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Precipitation Titration: Endpoint Detection Methods01:19

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In argentometric precipitation titrations, endpoints can be detected visually by the Mohr, Volhard, and Fajans methods. In the Mohr method, adding a soluble chromate indicator gives an initial yellow color to the analyte solution. As the titrant is added, the first excess of silver ions forms a red silver chromate precipitate, marking the endpoint. The solution pH should be maintained at about 8 by adding solid CaCO3.
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Controlled-Current Coulometry: Coulometric Titration01:18

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Coulometric titrations are a form of titrimetric analysis where the reagent is generated electrically, and its amount is evaluated based on current and generating time. The electron serves as the standard reagent. The procedure is similar to conventional titrations, such as endpoint detection.
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Coulometry is one of the rapid, most accurate, and precise analytical techniques that determine the quantity of an analyte by measuring the electrical charge needed for its complete electrolysis without using any analytical standards. The total charge passed during electrolysis correlates with the analyte amount by Faraday's laws of electrolysis. For accurate coulometric measurements, a charge equal to Faraday's constant multiplied by the number of electrons involved in the relevant...
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Potentiometric Titration: Overview01:31

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Potentiometric titration is a quantitative analytical technique that determines the concentration of an analyte by measuring the potential difference between the two electrodes in the solution. The endpoint of a potentiometric titration is the point at which there is a significant change in the potential difference. It occurs when the stoichiometric reaction between the analyte and the titrant is complete. The endpoint is usually determined graphically by plotting the measured potential...
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Controlled-Current Coulometry: Overview01:27

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Controlled current coulometry, also known as amperostatic coulometry, is a technique used in electrochemical analysis to measure the quantity of a substance through the controlled passage of current. It involves the application of a constant current to an electrochemical cell containing the analyte of interest. As the current flows through the cell, the analyte undergoes a redox reaction at the electrode surface, resulting in a charge transfer. By monitoring the time required for a certain...
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EDTA: Indirect and Alkalimetric Titration01:23

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Unlike direct titration, back-titration, and displacement titration, indirect titration is an EDTA titration method for quantifying anions. In the indirect titration method, anions are precipitated as their insoluble salts with excess metal ions. The filtrate containing the excess metal ions is directly titrated with standard EDTA until the endpoint is achieved. Another approach involves extracting the metal ion and back-titrating with standard EDTA to obtain the endpoint. In this way, the...
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Coulometric back titration based on all-solid-state electrodes for phenylephrine hydrochloride determination.

Qiuyu Kong1, Jinghao Wu1, Meng Chen2

  • 1School of Pharmaceutical Science, Sun Yat-Sen University, Guangzhou, 510006, Guangdong, China.

Analytical and Bioanalytical Chemistry
|April 15, 2022
PubMed
Summary

This study introduces an all-solid coulometric titration method using a glassy carbon electrode (GCE) for phenylephrine hydrochloride (PHE) analysis. This maintenance-free technique offers accurate and precise drug determination with improved operational simplicity.

Keywords:
Corrosion resistanceCoulometric titrationDrug determinationElectrochemistrySolid-state electrodes

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Area of Science:

  • Analytical Chemistry
  • Electrochemistry
  • Pharmaceutical Analysis

Background:

  • Traditional coulometric titration methods rely on liquid reference electrodes, posing challenges like frequent maintenance, leakage risks, and operational constraints.
  • These limitations necessitate the development of more robust and user-friendly analytical techniques for quantitative drug determination.

Purpose of the Study:

  • To develop and validate an all-solid coulometric titration method utilizing a glassy carbon electrode (GCE).
  • To assess the long-term stability and performance of the GCE in bromine and iodine solutions for pharmaceutical analysis.
  • To compare the proposed method with existing pharmacopoeial bromometry for accuracy, precision, and operational efficiency.

Main Methods:

  • Development of an all-solid coulometric titration system employing a glassy carbon electrode (GCE).
  • Application of a universal back titration program for the analysis of phenylephrine hydrochloride (PHE).
  • Comprehensive electrochemical characterization and titration measurements to evaluate the long-term stability of the GCE.

Main Results:

  • Demonstrated an excellent linear correlation between electrolysis time and PHE concentration (0.3–20 mM), with a low limit of detection (0.07 mM).
  • Achieved high standard recovery rates and rapid analysis times (<10 min).
  • The all-solid method showed superior accuracy and precision compared to pharmacopoeial bromometry, with simpler operation.

Conclusions:

  • The developed all-solid coulometric titration offers a maintenance-free, stable, and efficient alternative for long-term drug determination.
  • The GCE exhibits robust electrochemical properties, unaffected by potential difference mutations in bromine and iodine solutions.
  • This innovative technique facilitates easier integration and industrialization for pharmaceutical analysis.