ICP-OES测定TA31钛合金中化学成分的4种不同酸体系样品制备方法比较分析  

Comparison and Analysis of Four Kinds of Sample Preparation Methods with Different Acid Systems for Determining Chemical Composition in TA31 Titanium Alloy by ICP-OES

作　　者：罗策[1] 颜燕[2] 刘婷[1] 白焕焕 卢凡 马婉莹 张媛媛 LUO Ce;YAN Yan;LIU Ting;BAI Huan-huan;LU Fan;MA Wan-ying;ZHANG Yuan-yuan(BaoTi Group Co.,Ltd.,Baoji 721014,China;Baoji Education Institute of Shaanxi,Baoji 721000,China)

机构地区：[1]宝钛集团有限公司,陕西宝鸡721014 [2]陕西省宝鸡教育学院,陕西宝鸡721000

出　　处：《化学试剂》2021年第10期1399-1403,共5页Chemical Reagents

摘　　要：对ICP-OES测定TA31钛合金中铝、铌、锆、钼、铁、硅6种元素含量的硫酸-硝酸、氢氟酸-硝酸、氢氟酸-硫酸-硝酸和盐酸-氢氟酸-硝酸4种不同酸体系样品制备方法的试剂用量、处理温度和制备时间进行了比较,并对4种样品制备方法对应的检测方法的灵敏度、检出限、精密度、准确度等性能指标进行了比较分析。结果表明,氢氟酸-硝酸体系下的试剂用量最小,盐酸-氢氟酸-硝酸体系下的试剂用量最大,此两种样品制备方法均在常温下进行,无需加热,溶解时间较短;4种样品制备方法对应检测方法的灵敏度按照硫酸-硝酸、氢氟酸-硫酸-硝酸、盐酸-氢氟酸-硝酸、氢氟酸-硝酸的顺序依次升高;检出限和定量限基本一致;铝、铌、锆、钼、铁5种元素在4种制备方法下均可得到一致的检测结果,准确度和精密度整体上良好,氢氟酸-硫酸-硝酸制备方法下精密度略差;硫酸-硝酸和氢氟酸-硫酸-硝酸制备方法下,硅测定结果的精密度和准确度较差,不适合硅含量的测定。The reagent dosage,treatment temperature and preparation time of sample preparation methods in four different acid systems:sulfuric acid-nitric acid,hydrofluoric acid-nitric acid,hydrofluoric acid-sulfuric acid-nitric acid and hydrofluoric acid-hydrochloric acid-nitric acid for the content of aluminium,niobium,zirconium,molybdenum,iron and silicon in TA31 titanium alloy determined by ICP-OES were compared.And the test method performance indexes corresponding to each sample preparation method of sensitivity,detection limit,precision,accuracy and so on were compared and analyzed.The results showed that the amount of reagent in hydrofluoric acid-nitric acid system was the minimum,and the amount of reagent in hydrochloric acid-hydrofluoric acid-nitric acid system was the maximum.These two sample preparation methods were carried out at room temperature,without heating,and the dissolution time was short.The sensitivity of the test methods corresponding to the four sample preparation methods increased according to the order of sulfuric acid-nitric acid,hydrofluoric acid-sulfuric acid-nitric acid,hydrochloric acid-hydrofluoric acid-nitric acid,hydrofluoric acid-nitric acid.The limits of detection and limits of quantification are basically consistent.The detection results of aluminum,niobium,zirconium,molybdenum and iron were consistent under the four preparation methods,and the accuracy and precision were good on the whole,while the precision was slightly worse under the preparation method of hydrofluoric acid-sulfuric acid-nitric acid.Under the preparation methods of sulfuric acid-nitric acid and hydrofluoric acid-sulfuric acid-nitric acid,the precision and accuracy of silicon determination results are poor,so it is not suitable for the determination of silicon content.

关 键 词：电感耦合等离子体原子发射光谱法 TA31钛合金 样品制备方法 酸体系 化学成分 

分 类 号：O652.4[理学—分析化学]