QUALITY CONTROL 1

POST LABORATORY DISCUSSSION

Exercise No. 3 : Preparation and Standardization of 0.1N Sulfuric Acid

Type of Titration: Direct Titration
Type of Assay: Primary Standardization
Principle: Neutralization ( Acid-Base)
Reagents Used:
Prepared Sulfuric acid solution = titrant
Sodium Carbonate = Primary Standard
Indicator = Methyl red T.S.
Endpoint: Permanent Pink color

Formula: V x N = Wt. of the Primary Standard

mEq wt. of Primary Standard
Where:
V= Volume of titrant used
N = Normality
mEq wt = milliequivalent weight ( mw of
Notes:
 Primary Standard – reagent that is extremely pure, stable, has no waters of hydration and has a
high molecular weight, usually solid (g)

Degrees of Purity of Standards

1. Technical Grade – Least pure, least stable
2. USP/NF
3. Chemically Pure
4. Analytical Reagent Grade
5. Primary Standard Grade – Most pure

 Sodium Carbonate : mol wt= 105.99 g/mol

 Secondary Standard – Prepared and titrated against a primary standard , usually in solutions
 Neutralization Reactions – can be Alkalimetry of Acidimetry depensing on the titrant used ( if
acid or base)
Exercise No 4: Content Uniformity Test of Sodium Bicarbonate Tablets
Type of Titration: Direct Acidimetric Titration
Type of Assay: Secondary
Principle: Neutralization
Reagents/ Samples:
Sodium carbonate tablets – Analyte/ Assayed
0.1 N H2SO4 – Titrant
Methyl red T.S . – indicator (phenolphthalein cannot be used because it can be affected by the
carbonic acid liberated in the reaction  can cause color change before the reaction is
complete)
Endpoint – pink color
Reaction:
2NaHCO3 + H2SO4  Na2SO4 + 2 H2O + 2 CO2
Formula:
There are two ways to calculate for the content of NaHCO3 tablet, If you only have one sample
tablet you can use;

1. % NaHCO3 = mL titrant x N titrant x mEq NaHCO3 x 100

Sample weight
If you are getting the NaHCO3 content per tablet from the average weight of the 20 tablets, use
the formula;

1.1 NaHCO3 cont/tab = V x N x mew wt of NaHCO3 x Ave weight

Weight of tablet
Or using the titer value

Titer value = Weight of subsatance chemically equivalent to 1 mL of the standard solution, in

this case weight of NaHCO3 that can be neutralized by 1 mL of 0.1 N H2SO4. Titer values are
expressed in mg/mL

Titer Value = N of titrant x m.w.

F

NaHCO3 cont/tab = V x titer value x Ave weight

Wt of tablet
Percentage labelled amount

% labelled amount = Cont of NaHCO3 tablet x 100

Labeled claimed
USP REQUIREMENT
 Not less than 95% and not more than 105% of the labelled amount of NaHCO3.
 Content uniformity : The content of each of the 20 tablets is within limits of not less than 85 and
not more than 115 %
Exercise No 5: Preparation and Standardization of 1N NaOH Solution

Introduction:
Sodium hydroxide is hygroscopic and absorbs water from the air when you place it on the balance for
massing. This water will prevent you from being able to find the exact mass of sodium hydroxide. In
order to determine the exact concentration of a sodium hydroxide solution you must standardize it by
titrating with a solid acid that is not hygroscopic. Potassium hydrogen phthalate, KHC8H4O4
(abbreviated KHP), is a non-hygroscopic, crystalline, solid that behaves as a monoprotic acid. It is water
soluble and available in high purity. Because of its high purity, you can determine the number of moles
of KHP directly from its mass and it is referred to as a primary standard. You will use this primary
standard to determine the concentration of a sodium hydroxide solution. The structure of KHP is shown
below:

Equation: KHC8H4O4 + NaOH  KNaC8H4O4 + H2O

Type of Titration: Direct Titration
Type of Standardization: Primary Standardization with KHP
Principle: Acid-Base Neutralization
Reagents:
Potassium biphthalate ( dissolved in 75mL CO2 – free water) – Primary Standard (Analyte)
NaOH Solution ( 14.7g NaOH pellets in 100mL CO2-free water) – Titrant
Phenolphthalein – Indicator
Endpoint: Permanent pink color

Titer value:
Each mL of 1N NaOH is equivalent to 204.2mg of potassium biphthalate.

Note:
Solutions of alkali hydroxides absorb carbon dioxide when exposed to air. They should be preserved in
bottles having well-fitted, suitable stoppers. Re-standardize the solution frequently. Solutions can be
treated with Barium hydroxide to precipitate any carbonate formed through the action of CO2 on NaOH

This standardized solution can be used as titrants (or known solutions) in secondary standardization
Formula:
( from Eq No. 3)
N NaOH = Wt of Primary Standard (KHC8H4O4)
V x mEq wt. of KHC8H4O4

Ave of two trials = N (trial 1) + N (trial 2)

Exercise No 6: Preparation and Standardization of 1N H2SO4

Type of Titration: Direct Alkalimetric Titration

Principle: Acid-base Neutralization
Reagents:
Sulfuric acid ( 7.5mL H2SO4, C.P. + q.s. distilled water to make 250 mL)– Analyte
1 N NaOH – Titrant
Phenolphthalein – Indicator
Endpoint: Light pink
Formula:
(from Equation No 2) : V acid x N acid = V base x N base

N of H2SO4 = V of NaOH x N of NaOH

V of H2SO4
Note: Since H2SO4 is a diprotic acid, f= 2
Standard Solutions of Sulfuric acid are preserved in tightly stoppered, alkali-free bottles
Solutions of NaOH and KOH may be standardized by use of a standard solution of HCl or H2SO4
(like that of the experiment)

Exercise No 7: Assay of Milk of Magnesia

Type of Titration: Residual Alkalimetric Titration
Reagents:
Magnesium hydroxide in Milk of Magnesia : Analyte / sample assayed
1 N H2SO4 – excess acid
1 N NaOH – Titrant
Methyl red – indicator
Endpoint: yellow colored solution
Reactions:
(1) Mg(OH)2 +H2SO4  MgSO4 + 2H2O
(2) H2SO4 + 2 NaOH  Na2SO4 + 2H2O

Titer value:
Each mL of H2SO4 is equivalent to 29.16mg of Magnesium hydroxide
Titer = 1 N N2SO4 x ( 58.32)
2
Formula:
( Equation No 4) :

% = [ ( mL excess acid/base x N excesss acid/base) – (mL titrant x N titrant) ] x meq wt x 100

Sample wt.

So;

% Mg(OH)2 = [(V of H2SO4 x N H2SO4) – ( V of NaOH x N NaOH) ] x meq wt x 100

Sample wt

Note: The USP requires that milk of magnesia contain not less than 7 and not more than 8.5% Mg(OH)2
Exercise No. 8: Assay of Tartaric Acid (C4H6O6)
Type: Direct Alkalimetric Titration
Reagents:
Tartaric acid solution ( 1.5g + 40 mL distilled water)– Analyte
1N NaOH – Titrant
Phenolphthalein – Indicator
Endpoint: Permanent pink color
Equation no. 2

% C4H6O6 = V of NaOH x N of NaOH x mEq wt of C4H6O6 x 100

Weight of C4H4O6
Factor : 2
Requirement: Not less than 99.7% and not more than 100.5%
Exercise No. 9: Preparation and Standardization of 0.1N NaOH
See manual…..

Exercise No 10: Assay of Aspirin Capsule