Lab 3 Report

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University of Texas, El Paso *

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MISC

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Chemistry

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Apr 3, 2024

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docx

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UTEP Department of Chemistry and Biochemistry Laboratory for Instrumental Methods of Analytical Chemistry Identification of Unknown Compounds by IR Spectroscopy Jacqueline Guzman James February 27, 2024
Objective For this experiment, oxidation of acetaminophen will be performed with cyclic voltammetry which occurs by an electrochemical cell, and the process will be optimized by selection of a buffer solution at a particular pH and a scan rate in units of mV/s. Conditions that give a maximum response for oxidation of acetaminophen in solution will then be applied to a prepared solution which contains dissolved Tylenol. Peaks in the collected voltammograms will be compared and utilized to determine the concentration of acetaminophen in Tylenol. Introduction The electroanalytical technique known as cyclic voltammetry studies electron transfer reactions where the flow of electrons is related to chemical changes. For electrochemical redox reactions, a molecule undergoes reduction or oxidation by means of an electrode that transfers an electron heterogeneously. With the electrode as an electrical conductor, this transfer process is initiated by a voltage from an external power source which is applied to the electrode to control the energy of the electrons within it. The transfer occurs when the electrons in the electrode have a greater energy than the LUMO of the molecule. A trace is visualized in a graph where the x-axis represents the applied potential (E), or voltage, and the y-axis is the response of system, or the current (i) that passes through it. An arrow is assigned to each trace to indicate the sweep direction of the potential that was scanned to obtain data, and it also indicates the starting point of the “forward scan.” The forward scan refers to the cathodic trace where there is a negative sweep from the starting potential E1 to the switching potential E2; the anodic trace follows in the reverse scan that sweeps positively back to E1. A significant parameter known as the scan rate (v) describes the speed (V/s) at which the
potential was varied linearly during the reaction. Peaks arise in cyclic voltammograms due to the equilibrium between the oxidized and reduced form of a molecular species as described by the Nernst equation. The species’ standard potential (E0) along with the respective activities of the redox analytes, termed as Ox (for oxidized) and Red (for reduced), are correlated to the standard potential (E) of the electrochemical cell: E = E 0 + RT nF ln ( Ox ) ( ¿ ) = E 0 + 2.3026 RT nF log 10 ( Ox ) ( ¿ ) Eq. 1 where R is the universal gas constant, T is the temperature, n is the number of electrons, and F is Faraday’s constant. For practicality, the Nerst equation may be modified by replacement of the activities with the concentrations of the oxidized and reduced forms of the species that undergoes the electron transfer so that n is equal to 1 and a formal potential E0’ replaces the standard potential E0: E = E 0 ' + RT nF ln ¿¿ Eq. 2 In this way, the influence of variation in electrode potential and species’ concentration allows prediction of how the system will respond in respect to time. A schematic of the electrochemical cell used in cyclic voltammetry is given below.
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