电感耦合等离子体原子发射光谱法测定人造金刚石中7种元素

人造金刚石的合成一般使用合金触媒以降低合成时所需的高温高压,但触媒的使用会使杂质元素进入人造金刚石内部,严重影响金刚石的性能。采用750℃预灰化样品,加入硫酸与盐酸加热冒烟处理样品,而后将样品于950℃高温灼烧灰化后,再使用盐酸溶解。选择Cr267.716nm、Mn 257.610nm、Ni 221.648nm、Al 309.271nm、Fe 259.940nm、Mg 279.553nm、Ti 334.941nm为分析线,使用电感耦合等离子体原子发射光谱法(ICP-AES)测定金刚石中Cr、Mn、Ni、Al、Fe、Mg、Ti等7种元素。各元素校准曲线的线性相关系数r为0.999 4~0.999 9,线性关系良好;方法中各元素的测定下限为0.021~0.27μg/g。按照实验方法测定金刚石样品中Cr、Mn、Ni、Al、Fe、Mg、Ti,结果的相对标准偏差(RSD,n=6)为0.75%~1.9%,回收率为93%~107%。将按照实验方法前处理后的3个人造金刚石样品溶液分别采用ICP-AES和电感耦合等离子体质谱法(ICP-MS)进行测定,结果相吻合。

Determination of seven elements in artificial diamond by inductively coupled plasma atomic emission spectrometry

During the synthesis of artificial diamond, the alloy catalyst is usually used to reduce the required high temperature and high pressure. However, the impurity elements in catalyst will enter into the interior of artificial diamond, which seriously influences the properties. The artificial diamond sample was pre-ashed at 750 ℃. After treatment with sulfuric acid and hydrochloric acid by heating, the sample was burned and ashed at 950 ℃ followed by dissolution with hydrochloric acid. Cr 267.716 nm, Mn 257.610 nm, Ni 221.648 nm, Al 309.271 nm, Fe 259.940 nm, Mg 279.553 nm and Ti 334.941 nm were selected as analytical lines. The content of seven elements in artificial diamond including Cr, Mn, Ni, Al, Fe, Mg and Ti was determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). The linear correlation coefficients of calibration curves of elements were r=0.999 4-0.999 9, indicating good linearity. The low limit of determination of elements were between 0.021 μg/g and 0.27 μg/g. The content of Cr, Mn, Ni, Al, Fe, Mg and Ti in artificial diamond sample was determined according to the experimental method. The relative standard deviations (RSD, n=6) were in the range of 0.75%-1.9%. The recoveries were between 93% and 107%. Three artificial diamond samples were pretreated according to the experimental method. The sample solution was determined by ICP-AES and inductively coupled plasma mass spectrometry (ICP-MS), respectively. The results were consistent with each other.