摘要
采用盐酸-硝酸-氢氟酸-高氯酸溶解样品,建立了电感耦合等离子体质谱法(ICP-MS)测定低合金钢中镧、铈、镨、钕的含量。根据丰度高和无干扰的原则来选择139La(99.911)、140Ce(88.48)、141Pr(100)、146 Nd(17.62)为测量同位素;对仪器工作条件进行了优化,确定功率为1 200W,载气流量为0.84L/min;讨论了测定条件对结果的影响,确定测定介质为2%硝酸;考察了基体质量浓度对待测元素信号强度的影响,确定基体质量浓度在0.5g/L以下;以铑、铟、铯和铊为内标元素对仪器信号漂移和基体效应进行校正试验,选择10ng/mL铯为内标。基体浓度小于0.5mg/mL。方法检出限为0.00072~0.0017ng/mL,方法测定下限为0.0024~0.005 7ng/mL。采用实验方法对低合金钢实际样品进行测定,测定结果与电感耦合等离子体发射光谱法(ICP-AES)基本一致,相对标准偏差(RSD,n=6)在1.2%~4.0%之间。
The sample was dissolved with hydrochloric acid-nitric acid-hydrofluoric acid-perchloric acid.The determination method of lanthanum,cerium,praseodymium and neodymium contents in low alloy steel by inductively coupled plasma mass spectrometry(ICP-MS)was established.According to the principle of high abundance and no interference,139 La(99.911),140 Ce(88.48),141 Pr(100)and 146 Nd(17.62)were selected as the measuring isotopes.The working conditions of instrument were optimized:the power was 1 200 W and the carrier gas flow rate was 0.84 L/min.The effect of determination conditions on results was discussed,and 2% nitric acid was selected as the determination medium.Moreover,the influence of matrix mass concentration on signal intensity of testing elements was investigated.It was found that the suitable mass concentration of matrix should be lower than 0.5 g/L.The correction tests for instrumental signal drift and matrix effect were conducted using Rh,In,Cs and Tl as internal standard elements,and 10 ng/mL Cs was finally selected as the internal standard.The matrix concentration should be less than 0.5 mg/mL.The detection limits of method were between 0.000 72 and 0.001 7 ng/mL.The lower determination limit was in range of 0.002 4-0.005 7 ng/mL.The actual low alloy steel sample was determined according to the experimental method,and the found results were basically consistent with those obtained by inductively coupled plasma atomic emission spectrometry(ICP-AES).The relative standard deviation(RSD,n=6)were between 1.2% and 4.0%.
出处
《冶金分析》
CAS
CSCD
北大核心
2017年第11期17-21,共5页
Metallurgical Analysis
关键词
电感耦合等离子体质谱法
稀土元素
低合金钢
inductively coupled plasma mass spectrometry
rare earth element
low alloy steel
