同步辐射(Synchrotron Radiation,SR)红外光具有亮度高、光谱范围宽等优异的性质。基于上海同步辐射光源(Shanghai Synchrotron Radiation Facility,SSRF)建设的国家蛋白质科学研究(上海)设施(National Facility for Protein Science,NF...同步辐射(Synchrotron Radiation,SR)红外光具有亮度高、光谱范围宽等优异的性质。基于上海同步辐射光源(Shanghai Synchrotron Radiation Facility,SSRF)建设的国家蛋白质科学研究(上海)设施(National Facility for Protein Science,NFPS)BL01B红外线站可进行高分辨的傅里叶变换红外(FTIR)显微研究,空间分辨率可达衍射极限。自2015年红外线站正式开放以来,来自多个领域的课题组与红外线站合作做出了诸多创新性的重要成果。本综述将对近三年内BL01B红外线站的用户应用成果进行介绍,并对同步辐射傅里叶变换红外光谱(SR-FTIR)技术的发展和应用进行讨论。这些应用涉及材料科学、环境科学、药物科学、细胞生物学和高压科学等领域。展开更多
目的建立安钠咖样品中咖啡因和苯甲酸钠快速定性和定量分析的红外光谱方法。方法采用高纯度咖啡因和苯甲酸钠混合制样的方法制备定性和定量建模样品,通过分析混合样品的红外光谱图,确定安钠咖样品中咖啡因和苯甲酸钠的特征吸收峰。采用...目的建立安钠咖样品中咖啡因和苯甲酸钠快速定性和定量分析的红外光谱方法。方法采用高纯度咖啡因和苯甲酸钠混合制样的方法制备定性和定量建模样品,通过分析混合样品的红外光谱图,确定安钠咖样品中咖啡因和苯甲酸钠的特征吸收峰。采用偏最小二乘法(partial least squares,PLS)建立红外光谱定量模型。结果通过分析17个咖啡因和苯甲酸钠混合样品(咖啡因纯度范围10%~80%)的红外光谱图,确定了咖啡因的特征吸收峰为1698、1650、1237、972、743、609cm-1;苯甲酸钠的特征吸收峰为1596、1548、1406、845、708、679cm-1。将所有特征吸收峰均检出作为阳性判断依据时,48个安钠咖缴获样品中咖啡因和苯甲酸钠的阳性检出率均为100%。咖啡因PLS定量模型的线性范围为10%~80%,决定系数(R2)为99.9%,交叉验证均方差(root mean square error of cross validation,RMSECV)为0.68%,预测均方差(root mean square error of prediction,RMSEP)为0.91%;苯甲酸钠PLS定量模型的线性范围为20%~90%,R2为99.9%,RMSECV为0.91%,RMSEP为1.11%。配对样本t检验结果显示,高效液相色谱法和红外光谱法的测定结果差异无统计学意义。采用所建立的红外定量方法分析48个安钠咖缴获样品,咖啡因的纯度为27.6%~63.1%,苯甲酸钠的纯度为36.9%~72.3%。结论采用红外光谱法对安钠咖样品中的咖啡因和苯甲酸钠进行快速定性和定量分析,可提高检验鉴定效率、降低检验成本。展开更多
目的应用衰减全反射傅里叶变换红外(attenuated total reflection-Fourier transform infrared,ATRFTIR)光谱技术分析长白猪死后肋软骨和肋骨组织随死亡时间推移的化学降解过程,为死后较长时间段内推断死亡时间提供可行的新途径和方法...目的应用衰减全反射傅里叶变换红外(attenuated total reflection-Fourier transform infrared,ATRFTIR)光谱技术分析长白猪死后肋软骨和肋骨组织随死亡时间推移的化学降解过程,为死后较长时间段内推断死亡时间提供可行的新途径和方法。方法猪放血处死后取肋软骨和肋骨离体置于20℃环境,后每72 h提取部分组织样本,进行ATR-FTIR光谱分析,并与对应死亡时间点进行相关性分析。结果随死亡时间的延长,肋软骨与肋骨FTIR的主要吸收峰峰位没有发生明显变化,而其部分峰强比出现了不同时序性的变化趋势,并与死亡时间存在良好的相关性,肋软骨较肋骨组织有更好的时序性。结论应用ATRFTIR光谱技术发现死后猪肋软骨和肋骨组织光谱学变化存在一定的规律性,有望成为基于光谱学推断死亡时间的一种新途径。展开更多
Two kinds of UV curable polyurethane acrylate oligomers （PUPA and PUCA） were synthesized via the addition reaction between isophorone diisocyanate （IPDI） and polyethylene glycol monoacrylate （PEA6） or polycaprol...Two kinds of UV curable polyurethane acrylate oligomers （PUPA and PUCA） were synthesized via the addition reaction between isophorone diisocyanate （IPDI） and polyethylene glycol monoacrylate （PEA6） or polycaprolactone modified hydroxyethyl acrylate （PCLA2）. The structures of PUPA and PUCA were characterized by Fourier transform infrared spectroscopy （FT-IR）, IH nuclear magnetic resonance （^H NMR）, gel permeation chromatography （GPC） and differential scanning calorimeter （DSC）, and the thermal stability and dynamic mechanical thermal properties of their cured films were measured by thermogravimetric analysis （TGA） and dynamic mechanical analysis （DMA）, respectively. The viscosity of the oligomers and mechanical properties of the cured films were also studied. The results show that both oligomers have narrow molecular weight distribution. The viscosity of PUPA is 2.310 Pa.s at 25 ℃, while that of PUCA is： up to 3.980 Pa-s. The UV cured PUPA and PUCA films have homogeneous phase structure, and the PUCA film shows higher glass transition temperature and storage modulus. Furthermore, the PUCA film possesses better mechanical properties than PUPA, while the latter shows better alkali resistance.展开更多
In situ studies of catalysts play valuable roles in observing phase transformation, understanding the corresponding surface chemistry and the mechanism of the reaction. In this paper, ceria promoted cobalt oxide was p...In situ studies of catalysts play valuable roles in observing phase transformation, understanding the corresponding surface chemistry and the mechanism of the reaction. In this paper, ceria promoted cobalt oxide was prepared by the calcination method and investigated for the CO oxidation. The microstructure and morphology of CeO2-Co3O4 were investigated by the Scanning Electron Microscope, High-resolution transmission electron microscopy, Raman and X-ray photoelectron spectroscopy characterization. The effect of CeO2 doping on Co3O4 for CO oxidation was characterized by in situ X-ray Diffraction (in situ XRD) and in situ diffuse reflectance infrared Fourier transform spectroscopy (in situ DRIFTS). In situ XRD was carried out under H2 atmosphere to evaluate the redox property of catalysts. The results indicated that the ceria doping can enhance the reducibility of Co2+ and promote the Co3+-Co2+-Co3+ cycle, owing to the oxygen replenish property of CeO2. Furthermore, adsorbed carbonate species on the surface of CeO2-Co3O4 were investigated by in situ-DRIFTS experiment. It was turned out that carbonate species on ceria promoted cobalt oxide catalysts showed different IR peaks compared with pure cobalt oxide. The carbonate species on ceria promoted catalyst are more active, and similar to free state carbonate species with weak bonding to catalyst surface, which can effectively inhibit catalyst inactivation. This study revealed the mechanism of ceria promoting CO oxidation over cobalt oxide, which will provide theoretical support for the design of efficient CO oxidation catalysts.展开更多
The distribution and verticals variation of geochemical components in the Kasnau-Matasukh lignites of Nagaur Basin, Rajasthan, were investigated using microscopy, proximate and ultimate analyses, Rock-Eval Pyrolysis, ...The distribution and verticals variation of geochemical components in the Kasnau-Matasukh lignites of Nagaur Basin, Rajasthan, were investigated using microscopy, proximate and ultimate analyses, Rock-Eval Pyrolysis, X-ray diffraction and Fourier Transform Infrared analyses, and major/minor/trace element determination. The relationship of elements with ash content and with macerals have also been discussed. These lignites are stratified, black, dominantly composed of huminite group macerals with subordinated amounts of liptinite and inertinite groups. They are classified as type-III kerogen and are mainly gas prone in nature. The concentration （in vol%） of mineral matter is seen to increase towards upper part of seam and so is the concentration （in wt%） of the volatile matter, elemental carbon and sulphur. The common minerals present in these lignitesare mixed clay layer, chlorite, and quartz as identified by X-ray diffraction study. Compared with world average in brown coal, the bulk concentration of Cu is anomalously high in most of the samples while Cd is 2-3 times high and Zn is high in one band. Based on interrelationship, different pyrite forms are noticed to have different preferential enrichment of various elements. The concentration of disseminated pyrite is more than the other pyrite forms and is followed by discrete pyrite grains and massive pyrite.展开更多
文摘目的运用傅里叶变换红外(Fourier transform infrared,FTIR)光谱技术分析大鼠死后15d内背部皮肤的光谱变化,以此推断死亡时间。方法大鼠麻醉后颈椎脱臼处死,置于温度为25℃、湿度为50%的环境中,分别于不同时间点提取其背部皮肤,收集红外光谱数据,并利用机器学习技术对数据进行分析。结果大鼠死后背部皮肤组织光谱吸收峰的峰位未发生明显改变,其强度随死亡时间延长而发生变化;偏最小二乘(partial least squares,PLS)回归构建的死亡时间推断模型决定系数(R2)为0.92,预测均方根误差为1.30 d。根据模型中的变量投影重要性(variable importance for projection,VIP)指标确定推断死亡时间的贡献波段为1760~1700cm-1、1660~1640cm-1、1580~1540cm-1和1460~1420cm-1。结论应用FTIR技术检测大鼠死后皮肤组织的光谱学改变,为死亡时间推断提供了一种新的思路。
文摘同步辐射(Synchrotron Radiation,SR)红外光具有亮度高、光谱范围宽等优异的性质。基于上海同步辐射光源(Shanghai Synchrotron Radiation Facility,SSRF)建设的国家蛋白质科学研究(上海)设施(National Facility for Protein Science,NFPS)BL01B红外线站可进行高分辨的傅里叶变换红外(FTIR)显微研究,空间分辨率可达衍射极限。自2015年红外线站正式开放以来,来自多个领域的课题组与红外线站合作做出了诸多创新性的重要成果。本综述将对近三年内BL01B红外线站的用户应用成果进行介绍,并对同步辐射傅里叶变换红外光谱(SR-FTIR)技术的发展和应用进行讨论。这些应用涉及材料科学、环境科学、药物科学、细胞生物学和高压科学等领域。
文摘目的建立安钠咖样品中咖啡因和苯甲酸钠快速定性和定量分析的红外光谱方法。方法采用高纯度咖啡因和苯甲酸钠混合制样的方法制备定性和定量建模样品,通过分析混合样品的红外光谱图,确定安钠咖样品中咖啡因和苯甲酸钠的特征吸收峰。采用偏最小二乘法(partial least squares,PLS)建立红外光谱定量模型。结果通过分析17个咖啡因和苯甲酸钠混合样品(咖啡因纯度范围10%~80%)的红外光谱图,确定了咖啡因的特征吸收峰为1698、1650、1237、972、743、609cm-1;苯甲酸钠的特征吸收峰为1596、1548、1406、845、708、679cm-1。将所有特征吸收峰均检出作为阳性判断依据时,48个安钠咖缴获样品中咖啡因和苯甲酸钠的阳性检出率均为100%。咖啡因PLS定量模型的线性范围为10%~80%,决定系数(R2)为99.9%,交叉验证均方差(root mean square error of cross validation,RMSECV)为0.68%,预测均方差(root mean square error of prediction,RMSEP)为0.91%;苯甲酸钠PLS定量模型的线性范围为20%~90%,R2为99.9%,RMSECV为0.91%,RMSEP为1.11%。配对样本t检验结果显示,高效液相色谱法和红外光谱法的测定结果差异无统计学意义。采用所建立的红外定量方法分析48个安钠咖缴获样品,咖啡因的纯度为27.6%~63.1%,苯甲酸钠的纯度为36.9%~72.3%。结论采用红外光谱法对安钠咖样品中的咖啡因和苯甲酸钠进行快速定性和定量分析,可提高检验鉴定效率、降低检验成本。
基金Project(2007168303) supported by Guangdong-Hong Kong Technology Cooperation Funding
文摘Two kinds of UV curable polyurethane acrylate oligomers （PUPA and PUCA） were synthesized via the addition reaction between isophorone diisocyanate （IPDI） and polyethylene glycol monoacrylate （PEA6） or polycaprolactone modified hydroxyethyl acrylate （PCLA2）. The structures of PUPA and PUCA were characterized by Fourier transform infrared spectroscopy （FT-IR）, IH nuclear magnetic resonance （^H NMR）, gel permeation chromatography （GPC） and differential scanning calorimeter （DSC）, and the thermal stability and dynamic mechanical thermal properties of their cured films were measured by thermogravimetric analysis （TGA） and dynamic mechanical analysis （DMA）, respectively. The viscosity of the oligomers and mechanical properties of the cured films were also studied. The results show that both oligomers have narrow molecular weight distribution. The viscosity of PUPA is 2.310 Pa.s at 25 ℃, while that of PUCA is： up to 3.980 Pa-s. The UV cured PUPA and PUCA films have homogeneous phase structure, and the PUCA film shows higher glass transition temperature and storage modulus. Furthermore, the PUCA film possesses better mechanical properties than PUPA, while the latter shows better alkali resistance.
基金supported by the State Key Research Development Program of China(2016YFA0204200)the National Natural Science Foundation of China(21822603,21577036,21773062)+3 种基金the Shanghai Pujiang Program(17PJD011)the Zhejiang public welfare technology research plan/rural agriculture(LGN18B010001)the Zhejiang provincial Collaborative Innovation Center of Agricultural Biological Resources Biochemical Manufacturing(NO:2016KF0005)the scientific research project of Zhejiang provincial education department(Y201839892)~~
文摘In situ studies of catalysts play valuable roles in observing phase transformation, understanding the corresponding surface chemistry and the mechanism of the reaction. In this paper, ceria promoted cobalt oxide was prepared by the calcination method and investigated for the CO oxidation. The microstructure and morphology of CeO2-Co3O4 were investigated by the Scanning Electron Microscope, High-resolution transmission electron microscopy, Raman and X-ray photoelectron spectroscopy characterization. The effect of CeO2 doping on Co3O4 for CO oxidation was characterized by in situ X-ray Diffraction (in situ XRD) and in situ diffuse reflectance infrared Fourier transform spectroscopy (in situ DRIFTS). In situ XRD was carried out under H2 atmosphere to evaluate the redox property of catalysts. The results indicated that the ceria doping can enhance the reducibility of Co2+ and promote the Co3+-Co2+-Co3+ cycle, owing to the oxygen replenish property of CeO2. Furthermore, adsorbed carbonate species on the surface of CeO2-Co3O4 were investigated by in situ-DRIFTS experiment. It was turned out that carbonate species on ceria promoted cobalt oxide catalysts showed different IR peaks compared with pure cobalt oxide. The carbonate species on ceria promoted catalyst are more active, and similar to free state carbonate species with weak bonding to catalyst surface, which can effectively inhibit catalyst inactivation. This study revealed the mechanism of ceria promoting CO oxidation over cobalt oxide, which will provide theoretical support for the design of efficient CO oxidation catalysts.
文摘The distribution and verticals variation of geochemical components in the Kasnau-Matasukh lignites of Nagaur Basin, Rajasthan, were investigated using microscopy, proximate and ultimate analyses, Rock-Eval Pyrolysis, X-ray diffraction and Fourier Transform Infrared analyses, and major/minor/trace element determination. The relationship of elements with ash content and with macerals have also been discussed. These lignites are stratified, black, dominantly composed of huminite group macerals with subordinated amounts of liptinite and inertinite groups. They are classified as type-III kerogen and are mainly gas prone in nature. The concentration （in vol%） of mineral matter is seen to increase towards upper part of seam and so is the concentration （in wt%） of the volatile matter, elemental carbon and sulphur. The common minerals present in these lignitesare mixed clay layer, chlorite, and quartz as identified by X-ray diffraction study. Compared with world average in brown coal, the bulk concentration of Cu is anomalously high in most of the samples while Cd is 2-3 times high and Zn is high in one band. Based on interrelationship, different pyrite forms are noticed to have different preferential enrichment of various elements. The concentration of disseminated pyrite is more than the other pyrite forms and is followed by discrete pyrite grains and massive pyrite.
