Gomes D M C, Segundo M A, Lima J L F C, Rangel A O S S
REQUIMTE, Serviço de Química-Física, Faculdade de Farmácia, Universidade do Porto, Rua Aníbal Cunha 164, 4050-047 Porto, Portugal.
Talanta. 2005 Apr 30;66(3):703-11. doi: 10.1016/j.talanta.2004.12.011. Epub 2005 Jan 6.
In the last decade, significant advances in flow analysis have been reported, namely the extensive use of computer-controlled devices to enhance the autonomy and performance of analysers. In the present work, computer-controlled multi-syringe flow injection systems are proposed to perform the spectrophotometric determination of available iron and boron in soil extracts. The methodologies were based on the formation of ferroin complex (determination of iron) and azomethine-H reaction (determination of boron). Both determinations were performed in manifolds with similar configurations by changing the reagents present in the different syringes. In the determination of iron, elimination of Schlieren effect in the detection system was achieved through the binary sampling approach, where a three-way valve was actuated to intercalate small slugs of sample and reagent, promoting better mixing conditions for solutions with different values of refractive index. In the determination of boron, in-line sample blank measurement was attained by omitting the introduction of reagent through software control, without manifold reconfiguration. Linear calibration curves were established between 0.50 and 10.0mgFel(-1) and between 0.20 and 4.0mgBl(-1). No systematic difference was found when soil extracts were analysed by the proposed methodologies and compared to the respective reference procedures.
在过去十年中,已有报道称流动分析取得了重大进展,即广泛使用计算机控制设备来提高分析仪的自主性和性能。在本研究中,提出了计算机控制的多注射器流动注射系统,用于对土壤提取物中的有效铁和硼进行分光光度测定。这些方法基于亚铁菲绕啉络合物的形成(铁的测定)和甲亚胺 - H反应(硼的测定)。通过改变不同注射器中存在的试剂,在具有相似配置的流路中进行这两种测定。在铁的测定中,通过二元进样方法消除了检测系统中的纹影效应,即通过驱动三通阀插入小体积的样品和试剂段,为具有不同折射率值的溶液提供了更好的混合条件。在硼的测定中,通过软件控制省略试剂引入实现了在线样品空白测量,无需对流路进行重新配置。在0.50至10.0mg Fe l(-1)和0.20至4.0mg B l(-1)之间建立了线性校准曲线。当用所提出的方法分析土壤提取物并与各自的参考程序进行比较时,未发现系统差异。