Wójtowicz Marzena, Kozak Joanna, Danielewska Karolina, Kościelniak Paweł
Department of Analytical Chemistry, Faculty of Chemistry, Jagiellonian University, Ingardena 3, 30-060 Kraków, Poland.
Talanta. 2009 Sep 15;79(4):1006-10. doi: 10.1016/j.talanta.2009.02.053. Epub 2009 Mar 9.
The proposed approach relies on titration of a sample that is gradually diluted in strictly controlled way in the flow injection system developed. On each step of sample dilution equal volumes of the sample and titrant solutions are simultaneously injected into two carrier streams and the zones are merged with each other. Then, they are mixed completely in the mixing chamber, merged with a stream of indicator and directed to a detector. It has been revealed that the method provides the results with accuracy better than +/-3.3% (RE) and with mean repeatability lower than 1.0% (RSD). When the analyte concentration in a sample is too low to be determined directly, the procedure of titration with standard addition is exploited. The proposed approach has been successfully applied to the determination of total acidity in vinegar and magnesium and calcium in pharmaceutical products. The results obtained were comparable with those provided by the reference methods. The proposed procedure is characterized by low consumption of sample (usually less than 2 mL), titrant (about 3 mL) and indicator (about 0.6 mL). Average time of a single analysis is similar to time of traditional batch analysis.
所提出的方法依赖于在开发的流动注射系统中以严格控制的方式对逐渐稀释的样品进行滴定。在样品稀释的每个步骤中,将等体积的样品和滴定剂溶液同时注入两个载流中,然后将这些区域相互合并。接着,它们在混合室中完全混合,与指示剂流合并并导向检测器。结果表明,该方法提供的结果准确度优于±3.3%(相对误差),平均重复性低于1.0%(相对标准偏差)。当样品中分析物浓度过低无法直接测定时,采用标准加入滴定法。所提出的方法已成功应用于醋中总酸度以及药品中镁和钙的测定。所得结果与参考方法提供的结果相当。所提出的方法具有样品消耗量低(通常小于2 mL)、滴定剂消耗量低(约3 mL)和指示剂消耗量低(约0.6 mL)的特点。单次分析的平均时间与传统批量分析的时间相近。