Determination of sodium acetate with perchloric acid titration | Autotitrator - JM Science
HIRANUMA APPLICATION DATA Automatic Titrator Data No. B2 Sep. 12,2018
Drugs and Medicines Determination of sodium acetate with perchloric acid titration

1. Abstract

Sodium acetate is widely used in chemical and medical industry (E.g. Buffer, Antifreezing agent, Alkalizing supplements, Dye chemical, Hydragogue). Determination method of sodium acetate is described on Japanese Pharmacopoeia and Japanese Industrial Standard (JIS K8371). Both methods employ perchloric acid titration method, dissolve the sample in glacial acetic acid and titrate with perchloric acid – acetic acid standard solution. Endpoint is detected by potentiometric titration with glass / reference electrodes.

CH₃COONa + HClO₄ → CH₃COOH + NaClO₄

 

2. Configuration of instruments and Reagents

(1) Instruments    
  Main unit : Hiranuma Automatic Titrator COM Series
  Electrode : Glass electrode GE-101B
Reference electrode RE-201Z
(Inner solution should be changed; it is described below)
(2) Reagents    
  Titrant : 0.1 mol/L perchloric acid in glacial acetic acid standard solution
  Titration solvent : Glacial acetic acid
  Electrolyte : Saturated sodium perchlorate in glacial acetic acid
(For inner solution of reference electrode)

3. Measurement procedure

(1) Take 0.2 g of the sample into a 100 mL tall-beaker and accurately weigh it.
(2) Add 50 mL of acetic acid and dissolve the sample.
(3) Immerse the electrodes and start titration with 0.1 mol/L perchloric acid in glacial acetic acid standard solution. Perform blank test without sample.

4. Measurement conditions and results

Examples of titration conditions

Measurement of blank

Measurement of blank

Measurement of sample

Measurement of sample

Measurement results
Blank Measurement
Measurement
No.
Size
(g)
Titrant
volume (mL)
1 0.01
2 0.01
Statistical
result
Avg. (mL) 0.01
Sample Measurement
Measurement
No.
Size
(g)
Titrant
volume (mL)
Conc
(%)
1 0.2029 24.690 99.778
2 0.2021 24.553 99.617
3 0.2010 24.440 99.701
Statistical
result
  Avg. (%)
 SD (%)
RSD (%)
99.70
0.0805
0.08
Examples of measurement curves

 

  • Blank measurement

  • Sample measurement

 

5. Note

(1) Effect of water on perchloric acid titration
Water mixed in sample solution affects to the reaction system of perchloric acid titration because of the leveling effect, which results in a negative effect such as lowered quantitative performance or getting less sensitivity around the end point. Therefore please take care not to mix water in sample solution. Reference electrode for non-aqueous titration should be prepared as described in the following item (2), because water of KCl solution commonly used as inner solution for reference electrode could be mixed in sample solution.
(2) Preparation of inner solution for reference electrode
The inner solution of the reference electrode RE-201Z is filled with saturated KCl aqueous solution normally. For this measurement, it is necessary to replace inner solution to saturated sodium perchlorate in acetic acid solution. Replacement procedure is described below.
i) Prepare the saturated solution of sodium perchlorate in glacial acetic acid with reagent grade of these.
ii) Discharge inner solution from reference electrode RE-201Z and wash inside it with water and then acetic acid.
iii) Fill the prepared inner solution into reference electrode from the supply port.
iv) Cure the electrode for one day before use.
(3) Experiment temperature
Acetic acid used as a solvent for the titrant has a relatively large thermal expansion coefficient, and when the temperature changes by 1 °C, the titrant causes a volume change of 0.1 %. For accurate measurement, factor titration and sample measurement should be performed at the same room temperature as much as possible.

 

Keywords: Sodium acetate, Perchloric acid titration, Nonaqueous titration, Neutralization titration

*Some measurement would not be possible depending on optional configuration of system.

Drugs and medicines

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