直流辉光放电发射光谱法测定合金铸铁中13种元素  

Determination of 13 elements in alloy cast iron by direct current glow discharge emission spectrometry

作　　者：邓军华 徐强 胡忠新 亢德华 杨洁 DENG Junhua;XU Qiang;HU Zhongxin;KANG Dehua;YANG Jie(State Key Laboratory of Metal Material for Marine Equipment and Application,Anshan 114009,China;Iron&Steel Research Institute of Ansteel Group,Anshan 114009,China)

机构地区：[1]海洋装备用金属材料及其应用国家重点实验室,辽宁鞍山114009 [2]鞍钢集团钢铁研究院,辽宁鞍山114009

出　　处：《冶金分析》2025年第1期54-61,共8页Metallurgical Analysis

摘　　要：合金铸铁具有优秀的物理、化学性能,对合金铸铁中合金元素的监测有利于改进铸件生产工艺并提高产品质量。控制激发电压1 100 V,激发电流50 mA,预燃时间60 s,积分时间15 s,光电倍增管电压850 V,以铁元素为内标绘制校准曲线,通过系数法扣除钼对硼的光谱干扰,建立了直流辉光放电发射光谱法测定合金铸铁中碳、硅、锰、磷、硫、镍、铬、铜、钼、铝、硼、钒、钛共计13种元素的方法。以分析元素的相对浓度及其对应的相对强度绘制校准曲线,校准曲线相关系数均不小于0.998 9,各元素的检出限不大于0.000 25%。合金铸铁标准物质的各元素测定值与认定值一致,测量结果的相对标准偏差(RSD,n=8)小于4%。采用国家标准方法GB/T 6379.3—2012中三因素错层套设计试验对合金铸铁盲样中硅元素的重复性限r、再现性限R和中间精密度进行评定。结果表明,硅的测定均值为3.115%,重复性限为0.041 2%、时间因素的中间精密度为0.134%,再现性限为0.139%。其重复性限和再现性限与GB/T 38441—2019、GB/T 24234—2009、GB/T 223.79—2007这3个标准方法的重复性限和再现性限加权后得到的重复性限r′=0.049%和再现性限R′=0.134%相当,说明评定过程相对合理。研究表明方法的重复性限、再现性限和优化得到的中间精密度可用于实验室内部质量监控,为实验室的盲样质控监控提供一种新的手段。Alloy cast iron has excellent physical and chemical properties.The monitoring of alloying elements in alloy cast iron is beneficial to improving the casting production process and product quality.The experimental conditions were controlled as follows:the excitation voltage was 1 100 V,the excitation current was 50 mA,the pre-burning time was 60 s,the integration time was 15 s,and the photomultiplier voltage was 850 V.Iron was used as internal standard to prepare the calibration curve.The spectral interference of molybdenum to boron was deducted by coefficient method.The determination method for 13 elements in alloy cast iron(including carbon,silicon,manganese,phosphorus,sulfur,nickel,chromium,copper,molybdenum,aluminum,boron,vanadium,and titanium) by direct current glow discharge emission spectrometry was established.The relative concentration and corresponding relative strength of the analysis elements were used to draw the calibration curves,and the correlation coefficients were not less than 0.998 9.The limits of detection of elements were not more than 0.000 25%.The measured value of elements in alloy cast iron certified reference material was consistent with the certified values,and the relative standard deviations(RSD, n=8) of the measurement results were less than 4%.The repeatability limit(r),reproducibility limit(R) and intermediate precision of silicon element in alloy cast iron blind sample were evaluated by the three-factor staggered layer sleeve design test in GB/T 6379.3-2012.The results showed that the mean value of silicon was 3.115%,the repeatability limit(r) was 0.041 2%,the intermediate precision of time factor was 0.134%,and the reproducibility limit(R) was 0.139%.The obtained repeatability limit and reproducibility limit were equivalent to repeatability limit r′=0.049% and reproducibility limit R′=0.134%,which were obtained by weighting of repeatability limit and reproducibility limit of three standard methods,i.e.,GB/T 38441-2019,GB/T 24234-2009,and GB/T 223.79-2007.It indicated that the

关 键 词：直流辉光放电发射光谱法 合金铸铁 多元素 错层套设计 中间精密度 

分 类 号：O657.31[理学—分析化学] TF594[理学—化学]