电感耦合等离子体质谱快速测定水泥中7种金属氧化物

Rapid Determination of Seven Metal Oxides in Cement by Inductively Coupled Plasma Mass Spectrometry

采用氢氟酸-高氯酸-高氯酸-硝酸(5HF+0.5HClO_(4)+2HClO_(4)+5HNO_(3))混酸四阶段进行电热板消解模式,提取水泥中K、Na、Ca、Mg、Fe、Al、Ti七种金属组分,同时优化测试参数,消除电离和多原子间的干扰,结合HMI模式内标校正法,建立电感耦合等离子体质谱(ICP-MS)快速测定水泥中氧化钾、氧化钠、氧化钙、氧化镁、三氧化二铁、三氧化二铝、二氧化钛7种金属氧化物的检测方法。在选定的试验条件下,各组分的线性关系均不小于0.9991,同时采用两种水泥国家标准物质,测试结果均在标准认定值范围内,相对标准偏差(RSD,n=6)在0.33%~2.70%之间,加标回收率在96.80%~99.25%之间,准确度和精密度良好。此方法可快速、准确地测定出水泥中的7种氧化物组分,为水泥产品实现快速质量监督提供新方向。

Seven K,Na,Ca,Mg,Fe,Al,Ti in cement were extracted by four-stage mixed acid of hydrofluoric acid-perchloric acid-perchloric acid-nitric acid(5HF+0.5 HClO_(4)+2HClO_(4)+5HNO_(3))with electric heating plate digestion,at the same time,the test parameters are optimized to eliminate ionization and multi-atom interference,and the HMI mode internal standard correction method is adopted,to develop a rapid method for the deter-mination of potassium oxide,sodium oxide,calcium oxide,magnesium oxide,iron(III)oxide oxide,aluminium oxide oxide and titanium dioxide oxide in cement by Inductively coupled plasma mass spectrometry(ICP-MS).Under the selected test conditions,the linear relationship of each component is not less than 0.9991,and two national standard substances of cement are used at the same time,the relative standard deviation(RSD,N=6)was be-tween 0.33%and 2.70%,and the recoveries were between 96.80% and 99.25%.It can quickly and accurately determine 7 oxide components in cement,which provides a new direction for rapid quality supervision of cement products.