Chromatographic quantitation using fractions of the peak areas

Quantitative chromatographic analysis is liable to errors due to peak asymmetry because the uncertainty in the detected position of the end of the peak tail decreases the reliability of the computed peak area. This dependence may be a severe drawback whenever peaks of different areas must be compared, as in the case of calibration curves. A new approach to overcome the uncertainties of area calculation due to peak asymmetry is reported in this paper. The approach consists of calculating only the area included between the start and the maximum of the chromatographic peak. Simulated and experimental chromatographic data were used in this study. Both the peak start-to-peak maximum area (SMA) and the start-to-end or total area (TA) were calculated and the quantitative results were compared. Within the scope of this work it is concluded that the SMA yields calibration curves that are more linear and have intercepts closer to zero than the calibration curves obtained using the TA.     

Multiple melting peak analysis with gel-spun ultra-high molar mass polyethylene

The multiple melting peaks observed on differential scanning calorimetry (DSC) of ultrahigh molar-mass polyethylene fibers (UHMMPE) are analyzed as a function of sample mass. Using modern DSC capable of recognizing single fibers of microgram size, it is shown that the multiple peaks are in part or completely due to sample packing. Loosely packed fibers fill the entire volume of the pan with rather large thermal resistance to heat flow. On melting, the fibers contract and flow to collect ultimately at the bottom of the pan. This process seems to be able to cause an artifact of multistage melting dependent on the properties of the fibers. A method is proposed to greatly reduce, or even eliminate, errors of this type. The crucial elements of the analysis of melting behavior and melting temperature are decreasing the sample size and packing the individual fibers in a proper geometry, or to introduce inert media to enhance heat transport.This work was supported by the Division of Materials Research, National Science Foundation, Polymers Program, Grant # DMR 90-00520 and the Division of Materials Sciences, Office of Basic Energy Sciences, US Department of Energy at Oak Ridge National Laboratory, managed by Lockheed Martin Energy Research Corp. for the US Department of Energy, under contract number DE-ACOS-96OR22464. Support for instrumentation came from TA Instruments, Inc. and Mettler-Toledo, research support was also given by ICI Paints.     

Report on the 42nd IUVSTA workshop ‘Electron scattering in solids: from fundamental concepts to practical applications’

A summary is given of the workshop entitled ‘Electron Scattering in Solids: from fundamental concepts to practical applications,’ which was held in Debrecen, Hungary, on July 4–8, 2004, under the sponsorship of the International Union of Vacuum Science, Technique, and Applications (IUVSTA). This workshop was held to review the present status and level of understanding of electron‐scattering processes in solids, to identify issues of key importance (hot topics) in the light of the most recent scientific results, and to stimulate discussions leading to a deeper understanding and new solutions of current problems. This report contains summaries of presentations and discussions in sessions on elastic scattering of electrons by atoms and solids, inelastic scattering of electrons in solids, modeling of electron transport in solids and applications, and software. The principal areas of application include Auger‐electron spectroscopy (AES), X‐ray photoelectron spectroscopy, elastic‐peak electron spectroscopy (EPES), reflection electron energy‐loss spectroscopy (REELS), secondary‐electron microscopy, electron‐probe microanalysis (EPMA), and the use of coincidence techniques in electron‐scattering experiments. A major focus of the workshop was determination of the inelastic mean free path of electrons for various surface spectroscopies, particularly corrections for surface and core‐hole effects. Published in 2005 by John Wiley & Sons, Ltd.     

动力学-双波长法测定岩石矿物中痕量铼及负峰可测性研究

铼(Ⅳ)催化α-呋喃甲酰二肟(α-FDO)酸解反应,在一定条件下其光谱的正、负峰吸光度之和与时间星线性并与铼浓度相关。据此,建立了动力学一双波长测定痕量铼的方法。方法检出限为0.05ng/ml,铼浓度在<10ng/ml范围线性颇佳,表观摩尔吸光系数ε为4.5×10~7L·mol(-1)·cm~(-1)。方法用于辉钼矿和岩石中痕量铼的测定,结果与中子活化等方法相符。本文还就本体系为例对分光光度法中负峰的出现和可测规律进行了探讨。     

OBSERVATION OF ENERGY DISSIPATION PEAK IN POLYSTYRENE MELT ABOVE Tg

In this paper two different kinds of dynamic mechanical techniques(inversed torsion pendulum and energy dissipation apparatus)were used to study the dynamic behavior of atactic monodisperse polystyrene above glass transition. The plots of energy dissipation versus temperature were presented for two atactic polystyrene samples.An apparent energy dissipation peak occurred above T_g in each plot measured by the inversed torsion pendulum,and simultaneously the sample was found to flow assuredly at the moment.To exclude the influence of the flow and demonstrate there was a peak indeed above T_g,the energy dissipation apparatus was used,in which the samples were put into a cup.An obvious peak appeared, and it was in agreement with the peak observed by the inversed torsion pendulum.On basis of the results measured by the two kinds of apparatus,a conclusion is drawn that a peak occurrs above T_g,which gives a manifestation for the existence of the liquid-liquid transition.     

Dependence of the width of the chromatographic zone on retention time in capillary gas chromatography

The dependence of the width of the chromatographic zone on retention time for capillary columns was studied theoretically and experimentally. Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 2, pp. 320–322, February, 1997.     

非紧密堆积型光子晶体凝胶的胀缩行为

制备了Bragg衍射峰波长位置在700～800 nm之间的非紧密堆积型光子晶体凝胶(NCPPCGs). 通过自然干燥失水, 复水浸泡, 不同浓度的乙醇溶液浸泡和不同pH缓冲溶液浸泡等处理, 研究了NCPPCGs的溶胀、收缩(胀缩)行为和Bragg衍射峰迁移的关系; 在凝胶自然干燥失水过程中, Bragg衍射峰蓝移, 复水浸泡后, Bragg衍射峰快速红移至干燥前的位置; 凝胶经不同浓度的乙醇溶液浸泡后, 凝胶体积改变, 并且乙醇浓度升高时, Bragg衍射峰蓝移; 经水解处理的NCPPCGs具有pH 响应特性, 当其浸泡在pH为2.2～9.6的缓冲溶液中时, 随pH值的增大Bragg衍射峰红移, pH为9.6～10.6时, Bragg衍射峰蓝移. 外界因素导致NCPPCGs的Bragg衍射峰位置的迁移覆盖整个可见光区域.     

A cryogenic blackbody for millimeter wavelengths

We describe a cryogenic blackbody reference, or cold load for millimeter wavelength radiation. This blackbody has an emissivity 0.99 over a two octave wavelength range. We use it as a standard when calibrating sensitive infrared photometers. The particular geometry of the blackbody described is influenced by our application. The basic design data and philosophy are described so that other designs can be evaluated.     

Chromatogram surgery

A computer program is developed on a Hewlett-Packard 3354 B Laboratory Automation System to eliminate background in gas and liquid chromatograms. Moreover undesired peaks, such as solvent peaks and spikes, can be excluded by selecting appropriate method parameters or by application of the integrator-timed events directly affecting peak integration. Injudicious application of these codes deforms the chromatograms. Peaks can be labelled with retention times, areas or amounts.