Almost all of the applications of trihydric alcohols are included in the more than 150 uses of glycerol e.g., humectant, solvent, plasticizer, component of pharmaceuticals, and as a derivative employed in plastics, coatings, explosives and foods.1 Moreover, glycerol is one of the most important compounds to be monitored in a sugar-fermentation plant in order to improve the quality control of the process. 2 In the soap industry, monitoring of the glycerol concentration in lixivia and such is relevant in view of the related economical aspects.Advanced analytical characteristics are required for industrial control, and an increasing number on the applications of chemically modified electrodes as amperometric detectors in flow systems have been reported. [3][4][5][6][7][8][9] These include electrodes based on copper, cobalt and nickel for the electrocatalytic oxidation of carbohydrates in an alkaline solution at low potential.Nickel electrodes exhibit catalytic activity in the oxidation of a wide variety of organic compounds in alkaline solutions. The Ni(III) species is generated on the electrode surface at potentials in the region of 0.4 to 0.5 V vs. Ag/AgCl. The reactions are:Glycerol can be determinated by monitoring the Ni(II) and re-oxidizing this species by applying a suitable potential. Despite the versatility, simplicity and suitability of the nickel-chromium alloy as an amperometric detector, and the relevance of glycerol monitoring for the industrial production of soaps, detergents and such, the use of Ni-Cr alloy electrodes for this determination had not yet been reported.The main purpose of the present work was thus to develop a simple, fast and low-cost flow-injection procedure for glycerol determination in lixivia. Glycerol electrocatalytic oxidation in an alkaline medium at low potential was exploited. For this task, a Ni-Cr wire was used as an electrochemical detector, and its chemical composition and electrochemical characteristics were investigated.
Experimental
ApparatusThe electrochemical system comprised a MQPG-01 Microquimica computerized potenciostat (Florianópolis-SC, Brazil) equipped with Ag/AgCl (3 mol l −1 KCl) reference and platinum auxiliary electrodes (spiral, 0.2×100 mm) sealed in alkaline glass. The working electrode was made of Ni-Cr (ca. 80:20 w/w) by sealing the metal wire (o.d. 1.0 mm) in a glass tube so as to leave about 1-cm length exposed (microcylinder). Unless otherwise indicated, the potential scan rate was 100 mV s −1 . Flow-injection experiments were carried out in a system with an IPC-8 Ismatec peristaltic pump (Zürich, Switzerland) furnished with Tygon pumping tubes, a home-made injector 10 and 0.8 A flow-injection amperometric method for glycerol determination in samples relevant to the industrial production of soaps, detergents and such is presented. A nickel-chromium alloy micro-cylindric electrode was used as the electrochemical detector, which after a pretreatment exhibited good repeatability and stability. The method involved glycerol oxidation by an inactive Ni(OH...