电感耦合等离子体原子发射光谱法测定钒铬钛合金中11种元素

以V₂O₅、Cr₂O₃和TiO₂直接还原熔炼钒铬钛合金的新工艺具有显著降低生产成本优势,但需解决原料、还原剂以及熔炼设备所引入杂质对产品品质的影响,为此,建立了电感耦合等离子体原子发射光谱法(ICP-AES)测定V-4Cr-4Ti合金中Al、As、Co、Cu、Fe、Mg、Mn、Ni、P、K、Na等11种微量杂质元素分析方法。方法重点考察了在V、Cr、Ti三元合金组分共存体系下,基体效应、光谱干扰和连续背景叠加等影响因素,归纳了基体及共存组分对待测元素高灵敏分析谱线的光谱干扰情况,优选了待测元素的分析谱线、背景校正区域以及光谱仪工作条件等参数。采用基体匹配和同步背景校正法消除高V、高Cr和高Ti共存基体的影响。结果表明:Al、As、Co、Cu、Fe、Mg、Mn、Ni、P的检测范围为0.001%~0.25%,K、Na的检测范围为0.002%~0.25%;校准曲线线性相关系数不小于0.9995,方法的测定下限为0.0012%(K)、0.0015%(Na)、0.0003%~0.0009%(其余元素)。按照实验方法测定4个V-4Cr-4Ti合金样品中Al、As、Co、Cu、Fe、Mg、Mn、Ni、P、K、Na,0.x%水平测定结果的相对标准偏差(RSD,n=8)小于5%,0.0x%~0.00x%水平测定结果的相对标准偏差(RSD,n=8)小于10%,即使低于方法检测下限0.001%水平测定结果的相对标准偏差(RSD,n=8)也小于15%。按照实验方法对4个V-4Cr-4Ti合金样品中Al、As、Co、Cu、Fe、Mg、Mn、Ni、P、K、Na进行加标回收试验,回收率为90%~114%。实验方法用于测定3个V-4Cr-4Ti合金样品中Al、As、Co、Cu、Fe、Mg、Mn、Ni、P、K、Na,与电感耦合等离子体质谱法(ICP-MS)测定结果相吻合。

Determination of eleven elements in vanadium-chromium-titaniumalloy by inductively coupled plasma atomic emission spectrometry

The new technology, which used V₂O₅, Cr₂O₃ and TiO₂ for direct reduction and smelting of vanadium-chromium-titanium alloy, could significantly decrease the production cost. However, the influence of introduced impurities by raw materials, reducing reagents and smelting equipment on the product quality should be solved. Therefore, a determination method of 11 microelements including Al, As, Co, Cu, Fe, Mg, Mn, Ni, P, K and Na in vanadium-chromium-titanium (V-4Cr-4Ti) alloy was established by inductively coupled plasma atomic emission spectrometry (ICP-AES). The influencing factors such as matrix effect, spectral interference and continuous background superposition were focused in the system where V, Cr and Ti were coexisting. The interference of high-sensitivity spectral lines by matrix effect and coexisting components was investigated. The analytical lines of testing elements, the background correction area and the working conditions of spectrometer were optimized. The matrix matching and synchronous background correction were used to eliminate the influence of coexisting matrix with high V, high Cr and high Ti. The results showed that the detection range of Al, As, Co, Cu, Fe, Mg, Mn, Ni and P was 0.001%-0.25%, while the detection range of K and Na was 0.002%-0.25%. The linear correlation coefficients of calibration curve were not less than 0.9995. The low limit of determination was 0.0012% (K), 0.0015% (Na), and 0.0003%-0.0009% (other elements). The proposed method was applied for the determination of Al, As, Co, Cu, Fe, Mg, Mn, Ni, P, K and Na in four V-4Cr-4Ti alloy samples. The relative standard deviations (RSD, n=8) of determination results at 0.x% level were less than 5%, and the RSD (n=8) of determination results at 0.0x%-0.00x% were less than 10%. Even for the determination results which were lower than the determination limit of method (i.e., 0.001%), the RSD (n=8) was still less than 15%. The recovery tests of Al, As, Co, Cu, Fe, Mg, Mn, Ni, P, K and Na in four V-4Cr-4Ti alloy samples were conducted according to the experimental method. The recoveries were between 90% and 114%. The proposed method was applied for the determination of Al, As, Co, Cu, Fe, Mg, Mn, Ni, P, K and Na in three V-4Cr-4Ti alloy samples, and the results were consistent with those obtained by inductively coupled plasma mass spectrometry (ICP-MS).