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Voltammetry: A Look at Theory and Application: Bobby Diltz 14 March 2005

Voltammetry is an electroanalytical technique that uses three electrodes to measure current as the applied potential is changed over time. It is an extremely sensitive technique capable of detecting substances at trace levels down to parts per trillion. Various working electrodes like mercury and graphite allow voltammetry to analyze a wide range of concentrations in applications such as wastewater analysis, industrial water testing, and environmental studies. Different voltammetry techniques exist including polarography, stripping voltammetry, and cyclic voltammetry which provide different sensitivities and capabilities for qualitative or quantitative analysis.

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117 views15 pages

Voltammetry: A Look at Theory and Application: Bobby Diltz 14 March 2005

Voltammetry is an electroanalytical technique that uses three electrodes to measure current as the applied potential is changed over time. It is an extremely sensitive technique capable of detecting substances at trace levels down to parts per trillion. Various working electrodes like mercury and graphite allow voltammetry to analyze a wide range of concentrations in applications such as wastewater analysis, industrial water testing, and environmental studies. Different voltammetry techniques exist including polarography, stripping voltammetry, and cyclic voltammetry which provide different sensitivities and capabilities for qualitative or quantitative analysis.

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tila
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© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Voltammetry: A Look at Theory

and Application
Bobby Diltz
14 March 2005
Analytical Methods
• Chromatography
– Large amounts of materials used
– Not very sensitive
• Spectroscopy
– Very sensitive
– Able to separate species
• Voltammetry
– Extremely sensitive
– Few components used
– Wide range of concentrations
What is Voltammetry?
• As an applied potential is
changed over time a
current is measured
• Reduces ions in the
electrode
• Commonly uses three
electrodes
– Working Electrode (WE)
– Auxiliary Electrode (AE)
– Reference Electrode (RE)
Applications
• Ultra Trace range metals (sub ppb)
• Wastewater Analysis
• Industrial Water/Liquor Analysis
– “Polarographic Determination of Sulfur Compounds in
Pulping Liquors” Dr. J.J. Renard
• Sulfur compounds in weapons
• Pharmaceutics
• Environmental Studies
• Biological/Biochemical Analysis
• Plating Analysis
Techniques
• Polarography
– Uses direct reduction at the electrode
– This technique has limited sensitivity
– Uses the mercury drop electrode (SDME, DME)
• Voltammetry (Anodic Stripping/Adsorptive
Cathodic Stripping)
– Electrochemical deposition
– Determination by stripping
– Very high sensitivity, down to the parts per trillion range
– Uses a stationary electrode (HDME, RDE)
Working Electrode
• The working electrode is used to show the
response of the analyte to the potential
• Mercury Electrode
– Hanging Drop Mercury Electrode (HDME)
• Used in the ppb to low ppm range
– Static Drop Mercury Electrode (SDME)
• Used in the low ppm range
– Dropping Mercury Electrode (DME)
• Used in the ppm range
Working Electrode (cont)
• Rotating Disk Electrode (RDE)
– Ultra Trace Graphite
– Gold
– Glassy Carbon*
• Many other types of WE
Auxiliary Electrode
• Completes the circuit between the
potentiostat and the WE
• Two different types available
– Platinum
– Glassy Carbon
Reference Electrode
• Provides a reference potential to the
WE/AE circuit
• Two types of RE
– Ag/AgCl in KCl
– Hg/HgCl in saturated KCl
Electrolyte
• One of the most difficult parts of method
development with voltammetry!!
• Electrolyte selection is greatly based on type of
matrix
• Electrolytes reduce voltage drop and promote a
better flow of electrons through the solution, while
also stabilizing half-wave potentials of analytes
• Adjusts the pH
• Increases selectivity
Measurement Modes
• Direct Current
– Sensitivity of 10-5 mol/L
– Low separation ability
– Wave form of polarogram
• Differential Pulse
– Sensitivity of 10-8 mol/L
– High separation
– Peak form of polarogram
More Measurement Modes
• Alternating Current
– Only for reversible
reactions
• Square Wave
– Better for reversible
reactions
– Fast determinations
• Cyclic Voltammetry
– Useful in kinetic
studies/qualitative analysis
– Uses both oxidation and
reduction steps
Why Use Voltammetry?
• Handles high salt concentrations better than
chromatographic instrumentation
• Can differentiate between ionic species
– Example: Cr6+  Cr3+
• Extremely low detection limits
• Can detect a wide range of species
Summary
• Voltammetry is a very useful form of
instrumental analysis
• Wide range of applications
• Assortment of electrodes allows for a very
specific analysis of different chemicals
• Capable of very low to moderate detection
limits- parts per trillion to low ppm range
References
• “Chloride by Cathodic Stripping
Voltammetry” Princeton Applied
Research- Analytical Instrument Division
• “Voltammetric Determination of Zinc,
Cadmium, Lead, Copper, Thallium, Nickel,
and Cobalt in Water Samples” Application
note No. 231/2 E

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