Titulador automático baseado em filmes digitais para determinação de dureza e alcalinidade total em águas minerais/Titulador automático baseado em filmes digitais para determinação de dureza e alcalinidade total em águas minerais

Abstract

Total hardness and Total alkalinity are important physico-chemical parameters for the evaluation of water quality and are determined by volumetric analytical methods. These methods have difficult to detect the endpoint of the titration due to the difficult of viewing the color transition inherent to each of them. To circumvent this problem, here is proposed a new automatic method for the detection of the titration end point for the determination of total hardness and total alkalinity in mineral water samples. The proposed flow-batch titrator consists of a peristaltic pump, five three-way solenoid valves, a magnetic stirrer, an electronic actuator, an Arduino MEGA 2560TM board, a mixing chamber and a webcam. The webcam records the digital movie (DM) during the addition of the titrant towards mixing chamber, also recording the color variations resulting from chemical reactions between titrant and sample within chamber. While the DM is recorded, it is decompiled into frames ordered sequentially at a constant rate of 30 frames per second (FPS). The first frame is used as a reference to define the region of interest (RI) of 48 × 50 pixels and the R channel values, which are used to calculate the Pearson's correlation coefficient (r) values. r is calculated between the R values of the initial frame and each subsequent frame. The titration curves are plotted in real time using the values of r (ordinate axis) and the total opening time of the valve titrant (abscissa axis). The end point is estimated by the second derivative method. A software written in ActionScript 3.0 language manages all analytical steps and data treatment in real time. The feasibility of the method was attested by its application for the analysis of natural water samples. Results were compared with classical titration and did not present statistically significant differences when the paired ttest at the 95% confidence level was applied. The proposed method is able to process about 71 samples per hour, and its precision was confirmed by overall relative standard deviation (RSD) values, always lower than the 2,4% for total hardness and 1,4% for total alkalinity.