Department of Chemical Science and Technology, University of Udine, via Cotonificio 108, I-33100 Udine, Italy.
Talanta. 2010 Mar 15;80(5):1809-15. doi: 10.1016/j.talanta.2009.10.024. Epub 2009 Nov 8.
A sensitive and fast responding electrochemical sensor is described for the determination of free and total sulphur dioxide in wines and grape juices which prevents interferences coming from ethanol and other natural components. It consists of a cell provided with a porous gold working electrode supported on one face of an ion-exchange membrane, acting as a solid polymer electrolyte (SPE), which allows gaseous electroactive analytes to be detected. This sensor was used as an amperometric detector for a flow injection system in which controlled volumes of headspace equilibrated with samples were injected. This approach was adopted to make also possible the determination of total SO(2), avoiding drawbacks caused by the high relative humidity generated by the sample heating resulting from the neutralization reaction of excess NaOH, whose addition was required to release sulphur dioxide from its combined forms. Factors affecting the detection process were examined and optimised. Under the identified optimal conditions, SO(2) detection resulted in sharp peaks which allowed to infer detection limits for a signal-to-noise ratio of 3, referred to liquid samples, of 0.04 and 0.02 mg L(-1) for free and total SO(2) which were determined at 20 and 35 degrees C, respectively. Moreover, the responses were found to be characterized by good repeatability (+/-2% and +/-4%, respectively) and linear dependence on the SO(2) concentration over a wide range (0.2-500 mg L(-1) for both free and total SO(2)). Finally, the long-term stability of the sensor turned out to be totally satisfactory in that responses changed of +/-9% alone even after long periods of continuous use. The application to some commercial wines and grape juices is also presented.
一种用于测定葡萄酒和葡萄汁中游离和总二氧化硫的灵敏、快速响应电化学传感器,可防止来自乙醇和其他天然成分的干扰。它由一个带有多孔金工作电极的电池组成,该电极支撑在离子交换膜的一个面上,作为固体聚合物电解质(SPE),允许检测气态电活性分析物。该传感器被用作流动注射系统中的安培检测器,其中受控体积的顶空与样品平衡后被注入。这种方法也被采用来确定总 SO(2),避免了由于过量 NaOH 的中和反应导致样品加热产生的高相对湿度所带来的缺点,该反应需要添加 NaOH 才能将二氧化硫从其结合形式中释放出来。检查并优化了影响检测过程的因素。在所确定的最佳条件下,SO(2)检测得到了尖锐的峰,允许推断出液体样品的信噪比为 3 时的检测限,游离 SO(2)和总 SO(2)的检测限分别为 0.04 和 0.02mg/L,分别在 20 和 35°C 下进行测定。此外,发现响应具有良好的重复性(分别为+/-2%和+/-4%),并且在很宽的范围内(游离 SO(2)和总 SO(2)的浓度范围均为 0.2-500mg/L)与 SO(2)浓度呈线性关系。最后,传感器的长期稳定性完全令人满意,即使在长时间连续使用后,响应变化也仅为+/-9%。还介绍了该传感器在一些商业葡萄酒和葡萄汁中的应用。