Tuncel S G, Yenisoy-Karakas S, Dogangün A
Chemistry Department, Middle East Technical University, 06531 Ankara, Turkey.
Talanta. 2004 May 28;63(2):273-7. doi: 10.1016/j.talanta.2003.10.055.
Three digestion procedures have been tested on lichen samples for application in the determination of major, minor and trace elements (Al, Ca, Cd, Cr, Cu, Fe, K, Mg, Mn, Na, Ni, Pb, V and Zn) in lichen samples collected in Aegean Region of Turkey by inductively coupled plasma atomic emission spectrometer (ICP-AES). The acid mixture of concentrated HNO(3), H(2)O(2) and HF were used. The instrument was optimized using lichen matrix considering RF power, nebulizer pressure, auxiliary flow rate and pump rate. The accuracy of the overall analyses was first estimated by analysis of two certified reference materials. Good agreement between measured and reference values were found for almost all elements. As the second way of determining the accuracy, results obtained from independent analytical techniques (ICP-AES and instrumental neutron activation analysis (INAA)) were compared for all elements by analyzing real samples. Correlation coefficients of two techniques for the elements ranged between 0.70 (Mg) and 0.96 (Fe). Among the three digestion systems, namely microwave, open vessel and acid bomb, microwave digestion system gave the best recovery results. The method detection limit (MDL) was computed using reagent blanks of microwave digestion system since it provides cleaner sample preparation. Detection limit is adequate for all elements to determine the elements in lichen samples. The precision was assessed from the replicate analyses of reagent blanks of microwave digestion system and was found to be less than 1.5% relative standard deviation (R.S.D.).
针对土耳其爱琴海地区采集的地衣样本,采用电感耦合等离子体原子发射光谱仪(ICP - AES)测定其中的主要、次要和微量元素(铝、钙、镉、铬、铜、铁、钾、镁、锰、钠、镍、铅、钒和锌),已对三种消解程序进行了测试。使用了浓硝酸、过氧化氢和氢氟酸的混合酸。考虑到射频功率、雾化器压力、辅助流速和泵速,使用地衣基质对仪器进行了优化。首先通过分析两种有证标准物质来评估整体分析的准确性。几乎所有元素的测量值与参考值之间都有良好的一致性。作为确定准确性的第二种方法,通过分析实际样本,比较了独立分析技术(ICP - AES和仪器中子活化分析(INAA))对所有元素获得的结果。两种技术对各元素的相关系数在0.70(镁)至0.96(铁)之间。在微波消解、敞口容器消解和酸弹消解这三种消解系统中,微波消解系统给出了最佳的回收率结果。由于微波消解系统能提供更纯净的样品制备,因此使用其试剂空白计算方法检出限(MDL)。该检出限对于测定地衣样本中的所有元素来说是足够的。通过对微波消解系统试剂空白的重复分析评估精密度,发现相对标准偏差(R.S.D.)小于1.5%。