An analytical method using high resolution inductively coupled plasma mass spectrometry (HR-ICP-MS) for rapid simultaneous determination of Be, Mg, Al, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Ga, Ge, As, Se, Mo, Ag, Cd, Sn, ...An analytical method using high resolution inductively coupled plasma mass spectrometry (HR-ICP-MS) for rapid simultaneous determination of Be, Mg, Al, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Ga, Ge, As, Se, Mo, Ag, Cd, Sn, Sb, Ba, Pt, Au and Pb in high purity cobalt was described. Sample digestions were performed in closed microwave vessels using HNO3 and HCl. The matrix effects due to the presence of excess HCl and Co were evaluated. The usefulness of high mass resolution for overcoming some spectral interference was demonstrated. The optimum conditions for the determination was tested and discussed. Correction for matrix effects, Sc, Rh and Bi were used as internal standards. The detection limits is 0.003-0.57 μg/g, the recovery ratio is 92.2%-111.2%, and the RSD is less than 3.6%. The method is accurate, quick and convenient. It has been applied to the determination of trace impurities in high purity cobalt with satisfactory results.展开更多
In this study, we investigate the effect of nitrogen and hydrogen impurities on colors, morphologies, impurity structures and synthesis conditions of diamond crystals in Fe–C systems with C3N6H6 additives at pressure...In this study, we investigate the effect of nitrogen and hydrogen impurities on colors, morphologies, impurity structures and synthesis conditions of diamond crystals in Fe–C systems with C3N6H6 additives at pressures in the range 5.0–6.5 GPa and temperatures of 1400–1700℃ in detail. Our results reveal that the octahedron diamond nucleation in a Fe–C system is evidently inhibited by co-doped N–H elements, thereby resulting in the increase of minimum pressure and temperature of diamond synthesis by spontaneous nucleation. The octahedron diamond crystals synthesized from a pure Fe–C system are colorless, while they become green in the system with C3N6H6 additive. The surface defects of diamond will deteriorate when the nitrogen and hydrogen atoms simultaneously incorporate in the diamond growth environment in the Fe–C system. We believe that this study will provide some important information and be beneficial for the deep understanding of the crystallization of diamonds from different component systems.展开更多
An improved and practical synthesis of enzalutamide was accomplished in five steps.Starting from 4-bromo-2-fluoro-benzonic acid,a methyl esterification,Ullmann ligation,methyl esterification,ring closing reaction and ...An improved and practical synthesis of enzalutamide was accomplished in five steps.Starting from 4-bromo-2-fluoro-benzonic acid,a methyl esterification,Ullmann ligation,methyl esterification,ring closing reaction and final methyl amidation provided the target in 35% total yield with 99.8% purity.Five identified impurities were also synthesized.This efficient and economical procedure avoids the use of highly toxic reagents and multiple recrystallization operations,which is suitable for further industrialization.展开更多
基金supported by the Natural Science Foundation of Hunan Province(No.05JJ40017)Education Department of Hunan Province(No.05B064).
文摘An analytical method using high resolution inductively coupled plasma mass spectrometry (HR-ICP-MS) for rapid simultaneous determination of Be, Mg, Al, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Ga, Ge, As, Se, Mo, Ag, Cd, Sn, Sb, Ba, Pt, Au and Pb in high purity cobalt was described. Sample digestions were performed in closed microwave vessels using HNO3 and HCl. The matrix effects due to the presence of excess HCl and Co were evaluated. The usefulness of high mass resolution for overcoming some spectral interference was demonstrated. The optimum conditions for the determination was tested and discussed. Correction for matrix effects, Sc, Rh and Bi were used as internal standards. The detection limits is 0.003-0.57 μg/g, the recovery ratio is 92.2%-111.2%, and the RSD is less than 3.6%. The method is accurate, quick and convenient. It has been applied to the determination of trace impurities in high purity cobalt with satisfactory results.
基金Project supported by the National Natural Science Foundation of China(Grant Nos.11504267,11504269,and 51172089)the Open Project of State Key Laboratory of Superhard Materials,Jilin University,China(Grant No.201504)the Doctoral Fund of Tianjin Normal University,China(Grant No.52XB1518)
文摘In this study, we investigate the effect of nitrogen and hydrogen impurities on colors, morphologies, impurity structures and synthesis conditions of diamond crystals in Fe–C systems with C3N6H6 additives at pressures in the range 5.0–6.5 GPa and temperatures of 1400–1700℃ in detail. Our results reveal that the octahedron diamond nucleation in a Fe–C system is evidently inhibited by co-doped N–H elements, thereby resulting in the increase of minimum pressure and temperature of diamond synthesis by spontaneous nucleation. The octahedron diamond crystals synthesized from a pure Fe–C system are colorless, while they become green in the system with C3N6H6 additive. The surface defects of diamond will deteriorate when the nitrogen and hydrogen atoms simultaneously incorporate in the diamond growth environment in the Fe–C system. We believe that this study will provide some important information and be beneficial for the deep understanding of the crystallization of diamonds from different component systems.
基金the 2016 Shanghai Pujiang Talent program (No. 16PJ1432800)China State Institute of Pharmaceutical Institute Industry for financially supporting this program
文摘An improved and practical synthesis of enzalutamide was accomplished in five steps.Starting from 4-bromo-2-fluoro-benzonic acid,a methyl esterification,Ullmann ligation,methyl esterification,ring closing reaction and final methyl amidation provided the target in 35% total yield with 99.8% purity.Five identified impurities were also synthesized.This efficient and economical procedure avoids the use of highly toxic reagents and multiple recrystallization operations,which is suitable for further industrialization.