电感耦合等离子体发射光谱(ICP-OES)法测定石灰石中5种氧化物含量

Determination of Five Oxides in Limestone by Inductively Coupled Plasma Optical Emission Spectrometry

建立了电感耦合等离子体发射光谱(ICP-OES)法测定石灰石样品中5种氧化物氧化镁(MgO)、三氧化二铁(Fe2O3)、二氧化硅(SiO2)、氧化锰(MnO)、三氧化二铝(Al2O3)含量的方法。先将样品与无水碳酸钠和四硼酸钠高温熔融后,再用盐酸进行消解可以很好地溶解石灰石样品。选择Mg285.21nm、Fe238.20nm、Si251.61nm、Mn257.61nm、Al396.15nm为分析谱线,采用空白校正的方法校正基体的影响。在选定的实验条件下,各元素标准曲线的线性相关系数均不小于0.999,测定结果的相对标准偏差(RSD,n=6)在1.8%~2.4%,各测定元素的加标回收率也在94%~105%。按照实验方法将各元素测定结果与5种国家标准测定方法得出的结果进行比对,准确度、精密度、回收率均在理想范围内。结果表明,所建立的方法可以满足石灰石中5种元素联测的要求,并且更加快速、准确。

Inductively coupled plasma optical emission spectrometry (ICP-OES) has been used to determine magnesium oxide (MgO), ferric oxide (Fe 2O 3), silicon dioxide (SiO 2), manganese oxide (MnO) and aluminum oxide (Al 2O 3) contents in the limestone. After being fused with anhydrous sodium carbonate and sodium tetraborate at high temperature, the limestone sample can be well dissolved by acid hydrolysis with hydrochloric acid. The analytical spectral lines Mg 285.21 nm, Fe 238.20 nm, Si 251.61 nm, Mn 257.61 nm and Al 396.15 nm were selected respectively as analytical spectral lines. The effect of matrix is corrected by blank correction. Under the selected experimental conditions, the linear correlation coefficients of calibration curves of elements were all not less than 0.999 within the linear range. The relative standard deviation (RSD, n =6) of the test results were between 1.8% and 2.4%, and the labeled recovery of each measurement element was between 94% and 105%. In accordance with the experimental method, the test results of each element were compared with the results obtained by the five national standard test methods, and the accuracy, precision and recovery were within the ideal range. The results show that this method can meet the requirements of simultaneous measurement of five elements in limestone, and is more rapid and accurate. The study demonstrates the method will also play an important role in the analysis and characterization of limestone materials.