Quality Control: Lecture

04-March-2023
Prepared by: Emmanuel A. Caballero, RPh
 Topics
15 min Titrant
15 min Indicator
30 min pH
TBC Preparation and standardization of 1N HCl and 1N H2SO4
 Principles of Titrimetric/Volumetric Analysis

● Relationship of the stoichiometric point and the endpoint?

Standardization - determination of the normality/molarity of a solution

● Sources of error:
○ Rinse water adhering to walls of apparatus
○ Grease films and dirty apparatus
○ Parallax
○ Temperature
○ Air bubbles
○ Failure to use the apparatus
 Principles of Titrimetric/Volumetric Analysis

● Types of Chemical reactions:

○ Neutralization
○ Oxidation-reduction
○ Precipitation
○ Complexation

● Requirements for titrimetric analysis:

○ Reaction must proceed in a stoichiometric manner
○ A suitable endpoint-detecting device (chemical indicators, electrodes, etc) must be available
○ Reaction must be rapid so a sharp endpoint is discernible
 Principles of Titrimetric/Volumetric Analysis

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 Principles of Titrimetric/Volumetric Analysis

Acidimetry - Titrimetric analysis of bases using an accurately measured volume of acid

Direct Titration - conducted by introducing a standard acid solution gradually from a buret into a solution of
the base being assayed until chemically equivalent amounts of each have reacted

E.G. NaHCO3, NaOH, Na salicylate, Na benzoate

Residual Titration or Back Titration - used when a reaction proceeds slowly or when the substance to be
assayed does not give a distinct , sharp endpoint with an indicator by direct titration. Carried out by
dissolving the substance in an accurately measured quantity of standard solution (in excess) and titrating the
excess with another standard solution

E.G. ZnO (slow dissolution ) – add NH4Cl, heat, C4H4KNaO6, and other alkali salts of citric

tartaric, etc, MgO, Mg(OH)2, Methenamine

 Principles of Titrimetric/Volumetric Analysis

Alkalimetry - Titrimetric analysis of acids using an accurately measured volume of bases. Most inorganic
acids, MR or PH can be used, though the alkali should be standardized with a particular indicator used. For
organic acids, PH is freq used; though thymol blue, bromothymol blue, thymolphthalein are also used

Direct Titration - examples are HCl, Dil H3PO4, H3BO3

Residual Titration or Back Titration - used when a reaction proceeds slowly or when the substance to be
assayed does not give a distinct , sharp endpoint with an indicator by direct titration. Carried out by
dissolving the substance in an accurately measured quantity of standard solution (in excess) and titrating the
excess with another standard solution

E.G. Esters, acid anhydrides, acid chlorides, aldehydes, Aspirin, Formaldehyde

 Principles of Titrimetric/Volumetric Analysis

● Indicators - complex organic compounds used:

○ To determine the endpoint in neutralization process
○ To indicate that a desired change in pH has taken place
● The pH of the solution at the equivalence point determines which indicator is to be used for the
analytical determination (for neutralization reactions)
● Bronsted-Lowry acid-base model
○ Conjugate acid
■ Particle formed when a base gains H+
○ Conjugate base
■ Particle formed when an acid has donated a H+
 Principles of Titrimetric/Volumetric Analysis

Kw - Dissociation constant of water. At 22 C, is equal to 1 x 10^-14. Also equal to the concentration of acid times the concentration of the base.
Acid and base in water is neutralized

Concentrations of [H3O+] and [OH-]

• [H3O+] greater than 10-7 are ACIDS

• [H3O+] less than 10-7 are BASES

pH/pOH

• Power of the exponent

• Introduced by Sӧren Sӧrensen in 1909

• Negative logarithm of the hydrogen/hydroxide ion conc

• pH = - log [H+] ; pOH = -log [OH-]

 Principles of Titrimetric/Volumetric Analysis

Preparation and Standardization of 1N Sulfuric acid

Normal sulfuric acid solution may be standardized titrimetrically against pure sodium carbonate or standardized solution of
sodium hydroxide which has been recently standardized, or gravimetrically by precipitation of an equivalent amount of silver
chloride

Materials required: 30ml of Sulfuric acid, 1N sodium hydroxide solution

How many ml of 1N NaOH is required in titration of a solution Sulfuric acid?

Chemical formula 1: Na2CO3 + H2SO4 =(heat)=> Na2SO4 + H2O + CO2

Chemical formula 2: 2NaOH + H2SO4 => Na2SO4 + 2H2O