S.

N TITLE OF THE EXPERIMENT REMARKS

1 Preparation of N/10 KMnO4 solution and standardization by using oxalic
acid

2 Assay of hydrogen peroxide by Permangnetometry

3 Estimation of Fe(II) in Mohr’s salt solution using standard kmno4

solution via redox titration

4 Assay of aspirin tablets (acid base titration)

5 Identification and assay of paracetamol tablets

6 Assay of ascorbic acid (vit c tablets)

7 Determination of total chloride ion in ORS by Volhard method

8 Determination of chloride in normal saline by Mohr’s method

9 To study the neutralization titration curve

10 To perform the assay of iodine by Iodimetry

11 Assay of indomethacin by acid-base titration

Gr. Name of the students Gr Name of the students

1 5
2 6
3 7
4 8
 EXPERIMENT NO: 1
PREPARATION OF N/10 KMNO4 SOLUTION AND STANDARDIZATION BY USING
OXALIC ACID

Procedure
1. Transfer 10 ml of oxalic acid solution to the conical flask and add equivalent amount (10
ml) of dilute sulphuric acid (2N).
2. Warm the solution gently until the temperature of the solution reaches 60-80°C then add
the permanganate solution slowly from the burette until the solution acquires a light rose
color. Keep the solution hot during the titration. If a brown ppt is formed during the
titration, this may be due to one of the following reasons:
a. The temperature of the solution may be below 60°C.
b. The addition of permanganate solution was carried out rapidly.
c. The amount of sulphuric acid is insufficient.

3. Repeat the experiment three times and take the mean value of your reading.

EXPERIMENT NO: 2
ASSAY OF HYDROGEN PEROXIDE BY PERMANGNETOMETRY
Procedure
1. Take 5 ml of sample of Hydrogen peroxide (H2O2) in a conical flask and dilute it with
water to 100 ml, and add 25 ml of 1:3 sulfuric acid
2. With gentle swirling of solution, titrate with permanganate solution until fait pink is
attained that lasts for atleast 30 seconds
3. Perform the blank titration
4. Repeat the titration at least thrice and calculate the average and percent relative standard
deviation of your result
 EXPERIMENT NO: 3
ESTIMATION OF FE(II) IN MOHR’S SALT SOLUTION USING STANDARD KMNO4
SOLUTION VIA REDOX TITRATION
Procedure:
1. Primary standard Mohr’s salt solution was provided.
2. Secondary standard KMnO4 and unknown Fe (II) solution was provided.
3. Standardization of KMnO4 solution by standard Mohr’s salt solution: Pipette out 20 mL
of standard Mohr’s salt solution into a 100 mL conical flask, add 20 mL of dilute H2SO4 (1:8
V/V). Titrate with standard KMnO4 solution from the burette with constant stirring till the first
permanent pink color develops in the solution. Repeat thrice.
4. Estimation of Fe (II) in the given solution: Pipette out 20 mL of unknown Fe(II) solution in
a 100 mL conical flask, add 20 mL of dilute H2SO4 (1:8 V/V). Titrate with standard KMnO4
solution of known strength till the first permanent pink color develops throughout the whole mass
of the solution. Take minimum 3 readings.
Observations and Calculations:
Strength of standard Mohr’s salt solution (S1) = 0.01(N)
Table 1:- Standardization of KMnO4 solution
S.N Volume of Burette Reading (ml) Vol. of Mean Value
Mohr’s salt (ml) KMnO4 of KMnO4
Initial Final
(V1) (ml) (ml)

1 20
2 20
3 20
Therefore, strength of KMnO4 (S2) can be calculated as follows:
V1S1= V2S2
S2 = (V1S1/V2) (N)
Table 2:- Unknown Mohr’s salt with KMnO4 solution.
S.N Volume of Burette Reading (ml) Vol. of Mean Value
Mohr’s salt (ml) KMnO4 of KMnO4
Initial Final
(V1) (ml) (ml)

1 20
2 20
3 20
1000 mL of 1(N) KMnO4 solution = 1 equivalent of Fe = 56 g of Fe
V’ mL of S2 (N) KMnO4 solution = 0.056 x V’ x S2 g of Fe
20 mL solution contains (0.056 x V’ x S2) g of Fe
1000 mL solution contains (0.056 x V’ x S2 x 50) g of Fe
Therefore, Fe present in the solution = (0.056 X V’ X S2 X 50) g/L
= A g/L (say)
Result can also be expressed in terms of Mohr’s salt in g/L.
56 g of Fe present in 392 g of Mohr’s salt
A g of Fe present in (392 x A)/56 g of Mohr’s salt
Therefore, amount of Fe (II) in A g/L and amount of Mohr’s salt is (392 x A)/56 g/L

EXPERIMENT NO: 4
ASSAY OF ASPRIN TABLETS (ACID BASE TITRATION)
Introduction:
Aspirin is acetyl salicylic acid, occurs as white crystals, used as analgesic to relieve minor aches
and pain, as antipyretic to reduce fever and as anti- inflammatory medication. Its molecular formula
(C9H8O4).
It is a monoprotic weak acid, Ka = 2.8 x 10 4 at 25oC, so very little of the molecular aspirin
(acetylsalicylic acid) dissociates to form acetylsalicylate ions.
For the equilibrium dissociation reaction:
aspirin (acetylsalicylic acid) acetylsalicylate ion + H+

+ H+

It is slightly soluble in water (1:300) and soluble in alcohol (1:5), chloroform (1:17) and ether
(l: 15), Also it dissolves easily in glycerin. Its melting point (135°C), and Molecular weight =
180.2 g/mole. It slowly decomposed to acetic and salicylic acid in the presence of heat and
moisture.
The salicylates being acidic in nature are readily absorbed from stomach and small intestine.
Their absorption depends strongly on the pH of the environment, thus coadministration of antacid
or other buffering agent should be avoided because it greatly hinders their absorption. Salicylic
acid is the main metabolite of aspirin, it undergoes extensive phase-II metabolism and it excreted
via the kidneys as the water soluble glycine conjugate or acyl glucouronides.
Principle:
Titration method used to determine how much acid is in a solution by adding just enough
base of a known concentration to neutralize the acid. In neutralization,

the number of moles of acid, H+, is combined with an equal number of moles of base, OH_ In the
titration you will be performing, you will dispense base into a known amount of acid solution to
find the unknown concentration. If you wanted to know the concentration of an unknown base,
you could titrate the base with an acid in the same manner. The aspirin will be titrated against a
standard solution of base, 0.1 N NaOH. Base will be dispensed from a burette into a beaker
containing the dissolved acid (in ethanol) and phenolphthalein indicator, which show a faint pink
color in basic solutions.
C9H8O4+NaOH C9H7O4Na+H2O

Identification
Boil a quantity of the powdered tablets containing 0.5 g of Aspirin with 10 ml of sodium hydroxide
solution for 3 minutes, cool and add 10 ml of dilute sulphuric acid; a white, crystalline precipitate
is produced and the odour of acetic acid is perceptible. Filter, dissolve the precipitate in about 2
ml ofwater and add ferric chloride test solution; a deep violet colour is produced.

Assay: Weigh and powder 20 tablets. Weigh accurately a quantity of the powder containing about
0.5 g of Aspirin, add 30.0 ml of 0.5 M sodium hydroxide, boil gently for 10 minutes, cool and
titrate the excess of alkali with 0.5 M hydrochloric acid using Phenolpthalein as indicator. Repeat
the operation without the substance under examination. The difference between the titrations
represents the amount of sodium hydroxide required.
1 ml of 0.5 M sodium hydroxide is equivalent to 0.04504 g of C9H8O4.
 EXPERIMENT NO: 5
IDENTIFICATION AND ASSAY OF PARACETAMOL TABLETS
Introduction:
Paracetamol, (acetaminophen),chemically named N-acetyl-p-aminophenol, is a widely
used analgesic (pain reliever) and antipyretic (fever reduce). Paracetamol is classified as a mild
analgesic. It is commonly used for the relief of headache and other minor aches and pains and is
a major ingredient in numerous cold and flu remedies.
In combination with opioid analgesics, paracetamol can also be used in the management of more
severe pain such as pot-surgical pains and providing palliative care in advanced cancer
patients Though paracetamol is used to treat inflammatory pain, it is not generally classified as
an NSAID because it exhibits only weak anti-inflammatory activity.
Its content 99.0% to 101.0 % (dried substance). Its appearance: white crystal powder, sparingly
soluble in water freely soluble in alcohol,slightly soluble in methylene chloride, and its melting
point (168 °C to 172 °C). Asaturated aqueous solution has a pH of about 6 and is stable (half-life
over 20 years) but stability decreases in acid or alkaline conditions, the paracetamol being slowly
broken down into acetic acid.
H
N

O
HO

Paracetamol
ParacetamolM.wt. 151.2 g/mol

Paracetamol is 4-acetamidophenol and may be represented by the following formula

(C8H9NO2), with molecular weight (151.2), pKa (9.5).

Several papers in the literature describe the assay of Paracetamol and its combination in
pharmaceuticals or biological fluids. Determination of Paracetamol

using electrical method has been reported, Spectrophotometry high performance liquid
chromatography, and titration method.

Principle:
The British Pharmacopoeia method for the analysis of paracetamol involves heating it
under reflux with sulfuric acid. This is a straightforward, acid catalyzed, hydrolysis of an amide
to an amine and a carboxylic acid. The 4-aminophenol which is formed is then titrated with an
oxidizing agent, ammonium cerium (IV) sulfate using ferroin as the indicator. The first reaction
is as follows:

The titration step is much more interesting. 4-Aminophenol can easily be oxidized as
follows:

The role of the ammonium cerium(IV) sulfate is to oxidize the 4-aminophenol to the
iminoquinone. Only after all the 4-aminophenol has been oxidized will the cerium (IV) reagent
oxidize the ferroin indicator from Fe2+ to Fe3+ (ferriin).

During the titration the solution should be red, and the yellow end point is the transition
from red to pale blue. It is easy to work out that, since 1 mole of Ce4+ is equivalent to 0.5 mole of
paracetamol, the conversion factor given in the method is correct.
Identification
Extract a quantity of the powdered tablets containing 0.5 g of Paracetamol with 20 ml of acetone,
filter, evaporate the filtrate to dryness and dry at 105º. The residue complies with the following
tests.
A. Determine by infrared absorption spectrophotometry (2.4.6). Compare the spectrum with that
obtained with paracetamol RS or with the reference spectrum of paracetamol.
B. Boil 0.1 g in 1 ml of hydrochloric acid for 3 minutes, add 10 ml of water and cool; no
precipitate is produced. Add 0.05 ml of 0.0167 M potassium dichromate; a violet colour develops
which does not turn red.

Assay
 Weigh a quantity of powdered tablet equivalent to 0.300gm of paracetamol
 Dissolve it in a mixture of 10ml water and30ml of dil.H2SO4 (10% w/v)
 Boil under reflux condenser for 1 hour, cool and dilute to 100 ml water
 To 20 ml of solution add 40ml of ice, 15ml of dilute HCl(10% w/v) and 0.1 ml of ferroin
 Titrate with 0.1N ceric ammonium sulphate unitl a greenish yellow color is obtained
 Carry out the blank titration
Each ml of 0.1N ceric ammonium sulphate is equivalent to 0.007560gm of paracetamol

EXPERIMENT NO: 6
ASSAY OF ASCORBIC ACID (VIT C tablets)
Introduction
Ascorbic acid (Vitamin C), molecular formula (C6H8O6) is a naturally occurring organic
compound with antioxidant properties. It is a white solid, but impure samples can appear
yellowish. Its melting point ( 190°C) with decomposition. It dissolves well in water to give mildly
acidic solutions and sparingly soluble in ethanol. It is practically insoluble in ether and
chloroform. Ascorbic acid solution rapidly oxidized in air and alkali media. Because it is derived
from glucose, many animals are able to produce it (as a hormone), but humans require it as part
of their nutrition.

Ascorbic acid M.wt (176 g / mole)

Principle:
This method determines the vitamin C concentration in a solution by a redox titration with
potassium iodate in the presence of potassium iodide. Ascorbic acid is a reducing agent and can
be oxidized to form dehydroascorbic acid by iodine via the following reaction

When iodate ions (IO3−) are added to an acidic solution containing iodide ions (I−), an

oxidation-reduction reaction occurs;

- The iodate ions are reduced to form iodine.

IO3− + 6 H+ + 5 e− → ½ I2 + 3 H2O
- While the iodide ions are oxidized to form iodine.

2I− → I2 + 2 e−
Combining these half-equations demonstrates the reaction between iodate and iodide.
2 IO3- + 10 I− + 12 H+ → 6 I2 + 6 H2O
It is the iodine formed by this reaction that oxidizes the ascorbic acid to dehydroascorbic acid
as the iodine is reduced to iodide ions.

Ascorbic acid + I2 → 2 I− + dehydroascorbic acid

Due to this reaction the iodine formed is immediately reduced to iodide as long as there is any
ascorbic acid present. Once all the ascorbic acid has been oxidized, the excess iodine is free to
react with the starch indicator, forming the blue-black starch-iodine complex. This is the endpoint
of the titration.
The method is suitable for use with Vitamin C tablets, fresh or packaged fruit juices and solid
fruits and vegetable.

Procedure:
(A) Solutions Needed:
 Potassium iodate solution: (0.002 mol /L) If possible, dry 1 g of potassium iodate for several
hours or overnight at 100°C. Allow to cool and accurately weigh about 0.43g of potassium
iodate and dissolve in 1 L of distilled water in a volumetric flask.
 Starch indicator solution: (0.5%) Weigh 0.25 g of soluble starch and add it to 50 mL of near
boiling water in a 100 mL conical flask. Stir to dissolve and cool before using.
 Potassium iodide solution: (0.6 mol /L) Dissolve 10 g solid KI in about 50 mL of distilled
water in a 100 mL volumetric flask and dilute to 100 mL with distilled water.
 Dilute hydrochloric acid: (1mol /L).

Sample Preparation:
For vitamin C tablets: Weight then dissolves a single tablet in 200 mL of distilled water (in a
volumetric flask if possible).

(B) Titration:
1. Pipette 20 mL of the sample solution into a 250 mL conical flask and add about 150 mL of
distilled water, 5 mL of (0.6 mol /L) potassium iodide, 5 mL of (1 mol /L) hydrochloric acid
and 1 mL of starch indicator solution.
2. Titrate the sample with the (0.002 mol /L) potassium iodate solution. The endpoint of the
titration is the first permanent trace of a dark blue-black color due to the starch-iodine
complex.
3. Repeat the titration with further aliquots of sample solution until you obtain concordant results
(titers agreeing within 0.1 mL).
Calculations
1. Calculate the average volume of iodate solution used from your concordant titers?
2. Calculate the moles of iodate that reacted forming iodine?
3. Using the equation of the reaction between the iodate ions and iodide ions (below) calculate
the moles of iodine formed?
2 IO3− + 10 I− + 12 H+ → 6 I2 + 6 H2O
4. From the titration equation (below) determine the moles of ascorbic acid reacting.
Ascorbic acid + I2 → 2 I− + dehydroascorbic acid
5. Calculate the concentration in mol /L of ascorbic acid in the solution?
6. Calculate the Wt % of Vit C in the tablets?
 EXPERIMENT NO: 7
DETERMINATION OF TOTAL CHLORIDE ION IN ORS BY VOLHARD METHOD
Introduction
This method uses a back titration with potassium thiocyanate to determine the concentration of
chloride ions in a solution. Before the titration an excess volume of a silver nitrate solution is
added to the solution containing chloride ions, forming a precipitate of silver chloride. The term
‘excess‘ is used as the moles of silver nitrate added are known to exceed the moles of sodium
chloride present in the sample so that all the chloride ions present will react.
Ag+ (aq) + Cl– (aq) → AgCl(s)
The indicator Fe3+ (ferric ion) is then added and the solution is titrated with the potassium
thiocyanate solution. The titrate remains pale yellow as the excess (unreacted) silver ions react
with the thiocyanate ions to form a silver thiocyanate precipitate.
Ag+ (aq) + SCN– (aq) → AgSCN(s)
Once all the silver ions have reacted, the slightest excess of thiocyanate reacts with Fe3+ to form
a dark red complex.
Fe3+ (aq) + SCN– (aq) → [FeSCN]2+ (aq)
The concentration of chloride ions is determined by subtracting the titration findings of the moles
of silver ions that reacted with the thiocyanate from the total moles of silver nitrate added to the
solution. This method is used when the pH of the solution, after the sample has been prepared, is
acidic. If the pH is neutral or basic, Mohr’s method or the gravimetric method should be used.

Solutions Needed
 Concentrated nitric acid : (6 M)
 Silver nitrate solution: (0.1 M). If possible, dry 5 g of AgNO3 for 2 hours at 100°C and
allow to cool. Accurately weigh about 4.25 g of solid AgNO3 and dissolve it in 250 mL
of distilled water in a conical flask. Store the solution in a brown bottle.
 Potassium thiocyanate solution: (0.1 M): Weigh 2.43 g of solid KSCN and dissolve it in
250 mL of distilled water in a volumetric flask.
 Potassium permanganate solution: (5%) Add 1.5 g KMnO4 to 30 mL of distilled water.
 Ferric ammonium sulfate solution: (saturated) Add 8g of NH4Fe(SO4 )2.12H2O to 20 mL
of distilled water and add a few drops of concentrated nitric acid.
Titration
1. Weigh and dissolve all the ORS in 1 liter of distilled water and then Use a volumetric cylinder
to measure 100 mL of the ORS and pour it into a conical flask.
2. Add 1 mL of saturated ferric ammonium sulfate solution as indicator.
3. Titrate the unreacted silver ions with the 0.1 mol L−1 potassium thiocyanate solution. The end
point is the first appearance of a dark red colour due to the ferric thiocyanate complex (figure 1).
4. Repeat the titration with 100 mL samples of the ORS solution until you obtain concordant
results (titres agreeing within 0.1 mL).

EXPERIMENT NO: 8
DETERMINATION OF CHLORIDE IN NORMAL SALINE BY MOHR’S METHOD
Introduction
Titration is a process by which the concentration of an unknown substance in solution is
determined by adding measured amounts of a standard solution that reacts with the unknown.
Then the concentration of the unknown can be calculated using the stoichiometry of the reaction
and the number of moles of standard solution needed to reach the so called end point.

Precipitation titrations are based upon reactions that yield ionic compounds of limited solubility.
The most important precipitating reagent is silver nitrate. Titrimetric methods based upon silver
nitrate are sometimes termed argentometric methods. Potassium chromate can serve as an end
point indicator for the argentometric determination of chloride, bromide and cyanide ions by
reacting with silver ions to form a brick-red silver chromate precipitate in the equivalence point
region. The Mohr method uses chromate ions as an indicator in the titration of chloride ions with
a silver nitrate standard solution. After all the chloride has been precipitated as white silver
chloride, the first excess of titrant results in the formation of a silver chromate precipitate, which
signals the end point. The reactions are:
Ag+ + Cl- AgCl(s)
2Ag+ + CrO4-2 Ag2CrO4 (s)

By knowing the stoichiometry and moles consumed at the end point, the amount of chloride in an
unknown sample can be determined. This report describes experiments aimed at determining the
concentration of chloride in a solid sample.
Methods:
 Preparation of 5% K2CrO4(indicator): 1.0 g of K2CrO4 was dissolved in 20 mL of
distilled water.
 Preparation of standard AgNO3 solution: 9.0 g of AgNO was weighed out, transferred to
a 500 mL volumetric flask and made up to volume with distilled water. The resulting
solution was approximately 0.1 M. This solution was standardized against NaCl. Reagent-
grade NaCl was dried overnight and cooled to room temperature. 0.2500 g portions of
NaCl were weighed into Erlenmeyer flasks and dissolved in about 100 mL of distilled
water. In order to adjust the pH of the solutions, small quantities of NaHCO3 were added
until effervescence ceased. About 2 mL of K2CrO4 was added and the solution was
titrated to the first permanent appearance of red Ag2Cr2O4 .
Determination of Cl- in solid sample:
 Take about 100 mL of sample in a beaker and add small quantities of NaHCO3. Wait until
effervescence ceased.
 Now from above solution, pipette out 25 ml of the sample in a conical flask
 Add 2 mL of K2CrO4 and titrate the solution until the first permanent appearance of red
Ag2Cr2O4.
 Perform the blank titration

EXPERIMENT NO: 9
TO STUDY THE NEUTRALIZATION TITRATION CURVE (A) HCl VS NaOH
(B)CH3COOH VS NaOH (CONSULT WITH YOUR TEACHER)

EXPERIMENT NO: 10
TO PERFORM THE ASSAY OF IODINE BY IODIMETRY
Procedure
  Pipette out 10 ml of sample in a conical flask
 Add 1 gm of potassium iodide
 Dilute it with distilled water to about 50ml
 Add 1 ml of 3N HCl
 Titrate it with 0.1N sodium thiosulphate, adding 3 ml of starch paste as the endpoint is
approached
Each ml of 0.1N sodium thiosulphate is equivalent to 0.01269gm of I

EXPERIMENT: 11

ASSAY OF INDOMETHACIN BY ACID-BASE TITRATION:

Introduction:

Indomethacin is a white or yellow, crystalline powder, practically insoluble in

water sparingly soluble in alcohol. Its chemical formula is (C19H16ClNO4) , its
melting point is(158°C to 162°C) and its pka (4.5) Its action and uses are cyclo-
oxygenase inhibitor (COX), (the enzyme responsible for catalyzes the rate-limiting step in
prostaglandin synthesis via the arachidonic acid pathway); analgesic; and anti-

inflammatory. Its preparations are capsules and suppositories.

Indomethacin contains not less than 90% and not more than 110.0%of {1-(4-
chlorobenzoyl)-5-methoxy-2-methylindol-3-yl} acetic acid, calculated with
reference to the dried substance.
 Indomethacin M. wt. (357.8g /mol)

Principle:

Indomethacin contains an acidic group (COOH) so it considered as acid hence it

can be determined by titration against 0.01N NaOH using phenolphthalein (ph.ph)
indicator. At the end point the color changes to pink.

Procedure:

1. Dissolve the content of one capsule in a beaker by addition of 10 ml of neutral

acetone.

2. Shake then filter into a conical flask and wash twice with 10 ml of neutral acetone.

3. Titrate the filtrate with N/100 NaOH using phenolpthalein as an indicator.

4. Carry out a blank titration.

Calculations:

( 𝑽𝑩 𝑿𝑵𝑩 𝑿 𝑬𝒒.𝑾𝒕)
Recovery % = practical content/ theoretical = X 100
𝟐𝟓