目的研究在没有对照品的情况下鉴定检材中1-(4-氟苯基)-2-(N-吡咯烷基)-1-戊酮[1-(4-fluorophenyl)-2-(1-pyrrolidinyl)pentan-1-one,4-F-α-PVP]类似物1-(4-氟-3甲基苯基)-2-(N-吡咯烷基)-1-戊酮[1-(4-fluoro-3-methyl phenyl)-2-(1-py...目的研究在没有对照品的情况下鉴定检材中1-(4-氟苯基)-2-(N-吡咯烷基)-1-戊酮[1-(4-fluorophenyl)-2-(1-pyrrolidinyl)pentan-1-one,4-F-α-PVP]类似物1-(4-氟-3甲基苯基)-2-(N-吡咯烷基)-1-戊酮[1-(4-fluoro-3-methyl phenyl)-2-(1-pyrrolidinyl)pentan-1-one,4-F-3-Methyl-α-PVP]盐酸盐的方法。方法综合利用直接进样电子电离-质谱(electron ionization-mass spectrometry,EI-MS)、GCMS、电喷雾离子化-高分辨质谱(electrospray ionization-high resolution mass spectrometry,ESI-HRMS)、超高效液相色谱-高分辨串联质谱(ultra-high performance liquid chromatography-high resolution tandem mass spectrometry,UPLC-HRMS/MS)、核磁共振(nuclear magnetic resonance,NMR)、离子色谱和傅里叶变换红外光谱法(Fourier transform infrared spectroscopy,FTIR),实现对检材中未知化合物的结构解析与表征,并对该化合物在EI-MS和UPLC-HRMS/MS两种质谱分析方式下生成碎片离子的裂解机制进行推导。结果通过对检材中化合物的直接进样EI-MS、GC-MS、ESI-HRMS和UPLC-HRMS/MS分析,推断出未知化合物为4-F-α-PVP的结构类似物,可能苯环中多了1个甲基。根据核磁共振氢谱(1H-nuclear magnetic reso⁃nance,1 H-NMR)、核磁共振碳谱(13C-nuclear magnetic resonance,13C-NMR)等分析结果,进一步证明了甲基的位置在苯环的3-位。由于1H-NMR分析中实际氢的个数比4-F-3-Methyl-α-PVP中性分子多1个,推断该化合物以盐形式存在。离子色谱法分析结果表明该化合物含氯离子(含量11.14%~11.16%),结合FTIR对主要官能团信息的结构分析,最终确定该未知化合物为4-F-3-Methyl-α-PVP盐酸盐。结论建立了综合利用EI-MS、GC-MS、ESI-HRMS、UPLC-HRMS/MS、NMR、离子色谱和FTIR鉴定检材中4-F-3-Methyl-α-PVP盐酸盐的方法,将有助于法庭科学实验室在案件中鉴定该物质或其他具有类似结构的化合物。展开更多
The core-shell metastable intermolecular composites(MIC)have attracted much attention in the past few years due to their unique properties.Here,the preparation of Al-Core heterojunction fibers using PVP as a template ...The core-shell metastable intermolecular composites(MIC)have attracted much attention in the past few years due to their unique properties.Here,the preparation of Al-Core heterojunction fibers using PVP as a template is proposed.The nano-Al was directly added to the precursor solution of cupric acetate monohydrate(CAM)/Polyvinylpyrrolidone(PVP),and the initial Al@CAM/PVP fibers were obtained via electrospinning.The core-shell MIC fibers are then obtained by calcining the initial fibers.The morphology,structure,and composition of Al-core MIC fibers were characterized,that the energetic fibers calcined at 300℃,350℃,and 400℃have a core-shell structure with shell compositions CuxO and PVP,CuxO and Cu O,respectively.The energy release characteristics of Al-core MIC were investigated,and preliminary ignition tests were performed using an ignition temperature measuring instrument and a pulsed laser.The energetic fibers calcined at 300℃exhibited unique properties.The decomposition of PVP in the shell layer promoted exotherm,and a low-temperature exothermic peak was shown at 372-458℃.Lower ignition temperatures and higher flame heights were observed in the combustion tests than calcination at 350℃and 400℃.An unexpected result was that PVP can play a positive role in Al/CuO nanothermites.Simultaneously,this preparation method provided an idea for the integrated preparation of core-shell Al-Core MIC fibers and tuning the properties of MIC.展开更多
Spherical calcium carbonate was prepared by the reaction of sodium carbonate with calcium chloride at the presence of a protein like molecule, polyvinylpyrrolidone, as the template. The products were characterized by ...Spherical calcium carbonate was prepared by the reaction of sodium carbonate with calcium chloride at the presence of a protein like molecule, polyvinylpyrrolidone, as the template. The products were characterized by elemental analyses, XRD, SEM, and TG DSC respectively. The effects of polyvinylpyrrolidone on the crystal form and morphology of the as prepared CaCO3 were investigated. It was found that the aggregative shape of the produced calcium carbonate crystalline could be well controlled by adjusting the concentration of the polyvinylpyrrolidone template. This may be of important meanings to the biomimetic synthesis of novel inorganic materials.展开更多
文摘目的研究在没有对照品的情况下鉴定检材中1-(4-氟苯基)-2-(N-吡咯烷基)-1-戊酮[1-(4-fluorophenyl)-2-(1-pyrrolidinyl)pentan-1-one,4-F-α-PVP]类似物1-(4-氟-3甲基苯基)-2-(N-吡咯烷基)-1-戊酮[1-(4-fluoro-3-methyl phenyl)-2-(1-pyrrolidinyl)pentan-1-one,4-F-3-Methyl-α-PVP]盐酸盐的方法。方法综合利用直接进样电子电离-质谱(electron ionization-mass spectrometry,EI-MS)、GCMS、电喷雾离子化-高分辨质谱(electrospray ionization-high resolution mass spectrometry,ESI-HRMS)、超高效液相色谱-高分辨串联质谱(ultra-high performance liquid chromatography-high resolution tandem mass spectrometry,UPLC-HRMS/MS)、核磁共振(nuclear magnetic resonance,NMR)、离子色谱和傅里叶变换红外光谱法(Fourier transform infrared spectroscopy,FTIR),实现对检材中未知化合物的结构解析与表征,并对该化合物在EI-MS和UPLC-HRMS/MS两种质谱分析方式下生成碎片离子的裂解机制进行推导。结果通过对检材中化合物的直接进样EI-MS、GC-MS、ESI-HRMS和UPLC-HRMS/MS分析,推断出未知化合物为4-F-α-PVP的结构类似物,可能苯环中多了1个甲基。根据核磁共振氢谱(1H-nuclear magnetic reso⁃nance,1 H-NMR)、核磁共振碳谱(13C-nuclear magnetic resonance,13C-NMR)等分析结果,进一步证明了甲基的位置在苯环的3-位。由于1H-NMR分析中实际氢的个数比4-F-3-Methyl-α-PVP中性分子多1个,推断该化合物以盐形式存在。离子色谱法分析结果表明该化合物含氯离子(含量11.14%~11.16%),结合FTIR对主要官能团信息的结构分析,最终确定该未知化合物为4-F-3-Methyl-α-PVP盐酸盐。结论建立了综合利用EI-MS、GC-MS、ESI-HRMS、UPLC-HRMS/MS、NMR、离子色谱和FTIR鉴定检材中4-F-3-Methyl-α-PVP盐酸盐的方法,将有助于法庭科学实验室在案件中鉴定该物质或其他具有类似结构的化合物。
文摘The core-shell metastable intermolecular composites(MIC)have attracted much attention in the past few years due to their unique properties.Here,the preparation of Al-Core heterojunction fibers using PVP as a template is proposed.The nano-Al was directly added to the precursor solution of cupric acetate monohydrate(CAM)/Polyvinylpyrrolidone(PVP),and the initial Al@CAM/PVP fibers were obtained via electrospinning.The core-shell MIC fibers are then obtained by calcining the initial fibers.The morphology,structure,and composition of Al-core MIC fibers were characterized,that the energetic fibers calcined at 300℃,350℃,and 400℃have a core-shell structure with shell compositions CuxO and PVP,CuxO and Cu O,respectively.The energy release characteristics of Al-core MIC were investigated,and preliminary ignition tests were performed using an ignition temperature measuring instrument and a pulsed laser.The energetic fibers calcined at 300℃exhibited unique properties.The decomposition of PVP in the shell layer promoted exotherm,and a low-temperature exothermic peak was shown at 372-458℃.Lower ignition temperatures and higher flame heights were observed in the combustion tests than calcination at 350℃and 400℃.An unexpected result was that PVP can play a positive role in Al/CuO nanothermites.Simultaneously,this preparation method provided an idea for the integrated preparation of core-shell Al-Core MIC fibers and tuning the properties of MIC.
文摘Spherical calcium carbonate was prepared by the reaction of sodium carbonate with calcium chloride at the presence of a protein like molecule, polyvinylpyrrolidone, as the template. The products were characterized by elemental analyses, XRD, SEM, and TG DSC respectively. The effects of polyvinylpyrrolidone on the crystal form and morphology of the as prepared CaCO3 were investigated. It was found that the aggregative shape of the produced calcium carbonate crystalline could be well controlled by adjusting the concentration of the polyvinylpyrrolidone template. This may be of important meanings to the biomimetic synthesis of novel inorganic materials.
