高压微波消解-ICP-AES测定罗汉果中的微量元素

High Pressure Microwave Digestion and Determination of Microelements Siraitia grosvenorii by ICP-AES

关键词:  微量元素  微波消解  ICP-AES  罗汉果

Key words:  microwave digestion  ICP-AES  Siraitia grosvenorii

摘要:

采用密闭增压微波酸消解方式处理罗汉果试样,通过电感耦合等离子体光谱法(ICP-AES)测定罗汉果试样的9种微量元素:锌、铁、磷、锰、铅、铜、铝、镉和镁。罗汉果试样处理是先是在XT-9800型多用预处理加热仪上,用浓硝酸和过氧化氢混合液进行预消化后,用XT-9900型智能微波消解仪在3种(0.3MPa/120s;0.5MPa/240s;1.0MPa/90s)加压条件下进行彻底消化。电感耦合等离子体光源轴向同时观测9种微量元素的折中条件为:射频功率1100W,载气流量0.8L·min^-1。罗汉果试样测量结果令人满意。RSD(%,n=5)是铝1.21~9.81,镉0.89~1.18,铜0.85~4.72,铁4.48~6.71,镁0.27~1.16,锰0.51~1.00,磷0.20~0.91,铅0.86~4.33,锌0.042~0.87。加标回收率(%)是铝102.0~105.0,镉97.0~102.0,铜104.0,铁96.4~97.8,镁96.0~97.0,锰96.0~100.0,磷92.0~99.0,铅93.0~96.0,锌91.0~105.0。

Abstract:

For pretreatment, the Siraitia grosvenorii samples were pre-dissolved by nitric acid and hydrogen peroxid with the XT-9800 multifunctional heating device, then were digested completely using XT-9900 intelligent microwave digestion device.The three procedures of microwave digestion were:0.3MPa/120s, 0.5MPa/240s, 1.0MPa/90s.The compromise measurement conditions of inductively coupled plasma using axial viewing mode were RF power 1100W, carrier gas current 0.8L·min^-1. The results of two kinds of Siraitia grosvenorii samples were satisfying. RSD (%, n=5)Al 1.21~9.81, Cd 0.89~1.18, Cu 0.85~4.72, Fe 4.48~6.71, Mg 0.27~1.16, Mn 0.51~1.00, P 0.20~0.91, Pb 0.86~4.33, Zn 0.042~0.87, recovery (%)Al 102.0~105.0, Cd 97.0~102.0, Cu 104.0, Fe 96.4~97.8, Mg 96.0~97.0, Mn 96.0~100.0, P 92.0~99.0, Pb 93.09~6.0, Zn 91.01~05.0.