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机构地区:[1]西北大学化学系
出 处:《陕西师大学报(自然科学版)》1992年第4期90-91,共2页Journal of Shaanxi Normal University(Natural Science Edition)
基 金:国家基金局
摘 要:试验所用La(SCN)_3·7H_2O的制取已在文献中述及。安替比林系采用化学纯试剂重结晶得到。用标准EDTA溶液定镧确定La(SCN)_3的含量,C_(11)H_912)ON_2含量的测定用碘量法,在测定C_(11)H_(12)ON_2的含量之前,加入适量EDTA将La^(3+)掩蔽。使用溶解度等温法研究体系的相平衡,将所配的复体放在0℃的冰水浴中,搅拌平衡。溶液的折光指数值及化学分析结果表明,体系20昼夜可达平衡。静置后取样分析。平衡相的组成用Schreinemakers湿渣法确定,并用干燥后的平衡相的化学分析加以确证。所有计量仪器均校正。The solubilities of the ternary system La(SCN)_3-C_(11)-H_(12)-ON_2-H_2Oat 0℃ is determined and the related phase diagram has been constructed. The solubility isotherms of the system consist of three branches correspounding to La(SCN)_3·7H_2O, La(SCN)_3·4C_(11)H_(12)ON_2 (Ⅰ) and C_(11)H_(12)ON_2, respectively, and also a branch correspounding to a metastable compound La(SCN)_3·5C_(11)H_(12)ON_2 (Ⅱ)·(Ⅰ) is a crystalline compound, (Ⅱ) at dry state—a very sticky glue—like substance. They are all congruently soluble in water. From the phase diagram obtained, it is posible to explain why we often get (Ⅱ) in synthesizing the coordination compounds of antipyrine and La(SCN)_3 at first, and in solution (Ⅱ) becomes (Ⅰ) spontaneously at room temperature, and (Ⅰ) changes to (Ⅱ) by heating.
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