作者:Maria Lalia-Kantouri、L. Tzavellas、D. Paschalidis
DOI:10.1007/s10973-007-8487-8
日期:2008.3
The reaction of a hydrated nitrate salt of lanthanide(III) (Ln=Er, Ho, Tb, Gd) or yttrium(III) (Y) with the ligand di-2-pyridyl ketone-p-Cl-benzoylhydrazone (DpkClBH), afforded air stable solid compounds. The new complexes characterized by means of elemental analysis (C, H, N, Ln), magnetic moment determinations and spectroscopic data (IR, MS). It is proposed that they are cationic of the general type: [Ln(DpkClBH)2(NO3)2]NO3·nH2O, (n=2, 1, 1, 1, 1.5 for Ln=Y, Gd, Tb, Ho, Er, respectively). Their thermal decomposition was studied in nitrogen atmosphere, between 25–980°C, by using simultaneous TG/DTG-DTA technique. The IR spectroscopy used to determine the intermediates and the final products. The anhydrous nitrate complexes decomposed to the intermediates Ln(DpkClBH)(NO3)2, which upon further heating give a carbonaceous residue of Ln2O3 at 980°C. The mass spectra revealed the molecular ions of the complexes and their possible fragmentation pattern.
稀土元素(III)(Ln=Er, Ho, Tb, Gd)或钇(III)(Y)水合硝酸盐与配体二-2-吡啶酮-对氯苯甲肼酮(DpkClBH)反应,形成了在空气中稳定的固体化合物。通过元素分析(C, H, N, Ln)、磁矩测定和光谱数据(IR, MS)对这些新复合物进行了表征。建议其为一般类型的阳离子:[Ln(DpkClBH)2(NO3)2]NO3·nH2O,(n=2,1, 1, 1, 1.5,分别对应Ln=Y, Gd, Tb, Ho, Er)。在氮气氛围下研究了它们在25-980°C范围内的热分解,采用了同步TG/DTG-DTA技术。红外光谱用于确定中间体和最终产品。无水硝酸盐复合物分解为中间体Ln(DpkClBH)(NO3)2,进一步加热后在980°C生成Ln2O3的碳质残留物。质谱显示了复合物的分子离子及其可能的碎片模式。