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Recently, sediment samples were collected from Lake Nakuru and analyzed by ASV in the manner described above. Given the sample data in Table 4 , calculate the current concentration levels of the heavy metals Cu, Pb and Zn in the sediment samples obtained from Lake Nakuru.

Introduction

What do the data tell you about the heavy metal concentrations in the sediments at Lake Nakuru? Have the concentrations increased or decreased since the sampling? Sample number. Note: All samples analyzed were a The The exact concentration depending on standard mass weighed out can be determined via calculation. Data Analysis — Suspended Solids. Recently, suspended solid samples were collected from Lake Nakuru and analyzed by ASV in the manner described above. Given the sample data in Table 5 , calculate the current concentration levels of the heavy metals Cu, Pb and Zn in suspended solids in Lake Nakuru.

What do the data tell you about the heavy metal concentrations in the suspended solids at Lake Nakuru? The exact concentration depending on standard mass weighed out can be calculated. Chromium measurement. You may have noticed that the data analyzed so far was for lead, copper and zinc, while the Nelson paper has reported data for chromium.

If we wish to use voltammetry for chromium measurement, the technique of choice is Adsorptive Stripping Voltammetry. The key difference between Adsorptive and Anodic stripping voltammetry is in the deposition accumulation procedure. In this alternative technique, the accumulation step is purely adsorptive i. The stripping step for the adsorptive method can involve either anodic or cathodic removal of the analyte from the electrode.

During the accumulation step in adsorptive stripping voltammetry, does a redox reaction occur? Note also that the Nelson paper measured chromium by graphite furnace atomic absorption spectroscopy. Graphite furnace AAS is an excellent choice for a total chromium measurement. As previously mentioned, one advantage of electrochemical over spectroscopic methods is the speciation capabilities. While adsorptive stripping methods have been developed to differentiate between Cr III and Cr VI species Dominguez , the data below will reflect a total chromium measurement.

This analysis will keep this introductory material simpler and allow comparison with the graphite furnace AAS data in Nelson In a typical experiment for chromium measurement a HMDE Golimowski or mercury-based electrode Bas and Wang is employed as the working electrode. A complexing agent is added to complex with chromium III , forming a surface-active complex that adsorbs to the electrode surface.

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Introduction to Voltammetric Analysis: Theory and Practice - Francis Thomas and Gunter Henze RK

The Cr III complex adsorbs to the electrode surface. Subsequently, during the stripping step, the electrode is cathodically scanned and the complex is reduced, giving rise to the analytical signal. The reduction is a one electron process:. Differential Pulse Adsorptive Stripping Voltametry measurements of chromium. Simulated sample data acquired for Lake Nakuru sediment samples are given in Table 7. Sample preparation was similar to that described by Locatelli The sample underwent the adsorptive stripping procedure outlined above.

Hand-calculate the concentration for sample 1 then set up a spreadsheet to calculate the concentrations of the metals for all three samples. Recently, sediment and suspended solid samples were collected from Lake Nakuru and analyzed by ASV in the manner described above. Given the sample data in Tables 7 and 8 , calculate the current concentration levels of chromium in the sediment samples obtained from Lake Nakuru.

What do the data tell you about chromium concentration in the sediments and suspended solids in Lake Nakuru? Has the concentration increased or decreased since the sampling? The exact concentration depending on standard mass weighed out can be determined on the corresponding Excel spreadsheet. If your sample was known to contain metal ions that cannot be measured by ASV, what other techniques would you suggest trying? Brainina, K. Copeland, T. Dominguez, O. Chimica Acta, , , Golimowski, J.

Harvey , D. Kelly, R. Lau, O-W. Locatelli, C. Nelson, Y. Tercier, M. Wang, J. Learning Outcomes After reading about ASV and working through this learning module, you should be able to: Describe some advantages of anodic stripping voltammetry. Outline the general steps in an ASV experiment.

Free Introduction To Voltammetric Analysis Theory And Practice

List the important parameters that affect sensitivity and detection limits in an ASV experiment. Perform calculations for determination of metal ion content in unknowns analyzed by ASV. These calculations will utilize the single standard addition quantitation method. Purpose The purpose of this learning module is to introduce students to the electrochemical technique of anodic stripping voltammetry ASV. Content specific to voltammetric methods and ASV can be found in the citations listed in the reference section of this document and are available free of charge at the following websites: in the Analytical Electrochemistry module Kelly at the ASDL website click here to link directly to the ASV section A chapter on voltammetric techniques can be found in the eText Analytical Chemistry 2.

Additionally, you can perform a search with the key words anodic stripping voltammetry at the ASDL website click here for the voltammetry section of the ASDL collection accessed on June 26, Theory Read the Anodic Stripping Voltammetry section of the Analytical Electrochemistry eLearning module and answer the following questions.

Advantages of ASV Anodic stripping voltammetry, along with certain other electrochemical techniques, is capable of determining the oxidation state of a metal this is called speciation. Data and Analysis In the following section, you will review the data reported in Nelson for the analysis by atomic spectroscopy and XRF of Cr, Cu, Pb, and Zn in suspended solids and dried sediments from Lake Nakuru. Data from Nelson Study, Table 2 gives the levels for chromium, copper, lead, and zinc found in Lake Nakuru sediments and suspended solids collected by Nelson, et al.

Nelson Table 2.

CH403 13 Fundamentals of Electrochemistry

Sample Preparation and Data Analysis. Average 11 sites. Pulse repetition s. Pulse amplitude mV.


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