摘要
高品质稀土钢要求进行精确低氧含量控制,而依据现有GB/T 11261—2006标准进行氧含量测定,检测结果具有较大的不准确性。以具有不同镧、铈稀土元素含量的稀土钢为对象,以其氧含量精确测定为目标,基于惰气熔融-红外吸收光谱法,开展了分析功率、助熔剂和称样量对镧铈稀土钢中氧含量分析结果的影响研究。结果表明:对于不同镧、铈元素含量的稀土钢,需要采用不同的分析方法,当稀土钢中的镧、铈含量较低时,通过降低分析功率即可较为精确地测定稀土钢中的氧含量;对于镧、铈含量较高的稀土钢,在调控分析功率(4000~4500 W)的基础上,需同时采用锡作为助熔剂,并将助熔剂与样品比例设定为1∶1(称样量为0.3~0.6 g),即可实现氧含量的精确测定。精密度验证实验结果显示:采用所建立的方法测定氧含量的相对标准偏差(RSD)小于8.0%;采用钢标准样品进行加标回收实验,回收率在97.0%~108%,而加标回收率略有升高的原因在于助熔剂Sn降低了合金熔点,使少量难熔氧化物中的氧得到更充分释放。方法可用来准确测定不同镧、铈元素含量稀土钢中的氧含量。
High quality rare earth steel requires precise control of low oxygen content,but testing results for oxygen content determination based on existing GB/T 11261—2006 standards have significant inaccuracies.This study focused on rare earth steel with different levels of lanthanum and cerium rare earth elements,with the goal of accurately measuring its oxygen content.Based on inert gas melting infrared absorption technique,a study was conducted on the influence of analysis power,flux,and sample size on the analysis results of oxygen content in La-Ce rare earth steel.The results indicated that different analysis methods were needed for rare earth steels with different lanthanum and cerium content.When the content of lanthanum and cerium in rare earth steel was low,the oxygen content in rare earth steel can be accurately determined by reducing the analytical power.For the rare earth steel with high content of lanthanum and cerium,tin needs to be used as the flux at the same time,and the ratio of the flux to the sample should be set to 1∶1(weighing 0.3-0.6 g)to achieve accurate determination of oxygen content on the basis of regulating the analysis power(4000~4500 W),experiment for precision showed that the relative standard deviation(RSD)was less than 8.0%,and rates of recovery from 97.0%to 108%were confirmed by employing certified reference material.The reason for the slight increase in spiked recovery rate was that the fluxing agent Sn lowered the alloy melting point,allowing the oxygen in a small amount of refractory oxide to be more fully released.This method can be used for accurate determination of oxygen content in rare earth steel.
作者
张琳
陈玉凤
李辉
张重远
ZHANG Lin;CHEN Yufeng;LI Hui;ZHANG Zhongyuan(Institute of Metal Research,Chinese Academy of Sciences,Shenyang,Liaoning 110016,China)
出处
《中国无机分析化学》
北大核心
2024年第3期350-356,共7页
Chinese Journal of Inorganic Analytical Chemistry
基金
国家自然科学基金资助项目(52101165)。
关键词
稀土钢
氧
惰气熔融
红外吸收光谱法
rare earth steel
oxygen
inert gas fusion
infrared absorption spectrometry
