为提高ARL4460直读光谱仪测定钢铁中8种常规元素分析结果的准确性,对一些主要的影响因素特别对碳及硫量测定的影响因素做了试验,并对其结果作了探讨,从中得到了一些有利于提高测定准确性和精密度的方法和措施,主要有以下几点:① 改变了仪器出厂时设定的光源参数(冲洗时间由10 s降为2 s,预燃时间由7 s降为6 s,曝光时间由8 s降为3 s);② 测定碳、硫、磷须用99.999%的高纯氩,且应控制其压力在0.30 MPa左右;③ 试样表面要干净平整,纹路清晰,应用细砂砂轮机处理试样表面;④ 制备定碳样品时,样品温度不能高于40 ℃,且保持其起始状态的纹路粗细程度;⑤ 分析室环境温度应保持恒定(25 ℃左右),每8 h进行一次工作曲线的校正;⑥ 测定硫的试样若温度过高,宜先将其冷却至接近室温再作分析,且在分析时应至少取3个分布均匀的激发点,且需根据试样特点作现场校正曲线,用控制试样进行类型标准化。

Aiming to raising of accuracy of analytical results of 8 common elements in iron and steel by the ARL 4460 direct-reading spectrometer, testing for some influential factors, especially for determinations of carbon and sulfur, was made. The following measures were found to be effective for improving both the accuracy and precision of the determinations: ① light source parameters set during manufacturing were modified by lowering the time of development from 10 s to 2 s, the time of pre-ignition from 7 s to 6 s, and time of exposure from 8 s to 3 s; ② for the determination of C, S and P, high-purity argon (99.999%) with its pressure of 0.30 MPa, should be used; ③ a fine grinder should be used in preparing sample in order to make the surface of sample clear and plain, as well as to have clear grain; ④ in determination of carbon, temperature of sample should be kept below 40 ℃, and to keep the finess of its grain in its original state; ⑤ room temperature of the lab should be kept constant around 25 ℃, and correction of working curves should be made every 8 h; ⑥ in determination of sulfur, samples with relatively higher temperature should be cooled to near room temperature before analysis, and at least 3 evenly deposited excitation sites should be taken as well as correction and standardization of the standard working curve should be made.