甲基苯丙胺标准物质的定值与不确定度分析

为了建立法庭科学毒品检测量值溯源体系,研制了甲基苯丙胺纯度标准物质。通过红外光谱、质谱法对甲基苯丙胺样品进行定性分析,优化并建立了高效液相色谱(HPLC)、差示扫描量热法(DSC)两种定值分析方法。采用热重分析法和电感耦合等离子体质谱法测定水分和无机离子的含量。通过均匀性与稳定性检验结果表明,甲基苯丙胺标准物质的均匀性良好,稳定性至少1年,同时对其进行了不确定度评定。研制的甲基苯丙胺标准物质的纯度为99.8%,扩展不确定度为0.2%(k=2)。     

Characterization of different types of cellulose by dielectric spectroscopy

Various well dried solid celluloses, such as nativecelluloses from different sources, different pulps and regenerated cellulosefibers were compared by dielectric relaxation spectroscopy (DRS) in the lowfrequency (10 mHz to 5 MHz) and low temperature(–130 to 20 °C) range. No significant differences werefound in the polymeric dynamics. In addition, the influence of the watercontenton the -relaxation and the _wet relaxation wasinvestigated for morphologically very different celluloses such as cottonlinters, highly amorphous bead cellulose and lyocell fibers. The lyocell fiberswere investigated in the unmodified form and after modification by a treatmentwith alkali, after mild bleaching and after chemical crosslinking. It was foundthat the water content influences the dielectric dynamics and the intensityparameters differently for these different materials. NaOH-activation usingdifferent lye concentrations also influenced the dielectric dynamics. Finally,opportunities and limitations of DRS as a diagnostic tool are discussed.     

A consecutive one-pot two-step approach to novel trifluoromethyl-substituted bis(indolyl)methane derivatives promoted by Sc(OTf)3 and p-TSA

A one-pot two-step reaction of 3-(trifluoroacetyl)coumarin and indole afforded trifluoromethyl-substituted bis(indolyl)methane compounds containing coumarin skeleton. The atomic economic and simply manipulative reaction involved premier treatment of reaction mixtures with Sc(OTf)₃, followed by p-TSA in one-pot process. The reaction proceeded to give the title compounds in high yields (up to 95% yield).