复合金属氧化物CexZr1-xO2-δ的氧非化学计量值的测定
Determination of the Non-stoichiometric Value of Oxygen in the Compound Metal Oxide CexZr1-xO2-δ
摘 要
在含有硝酸铈和硝酸锆的溶液中加入氨水并用聚丙烯酰胺作分散剂制得金属离子的沉淀,抽滤所得沉淀经110 ℃烘干后,在600 ℃(空气中)焙烧2 h,制得复合金属氧化物CexZr1-xO2-δ粉状固体.以此为样品,溶于3 mol·L-1硫酸溶液中,加入已知且过量的硫酸亚铁铵标准溶液将试样中的铈(Ⅳ)还原为3价;用K2Cr2O7标准溶液滴定溶液中过量的亚铁.根据给出的公式计算氧非化学计量值δ.根据样品的测定结果,算得方法的相对标准偏差(n=6)为1.0%,经与热重法对照,两方法所得结果相符.
氧非化学计量值
氧化还原滴定法
返滴定法
Compound metal oxide of CexZr1-xO2-δ
Non-stoichiometric value of oxygen
Redox titration
Back titration
Abstract
The compound metal oxide of CexZr1-xO2-δ was prepared by adding aq.ammonia to a mixed solution containing ceric nitrate and zirconium nitrate with polyacrylamide as dispersing agent.The precipitate was filtered by suction,dried at 110 ℃ and calcined for 2 h in air at 600 ℃.The powdery solid sample was dissolved in 3 mol·L-1 H2SO4,a definite and known amount of Fe2+ ion (in form of standard solution of Fe(NH4)2(SO4)2 solution) to reduce Ce4+ ion,and the excess amount of Fe2+ ion in the solution was titrated with standard K2Cr2O7 solution.The non-stoichiometric value of oxygen (δ) was calculated by the formula given.Value of RSD′s (n=6) found was 1.0%.Results found by this method were in conformity with those obtained by the thermogravimetry.
中图分类号 O657
所属栏目 工作简报
基金项目 江苏省高校自然科学基金资助项目(07KJB150112),徐州师范大学自然科学基金重点资助项目(04XLA04)
收稿日期 2007/7/2
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备注田久英(1973-),女,河北新城人,硕士,讲师,主要从事催化材料制备及分析研究工作.
引用该论文: TIAN Jiu-ying. Determination of the Non-stoichiometric Value of Oxygen in the Compound Metal Oxide CexZr1-xO2-δ[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2008, 44(11): 1071～1073
田久英. 复合金属氧化物CexZr1-xO2-δ的氧非化学计量值的测定[J]. 理化检验－化学分册, 2008, 44(11): 1071～1073
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参考文献
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