da Silva Iranaldo Santos, Richter Eduardo Mathias, do Lago Claudimir Lúcio, Gutz Ivano G R, Tanaka Auro Atsushi, Angnes Lúcio
Departamento de Química, CCET, Universidade Federal do Maranhão, São Luís, MA, Brazil.
Talanta. 2005 Sep 15;67(3):651-7. doi: 10.1016/j.talanta.2005.03.010. Epub 2005 Apr 18.
A simple and reliable FIA-potentiometric system for rapid assays of chloride in certain food samples is described and evaluated. The system is constituted by an aquarium air pump to propel the carrier solution, a manually operated injector, a homemade dialysis flow cell, a solid-state chloride detector (Ag/AgCl), a reference electrode and a multimeter connected to a microcomputer for data acquisition. The dialysis unit enables direct analysis of liquid food samples without any other previous treatment. The principal novelties are the precision (R.S.D. of 1.2% for whole milk) and rapidity (90 determinations/h) of FIA measurements near and below the lower end of the linear (Nernstian) response region of the chloride ion-selective electrode (ISE), with an estimated detection limit (3s) of 0.4mgL(-1) Cl(-) in the sample injected in donor stream. Data of peak potential versus sample chloride concentration (donor stream) was accurately fitted with a quadratic polynomial over the range between 4 and 1000mgL(-1) (r(2)=0.9999) and used as a calibration curve. The method was applied to the determination of chloride in milk and in coconut water samples. The validation of the results was done by comparison with a NIST reference material (milk) or by capillary electrophoresis (coconut water). For all analysis, no significant difference at a 95% confidence level was observed.
本文描述并评估了一种用于快速测定某些食品样品中氯离子的简单可靠的流动注射电位分析系统。该系统由一个用于推动载液的水族箱气泵、一个手动进样器、一个自制的透析流通池、一个固态氯离子检测器(Ag/AgCl)、一个参比电极以及一个连接到微型计算机用于数据采集的万用表组成。透析单元能够直接分析液体食品样品,无需任何其他预处理。主要创新点在于,在氯离子选择性电极(ISE)线性(能斯特)响应区域下限及以下附近进行流动注射分析测量时具有高精度(全脂牛奶的相对标准偏差为1.2%)和快速性(每小时90次测定),注入供体流中的样品中氯离子的估计检测限(3s)为0.4mgL⁻¹ Cl⁻。峰电位与样品氯离子浓度(供体流)的数据在4至1000mgL⁻¹范围内用二次多项式精确拟合(r² = 0.9999),并用作校准曲线。该方法应用于牛奶和椰子水样品中氯离子的测定。通过与美国国家标准与技术研究院(NIST)标准物质(牛奶)比较或通过毛细管电泳(椰子水)对结果进行验证。对于所有分析,在95%置信水平下未观察到显著差异。