火花源原子发射光谱法测定海绵钛样品及样品制备方法的影响  

Determination of sponge titanium by spark source atomic emission spectrometry and the impact of sample preparation method on determination

作　　者：俞超[1] 汪永喜 蒋增辉[1] 曾次元[1] 

机构地区：[1]上海市供水调度监测中心,上海200002 [2]金川有限公司检测中心,甘肃金昌737100

出　　处：《冶金分析》2016年第6期46-49,共4页Metallurgical Analysis

摘　　要：从样品制备评价和校准曲线的建立两方面开展对火花源原子发射光谱法测定海绵钛中Si、Fe、Mn、Mg等元素的实验研究。主要考察了样品表面的均匀性、车削纹和车削深度对测定结果的影响。研究表明,保持激发表面平整、光洁、无明显车削纹(表面粗糙度Ra≤1.6μm)、车削深度控制在12mm以内,可获得相对稳定的测定结果。利用电感耦合等离子体原子发射光谱法(ICP-AES)测定并经化学分析法确认后定值的样品绘制校准曲线避免了绘制曲线的标样与实际样品存在基体不匹配的问题,拓展了火花源原子发射光谱仪中内置的Si、Fe、Mn等曲线的测定范围,并建立了Mg的校准曲线,各曲线相关系数R2≥0.995。采用实验方法对海绵钛样品中Si、Fe、Mn、Mg进行测定,并与ICP-AES法进行对照,结果吻合性良好。t检验结果表明,实验方法与ICP-AES法无显著性差异。The spark source atomic emission spectrometry for the determination of Si, Fe, Mn and Mg is studied through evaluation of the sample preparations and establishment of the calibration curves. The influence of uniformity and cutting traces of the sample surfaces and cutting depth of the samples on determi- nation are investigated. The results demonstrate that stable detecting results can be acquired on the condition of keeping the excited surfaces smooth without cutting traces （surface roughness R_a≤1.6 μm） and keeping cutting depth of the samples within 12 mm. The calibration curves established by virtue of the in- ductively coupled plasma atomic emission spectrometry（ICP-AES） which are confirmed by the chemical a- nalysis can avoid matrix mismatch of the standards used to draw the calibration curves that have been es- tablished in the facililLy with the actual samples. The measuring ranges of Si, Fe and Mn are extended and the calibration curve of Mg is established with R^2 of the curves above 0. 995 totally. Moreover, the pro- posed method is applied to the determination of Si, Fe, Mn and Mg in sponge titanium and is compared with the ICP-AES. The results of t-test demonstrate that there is no significant difference between the spark source atomic emission spectrometry and the ICP-AES.

关 键 词：火花源原子发射光谱法 海绵钛 硅 铁 锰 镁 样品制备评价 校准曲线建立 

分 类 号：O657.31[理学—分析化学]