实验技术与管理

以草酸钾与氯化铁为原料,通过室温固相SH反应合成了三草酸合铁(Ⅲ)酸钾配合物,用滴定分析、X射线单晶衍射、X射线粉末衍射、红外光谱、热分析等方法对其组成和结构进行了表征。实验结果表明:三草酸合铁(Ⅲ)酸钾的晶体结构属于单斜晶系,P2(1)/c空间群;草酸根中的氧原子与铁(Ⅲ)形成配位数为6的变形八面体配合物;在氮气气氛中的热分解过程分4步,最后的残余物为FeO和K_2CO₃。这些测试表征结果可为学生更好地完成实验提供重要的参考信息。

The complex of potassium ferrioxalate(III)was synthesized with potassium oxalate and ferric chloride as the raw materials by room temperature solid-solid reaction.The composition and structure of the complex were characterized by titration analyses,single crystal X-ray diffraction,X-ray powder diffraction,infrared spectrum and thermal analysis.The crystal structure of complex K₃[Fe(C_2O₄)₃]·3H_2O belongs to monoclinic system with space group P2(1)/c.The Fe(III)ion was hexacoordinated by six O atoms from the ligand oxalate anions,and forming a distorted octahedral geometry.The thermal decomposition process of the complex in the nitrogen atmosphere was divided into four steps,and the final residues were FeO and K_2CO₃.The testing characterization results can provide important reference information for the students to complete the experiment.