电感耦合等离子体原子发射光谱法测定Ti80钛合金中铝铌锆钼铁的酸体系溶解条件探讨

Discussion on acid dissolution conditions for the determination of aluminum,niobium,zirconium,molybdenum and iron in Ti80 titanium alloy by inductively coupled plasma atomic emission spectrometry

为实现Ti80钛合金样品的快速有效溶解,并制得适用于电感耦合等离子体原子发射光谱法（ICP-AES）测定Ti80钛合金中铝、铌、锆、钼、铁含量的样品溶液,对硫酸-硝酸、硝酸-氢氟酸、硫酸-氢氟酸-硝酸及盐酸-氢氟酸-硝酸4种酸体系对应的溶解条件进行了探讨。对4种溶解体系分别进行不同条件试验,根据溶解现象及样品溶解的完全程度初步确定了每种酸体系的溶解条件。硫酸-硝酸溶解体系的溶解条件为：10.0mL硫酸（1＋1）,290～310℃下加热溶解,溶解完全后逐滴加入硝酸至溶液褪色;硝酸-氢氟酸溶解体系的溶解条件为：预先在样品中加入10.0mL水,然后相继加入2.0mL硝酸和2.0mL氢氟酸,直至样品溶解完全;硫酸-氢氟酸-硝酸溶解体系的溶解条件为：预先在样品中加入10.0 mL硫酸（1＋3）,然后加入2.0mL氢氟酸使样品溶解完全,加入2.0mL硝酸至溶液褪色,再加热至冒烟;盐酸-氢氟酸-硝酸溶解体系的溶解条件为：预先在样品中加入15.0mL盐酸（1＋1）,然后加入1.0mL氢氟酸使样品溶解完全,加入2.0mL硝酸使溶液褪色。在初步确定的溶解条件下,分别采用4种溶解体系对Ti80钛合金样品进行溶解,制得样品溶液;对样品溶液中铝、铌、锆、钼和铁的稳定性进行了考察并对其含量进行了测定,结果表明4种酸体系对应的溶解条件下制得的样品溶液均适用于电感耦合等离子体原子发射光谱法（ICP-AES）测定Ti80钛合金中铝、铌、锆、钼和铁含量,确定的4种酸体系对应溶解条件合理。

The dissolution conditions of Ti80 titanium alloy samples by four acid systems（including sulfuric acid-nitric acid,nitric acid-hydrofluoric acid,sulfuric acid-hydrofluoric acid-nitric acid and hydrochloric acid-hydrofluoric acid-nitric acid）were investigated,realizing the rapid and effective dissolution of Ti80 titanium alloy samples.Then,the content of aluminum,niobium,zirconium,molybdenum and iron in sample solution was determined by inductively coupled plasma atomic emission spectrometry（ICP-AES）.The conditional tests were conducted for four acid dissolution systems.The dissolution conditions for each acid system were preliminarily obtained based on the dissolution phenomenon and the dissolution extent of samples.The dissolution conditions for sulfuric acid-nitric acid system were as follows：the sample was dissolved in 10.0mL of sulfuric acid（1＋1）by heating at 290-310 ℃;after dissolving completely,the nitric acid was added dropwise until the color of solution was faded.The dissolution conditions for nitric acidhydrofluoric acid system were as follows：10.0mL of water was firstly added into sample;then,2.0mL of nitric acid and 2.0mL of hydrofluoric acid were added to fully dissolve the sample.The dissolution conditions for sulfuric acid-hydrofluoric acid-nitric acid system were as follows：10.0mL of sulfuric acid（1＋3）was firstly added into sample;then,2.0mL of hydrofluoric acid was added to fully dissolve the sample;2.0mL of nitric acid was added until the color of solution was faded;finally,the solution was heated until fume was observed.The dissolution conditions for hydrochloric acid-hydrofluoric acid-nitric acid system were as follows：15.0 mL of hydrochloric acid（1＋1）was firstly added into sample;then,1.0 mL of hydrofluoric acid was added to fully dissolve the sample;finally,2.0mL of nitric acid was added until the color of solution was faded.According to the dissolution conditions above,the Ti80 titanium alloy sample was dissolved by four acid systems to prepare the sample solution.The stability of aluminum,niobium,zirconium,molybdenum and iron in solution was investigated.The content of these elements was also determined.The results showed that four acid dissolution conditions were applicable for the sample preparation for the determination of aluminum,niobium,zirconium,molybdenum and iron in Ti80 titanium alloy by ICP-AES.The obtained dissolution conditions of four acid systems were all reasonable.