Name: trace analysis by stripping voltammetry
Uploaded: 2024-12-05T18:31:57.000Z
Duration: 1 min 13 s
Channel: JoVE

Bei der Stripping-Voltammetrie werden Spurenmetallanalyten auf einer Elektrodenoberfläche abgeschieden. Darauf folgt das Abisolieren – anodisch, kathodisch oder adsorptiv –, wenn der Strom in Abhängigkeit vom angelegten Potential überwacht wird.
Die voltammetologische Voltammetrie des anodischen umfasst zwei Schritte. Zunächst wird ein konstantes kathodisches Potential an die Arbeitselektrode angelegt, wodurch die Ionen auf das entsprechende Metall reduziert werden, das auf der Elektrode abgeschieden ist.
Als nächstes werden die abgeschiedenen Metalle beim Anlegen eines anodischen Potentials in ihren ionischen Zustand oxidiert und von der Elektrodenoberfläche abgestreift. Der resultierende gemessene anodische Strom ist proportional zur Analytkonzentration der Probe.
Bei der kathodischen Stripping-Voltammetrie wird die Quecksilberelektrode oxidiert, die sich mit dem Analyten verbindet und sich als unlöslicher Film ablagert. Dies wird in die Lösung zurückgeführt, indem auf ein negativeres Potential abgetastet und der kathodische Strom gemessen wird.
Die adsorptive Stripping-Voltammetrie beinhaltet die Adsorption des Analyten auf der Elektrodenoberfläche ohne Elektrolyse, gefolgt von einem anodischen oder kathodischen.

voltammetrie: stripping-methoden

Voltammetry: Stripping Methods

Die anodische Stripping-Voltammetrie (ASV), die kathodische Stripping-Voltammetrie (CSV) und die adsorptive Stripping-Voltammetrie (AdSV) sind elektrochemische Techniken, die zur Bestimmung von Spurenmengen von Analyten in Lösungen verwendet werden. Bei diesen Methoden wird ein Potential an eine Elektrode angelegt und der resultierende Strom gemessen.

Anodische Stripping-Voltammetrie (ASV)

Die ASV wird zur Bestimmung von Metallen und Halbmetallen auf Spurenebene verwendet. Sie umfasst zwei Schritte: Abscheidung und Stripping (Ablösen). Zuerst wird ein negatives Potential an die Arbeitselektrode angelegt, wodurch die Analytionen reduziert und auf der Elektrodenoberfläche abgeschieden werden. Nach der Abscheidung wird das Potential in positiver Richtung gescannt, wodurch die abgeschiedenen Analytionen oxidieren und sich von der Elektrodenoberfläche ablösen. Der während dieser Prozesse resultierende Strom wird gemessen und aufgezeichnet und zeigt die proportionale Beziehung zur Analytkonzentration.

<ul style="list-style-type: disc; padding-left: 35px; margin: 0;">
	<li>Optimale Bedingungen: Sorgen Sie für eine saubere und gut polierte Elektrodenoberfläche, kontrollieren Sie die Abscheidungszeit und halten Sie einen stabilen pH-Wert in der Lösung aufrecht.</li>
	<li>Herausforderungen: Störungen durch andere Ionen, Elektrodenverschmutzung (Fouling) und die Notwendigkeit einer präzisen Potentialkontrolle.</li>
</ul>

Kathodische Stripping-Voltammetrie (CSV)

Bei der CSV wird die Quecksilberelektrode bei der Interaktion mit dem Analyten oxidiert, wodurch ein unlöslicher Film auf ihrer Oberfläche entsteht. Anschließend wird das Potential in negativer Richtung gescannt, wodurch der Analyt reduziert und von der Elektrodenoberfläche abgelöst wird. Der resultierende Strom wird gemessen und ist proportional zur Konzentration des Analyten. Die CSV wird typischerweise verwendet, um organische Verbindungen wie bestimmte Schadstoffe und Medikamente zu bestimmen.

<ul style="list-style-type: disc; padding-left: 35px; margin: 0;">
	<li>Optimale Bedingungen: Wählen Sie einen geeigneten Leitelektrolyt und sorgen Sie für eine ordnungsgemäße Temperaturkontrolle.</li>
	<li>Herausforderungen: Handhabung der Quecksilberelektrode aufgrund ihrer Toxizität und Sicherstellung einer reproduzierbaren Filmbildung.</li>
</ul>

Adsorptive Stripping-Voltammetrie (AdSV)

Die AdSV ist eine Variante der Stripping-Voltammetrie, bei der die Analyten vor dem Stripping-Schritt auf der Elektrodenoberfläche adsorbiert werden. An die Arbeitselektrode wird ein Potential angelegt, was zur Adsorption der Analyten führt. Nach der Adsorption wird der Analyt durch Änderung des Potentials von der Elektrode entfernt und der resultierende Strom gemessen, um die Konzentration des Analyten zu quantifizieren. Die AdSV wird häufig verwendet, um sowohl organische als auch anorganische Spezies zu bestimmen, darunter verschiedene Schadstoffe, Pestizide und Schwermetalle.

<ul style="list-style-type: disc; padding-left: 35px; margin: 0;">
	<li>Optimale Bedingungen: Wählen Sie die geeignete Adsorptionszeit, das geeignete Potential und das geeignete Elektrodenmaterial.</li>
	<li>Herausforderungen: Konkurrenz um Adsorptionsstellen auf der Elektrode und Empfindlichkeit gegenüber Verunreinigungen in der Lösung.</li>
</ul>

Voltammetrie: Stripping-Methoden

Die anodische Stripping-Voltammetrie (ASV), die kathodische Stripping-Voltammetrie (CSV) und die adsorptive Stripping-Voltammetrie (AdSV) sind elektrochemische Techniken, die ...

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Analytical Chemistry

Analytische Chemie

Unit 1

Einheit 1

Electrochemical Analyses and Redox Titration

Elektrochemische Analysen und Redoxtitration

electrochemical-analyses-and-redox-titration

KEY TERMS AND CONCEPTS

ZENTRALE BEGRIFFE UND KONZEPTE

trace analysis by stripping voltammetry

Stripping voltammetry is an electrochemical method used to detect trace amounts of analytes in solution. It works by applying a potential to an electrode and measuring the current that results. The current is then used to estimate the analyte concentration.

Anodic Stripping Voltammetry, or ASV, is used for metals and metalloids at very low levels. It has two main steps: deposition and stripping. First, a negative potential reduces analyte ions and deposits them on the working electrode surface. Then the potential is scanned in the positive direction, and the deposited ions oxidize and strip off the surface. The measured current is proportional to the analyte concentration. A clean, well-polished electrode surface, controlled deposition time, and stable pH help ASV work well. Common problems include interference from other ions, electrode fouling, and the need for precise control of potential.

Cathodic Stripping Voltammetry, or CSV, uses a different stripping step. In this method, a mercury electrode is oxidized while it interacts with the analyte, which forms an insoluble film on the surface. The potential is then scanned in the negative direction, reducing and stripping the analyte from the electrode. The current that appears is proportional to analyte concentration. CSV is often used for organic compounds, including some pollutants and drugs. It works best with the right supporting electrolyte and good temperature control. Its challenges include the toxicity of mercury and the need for reproducible film formation.

Adsorptive Stripping Voltammetry, or AdSV, depends on adsorption before stripping. Adsorption means the analyte species stick to the electrode surface. After this step, the potential is changed and the analyte is stripped off, and the resulting current is measured to find the concentration. AdSV can be used for organic and inorganic species, including pollutants, pesticides, and heavy metals. The method depends on the right adsorption time, potential, and electrode material. It can also be affected by competition for adsorption sites and by impurities in the solution.

Trace Analysis by Stripping Voltammetry

electrochemistry: overview

Electrochemistry and Redox Reactions

Electrochemistry connects electrical measurements with chemical reactions, especially oxidation and reduction. It focuses on how electron movement helps explain reaction behavior. Oxidation is the loss of electrons from a substance, and reduction is the gain of electrons. A species with strong electron affinity is an oxidizing agent, or oxidant. A species that donates electrons is a reducing agent, or reductant. These redox steps are often described with half-reactions. When electrons move...

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Static and dynamic electrochemical methods study what happens at the boundary between an electrode and a solution. These interfacial methods focus on the electrode-solution interface rather than the overall properties of the liquid. They are useful in electroanalytical chemistry because they can detect very small changes in analyte concentration. These methods are grouped by whether a nonzero current flows through the cell. Static methods, such as potentiometry, measure the cell potential...

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Reference and Indicator Electrodes in Potentiometry

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redox titration: overview

Redox Titration Endpoints and Indicators

Redox titration uses electron transfer in a redox, or reduction-oxidation, reaction to find the concentration of an unknown solution. The titrant has a known concentration, and it is added gradually to the analyte, which is the solution being tested. The endpoint shows when the reaction between the two substances is complete. Before a redox titration begins, the analyte should be in a single oxidation state. If needed, this is done by pre-oxidizing or pre-reducing the sample with an auxiliary...

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Choosing Oxidizing Titrants in Redox Titration

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Endpoint Detection in Potentiometric Titration

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Electrode Weighing in Electrogravimetric Analysis

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Coulometry and Electrical Charge Analysis

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Measuring Analyte Charge by Potentiostatic Coulometry

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Controlled-Current Coulometry in Redox Analysis

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Electrically Generated Reagents in Titration

Coulometric titrations use an electrically generated reagent to measure the amount of a substance in a sample. The electron acts as the standard reagent, and the result depends on the current and the time used to generate it. The method follows the same basic idea as a regular titration, including endpoint detection. Two conditions are essential for this type of titration. First, the electrode reaction that makes the reagent must be 100% efficient. Second, the generated reagent must react...

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Voltammetry for Detecting Redox Species

Voltammetry measures current in an electrochemical cell as the applied potential changes. It is an electroanalytical method used to study redox-active species. The current response is shown on a graph called a voltammogram. A voltammetric cell uses three electrodes: a working electrode, a reference electrode, and an auxiliary electrode. Redox reactions happen at the working electrode, and a potentiostat controls its potential. The reference electrode, such as a saturated calomel electrode or a...

voltammetry: factors affecting measurements

voltammetry-factors-affecting-measurements

Voltammetry and Faradaic Current

Voltammetry measures faradaic current, which is the current created by redox reactions of an analyte at the working and auxiliary electrodes. The current from reduction is called cathodic current and carries a positive charge. The current from oxidation is called anodic current and has a negative charge. The applied potential at the working electrode controls the flow of faradaic current. The size of that current depends on how fast the oxidation or reduction reaction occurs at the electrode...

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Voltammogram Shapes and Redox Analysis

Voltammograms are current plots made against applied potential. They help show how an electrochemical system behaves during a redox reaction. The shape of the plot depends on how the current is measured and on whether convection, or fluid movement, is present. When convection is present, as in hydrodynamic voltammetry, the voltammogram usually has a sigmoid shape. In this case, the current rises from a residual current to a limiting current at the analyte’s oxidation or reduction potential.

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Polarography and Voltammetry with Mercury Drops

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voltammetry: stripping methods

Stripping voltammetry is an electrochemical method used to detect trace amounts of analytes in solution. It works by applying a potential to an electrode and measuring the current that results. The current is then used to estimate the analyte concentration. Anodic Stripping Voltammetry, or ASV, is used for metals and metalloids at very low levels. It has two main steps: deposition and stripping. First, a negative potential reduces analyte ions and deposits them on the working electrode surface.

amperometry: overview

Measuring Analytes with Amperometric Sensors

Amperometry measures specific analytes in a solution by tracking the electric current from an electrochemical reaction. A constant potential is applied between a working electrode and a reference electrode. The current that results is proportional to the analyte concentration. The Clark oxygen electrode is a common example of amperometry. It uses a cathode and an anode sealed inside a gas-permeable membrane. The cathode is typically platinum or gold, and the anode is silver. When a potential...

key terms and concepts

Learn how ASV, CSV, and AdSV detect trace analytes by measuring current changes at an electrode, with uses, setup needs, and common challenges.

Trace Analysis by Stripping Voltammetry | JoVE K12

analytical chemistry

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Trace Analysis by Stripping Voltammetry

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