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Mechanism of action of indicator:
During an EDTA titration 2 complexes are formed:
- M-EDTA complex and
- M-indicator complex.
The metal-indicator complex must be less stable than the metal-indicator complex.
M-In + EDTA → M-EDTA + In
Erichrome black T is a metal ion indicator. In the pH range 7-11 the dye itself has a blue colour. In this pH range addition of metallic salts produces a brilliant change in colour from blue to red.
M2+ + HIn2- → MIn– + H+
(Blue) (Red)
This colour change can be obtained with the metal ions. As the EDTA solution is added, the concentration of the metal ion in the solution decreases due to the formation of metal-EDTA complex. At the end point no more free metal ions are present in the solution. At this stage, the free indicator is liberated and hence the colour changes from red to blue.
Preparation of Complex Solutions
Experimental procedure
The following experiment demonstrates how a complex solution i.e. EDTA solution is prepared and standardized with standard calcium solution. The standardized EDTA is then used to analyze an unknown sample.
Standard Calcium Solution
- Accurately weigh 0.5 g of dried, pure CaCO3into a 250 mL beaker.
- Add approximately 25 mL of distilled H2O, then add 1 mL of conc. HCl carefully (operate in hood!), cover with watch glass spaced with glass hooks until dissolved.
- Note: If CaCO3 does not dissolve completely, add another 0.5 mL of conc. HCl (operate in hood!). Next, evaporate volume to about 2 mL maintaining watch glass on beaker to expel carbon dioxide. Rinse watch glass, transfer quantitatively into a 500 mL volumetric flask and make up to 500 ml.
- Calculate the molarity of your standard calcium solution.
EDTA Solution Preparation
Weigh out approximately 2 g of reagent grade disodium EDTA into a 250 mL beaker.
Add 0.05 g magnesium chloride hexahydrate, three pellets of NaOH and add about 200 mL of distilled water to dissolve. The EDTA will dissolve slowly over a period of a half an hour.
Magnesium chloride is added to enhance the sharpness of the endpoint (It forms a more stable complex with the indicator).
Filter the EDTA solution into a 0.5 or 1 L bottle, then add approximately 250 mL of distilled water.
Titration Procedure
- Standardization Titration for EDTA
- Fill your burette with the EDTA solution.
- Pipet three 25 mL aliquots of standard calcium
- solution into 250 mL Erlenmeyer flasks, add 3 mL ammonium chloride buffer (pH 10) (operate in hood!) and 2-3 drops of Eriochrome Black T indicator solution.
- Titrate with EDTA from violet through wine-red to blue. It is recommended to experiment with a 5 mL aliquot to get an idea of the color and titre.
- The indicator color changes slowly, thus, the titrant must be added slowly near the endpoint with thorough stirring. Calculate the molarity of the EDTA.
- Now you have your EDTA solution standardized and your standard EDTA solution should be ~0.01 M. Titration of Unknown Calcium Sample
- Prepare a clean beaker and ask your GA for 100 mL of unknown solution. Titrate with standard EDTA, 25 mL of unknown solution after addition of 3 mL ammonium chloride buffer (pH 10) (operate in hood!) and 2-3 drops of Eriochrome Black T indicator solution following the procedure above.
- Repeat this in triplicate. Express the concentration of calcium carbonate in the unknown sample in ppm
Applications of Complexometric titration:
- Complexometric titration is widely used in the medical industry because of the micro litre size sample involved. The method is efficient in research related to the biological cell.
- Ability to titrate the amount of ions available in a living cell.
- Ability to introduce ions into a cell in case of deficiencies. Complexometric titration involves the treatment of complex ions such as magnesium, calcium, copper, iron, nickel, lead and zinc with EDTA as the complexing agent.
- Complexometric titration is an efficient method for determining the level of hardness of water.