PHA 039: PHARMACEUTICAL ANALYSIS I

Laboratory Activity Sheet 5

Exercise No. 5
Preparation and Standardization of 1N Sodium Hydroxide Solution

OBJECTIVES: At the end of the exercise you should be able to:

1. To prepare and standardized 1N sodium hydroxide for use in the Assay of Milk of Magnesia
2. To know the importance of standardizing solution of known concentration

DISCUSSION

Solutions of sodium hydroxide in any concentration maybe standardized using standard solutions of
hydrochloric acid, or sulfuric acid as a secondary standard or potassium biphthalate as a primary standard. Thus, the
solution is conducted in a direct acidimetric neutralization analysis.

Carbon dioxide free water was used in order to avoid chemical reaction that leads to formation of
carbonates and to accurately compute for the normality of a substance. The solution can be treated also with barium
hydroxide to precipitate any carbonate formed through the action of carbon dioxide on the sodium hydroxide.

The solution is preserved in a tightly stoppered bottle fitted with a soda-lime tube to protect it from the
carbon dioxide of the air. Solutions which contain carbonates are not suitable for titration if phenolphthalein indicator
is used but methyl orange can be used in the titration which will provide the same results as long as all the sodium
present were combined as hydroxides.

The solution is under the direct acidimetric neutralization analysis used in Exercise (Preparation and
Standardization of 1 N Sulfuric Acid) and Exercise (Assay of Milk of Magnesia). The solution can also be used in the
Assay of Tartaric acid, Preparation and Standardization of 0.1N Iodine Solution and Assay of Caffeine Alkaloid from
Instant Coffee Powder.

MATERIALS:
1. Iron stand
7. Stirring rod
2. Pipet, 1mL
8. Base burette
3. Glass funnel
9. Burette clamp
4. Volumetric flask, 250 mL
10. Aspirator pump
5. Erlenmeyer flask, 250mL
11. Reagent bottle, 500 mL
6. Graduated cylinder

PROCEDURE:

I. Preparation

Dissolve 11.25g of sodium hydroxide pellets in 100ml distilled water. Cool the solution to room
temperature and filter. Transfer it in a 250ml volumetric flask then add sufficient quantity of distilled water to make
250ml.

II. Standardization

Weigh accurately about 5g of potassium biphthalate, previously crushed lightly and dried at 120C for 2
hours and dissolve it in 75ml distilled water. Add 2 drops of phenolphthalein TS and titrate with the sodium
hydroxide solution until it produces a permanent pink color. (Perform 2 trials)

Note: solutions of alkali hydroxides absorb carbon dioxide when exposed to air. They should be preserved
in bottles having well-fitted, suitable stoppers. Standardize the solution frequently.
 PHA 039: PHARMACEUTICAL ANALYSIS I
Laboratory Activity Sheet 5

Group #: _______________ Date: ____________________________

Name: ___________________________________________________________________________ Score: ___________________________

Exercise No. 5 Worksheet

Preparation and Standardization of 1N Sodium Hydroxide Solution

Average
Data Trial 1 Trial 2 concentration
Weight of potassium biphthalate (g) 1.6310
1.5433g
Volume of NaOH (mL) 27mL =1.0336N
31.4mL
Normality of NaOH
0.9274N 1.1398N

Calculate the normality using the general formula as follows:

wt. of KHC8H4 O4
where in:
N= _________________________ V = volume
N = normality
V x mEq wt. of KHC8H4 O4 wt = weight
mEq wt = milliequivalent weight

Calculation of Normality:

TRIAL 1 TRIAL 2

N TRIAL 1 + N TRIAL 2
Average of two trials = ________________________
2
 PHA 039: PHARMACEUTICAL ANALYSIS I
Laboratory Activity Sheet 5

Conclusion:

Questions to answer:

1. Define Normality and Milliequivalent.

Normality is described as the number of gram or mole equivalents of solute present in

one litre of a solution. A milliequivalent is one-thousandth of an equivalent. A liter
measures fluid volume. It is a little bigger than a quart.

2. How will an alkali solution like sodium hydroxide be standardized?

To standardize NaOH, start by pipetting 10.0 ml of 0.1 N hydrochloric acid (HC1) into a
flask. Add approximately 50 ml of water and two drops of methyl red indicator. Fill a 25
ml buret with the 0.1 N sodium hydroxide solution and record the initial volume.

3. Differentiate primary standard from secondary standard.

The difference between primary and secondary standard solutions is that primary
standard solutions have a high purity and less reactivity whereas secondary solutions
have a less purity and high reactivity.

4. Indicate the chemical reaction involved in the standardization.

A double displacement reaction occurs when sodium carbonate is introduced into

hydrochloric acid, when 2 drops of methyl red is added into the titration flask the color
changes to light pink.

5. If 25 ml of a sodium hydroxide solution required 40ml of a sulfuric acid solution in a titration and 25 ml of the
sulfuric acid solution was required in the titration of 0.3060g of pure sodium carbonate, what was the normality of
the sodium hydroxide solution?