The solubility of poly(phenyl glycidyl ether)s (PPGEs) depends on the stereoregularity.Different solvents and temperatures (CDCl 3/300 K or TCE d 2/350 K)were used in 13 C\|NMR characterization of these polymers.It wa...The solubility of poly(phenyl glycidyl ether)s (PPGEs) depends on the stereoregularity.Different solvents and temperatures (CDCl 3/300 K or TCE d 2/350 K)were used in 13 C\|NMR characterization of these polymers.It was necessary to investigate first the effect of temperature on the 13 C\|NMR spectra of PPGEs.It was found that all the 13 C NMR signals of PPGE were shifted to the lower magnetic field with the increase of the temperature.The temperature sensitivity of the 13 C NMR chemical shifts for different carbon atoms was different.The pendent CH 2 group was most sensitive to the temperature.The change of the 13 C\|NMR chemical shift for the pendent CH 2 group was mainly caused by the temperature change,and the effects of the solvent kind and the stereoregularity of the polymer were of minor importance.The change of temperature did not make any significant influence on the result of the stereoregularity calculation according to the 13 C\|NMR spectra for PPGEs.Utilizing the different temperature sensitivity of 13 C\|NMR signals for different groups,it is possible to separate the overlapped signals by choosing an appropriate temperature.This method was found especially useful in the 13 C\|NMR characterization of complex polymer samples.展开更多
近年来,生物质碳(biochar)作为新型吸附剂被广泛研究。但由于制备biochar的生物质原料和热解温度的不同,使biochar的结构和组成存在差异,从而影响其对污染物的吸附。目前关于biochar的结构和组成的研究还不够全面。因此,结合了能谱与光...近年来,生物质碳(biochar)作为新型吸附剂被广泛研究。但由于制备biochar的生物质原料和热解温度的不同,使biochar的结构和组成存在差异,从而影响其对污染物的吸附。目前关于biochar的结构和组成的研究还不够全面。因此,结合了能谱与光谱分析的手段,对biochar的结构和组成进行了深入的分析。选取木质类(柳树枝条)和草类(水稻秸秆)作为原料,分别在不同热解温度(300,450和600℃)下制得biochars,并对biochars样品进行元素分析、X射线光电子能谱分析(XPS)和固态13 C核磁共振(13 C NMR)研究,以阐明不同热解温度和生物质来源的biochars的结构和组成。结果显示:biochar的H/C,O/C和(O+N)/C的比值随着热解温度的升高而降低;草类biochar比木质类biochar具有更高的灰分含量和表面极性;木质类biochar的矿物主要分布在样品颗粒内部,其表面被有机质覆盖,而草类biochar部分矿物暴露在样品颗粒表面;13 C NMR显示低温制得的biochar主要由芳香碳、脂肪碳、羧基和羰基碳组成,高温制得的biochar主要由芳香碳组成,且低温制得biochars中,木质类biochars比草类biochars含有更高的木质素的残留碳结构,这是由于木质类biochars原材料中含有更高的木质素。展开更多
文摘The solubility of poly(phenyl glycidyl ether)s (PPGEs) depends on the stereoregularity.Different solvents and temperatures (CDCl 3/300 K or TCE d 2/350 K)were used in 13 C\|NMR characterization of these polymers.It was necessary to investigate first the effect of temperature on the 13 C\|NMR spectra of PPGEs.It was found that all the 13 C NMR signals of PPGE were shifted to the lower magnetic field with the increase of the temperature.The temperature sensitivity of the 13 C NMR chemical shifts for different carbon atoms was different.The pendent CH 2 group was most sensitive to the temperature.The change of the 13 C\|NMR chemical shift for the pendent CH 2 group was mainly caused by the temperature change,and the effects of the solvent kind and the stereoregularity of the polymer were of minor importance.The change of temperature did not make any significant influence on the result of the stereoregularity calculation according to the 13 C\|NMR spectra for PPGEs.Utilizing the different temperature sensitivity of 13 C\|NMR signals for different groups,it is possible to separate the overlapped signals by choosing an appropriate temperature.This method was found especially useful in the 13 C\|NMR characterization of complex polymer samples.
文摘近年来,生物质碳(biochar)作为新型吸附剂被广泛研究。但由于制备biochar的生物质原料和热解温度的不同,使biochar的结构和组成存在差异,从而影响其对污染物的吸附。目前关于biochar的结构和组成的研究还不够全面。因此,结合了能谱与光谱分析的手段,对biochar的结构和组成进行了深入的分析。选取木质类(柳树枝条)和草类(水稻秸秆)作为原料,分别在不同热解温度(300,450和600℃)下制得biochars,并对biochars样品进行元素分析、X射线光电子能谱分析(XPS)和固态13 C核磁共振(13 C NMR)研究,以阐明不同热解温度和生物质来源的biochars的结构和组成。结果显示:biochar的H/C,O/C和(O+N)/C的比值随着热解温度的升高而降低;草类biochar比木质类biochar具有更高的灰分含量和表面极性;木质类biochar的矿物主要分布在样品颗粒内部,其表面被有机质覆盖,而草类biochar部分矿物暴露在样品颗粒表面;13 C NMR显示低温制得的biochar主要由芳香碳、脂肪碳、羧基和羰基碳组成,高温制得的biochar主要由芳香碳组成,且低温制得biochars中,木质类biochars比草类biochars含有更高的木质素的残留碳结构,这是由于木质类biochars原材料中含有更高的木质素。