摘要
合成了新显色剂9-(2-羟基-5-偶氮对甲苯)苯基荧光酮(HMAPPF),并采用红外、核磁和质谱分析确定其分子结构。在研究新试剂与钼Ⅵ显色反应基础上,建立了测定合金钢中微量钼的光度分析方法。在盐酸、磷酸及CTMAB存在下,钼Ⅵ与HMAPPF室温立即反应,生成红色络合物,体系至少可以稳定12h以上。钼络合物的最大吸收峰位于522nm,表观摩尔吸光系数达1·54×105L·mol-1·cm-1,在25mL溶液中,钼Ⅵ量在0～12μg范围内符合比尔定律。此外,该显色反应体系具有良好的选择性,绝大多数金属离子有较大的允许量,可用于复杂样品中微量钼的直接测定。方法应用于合金钢中微量钼的分析,结果与原子吸收光谱法一致,加标回收率和相对标准偏差分别在97·8%～102·5%和0·25%～0·30%之间。
A new chromogenic reagent 9-（2-hydroxyl-5-p-methylazophenyl） phenylfluorone （HMAP-PF） has been synthesized and developed for spectrophotometric determination of trace molybdenum in alloy steel samples in the work, and the molecule structure of HMAPPF was also confirmed by using IR, NMR and MS analysis. In the mixed acid of HCl and H3PO4, Mo（Ⅵ） reacts with the reagent to form a red complex with a maximum absorption peak at 522 nm in the presence of CTMAB, which apparent molar absorptivity is found to be 1.54×10^5L·mol^-1·cm^-1. The reaction can be completed rapidly under room temperature and the absorbance of the complex can be stable for 12 h at least. In 25 mL solution, Beer＇s law is obeyed in the range of 0-12 μg for molybdenum（Ⅵ）. Moreover, the color reation system has good selectivity, most of metal ions can be tolerated in considerable amounts, the property is beneficial to determine trace molybdenum in various complex samples. Proposed method has been applied to measure molybdenum in alloy steel with satisfactory results, the recovery and RSD obtained using standard addition method were 97.8%-102.5% and 0.25%-0. 30%, respectively.
出处
《冶金分析》
EI
CAS
CSCD
北大核心
2007年第3期33-36,共4页
Metallurgical Analysis
