火花放电原子发射光谱法测定铁铬铝不锈钢中高含量铝  

Determination of high content of aluminum in iron-chromium-aluminum stainless steel by spark discharge atomic emission spectrometry

作　　者：张爽[1,2] 张文诚[1,2] 张征宇 ZHANG Shuang;ZHANG Wencheng;ZHANG Zhengyu(State Key Laboratory of Advanced Stainless Steel Materials,Taiyuan Iron&SteelGroup Co.,Ltd.,Taiyuan 030003,China;Technology Center,Shanxi Taiyuan Stainless Steel Co.,Ltd.,Taiyuan 030003,China)

机构地区：[1]太原钢铁(集团)有限公司,先进不锈钢材料国家重点实验室,山西太原030003 [2]山西太钢不锈钢股份有限公司技术中心,山西太原030003

出　　处：《冶金分析》2023年第5期46-51,共6页Metallurgical Analysis

摘　　要：铁铬铝不锈钢是非常重要的电热合金材料,铝含量的精准控制对提高其性能有重要的影响。用国际标准样品结合自制的太钢铁铬铝不锈钢控制样品绘制校准曲线,选择Al 308.22 nm为分析谱线,建立了火花放电原子发射光谱法测定铁铬铝不锈钢中高含量铝(Al质量分数在0.46%~6.12%之间)的方法。选择除了Al之外其他元素含量都比较接近的普通不锈钢样品与铁铬铝不锈钢样品作为对照组,进行金相观察。结果表明,普通不锈钢样品的晶粒尺寸较小,而铁铬铝不锈钢样品的晶粒明显细化,且边界轮廓致密、清晰,说明铁铬铝不锈钢样品的表面较为致密,这可能是铁铬铝不锈钢样品激发强度受其表面影响更大、测定结果波动较大的原因。重点考察了预燃时间对测定的影响,结果表明,Al的激发强度在预燃时间为8~11 s范围内相对稳定,最终选择预燃时间为11 s。取3块Al含量不同的铁铬铝不锈钢样品,按照实验方法进行10次平行分析,同时采用电感耦合等离子体原子发射光谱法(ICP-AES)进行方法对照试验,结果表明,两种方法测定结果具有良好的一致性,实验方法测定结果的相对标准偏差(RSD,n=10)为0.53%~0.98%。Iron-chromium-aluminum(FeCrAl)stainless steel is a very important electrothermal alloy material.The precise control of Al content has an important effect on improving its performance.The calibration curve was prepared using international standard samples and self-made control samples of Taigang FeCrAl stainless steel.Al 308.22 nm was selected as the analytical line.A method for the determination of high content Al(the mass fraction of Al was in range of 0.46%-6.12%)in FeCrAl stainless steel by spark discharge atomic emission spectrometry was established.The ordinary stainless steel and FeCrAl stainless steel samples with similar contents of other elements except for Al were used as the control group for metallographic observation.The results showed that the grain size of the ordinary stainless steel sample was small,while the grain size of the FeCrAl stainless steel sample was obviously refined,and the boundary contour was dense and clear,indicating that the surface of the FeCrAl stainless steel sample was relatively dense.It may be the reason that why the excitation intensity of the FeCrAl stainless steel sample was more affected by its surface,and the measurement results fluctuated greatly.The effect of pre-burning time on the determination was investigated.The results showed that the excitation intensity of Al was relatively stable when the pre-burning time was 8-11 s,so the pre-burning time of 11 s was finally adopted.Three FeCrAl stainless steel samples with different Al contents were selected and analyzed for 10 times according to the experimental method.Meanwhile,the inductively coupled plasma atomic emission spectrometry(ICP-AES)was used for method control test.The results showed that the determination results of two methods had a good consistency.The relative standard deviations(RSD,n=10)of determination results of experimental method were between 0.53%and 0.98%.

关 键 词：铁铬铝不锈钢 火花放电原子发射光谱法 铝 预燃时间 

分 类 号：O657.31[理学—分析化学] TF031[理学—化学]