The reaction of Mo(CO)6 with m-CH_3-C6H4SNa and Et4NCl(H_2O in CH_3CN afforded a dinuclear molybdenum(0) compound [Et4N]2[Mo2(CO)8(SC6H4-CH_3-m)2] (1). The crystal structure was determined by X-ray crystallography. Th...The reaction of Mo(CO)6 with m-CH_3-C6H4SNa and Et4NCl(H_2O in CH_3CN afforded a dinuclear molybdenum(0) compound [Et4N]2[Mo2(CO)8(SC6H4-CH_3-m)2] (1). The crystal structure was determined by X-ray crystallography. The crystallographic data: C38H54Mo2N2O8S2, Mr = 922.87, triclinic, P_ 1, a =10.336(2), b=10.753(2), c=11.121(2) ?, ( =88.88(2), ( =68.64(1), ( =69.71(1)(, V=1071.5(1) ?3, Z=1, Dc=1.43 g/cm3, F(000) = 476, ( = 7.1cm－1, Final R = 0.036 and Rw = 0.045 for 3423 reflections with I >3.0( (I). The X-ray structure analysis revealed that the Mo2S2 core is planar. The geometry around each Mo atom is a distorted octahedron, both of which form an edge-sharing bioctahedron. The Mo...Mo distance is 4.0665(1)(, which obviously indicates the absence of Mo-Mo bond.展开更多
目的建立微波消解-电感耦合等离子体质谱（ICP-MS）直接稀释测定脉络宁注射液中25种矿物质元素（Mg、Ca、Fe、Cu、Zn、Mn、Al、B、Ba、Co、Cr、K、Li、Mo、Na、Ni、P、Pb、Sr、Th、Ti、V、As、Cd和Hg）的方法。方法分别对微波消解条件...目的建立微波消解-电感耦合等离子体质谱（ICP-MS）直接稀释测定脉络宁注射液中25种矿物质元素（Mg、Ca、Fe、Cu、Zn、Mn、Al、B、Ba、Co、Cr、K、Li、Mo、Na、Ni、P、Pb、Sr、Th、Ti、V、As、Cd和Hg）的方法。方法分别对微波消解条件和测试条件进行考察;样品经微波消解后,采用电感耦合质谱仪测定25种矿物质元素,并对测定方法学进行考察。结果确定最佳消解条件为3步缓慢升温：400 W 80℃升温10 min,保留5 min;600 W 120℃升温10 min,保留5 min;900 W 200℃升温20 min,保留20 min;25种矿物质元素在各自的线性范围内线性关系良好,r≥0.999 6,精密度、稳定性和重复性试验的RSD均符合定量分析要求;加标回收率为94.7%~106.1%,RSD在0.34%~2.79%。脉络宁注射液中检测出Mg、Ca、Fe、Cu、Zn、Mn、Al、B、Ba、Co、Cr、K、Li、Mo、Na、Ni、P、Pb、Sr、Th、Ti、V,未检出As、Cd和Hg。结论该方法简便、迅速、准确,适用于脉络宁注射液中25种矿物质元素的同时测定。展开更多
文摘The reaction of Mo(CO)6 with m-CH_3-C6H4SNa and Et4NCl(H_2O in CH_3CN afforded a dinuclear molybdenum(0) compound [Et4N]2[Mo2(CO)8(SC6H4-CH_3-m)2] (1). The crystal structure was determined by X-ray crystallography. The crystallographic data: C38H54Mo2N2O8S2, Mr = 922.87, triclinic, P_ 1, a =10.336(2), b=10.753(2), c=11.121(2) ?, ( =88.88(2), ( =68.64(1), ( =69.71(1)(, V=1071.5(1) ?3, Z=1, Dc=1.43 g/cm3, F(000) = 476, ( = 7.1cm－1, Final R = 0.036 and Rw = 0.045 for 3423 reflections with I >3.0( (I). The X-ray structure analysis revealed that the Mo2S2 core is planar. The geometry around each Mo atom is a distorted octahedron, both of which form an edge-sharing bioctahedron. The Mo...Mo distance is 4.0665(1)(, which obviously indicates the absence of Mo-Mo bond.
文摘目的建立微波消解-电感耦合等离子体质谱（ICP-MS）直接稀释测定脉络宁注射液中25种矿物质元素（Mg、Ca、Fe、Cu、Zn、Mn、Al、B、Ba、Co、Cr、K、Li、Mo、Na、Ni、P、Pb、Sr、Th、Ti、V、As、Cd和Hg）的方法。方法分别对微波消解条件和测试条件进行考察;样品经微波消解后,采用电感耦合质谱仪测定25种矿物质元素,并对测定方法学进行考察。结果确定最佳消解条件为3步缓慢升温：400 W 80℃升温10 min,保留5 min;600 W 120℃升温10 min,保留5 min;900 W 200℃升温20 min,保留20 min;25种矿物质元素在各自的线性范围内线性关系良好,r≥0.999 6,精密度、稳定性和重复性试验的RSD均符合定量分析要求;加标回收率为94.7%~106.1%,RSD在0.34%~2.79%。脉络宁注射液中检测出Mg、Ca、Fe、Cu、Zn、Mn、Al、B、Ba、Co、Cr、K、Li、Mo、Na、Ni、P、Pb、Sr、Th、Ti、V,未检出As、Cd和Hg。结论该方法简便、迅速、准确,适用于脉络宁注射液中25种矿物质元素的同时测定。
