会聚光在柱状模拟生物组织中的实验研究

在中空的柱状有机玻璃中充入Intralipid-10%溶液构成单层圆柱模拟样品.在会聚单色光入射Intralipid-10%溶液的情况下,利用特制的光纤探头、锁相放大器、斩波器和微动平台等组成测试装置,测量了柱状Intralipid-10%溶液内后向散射光、能流率的空间分布情况,并对测量结果进行分析.对参量不同的溶液中的光分布进行了比较,得出了柱状溶液中光分布的初步规律.     

Vacuum-assisted headspace solid phase microextraction: Improved extraction of semivolatiles by non-equilibrium headspace sampling under reduced pressure conditions

A new headspace solid-phase microextraction (HSSPME) procedure carried out under vacuum conditions is proposed here where sample volumes commonly used in HSSPME (9 mL) were introduced into pre-evacuated commercially available large sampling chambers (1000 mL) prior to HSSPME sampling. The proposed procedure ensured reproducible conditions for HSSPME and excluded the possibility of analyte losses. A theoretical model was formulated demonstrating for the first time the pressure dependence of HSSPME sampling procedure under non equilibrium conditions. Although reduced pressure conditions during HSSPME sampling are not expected to increase the amount of analytes extracted at equilibrium, they greatly increase extraction rates compared to HSSPME under atmospheric pressure due to the enhancement of evaporation rates in the presence of an air-evacuated headspace. The effect is larger for semivolatiles whose evaporation rates are controlled by mass transfer resistance in the thin gas film adjacent to the sample/headspace interface. Parameters that affect HSSPME extraction were investigated under both vacuum and atmospheric conditions and the experimental data obtained were used to discuss and verify the theory. The use of an excessively large headspace volume was also considered. The applicability of Vac-HSSPME was assessed using chlorophenols as model compounds yielding linearities better than 0.9915 and detection limits in the low-ppt level. The repeatability was found to vary from 3.1 to 8.6%.     

Disposable pipette tips extraction: Fundamentals,applications and state of the art

Disposable pipette tips extraction consists of a solid‐phase extraction in which the sorbent is poorly dispersed in a pipette tip, which allows a quick and dynamic contact between the aspirated analyte from the sample and the solid phase. It is a technique used particularly in food and forensic analysis, since it requires a small amount of sample and solvent. This article highlights the principles, advantages and disadvantages of the disposable pipette tips extraction method and reviews recent applications.     

X-Ray powder diffraction study of structural phase transitions in (Ba0.5Sr0.5)PbO3 perovskite

Study of structural properties of (Ba_0.5Sr_0.5)PbO₃ has been carried out in a wide temperature range from 10 to 1223 K using the X-ray powder diffraction technique. Two temperature-induced structural phase transitions at 948 and 1198 K have been found. For polycrystallines the XPS and electrical resistivity measurements have been performed.     

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.     

Alkyne oligomerization catalyzed by molybdenum(0) complexes

Three new molybdenum(0) complexes, [Mo(CO)₃(Hpz)₃] (1), [Mo(CO)₂(Hpz)₂(DMAD)₂] (2), (DMAD=dimethyl acetylenedicarboxylate) and [Mo(CO)₃(1-Me-imidazole)₃] (3) were synthesized and characterized. Their activity and selectivity in alkyne cyclotrimerization and co-trimerization reactions was investigated. The molecular structures of 1 and 2 have been determined by unconventional powder and standard single-crystal diffraction methods, respectively. 1 consists of a pseudo-octahedral complex of C₃ symmetry, with the ligands in fac disposition; complex 2, of idealized C₂ symmetry, is obtained by substitution of one CO and one pyrazole in 1 by two DMAD ligands, and shows the rare trans configuration of π-bound acetylenic moieties.     

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.