目的建立液相色谱-串联质谱法检测金属罐中三(壬基酚)亚磷酸酯迁移量的分析方法。方法金属罐经水、4%乙酸、10%乙醇、20%乙醇、50%乙醇等食品模拟物迁移后,过滤,采用大气压化学电离(atmosphere pressure chemical ionization,APCI)和多...目的建立液相色谱-串联质谱法检测金属罐中三(壬基酚)亚磷酸酯迁移量的分析方法。方法金属罐经水、4%乙酸、10%乙醇、20%乙醇、50%乙醇等食品模拟物迁移后,过滤,采用大气压化学电离(atmosphere pressure chemical ionization,APCI)和多反应监测模式(multiple reaction monitoring,MRM)进行检测,外标法定量。结果三(壬基酚)亚磷酸酯在10~500μg/L范围内呈现良好的线性关系,相关系数不低于0.9997,检出限为0.005 mg/L,测定结果的相对标准偏差不大于5%(n=6),加标回收率为94.20%~106.40%。结论该方法准确、精密度好,可用于金属罐中三(壬基酚)亚磷酸酯迁移量的快速检测。展开更多
Silicon oxide(SiO_(x))has received remarkable attention as a next-generation battery material;however,the sudden decrease in the cycling retention constitutes a significant challenge in facilitating its application.Tr...Silicon oxide(SiO_(x))has received remarkable attention as a next-generation battery material;however,the sudden decrease in the cycling retention constitutes a significant challenge in facilitating its application.Tris(2,2,2-trifluoroethyl)phosphite(TTFP),which can control parasitic reactions such as the pulverization of SiO_(x)anode materials and electrolyte decomposition,has been proposed to improve the lifespan of the cell.The electrochemical reduction of TTFP results in solid-electrolyte interphase(SEI)layers that are mainly composed of LiF,which occur at a higher potential than the working potential of the SiO_(x)anode and carbonate-based solvents.The electrolyte with TTFP exhibited a substantial improvement in cycling retention after 100 cycles,whereas the standard electrolyte showed acutely decreased retention.The thickness of the SiO_(x)anode with TTFP also changed only slightly without any considerable delamination spots,whereas the SiO_(x)anode without TTFP was prominently deformed by an enormous volume expansion with several internal cracks.The cycled SiO_(x)anode with TTFP exhibited less increase in resistance after cycling than that in the absence of TTFP,in addition to fewer decomposition adducts in corresponding X-ray photoelectron spectroscopy(XPS)analyses between the cycled SiO_(x)anodes.These results demonstrate that TTFP formed SEI layers at the SiO_(x)interface,which substantially reduced the pulverization of the SiO_(x)anode materials;in addition,electrolyte decomposition at the interface decreased,which led to improved cycling retention.展开更多
基金This work was financially supported by the National Research Foundation of Korea financially(NRF)(No.NRF-2022R1F1A1069039)the Core Research Institute(CRI)Program,the Basic Science Research Program through the National Research Foundation of Korea(NRF),Ministry of Education(No.NRF-2017R1A6A1A06015181)the Technology Innovation Program(No.20011905)funded by the Ministry of Trade,Industry&Energy(MOTIE,Korea).
文摘Silicon oxide(SiO_(x))has received remarkable attention as a next-generation battery material;however,the sudden decrease in the cycling retention constitutes a significant challenge in facilitating its application.Tris(2,2,2-trifluoroethyl)phosphite(TTFP),which can control parasitic reactions such as the pulverization of SiO_(x)anode materials and electrolyte decomposition,has been proposed to improve the lifespan of the cell.The electrochemical reduction of TTFP results in solid-electrolyte interphase(SEI)layers that are mainly composed of LiF,which occur at a higher potential than the working potential of the SiO_(x)anode and carbonate-based solvents.The electrolyte with TTFP exhibited a substantial improvement in cycling retention after 100 cycles,whereas the standard electrolyte showed acutely decreased retention.The thickness of the SiO_(x)anode with TTFP also changed only slightly without any considerable delamination spots,whereas the SiO_(x)anode without TTFP was prominently deformed by an enormous volume expansion with several internal cracks.The cycled SiO_(x)anode with TTFP exhibited less increase in resistance after cycling than that in the absence of TTFP,in addition to fewer decomposition adducts in corresponding X-ray photoelectron spectroscopy(XPS)analyses between the cycled SiO_(x)anodes.These results demonstrate that TTFP formed SEI layers at the SiO_(x)interface,which substantially reduced the pulverization of the SiO_(x)anode materials;in addition,electrolyte decomposition at the interface decreased,which led to improved cycling retention.
