridge. The differential 3ω calorimeter provides enhancements over traditional dynamic methods in dynamic range (up to 30 kHz), resolution, and ease of operation.     

Preparation and characterization of bismaleimide/1,3-dicyanatobenzene modified epoxy intercrosslinked matrices

An intercrosslinked network of cyanate ester (CE)-bismaleimide (BMI) modified epoxy matrix system was made by using epoxy resin, 1,3-dicyanatobenzene and bismaleimide (N,N^′-bismaleimido-4,4^′-diphenyl methane) with diaminodiphenylmethane as curing agent. BMI-CE-epoxy matrices were characterised using differential scanning calorimetry (DSC), thermogravimetric analysis (TGA) and heat deflection temperature (HDT) analysis. The matrices, in the form of castings, were characterised for their mechanical properties such as tensile strength, flexural strength and unnotched Izod impact test as per ASTM methods. Mechanical studies indicated that the introduction of cyanate ester into epoxy resin improves the toughness and flexural strength with reduction in tensile strength and glass transition temperature, whereas the incorporation of bismaleimide into epoxy resin influences the mechanical and thermal properties according to its percentage content. DSC thermograms of cyanate ester as well as BMI modified epoxy resin show an unimodal reaction exotherm. Electrical properties were studied as per ASTM method and the morphology of the BMI modified epoxy and CE-epoxy systems were studied by scanning electron microscope.     

电感耦合等离子体原子发射光谱法测定玻璃中总硫

应用电感耦合等离子体原子发射光谱法(ICP-AES)测定了玻璃中总硫量。对测定条件,包括试样的溶解方法,分析谱线的选择,共存元素的光谱干扰及仪器的工作参数等作了系统研究。测定中选择了在紫外区的谱线(S 181.972 nm)作分析线可有效地避免了基体中大量钙的干扰。选取5件标准样品或已知样品按所提出方法各进行5次分析,算得方法的RSD值均小于1.5%,进行11次空白试验,算得方法的检出限(3S)为0.01 mg.L-1。通过对两件标准参考物质(NBS 89和GBW 03117)及一件已知样品的分析,验证了方法的准确度,所得测定结果与证书值或已知值相符。     

吸收湿气对微电子塑料封装影响的研究进展

微电子塑料封装中常用的聚合物材料因易于吸收周围环境中的湿气而对器件本身的可靠性带 来很大影响, 本文回顾了封装材料中湿气扩散、湿应力及蒸汽压力的产生这3个互相联系过 程的研究情况, 从理论分析、特征参数描述及其实验测定、有限元模拟分析的角度来分别予 以介绍.从已有的理论分析与实验结果中可以看出, 塑封材料吸收湿气会给器件的可靠性带 来诸多影响, 湿气的吸收、扩散、蒸发等过程, 实验测量, 以及由湿气带来的其它相关问题正 成为微电子封装可靠性研究领域中的新热点, 受到越来越多的关注与重视.     

一种用于Z箍缩实验的软X射线成像系统

基于塑料闪烁体转换和光学条纹相机的方法建立了一套用于Z箍缩实验中的软X射线条纹图像诊断系统,解决了以往实验中使用的X射线条纹相机易被电磁环境干扰以及相机电极部件易被实验产生的高速粒子损伤的问题.诊断系统的光谱响应范围主要集中在0.2—10 keV,系统的空间分辨率经过理论评估小于120μm,通过标定闪烁体对X射线的时间...     

X射线荧光光谱法分析玻璃纤维中主、次量元素成分

采用粉末压片-波长色散X射线荧光光谱法分析了中碱及无碱玻璃纤维中硅、铝、钙、镁、铁、钛、钾、钠、砷、氟等10种主、次量元素成分含量。以6个标准样品并结合两个参考样品建立校准曲线,采用DeJongh模式方程有效校正玻璃基体中元素间的吸收增强效应和重叠效应。该方法测定10个元素的精密度和准确度均较好,其相对标准偏差在0．35％～2．86％之间,对实际样品的分析结果与化学法相吻合,可应用于玻璃纤维中多元素成分的快速分析。     

孔梯度陶瓷纤维复合膜管的制备及特性

陶瓷过滤管具有孔隙率高、耐腐蚀、耐高温、机械强度高、便于清洗、使用寿命长等优点,是高温烟尘处理用的高效过滤元件.本文研制了一种具有梯度孔结构堇青石陶瓷纤维复合膜过滤元件,该过滤元件是由多孔支撑体、过渡层和分离膜层组成.其中支撑体、过渡层和分离层的气孔率分别为35～40;、50～60;和60～70;.文中主要分析了孔梯度陶瓷纤维复合膜管的材料结构和抗热震性能,同时对复合膜管进行含尘气体过滤的冷态模拟试验.对于烟气中粒径大于或等于0.1μm的颗粒,复合膜管的截留率达到99.8;以上.