首页|单宁酸沉淀分离-硫酸高铈滴定法测定钛铝铌合金中铌

单宁酸沉淀分离-硫酸高铈滴定法测定钛铝铌合金中铌

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钛铝铌合金因其密度小、抗氧化、耐高温等良好的性能在航空航天领域得到广泛应用,准确测定钛铝铌合金中铌具有重要意义.采用硫酸高铈标准溶液滴定铌元素时,大量存在的钛会对滴定结果产生影响.实验将钛铝铌合金经硫酸、氢氟酸、硝酸溶解后,用单宁酸沉淀铌与大部分钛分离;再将沉淀溶解之后,在硫酸介质中加入过氧化氢与铌元素形成稳定的1∶1过氧化氢铌络合物;通过定量加入过量的硫酸亚铁铵标准溶液将过氧化氢铌络合物破坏,剩余的硫酸亚铁铵标准溶液再用硫酸高铈标准溶液进行滴定,最终通过计算得到铌含量,从而建立了钛铝铌合金中铌元素的测定方法.试验考察了钛元素对铌的干扰,在含有4.00 mg铌的待滴定溶液中钛的最大允许量是1.60 mg,钛铝铌合金经单宁酸沉淀分离后待测液中钛含量远小于1.60 mg,因此不影响铌的滴定.按照实验方法测定钛铝铌合金样品中铌,结果的相对标准偏差(RSD,n=11)为0.21%~0.25%,极差为0.30%~0.33%;回收率为99%~101%.
Determination of niobium in titanium-aluminum-niobium alloy by tannic acid precipitation separation-ceric sulfate titration method
Titanium-aluminum-niobium(Ti-Al-Nb)alloy has been widely used in the field of aerospace be-cause of its good properties such as low density,oxidation resistance and high temperature resistance.The accurate determination of niobium content in Ti-Al-Nb alloy is of great significance.When niobium is titra-ted with ceric sulfate standard solution,the titration result will be influence by the coexisting titanium.In experiments,the Ti-Al-Nb alloy was dissolved with sulfuric acid,hydrofluoric acid and nitric acid.The tannic acid was added to precipitate niobium,realizing the separation from most of titanium.After dissol-ving the precipitate,hydrogen peroxide was added into sulfuric acid medium to form stable niobium-hydro-gen peroxide complex(1∶1)with niobium.Then excessive ammonium ferrous sulfate standard solution was added quantitatively to destroy the niobium-hydrogen peroxide complex,and the residual ammonium ferrous sulfate standard solution was titrated with ceric sulfate standard solution.Finally,the content of niobium could be calculated.Consequently,the method for the determination of niobium in titanium-alu-minum-niobium alloy was established.The interference of titanium with the determination of niobium was investigated.The results showed that the maximum allowable amount of titanium was 1.60 mg for the so-lution containing 4.00 mg of niobium.Since the content of titanium in the testing solution after tannic acid precipitation separation was much lower than 1.60 mg,the titration of niobium would be not affected.The content of niobium in Ti-Al-Nb alloy sample was determined according to the experimental method.The relative standard deviations(RSD,n=11)of determination results were between 0.21%and 0.25%,and the range was 0.30%-0.33%.The spiked recoveries were between 99%and 101%.

titanium-aluminum-niobium alloyniobiumtitaniumtannic acidprecipitation separationceric sulfatetitrationhydrogen peroxideammonium ferrous sulfate

张霞、谈笑、王艳敏、于雪、陈静

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钢研纳克检测技术股份有限公司,北京 100094

钛铝铌合金 单宁酸 沉淀分离 硫酸高铈 滴定法 过氧化氢 硫酸亚铁铵

2024

冶金分析
中国钢研科技集团有限公司(钢铁研究总院) 中国金属学会

冶金分析

CSTPCD北大核心
影响因子:1.124
ISSN:1000-7571
年,卷(期):2024.44(2)
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