Preparation and standardization of 1 M NaOH

Preparation of NaOH solution-

Dissolve 42 g of NaOH in sufficient carbon dioxide free water to
produce 1000 ml
Standardization of NaOH solution-
Standardize NaOH solution by using potassium hydrogen
phthalate.
Weigh accurately about 05 g of KHP previously powdered & dried
at 120 ° C for 2 hrs and dissolve in 75 ml carbon dioxide free
water. Add 0.1 ml of phenolphthalein solution and titrate with
NaOH solution until a permanent pink color is produced.

Each ml of 01 M NaOH is equivalent to 0.2042 g of C8H5KO4

NaOH solution can also be standardise using primary standard
such as oxalic acid, benzoic acid, adipic acid
 Preparation and standardization of 1 M HCl
Preparation of HCl solution-
Dilute 85 ml of HCl with water to produce 1000 ml
Standardization of HCl solution-
It is Standardized by using anhydrous sodium carbonate as weighed
accurately.
Weigh accurately about 1.5 g of anhydrous sodium carbonate previously
heated at 170 ° C for 1 hr.
Dissolve it in 100 ml water. Add 0.1 ml of methyl red solution.
Add acid slowly with constant stirring until the solution becomes faint
pink. Heat the solution to boiling, cool and continue the titration. Heat
again to boiling and titrate further as necessary until the faint pink color
is no longer affected by boiling.

Each ml of 01 M HCl is equivalent to 0.05299 g of Na2CO3

NaOH solution can also be standardise using primary standard such as
thallous carbonate, borax, potassium hydrogen phthalate
The neutralization reactions that take place in two steps
are as follows:
Na2CO3(aq) + 2HCl(aq) → 2NaCl(aq) + CO2(g) + H2O(l)
 Volume of Burette reading of Volume of Mean
Na2CO3 HCl Burette
Sr no HCl (ml)
consumed reading
taken (ml) IR FR
(ml) (ml)
1

3
 Preparation and standardization of H2SO4

• Principle:
Sulphuric acid is a diprotic acid and 1 N solution contain 98.08/2 = 49.04 g
H2SO4. Taking into consideration specific gravity (1.83) of sulphuric acid
about 49.0 ml of conc. Sulphuric acid is required to prepare 1000 ml
solution. It is an example of alkalimetry.
When a strong acid is titrated with a strong base, the salt produced in the
reaction is not hydrolysed and therefore the ph of the resultant solution at
the end point is exactly 7.0. sulphuric acid is a strong acid, is standardized
by titrating with a strong base i.e. sodium carbonate (primary standard).
The following reaction takes place when sodium carbonate is titrated with
sulphuric acid. In this titration, end point detection is carried out by using
methyl orange indicator.
Preparation of 0.5 M Sulphuric acid:
Add slowly, with stirring 30 ml sulphuric acid to about 800 ml of
purified water. Makeup to 1000 ml with purified water. Allow
cooling at 25 °C.
Standardization of 0.5 M Sulphuric acid:
• Weigh accurately about 0.8 gm of anhydrous sodium carbonate,
previously heated at about 270 °C about 1 hr.
• Dissolve it in 100 ml of water and add 0.1 ml of methyl red
solution.
• Add the acid slowly from a burette, with constant stirring, until
the solution becomes faintly pink.
• Heat the solution to boiling, cool and continue the titration.
• Heat again to boiling & titrate further as necessary until the faint
color no longer affected by continued boiling.
• Repeat the experiment three times and tabulate your results then
take the mean of the three readings.
• Calculate the molarity of solution.
• Factor: 1ml of 0.5 M H2SO4 is equivalent to 0.05299 g of Na2CO3.
 Estimation of ammonium chloride
THEORY
• % purity is the percentage of the material which is the actually
desired chemical in a sample of it. In pharmaceutical industry, it
would not be acceptable to manufacture a drug with impurities in
it that may be harmful to health. However in any chemical
process it is almost impossible to get 100.00 % purity and so
sample should be analyzed in industry for % purity to monitor the
quality of the product.
• Ammonium chloride is also known as the salt of ammonia. It is
represented by a chemical formula NH4Cl.
• Ammonium chloride when dissolve in water form acidic solution.
Reaction between ammonium chloride and sodium hydroxide
produces some new compounds like ammonia, water and sodium
chloride.
• Ammonia gas liberated may combine with hydrochloric acid to
form ammonium chloride and hence direct titration of
ammonium chloride with sodium hydroxide produce erroneous
results.
• So for the titration of ammonia chloride with base, the
addition of formaldehyde would improve the titration.
• The ammonium chloride reacts with formaldehyde to form
hexamethylene tetramine. Because the weak acid ammonium
(pKa 9.3) is converted to the stronger hexamethylene
tetramine ion (pKa 4.9). This improves the end point.
 PROCEDURE
Step 1- Preparation and standardization of 0.1 N NaOH
Step 2- Assay of ammonium chloride
➢Weigh accurately about 0.1 g of ammonium Chloride, add 20
ml of water.
➢Add a mixture of 5.0 ml of formaldehyde solution (previously
neutralize to dilute phenolphthalein) and 20 ml of water.
➢After two minutes, add 2-3 drops of phenolphthalein indicator
and titrate solution slowly against 0.1 N NaOH till faint pink
colour appear.
➢Each ml of 0.1N NaOH is equivalent to 0.005349 gm of NH4Cl.
➢Note down the burette reading. Repeat the titration with
other two flasks and take the average readings of sample
taken
Note: and volume
Neutralization of NaOH used.
of formaldehyde: Formaldehyde is neutralized by taking in a
conical flask 20 ml formaldehyde solution and two drops of phenolphthalein then
titrate against 0.1 N NaOH till faint pink colour appear.
Acid Base Titration Curves
 What is a titration curve?

A titration curve is the plot of the pH of the analyte solution

versus the volume of the titrant added as the titration
progresses.
• In an acid–base titration, the titration curve represents
the strength of the corresponding acid and base.
• For a strong acid and a strong base, the curve will be
relatively smooth and very steep near the equivalence
point.
• Because of this, a small change in titrant volume near
the equivalence point results in a large pH change and
many indicators would be appropriate.
 A) Titration of Strong acid with a strong base
Running alkali into the acid
Point 1:
No NaOH added yet, so the pH of the analyte is low (it
predominantly contains H3O+ from dissociation of HCl)

As NaOH is added dropwise, H3O+ slowly starts getting consumed by

OH- produced by dissociation of NaOH. Analyte is still acidic due to
predominance of H3O+ ions.
Point 2:
This is the pH recorded at a time point just before complete
neutralization takes place.
Point 3: This is the equivalence point (halfway up the steep curve).
At this point, moles of NaOH added = moles of HCl in the analyte. At
this point, H3O+ ions are completely neutralized by OH-
The solution only has salt (NaCl) and water and therefore the pH is
neutral i.e. pH = 7.
Point 4:
Addition of NaOH continues, pH starts becoming basic because
HCl has been completely neutralized and now excess of OH- ions
are present in the solution (from dissociation of NaOH).
 B) Titration of weak acid with a strong base
• If we start plotting the pH of the analyte against the volume
of NaOH that we are adding from the burette, we will get a
titration curve as shown below.
Point 1:
No NaOH added yet, so the pH of the analyte is low (it
predominantly contains H3O+ from dissociation of CH3COOH) But
acetic acid is a weak acid, so the starting pH is higher than what we
noticed in case 1 where we had a strong acid (HCl).

As NaOH is added dropwise, H3O+ slowly starts getting consumed

by OH-(produced by dissociation of NaOH). But analyte is still acidic
due to predominance of H3O+ ions.
Point 2: This is the pH recorded at a time point just before
complete neutralization takes place.
Point 3: This is the equivalence point (halfway up the steep curve).
At this point, moles of NaOH added = moles of CH3COOH in the
analyte.The H3O+ ions are completely neutralized by OH- ions. The
solution contains only CH3COONa salt and H2O
 In the case of a weak acid versus a strong base, the pH is not
neutral at the equivalence point. Why????

Point 4: Beyond the equivalence point (when sodium hydroxide is

in excess) the curve is identical to HCl-NaOH titration curve (1) as
shown below.
 C) Titration of strong acid with a weak base
➢Suppose our analyte is hydrochloric acid HCl (strong acid) and the
titrant is ammonia NH3 (weak base).
➢If we start plotting the pH of the analyte against the volume of
NH3, that we are adding from the burette, we will get a titration
curve as shown below.
Point 1:
No NH3 added yet, so the pH of the analyte is low (it
predominantly contains H3O+ from dissociation of HCl).

As NH3 is added dropwise H3O+ slowly start getting

consumed by NH3. the analyte is still acidic due to
predominance of H3O+ ions.

Point 2: This is the pH recorded at a time point just

before complete neutralization takes place.
Point 3: This is the equivalence point (halfway up the
steep curve).
At this point, moles of NH3 added = moles of HCl in the
analyte. The H3O+ions are completely neutralized by NH3
But again do you spot a difference here???
In the case of a weak base versus a strong acid, the pH is
not neutral at the equivalence point. The solution is in
fact acidic (pH ~ 5.5) at the equivalence point.
Running alkali into the acid
Running acid into the alkali
To summarize
• In an acid-base titration, a known volume of either the acid or the
base (of unknown concentration) is placed in a conical flask.
• The second reagent (of known concentration) is placed in a burette.
• The reagent from the burette is slowly added to the reagent in the
conical flask.
• A titration curve is a plot showing the change in pH of the solution in
the conical flask as the reagent is added from the burette.
• A titration curve can be used to determine:
1) The equivalence point of an acid-base reaction (the point at which
the amounts of acid and of base are just sufficient to cause complete
neutralization).
2) The pH of the solution at equivalence point is dependent on the
strength of the acid and strength of the base used in the titration.
- For strong acid-strong base titration, pH = 7 at equivalence point
- For weak acid-strong base titration, pH > 7 at equivalence point
- For strong acid-weak base titration, pH < 7 at equivalence point