Luiz Raposo Jorge, de Oliveira Silvana Ruella, Caldas Naíse Mary, Neto José Anchieta Gomes
São Paulo State University - Unesp, Analytical Chemistry Department, P.O. Box 355, 14801-970 Araraquara, SP, Brazil.
Anal Chim Acta. 2008 Oct 10;627(2):198-202. doi: 10.1016/j.aca.2008.08.016. Epub 2008 Aug 27.
The usefulness of the secondary line at 252.744nm and the approach of side pixel registration were evaluated for the development of a method for sequential multi-element determination of Cu, Fe, Mn and Zn in soil extracts by high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS). The influence of side pixel registration on the sensitivity and linearity was investigated by measuring at wings (248.325, 248.323, 248.321, 248.329, and 248.332nm) of the main line for Fe at 248.327nm. For the secondary line at 252.744nm or side pixel registration at 248.325nm, main lines for Cu (324.754nm), Mn (279.482nm) and Zn (213.875nm), sample flow-rate of 5.0mLmin(-1) and calibration by matrix matching, analytical curves in the 0.2-1.0mgL(-1) Cu, 1.0-20.0mgL(-1) Fe, 0.2-2.0mgL(-1) Mn, 0.1-1.0mgL(-1) Zn ranges were obtained with linear correlations better than 0.998. The proposed method was applied to seven soil samples and two soil reference materials (IAC 277; IAC 280). Results were in agreement at a 95% confidence level (paired t-test) with reference values. Recoveries of analytes added to soil extracts containing 0.15 and 0.30mgL(-1) Cu, 7.0 and 14mgL(-1) Fe, 0.60 and 1.20mgL(-1) Mn, 0.07 and 0.15mgL(-1) Zn, varied within the 94-99, 92-98, 93-101, and 93-103% intervals, respectively. The relative standard deviations (n=12) were 2.7% (Cu), 1.4% (Fe - 252.744nm), 5.7% (Fe - 248.325nm), 3.2% (Mn) and 2.8% (Zn) for an extract containing 0.35mgL(-1) Cu, 14mgL(-1) Fe, 1.1mgL(-1) Mn and 0.12mgL(-1) Zn. Detection limits were 5.4microgL(-1) Cu, 55microgL(-1) Fe (252.744nm), 147microgL(-1) Fe (248.325nm), 3.0microgL(-1) Mn and 4.2microgL(-1) Zn.
为开发一种通过高分辨率连续光源火焰原子吸收光谱法(HR-CS FAAS)顺序多元素测定土壤提取物中铜、铁、锰和锌的方法,评估了252.744nm处的二级谱线和侧像素校准方法的实用性。通过在铁的248.327nm主线的翼部(248.325、248.323、248.321、248.329和248.332nm)进行测量,研究了侧像素校准对灵敏度和线性的影响。对于252.744nm处的二级谱线或248.325nm处的侧像素校准、铜(324.754nm)、锰(279.482nm)和锌(213.875nm)的主线、5.0mLmin(-1)的样品流速以及通过基体匹配进行校准,在0.2 - 1.0mgL(-1)铜、1.0 - 20.0mgL(-1)铁、0.2 - 2.0mgL(-1)锰、0.1 - 1.0mgL(-1)锌范围内获得了线性相关性优于0.998的分析曲线。所提出的方法应用于七个土壤样品和两种土壤标准物质(IAC 277;IAC 280)。在95%置信水平(配对t检验)下,结果与参考值一致。添加到含有0.15和0.30mgL(-1)铜、7.0和14mgL(-1)铁、0.60和1.20mgL(-1)锰、0.07和0.15mgL(-1)锌的土壤提取物中的分析物回收率分别在94 - 99%、92 - 98%、93 - 101%和93 - 103%区间内变化。对于含有0.35mgL(-1)铜、14mgL(-1)铁、1.1mgL(-1)锰和0.12mgL(-1)锌的提取物,相对标准偏差(n = 12)分别为2.7%(铜)、1.4%(铁 - 252.744nm)、5.7%(铁 - 248.325nm)、3.2%(锰)和2.8%(锌)。检测限分别为5.4μg L(-1)铜、55μg L(-1)铁(252.744nm)、147μg L(-1)铁(248.325nm)、3.0μg L(-1)锰和4.2μg L(-1)锌。