Shorter nonparametric prediction intervals for an order statistic from a future sample

Standard nonparametric prediction intervals for a future order statistic are obtained by taking the interval between two order statistics of the initial sample. We obtain improved prediction intervals by taking the shortest of two or more standard intervals.     

微通道板表面发雾的AES分析

应用俄歇电子能谱对微通道板表面发雾区域进行分析。分析结果表明,发雾区碳含量比正常区高三倍。由此可推测出,发雾是由碳污染引起的,而这种碳污染很可能是残留于微通道板上的某些有机物在烧氢时碳化所致。     

Optimal electric fields for different sample shapes in high resolution NMR spectroscopy

For many applications, reducing sample resistance, rather than increasing probe Q or filling factor, is the only way to further improve the signal-to-noise ratio of cryogenically cooled NMR probes. In this paper, bounds are calculated for the minimum sample resistance that can be achieved for various sample geometries. The sample resistance of 100 mM NaCl in H(2)O in 5 mm sample tubes was measured on a 600 MHz cold probe to be within 14% of the optimum value. The minimum sample resistance can however be lowered by altering the tube cross section. Rectangular tubes oriented with the long axis along the RF magnetic field are particularly favourable.     

Variable temperature system using vortex tube cooling and fiber optic temperature measurement for low temperature magic angle spinning NMR

We describe the construction and operation of a variable temperature (VT) system for a high field fast magic angle spinning (MAS) probe. The probe is used in NMR investigations of biological macromolecules, where stable setting and continuous measurement of the temperature over periods of several days are required in order to prevent sample overheating and degradation. The VT system described is used at and below room temperature. A vortex tube is used to provide cooling in the temperature range of -20 to 20 degrees C, while a liquid nitrogen-cooled heat exchanger is used below -20 degrees C. Using this arrangement, the lowest temperature that is practically achievable is -140 degrees C. Measurement of the air temperature near the spinning rotor is accomplished using a fiber optic thermometer that utilizes the temperature dependence of the absorption edge of GaAs. The absorption edge of GaAs also has a magnetic field dependence that we have measured and corrected for. This dependence was calibrated at several field strengths using the well-known temperature dependence of the (1)H chemical shift difference of the protons in methanol.     

Liquid-liquid extraction followed by solid-phase extraction for the determination of lipophilic pesticides in beeswax by gas chromatography-electron-capture detection and matrix-matched calibration

Analytical methods for the simultaneous analysis of lindane, chlorpyriphos, z-chlorfenvinphos, endosulfan A and B, 4,4'-DDE, 4,4'-TDE, acrinathrine, bromopropylate, tetradifon, coumaphos and fluvalinate in pure beeswax samples are studied. For the analysis of bleached beeswaxes, a liquid-liquid extraction with acetonitrile followed by a clean-up on polymeric cartridges is the best option in terms of recovery and precision. However, some interferences that hinder the identification and quantification of important varroacides are found when non-bleached beeswaxes are analyzed. The analysis of all compounds in the latter samples require a clean-up by coupling an ODS cartridge before the polymeric cartridge. Considerations about the influence of the matrix in the quantitative analysis by a classical external standard calibration are also made and the use of a matrix-matched calibration is advised. Recoveries resulted to be about 100% with coefficients of variation between 10% and 20% (n = 5) for concentrations of 0.5 and 5 mg/kg.     

无溶剂顶空气相色谱法测定盐酸左氧氟沙星残留溶剂

采用无溶剂-顶空-气相色谱直接测定盐酸左氧氟沙星中残留溶剂乙醇、甲苯、二甲基亚砜(DMSO)等.各残留溶剂的检出限分别在0.007-0.032 μg,6次测定的相对标准偏差RSD在1.84%-1.92%,加标回收在90.9%-110%.方法简便、快速、灵敏,可应用于其他药品中残留溶剂的分析.     

Total analysis of surface structure and properties by UHV transfer system

We have developed an ultrahigh-vacuum (UHV) complex sample preparation and analysis system, which realizes a reliable surface science analyzing various characters on an identical surface. The system contains three sample-preparation-and-characterization chambers and five analysis chambers. They are (1) an electronic-properties-characterization chamber, (2) a magnetic-properties-characterization chamber, (3) an organic-molecule chamber, (4) UHV SEM, (5) a high-energy-resolution angle-resolved photoelectron spectrometer, (6) a high-energy-resolution display-type spherical mirror analyzer, (7) a room-temperature (RT) STM, and (8) an optical-properties characterization chamber. A special sample holder is used with six electrodes on it, which enables accurate temperature measurement of a sample by connecting a thermocouple directly to the sample even if it is transferred. Four other electrodes can be used for construction of various circuits including evaporators. Some examples are shown.     

Pervaporation in chemical analysis

Unlike thermal processes such as distillation, pervaporation relies on the relative rates of solute permeation through a membrane and is a combination of evaporation and gas diffusion. The analytical pervaporation systems consist of a membrane module suitable for liquid sample introduction and a vacuum (or a sweeping gas) on the permeate side. It has been used in a wide range of applications including the analysis of various organic and inorganic compounds, and sample concentration. It has been directly interfaced with gas chromatography, spectrophotometry, capillary electrophoresis, electrochemical detectors, liquid chromatography, and mass spectrometry. A wide range of liquids, slurries, and solids samples has been analyzed using these techniques. This review highlights the basic principles of the pervaporation and the state of its current development as applied to analytical chemistry.