Sn-Pb合金颗粒异质成核及其冷却凝固行为预测

采用均匀颗粒成型法 (UniformDropletSpray ,UDS)在氮气氛下 (氧含量为 1.3 6μmol/L)制备了 15 0和 185μmSn 5 %Pb合金颗粒 .采用光学显微镜观测颗粒的外观形貌 ,结果表明 ,UDS方法制备的微粒是粒度均匀的球状颗粒 ;利用非绝热容量法确定了颗粒的形核点及过冷度 ;计算了以时间和温度为函数的颗粒表面被氧化的比例 ,提出了以颗粒表面氧化为催化媒质的异质成核理论模型 ,合理反映了颗粒的异质成核过程 .在此基础上计算了微粒表面异质形核条件下的连续冷却转变 (ContinuousCoolingTransformation ,CCT)曲线 ,同时以线性冷却条件为例预测了颗粒的冷却凝固行为 .     

Quantification of two chromatographic unresolved dichlorophenols using gas chromatography-direct deposition-fourier transform infrared spectrometry and multivariate calibration

A method for the quantification of two chromatographically unresolved dichlorophenol isomers in water is described. Acetylation and concentration on graphitized carbon cartridges are carried out as a preliminary step. Detection is made by gas chromatography (GC) coupled to Fourier transform infrared spectroscopy (FTIR), using a direct deposition interface (DD). Infrared spectra in the maximum of the unresolved peak of 2,5- and 2,4-dichlorophenol for a series of standards with different amounts of these two compounds are used, to elaborate a multivariate calibration model (PLS-1 algorithm). By the method described, concentrations of dichlorophenol isomers in water at ng/ml level can be determined.     

超声波作用下天然气水合物的形成

实验搭建了一套高压条件下超声波作用于天然气水合物反应的装置系统，该系统中超声波的频率为20kHz，功率为0-150W可调。利用该装置研究了超声波对天然气水合物生成过程和引导时间的影响。实验发现声场中生成特征曲线诸如温度、压力、流量等随着时间的推迟与静态反应时不同，反应引导时间约缩短至静态时的1／6，分解后重新反应引导时间甚至缩短至静态的1／10。水合物成核速率提高是由于超声波提高了传质系数、成核点浓度和过饱和度，而降低了界面能。     

Determination of alcohol content in beverages using short-wave near-infrared spectroscopy and temperature correction by transfer calibration procedures

This paper reports the utilization of short-wave near-infrared (SW-NIR) transmission spectroscopy for rapid and conclusive analysis of alcoholic content (% v/v) in beverages. This spectral region is interesting because common visible diode array spectrometers can be utilized, reducing time and costs in comparison with traditional near-infrared or mid-infrared instruments. A correction of external temperature influence is necessary, and for this purposes two calibration transfer procedures were compared: piecewise direct standardization (PDS) and orthogonal signal correction (OSC). The RMSEP found for the alcoholic content model at 20 °C was 0.13% v/v and, after application of transfer calibration procedures at other temperatures (15, 25, 30 and 35 °C) using the model built at 20 °C, errors of the same order of magnitude were obtained.     

Infrared spectroscopy and the characterization of terfenadine crystallized from solvents

In this paper the structural characterization of terfenadine crystallized from ethanol-water, ethanol and methanol is performed by infrared spectroscopy. The OH stretching vibration, composed of three markedly overlapped bands, is analyzed by peak fitting. The assignment of the hydrogen bonds was conducted making use of band parameters, spectroscopic data for CCl₄ solutions, and molecular dynamics calculations from dimeric systems. Terfenadine just precipitated from solvents is never in the highest crystalline state. This state is reached when the samples are heated at a temperature above 100°C. Some amorphous solid is coprecipitated with the crystalline phase, particularly in methanol. This revised version was published online in August 2006 with corrections to the Cover Date.     

碘标准溶液配制方法改进

提出了直接法配制碘标准溶液。首先在强碱性环境下完成碘的歧化,然后以碘化钾作助溶剂,强酸环境下实现反歧化,再静置36 h,即可得到碘标准溶液。进行了硫代硫酸钠标定实验和维生素C测定实验,探讨了碘溶液浓度的稳定性。结果表明,直接法配制的碘标准溶液,准确度高,保存时间长,标定误差小于0.1%;样品分析偏差小于0.2%。     

Chemometrics‐assisted liquid chromatography with full scan mass spectrometry for the interference‐free determination of glucocorticoids illegally added to face masks

A smart chemometrics‐assisted strategy that combines the full scan mode of liquid chromatography with mass spectrometry with second‐order calibration method based on alternating trilinear decomposition algorithm was developed for the rapid determination of 15 glucocorticoids including the epimers betamethasone and dexamethasone illegally added into face masks. Fifteen glucocorticoids were rapidly eluted (11 min) under a simple elution program. By means of the second‐order calibration method, 15 target analytes were successfully quantified in the presence of peak overlaps, unknown interferences and baseline drifts. Notably, the epimers, namely, betamethasone and dexamethasone, were simultaneously quantified by the proposed method under a simple elution program. The average spiked recoveries for all target analytes ranged from 87.3 ± 2.2 to 119.4 ± 5.8%. The validation parameters including sensitivity, selectivity, limit of detection, limit of quantitation, and precision were calculated to validate the accuracy of the proposed method, and the quantitative analysis results were further confirmed by liquid chromatography with tandem mass spectrometry. All results proved that the proposed chemometrics‐assisted liquid chromatography with mass spectrometry strategy was an accurate and fast method to determine epimers and multiple glucocorticoids in complex face mask samples.