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Post-lab Questions: 1. Compare a classical titration (endpoint determined using an indicator) and a potentiometric titration in terms of: a.

Precision and accuracy b. Advantages and disadvantages In terms of precision and accuracy the classical method depends mostly on choosing the right indicator whose physical change (the endpoint) occurs in an interval close to the equivalence point of the reaction. Also, the physical change must be big enough to be noticeable by the human eye. In potentiometric titrations, since a pH/mV meter is used to measure the change in Volts while the reaction is occurring, there is no need to rely only on changes in color (for example) to determine the endpoint. Since the electrode perceives the change in potential while it is occurring, the endpoint in the reaction can be accurately determined but its precision is limited by the sensitivity of the electrodes. Potentiometric titrations should be more precise and accurate. Still, potentiometric titrations do have disadvantages. For example, they are time consuming. For some reactions, for the electrode in the reaction solution to accurately give changes in potentials time must pass for the reaction to stabilize every time the titrating solution is added. In classical titrations, although there are limitations caused by the perception of visual changes in the indicator and the precision with which the endpoint volume is measured, this procedure can be relatively convenient and fast. Also, it could be less costly than potentiometric titrations. 2. Compare the two graphical methods (normal E vs. Volume, and first derivative curves) used to determine the equivalence point. Which is better, if any, and why? The equivalence point in the graphical method E vs. Volume occurs in the steepest part of the curve because the potential is plotted as a function of the volume of titrant added. 1 In the curve of the first derivative, the equivalence point occurs in the maximum or peak of the curve. 1 The plot of the first derivative is better because the endpoint can be seen clearly. 3. What is the primary function of the phosphoric acid in this titration? What makes potassium dichromate an excellent oxidizing agent for this titration? Phosphoric acid interacts with Fe+3, lowering the Fe+3concentration and in turn the potential of the Fe+3/ Fe+2 pair.1 This results in a more drastic change in potential around the endpoint.1 Potassium dichromate is a perfect oxidizing agent in this experiment because: a. Dichromate and iron (II) react quantitatively and with a known stoichiometry b. The reaction is sufficiently fast to be practical for titration c. The change in potential is large enough to produce a well-defined endpoint d. Standard solutions of potassium dichromate can be prepared from a weighted quantity of the dried solid and need not be standardized; the prepared solutions are very stable.1

4. Is the percent difference between the average indicator and potentiometric results significant? Justify your answer. The larger the difference in standard potentials between titrant and analyte, the greater the break in the titration curves at the equivalence point. A redox titration is usually feasible if the difference in potentials is >0.2 V. However, the end point of such a titration is not very sharp and is best-detected potentiometrically. If the difference in formal potentials is 0.4 V, then a redox indicator usually gives a satisfactory end point.1 5. Is the oxidation efficiency of potassium dichromate pH dependent? Justify your answer. Yes, in basic solution, Cr2O2-7 is converted into yellow chromate ion (CrO2-4), whose oxidizing power is nil.2 Reference: 1. De Jess, M.A.; Vera, M.; Areizaga, H.I. Analitycal Chemistry for Engineers Laboratory Manual [Online]; 2011. https://moodle.uprm.edu/file.php/664/Manuals/Manual_CHEM_3055L.pdf 2. Harris, D.C. Quantitative Chemical Analysis, 8th ed.; W.H. Freeman: New York, 2010.