The flame retardant mechanism of the copolyester phosphorus containing linked pendant groups was investigated by thermogravimetric （TG）, X-ray photoelectron spectroscopy （XPS） and direct insertion probe pyrolysis ...The flame retardant mechanism of the copolyester phosphorus containing linked pendant groups was investigated by thermogravimetric （TG）, X-ray photoelectron spectroscopy （XPS） and direct insertion probe pyrolysis mass spectrometry （DP-MS） technique. TG results show that the incorporation of phosphorus containing unit linked pendant groups can destabilize the copolyester due to the cleavage of P-CH2 bond, and phosphorus containing units cannot promote the char-formation of the copolyester during the thermal degradation of the copolyester. XPS spectra indicate that with the increase of the temperature, the P-CH2 bonds of the copolyester break down gradually, the concentration of phosphorus in the condensed phase products decrease gradually and the chemical state of phosphorus does not change in the temperature of 250-380 ℃. Direct pyrolysis MS suggests that the P-CH2 bonds cleavage occurs at pendant groups and species containing phosphorus can volatilize into the gas phase. A flame retardant mechanism is proposed for the gas phase mode of action of the halogen-free copolyester phosphorus containing linked pendant groups.展开更多
江西南昌西汉海昏侯墓是近年来汉代考古的重要发现,其出土的大量珍贵文物为研究西汉列侯葬制、复原汉代社会生活提供了难能可贵的实物资料。其中墓园M1和M5棺内各出土了玻璃席,作为玉敛葬中的一种葬具,是西汉手工业水平的重要见证,也是...江西南昌西汉海昏侯墓是近年来汉代考古的重要发现,其出土的大量珍贵文物为研究西汉列侯葬制、复原汉代社会生活提供了难能可贵的实物资料。其中墓园M1和M5棺内各出土了玻璃席,作为玉敛葬中的一种葬具,是西汉手工业水平的重要见证,也是列侯丧葬等级和汉代法赙制度的具体表征。本研究使用傅里叶变换显微红外光谱(micro-FTIR)、热裂解气相色谱-质谱分析(Py-GC/MS)以及基于质谱的动物考古学技术(zooarchaeology by mass spectrometry,ZooMS)等多种手段,对海昏侯墓出土玻璃席包边及疑似胶结材料进行了科学分析。首先利用傅里叶变换显微红外光谱确定样品中均含有蛋白质成分,再利用热裂解气相色谱质谱技术检测包边残留物和疑似胶结材料的主要成分,判断包边样品应为动物性来源,最后使用基于质谱的动物考古学技术,确定了M1刘贺墓玻璃席包边残留物的生物来源为普通牛,推测包边残留物材料为牛皮。包边样品中检测到的少量酚类物质,表明牛皮在鞣制过程中可能使用了植物鞣剂。样品中含量较高的脂肪酸类物质可能来源于皮革鞣制中的加脂处理。此外,两件胶结材料样品中含有吲哚类、脯氨酸类化合物以及磷酸三甲脂,但未发现胆固醇类化合物,判断胶结材料应为蛋清。本研究明确了玻璃席包边制作材料,为了解古代制席工艺、制作技法提供了科学认知,两张玻璃席制作精美、工艺复杂,展现了西汉中期高超的制席工艺,为后续针对玻璃席开展的保护修复工作提供了重要参考依据。展开更多
文摘The flame retardant mechanism of the copolyester phosphorus containing linked pendant groups was investigated by thermogravimetric （TG）, X-ray photoelectron spectroscopy （XPS） and direct insertion probe pyrolysis mass spectrometry （DP-MS） technique. TG results show that the incorporation of phosphorus containing unit linked pendant groups can destabilize the copolyester due to the cleavage of P-CH2 bond, and phosphorus containing units cannot promote the char-formation of the copolyester during the thermal degradation of the copolyester. XPS spectra indicate that with the increase of the temperature, the P-CH2 bonds of the copolyester break down gradually, the concentration of phosphorus in the condensed phase products decrease gradually and the chemical state of phosphorus does not change in the temperature of 250-380 ℃. Direct pyrolysis MS suggests that the P-CH2 bonds cleavage occurs at pendant groups and species containing phosphorus can volatilize into the gas phase. A flame retardant mechanism is proposed for the gas phase mode of action of the halogen-free copolyester phosphorus containing linked pendant groups.
文摘江西南昌西汉海昏侯墓是近年来汉代考古的重要发现,其出土的大量珍贵文物为研究西汉列侯葬制、复原汉代社会生活提供了难能可贵的实物资料。其中墓园M1和M5棺内各出土了玻璃席,作为玉敛葬中的一种葬具,是西汉手工业水平的重要见证,也是列侯丧葬等级和汉代法赙制度的具体表征。本研究使用傅里叶变换显微红外光谱(micro-FTIR)、热裂解气相色谱-质谱分析(Py-GC/MS)以及基于质谱的动物考古学技术(zooarchaeology by mass spectrometry,ZooMS)等多种手段,对海昏侯墓出土玻璃席包边及疑似胶结材料进行了科学分析。首先利用傅里叶变换显微红外光谱确定样品中均含有蛋白质成分,再利用热裂解气相色谱质谱技术检测包边残留物和疑似胶结材料的主要成分,判断包边样品应为动物性来源,最后使用基于质谱的动物考古学技术,确定了M1刘贺墓玻璃席包边残留物的生物来源为普通牛,推测包边残留物材料为牛皮。包边样品中检测到的少量酚类物质,表明牛皮在鞣制过程中可能使用了植物鞣剂。样品中含量较高的脂肪酸类物质可能来源于皮革鞣制中的加脂处理。此外,两件胶结材料样品中含有吲哚类、脯氨酸类化合物以及磷酸三甲脂,但未发现胆固醇类化合物,判断胶结材料应为蛋清。本研究明确了玻璃席包边制作材料,为了解古代制席工艺、制作技法提供了科学认知,两张玻璃席制作精美、工艺复杂,展现了西汉中期高超的制席工艺,为后续针对玻璃席开展的保护修复工作提供了重要参考依据。
