火花放电原子发射光谱法测定轴承钢中残余元素

Determination of residual elements in bearing steel by spark discharge atomic emission spectrometry

残余元素含量已成为衡量轴承钢质量的重要指标,因此有必要对轴承钢中残余元素进行监测和控制。通过对试样制备的条件进行优化,建立了用火花放电原子发射光谱法(SparkAES)对轴承钢中Ca、Ni、Mo、Cu、Nb、V、Ti、As、Sn、Pb、Sb这11种残余元素含量进行测定的方法。结果表明,采用铣样机对试样进行制备,控制铣样总深度为1.0mm,刀头平移速度为150mm/min时,测定结果的相对标准偏差相对最小。采用钢光谱标样对设备的准确性进行验证,并通过调整响应曲线修正系统偏差。平行取6块GCr15轴承钢样品,按照实验方法进行制备和分析,各元素测定结果的相对标准偏差(RSD,n=6)均小于5%。采用实验方法分别对6个轴承钢标准物质中Ca、Ni、Mo、Cu、Nb、V、Ti、As、Sn、Pb、Sb进行测定,测定结果与认定值相符。

The content of residual elements had become an important index to measure the quality of bearing steel.Therefore,it was necessary to monitor and control the residual elements in bearing steel.The sample preparation conditions were optimized.The determination method of eleven residual elements(including Ca,Ni,Mo,Cu,Nb,V,Ti,As,Sn,Pb and Sb)in bearing steel by spark discharge atomic emission spectrometry(Spark-AES)was established.It was found that the relative standard deviation of determination results was smallest under the following experimental conditions:the sample was prepared with milling machine;the total milling depth of sample was controlled at 1.0 mm;the translational velocity of milling head was 150 mm/min.The accuracy of instrument was verified with the certified reference material for steel spectral analysis.The systematic deviation was corrected by adjusting the response curves.Six parallel samples of GCr15 bearing steel were prepared and determined according to the experimental method.The relative standard deviations(RSD,n=6)of determination results of the above eleven elements were all less than 5%.The proposed method was applied for the determination of Ca,Ni,Mo,Cu,Nb,V,Ti,As,Sn,Pb and Sb in six certified reference materials of bearing steel,and the results were consistent with the certified values.