Abstract：The zirconium alloy sample was dissolved with ammonium sulfate and sulfuric acid. The ethanol solution of 5-Br-PADAP was selected as coloring agent in sulfuric acid medium. After reaction in boiling water bath for 10 min, the solution was cooled to room temperature with flow water. The determination was conducted at wavelength of 610 nm. Thus the analysis method of niobium in zirconium alloys by 5-Br-PADAP spectrophotometry was established. Under the optimal analysis conditions, the mass concentration of niobium in range of 0-0.8 μg/mL was linear to the corresponding absorbance. The correlation coefficient was r=0.999 0, and the molar absorptivity was ε=5.9×104 L/(mol·cm). The content of niobium in zirconium alloy was determined according to the experimental method. The relative standard deviation (RSD, n=11) was 2.9% and 1.9%, respectively. The found results were consistent with those obtained by inductively coupled plasma atomic emission spectrometry (ICP-AES).
王峰,王快社,马林生,等.核级锆及锆合金研究状况及发展前景[J].兵器材料科学与工程,2013,35(1): 107-110.WANG Feng,WANG Kuan-she,MA Lin-sheng,et al.Current situation and development of zirconium and zirconium alloys[J].Ordnance Material Science and Engineering,2013,35(1):107-110.
胡明,万兵,任志海,等.高压消解-电感耦合等离子体质谱(ICP-MS)法测定地质样品中的铌和钽[J].中国无机分析化学,2016,6(3):35-38.HU Ming,WAN Bing,REN Zhi-hai,et al.Determination of niobium and tantalum in mineral by high pressure dissolution-inductively coupled plasma mass spectrometry[J].Chinese Journal of Inorganic Analytical Chemistry,2016,6(3):35-38.
[4]
彭慧仙.熔融制样-X射线荧光光谱法测定硬质合金中钨钴镍铁铌钽铬[J].冶金分析,2015,35(7):20-26.PENG Hui-xian.Determination of tungsten,cobalt,nickel,iron,niobium,tantalum and chromium in hard alloy by X-ray fluorescence spectrometry with fusion sample preparation[J].Metallurgical Analysis,2015,35(7):20-26.
[5]
王影,李艳杰,沈亮亮,等.铌-酒石酸-铬天青S-溴化十六烷基吡啶分光光度法测定微量铌[J].光谱实验室,2013,30(1):220-223.WANG Ying,LI Yan-jie,SHEN Liang-liang,et al.Determination of micro niobium Nb-tartaric acid-chrom azurol S-cetylpyridinium bromide spectrpphotometry[J].Chinese Journal of Spectroscopy Laboratory,2013,30(1):220-223.
[6]
王宏鉴,李晓雨,王静.分光光度法测定Fe-Si-B-Nb-Cu合金中的铌含量[J].材料导报,2013,27(21):26-28.WANG Hong-jian,LI Xiao-yu,WANG Jing.Determination of quantity of niobium in nanocrystal Fe-Si-B-Nb-Cu by spetrophotometric method[J].Materials Review,2013,27(21):26-28.
[7]
杨军红,李陀,石新层.电感耦合等离子体原子发射光谱法(ICP-AES)测定N18锆合金中Nb、Sn、Fe、Cr元素含量[J].中国无机分析化学,2015,5(2):47-49.YANG Jun-hong,LI Tuo,SHI Xin-ceng.Determination of Nb,Sn,Fe and Cr in N18 alloy by inductively coupled plasma atomic emission spectrometry[J].Chinese Journal of Inorganic Analytical Chemistry,2015,5(2):47-49.
[8]
高红波,禄妮,李波,等.ICP-AES法测定锆合金中常量及微量元素[J].现代科学仪器,2007(2):87-89.GAO Hong-bo,LU Ni,LI Bo,et al.Determination of major and trace elements in zirconium alloys by ICP-AES[J].Modern Scientific Instruments,2007(2):87-89.
[9]
邹阳,杨远,罗悠,等.电感耦合等离子体原子发射光谱(ICP-AES)法测定锂云母中的锂、钽、铌等7种元素[J].中国无机分析化学,2016,6(1):41-44.ZOU Yang,YANG Yuan,LUO You,et al.Determination of seven elements(lithium,tantalum,niobium ect.) in lepidolite by inductively coupled plasma emission spectrometry[J].Chinese Journal of Inorganic Analytical Chemistry,2016,6(1):41-44.
[10]
李延超,林小辉,梁静,等.电感耦合等离子体原子发射光谱法测定TaNb6合金中铌和10种杂质元素[J].冶金分析,2016,36(5):64-68.LI Yan-chao,LIN Xiao-hui,LIANG Jing,et al.Determination of niobium and ten impurity elements in TaNb6 alloy by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2016,36(5):64-68.
