碱熔-电感耦合等离子体原子发射光谱法测定海洋沉积物中铝铁锰钛

准确测定海洋沉积物中Al、Fe、Mn、Ti,对寻找金属矿产资源有着重要意义,因此有必要建立一种快速、低成本的分析方法。样品加入1.0 g NaOH,选择镍坩埚在700 ℃下熔融15 min,用5%HNO₃溶解后,加入25 μg Cd内标克服仪器漂移带来的影响,选择各元素的分析谱线为Al 396.152 nm、Fe 238.204 nm、Mn 259.373 nm、Ti 336.121 nm,采用海洋沉积物标准物质绘制校准曲线消除基体效应的影响,使用电感耦合等离子体原子发射光谱法(ICP-AES)测定海洋沉积物中Al、Fe、Mn、Ti。方法中Al₂O₃、Fe₂O₃、MnO、TiO₂检出限分别为0.914、0.096、0.022、0.068 mg/g。按照实验方法测定海洋沉积物实际样品与标准物质,各组分测定结果的相对标准偏差(RSD,n=5)为0.62%~3.7%,且标准物质的测定结果与认定值相一致。

Determination of aluminum,iron, manganese,titanium in marine sediments by inductively coupled plasma atomic emission spectrometry with alkali fusion

Accurate determination of Al, Fe, Mn and Ti in marine sediments had important significance to search for metallic mineral resources. Therefore, it was necessary to establish a fast and low-cost analysis method. 1.0 g of NaOH was added into the sample. The mixture was fused in nickel crucible at 700 ℃ for 15 min. After dissolving with 5% HNO₃, 25 μg of Cd internal standard was added to overcome the influence of instrument drift. Al 396.152 nm, Fe 238.204 nm, Mn 259.373 nm and Ti 336.121 were selected as the analytical lines. The calibration curves were prepared with the certified reference materials of marine sediment in order to eliminate the influence of matrix effect. The contents of Al, Fe, Mn and Ti in marine sediment sample were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). The limits of detection for Al₂O₃, Fe₂O₃, MnO and TiO₂ were 0.914, 0.096, 0.022 and 0.068 mg/g, respectively. The actual samples and certified reference materials of marine sediment were determined according to the experimental methods. The relative standard deviations (RSD, n=5) of determination results were between 0.62% and 3.7%. The determination results were consistent with the certified values.