火花放电原子发射光谱法分析不锈钢中铬镍元素精密度和准确度的影响因素探讨

Discussion of factors influencing precision and accuracy in determination of chromium and nickel in stainless steel by spark discharge atomic emission spectrometry

在冶金行业的生产应用中,原子发射光谱仪被广泛应用于钢铁冶炼中。不锈钢冶炼过程中铬、镍元素的快速准确分析可以有效的提高生产效率,降低冶炼成本。实验就火花放电原子发射光谱法分析不锈钢中铬、镍元素的影响因素进行了探讨,研究发现光谱仪排气管堵塞、电极清洁程度、激发台污染、激发台冷却不良、电器元件老化等对铬和镍元素的分析精密度有显著影响,因此在进行样品分析时,要确保排气管路畅通,激发台冷却良好,并在激发前进行电极和激发台的清洁。对电极的距离、使用氩气压力、仪器维护周期、真空度、激发点重叠、样品分析温度等对铬和镍元素的准确度有显著影响,因此在进行样品分析时,要确保仪器真空度和氩气压力的正常稳定,要进行定期的仪器维护,要保证对电极的正确极距,分析样品要确保室温且激发点不得重叠等。而透镜污染程度则对铬和镍元素的影响不显著。在分析过程中,通过控制影响因素,可有效提高铬、镍元素的分析精密度和准确度,从而在提高生产效率的同时有效控制冶炼成本。

The atomic emission spectrometry has been widely used in metallurgical industry such as iron and steel smelting.The rapid and accurate analysis of chromium and nickel in smelting process of stainless steel can effectively improve the production efficiency and reduce the production cost.The influencing factors in determination of chromium and nickel in stainless steel by spark discharge atomic emission spectrometry were discussed.It was found that the analytical precision of chromium and nickel was greatly affected by the exhaust pipe blocking of spectrometer,the cleanliness of electrode,the pollution and bad cooling of excitation platform as well as the ageing of electrical apparatus.Therefore,during the analysis of sample,it should be sure that the exhaust pipe was unblocked,the cooling of excitation platform was good,and the electrode and excitation platform should be also well cleaned.The determination accuracy of chromium and nickel was significantly influenced by the electrode spacing,argon pressure,instrumental maintenance period,vacuum degree,excitation point overlapping and the analysis temperature of sample.Therefore,the vacuum degree and argon pressure should be normal and stable;the instrument should be also irregularly maintained;the electrode spacing should be proper;the sample should be analyzed at room temperature;the excitation points could not be overlapped.In addition,the pollution of lens had little influence on the analysis of chromium and nickel.The determination precision and accuracy of chromium and nickel could be effectively improved by controlling the influencing factors.Consequently,the production efficiency could be improved and the smelting cost could be also effectively controlled.