摘要
实验验证了采用电感耦合等离子体原子发射光谱法(ICP-OES)测定保护渣中钾、钠、锂含量的可行性。采用盐酸-硝酸-氢氟酸加热冒高氯酸烟和微波消解两种方法均可较彻底地溶解样品。选择K317.933 nm、Na589.592 nm、Li670.784 nm为分析线,Y371.029为内标元素谱线,采用碳酸钙溶解作为基体匹配,配制标准溶液并绘制工作曲线,以减少基体效应。钠的质量分数在1.00~12.00%,钾、锂质量分数在0.10~1.00%范围内,各元素的质量分数与对应的发射强度呈线性,工作曲线线性相关系数大于0.999。ICP-OES法测定保护渣中钾、钠、锂的相对标准偏差分别为5.66~6.08%、2.19~2.43%、4.35~4.50%,略低于火焰原子吸收光谱法,两种方法检测结果之差未超过标准YB/T190.5和YB/T190.9中的实验室间允许差,证实了检测方法可用于生产和科研检测。
The feasibility of the testing of potassium,sodium and lithium in the mold fluxes by ICP-AES was verified.Using hydrochloric acid nitric acid hydrofluoric acid to heat perchloric acid smoke and microwave digestion,the samples can be completely dissolved.K 317.933 nm,Na 589.592 nm and Li 670.784nm are selected as analysis lines,Y371.029 nm as internal standard element spectrum lines,calcium carbonate dissolution is used as matrix matching to prepare standard solution and draw working curve to reduce base rest effect.The mass fraction of sodium is in the range of 1.00~12.00%,the mass fraction of potassium and lithium is in the range of 0.10~1.00%,the mass fraction of each element is linear with the corresponding emission intensity,and the linear correlation coefficient of the working curve is greater than 0.999.The relative standard deviations of potassium,sodium and lithium in protective slag determined by ICP-OES are 5.66~6.08%,2.19~2.43%and 4.35~4.50%respectively,which are slightly lower than that of flame atomic absorption spectrometry.The difference between the two methods is not more than the allowable difference between laboratories in YB/T190.5 and YB/T190.9,which proves that the method can be used in production testing and scientific research.
作者
赵二敏
郑兴跃
赵炳建
袁辉
尧建莉
史琦
ZHAO Er-minZHENG Xing-yue;ZHAO Bing-jian;YUAN Hui;YAO Jian-li;SHI Qi(Tangshan Iron and Steel Group Co.,Ltd.,HEBEI 063016;HBIS Laoting Iron and Steel Co.,Ltd.,HEBEI 063000)
出处
《天津冶金》
CAS
2020年第4期59-62,共4页
Tianjin Metallurgy
关键词
电感耦合等离子体原子发射光谱法
微波消解
保护渣
曲线
inductively coupled plasma atomic emission spectrometry
microwave digestion
mold fluxes
curve
