Lab manual – Pharmaceutical Chemistry-I

EXPERIMENT NO- 1

Object- To Perform the identification of various equipment used in pharmaceutical chemistry.

Reference- Indian Pharmacopoeia 2010.
Glasswares & Apparatus – Beakers, Flasks, Bottles, Jars, Test tubes, Desiccators, Petri dishes,
Volumetric flasks, Graduated cylinders, Burettes, pipettes etc.
 Beakers are simple cylindrical shaped containers usepipettesd to hold reagents or samples.
 Flasks are narrow-necked glass containers, typically conical or spherical, used in a laboratory to hold
reagents or samples. Examples flasks include the Erlenmeyer flask, Florence flask, and Schlenk flask.
 Bottles are containers with narrow openings generally used to store reagents or samples. Small bottles
are called vials.
 Jars are cylindrical containers with wide openings that may be sealed. Bell jars are used to contain
vacuums.
 Test tubes are used by chemists to hold, mix, or heat small quantities of solid or liquid chemicals,
especially for qualitative experiments and assays
 Desiccators of glass construction are used to dry materials or keep material dry.
 Glass evaporating dishes, such as watch glasses, are primarily used as an evaporating surface (though
they may be used to cover a beaker.)
 Glass Petri dishes are used to culture living cells.
 Microscope slides are thin strips used to hold items under a microscope.
Examples of glassware used for measurements include:
 Graduated cylinders are cylindrical containers used for volumetric measurements.
 Volumetric flasks are for measuring a specific volume of fluid.
 Burettes are used to disperse precise amounts of liquid reagents.
 Glass pipettes are used to transfer precise quantities of fluids.
 Glass Ebulliometers are used to accurately measure the boiling point of liquids.
Other examples of glassware includes:
 Stirring rods are used to mix chemicals.
 Condensers are used to cool hot liquids or vapors.
 Glass retorts are used for distillation.
 Drying pistols are used to free samples from traces of water, or other impurities.

Result- the identification of various equipment used in pharmaceutical chemistry were identify.

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 EXPERIMENT NO- 2

Object- To Perform the visual identification of few chemicals used in pharmaceutical chemistry.
Reference- Indian Pharmacopoeia 2010.
Chemicals – Ammonium sulfate, Barium chloride, Zinc oxide, Sodium chloride, Sodium chloride,
Sodium chloride, Magnesium carbonate, Ethanol, Methanol, boric acid etc.
Ammonium sulfate
Ammonium sulfate; (NH₄)₂SO₄, is an inorganic salt with a number of commercial uses. The most
common use is as a soil fertilizer. It contains 21% nitrogen and 24% sulfur.
Formula: (NH4)2SO4
Molar mass: 132.14 g/mol
IUPAC ID: Diazanium sulfate
Soluble in: Water
Other cations: Sodium sulfate; Potassium sulfate
LD50 (median dose): 2840 mg/kg, rat (oral)
Barium chloride
Barium chloride is the inorganic compound with the formula BaCl₂. It is one of the most common water-
soluble salts of barium. Like most other barium salts, it is white, toxic, and imparts a yellow-green
coloration to a flame. It is also hygroscopic, converting first to the dihydrate BaCl₂(H₂O)₂.
Formula: BaCl2
Molar mass: 208.23 g/mol
Melting point: 962 °C
Boiling point: 1,560 °C
Density: 3.86 g/cm³
ChemSpider ID: 23540

Zinc oxide
Zinc oxide is an inorganic compound with the formula ZnO. ZnO is a white powder that is insoluble in
water, and it is widely used as an additive in numerous materials and products including rubbers, ..
Formula: ZnO
Molar mass: 81.38 g/mol
Melting point: 1,975 °C
Density: 5.61 g/cm³
Boiling point: 2,360 °C
Sodium chloride
Sodium chloride, commonly known as salt, is an ionic compound with the chemical formula NaCl,
representing a 1:1 ratio of sodium and chloride ions. With molar masses of 22.99 and 35.45 g/mol
respectively, 100 g of NaCl contains 39.34 g Na and 60.66 g Cl.
Formula: NaCl
Molar mass: 58.44 g/mol
IUPAC ID: Sodium chloride
Melting point: 801 °C
Soluble in: Water, Ammonia, Methanol, Glycerol, Formic acid, Propylene glycol, Formamide

Magnesium carbonate
Magnesium carbonate is a magnesium salt with formula CMgO3. Its hydrated forms, particularly the
di-, tri-, and tetrahydrates occur as minerals. It has a role as an antacid and a fertilizer. It is
a magnesium salt, a carbonate salt and a one-carbon compound
Formula: MgCO3
Molar mass: 84.3139 g/mol

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Melting point: 540 °C
Density: 2.96 g/cm³
Sodium sulfide
Sodium sulfide is the chemical compound with the formula Na₂S, or more commonly its hydrate
Na₂S·9H₂O. Both are colorless water-soluble salts that give strongly alkaline solutions. When exposed to
moist air, Na₂S and its hydrates emit hydrogen sulfide, which smells like rotten eggs. Wikipedia
Formula: Na2S
Molar mass: 78.0452 g/mol
Melting point: 1,176 °C
Density: 1.86 g/cm³
ChemSpider ID: 207721
Appearance: colorless, hygroscopic solid
Starch
Starch, a white, granular, organic chemical that is produced by all green plants. Starch is a soft, white,
tasteless powder that is insoluble in cold water, alcohol, or other solvents. The basic chemical formula of
the starch molecule is (C6H10O5)n. Starch is a polysaccharide comprising glucose monomers joined
in α 1,4 linkages. The simplest form of starch is the linear polymer amylose; amylopectin is the branched
form. Starch or amylum is a polymeric carbohydrate consisting of numerous glucose units joined by
glycosidic bonds. This polysaccharide is produced by most green plants as energy storage.
IUPAC ID: (2R,3S,4S,5R,6R)-2-(hydroxymethyl)-6-[(2R,3S,4R,5R,6S)-4,5,6-trihydroxy-2-
(hydroxymethyl)oxan-3-yl]oxy-oxane-3,4,5-triol
Density: 1.5 g/cm³
Classification: Carbohydrate, Polysaccharide

Sodium hydroxide
Sodium hydroxide, also known as lye and caustic soda, is an inorganic compound with the formula
NaOH. It is a white solid ionic compound consisting of sodium cations Na⁺ and hydroxide anions OH⁻ .
Formula: NaOH
Molar mass: 39.997 g/mol
Density: 2.13 g/cm³
Boiling point: 1,388 °C
IUPAC ID: Sodium oxidanide, Sodium hydroxide
Soluble in: Water, Ethanol, Methanol

Potassium iodide
Potassium iodide is a chemical compound, medication, and dietary supplement. As a medication it is used
to treat hyperthyroidism, in radiation emergencies, and to protect the thyroid gland when certain types of
radiopharmaceuticals are used.
Formula: KI
Molar mass: 166.0028 g/mol
IUPAC ID: Potassium iodide
Melting point: 681 °C
Density: 3.12 g/cm³
Soluble in: Water
Boric acid
Boric acid, also called hydrogen borate, boracic acid, and orthoboric acid is a weak, monobasic Lewis
acid of boron. However, some of its behaviour towards some chemical reactions suggest it to be tribasic
acid in Bronsted sense as well. Wikipedia
Formula: H3BO3
Molar mass: 61.83 g/mol
Melting point: 170.9 °C

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 PH: 5.1
IUPAC ID: Trihydrooxidoboron, Boric acid
Soluble in: Water, Alcohol
Ethanol
Ethanol is a chemical compound, a simple alcohol with the chemical formula C ₂H ₆O. Its formula can be
also written as CH ₃−CH ₂−OH or C ₂H ₅OH, and is often abbreviated as EtOH. Ethanol is a volatile,
flammable, colorless liquid with a slight characteristic odor. Wikipedia
Formula: C2H5OH
Boiling point: 78.37 °C
Molar mass: 46.07 g/mol
Density: 789 kg/m³
IUPAC ID: ethanol
Melting point: -114.1 °C

Result- The visual identification of few chemicals used in pharmaceutical chemistry were identify.

EXPERIMENT NO- 3

Object – To perform the limit test for Chlorides.

Reference – Chatwal G.R., Pharmaceutical Chemistry-Inorganic, Volume I, Himalaya Publishing House,
Mumbai, II Edition, 1996, 45-46
Materials required –
Chemicals – Nitric acid, Silver nitrate solution, Sodium Chloride, Distill water
Glasswares & Apparatus – Nessler cylinder, Measuring cylinder, Pipette, Glass rod, Spatula, Weighing
balance
Theory – Limit tests are quantitative or semi quantitative tests designed to identify and control small
quantities of impurity which are likely to be present in the substance. The limit tests for chlorides is based
on the reaction between silver nitrate and soluble chlorides to obtain silver chloride which is insoluble in
dilute nitric acid. The silver chloride produced in the presence of dilute nitric acid makes the test solution
turbid, the extent of turbidity depends on the amount of chloride present in the substance is compared
with the standard opalescence produced by addition of silver nitrate to a standard solution having a known
amount of chloride and the same volume of dilute nitric acid as used in the test solution. If the turbidity
from the sample is less than the standard turbidity, the sample will pass the limit test and vice versa.
Reactions involved in the test –
1. Soluble chlorides in substance + silver nitrate in presence of dilute nitric acid gives silver chloride and
nitrate ions
2. Sodium chloride + silver nitrate (in presence of dilute nitric acid) gives silver chloride and sodium
nitrate
Procedure –
Test solution –

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1. First of all, cleaned and dried Nessler cylinder was taken.
2. In the Nessler cylinder, 1 gram of sample was taken.
3. Then, 10 ml of water and 1 ml of nitric acid was added to it.
4. Now, the volume was made upto 50 ml with water.
5. Then, 1 ml of silver nitrate solution was added.
6. It was stirred well.
7. Finally it was kept aside for 5 minutes and then turbidity or opalescence was observed.
Standard solution –
1. First of all, cleaned and dried Nessler cylinder was taken.
2. In the Nessler cylinder, 1 ml of 0.058455% w/v solution of sodium chloride was taken.
3. Then, 1 ml of nitric acid was added to it.
4. Now, the volume was made upto 50 ml with water.
5. Then, 1 ml of silver nitrate solution was added.
6. It was stirred well.
7. Finally it was kept aside for 5 minutes and then turbidity or opalescence was observed.
Inference –
1. Turbidity of test solution > turbidity of standard solution – test failed
2. Turbidity of test solution < turbidity of standard solution – test passed
3. Turbidity of test solution = turbidity of standard solution – test passed
Result – On comparing the turbidity / Opalescence of test solution and standard solution, it was found
that the turbidity of test solution is…………………………….. (more than/ less tan / equal to) the
standard solution. Hence the sample ……………………………..(passed / failed) the limit test for
chlorides.

EXPERIMENT NO- 4

Object – To perform the limit test for Sulphate as per I.P..

Reference – Sharma N. etal, Practical Inorganic Pharmaceutical Chemistry & Viva voce, Birla
publications Pvt. Ltd., Delhi, I Edition, 2007-08, 96.
Materials required –
Chemicals – Barium sulphate reagent, dilute hydrochloric acid, Sodium Chloride, Potassium sulphate,
Distill water
Glasswares & Apparatus – Nessler cylinder, Measuring cylinder, Pipette, Glass rod, Spatula, Weighing
balance
Theory – Limit tests are quantitative or semi quantitative tests designed to identify and control small
quantities of impurity which are likely to be present in the substance. The limit tests for sulphates is based
on the reaction between sulphate and barium chloride in presence of hydrochloric acid.
Reaction involved-
BaCl2 + So42- → BaSO4 + 2Cl–
Hydrochloric acid prevents precipitation of other acid radicals with barium chloride, and in presence of
hydrochloric acid only sulphate get precipitated. The turbidity produced in each nessler cylinder was
compared transversely. If the turbidity from the sample is less than the standard turbidity, the sample will
pass the limit test and vice versa.

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 Fig : Nessler cylinder
Procedure –
Test solution –
1. First of all, cleaned and dried Nessler cylinder was taken.
2. In the Nessler cylinder, 2 gram of sample (NaCl) was taken.
3. Then, 2 ml of dilute hydrochloric acid was added to it.
4. Now, 45 ml with water was added.
5. Then, 5 ml of Barium sulphate reagent was added.
6. It was stirred well.
7. Finally it was kept aside for 5 minutes and then turbidity or opalescence was observed.
Standard solution –
1. First of all, cleaned and dried Nessler cylinder was taken.
2. In the Nessler cylinder, 1 ml of 0.01089% w/v solution of potassium sulphate and 9 ml of distill water
was taken.
3. Then, 2 ml of dilute hydrochloric acid was added to it.
4. Now, 45 ml with water was added to it.
5. Then, 5 ml of barium sulphate reagent was added.
6. It was stirred well.
7. Finally it was kept aside for 5 minutes and then turbidity or opalescence was observed.
Inference –
1. Turbidity of test solution > turbidity of standard solution – test failed
2. Turbidity of test solution < turbidity of standard solution – test passed
3. Turbidity of test solution = turbidity of standard solution – test passed
Result – On comparing the turbidity / Opalescence of test solution and standard solution, it was found
that the turbidity of test solution is…………………………….. (more than/ less tan / equal to) the
standard solution. Hence the sample ……………………………..(passed / failed) the limit test for
sulphate.

EXPERIMENT NO- 5

Object – To perform the limit test for Iron as per I.P..

Reference – Sharma N. etal, Practical Inorganic Pharmaceutical Chemistry & Viva voce, Birla
publications Pvt. Ltd., Delhi, I Edition, 2007-08, 96.
Materials required –
Chemicals – Thioglycollic acid, Iron free citric acid (20% w/v), Iron free ammonia, Ferric ammonium
Sulphate, Sulphuric acid, Sample

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Glasswares & Apparatus – Nessler cylinder, Measuring cylinder, Pipette, Glass rod, Spatula, Weighing
balance
Principle:

Limit test of Iron is based on the reaction of iron in ammonical solution with thioglycollic acid in
presence of citric acid to form iron thioglycolate which is pale pink to deep reddish purple in color.

Procedure:

Test sample Standard compound

Sample is dissolved in specific amount of water
and then volume is made up to 40 ml
Add 2 ml of 20 % w/v of citric acid (iron free)
Add 2 drops of thioglycollic acid
Add ammonia to make the solution alkaline and
adjust the volume to 50 ml
Keep aside for 5 min
Color developed is viewed vertically and
compared with standard solution
2 ml of standard solution of iron diluted with water
upto 40ml
Add 2 ml of 20 % w/v of citric acid (iron free)
Add 2 drops of thioglycollic acid
Add ammonia to make the solution alkaline and
adjust the volume to 50 ml
Keep aside for 5 min
Color developed is viewed vertically and compared
with standard solution

Earlier aamonium thiocyanate reagent was used for the limit test of iron. Since thioglycolic acid is more
sensitive reagent, it has replaced ammonium thiocyanate in the test.

Observation:

The purple color produce in sample solution should not be greater than standard solution. If purple color
produces in sample solution is less than the standard solution, the sample will pass the limit test of iron
and vice versa.

Result – On comparing the turbidity / Opalescence of test solution and standard solution, it was found
that the turbidity of test solution is…………………………….. (more than/ less tan / equal to) the
standard solution. Hence the sample ……………………………..(passed / failed) the limit test for Iron.

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 EXPERIMENT NO- 6

Object – To perform the identification test for the given sample of sodium bicarbonate.

Reference -
Practical Pharmaceutical Chemistry Anees Ahmed Siddiqui and M. Ali
Pharmaceutical Chemistry Practical -11 Laboratory Manual Amrita Parle New Dehli9.
Practical Pharmaceutical Chemistry-1 by Anil Bhandari , G.K. Singh

Materials required –
Chemicals – sodium carbonate, phenolphthalein solution, acetic acid, Distill water
Glasswares & Apparatus – Test tube, test tube holder, Measuring cylinder, Pipette, Glass rod, Spatula,
Weighing balance

Theory-
Sodium bicarbonate (IUPAC name: sodium hydrogen carbonate), commonly known as baking soda,
is a chemical compound with the formula NaHCO3. It is a salt composed of a sodium cation (Na+)
and a bicarbonate anion (HCO3−). Sodium bicarbonate is a white solid that is crystalline, but often
appears as a fine powder. It has a slightly salty, alkaline taste resembling that of washing soda
(sodium carbonate). The natural mineral form is nahcolite. It is a component of the
mineral natron and is found dissolved in many mineral springs.

IUPAC name

Sodium hydrogen carbonate

Other names
Baking soda, bicarb (laboratory slang), bicarbonate of soda,

Sodium bicarbonate reacts with acetic acid (found in vinegar), producing sodium acetate, water,
and carbon dioxide:
NaHCO3 + CH3COOH → CH3COONa + H2O + CO2(g)
Baking soda is the common name of sodium bicarbonate. The chemical formula of baking soda is
NaHCO3.
Baking Soda is also defined as Sodium Bicarbonate. The Medieval Egyptians first quarried Natron, a
natural deposit which mainly consists of Na2CO3. They used it as soap. In the year 1971,
NaHCO3 was first manufactured by a French chemist named Nicolas Leblanc. It was in the year
1846, John Dwight and Austin Church started a manufacturing unit to produce baking soda using
sodium carbonate and carbon dioxide.
We can see various applications of chemistry that are being exhibited in every part of a household
like in the bathroom, kitchen, etc. One such compound is Sodium bicarbonate, which is used mainly
because of its versatility, usefulness and its cheap price.

Preparation of Baking Soda

Solvay process is used for the production of sodium bicarbonate and sodium carbonate industrially.
In this process carbon dioxide, water, ammonia and brine solution in its concentrated form, are

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used as raw materials. This process is used mainly because it is inexpensive and less number of raw
materials are used to produce necessary chemicals. The important chemical reaction that is used in
the production of baking soda and sodium carbonate is:
CO2+H2o+NH3+Na+ → NaHCO3+NH+4
NaHCO3 → Na2CO3+CO2+H2O
Carbon dioxide produced is recycled to produce NaHCO3

Properties of Sodium Bicarbonate

 It is non-flammable.
 Powder dust is not as explosive.
 It has a melting point of 500
 NaHCO3 is a white crystalline solid which is odourless.
 It is basic in nature.

Uses of Baking Soda

 Reduces the acidity in the stomach

 Acts as an antacid which is used to treat stomach upset and indigestion
 Used in the process of washing as a water softener
 Due to the formation of soapy foam, it is used in fire extinguishers
 Used in baking industries as carbon dioxide is generated (due to the decomposition of
NaHCO3) which helps in the raising of the dough

Procedure-

EXPERIMENT NO- 7

Object – To perform the identification test for magnesium sulphate.

Reference -
Practical Pharmaceutical Chemistry Anees Ahmed Siddiqui and M. Ali
Pharmaceutical Chemistry Practical -11 Laboratory Manual Amrita Parle New Dehli9.
Practical Pharmaceutical Chemistry-1 by Anil Bhandari , G.K. Singh

Materials required –
Chemicals – magnesium sulphate, dilute ammonia solution, barium chloride solution., acetic acid, Distill
water
Glassware’s & Apparatus – Test tube, test tube holder, Measuring cylinder, Pipette, Glass rod, Spatula,
Weighing balance

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Theory- Magnesium sulfate is an inorganic salt with the formula MgSO4(H2O)x where 0≤x≤7. It is
often encountered as the heptahydrate sulfate mineral epsomite (MgSO4·7H2O), commonly
called Epsom salt. The overall global annual usage in the mid-1970s of the monohydrate was 2.3
million tons, of which the majority was used in agriculture.
Magnesium sulfate is a naturally occurring mineral used to control low blood levels of magnesium.
Magnesium sulfate injection is also used for pediatric acute nephritis and to prevent
seizures in severe pre-eclampsia, eclampsia, or toxemia of pregnancy.
Magnesium sulfate Formula
Magnesium sulfate is a widely used inorganic compound which is also called as Epsom salt or bath
salts.
Formula and structure: The chemical formula of magnesium sulfate is MgSO4 and its molar mass
is 120.366 g/mol. It also commonly exists as the monohydrate form (with one molecule of water)
which has the chemical formula of MgSO4.H2O, and molar mass of 138.38 g/mol. Magnesium sulfate
is a salt composed of the bivalent magnesium cation (Mg2+) and the sulfate anion (SO42-), in which
the central sulfur atom is attached to four oxygen atoms through two single and two double bonds.
Solid MgSO4 adopts an orthorhombic crystalline structure.

Occurrence: Magnesium sulfate occurs in nature in its hydrated forms in different minerals. It is
most commonly found in its heptahydrate form, as the mineral epsomite (MgSO4·7H2O), or Epsom
salt. It also occurs in its monohydrate form as the mineral kieserite (MgSO4·H2O).
Preparation: The naturally occurring MgSO4 minerals are the major source of magnesium sulfate
after mining, processing and dehydration of the hydrated forms. It can also be prepared chemically
by the reaction of sulfuric acid with either magnesium carbonate, magnesium hydroxide or
magnesium oxide.
Physical properties: Magnesium sulfate exists as an odorless, white crystalline solid with a density
of 2.66 g/mL, and melting point of 1,124°C. The monohydrate form of magnesium sulfate has a
density of 2.45 g/mL, and melting point of 200°C.
Chemical properties: MgSO4 is highly soluble in water, and is also extremely hygroscopic (absorbs
moisture from atmosphere). It can absorb large amounts of water in its anhydrous form (dry,
without any water molecules), and is an important laboratory desiccant. It is stable at normal
conditions. When heated to high temperatures, it decomposes to give toxic fumes of sulfur oxides.
Uses: Magnesium sulfate has many medical and household uses such as in bathing salts, beauty
products, anticonvulsants, muscle relaxants, laxative and electrolyte source (of Mg, an essential
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nutrient), among others. It also has important industrial applications such as electrolyte, bleaching
agent, desiccant, absorbent, fertilizer, brewing salt, etc
Procedure-

EXPERIMENT NO- 8

Object – To perform the assay of boric acid .

Reference -
Practical Pharmaceutical Chemistry Anees Ahmed Siddiqui and M. Ali
Pharmaceutical Chemistry Practical -11 Laboratory Manual Amrita Parle New Dehli9.
Practical Pharmaceutical Chemistry-1 by Anil Bhandari , G.K. Singh

Materials required –
APPARATUS: Volumetric flask, conical flask, Measuring cylinder and Burette.

CHEMICALS: Glycerin, NaoH solution, Boric acid and Phenolphthalein.

PRINCIPLE: Boric acid is a local infective. It is very weak acid and hence it can be titrated with

glycerin, glyceryl-boric acid is formed which behaves as a strong acid and can be titrated against

sodium hydroxide using phenolphthalein indicator.

PREPARATION OF REAGENTS:

PREPARATION OF 1M NaoH: 4gms of NaoH was accurately weighed and taken in a volumetric

flask and dissolved in water and make up to 100 with distilled water.

STANDARDIZATION OF 1M NaoH: 5gms of potassium hydrogen phthalate is weighed accurately

and taken in conical flask and dissolved in 20 ml of distilled water, phenolphthalein indicator is

added and titrated against with 1M NaoH.

ASSAY:

1gm of boric acid is taken in conical flask and dissolved in distilled water to it add glycerin and
phenolphthalein indicator titrated against with1M NaoH until a faint pink colour was produced.

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