DPHARM - 1Y - 12T - Pharm - Chemistry I

D.
PHARM (PART-I) SYLLABUS FOR PHARMACEUTICAL CHEMISTRY - I
(75 hours)
1) General discussions on the following inorganic compounds including important

physical and chemical properties, medicinal and pharmaceutical uses storage
conditions and chemical incompatibility.
a) Acids, bases and buffers - Boric acid*, hydrochloric acid; strong ammonium
hydroxide, calcium hydroxide, sodium hydroxide, and official buffers.
b) Antioxidants-Hypophosphorous acid, Sulphur dioxide, Sodium bisulphite,

Sodium meta bisulphite, Sodium thiosulphate, Nitrogen and Sodium Nitrite.
c) Gastrointestinal agents
i) Acidifying agents - Dilute hydrochloric acid
ii) Antacid - Sodium bicarbonate, aluminium hydroxidegel, aluminium

phosphate, calcium carbonate, magnesium carbonate, magnesium
trisilicate, magnesium oxide, combinations of antacid preparations.
iii) Protectives and Adsorbent - Bismuth subcarbonate, Kaolin.
iv) Saline cathartics, Sodium Pottassium tartate and magnesium sulphate,
d) Topical agents
i) Protectives, Zinc Oxide, calamine, Zinc stearate, Titanium dioxide,

Silicon polymers.
ii) Antimicrobials and Astringents-Hydrogen peroxide*, Potassium .

permanganate. Chlorinated lime, iodine, Solutions of iodine, Providone-
iodine, Boric acid, Borax. Silver nitrate, Mild silver protein, Mercury,
yellow mercuricoxide, Ammoniated mercury.
iii) Sulphur and its compounds Sublimed sulphur, precipitated sulphur,

Selenium sulphide.
iv) Astringents: Alum and Zinc Sulphate.

e. Dental products - Sodium fluroide, stannous fluoride, Calcium carbonate,
sodiummetaphosphate, dicalcium phosphate, Strontium chloride, Zinc chloride.
f. Inhalants - Oxygen, Carbon dioxide, Nitrous oxide.
g. Respiratory stimulants - Ammonium carbonate. Expectorants and Emetics -

Ammonium chloride, Potassium iodide. Antimony Potassium tartrate.
1) Antidotes - Sodium nitrite
2) Major Intra and Extracellular eletrolytes.
a) Electrolytes used for replacement therapy-Sodium chloride and its

preparations, Potassium chloride and its preparations.
b) Physiological acid base balance and electrolytes used, sodium acetate,

potassium acetate, sodium bicarbonate injection, sodium citrate,
potassium citrate, sodium lactate injection Ammonium chloride and
its injection
c) Combination of oral electrolyte powders and solutions.
3) Inorganic Official compounds of Iron Iodine, and Calcium Ferrous Sulfate and
calcium gluconate.
4) Radio pharmaceuticals and Contrast media - Radio activity - Alpha, Beta and Gamma
Radiations, Biological effects of radiations, Measurement of radio activity G.M.
Counter - Radio Isotopes - their uses storage and precautions with special reference to
the official preparations. Radio opaque Contrast media-Barium sulphate.
5) Quality control of Drugs and Pharmaceuticals importance of quality control,

Significant errors, methods used for quality control, sources of impurities in
Pharmaceuticals, Limit tests for Arsenic, chloride, sulfate, Iron and Heavy metals.
6) Identification tests for cations and anions as per Indian Pharmacopoeia.
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ACIDS, BASES AND BUFFERS
Theories of Acid and Base
Three important theories are
1. Arrhenius theory
2. Lowry and Bronsted theory
3. Lewis theory
1. Arrhenius Theory (Dissociation concept) According to this theory
i. Acid is a substance, dissociates to give hydrogen ions (H+) in water.
eg: HCl ⎯H⎯
⎯
2O
→ H+ + Cl-
ii. Base is substance, dissociates to give hydroxide ions (OH-) in water.
eg: NaOH ⎯H⎯
⎯O
→ Na+ + OH-
2
2. Lowry-Bronsted Theory (Proton Concept)

According to them
i. Acids are called as proton donors which donates protons in solution to any other
substance
ii. Bases are called as proton acceptors which accept protons in solution from any
other substance.
NH3 +HCl → NH4+Cl-
In the above reaction, HCl donates a proton and ammonia accepts that proton
forming ammonium chloride.
So, according to this theory HCl is an acid and ammonia is a base.
3. Lewis Theory (Electron Concept)
Based on this theory, acids are called as electron acceptors which accept a lone pair
of electrons. Bases are called as electron donors which donate a lone pair of electrons in
solution.
Eg : H+ + NH3 → NH4+
In the above reaction, proton (H+) accepts one electron pair from NH3 and is
therefore an acid, where as NH3 molecule donates an electron pair is a base.
BORIC ACID
M.F. H3 BO3
Syn : Ortho Boric Acid
Preparation :
(i) Laboratory Method
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Adding a mixture of concentrated sulphuric acid and water to a boiling solution of
borax, the solution is allowed to cool. The boric acid is filtered and then washed until they
become free from sulphate ions.
Na2 B4O7 + H2SO4 + 5H2O → Na2 SO4 + 4H3 BO3
(ii) Commercial Method or Industrial Method
It is prepared commercially by decomposing certain naturally occurring borates
such as colemanite, resonite, borax, etc. eg. Cole manite is suspended in boiling water then
sulphur-di-oxide gas is passed through the suspension to liberate boric acid.
Ca2 B6 O11. 5 H2O + 2SO2 + 4H2O
(Colemanite)
6H3BO3 + 2 CaSO3
(Calcium Sulphite)
Physical Properties
i. White odourless, crystalline powder, soft to touch.
ii. Slightly acidic to taste.
iii. Freely soluble in boiling water, boiling alcohol and glycerin.
Chemical Properties
i. Boric acid is a weak acid. On heating to 100C loses one molecule of water to
give meta boric acid.
C
H3BO3 ⎯100
⎯⎯ → HBO2 + H2O
(metaboric acid)
ii. Upon further heating to 160C, further loss of water from metaboric acid to tetra
boric acid.
160C
4HBO2 ⎯⎯⎯→ H2 B4O7 + H2O (Tetraboric acid)
iii. On heating tetra boric acid produces the boric acid anhydride, boron trioxide
B2O3
C
H2 B4O7 ⎯160
⎯⎯ → 2B2O3 + H2O
(Boron trioxide)
iv. One molecule of acid reacts with only one mole of sodium hydroxide.
NaOH + H3BO3 → NaBO2 + 2H2O
Assay
Boric acid is assayed by titrimetric method. It is a very weak acid, hence it cannot
be titrated directly with a base to a sharp end point. It is dissolved in a mixture of water
and glycerin and it is made as strong acid i.e., Glyceroboric acid and then it can be
titratred with sodium hydroxide to phenolphthalein as indicator. The end point is
appearance of permanent pale pink colour.
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CH2OH HO H2C – OH HO – H2C
| | |
CH – OH + HO B HC – O O – CH2
| | B | + 2H2O
CH2OH HO H 2C – O O – CH2
Glycerin Boric acid Glycero boric acid
Storage : Well closed container
Use : Anti infective
HYDROCHLORIC ACID
M.F. : HCl
Preparation
(i) It is manufactured by the action of sulphuric acid on sodium chloride (common
salt)
2NaCl + H2SO4 → Na2SO4 + 2HCl
(ii) Hydrogen and chloride gases (obtained from Electrolysis of sodium chloride
solution) are combined to give hydrogen chloride gas which is dissolved in water to
yield hydrochloric acid.
H2 + Cl2 → 2HCl
Properties (Physical & Chemical)
i. It is a colourless, fuming liquid having a pungent odour.
ii. It gives white precipitate with silver nitrate.
AgNO3 + HCl → AgCl  HNO3
Identification Test
i. When it is added to KMnO4, chlorine gas is liberated.
Assay : Titremetric method (acid-base titration)
It is assayed by titration with sodium hydroxide using methyl orange as an
indicator.
NaOH + HCl → NaCl + H2O
Storage It should be stored in well closed non-metallic container.
Use : as solvent, catalyst and also as an acidifier.
STRONG AMMONIA SOLUTION

M.F. : NH3
Syn : Liquior ammonia fortis
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Preparation : Laboratory Method
i. Heating ammonium chloride with calcium hydroxide.
2 NH4Cl + Ca(OH)2 → 2NH3  + CaCl2 +2 H2O
Commercial or Industrial Method
i. Haber Synthesis
Hydrogen and nitrogen gases are combined to give ammonia gas.
Fe
N2 + 3H2 2NH3
Mo
Physical Properties
i. It is clear, colourless, transparent liquid having characteristic strong pungent
odour.
ii. Highly soluble in water.
Chemical Properties
i. Ammonia is able to reduce potassium permanganate to MnO2.
2NH3 + 2KMnO4 → 2KOH + 2MnO2 + 2H2O + N2 
ii. Ammonia is a strong base. Therefore it reacts with acids to form salts.
NH3 + HCl → NH4Cl
Identification
When a glass rod dipped in HCl is brought near the surface of the solution,
white fumes will be produced.
Assay : Back Titration Method
Weighed amount of ammonia is added to the excess of sulphuric acid. The
excess or unreacted sulphuric acid is back titrated by titration with sodium hydroxide
solution using methyl red as indicator.
2NH3 + H2SO4 → (NH4)2 SO4
H2SO4 + 2NaOH → Na2 SO4 + 2H2O
Storage: It is stored in well closed amber coloured container having a rubber stopper in
cool place.
Use : Laboratory reagent, antacid, stimulant, counter irritant.
CALCIUM HYDROXIDE
M.F. : Ca(OH)2
Syn.: : Slaked lime
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Preparation Slaking Process
Spraying water on quicklime
CaO + H2O → Ca(OH)2
i. It is a soft white powder, having slightly bitter taste.
ii. It is soluble in water and in alcohol.
iii. On exposure to air, it absorbs atmospheric CO2 and forms CaCO3.
iv. When it is heated strongly, it loses water and is converted to CaO.
Ca(OH)2 → CaO + H2O
A clear saturated solution of calcium hydroxide in water is called lime
water.
Assay : Complexometric Method
A weighed amount of calcium hydroxide is mixed with sufficient amount of dilute
HCl. A known volume of the above solution is mixed with 15 ml of NaOH solution and 3
ml of napthol green are added titrated with disodium ethylene diamine tetra acetate
(EDTA) to the deep blue colour end point using murexide as an indicator.
Storage
It should be stored in well closed container, protected from moisture and carbon-di-
oxide.
Use :
(i) antacid, (ii) as an astringent (iii) Topically as a protective.
SODIUM HYDROXIDE
M.F : NaOH
Syn : Caustic Soda.
Preparation : Industrial method
Soda Lime Process
1. Sodium carbonate is heated with milk of lime.
Na2CO3 + Ca (OH)2 → CaCO3  + 2NaOH
i. It occurs in the form of flakes, sticks and pellets.
ii. It is very deliquescent.
iii. It is strongly alkaline and corrosive.
iv. It is soluble in water, alcohol and in glycerin with the production of heat.
v. It absorbs carbon-di-oxide and gets partially converted into sodium carbonate.
H2O + CO2 → H2CO3
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2NaOH + H2CO3 → Na2CO3 + 2H2O
Assay
As sodium hydroxide absorbs CO2, it contains a little sodium carbonate. Hence it
is assayed by two steps (for the estimation of total alkali and sodium carbonate in the
sample).
1st Step
Weighed sample is dissolved in CO2 free water and titrated with sulphuric acid
using phenolphthalein solution as an indicator, until the pink colour of the solution in
discharged.
2 NaOH + H2SO4 → Na2SO4 + 2H2O
2 Na2CO3 + H2SO4 → Na2 SO4 + 2NaHCO3
As per the above equations, all the NaOH has been neutralized by H2SO4 and
Na2CO3 is converted into NaHCO3. This step is called as half neutralization of sodium
carbonate.
IInd Step
To the above solution, methyl orange is added and the titration is continued until a
permanent pink colour is produced.
2NaHCO3 + H2SO4 → Na2SO4 + H2O + CO2
Storage
It must be stored in tightly closed container.
Use : Laboratory reagent
OFFICIAL BUFFERS
Buffer Solutions
Such solutions for which the pH will not be changed when a small amount of acid
or base is added. Buffer solutions consists of a mixture of weak acid and salt of its strong
base or weak base, and the salt of its strong acid.
Types of buffers:
1. Acidic buffer solutions, (Mixture of weak acid and the salt is called as above.
e.g., CH3COOH + CH3COONa
2.Basic Buffer
Mixture weak base and the salt. eg : NH4OH and NH4Cl
Buffer Action
The resistance possessed by buffers to change in pH is defined as buffer action.
Standard Buffer Solutions
Standard buffer solutions are solutions of standard pH.
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Official Buffers
The buffer solutions recommended by pharmacopoeia are called as official buffers.
e.g.
1. Acid phthalate buffer : It contains potassium hydrogen phthalate and hydro chloric
acid.
2. Alkaline borate buffer : It contains boric acid, potassium chloride and sodium
hydroxide.
3. Phosphate buffer : It contains potassium dihydrogen phosphate and sodium
hydroxide.
4. Acetate Buffer : (pH 2.8) : It contains sodium acetate and glacial acetic acid.
Uses of Buffers
Buffers are used to maintain the pH value.
i. pH of the blood is maintained by buffer system present in our body.
ii. Solubility of the many compounds can be controlled by providing suitable pH.
iii. It provides a particular pH for maximum enzyme activity. Hence it is used in
the assay of enzyme activity.
iv. They are very much useful in the estimation of metallic salts by complexometric
titrations, since the EDTA – metal complex is more stable at particular pH.
v. Certain pharmaceutical preparations are stabilized by adding suitable buffers.
ANTIOXIDANTS
Definition
Antioxidants are reducing agents which are added to the drugs or other
pharmaceutical preparations to prevent their oxidation.
Requirements of an Ideal Antioxidant
i. It should be chemically and pharmacologically inert.
ii. Effective in low concentration.
iii. It should not be toxic.
iv. It should be easily soluble.
HYPO PHOSPHORUS ACID
M.F. : H3PO2
Preparation
It is prepared by mixing calcium hypophosphite with sulphuric acid or oxalic acid.
The insoluble calcium salt is filtered and collected.
Ca(H2PO2)2 + H2SO4 → CaSO4 + 2H3PO2
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Calcium hypophosphite
Ca(H2PO2)2 + H2C2O4 → CaSO4 + 2H3PO2
(Calcium hypophosphite) oxalic acid
1. Clear yellowish liquid with slight acidic odour.
2. Soluble in water and alcohol.
3. It acts as monoprotic acid and ionizes to give
H3PO2 + H2O H3O+ + H2PO2-
4. It acts as a powerful reducing agent. With iodine it forms iodide.
H3PO2 + 2I2 + 2H2O → 4HI + H3PO4 (phosphoric acid)
5. It decolurise the KMnO4 solution.
Identification test
i. Upon heating with copper sulphate solution gives reddish brown precipitate.
Assay (Titremetric method)
Hypophosphorous acid is first diluted with water. Then it is titrated with sodium
hydroxide using methyl orange as indicator.
Incompatability
Since it is a reducing agent, it is incomptabale with oxidizing agents.
Storage
It should be stored in well closed container.
Use : As an antioxidant in pharmaceutical preparations.
SULPHUR DIOXIDE
M.F : SO2
Preparation : Laboratory Method
1. Burning sulphur in presence of air (or) oxgen.
2S + 2O2 → 2SO2
2. Decomposition of sodium sulphite with H2SO4 acid.
NaHSO3 + H2SO4 → NaHSO4 + SO2  + H2O
Industrial Method
Roasting of metallic sulphides such as
Cu2S + 2O2 → 2CuO + SO2 
(Copper sulphide)
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2ZnS + 3O2 → 2ZnO + 2SO2  etc.
(Zinc sulphide)
1. Colourless, non-inflammable gas with pungent odour.
2. Easily liquified.
3. Aqueous solution is acidic to litmus.
4. It is a very good reducing agent.
5. With iodine forms hydroiodic acid.
6. It decolurise the KMnO4 solution
2KMnO4 + 2H2O + 5SO2 → 2MnSO4 + 2H2SO4 + K2SO4
Assay
The method based upon the absorption of SO2 into NaOH solution to form sodium
bisulphite. Then bisulphite so formed is titrated with iodine solution using starch mucilage
as an indicator to a blue colour end point.
Storage
Should be stored in well closed container.
Incompatability
Generally incompatible with oxidizing agents (since it is a reducing agent).
Use :
1. It act as an antioxidant.
2. Used for the manufacture of sulphuric acid.
SODIUM META BISULPHITE

M.F : Na2S2O5
Preparation : It involves two steps
1st Step
Passing SO2 gas through a hot strong solution of sodium hydroxide until the
solution is saturated. Sodium bisulphite is formed.
NaOH + SO2 → NaHSO3
IInd Step
Sodium bisulphite loses water and gives sodium meta bisulphite on cooling.
2 NaHSO3 → Na2S2O5 + H2O
Properties:
1. Colourless crystals having sulphurous odour with saline taste.
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2. Freely soluble in water.
3. Aqueous solution is acidic.
Assay
Oxidation-reduction reaction. Weighed amount of sample is dissolved in water.
Then excess of iodine solution is added. (Which oxidizes the sodium metabisulphite
(reducing agent) to sodium meta sulphate.
Excess of iodine is titrated with sodium thiosulphate using starch mucilage as an
indicator.
Identification Test
(i) Decolurises the iodine solution.
Incompatibility
Generally incompatible with oxidizing agents.
Storage
Use
1. As an antioxidant in injections.
2. Preservation of food materials.
SODIUM THIOSULPHATE
M.F. Na2S2O3
Syn : Sodium hyposulphate or antichlor.
Preparation : Aqueous solution of a sodium sulphite is heated with sulphur. The
solution is concentrated, then the crystals are separated.
Na2SO3 + S → Na2S2O3
Properties
1. Colourless crystals or coarse crystalline powder, odourless, with alkaline taste.
2. It melts at 50C while decomposes on being heated at 100C.
3. It effloresces in dry air and deliquesces in moist air.
4. Soluble in water.
5. It reduces halogens.
2Na2S2O3 + I2 → 2Na I + Na2S4O6 (sodium tetrathionate)
6. Upon treating with HCl
7. It liberates, sulphur, sulphur dioxide
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Assay
Weighed amount is dissolved in water and titrated with iodine solution using starch
mucilage as an indicator.
2Na2 S2O2 + I2 → Na2S4O6 + 2NaI (soda. Tetra thionate)
Storage : Well closed container
Use :
i. With sod. nitrite as an Antidote in the treatment of cyanide poisonings (for
mingthiocyanate)
ii. Useful in skin diseases.
NITROGEN
M.F : N2
Atmospheric air contains nearly 78% of nitrogen. It also occurs as nitrate deposits.
Preparation
1. Distillation of liquid air.
2. Decomposition of NH3. (Haber Synthesis)
2NH3 N2 + 3H2
3. When burning the phosphorous in a closed container, phosphorous taken up the
oxygen and converted in phosphorous pentoxide (P2O5), leaving the nitrogen in the
container.
Properties
1. Colourless, odourless, tasteless gas.
2. It is soluble in alcohol, slightly in water.
3. It can be liquified.
4. It is inert gas (inactive)
Storage
Stored in metal cylinder under pressure. The cylinder is painted grey with black on
the neck and shoulders. The name should be stencilled or painted on the body of the
cylinder.
Use :
1. For the packaging of pharmaceuticals (as it is inert gas).
2. Diluent for oxygen
3. Liquid nitrogen is used in surgery to remove some tumours.
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SODIUM NITRITE
M.F. : NaNO2
Preparation
Most common suitable method
Absorbing of nitrogen oxide gas (NO) by sodium carbonate solution. The
solution is concentrated to crystallize out the product.
2Na2CO3 + 4NO + O2→ 4NaNO2 + 2CO2
Properties
1. Colourless to slightly yellow crystals, odourless, saline taste.
2. It is deliquescent. Absorb moisture and slowly gets oxidized to sodium nitrate.
4. It is a reducing agent.
Assay
The method is based upon the oxidation of nitrite to nitrate. weighed sample is
dissolved in water and mixed with excess volume of potassium permanganate solution.
Then 5ml of sulphuric acid was added. Then excess of oxalic acid is added, the mixture is
heated to 80 and the excess oxalic acid is back titrated with the std KMnO4 solution.
NaNO2 + H2SO4 → NaHSO4 + HNO2
HNO2 + O → HNO3
Storage
It should be preserved in tightly closed container.
Use
1. Antidote for cyanide poisoning.
2. Food preservative.
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GASTRO INTESTINAL AGENTS
ACIDIFYING AGENTS
Definition
These are drugs which are able to increase the acidity in GIT.
Types : Generally four types are there
(i) Gastric Acidifiers: (Drugs restoring temporarily the acidity of stomach incase
of achlorhydria or hypochlorhydria).
(ii) Urinary Acidifiers: (Drugs used to render urine acidic).
(iii) Systemic Acidifiers: Drugs which are able to neutralize the alkaline body fluids
particularly blood.
(iv) Acids: Used as pharmaceutical acids in preparation, laboratory quality control
etc.
DILUTE HYDROCHLORIC ACID I.P

Preparation
It is prepared by diluting concentrated hydrochloric acid with water i.e., about 10%
W/V of HCl (Limits 9.5 to 10.5%).
Properties
(i) It is a colourless liquid.
(ii) It’s specific gravity is 1.045.
(iii) When KMnO4 is added, chlorine is evolved.
Assay
It is assayed by titration with standard sodium hydroxide solution, using methyl
orange solution as indicator.
Acidifying agents are used in following conditions.
(i) Hypochlorhydria (decreased acid secretion).
(ii) Achlorhydria (No acid secretion).
ANTACID
These are drugs used for neutralizing excess acid in the stomach.
Classification
(i) Systemic antacids.
(ii) Non-systemic antacids.
(i) Systemic Antacids
They are used to reduce the acidity of blood.
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Eg. Sodium bicarbonate injsodium citrate.
(ii) Non-Systemic Antacids
They are used to reduce gastric acidify. (Not absorbed into systemic circulation).
Eg.
Aluminium hydroxide
Magnesium trisilicate
Magnesium hydroxide
Magnesium oxide
Aluminium phosphate
Calcium carbonate
SODIUM BICARBONATE
M.F. NaHCO3
Syn: Baking Soda
PREPARATION
Laboratory Method
It is prepared by passing CO2 gas through a solution of sodium hydroxide. The
solution is concentrated to get the product.
2NaOH + CO2 → Na2 CO3 + H2O
Na2CO3 + H2O + CO2 → 2 NaHCO3
Industrial Method
Solvay Process
Brine solution (NaCl) is saturated with ammonia (to remove impurities). The
solution is filtered, CO2 is passed through the solution. The precipitate is filtered and
dried.
H2O + CO2 → H2CO3
NH3 + H2CO3 → NH4HCO3
NaCl + NH4HCO3 → NaHCO3 + NH4Cl
Properties
(i) White crystalline or amorphous powder having saline taste.
(ii) It is freely soluble in water.
(iii) Practically insoluble in alcohol.
(iv) It gives an effervescence with acids.
(v) Its solution is alkaline in nature.
(vi) When heated, it gives sodium carbonate, CO2 and water.
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2NaHCO3 → Na2CO3 + H2O + CO2
Assay: Acid-Base Titration Method
Weighed amount is dissolved in water and titrated with sulphuric acid using methyl
orange as indicator.
2NaHCO3 + H2SO4 → Na2 SO4 + 2CO2 + 2H2O
Storage
It is stored in well closed container.
Use:
(i) Used in systemic acidosis.
(ii) Local application for burns, insect bites etc.
(iii) Used as a constituent in ear drops to soften and remove wax.
ALUMINIUM HYDROXIDE GEL

It is an aqueous suspension of hydrated aluminium oxide together with varying
amounts of basic aluminium carbonate. It contains aluminium oxide, glycerin, sucrose or
saccharin as a sweetening agent, peppermint oil as a flavouring agent and sodium benzoate
as a preservative.
Preparation
It is prepared by the reaction of an aluminium sulphate or aluminium chloride with
sodium carbonate or sodium bicarbonate. The precipitate of aluminium hydroxide is
collected, washed and resuspended in water and finally homogenized.
3Na2 CO3 + 3H2O → 3NaHCO3 + 3 NaOH
AlCl3 + 3NaOH + H2O → 3 NaCl + Al(OH)3. 3H2O
2NaHCO3 → Na2CO3 + H2O + CO2
Properties
1. It is a white viscous suspension.
2. A clear liquid gets separated when it is kept standing for sometime.
Assay: Complexometric Titration
Weighed amount is dissolved in hydrochloric acid by warming. Excess of std
EDTA is added. The mixture is neutralized by adding 1 N NaOH. This is warmed on a
water bath for half an hour (to ensure complexation between aluminium and EDTA). Then
hexamine is added (to maintain alkaline pH) and the excess of EDTA is back titrated with
std lead nitrate using xylerol orange as indicator.
Use
1. As an antacid.
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2. Since aluminium salts produce constipation, and are therefore generally
administered along with magnesium salts to counteract this effect.
ALUMINIUM PHOSPHATE
It consists mainly hydrated aluminium ortho phosphate (AlPO4).
Preparation
It is prepared by interaction between aqueous solutions of aluminium chloride and
sodium phosphate. The soluble salt is filtered and dried.
Properties
1. White powder.
2. Insoluble in water, ethanol and alkali hydroxides.
3. Soluble in dilute mineral acids.
Assay: (Complexometric Titration)
Weighed amount is dissolved in HCl, then excess EDTA is added. The solution is
made just alkaline. After boiling it for 5 mts, ammonium acetate and glacial acetic acid are
added. Then the pH is adjusted to 4.5 and titrate with zinc chloride (ZnCl2).
Use
1. Antacid.
2. Adsorbent for bacterial toxoids.
CALCIUM CARBONATE
M.F. (CaCO3)
Syn: Precipitated chalk
Occurence
In nature, it is found as chalk, marble, limestone, aragonite and calcite (one of the
main constituents of corals, pearls and shells).
Preparation (Commercial Method)

It is obtained by mixing the boiling solutions of calcium chloride and sodium
carbonate.
CaCl2 + Na2 CO3 → CaCO3  + 2 NaCl
The precipitate is collected, washed with boiling water (until it free from chloride
ions) and dried.
Properties
1. It occurs as fine, white, micro-crystalline powder.
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2. It is odourless and tasteless.
3. It is almost insoluble in water and alcohol.
4. Calcium carbonate neutralizes acids with effervescence.
CaCO3 + 2HCl → CaCl2 + CO2  + H2O
5. It produces constipation.
Assay: Complexometric Titration
Weighed amount is dissolved in HCl. Then the pH is adjusted to 12 by NaOH.
Then it is titrated with EDTA using murexide and napthol green mixture as indicator to a
deep blue color end point.
Use
1. Externally as dentrifice.
2. Internally as an antacid.
Generally it is administered along with magnesium salts (Laxative).
MAGNESIUM CARBONATE
M.F. 3Mg CO3. Mg(OH)2. 5H2O
It occurs in nature as magnesite (MgCO3) and dolomite (MgCO3. CaCO3).
Preparation
It is obtained by the double decomposition from magnesium sulphate and sodium
carbonate. They are dissolved separately in water and the solutions are mixed. The residue
is filtered and washed with water until it becomes free from sulphate ions.
MgSO4 + Na2CO3 → MgCO3  + Na2SO4
Properties
1. It is a white granular powder.
3. When heated to redness, it gets converted to MgO, losing CO2 and H2O.
3MgCO3. Mg(OH)2. 4H2O → 4 MgO + 3CO2 + 5H2O
Assay
It is assayed by complexometric titration.
Weighed sample is dissolved in dilute HCl small amount of NaOH solution is
added. Then it is titrated with EDTA using murexide as indicator.
Use:
Antacid
Laxative
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MAGNESIUM TRISILICATE
Formula: 2MgO. 3SiO2. 3H2O
Syn: Hydrated Magnesium silicate
This compound is having magnesium oxide and silicon oxide with varying
proportions of water of crystallization.
Preparation
It is obtained from sodium silicate and magnesium sulphate. The magnesium
trisilicate is precipitated out by slowly running a solution of magnesium sulphate into a
solution of sodium silicate. The precipitate is filtered, washed and dried.
Properties
1. White fine powder.
3. It is insoluble in water and alcohol.
Assay
It is assayed for magnesium oxide by conversion to magnesium chloride by
complexometric titration and for silicon dioxide by gravimetric method.
For Magnesium Oxide (MgO)
It is done by complexometric titration. Weighed sample is dissolved in
hydrochloric acid, small amount of NaOH solution is added. Then it is titrated with 0.05
M disodium edetate using Murexide indicator.
For Silicon dioxide (SiO2)
To the weighed sample, sulphuric acid is added and filtered. The insoluble SiO2 is
washed until free from sulphate and ignited for 5 minutes, cooled and weighed.
Use:
Antacid, adsorbent
MAGNESIUM OXIDE
M.F. MgO
There are two varieties of magnesium oxide are available.
1. Light MgO
2. Heavy MgO
Heating light or heavy magnesium carbonate, corresponding light or heavy
magnesium oxide is obtained.
Red heat
MgCO3  MgO + CO2 
Properties
1. It is a white powder.
2. It is odourless.
20
4. It is soluble in dilute acids.
Assay: By Complexometric Titration
Weighed sample is dissolved in dilute hydrochloric acid. Small amount of strong
ammonia – ammonium chloride solution is added, then it is titrated with 0.05 m EDTA
using mordant black II mixture as indicator.
Use: Antacid and Laxative
Combinations of Antacid
Preparations
Antacid preparations are formulated with one more than one antacid as
combinations to counteract the side effect of one by another or to be used for specific
conditions.
(i) Aluminium hydroxide gel – Magnesium hydroxide combination.
Preparation: Available as oral suspension and tablets.
Adv: Since aluminium salts causes constipation, this effect is balanced by laxative effect
of magnesium.
(ii) Simethicone containing antacids
It is formulated along with aluminium hydroxide gel and magnesium hydroxide.
It is available as oral suspension and tablet.
Advantage: Simethicone relieves flatulence.
(iii) Aluminium hydroxide gel – magnesium trisilicate combination
It is available as oral suspension and tablet.
Advantage:
Magnesium trisilicate has protective effect.
21
PROTECTIVES AND ADSORBENTS
1. They are generally insoluble.

2. Non-toxic
3. Chemically inert
4. They cover skin or mucous membrane from irritants.
Protectives
Definition : Chemically inert substance used to form a protective layer in GIT.
Adsorbents
Chemically inert substance used for removing toxic substances from GIT.
LIGHT KAOLIN I.P.

M.F : Al2O3. 2SiO2. 2H2O
Preparation :
It is prepared from the native clays, available as deposits in earth.
Procedure
1. Suspension of clay is prepared in water.
2. Larger particles (quartz, mica) are removed by elutriation.
3. Upon successive treatment with sodium pyrophosphate and HCl (to remove acid
soluble and basic soluble impurities) and finally subjected to evaporation gives the
fine particles of Kaolin.
Properties
1. It is a light white powder, soft to touch.
2. Insoluble in water, mineral acids and organic solvents.
I.P. includes two varieties of kaolin one is heavy kaolin and the other is light
kaolin. The light kaolin is purer and smaller in particle size than the heavy variety. Only
light kaolin is intended for internal use.
Use : as an adsorbent for toxic substances from G.I.T. tract.
Storage
It should be stored in a well closed container
22
BISMUTH SUB-CARBONATE
M.F. [(Bio)2 CO3]2 H2O).
Preparation
It involves two steps.
st
1 Step : Bismuth nitrate is prepared by treating metallic bismuth with nitric acid.
2Bi + 8 HNO3 → 2 Bi(NO3)3 + 2NO + 4H2O
2nd Step : Adding bismuth nitrate solution to a cold sodium carbonate solution with
constant stirring. The white precipitate is washed with water and dried.
4 Bi (NO3)3 + 6 Na2. CO3 + H2O →
[(Bio)2 CO3]2 H2O  + 12 NaNO3 + 4CO2 
White or pale yellowish odourless, tasteless powder, affected by light.
1. With acids, it produces effervescence.
2. On heating it yields bimuth oxide (90%)

[(BiO2) CO3]2 H2O ⎯ ⎯→ 2 Bi2 O3 + 2 CO2 + H2O
Assay : Gravimetric method
Weighted sample is ignited to constant weight. It is required to yield not less than
90% of Bismuth oxide.

[(BiO)2 CO3]2 H2O ⎯ ⎯→ 2 Bi2 O3 + 2 CO2  + H2O
Use : used in diarrhoea and dysentry.
Storage : It should be stored in well closed air tight container.
SALINE CATHARTICS
These are drugs, when given orally retained in GIT, increases the intestinal bulk by
drawing water from circulation by osmosis. They acts as mechanical stimulus, produces
increased peristalic movement causing diarrhoea. They are also called as saline purgatives
or osmotic laxatives.
SODIUM POTASSIUM TARTRATE

Syn. : Rochelle salt
M.F : CH (OH) – COONa
CH (OH) – COOK
Preparation
It is obtained by neutralizing a solution of sodium carbonate with potassium
bitartrate. The solution is boiled for few mts and then allowed to stand at 60C for the
completion of the reaction. (till the CO2 ceases). The solution is filtered and evaporated.
23
2 CH OH − COOH
+ Na2 CO3 →
CH OH − COOK
(Potassium bitartrate)

2 CH OH − COONa
+ CO2  + H2O
CHOH − COOK
Properties
Colourless, crystalline efflorescent powder soluble in water, insoluble in alcohol.
Upon heating at high temperature gives sodium and potassium carbonates.
2 KNa C4H4O6 + 5O2 → K2CO3 + Na2CO3 + 6 CO2 + 4H2O
Assay : Back titration method
An accurately weighted sample is ignited or heated until carbonized. The residue is
boiled with excess of standard sulphuric acid and filtered. Excess of acid is back titrated
with standard sodium hydroxide using methyl orange as an indicator.
CH (OH) − COONa
| + 5O2 → + K2CO3 + Na2 CO3 + 6CO2 + 4H2O
CH – (OH) COOK
K2CO3 + Na2CO3 + 2H2SO4 → K2SO4 + Na2SO4 + 2CO2 + 2H2O

Excess H2SO4 + 2 NaOH → Na2SO4 + 2H2O.
Identification Test :
When heated the salt emits an odour of burning sugar and leaves a residue which is
alkaline to litmus paper.
Storage
It should be stored in air tight container.
MAGNESIUM SULPHATE
M.F. MgSO4. 7H2O Syn.: Epsom salt.
It can be prepared by alizing sulphuric acid with magnesium oxide or magnesium
carbonate or native dolomite
MgO + H2SO4 → MgSO4 + H2O
MgCO3 CaCO3 + 2H2SO4 → MgSO4 + 2H2O + 2CO2 + CaSO4
(Dolomite)
24
The impurities are precipitated only mag. Sulphate remains in solution. The
solution is filtered, and evaporated.
Properties
1. White powder or colourless crystals, odourless with a bitter taste.
2. In warm dry air it may lose water by efflorescence.
3. Freely soluble in water, insoluble in alcohol.
Assay : By complexometric titration
Weighed amount is dissolved in water, strong ammonia-ammonium chloride buffer
is added and titrated against 0.05 m EDTA using Mordant Black II mixture as an
indicator. The end point is change of wine red to blue colour.
EDTA + Mg2+ →
NaOOCH2C CH2COONa
N – CH2 – CH2 - N Use :

1. Used for constipation.
H2C Mg CH2
2. Evacuation of gall
C C bladder (in case of
chole cystitis)
O O O O Storage It should be stored in
air tight container.
TOPICAL AGENTS
PROTECTIVES
They are group of insoluble substances, applied to the skin to protect from
irritation. They are non toxic and biologically inactive.
TALC I.P
M.F. Mg6 (Si2O5)4 (OH)4
It is a purified natural hydrated magnesium silicate, and may contain small amounts
of aluminum silicate.
Preparation
The native talc is finely powdered and boiled with dilute HCl (to remove impurities
like iron, Cao, iron etc.). The insoluble talc is completely washed with water until it
becomes free from acid. The residue is then dried.
Properties
i. Very fine, white or grayish white powder.
25
ii. It is smooth to touch.
iii. Odourless and tasteless.
iv. Its solution is neutral to litmus.
v. Practically insoluble in water, dilute acids and alkalies.
Storage
Use
1. As a base for dusting powders.
2. As a lubricant for tablet making.
3. As a filtering and distributing agent.
]
ZINC OXIDE
M.F: ZnO
Preparation :
1. Large Scale: Heating metallic zinc, in a current of air to a high temperature. The
metal vapour burns to form the oxide, collected as a fine white powder.

2Zn + O2 ⎯
⎯→ 2 ZnO
2. Medicinal Grade : Zinc oxide is obtained by adding zinc sulphate to a boiling
solution of sodium carbonate. The precipitated zinc carbonate is washed until it
becomes free from sulphate. Now it is dried and ignited, loses CO2 and water, giving
the oxide.
ZnSO4 + Na2 CO3 → ZnCO3 + Na2SO4

ZnCO3 ⎯
⎯→ ZnO + Co2
1. White or faintly white very fine powder.
4. It slowly absorbs CO2 from the air and forms basic zinc
carbonate.
5. It reacts with acids forming zinc salts.
ZnO + 2 NaOH → ZnCl2 + H2O
6. It reacts with base forms zincates.
ZnO + 2NaOH → Na2 ZnO2 + H2O
26
Assay : Back Titration Method
Weighed amount of the sample is dissolved in excess of std H2SO4 acid, small
amount of ammonium chloride is added and heated if necessary. The excess of sulphuric
acid is back titrated with std NaOH using methyl orange as an indicator.
(Ammonium chloride prevents the precipitation of zinc hydroxide by the NaOH
near the end point).
ZnO + H2SO4 → ZnSO4 + H2O
Unreacted H2SO4 + NaOH → Na2SO4 + H2O
Storage
Use :
1. as a mild antiseptic and an astringent.
2. for making dental cement.
3. used in various skin diseases.
4. manufacture of adhesive tapes and bandages.
CALAMINE
Calamine is zinc oxide having a small amount of ferric oxide.
Preparation (Large Scale)
1st Step
Zinc oxide is prepared by heating zinc carbonate.
ZnCO3 → ZnO + CO2
2nd Step
The calamine is then prepared by mixing zinc oxide with ferric oxide (up to 1.0 per
cent) thoroughly.
Properties
1. It is pink powder.
2. Almost odourless and tasteless.
3. Almost insoluble in water but dissolved completely in mineral acids.
Assay
It is dissolved in excess of std. sulphuric acid and filtered then a small amount of
ammonium chloride is added. The excess acid is back titrated with NaOH solution using
methyl orange as an indicator.
NH4Cl is added to prevent the precipitation of zinc hydroxide during titration.
27
Storage
Use
Astringent, antiseptic and protectant for the skin.
ZINC STEARATE
M.F. (C17H35COO)2 Zn
Zinc stearate contains mainly zinc stearate with variable proportion of zinc
palmitate. It also contains 13% of zinc oxide (ZnO).
Preparation
It is prepared by adding zinc sulphate to a solution of sodium stearate.
2C17H35 COONa + ZnSO4 → (C17 H35 COO)2 Zn + Na2SO4
The precipitate is washed and dried.
Properties
1. White, amorphous powder free from grittiness.
2. It has faint characteristic odour.
3. It is insoluble in water, alcohol and other.
Assay : By Complexometric Method

Weighed amount of sample is boiled with H2SO4 (to convert the zinc present in Zn.
Stearate to zinc sulphate). Then the solution is treated with ammonia - ammonium
chloride buffer to adjust the pH = 10 an titrated with std EDTA using eriochrome black T
as indicator at 40C.
(C17 H35 COO)2 Zn + H2SO4 → ZnSO4 + 2C17H35 COOH.
EDTA + Zn2+ → (EPTA Zn complex)
Use
Astringent and antimicrobial agent
As a protectant in skin disorder.
Storage
TITANIUM DIOXIDE
M.F. TiO2
It is an oxide of Titanium (Ti)
28
Preparation
It is obtained natural samples of ilmenite (ore). The ore is heated with conc.
sulphuric acid. The precipitate of titanium dioxide is obtained by hydrolysis.
Properties
1. White powder, odourless and tasteless.
2. Insoluble in water and in dilute mineral acids.
3. It dissolves slowly in hot H2SO4 and ammonium sulphate forms double salt.
Assay : By Complexometric Method
Weighed sample is dissolved in a mixture of H2SO4 and ammonium sulphate. The
solution is filtered and washed several times with water. Then 50 ml of EDTA is added
and the pH is adjusted to 5 and the resulting solution is titrated with ZnCl2 (zinc chloride)
using xylenol orange solution as indicator.
Use
1. Very good topical protective.
Storage
It is stored in well closed container.
Silicon Polymers
They are polymers having the general formula
R R
Si O Si O
R R
1. Highly viscous liquids.
2. Viscosity increases with increase in molecular weight.
3. They are stable towards heat and chemical reagents.
4. They can be used as lubricants over a wide range of temperature.
ASTRINGENTS
Astringents are the substances which precipitates the protein.
Alum
Formula Kal (SO4)2. 2H2O. Alum is potassium aluminium sulphate. It is a double
salt containing potassium and aluminium sulphate.
Preparation
It is prepared by adding a concentrated solution of potassium sulphate to a hot
solution of an equal amount aluminium sulphate.
K2SO4 + Al2 (SO4)3 + 24 H2O → 2KAl (SO4)2. 12H2O
29
The solution is concentrated, cooled and the crystals are separated.
Properties
1. Colourless transparent crystals having a sweet astringent taste.
2. It is soluble in water but insoluble in alcohol.
3. At 200C it loses its water at crystallization and becomes anhydrous.
Assay
Complexometric Titration Method
Weighed amount is dissolved in water, treated with known volume of Std EDTA
(Aluminium forms complex with EDTA). The unreacted EDTA is back titrated with
standard lead nitrate in presence of hexamine buffer using xylenol orange as indicator.
Use
1. Used in the preparation of toxoids.
2. Antiseptic and local styptic (to stop bleeding from cuts).
ZINC SULPHATE
M.F. ZnSO4. 7H2o
Preparation
It is prepared by two methods.
1st Method
It is prepared by heating zinc sulphide in presence of air. The heated mass is
dissolved in hot water, and filtered.
ZnS + 2O2 → ZnSO4
Offecial Method
It is obtained by digesting metallic zinc aranules in dil. H2SO4.
Zn + H2SO4 → ZnSO4 + H2 
Properties
1. Granular crystalline powder.
2. It is odourless and metallic taste.
3. It effloresces in dry air.
4. It is very soluble in water and glycerine.
5. Insoluble in alcohol.
6. It forms double salts with potassium and ammonium sulphate.
ZnSO4 + (NH4)2 SO4 → ZnSO4 (NH4)2. SO4 6H2
30
Assay:
Complex metric Titration Method
It is titrated with EDTA in presence of ammonia – ammonium chloride buffer using
eriochrome black T as an indicator.
Use
1. Internally acts as an emetic.
2. Externally as an astringent.
3. 0.25% solution is used as eye lotion.
SULPHUR AND ITS COMPOUNDS
SUBLIMED SULPHUR
Symbol : S
Syn : Flowers of Sulphur
Preparation
It is prepared by heating any kind of sulphur and condensing the vapour.
Properties
1. Fine crystalline powder.
2. It has faint characteristic odour but tasteless.
3. It is insoluble in water.
Use :
Antiseptic and scabicide.
PRECIPITATED SULPHUR
Symbol : S
Preparation (Small Scale)
It is prepared by acidifying sodium thiosulphate solution with hydrochloric acid.
The unstable thiosulphuric acid is liberated, gets rapidly decomposed to give precipitated
sulphur.
Na2 S2O3 + 2 HCl → H2S2O3 + 2 NaCl
H2S2O3 → S + SO2 + H2O
Industrial Method
It is prepared by heating together sublimed sulphur and milk of lime for an hour.
2 Ca (OH)2 + 12S → 2 CaS5 + CaS2O
(cal. Penta sulphide)
31
CaS5 + 2 HCl → CaCl2 + H2S + 4S
(Calciumpenta
Sulphide)
Properties
1. Pale greenish yellow soft powder.
2. Odourless and tasteless.
3. Upon heating it burns with a blue flame.
S + O2  SO2
Use:
1. Good scabicide.
2. Antiseptic
3. Used in treatment of acne.
4. Parasiticide.
SELENIUM SULPHIDE
M.F. SeS2
Preparation
It is prepared by passing hydrogen sulphide gas into selenious acid. The precipitate
is filtered and dried.
H2SeO3 + 2H2S → SeS2  + 5H2O
Selenious acid
Properties
1. It is orange powder having faint sulphide odour.
2. Insoluble in water, alcohol and organic solvents.
3. It dissolves in nitric acid and form selenious and sulphuric acid.
SeS2 + 16 HNO3→ H2SeO3 + 2H2SO4 + 16NO2  + S H2O
Use:.
1. Anti dandruff
DENTAL PRODUCTS
Dental Caries (Tooth decay)

It is a disease of the teeth caused by acids produced by the action of micro
organisms on food materials. This is disease is characterized by decalcification of tooth
accompanied by foul mouth odour. To prevent dental caries and to maintain clean and
32
healthy teeth it becomes necessary to use dentrifices. Main function of dentrifices is to
clean the surface of the teeth.
Role of Fluoride
Small quantity of fluoride is necessary to prevent dental caries. The fluoride which
are deposited on the surface of teeth does not allow the action of acids or enzymes in
producing lesions. The anticaries agents used are dentrifices and fluoride salts.
SODIUM FLUORIDE
M.F. : NaF
Preparation
It may be prepared by neutralization of hydro fluoric acid with (NaOH) sodium
carbonate.
2HF + Na2CO3 → 2NaF + H2O + CO2 
Another Method
It is prepared by double decomposition of calcium fluoride with sodium carbonate.
CaF2 + Na2CO3 → 2 NaF + CaCO3 
Properties
1. It is a white powder.
2. Colorless and odourless.
3. It is soluble in water.
4. Insoluble in alcohol.
5. Upon acidification ; hydrofluoric acid is produced.
NaF + HCl → HF + NaCl
Assay
It is assayed by complexometric titration.
Weighed quantity is dissolved in water, sodium chloride and alcohol is added. Then
the solution is treated with excess of lead nitrate.
2 NaF + pb (NO3)2 → pbF2 + 2NaNO3
The precipitate is filtered. The filtrate and the washings are titrated with disodium
edetate using xylerol orange as indicator.
Use
To prevent dental caries.
Storage
Should be stored in well closed container.
33
STANNOUS FLUORIDE
M.F. : SnF2
Preparation
It is prepared by dissolving stannous hydroxide in hydro fluoric acid.
Sn(OH)2 + 2HF → SnF2 + 2H2O
Properties
1. it is a white crystalline powder having salty taste.
2. It is soluble in water.
3. Insoluble in alcohol and organic solvents.
4. Aqueous solution of stannous fluoride decomposes rapidly because of its oxidation
from stannous to stannic form causing turbidity.
5. It must be freshly made.
Use:
To prevent dental caries.
Assay
Iodimetry method weighed amount is dissolved in hot recently boiled dilute
hydrochloric acid. The flask is cooled, potassium iodide is added, then it is titrated with
potassium iodide using starch as an indicator.
Dentrifice is a material used for cleaning of teeth and adjacent gums.
CALCIUM CARBONATE
Calcium carbonate is a fine powder used as dentrifices in tooth powders and in
toothpastes. For other details please refer antacids.
SODIUM METAPHOSPHATE
It is the sodium salt of polymeta phosphoric acid.
M.F. (NaPO3)
It occurs as a white powder soluble in water. It is used in dentrifices as an abrasive.
Also used as an anti-rusting agent (for surgical instruments). Also as a stabilizing,
emulsifying and chelating agent in food industry.
DICALCIUM PHOSPHATE
M.F. Ca HPO4. 2H2O
Syn : Dibasic calcium phosphate.
34
Preparation
It is obtained by mixing neutral calcium chloride with disodium hydrogen
phosphate solution.
CaCl2 + Na2 HPO4 → CaHPO4  + 2 NaCl
The precipitate is filtered, washed and dried.
Properties
1. Very fine powder.
3. When exposed to air, it effloresces losing waters (forms anhydrous form).
Assay
Complexometric Titration
Weighed amount is dissolved in hydrochloric acid and titrated with EDTA using
hydroxy naphthol blue as indicator.
Use:
Externally as a dentrifice, orally as an electrolyte replenisher.
STRONTINUM CHLORIDE
SrCl2. 6 H2O
Preparation
It is prepared by treating HCl with strontium oxide.
SrO + 2HCl → SrCl2 + H2O
Properties
1. Grayish – white powder.
3. It is insoluble in water.
Use:
To relieve dental hypersensitivity (reduce the sensitivity of teeth to heat and cold).
ZINC CHLORIDE
M.F. ZnCl2
Preparation
It is prepared by reaction of hydrochloric acid, on zinc oxide or metallic zinc or
zinc carbonate.
Zn + 2 HCl → ZnCl2 + H2
35
Properties
1. White crystalline odourless powder.
2. It is very deliquescent.
3. It is soluble in water, alcohol, acetone and glycerin.
4. It is incompatible with soluble carbonates, phosphates, tannic acid.
Assay:
Complexometric Titration Method
Weighed amount is dissolved in water, and ammonia-ammonium chloride buffer is
added, titrated with std EDTA using eriochrome black as an indicator.
Use
1. It act as desensitizing agent in dental remedies.
2. Used as antiseptic lotion for foul – smelling wounds.
INHALANTS
These are the drugs in the vapour form are inhaled or administered through the
respiratory system in our body.
OXYGEN
M.F. O2
Preparation
It occurs free in air up to 21%.
Preparation: By two methods
1. Fractional distillation of liquified air yields oxygen at - 183C (90K).
2. Electrolysis of slightly alkaline water (pure water is bad conductor of electricity).
2H2O → 2H2 + O2
Properties
1. Colourless, odourless and tasteless gas.
2. It supports combustion but is not inflammable.
3. When mixed with equal volumes of nitric oxide, red fumes of nitrogen dioxide is
formed.
2NO + O2 → 2NO2
4. It is soluble 1 in 32 parts by volume of water.
Assay:
36
Assay is based on its complete absorption by alkaline pyrogallol solution using
specific apparatus for determination of medicinal gases.
Storage
Oxygen is usually stored in metal cylinders under compression, should be painted
black. The shoulders of the cylinder should be painted white. The name of the gas or the
symbol “O2” properly stenciled on it. The cylinders are recommended to be stored in cool
room free from other inflammable materials.
Uses
1. as inhalant for supporting respiration during anaesthesia or post operative
conditions.
2. inhalant for poisoning due to other gases.
3. Diluent for volatile and gaseous anaesthetics.
CARBON DIOXIDE
M.F. CO2
Syn : Carbonic acid gas, carbonic anhydride.
Preparation
It is obtained from calcium carbonate (lime stone) either by direct strong heating or
by treatment with dilute mineral acids.
CaCO3 CaO + CO2 (g)
CaCO3 + 2HCl Heat CaCl2 + H2O + CO2 (g)
Commercial Method
Large quantities of the gas are obtained as by – products of fermentation industries
or fertilizer factories.
Properties
1. Colourless, odourless gas.
2. Does not support combustion.
3. It is heavies than air, soluble in water.
4. The solution is slightly acidic due to the formation of carbonic acid.
CO2 + H2O → H2CO3
5. It can be liquified under compression.
6. It can be solidified called as dry ice.
7. It extinguishes fire.
37
Storage
It is stored in metal cylinders painted qrey. The name of the gas or the formula CO2
should be stenciled on the shoulder of the cylinder.
Assay
Assay is based on its absorption by 50% KOH solution. The un absorbed gas is
measured.
Uses
1. It is essential for regulating acid base balance in the body.
2. Respiratory stimulant.
3. To give relief in hick-up.
4. For rapid excretion of inhalation anaesthetics.
5. Liquid orals treated with CO2 gas are used to mask the taste.
6. It can also be used as an inert gas in the containers containing easily oxidization
substances.
NITROUS OXIDE
M.F. N2O
Syn : Laughing gas
Preparation
1. It is obtained by heating ammonium nitrate to about 170C.
NH4 NO3 (S) → N2O (g) + 2H2O
2. It can also be prepared by heating a mixture of sodium nitrate and ammonium
sulphate.
2NaNO3 + (NH4) SO4 → Na2SO4 + 2N2O + 4H2O
Properties
1. Colourless, odourless and tasteless gas.
2. Soluble in water, alcohol, chloroform ether and in oils.
3. It supports combustion.
4. It is not absorbed by alkaline pyrogallol solution (differ from oxygen).
5. It is heavier than air and can be compressed to a liquid.
Assay
It is assayed by determining uncondensible gas in a particular apparatus
(gaseometric set up) using liquid nitrogen for condensation of N2O. The uncondensible
part should not exceed 5% V/V.
Use
Used as general anaesthetic along with oxygen (20 to 50%) indental practice.
38
RESPIRATORY STIMULANTS
These are drugs used to increase the activities of various functions of the CNS,
mainly to stimulate respiration.
Ammonium Carbonate N.F.
It contains variable proportion of ammonium bicarbonate and ammonium
carbonate.
Preparation
1. Ammonium carbonate is manufactured by subliming a mixture of ammonium
sulphae and calcium carbonate.
2(NH4)2 SO4 + 2CaCO3 → NH4 HCO3 + NH2 COONH4
(Ammonium carbonate)
2. It is also prepared by the reaction of CO2 and ammonia in presence of stream.
3NH3 + 2CO2 + H2O + NH4HCO3 + NH2 COONH4
Properties
1. White powder, alkaline to litmus.
3. On exposure to air, it decomposes into ammonia and carbon dioxide.
Assay: Back Titration Method
Weighed amount is dissolved in excess of sulphuric acid. Excess of sulphuric acid
is back titrated with standard sodium hydroxide using methyl orange as indicator.
Storage
It should be stored in air tight container.
Use: As expectorant
39
EXPECTORANTS AND EMETICS
These are drugs, eliminate the secretions of respiratory tract by inducing cough.
Ammonium Chloride
M.F. NH4Cl
Preparation
It is prepared by neutralizing hydrochloric acid with ammonium hydroxide.
Properties
1. White crystalline, odourless powder with saline taste.
2. It is hygroscopic.
3. Freely soluble in water.
Assay
Weighed amount is dissolved in water and treated with pre-neutralised
formaldelyde solution. The ammonium chloride is decomposed to methyleneimine and an
equivalent amount of hydrochloric acid. The liberated acid is titrated with standard NaOH
using phenolphthalein indicator.
Use:
1. Expectorant
2. Diuretic
3. Systemic acidifier
POTASSIUM IODIDE
M.F.: KI
Preparation
It is prepared by the action of potassium hydroxide on iodine, potassium. Iodate is
converted to Iodide.
6 KOH + 3I2 → KIO3 + 5KI + 3H2O
KIO3 + 3C → KI + 3CO
Properties
Colourless, crystalline or white powder.
Odourless with slight bitter taste, soluble in water, glycerin and in alcohol. On
standing becomes yellow particularly exposed to light due to the liberation of free iodine.
Assay
It is assayed by titration with potassium iodate. It is dissolved in water, conc. HCl is
added into it and is then titrated with a standard potassium Iodate solution.
KIO3 + 5KI + 6 HCl → 6 KCl + 3I2 + 3H2O
40
KIO3 + 2I2 + 6 HCl → KCl + 5I Cl + 3H2O
Use
1. For thyroid deficiency
2. Expect or ant
Emetics
Emetics are drugs used to produce vomiting.
ANTIMONY POTASSIUM TARTRATE

M.F. C4H4KO7 Sb
Syn : Taster emetic
Preparation
It is prepared by mixing antimony trioxide with potassium acid tartrate. It is then
boiled for few mts. Then the liquid is filtered and dried.
2 KHC4H4O6 + Sb2O3 → 2K (SbO) C4H4O6 + H2O
Properties
1. Colourless, odourless crystals having sweet taste.
2. It is soluble in water but insoluble in alcohol.
3. On exposure to air, crystals effloresces.
Assay: Iodometric Method
Weighed amount is dissolved in water, small amount (about 2g) of sodium
bicarbonate is added. Then it is titrated with iodine using starch mucilage as indicator.
2 C4H4O7 Sb K + 3H2O + I2 → 2k H C4H4O6 + Sb2 O5 + 4 HI
Storage
It is stored in air tight container.
Use
1. to treat schistosomiosis.
2. It is acting as an emetic.
ANTIDOTES
These are drugs or remedies which neutralize the poison or converting them to non-
toxic.
Sodium Nitrite (NaNO2)
Refer under Antioxidants.
41
MAJOR INTRA AND EXTRA CELLULAR ELECTROLYTES
The body fluids are solutions of inorganic and organic solutes. The concentration
balances of the various components are maintained in order for the cells and tissues to
have a constant environment. To maintain the electrolyte balance, there are regulatory
mechanisms which controls pH, ionic balances, osmotic balances, etc.
Electrolytes used in replacement therapy
The electrolytic concentration will vary with a particular fluid compartment.
1. Intracelluar fluid – (45 – 50% of body weight and present with in the cell).
2. Extracellular fluid – (12 – 15% of body weight and present outside the cell).
a. Interstitial fluid – (12 – 15% of body weight and
b. Plasma or vascular fluid (4 – 5% of body weight)
The electrolytes are necessary for maintaining osmotic pressure and electro
neutrality (equal number of cations and anions). The electrolytes also essential to transmit
impulses.
In case of loss of electrolytes in the body due to water imbalance like diarrhoea,
vomiting, excessive use of diuretics etc. the above functions of electrolytes will be
affected. During this condition, the patient should be given with suitable electrolyte in the
form of injection or oral solutions to maintain the normal level of electrolyte.
The electrolytes used for replacement therapy
1. Sodium chloride
2. Potassium chloride
3. Calcium chloride
4. Calcium gluconate
5. Potassium gluconate
6. Calcium lactate
7. Dibasic calcium phosphate
8. Tribasic calcium phosphate
9. Magnesium sulfate.
SODIUM CHLORIDE (NaCl)
Preparation
It can be prepared from sea-water, under ground rock-salt deposits and by chemical
means. Sea water contains about 3% of sodium chloride. Purest form of analytical grade
sodium chloride is prepared by passing hydrogen chloride gas into a standard solution of
the salt. Very pure sodium chloride precipitates out. The crystals are then centrifuged and
dried.
Physical Properties
42
It occurs in the form of colourless, transparent cubical crystals, or as a white
crystalline powder. It is odourless and slight saline test. It is slightly hygroscopic due to
the presence of small amount of magnesium or calcium chloride. It is freely soluble in
water and slightly soluble in alcohol.
Chemical Properties
1. Sodium chloride gives white precipitate of silver chloride with solution of silver
nitrate.
NaCl + AgNO3 → AgCl  + NaNO3
The precipitate is light sensitive (affected by light) and it is soluble in dilute
ammonia and in soluble in nitric acid.
2. It reacts with sulphuric acid or phosphoric acid to give hydrochloric acid.
2NaCl + H2SO4 → 2HCl + Na2SO4
3. Sodium chloride is easily oxidized to liberate free chlorine.
Heating with Manganese dioxide and concentrated sulphuric acid produces
chlorine.
2NaCl + MnO2 + 2H2SO4 → MnSO4 + Na2SO4 + 2H2O + Cl2 
Oxidation of solution of sodium chloride is used to prepare sodium
hydroxide and chlorine.
Assay :
Modified Volhard’s Method :
An accurately weighed quantity is dissolved in water and a known excess of N / 10
silver nitrate solution, concentrated nitric acid and nitrobenzene are added. It is titrated
against N/10 ammonium thiocyanate solution using cerric ammonium sulphate as
indicator.
Sodium chloride is precipitated as silver chloride by the addition of silver nitrate.
Nitrobenzene is added to coagulate the silver chloride so that it will not interfere with the
titration of the excess of silver nitrate with N/10 ammonium thiocyanate, since silver
chloride reacts slowly with ammonium thiocyante.
AgNO3 + NaCl → AgCl  + NaNO3
AgNO3 + NH4SCN → AgSCN + NH4NO3
Storage
It should be stored in a well closed container.
Chemical Incompatibility
When sodium chloride is treated with soluble salt of silver, mercurous or lead, the
corresponding metallic chloride is precipitated.
AgNO3 + NaCl → AgCl  + NaNO3
Uses
43
It produces effect of both chloride ion and sodium ion. Deficiency of sodium
chloride leads to “salt Hunger” as indicated by metabolic disturbances etc.
1. It is used as fluid and electrolyte replenisher.
2. It maintains normal osmotic pressure of blood.
3. It is used as saline diuretics.
4. It is used in the formulations of I.V. fluids to maintain the iso-osmotic with blood
serum.
Official Preparations of Sodium Chloride
1. Sodium chloride injection, U.S.P.
Contains 0.9% NaCl.
Use : Fluid and Electrolyte replenisher, irrigation solution.
Dose : I.V. infusion 1 Litre.
2. Bacteriostatic sodium chloride injection, U.S.P
Contains 0.9% NaCl.
Use : Sterile vehicle
3. Sodium chloride solution, U.S. P
Contains 0.9% NaCl.
Use : Isotonic vehicle.
4. Sodium chloride tablets, U.S.P
Usually 600mg, 1 and 2.25 g tablets are available.
Use : Electrolyte replenisher.
5. Dextrose and sodium chloride injection U.S.P.
Available in different strengths and different volumes.
% Dextrose % NaCl m. eq/lit Available volume (ml)
5 0.11 18.8 250, 500 & 1000
5 0.20 34.2 250, 500 & 1000
5 0.225 38.5 250, 500 & 1000
Use : Fluid, nutrient & electrolyte replenisher.

6. Sodium chloride and dextrose tablets N.F.
Usually 200 mg of sodium chloride and 450 mg of dextrose tablets are available.
7. Mannitol and sodium chloride injection, USP
Different strengths and different volume are available.
44
% % NaCl m. Eq/lit Available volume (ml)
Mannitol
5 0.3 51.3 500 & 1000
10 0.3 51.3 500 & 1000
15 0.45 76.9 150 & 500
20 0.45 76.9 250 & 500
POTASSIUM CHLORIDE (KCl)

Preparation
It may be obtained by separation and purification from its minerals like carnalite
(KCl, MgCl2. 6H2O). On laboratory scale it may be prepared by reacting potassium
carbonate and hydrochloric acid.
K2CO3 + 2HCl → 2KCl + H2O + CO2
Physical Properties
It occurs as colourless elongated, or cubical crystals, or as a white granular powder.
It is odourless, has a saline taste. It is freely soluble in water, that is neutral to litmus. It is
insoluble in alcohol.
Chemical Properties
Potassium chloride reacts with silver nitrate to give silver chloride as precipitate
and potassium nitrate. This property is used to estimate the amount of potassium chloride
in the pharmaceutical preparations.
Assay
A weighed quantity of substance is dissolved in water and titrated against
standardized silver nitrate using potassium chromate as indicator. The end point is
formation of brick red colour.
AgNO3 + KCl → AgCl  + KNO3
Uses
1. Potassium chloride is used as an electrolyte replenisher, along with sodium chloride
and calcium chloride.
2. It is administered orally as solution, elixer or tablets in the case of potassium
deficiency.
3. It is also used in the digitalis poisoning
Official preparations of potassium chloride
1. Potassium chloride injection, BP, USP
45
Available as 1.5g in 10 ml
3 g in 12.5 ml & 20 ml
4.5 & 6g in 30 ml
2. Potassium chloride tablets, USP
Available as enteric-coated tablets containing 300 mg or 1g.
3. Ringers injection, USP
Contains 0.03% KCl
Use : Fluid and electrolyte replenisher
Usual dose : Intravenous infusion, 1 litre
4. Lactated Ringer’s Injection USP
Contains 0.03% KCl.
Use : Systemic alkaliserdose : 1.V. 1 litre
18. PHYSIOLOGICAL ACID – BASE BALANCE
Acids are produced during metabolism, since most metablic reactions occurs only
with in a very narrow pH range (7.35 – 7.42). The body utilizes several efficient buffer
systems.
Three of the major buffer systems.
1. Bicarbonate / carbonic acid (HCO3- / H2CO3) found in plasma and kidneys.
2. Mono Hydrogen Phosphate and Dihydrogen Phosphate (HPO42-/ H2PO4-) found in cells
and kidneys.
3. Red blood cells in the Haemoglobin (Hb) buffer system.
Therefore it is necessary to maintain the pH of the system respectively. If there is
any change in pH due to the diseased condition or physiological change, we must provide
official Acid-or base to balance the required pH.
Electrolytes used in Acid-base-balance
Metabolic acidosis is treated with sodium salt of bicarbonate, lactate, acetate and
rarely citrate. Administration of bicarbonate increases the HCO3- / H2CO3 ratio when there
is a bicarbonate deficit. Lactate, acetate and citrate ions are normal components of
metabolism and will be degrade to carbon dioxide and water by the tricarboxylic acid
cycle.
Metabolic acidosis has been treated with ammonium salt. Its action is in the
kidneys where it prevents the Na+ - H+ exchange.
Official compounds used in Acid-base therapy.
1. Sodium acetate, N.F.
46
2. Potassium acetate N.F.
3. Sodium bicarbonate USP
4. Sodium Citrate, USP
5. Potassium Citrate, NF
6. Sodium Lactate Injection USP
7. Ammonium Chloride USP.
ELECTROLYTES USED TO BALANCE PHYSIOLOGICAL ACIDS AND BASES

SODIUM ACETATE (CH3 COO Na, 3H2O)
Preparation
It is prepared by neutralization of acetic acid with sodium carbonate, (or)
sodium hydroxide.
2CH3COOH + Na2CO3 → 2CH3COONa + CO2 + H2O
CH3COOH + NaOH → CH3 COONa + H2O
Physical Properties
It occurs as colourles, transparent crystals, as granular crystalline powder or
as white flakes. It is odourless or has a faint, acetous odour. It is efflorescent in warm dry
air. It is very soluble in water and is soluble in alcohol.
Buffer Mechanism
It is metabolized to carbon dioxide and then to bicarbonate, can be used as
an effective buffer in metabolic acidosis.
(O)
CH3COO Na Metabolized HCO3-
When acid is added, the pH does not change much because H+ ion of acid, is
captured by bicarbonate ion and to form carbon dioxide and water.
HCO3- + H+ H2O + CO2 
Chemical Properties (from acid)
1. It converts in to sodium carbonate when it is ignited.
2CH3COONa. 3H2O + 4O2 → Na2CO3 + 6H2O + 3CO2
2. It gives deep red colour with ferric chloride due to the formation of ferric acetate.
FeCl3 + 3CH3 COONa (CH3COO)3 Fe + 3 NaCl.
3. It is oxidized to sodium bicarbonate.
4(O)
CH3COONa NaHCO3 + H2O + CO2
Assay: Non-Aqueous Titration
During the assay no water should be contacted. Accurately weighed quantity is
dissolved in glacial acetic acid; a small amount of acetic anhydride is added and allowed
47
to stand for half an hour. It is titrated against standard perchloric acid using 1-naphthol
benzein solution as indicator. The end point is change of colour from blue to dark green.
CH3 COONa + HClO4 → NaClO4
Perchloric Sodium
acid Perchlorate
Storage
Dose: 1.5 g
Uses: 1. Acidic urine is corrected by infusion of sodium acetate.
2. Used as antacid
POTASSIUM ACETATE (CH3COOK)

Preparation
Potassium acetate is prepared by neutralization of potassium carbonate or
potassium bicarbonate by an acetic acid.
2CH3COOH + K2CO3 → 2CH3COOK + CO2 + H2O
CH3COOH + KHCO3 → CH3COOK + CO2 + H2O
Physical Properties
It occurs as colourless, mono clinic crystals, or as white crystalline powder. It has
saline and slightly alkaline taste. It is deliquescent on exposure to moist air.
It is very soluble in water and is freely soluble in alcohol.
Chemical Properties
On heating with high temperature, it decomposes in to potassium carbonate, carbon
dioxide and water.
2CH3COOK + 4O2  K2CO3 + 3H2O + 3CO2 
Incompatibility: It is incompatible with acids, silver, mercury and iron salts.

Assays
An accurately weigh the potassium acetate and heat until it carbonizes and
produces potassium carbonate. Dissolve the residue in excess of standard sulphuric acid.
Some amount of acid neutralizes the potassium carbonate and back titrate remaining
unreacted acid with standard sodium hydroxide using methyl orange indicator until the
colour changes from pink to straw yellow.
2CH3COOK + 4O2 → K2CO3 + 3H2O + 3CO2 
K2CO3 + H2SO4 → K2SO4 + CO2 + H2O
48
Storage
It should be stored in air tight container since the potassium acetate salt is
deliquescent.
Use:
1. It is used as alkaliser.
2. Haemodialysis and peritoneal dialysis.
3. Used in potassium deficiency.
SODIUM BICARBONATE INJECTION

It is official in 1P 1966 and USP XVIII sodium bicarbonate injection USP XVIII is
a sterile solution available in different strengths and volumes. For intravenous infusion,
500 ml of a 1.4% w/v solution is available. It is also available as 1% in 20 ml; 5% in 500
ml; 1.4% in 500 ml, 7.5% in 50 ml; and 8.4% in 30ml.
Sodium bicarbonate injection 1P 1966 is a sterile solution of 1.4% w/v of sodium
bicarbonate in water for injection.
Uses
1. Drug of choice for systemic acidosis.
2. Used in the treatment of methyl alcohol poisoning.
SODIUM CITRATE
This is prepared by mixing hot solution of citric acid and sodium carbonate in the
calculated proportions and crystallizing the product.
CH2 – COOH CH2 – COONa + 3 CO2 + 3H2O
2 CH2 (OH)COOH + 3 Na2CO3 → 2 CH(OH) – COONa
CH2 – COOH CH2 COONa
Physical Properties
It occurs as colourless crystals, or as white crystalline powder. It may be either
anhydrous or contain, two moles of water of hydration. It is freely soluble in water and
very soluble in boiling water, it is insoluble in alcohol. The salt should be neutral to
phenolphthalein.
Chemical Properties
On heating it is decomposes to sodium carbonate carbon dioxide and water.
CH2- COONa
2 CH (OH) – COONa → 3Na2CO3 + 3CO2 + 3H2O
CH2 - COONa
49
Assay
A weighed quantity of substance is heated to get charred residue. Dissolve
and heat the residue in water and measured volume of hydrochloric acid, filter the residue,
excess of acid in the combined filtrate is treated with standard sodium hydroxide using
methyl orange as indicator.
CH2COONa
CH (OH) COONa. 2H2O → 3Na2CO3 + 3CO2 + 3H2O
CH2 COONa
3 Na2CO3 is equivalent to 6 HCl.
Uses
1. Used as an anticoagulant for whole blood.
2. Used for chelation of cations. (e.g.) Ferrous ions.
3. Used as buffering agent.
4. Systemic alkaliser.
POTASSIUM CITRATE
Preparation
This is prepared in a similar way to sodium citrate from potassium carbonate
and citric acid.
CH2 – COOH CH2 – COOK
CH (OH)COOH + 3 K2CO3 → 2 CH(OH). COOK + 3CO2 + 3H2O
CH2 – COOH CH2- COOK
Physical Properties
It occurs as transparent crystals or as a white granular powder, it is odourless, has a
cooling saline taste and is deliquescent when exposed to moist air. It is freely soluble in
water and almost insoluble in alcohol.
Incompatibility
It is incompatible with calcium and strontium salts.
Assay
Ignition and titration of the alkaline residue, as described under sodium citrate.
CH2 COOK
2 CH (OH). COOK, H2O → 3K2CO3
CH2 COOK
Uses
1. Used as systemic alkaliser
2. Expectonent
50
SODIUM LACTATE INJECTION
Sodium lactate injection USP is a sterile solution of lactic acid in water for
injection which has been neutralized with sodium hydroxide. It must be between pH 6.0
and 7.3. It is available as 1/6 molar solution in 1, 50, 250 and 1000-ml containers as fluid
and electrolyte replenisher used in the treatment of metabolic acidosis.
Sodium lactate injection BP is administered by intravenous route and it is a sterile
solution containing 1.85% w/v of sodium lactate in water for injection. It may be prepared
from sodium lactate solution or from lactic acid. Content of sodium lactate, C3H5NaO3
1.75 to 1.95% w/v.
The label states that
1. Solution containing visible particles should not be used.
2. The intravenous infusion is one sixth molar and contains, in one litre,
approximately 167 millimoles of sodium ions and bicarbonate ions (as lactate).
Uses
1. Fluid and electrolyte replenisher.
2. For the treatment of metabolic acidosis.
AMMONIUM CHLORIDE (NH4Cl)

Preparation
It is easily prepared by neutralizing hydrochloric acid with ammonia solution and
evaporating the solution to dryness. Unreacted excess of either ammonia or hydrogen
chloride will voltalize.
NH4OH + HCl → NH4Cl +H2O
It can be purified by crystallization or by sublimation.
Physical Properties
It occurs as colourless crystals or as a white fine or coarse crystalline powder which
has a cool saline taste and is some what hygroscopic. It is freely soluble in water and in
glycerin and even more soluble in boiling water it is sparingly soluble in alcohol.
Chemical Properties
Ammonium chloride volatilizes on heating and the vapour dissociates into
ammonia and hydrogen chloride.
NH4Cl HCl + NH3

Assay
An accurately weighed amount of the ammonium chloride is dissolved in
water and treated with formaldehyde solution. So that entire ammonium chloride liberates
equivalent amount of hydrogen chloride, which is then titrated with standard sodium
hydroxide solution.
51
NH4Cl + H2O → NH4OH + HCl
4NH4OH + 6 HCHO → C6H12N4 + 10H2O
Hexamine
HCl + NaOH → NaCl + H2O
Previously it was assayed by Volhard’s method as described under sodium
chloride.
Uses :
1. It is used as expectorent in cough mixture.
2. It is also used as a substitute for sodium chloride as an electrolyte replanisher.
3. Used as systemic acidifier.
AMMONIUM CHLORIDE INJECTION

Ammonium chloride injection USP is a sterile solution of ammonium chloride in
water for injection. It contains not less than 95% and not more than 105% of labeled
amount of NH4Cl, Hydrochloric acid is added to adjust the pH.
Storage
Preserve in single dose – or in multi dose containers, preferably of Type I or Type II glass.
COMBINATION OF ORAL ELECTROLYTE POWDERS AND SOLUTIONS
(FOR INJECTION)
These combination products can be divided into two groups: 1) Fluid

maintenance and 2) Electrolyte replacement. Maintenance therapy with intravenous fluids
is intended to supply normal requirements of water and electrolytes to patients who can
not take them orally. All maintenance solutions must contain at least 5% dextrose.
Replacement therapy is needed when there is heavy loss of water and
electrolytes as in prolonged fever, severe vomiting and diarrhoea. Usually there are two
types of solutions used in replacement therapy : a solution for rapid initial replacement and
a solution for subsequent replacement.
Official combination of electrolyte infusions.
Ringer’s Injection, U.S.P.
Sodium Chloride 8.6 g

Potassium chloride 0.3 g
Calcium chloride (as dihydrate) 0.33 g
52
Water for injection q.s. to 1000 ml
It is usually available in 500 ml and 1000 ml injections.
Lactated Ringer’s Injection, USP

Sodium chloride - 600 mg
Sodium lactate - 600 mg
Sodium lactate - 310 mg
Potassium chloride - 30 mg
Calcium chloride - 20mg
(as dihydrate)
Water for injection q.s. to 100 ml
It is usually available as 150, 250, 500 and 1000 ml injections.
Oral Rehydration Salts I.P.
Oral rehydration salts are dry, homogeneously mixed powder containing

dextrose, sodium chloride, potassium chloride and either sodium bicarbonate or sodium
citrate for use in oral rehydration therapy after being dissolved in requisite amount of
water.
Oral rehydration salts-A (ORS-A) commonly used in India for treatment of

non-choleraic diarrhoea oral-rehydration salts-citrates (ORS-citrate) recommended by the
Diarrhoeal disease control programme of the World Health Organization (WHO) and the
United Nations Children’s Funds (UNICEF), in amounts to be dissolved in the stated
amounts of water.
53
The composition of the two formulations are described below in terms of the
amounting, to be dissolved in sufficient water to produce 1000 ml.
Formula g / litre
ORS-A ORS-Citrate
Sodium Chloride 1.25 3.5
Potassium Chloride 1.5 1.5
Sodium citrate 2.9 2.9
Anhydrous Dextrose 27.0 20.0
Dextrose Monohydrate 29.7 22.0
INORGANIC OFFICIAL COMPOUNDS OF IRON, IODINE AND CALCIUM:
FERROUS SULPHATE AND CALCIUM GLUCONATE.
Official Compounds
Official compounds are the drugs or a dosage forms of a drug for which a
monograph (systematic informations) is given in the pharmacopoeia published by the
respective governments. (In India-Indian Pharmacopoeia).
Official Compounds of Iron

1. Ferrous fumarate I.P.
2. Ferrous gluconate I.P.
3. Ferrous Sulphate I.P.
4. Dried Ferrous Sulphate I.P.
5. Iron and Ammonium Citrate I.P.
6. Iron Dextran Injection, U.S.P.
54
7. Iron Sorbitex Injection, USP.
Ferrous Sulphate (Fe SO4. 7H2O)
Preparation
It is prepared by dissolving a slight excess of scrap iron in dilute sulphuric
acid and concentrating to get green crystals of ferrous sulphate
Fe + H2So4 → FeSO4 + H2 
Physical Properties
This is crystalline ferrous sulphate containing seven molecules of water of
hydration. It occurs in the form of transparent, green crystals or as a pale bluish – green
crystalline powder. It is odourless and has a metallic, astringent taste. It effloresces in dry
air. When exposed to moist air, it is slowly oxidized and is coated with a brown, basic
ferric sulphate. When this takes place, the sample should not be used.
Solubility
It is soluble in water and practically in soluble in alcohol.
Chemical Properties
Ferrous sulphates combine with alkali sulphates to form double salts. One
such products is ferrous ammonium sulphate, FeSO4 (NH4)2 SO4.6H2O, it is used in
analytical chemistry.
Assay
An accurately weighed quantity is dissolved in dilute sulphuric acid and

titrated against N/10 ceric ammonium sulphate using ferroin sulphate as indicator.
Ferrous sulphate is reducing agent, which is oxidized to ferric sulphate by

the ceric ammonium sulphate. The indicator ferroin sulphate solution is ortho-
phenanthroline ferrous complex. The end point is the appearance of a light blue colour.
Storage
Stored in a well-closed container.
55
Use
1. Haematinic
2. Used for Anaemia due to iron deficiency.
Official Compounds of Calcium

1. Calcium amino salicylate
2. Calcium carbonate
3. Calcium chloride
4. Calcium gluconate
5. Calcium hydroxide
6. Calcium lactate
7. Calcium levulinate
8. Calcium pantothenate
9. Dibasic Calcium Phosphate
10. Tribasic calcium phosphate
Calcium gluconate (OHCH2 [CHOH]4 COO)2 Ca. H2O
Physical Properties
It occurs as a white, crystalline or granular powder. It is tasteless and
odourless it is stable in air. It loses its water of crystallization with decomposition above
100C. It is soluble in 1 in 30 in cold water and 1 in 50 in boiling water and insoluble in
ethyl alcohol, chloroform and solvent ether.
Chemical Properties
To the aqueous solution of calcium gloconate, ferric chloride solution is

added, A yellow colour is produced.
56
Assay
This is a complexometric assay. A known quantity is dissolved in warm

water and a definite quantity of 0.05 M magnesium sulphate solution and strong Ammonia
– Ammonium chloride solution are added. The mixture is titrated against M/20 disodium
ethylene diamine tetra acetate (EDTA) using Moderant black mixture as indicator. The
end point is change of colour from red to blue. A blank determination should be done
omitting the sample.
The buffer of strong ammonia-ammonium chloride solution is added to raise

and maintain the pH at 10, because at this pH only complexation takes place. The
magnesium salts are added to get sharp end point.
NaOOCH2C CH2COONa
Ca++ + N – CH2 – CH2 – N →
HOOCH2C CH2COOH
NaOOCH2C CH2COONa
N – CH2 – CH2 - N
H2C Ca CH2
C C
O O O O
Storage :
Store in a well closed container.
Use
1. Used as electrolyte replenisher
2. It is administered in the form of tablets or injections incase of calcium deficiency.
Official compounds of Iodine

57
1. Iodine I.P.
2. Potassium Iodide I.P.
3. Sodium Iodide I.P.
4. Sodium Iodide I 125 USP
5. Sodium Iodide I 131 USP.
RADIO PHARMACEUTICALS AND CONTRAST MEDIA
Atomic Structure:
All the matters are made up of atoms. Bonding of atoms of same or different
elements forms the molecule. An atom consist of nucleus and electrons revolving around
the nucleus in different orbitals. The electrons have negative charge. The nucleus contains
positively charged protons and neutral neutrons. The protons and neutrons have definite
mass. An atom consist of an equal number of protons and electrons, then the atom is
electrically neutral, for that atom the total electrical charge is zero.
Atomic Number:
Number of protons (Z) which is equal to the number of electrons in a neutral
atom.
Mass Number (A):
Total number of protons (Z) and neutrons (N).
 Mass number (A) = Z + N
To represent an atom with all the above details it is written as below:
A where, X = Symbol of element
X A = Mass number
Z Z = Atomic number
Examples: 12 59 7 14
C CO Li N
6 27 3 7
Isotopes
Atoms having the same atomic number but different mass numbers.
Examples: 12 13 16 17 18 54 56
C C ; O O O; Fe and Fe
6 6 8 8 8 26 26
58
Ferrous 54 and Ferrous 56 both have the same atomic number of 26, but the mass
number is different 54 and 56. This is due to the difference in the number of neutrons.
54
Fe contains (54-26) 28 neutrons
56
Fe contains (56-26) 26 neutrons.
Therefore, 56Fe is isotope of 54Fe.
Isobars:
Atoms having the same mass number but different atomic number are called
isobars.
Examples: 197 197 60 60
Hg Au ; Co Ni
80 79 27 28
Radio Activity:
Some elements are able to emit certain invisible rays which affect a photographic
plate in the dark. These rays are also able to penetrate solid matter, ionise gases and
produce luminescence in substance like zinc sulphate and barium salts. Such substances
are called radio-active and the property is called radio-activity. Naturally, radio-active
elements are uranium, radium, thorium etc.
A nucleus of an atom having same number of neutrons and protons are stable that is
neutron to proton ratio is 1:1 and these atoms does not emit any type of radiation. A
nucleus in which the number of neutron is different than the number of protons that is
neutron to proton ratio is not equal and these atoms emits radiation. While emitting
radiation the parent atom undergoes transformation and produces another daughter atom,
and emitted radiation may be alpha rays (-particle) Beeta rays (-particles) and gamma
radiation.
The Properties of radiations
Radiations emitted by atoms are of two types. They are particulate and
electromagnetic. The most important particulate radiations are the alpha () and beta ()
radiations emitted by disintegrating atoms of radio nuclides.
Alpha Particles ()
1. The alpha particles are positively charged.
2. When radio active element emits alpha particles the resulting nucleus of the atom will
have two positive charges less than the original nucleus. It can be illustrated by the
decay of Radium nucleus to give randon nucleus.
226 222 4
Ra → Rn + He
88 86 2
3. They are very much heavier than  - particles.
4. They have less penetrating power.
5. They have very great ionising powers (high specific ionisation).
59
Beta Particles ()
1. Beta particles are negatively charged.
2. They are heavier than  - particles.
3. They have more penetrating power than  - particles as it can penetrate tissues.
4. They are relatively less ionizing powers than  - particles.
5.  - particles sometimes referred as negatrons which are emitted by unstable nuclei in
which the neutron / proton ratio exceeds the stability limit and in such case neutrons
are transformed protons with beta emission.
1 1
N→ P + -
0 1
Gamma Radiations
1. Gamma radiations are electromagnetic radiation similar to light and X-rays but of
higher energy.
2. These radiations do not have any charge and thus are not affected by electric or
magnetic field.
3. They are very short wave length resembling X-rays and travel with the velocity of
light.
4. They have poor ionizing power and very high penetrating power.
5. They can interact with molecules and atoms in specific media and can produce ions
and free radicals.
Biological Effects of Radiations
1. These chemical species can alter the local pH resulting in the production of other
toxic compounds.
2. Life period may be shortening if a person is exposed to a smaller dose of radiation.
3. It may cause sterility and it also may induce cancer.
4. These radiations may alter the DNA leading to destruction of tissues or organs.
5. Radiation may cause anaemia and decreases the blood cells.
Measurement of Radioactivity
The different kinds of particles and rays produced during the disintegration of a
radioactive material leave number of ions along their paths. These ions are normally
detected and measured. Measurement of radioactivity is based on the following properties
of radiation.
1. Radiation to cause ionization of gases.
2. Radiation to cause flash of light.
3. Radiation to cause chemical change.
The different devices used to measure the radiations are
60
1. Ionization chamber
2. Proportional counters
3. The Geiger Muller counter
4. Scintillation counters
5. Semi conductor detectors
6. Photographic plate method
Geiger-Muller Counter
This is the most popular radiation detector because, it does not need a well-
stabilized high voltage supply. It is most frequently used for detecting  - particles.
It contains a central wire anode, usually made of tungsten, and a cathode, silver, is
coated in the innerside of the cylinder. The space between the electrodes (anode and
cathode) contains a gas, which is usually an argon at a pressure of a few mm of mercury.
The chamber is filled with argon gas and if the radiation is passed through the mica
window of the chamber, the gas is ionized and there is a flow of current each particles of
radiation causes a brief flow or pulses of current which is recorded by a device known as
scalar which shows the total number of pulses.
Source of voltage
+ + To Amplifier
−
−
Mica
+ − Anode
window +
Cathode Argon gas
Fig.1. Geiger – Muller Counter

Radio Isotopes
The isotopes which limits radiations are called radio isotopes. There are several
radio isotopes have medicinal values.
Biological Half Life (t½ )
It is defined as the time in which the amount of radio nuclide decays (decomposes)
to half of its initial value. It is related to decay constant .
61
0.693
t ½ = ⎯⎯⎯

General Storage and Precautions of Radio Active Compounds
1. Great care must be taken in the use and storage of radio active materials.
2. Special shielding is necessary for protecting ,  and  radiations.
3. For protecting  and  radiations, requires thick glass containers or Perspex
containers are necessary.
4. For protection  radiations requires havier lead shielding or containers are
necessary.
5. Areas where radioactive materials are stored or used should be monitored, that is
tested for radioactivity regularly.
6. Radioactive materials should never be touched with hand, it should be handled by
means of forceps or suitable instruments.
7. Smoking, drinking or eating activities are to be avoided in the laboratory where the
radioactive materials are handled.
8. Sufficient protective clothing or shielding must be used while handling the
materials.
9. Radioactive materials should be kept in suitable labeled containers and kept
preferably in a remote corner.
10. There should be proper disposal of radioactive materials.
Official preparations of Radio Pharmaceuticals and their Applications

Radioisotopes are used in medicines in two different ways. They are 1) sources of
radiation in therapy 2) Radioactive tracers are used for diagnostic purposes.
The therapeutic uses of radioisotope depend mainly on their ability to ionize atoms.
Radioactive tracers are used to find out the diseased portion of the organ and the parts of
the system.
Sodium Chromate (Cr51) Solution
24
It is radioactive chromium51 ion in the form of Na2Cr51O4. It has a half life of 26.5
days. It is used to study red cell mass, volume and its survival time and for scanning the
spleen.
Sodium Iodide (I131) Capsules
54
and Solution
It is a radioactive isotope of iodine 131 in the form of sodium iodide 131. It emits 
and  rays. It has a biological half life of 8 days. It is used as a diagnostic and therapeutic
agent in thyroid conditions and Myxedema. It is also used to determine the plasma volume
and simultaneous use with sodium chromate Cr-51 and Ferrous citrate Fe-59 to determine
total blood volumes is also possible.
62
Cobalt 57 and 60
Cyanocobalamin Co 57 capsules and solutions.
Cyano cobalamin Co 60 capsules and solutions.
Biological half life of Co 57 is 270 days and Co 60 is 5.27 years, emitting both beta
and gamma radiation. Cobalt 60 is used in therapy where X-rays are used. It is also used
for the sterilization of surgical materials and dressings by its gamma radiation. Cobalt 57
is used in the diagnosis of pernicious anaemia.
Sodium Phosphate P 32 Solution
It emits beta radiations, its half life is 14.3 days, it is used in both diagnosis and
treatment of various neoplastic diseases. Phosphate is utilized in cell metabolism. Primary
diagnostic use of phosphate p-32 is in the localization of intra ocular tumors and cerebral
tumors.
Gold Au 198 Injection
It produces both  and  radiation, its half life is 2.7 days. It is used for therapeutic
purpose. It is administered intracavitary injection in to the pleural and peritoneal cavities
as an acid in the management of plural effusion and accumulation of serous fluid in the
peritoneal cavity.
Sodium Iodide I 125 Solution
It produces both X-rays (K-capture) and -rays, its half life is 60 days. It is used in
the treatment of Hyper thyroidism.
Calcium (Ca 44 and Ca 45)
Radioactive calcium is used to study bone structure and in the treatment of
carcinoma of bone.
Carbon 14 (C 14)
It is most widely used in various studies for eg. in metabolism of carbohydrate and
fats, drug excretion, decomposition of pharmaceutical products.
Iron 59, 55 (Fe 59 and Fe 55)

It emits both beta particles and high energy gamma rays. The half life of Iron 59 is
45 days. It is used in research studies about utilization and absorption of iron salts, it is
also used to measure red blood cell life span.
Hydrogen (H2 and H3)
The deuterium (H2) and tritium (H3) are useful to determine total body water.
Sodium (Na 22 and Na 24)
It is used in estimation of extra cellular fluid, blood circulation rate, studies in cell
permeability, excretion and distribution of water.
63
RADIO OPAQUE CONTRAST MEDIA
Radio opaque substances are those compounds (both inorganic and organic) that
have the property of casing a shadow on X-ray films. These substances have the ability to
stop the passage of X-rays and these are the elements of high atomic numbers.
Inorganic compounds like barium sulphate and some bismuth compounds thus are
useful as radio-opaque contrast media for diagnostic uses. A large number of organic
iodinated compounds are also used as radio opaque contrast media.
These compounds are useful for examination of gasterointestinal tract, kidney,
liver, gallbladder and blood vessels of heart, brancheal tract and that of urethra, vagina etc.
Barium Sulphate (BaSO4)
Preparation
It is prepared by precipitating barium ions from cold dilute solutions of barium salt
with dilute sulphuric acid.
Ba(OH)2 + H2SO4 → BaSO4  + 2H2O
BaCl2 + H2SO4 → BaSO4  + 2HCl
Physical Properties
It is a fine, white, odourless, tasteless and bulky powder that is free from grittiness.
The salt is insoluble in water, organic solvents, and dilute acids and alkalies it is soluble in
concentrated sulphuric acid.
Assay
It is assayed by gravimetrically. First step involves conversion of barium sulphate
into barium carbonate by adding sodium or potassium carbonate and heating to 1000C.
Then the residue is extracted with hydrochloric acid. The barium in the extract is
precipitated as barium chromate by treating with potassium dichromate in alkaline
medium. The precipitate is washed, dried to get constant weight and weighed.
Uses
It is used as a contrast medium for X-ray examination of the alimentary tract.
It is administered orally by enema for examination of the colon.
Dose : 200-400 g oral
64
QUALITY CONTROL OF DRUGS AND PHARMACEUTICALS
Quality assurance plays a central role in determining the safety and efficacy of
medicines. Highly specific and sensitive analytical method holds the key to the design,
development, standardization and quality control of medicinal products.
Total quality control will include all those aspects starting with the procurement of
raw materials to the finished products available at the drug stores and till it is consumed by
the patient. Thus it will include not only the parameters of Good Manufacturing Practice
(GMP) but also to the storage, handling and preserving the sample till ultimate use.
The major areas of quality control include:
1. Good quality and nature
2. Physically and chemically pure
3. It contains the amount of ingredients as stated in the label.
4. It is to be effective after administration
5. It retains quality in terms of shelf-life (or) stability.
The importance of quality control is to test a drug for stated quality and quantity. In
order to maintain both the above parameters of qualitative identification and quantitative
determinations. The procedures and standards are prescribed in the pharmacopoeias
published by the respective government of most of all countries.
Methods used for Quality Control
Various tests and procedures for analysis including finding and determining
impurities are given in official pharmacopoeias.
In the quantitative analysis, depending upon the characteristics of drugs and its
formulation various analytical methods are followed. These includes,
Physiochemical methods, includes determination of specific gravity, density,
viscosity, surface tension, refractive index, optical rotation, and all the types of volumetric
analysis.
For determining physiochemical properties, use of instruments like potentiometer,
conductometer, polarography, colourimeter, spectrophotometer, fluorimeter, flame
photometer, are necessary.
Other methods for quantitative determination will include the separation technique
like chromatographic, (HPLC, HPTLC, TLC etc), determination by weight like
gravimetric and precipitation method.
Apart from the routine qualitative and quantitative analysis, pharmaceutical
products also evaluated for their quality. They are tests like disintegration, dissolution,
hardness, friability, weight variation, content uniformity, for unit solid dosage forms like
tablets and capsules. Bio availability studies, pharmacokinetic studies biological assays
(bio assays) and microbiological studies are also carried out.
65
Errors in Pharmaceutical Analysis
In pharmaceutical analysis, ultimate result of analysis is important from accuracy
and reliability point of view. The term accuracy refer to the agreement of experimental
result with the true value and it is usually expressed in terms of errors.
Precision is defined as the degree of agreement between various results of the same
quantity that is the reproducibility of a result.
Sources of Errors
There are two main classes of errors which affect the accuracy and precision of a
measured quantity.
1. Determinate Errors: These are determinable, and can be either avoided or corrected.
The error may be constant as in the case of
❖ Weighing with uncalibrated weights,
❖ Measuring a volume using uncalibrated burette or
pipette.
These are also called as systematic errors. They arise due to
a) Instrumental errors - by using uncalibrated equipment
b) Operative errors - by person operating or doing analysis (personal error)
c) Chemical error - due to impurities in chemicals solvents and reagents.
d) Errors in methodology: error due to unvalidated method:
e) Errors of above categories are usually detectable and can be eliminated to the large
extent.
2. Indeterminate Errors
These are often called accidental or random errors. They are found by small
differences in series of measurements made by the same analyst under identical
conditions. They can not be predicted and hence cannot be eliminated.
Sources of Impurities in Pharmaceuticals
The substances used in pharmaceutical field should be almost pure. The purity of
the substances varies with different factors such as, their methods of manufacture, types of
their purification etc. Impurity means presence of other materials than drug or presence of
unwanted foreign particle other than active drugs. The impurities may be toxic or non-
toxic even if it is non-toxic it may be used intentionally as adulterant to increase the
weight of the active ingredient. Non toxic impurities also reduce the activity of the drug,
so that one must avoid impurities in pharmaceuticals, cannot eliminate all the impurities.
The official pharmacopoeias prescribe limits for particular impurities like sulphate,
chloride, iron, heavy metals and arsenic.
Some factors which are responsible for pharmaceutical impurities are discussed
below:
1. Raw Material Employed in Manufacture
The raw materials, from which these are prepared, often contain impurities. It is
therefore necessary to employ pure chemicals and substances as raw materials.
E.g.
1. Presence of tin, lead, silver, copper, cobalt and gold in bismuth salts.
66
2. Rock salt contains small amounts of calcium sulphate and magnesium chloride. So
sodium chloride prepared from rock salt will almost contains trace of calcium and
magnesium compounds as impurity.
2. Method used in Manufacture
Some impurities get incorporated into the materials during the manufacturing
process.
a) Intermediates
For certain drugs a multiple-step-synthesis procedure is involved, which produces
intermediate compounds. The purification of the intermediates is essential, otherwise
impurities present in the intermediates will get into the final product.
(e.g.) Potassium iodide is prepared by treating potassium hydroxide with iodine.
The intermediate potassium iodate formed is reduced to iodide. If the iodide is not reduced
completely, the final product potassium iodide, will contain traces of potassium iodate as
impurity.
b) Reagents used in the Process

The final product may contain unreacted reagents as impurities, if it is not washed
properly.
e.g.,
1. Lead as an impurity may result from the sulphuric acid used as reagent.
2. Soluble alkali may be an impurity in calcium carbonate if the calcium carbonate is
made by reacting calcium chloride and sodium carbonate and not properly washed.
c) Solvents
Water is a common solvent in large scale manufacturing of pharmaceuticals. This
can give rise to trace impurities such as sodium, calcium, magnesium, carbonate, chloride
and sulphate ions. These impurities can be avoided by using purified water.
d) Catalyst
Generally, catalysts are used to induce the reaction. There may be possibility of
incorporation of traces of catalyst in the final products.
e.g.,
1. Presence of palladium catalyst in phenanthrene.
2. Presence of copper chloride in the synthesis of phenol.
e) The Reaction Vessels
The vessels used in manufacturing process are made of metals like copper, iron,
aluminium, zinc, tin though these days many of these metals are replaced by stainless
steel. Traces of these metal ions may contaminate the final products.
Glass vessels may give rise to traces of alkali to the product.
Metal particles of aluminium containers may contaminate the products like
ointments and pastes stored in it.
f) Atmospheric Contaminants
67
Dust, sulphur dioxide, hydrogen sulphide, arsenic and water vapour from
atmosphere may affect a drug. Presence of carbon dioxide, carbon monoxide and
hydrogen cyanide from environment also affect the drug products if it is not manufactured
under controlled conditions.
g) Decomposition of the Product during Storage
Many drugs undergo changes due to improper storage conditions. If the drugs are
not stored properly, they will expire before the date of expiry. These decomposition may
be due to light, water vapour, air, carbon dioxide and metallic ions.
e.g,
1. Ferrous sulphate slowly changed into insoluble ferric oxide by air and moisture.
2. Solutions of potassium hydroxide absorbs carbon dioxide on exposure to air.
3. Bismuth carbonate turns black on exposure to sunlight for a long period.
Therefore, the products which are prove to decompose due to environmental factors
should be stored in well-closed containers. If the products are prone to decompose due to
light should be stored in light-resistant containers like amber colour bottles for liquids and
opaque packaging for solid dosage forms.
Deliberate Adultration
A drug may be deliberately adulterated with cheaper and inert materials for the
sake of more profit. This will reduce the potency of the active ingredient present in the
formulation quantitatively. These practices are prevented by central and state drug control
departments.
LIMIT TESTS
Limit tests are quantitative tests which are designed to detect and limit small
quantities of impurities present in the substance. All the limit tests that are prescribed in
the pharmacopoeias are based on the comparison of standard turbidity or colour with that
of the sample under test. For the preparation of standard turbidity or colour the
pharmacopoeias prescribe the limit of particular impurities for particular substances and it
varies for different compounds. Usually the limits are prescribed in parts per million
(PPM). The amount of test samples to be taken is mentioned in the individual monograph
of the pharmacopoeias.
Limit Test for Chlorides
A solution of the substance is acidified with nitric acid, diluted to definite volume
and treated with silver nitrate and the opalescence so produced is compared with that of
standard opalescence containing known amount of sodium chloride solution.
Cl- + AgNO3 → AgCl + NO3-
Presence of nitric acid prevents the precipitation caused by silver carbonate or
silver hydroxide which may result due to alkaline impurities in the solution.
2. Limit Test for Sulphate
68
It depends upon the precipitation of the sulphate with barium chloride in the
presence of hydrochloric acid, ethyl alcohol and traces of potassium sulphate.
The turbidity produced is compared with that of turbidity produced by addition of
the above reagents to a standard solution containing a definite quantity of potassium
sulphate.
SO4− − + BaCl2 → BaSO4  + 2Cl−
The potassium sulphate increases the sensitivity of the test by giving ionic
concentrations in the reagent which just exceed the solubility product of barium sulphate.
Presence of alcohol helps to prevent super saturation. Hydrochloric acid is added to
prevent precipitation due to barium carbonate which is also sparingly soluble in water.
3) Limit Test for Iron
Specified amount of the drug is dissolved in water and treated with citric acid and
thioglycollic acid. It is made alkaline with dilute ammonia solution. The purple colour
produced is compared with that of standard ferric ammonium sulphate treated in the same
way as the test solution.
S – CH2 – COOH
2 Fe+++ + 2HS – CH2COOH → | + 2Fe++ + 2H+
Ferric ion Thioglycollic acid S – CH2 – COOH
CH2 – COO SH
Fe++ + 2HS – CH2COOH → + 2H+
Ferrous ion Thioglycollic acid Fe
HS OOC – CH2
Ferrous Thioglycollate complex

(purple colour)
Ferric ion is reduced to ferrous ion by the thioglycolic acid. Citric acid is added to prevent
precipitation of the iron by the ammonia (citric acid forms a soluble complex). Ammonia
is added to make alkaline the solution, and the purple colour is stable in alkaline medium.
Purple colour is due to the formation of co-ordination compound, ferrous thioglycollate.
4. Limit Test for Heavy Metals
All metals like Copper, Bismuth, Lead, Mercury, Arsenic, Antimony, Silver, etc
(except alkali metals and alkaline earth metals) are coloured by sulphide ions (H2S or
Na2S) under specified conditions. Depends upon the quantity of the metal the colour varies
from brown to black.
69
There are three methods are prescribed in I.P to determine the presence of heavy
metals.
Method A and B are carried out in acid conditions with hydrogen sulphide reagent
and method C involves alkaline medium with the use of sodium sulphide reagent.
Method A
A solution of substance is adjusted to a pH 3 to 4 (by adding ammonia (or) acetic
acid) and hydrogen sulphide reagent is mixed with this and comparison of black colour
produced with a standard colour containing a known amount of lead.
Method B (For Organic Compounds)
The substance is ignited well in presence of conc. sulphuric acid and treated with
mixture of nitric and sulphuric acids. The resulting solution is digested with dilute
hydrochloric acid. Then extracted with hot water and proceeded as in method A.
Pb++ + H2S → PbS + 2 H+
Method C
The solution of the substance is treated with sodium hydroxide solution and sodium
sulphide reagent. Then it is compared with that a standard colour.
Pb++ + Na2S → PbS + 2Na+
5. Limit Test for Arsenic
In this test arsenic impurities if at all present is converted in to arsine gas (ASH3)
which when contact with a mercuric chloride paper produces yellow stain. The intensity of
the stain is proportional to the amount of arsenic present. A standard stain produced from a
definite amount of arsenic is used for comparison.
Apparatus used for arsenic limit test is called Gutzeit apparatus.
A drug solution is prepared and placed in wide monthed bottle, potassium iodide,
zinc dust, hydrochloric acid, stannous chloride are added into it and the apparatus is set up
as given in the figure 2.
Hydrogen gas is generated in the solution by the presence of stannous chloride,
hydrochloric acid (stannated hydrochloride) and potassium iodide on arsenic free
granulated zinc. Stannous chloride and potassium iodide are acts as a reducing agents so
that any pentavalent arsenic is reduced to the trivalent state. The presence of stannous
chloride and hydrochloric acid ensures rapid reaction between acid and potassium iodide
and produces nascent hydrogen gas.
The reactions are:
Zn + 2HCl → ZnCl2 + 2 [H]+

H3ASO4 + 2 [H] → H3ASO3 + H2O
H3ASO3 +6 [H] → ASH3 + 3H2O
2ASH3 + HgCl2 → Hg (ASH3)2 + 2HCl
70
The arsine gas produced in the bottle escapes through the tube and the lead acetate
impregnated cotton wool kept in the centre of the tube entraps the hydrogen sulphide if
any from the arsine gas. The gas escapes through glass tube and reacts with mercuric
chloride paper kept in the clips and produces yellow stain. The reaction is allowed to
proceed for forty minutes maintained at 40C.
Rubber
bung
Clip
Mercuric
chloride paper
Lead acetate cotton wool
Cork
Wide mouth bottle

Glass tube
.
Drug solution + HCl + Zn +

SnCl2 + KI
Figure 2 : Gutzeit apparatus for limit test for Arsenic
71
ANTIMICROBIALS AND ASTRINGENT
Anti microbial is a broad terminology describing activity against microbes.
Specific terminology gives exact mode of action.
1. Antiseptics are substances that kill or prevent the growth of micro organism. This
is specific for preparation intended to be used for living tissues.
2. Disinfectant is prevent infection by the destruction of pathogenic micro organism.
It is generally used to inanimate objects.
3. Germicide is an agent which kills micro organisms. More specific terminologies
like ‘bactericide’ (against bacteria), ‘fungicide’ (against fungi), virucide (against
virus) denotes exact action.
4. Bacteriostatics is an agent which function by inhibiting the growth of bacteria.
Thus bacteriostatic agents do not kill but stops the growth of bacteria.
Mechanism of Action
Inorganic compounds generally exhibit antimicrobial action by three
different mechanism.
They are 1) Oxidation mechanism
2) Halogenation mechanism
3) Protein precipitation
1. Oxidation Mechanism: This belongs to class of peroxides, peroxy acids, oxygen
liberating like permangante. They act on proteins containing sulph hydryl group
and oxidises free sulphydryl to disulphide bridge and inactivate its function.
2. Halogenation Mechanisms: Compounds which liberates chlorine or hypochlorite
or iodine act by this mechanism. They act on peptide linkages and alter it’s
property. The destruction of specific function of protein results in death of micro
organism.
3. Protein Precipitation: Many cations exhibit protein binding or protein
precipitation. The interaction with protein occurs through polar group of protein
which acts as ligands and metal cation as lewis acid. The complex formed may be
strong chelate leading to inactivation of proteins.
HYDROGEN PEROXIDE (H2O2)

Preparation
It is prepared by adding a paste of barium peroxide in ice cold water to a calculated
quantity of ice cold dilute sulphuric acid. The insoluble barium sulphate is filtered off.
BaO2 + H2SO4 → BaSO4  + H2O2
It is also manufactured by electrolysis process. Electrolysis of sulphuric acid to
peroxy sulphuric acid which is hydrolyzed to give the product. Sulphuric acid is oxidized
to give peroxydisulphuric acid (H2S2O8)
72
Oxidation
2H2SO4 (O) H2S2O8 + H2 
Hydrolysis (H2O)
H2S2O8 H2SO5 + H2SO4
Peroxy sulphuric acid
H2SO5 + H2O H2O2 + H2SO4

Properties
Hydrogen peroxide solution is a colourless liquid with slightly acidic taste. The
solution is decompases in contact with oxidisable matter, reducing agent, when made
alkaline or even on standing.
2H2O2 → 2H2O + O2 
The solution is stabilized by the addition of small amount of acid and adjusting the
pH between 2 and 3. Polyvalent metal ions catalyse decomposition of hydrogen peroxide
and complexing agent prevent it by acting as stabilizer.
Hydrogen peroxide acts as oxidizing or reducing agent depending upon the
chemical environment.
In oxidation reaction (in acidic medium) it accepts two electrons.
H2O2 + 2H+ + 2e- → 2H2O
In reduction – release of two electrons.
Decolourisation of permanganate solution.
5H2O2 + 2KMnO4 + 3H2SO4 → K2SO4 + 2MnSO4 + 8H2O + 5O2 
Assay
It is estimated by titration with potassium permanganate in presence of 4 N
sulphuric acid. Potassium permanganate is reduced to manganese sulphate. This
determination depends on mutual oxidation – reduction as expressed by following
equations.
2KMnO4 + 3H2SO4 → K2SO4 + 2MnSO4 + 3H2O + 5(O)
H2O2 + (O) → H2O + O2
Hydrogen peroxide is oxidized to oxygen by nascent oxygen produced from the reaction
between potassium permanganate and dilute sulphuric acid. The appearance of permanent
pale pink colour indicates the end point.
Storage
It should be stored in light resistant container in a cool place.
Use
1. Used as an Antiseptic and topical Anti-infective.
73
2. It arrests the bleeding of wounds.
3. It is used to clean the wounds and ears.
2. POTASSIUM PERMANGANATE (KMnO4)
Preparation
Manganese dioxide is fused with solid potassium hydroxide along with potassium
chlorate, a green mass potassium manganate is obtained. The mass is cooled is extracted
with water and filtered.
3MnO2 + 6KOH + KClO3 → 3K2MnO4 + KCl + 3H2O
The filtrate is treated with carbon dioxide followed by chlorine. By this potassium
manganate is converted into potassium permanganate.
3K2MnO4 + 2 CO2 → 2KMnO4 + MnO2 + 2K2CO3
2K2MnO4 + Cl2 → 2KMnO4 + 2KCl
Potassium permanganate can also be prepared by electrically, by electrolysing warm
solution of the manganate.
2K2MnO4 + 2 H2O → 2KMnO4 + H2  + 2KOH
Physical Properties
It occurs in the form of deep, dark purple, monoclinic prismatic crystals and
moderately soluble in water. The taste is sweet and astringent.
Chemical Properties
It is very powerful oxidizing agent both in dry state and in solution.
Explosions may occur when it comes in contact with organic or other readily oxidisable
materials.
It act as an oxidizing agent because it produces nascent oxygen in solution.
2KMnO4 + 3H2SO4 → K2SO4 + 2MnSO4 + 3H2O + 5(O) (acid solution)
2KMnO4 + H2O → 2MnO2 + 2KOH + 3(O) (Alkaline (or) neutral solution)
Potassium permangante oxidizes iodides, bromides, chlorides, ferrous salts,
nitrites, sulphites, thio sulphates peroxides and oxalates. Organic materials such as ethyl
alcohol and charcoal are readily oxidized.
Assay
It is assayed by titrating it with N/10 oxalic acid in presence of disulphuric
acid at 70C. If the temperature is not maintained at 70C, the reaction will become slow.
2KMnO4 + 3H2SO4 → K2SO4 + 2MnSO4 + 3H2O + 5(O)
COOH
5 + 5(O) → 10CO2 + 5H2O
COOH
Storage:
74
Use
1. It is used as local anti infective.
2. It is used as mouthwash and gargle (more than 1 in 1000 solution).
3. It is also used as stomach wash in the treatment of Narcotic drug poisoning.
CHLORINATED LIME [Ca(OCl) Cl]

Syn: Bleaching powder
Calcium chloro hypochlorite.
Preparation
It is obtained by the action of chlorine on calcium hydroxide. Slaked lime is
spread on stable shelves in a container and chlorine gas is introduced at the top of the
chamber and passed through the contents of the shelves. This is done at 25C to minimize
the formation of calcium chloride.
Ca(OH)2 + Cl2 → Ca(OCl) Cl + H2O
Properties
It is dull white powder with characteristic odour, on exposure to air it absorbs
moisture and decomposes by liberating chlorine. It is sparingly soluble in water and
insoluble in alcohol.
When bleaching powder is added to water hypochlorite goes into solution and
oxygen is liberated. The oxidizing and bleaching properties are shown.
Bleaching powder is incompatible with ammonium salts sulphur and many organic
compounds.
Assay
For the estimation, an aqueous suspension of chlorinated lime is mixed with acetic
acid in the presence of potassium iodide and the liberated chlorine displaces an equivalent
amount of iodine from potassium iodide. The liberated iodine is titrated with standardized
solution of sodium thiosulphate using starch as an indicator.
Ca(OCl)Cl + 2CH3COOH → (CH3 COO)2 Ca + Cl2 + H2O
Cl2 + 2 KI → I2 + 2 KCl
I2 + 2Na2S2O3 → Na2S4O6 + 2NaI
Storage:
It is slowly decomposing with loss of chlorine due to atmospheric carbon dioxide
and moisture and for this reason, it should be stored in air tight containers.
Use:
1. It is used as disinfectant, deodorant.
75
2. Commonly used in chlorination of water and in treatment of swimming tank.
IODINE (I2)
Preparation
Iodine is manufactured by extracting kelp (sea weed ash) with water and the
solution is concentrated. The sulphate and chloride of sodium and potassium are
crystallized out, leaving soluble sodium and potassium iodides in the mother liquor.
Sulphuric acid is added to the mother liquor and sulphur which is liberated from small
amount of thiosulphate and sulphide is allowed to settle. The mother liquor is decanted
and to this MnO2 is then added and the Iodine is distilled out.
2NaI + 3H2SO4 + MnO2 → MnSO4 + 2 NaHSO4 + I2 + 2H2O
Impurities like I Cl, I Br and I CN are removed by heating crude iodine with
potassium iodide.
ICl + KI → KCl + I2
Physical Properties
It occurs as heavy, bluish-black rhombic plates with metallic luster. It has peculiar
odour and volatilizes at ordinary temperature. It melts at higher temperature. It is
practically insoluble in water but soluble in alcohol. It is freely soluble in chloroform and
ether.
Chemical Properties
1. It combines directly with some non-metals and with many metals.
2P + 3 I2 → 2PI3
Fe + I2 → FeI2
Reducing agent reacts with aqueous iodine solution and gets oxidized.
H3ASO3 + I2 + H2O → 2HI + H3ASO4
H2S + I2 → 2HI + S
Iodine reacts with alkali to form an iodide and iodate when heated.
3I2 + 6NaOH → 2NaI + NaIO3 + 3H2O

Potassium iodide dissolves large quantity of iodine in water, because of the
formation of poly iodide. (I3−)
KI + I2 → KI3
Assay
It is estimated by addition of potassium iodide solution, and acidified with acetic
acid and titrated with sodium thiosulphate using starch mucillage as indicator. The end
point is appearance of blue colour.
76
2Na2S2O3 + I2 → 2NaI + Na2S4O6
Sodium Tetrathionate
Incompatiability
It oxidizes hypophosphite, sulphite, some metals and reducing agents and iodine
itself gets reduced to iodide. It reacts with ammonia or ammoniated mercury to form
explosive iodide or nitrogen.
Storage
It is volatile at room temperature and reacts with rubber and corks. So it should be
stored in amber colour bottles with tight glass stopper and kept in a cool place.
SOLUTIONS OF IODINE
Iodine is insoluble in water but it is soluble in water in presence of potassium or
sodium iodide due to the formation of poly iodides. The following are the solution
preparations containing iodine.
1. Strong iodine solution (10% W/V solution of iodine)
2. Weak iodine solution (2% W/V solution of iodine)
3. Aqueous iodine solution (5% W/V solution of iodine)
4. Iodine tincture USP.
5. Mandl’s paint.
1. Strong Iodine Solution (strong tincture of iodine): Contains 10% W/V solution
of iodine and 6% W/V solution of potassium iodide in alcohol.
2. Weak solution of Iodine (weak tincture of iodine): Contains 2.5% W/V solution
of Iodine and 2.5% W/V solution of potassium iodide in alcohol.
3. Aqueous solution of Iodine (Lugal’s Solution): Contains 5% W/V solution of
iodine and 10% W/V solution of potassium iodide in water.
4. Iodine Tincture USP: Contains 2% W/V solution of iodine and 2.4% W/V
solution of potassium iodide and alcohol 50 ml and water up to 100 ml. It is used
for external use only.
5. Mandl’s Paint: Contains 1.25% W/V solution of iodine in glycerin. Glycerin is
used to hold the iodine in the applied area (throat).
Use: All the above solutions are used as antiseptics and disinfectants.
POVIDONE – IODINE (PVP – IODINE)

(Polyvinyl Pyrrolidone – Iodine Complex)
It is a complex of polyvinyl pyrrolidone and iodine containing not less than 9% and
not more than 12% W/V of available I2 (iodine).
77
The complex is yellowish brown amorphous powder and has slight characteristic
odour, its aqueous solution is acid to litmus. It is soluble in alcohol, but insoluble in
organic solvents.
It is available as Aerosol and solution. The solution is a transparent liquid having
reddish brown colour and a pH of not more than 6.0.
Uses
Major advantages over other iodine preparation is lack of tissue irritation. Solutions
are used for surgical scrubs and for pre operative antisepsis for the skin.
It is also used in gargles and mouth washes for the treatment of infections in the
oral cavity.
BORIC ACID
Refer under ‘Acids and Bases’
BORAX (Na2 B4O7. 10 H2O)

It is known as sodium borate.
Preparation
1. The mineral colemanate is mixed with sodium sulphate and heated to redness but
not to fusion in a rotary furnace. This mass has cooled, borax is dissolved in water and
allowed to crystallize, after removing insoluble calcium sulphate.
2Ca2B6O11 + 3Na2SO4 → 3CaSO4  + CaO + 3Na2B4O7
2. The mineral borocalcite is also converted into borax by this method.
Ca2B2O7. 4H2O + Na2SO4 → Na2B4O7 + CaSO4  + 4H2O
Properties
Borax occurs as colourless, odourless crystals or as a white crystalline powder that
has sweetish, alkaline taste. It effloresces in warm dry air. It is soluble in water and more
in boiling water and in glycerine. It is soluble in alcohol.
On heating it losses part of water of hydration. It is hydrolyzed partially to sodium
metaborate and boric acid.
→
Na2B4O7 + 3H2O 2NaBO2 + 2H3BO3
The metaborate is largely hydrolysed on dilution with water.

NaBO2 + 2H2O →  NaOH + H3BO3
Use
1. It is germicide and used as bacteriostatic.
2. It is used in preparations of eye wash (1-2%).
78
3. It is used as mouth wash and gargles.
4. Borax is used as food preservative. It is used in cosmetic preparations as emulsifier
and also in lotions.
SILVER NITRATE (AgNO3)

Preparation
It is prepared by action of dilute nitric acid on pure silver. 3 parts of silver are
added to the solution of 25% nitric acid (10 parts) and warmed. Then it is heated to expel
the nitrous fumes, filtered and evaporated until it is dry.
3 Ag + 4 HNO3 → 3 Ag NO3 + NO + 2H2O
Properties
It occurs as colourless crystalline compound odourless, bitter in taste. When it is
exposed to light or organic matter it turns grey or greyish black. It is more soluble in water
and in alcohol.
When it is heated, it melts at 212C to yellowish liquid and when heated further it
→
decomposes in to metallic silver with evolution of NO2 and O2.
2AgNO3  2Ag + 2NO2  + O2 
It gives white yellow-white precipitate with hydrochloric acid and other halogen
salts.
Silver Mirror Test
Ammonium hydroxide with silver nitrate forms silver-ammonium complex. To this
solution, if reducing agent like glucose is added the silver ions are reduced to metallic
silver and silver mirror is formed.
Incompatibilities
It is incompatible with reducing agents, tartrates, sugars and tannins. In neutral and
alkaline conditions precipitation results with halides, borax, hydroxide, phosphate sulphate
etc.
Assay
It is estimated by dissolving in water, nitric acid is added to it and titrated against
standard ammonium thiocyanate using ferric alum as indicator. The end point is the
formation of reddish-brown colour.
AgNO3 + NH4 SCN → AgSCN  + NH4 NO3
Storage
It is decomposed (reduction) by light so it should be stored in well closed, glass
container and protected from light.
Uses
79
1. It is used as antibacterial (0.01 – 0.5%).
2. At higher concentration it is used as Astringent (1% and above).
3. At very low concentration acts as bacteriostatic (0.0025 to 0.0050%).
4. Silver nitrate ophthalmic solution in 1% strength is used as eye wash.
MILD SILVER PROTEIN

It is a preparation with silver available in colloidal form by the presence of proteins
or in combination with it. It contains not less than 19% and not more than 23.0% of silver.
Preparation
It is prepared by using silver salt with an excess of denatured protein (serum
albumin, casein, or gelatin). The product is dried in vacuum and stored in amber coloured
bottles.
Properties
It is a dark brown – blackish shining scales or granules, odourless and is
hygroscopic, it is soluble in water but insoluble in alcohol, ether and chloroform.
Assay:
Same as that of silver nitrate.
Storage
It is stored in tightly closed amber-coloured glass containers, in dry and dark place.
Disodium edetate (EDTA) in 10 mg/ml is used as stabilizer for aqueous solution.
Uses
1. Aqueous solution of 1-2% are used as antibacterial.
2. For rhinitis, tonsilities it is used in 0.5 – 10% of concentration.
Only freshly prepared solutions are to be used. Since it has less free silver
ions, it is effective antimicrobial and show less irritation and astringent effect.
MERCURY (Hg)
Preparation
It occurs naturally as a sulphide called cinnabar.
It is obtained by roasting cinnabar in a current of air.
HgS + O2 → Hg + SO2
Properties
It is shining silvery white heavy liquid and extremely mobile. Practically insoluble
in water, alcohol and hydrochloric acid but completely soluble in nitric acid and boiling
sulphuric acid. It boils at 350C.
Assay
80
An accurately weighed quantity is dissolved in equal volume of nitric acid and
water by heating to form mercuric nitrate. It is titrated against ammonium thiocyanate
using ferric ammonium sulphate as an indicator.
Storage
Since it is volatile, it should be stored in tightly closed container in a cool place.
Uses
1. In general mercury being toxic, is not used medicinally.
2. There are number of other pharmaceutical uses of mercury like preparation of
mercury compounds, amalgams etc.
3. A preparation known as mercury with chalk acts as purgative because of irritant
action of mercury ion.
YELLOW MERCURIC OXIDE (HgO)

Preparation
It is prepared by pouring concentrated solution of mercuric chloride into a dilute
solution of sodium hydroxide with constant agitation. This is then allowed to stand at
room temperature for about an hour. Then the supernated liquid is decanted off and the
precipitate is washed with water until the washings are free from alkali. The yellow
precipitate is collected and dried on absorbent paper at 30C. The above steps are carried
out in dark place to get bright orange-yellow product.
HgCl2 + 2NaOH → Hg (OH)2 + 2NaCl
Hg(OH)2 → HgO + H2O
Properties
It is an orange-yellow heavy amorphous powder, odourless and gets decolourized
on exposure to light. It is practically insoluble in water and alcohol but readily soluble in
dilute hydrochloric acid and dilute nitric acid.
On heating to red hot it decomposes into oxygen and vapour of metallic mercury.
2HgO → O2 + 2 Hg
Assay
It is estimated by volumetric thiocyanate method. An accurately weighed quantity
is dissolved in nitric acid and water. The solution is titrated against ammonium
thiocyanate solution using ferric ammonium sulphate as an indicator.
Storage
It should be stored in tightly closed containers and protected from light.
Uses
81
1. It is used as mild antiseptic.
2. It is used as 1% solution for ophthalmic purpose to treat inflammation and
conjunctivitis.
AMMONIATED MERCURY (NH2 (Hg) Cl)
Preparation
It is prepared by adding 5% mercuric chloride solution to a mixture of 4 parts of
dilute ammonia and 20 parts of water with constant stirring. The precipitate is collected,
washed with cold water and dried below 30.
NH2
HgCl2 + NH3 Hg + NH4Cl
Cl
Properties
It is white amorphous powder and is odourless, darkens on exposure to light. It is
practically insoluble in water alcohol and ether.
Assay
It is treated with potassium iodide solution with stirring. The mercuric iodide
formed in the reaction is converted into potassium mercuric iodide (K2HgI4) by potassium
iodide. The liberated (alkali) ammonia and potassium hydroxide is titrated with
hydrochloric acid using methyl orange as an indicator.
NH2 HgCl + 2KI + H2O → HgI2 + NH3 + KOH + KCl
HgI2 + 2KI → K2HgI4
Uses
1. It is acting as mild antiseptic.
2. It is used in various skin infections caused by fungi, lice and other infestation.
3. It is used as an ointment and dusting powder in the strength of 5%.
Pharmaceutical Preparations of Mercuric Compound
1. Mercuric oxide eye ointment.
Preparation contains 0.9 to 1.1% of HgO in simple ointment.
Ointment is used to reduce inflammation and as antiseptic in conjuctivitis.
2. Ammoniated mercuric ointment
It contains 2.25 to 2.75% of NH2 HgCl. The preparation is used as mild antiseptics.
82
A. IDENTIFICATION TEST OF SOME ANIONS
1. BENZOATES : a) To 1 ml of a 10 percent w/v neutral solution add 0.5 ml of

ferric chloride solution, a dull-yellow precipitate, soluble in solvent ether is formed.
b) Moisten 0.2 g of the substance being examined with 0.2 ml of sulphuric acid and
gently warm the bottom of the tube, a white sublimate is deposited on the inner walls of
the tube and no charring occurs.
c) Dissolve 0.5 g of the substance being examined in 10 ml of water add 0.5 ml of
hydrochloric acid. The precipitate obtained, after crystallisation from water and drying
under reduced pressure melts at about 122C.
2. BICARBONATES :
a) Solutions of bicarbontates, when boiled liberates carbon dioxide.
b) Treat a solution of the substance being examined with a solution of magnesium
sulphate, no precipitate is formed (distinction from carbonates). Boil, a white
precipitate is formed.
c) Introduce into a test-tube 0.1 g of the substance being examined suspended in 2 ml
of water. Add 2 ml of 2M acetic acid. Close the tube immediately using a stopper
fitted with a glass tube bent at two right-angles. Heat gently and collect the gas in 5
ml of barium hydroxide solution, a white precipitate forms that dissolves on
addition of an excess of dilute hydrochloric acid.
3. BROMIDES : a) Dissolve 10 mg of the substance being examined in 2 ml of
water. Acidify with 2 M nitric acid and add 1 ml of 0.1 M silver nitrate. Shake and allow
to stand, a curdy, pale-yellow precipitate forms. Centrifuge and wash the precipitate
rapidly with three quantities, each of 1 ml, of water in subdued light. Suspend the
precipitate in 2 ml of water and add 1.5 ml of 10M ammonia; the precipitate dissolves
with difficulty.
b) Dissolve about 10 mg in 2 ml of water and add 1 ml of chlorine solution,
bromine is evolved, which is soluble in two or three drops of chloroform, forming a
reddish solution. The addition of phenol solution to the aqueous solution containing
liberated bromine yields a white precipitate.
NOTE : In testing for bromides in the presence of iodides, all iodine must first be
removed by boiling the aqueous solution with an excess of lead dioxide.
4. CARBONATES : a) Suspend 0.1 g of the substance being examined in a test-
tube in 2 ml of water. Add 3 ml of 2 M acetic acid. Close the tube immediately using a
stopper fitted with a glass tube bent at two right angles. Heat gently and collect the gas in
5 ml of 0.1 M barium hydroxide, a white precipitate is formed that dissolves on addition of
an excess of dilute hydrochloric acid.
b) Treat a solution of substance being examined with a solution of magnesium
sulphate, a white precipitate is formed (distinction from bicarbonates).
5. CHLORIDE : a) Dissolve 10 mg of the substance being examined in 2 ml of
water. Acidify with dilute nitric acid and add 0.5 ml of silver nitrate solution. Shake and
83
allow to stand, a curdy, white precipitate is formed, which is insoluble in nitric acid, but
soluble, after being well washed with water, in dilute ammonia solution, from which it is
reprecipitated by the addition of nitric acid.
b) Introduce into a test-tube 0.1g of the substance being examined, add 0.2 g of
potassium dichromate and 1 ml of sulphuric acid. Place a filter-paper strip moistened with
0.1 ml of dipnenylcarbazide solution over the opening of the test-tube, the paper turns to
violet-red. (Do not bring the moistened paper into contact with the potassium dichromate
solution).
6. CITRATES : a) To a neutral solution of the substance being examined add a
solution of calcium chloride, no precipitate is produced. Boil the solution, a white
precipitate, soluble in 6 M acetic acid, forms.
b) Dissolve 0.1 g of the substance being examined in 5 ml water. Add 0.5 ml of
sulphuric acid and 3 ml of potassium permanganate solution. Warm until the colour of the
permanganate is discharged and add 0.5 ml of a 10 per cent solution of sodium
nitroprusside in 1 M sulphuric acid and 4 g of sulphamic acid. Make alkaline with strong
ammonia solution, added dropwise, until all the sulphamic acid has dissolved, further
addition of strong ammonia solution produces a violet colour, turning to violet blue.
7. IODIDE: a) Dissolve 0.1 g of the substance being examined in 2 ml of water.
Acidify with dilute nitric acid and add 0.5 ml of silver nitrate solution. Shake and allow to
stand, a curdy, pale-yellow precipitate forms. Centrifuge and wash the precipitate rapidly
with three quantities, each of I ml of water in subdued light. Suspend the precipitate in 2
ml of water and add 1.5 ml of 10 M ammonia, the precipitate does not dissolve.
b) To 0.2 ml of a solution of the substance being examined add 0.5 ml of 1 M
sulphuric acid, 0.15 ml of potassium dichromate solution, 2 ml of water and 2 ml of
chloroform. Shake for a few seconds and allow to stand ; the chloroform layer is violet or
violet-red.
c) To 1 ml of a solution of the substance being examined add 0.5 ml of mercuric
chloride solution, a dark red precipitate is formed which is slightly soluble in an excess of
this reagent and very soluble in an excess of potassium iodide solution.
8. SULPHATE : a) Dissolve about 50 mg of the substance being examined in 5 ml
of water Add 1 ml of dilute hydrochloric acid and 1 ml of barium chloride solution a white
precipitate forms.
b) Dissolve about 50 mg of the substance being examined in 5 ml of water and add
2 ml of lead acetate solution, a white precipitate is formed which is soluble in ammonium
acetate solution and in sodium hydroxide solution.
9. THIOSULPHATES: a) Dissolve 0.1 g of the substance being examined in 5 ml
of water, add 2 ml of hydrochloric acid, a white precipitate is formed which soon turns
yellow and sulphur dioxide is evolved recognizable by its odour.
b) Dissolve 0.1 g of the substance being examined in 5 ml of water, add 2 ml of
ferric chloride test solution, a dark violet colour is produced which quickly disappears.
c) Solutions of thiosulphatcs decolorises iodine solution, the decolorised solutions
do not give the reactions of sulphates.
84
d) Solutions of thiosulphates decolorise bromine solution, the decolorised solutions
give the reactions of sulphates.
IDENTIFICATION TEST OF SOME CATIONS
1. ALUMINIUM : a) Dissolve about 20 mg of the substance being examined in 2
ml of water. Add about 0.5 ml of 2 M hydrochloric acid and about 0.5 ml of thiacetamide
reagent, no precipitate forms. Add dropwise 2M sodium hydroxide solution, a gelatinous
white precipitate appears that redissolves on addition of further sodium hydroxide
solution. Gradually add ammonium chloride solution, the gelatinous white precipitate
reapperars.
b) Dissolve about 20 mg of the substance being examined in 5 ml of water add five
drops of ammonium acetate solution and five drops of a 0.1% w/v solution of mordant
blue 3, an intense purple colour is produced.
c) To a solution of the substance being examined in water add dilute ammonia
solution until a faint precipitate is produced and then add 0.25 ml of freshly prepared
O.05% w/v solution of quinalizarin in a 1% w/v solution of sodium hydroxide. Heat to
boiling, cool and acidify with an excess of acetic acid, a reddish-violet colour is produced.
2. AMMONIUM SALTS : a) Heat a few mg of the substance being examined
with sodium hydroxide solution, ammonia is evolved, which is recognisable by its odour
and by its action on moist red litmus paper (colour changes to blue).
b) To the prescribed solution add 0.2 g of light Magneisum oxide. Pass a current of
air through the mixture and direct the gas that is evolved to just beneath the surface of a
mixture of 1 ml of 0.1 M HCl and 0.05 ml of methyl red solution, the colour of the
solution changes to yellow. On addition of 1 ml of a freshly prepared 10% w/v solution of
sodium cobaltinitrite, a yellow precipitate forms.
3. ANTIMONY : Dissolve with gentle healing about 10 mg of the substance being
examined in a solution of 0.5 g of sodium potassium tartrate in 10 ml of water and allow
to cool. To 2 ml of this solution add sodium sulphide solution drop wise, gives a reddish
orange precipitate which dissolves on adding sodium hydroxide solution.
4. ARSENIC : Heat 5 ml of the prescribed solution on a water-bath with an equal
volume of hypophosphorus reagent, a brown precipitate is formed.
5. BARIUM : a) Barium salts impart a yellowish-green colour to a nonluminous
flame, appearing blue when viewed through green glass.
b) Dissolve about 20 mg of the substance being examined in 5 ml of dil HCl, add 2
ml of dil. sulphuric acid a white precipitate forms which is insoluble in nitric acid.
6. BISMUTH : a) To 0.5 g of the substance being examined add 10 ml of dil. HCl.
Heat to boiling for one minute, cool and filter if necessary. To 1 ml of the solution
obtained add 20 ml of water, a white or slightly yellow precipitate appears which on
addition of 0.05 to 0.1 ml of sodium sulphide solution turns brown,
b) To about 50 mg of the substance being examined add 10 ml dil. nitric acid. Heat
to boiling for one minute, allow to cool and filter if necessary. To 5 ml of the solution
obtained add 2 ml of a 10% w/v solution of thiourea, an orange yellow colour or an orange
85
precipitate is produced. Add 4 ml of a 2.5% w/v solution of sodium flouride, the solution
is not decolourised within 30 minutes,
7. CALCIUM: a) Dissolve 20 mg of the substance being examined in 5 ml of 5M
acetic acid. Add 0.5 ml of potassium ferrocyanide solution, the solution remains clear.
Add about 50 mg of ammonium chloride, a white, crystalline precipitate is formed.
b) To a solution of the substance being examined add a few drops of a solution of
ammonium oxalate, a white precipitate is obtained that is, only sparingly soluble in dilute
acetic acid but is soluble in HCI.
c) Dissolve 20 mg of the substance being examined in 2 ml of HCI and dilute with
NaOH solution, add 5 ml of ammonium carbonate solution, a white precipitate is formed
which after boiling and cooling the mixture, is only sparingly soluble in ammonium
chloride solution.
8. FERRIC SALTS : a) Dissolve 0.1 g of the substance in 1 ml of water. Add 1 ml
of a 5% w/v solution of potassium ferrocyanide, an intense blue precipitate is formed that
is Insoluble in dil HCI.
b) To 3 ml of a solution containing 0.1 mg of iron add 1 ml of 2N.HC1 add 1 ml of
ammonium thiocyanate solution, the solution becomes blood-red in colour. Take two
portions, each of I ml, of the mixture. To one portion add 5 ml of solvent ether, shake and
allow to stand, the ether layer is pink. To the other portion add 3 ml of 0.2 M mercuric
chloride, the red colour disappears.
c) To 2 ml of a solution containing about 0.1 mg of iron add 3 ml acetic acid until
the solution is strongly acidic and add 2 ml of a 0.2% w/v solution of 8 hydroxy-7-
iodoquinoline-5-sulphonic acid. A stable green colour is produced.
9.FERROUS SALTS : a) About 10 mg of iron in 2 ml of water, add 2 ml of dil.
sulphuric acid and 1 ml of a 0.1 % w/v solution of 1,10 phenanthroline. An intense red
colour is produced, the colour is discharged by addition of a slight excess of 0.1 M ceric
ammonium sulphate.
b) To 1 ml of a solution not less than 1 mg of iron, add 1 ml of potassium
ferricyanide solution, a dark blue precipitate is formed that is insoluble in dil.HCI and is
decomposed by sodium hydroxide solution.
c) To 1 ml of a solution containing not less than 1 mg of iron add 1 ml of potassium
ferrocyanide solution, a white precipitate is formed which rapidly becomes blue and is
insoluble in dil.HCI.
10. LEAD: a) Dissolve 0.1g of the substance being examined in 1 ml of dil. acetic
acid, add 2 ml of potassium chromate solution, a yellow precipitate forms that is insoluble
in 2 ml of sodium hydroxide solution.
b) Dissolve 50 mg of the substance being examined in 1 ml of dil. aceticacid add 10
ml of water and 0.2 ml of 1M potassium iodide, a yellow precipitate forms. Heat to
boiling for one or two minutes, and allow to cool, the precipitate is reformed as glistening
yellow plates (Golden spangles).
11. MAGNESIUM: a) Dissolve about 15 mg of the substance being examined in 2
ml of water, add 1 ml of dil. ammonia solution, a white precipitate forms that is
86
redissolved by adding 1 ml of ammonium chloride. Add 1 ml of 0.25 M disodium
hydrogen phosphate a white crystalline precipitate form.
b) To 0.5 ml of a neutral or slightly acidic solution of the substance being examined
add 0.2 ml of a 0.1% w/v solution of titan yellow and 0.5 ml of 0.1 m sodium hydroxide, a
bright red turbididy develops which gradually settles to give a bright red precipitate.
12. POTASSIUM: a) Dissolve about 50 mg of the substance being examined in 1
ml of water, add 1 ml of dil. acetic acid and 1 ml of a freshly prepared 10% w/v solution
of sodium cobalt nitrite, a yellow or orange yellow precipitate forms immediately.
b) Dissolve 0.1 g of the substance being examined in 2 ml of water. Heat the
solution with 1 ml of sodium carbonate solution, no precipitate forms. Add 0.05 ml of
sodium sulphide solution, no precipitate forms. Cool in ice water and add 2 ml of a 15%
w/v solution of tartaric acid and allow to stand, a white, crystalline precipitate forms.
c) Ignite a few mg of the substance being examined and dissolve in the minimum
quantity of water. To this solution add 1 ml of platinic chloride solution in the presence of
1 ml of HCI a yellow, crystalline precipitate forms, which on ignition leaves a residue of
potassium chloride and platinum.
13. SILVER: a) Dissolve 10 mg of the substance being examined in 10 ml of
water, add 0.3 ml of dilute HCI, a curdy white preciptitate is formed that is soluble in
dil.ammonia solution. Add potassium iodide solution, a yellow precipitate is formed.
b) Dissolve 10 mg of the substance being examined in 20 ml of water, add 2 ml of
potassium chromate solution, a red precipitate is formed which is soluble in nitric acid.
14. SODIUM: a) Dissolve 0.1g of the substance being examined in 2 ml of water,
add 2 ml of a 15% w/v solution of potassium carbonate and heat to boiling, no precipitate
forms. Add 4 ml of freshly prepared potassium antimonate solution and heat to boiling.
Allow to cool in ice water and if necessary, rub the inside of the test-tube with a glass rod,
a dense white precipitate is formed.
b) Acidify a solution of the substance being examined with 1M acetic acid and add
a large excess of magnesium uranyl acetate solution, a yellow, crystalline precipitate is
formed.
15. ZINC: a) Dissolve 0.1 g of the substance being examined in 5 ml of water, add
0.2 ml of sodium hydroxide solution, a white precipitate form. Add a further 2 ml of
sodium hydroxide solution, the precipitate dissolves. Add 10 ml of ammonium chloride
solution, the solution remains clear but a flocculent, white precipitate forms on addition of
0.1 ml of sodium sulphide solution.
b) Dissolve 0.1 g of the substance being examined in 5 ml of water, acidify with
dil.sulphuric acid and add one drop of a 0.1% w/v solution of copper sulphate and 2 ml of
ammonium mercuri-thio-cyanate solution, a violet precipitate is formed.
c) Dissolve 0.1 g of the substance being examined in 5 ml of water, add 2 ml of
potassium ferrocyanide solution, a white precipitate is formed which is insoluble in dil.
HCl.
87
MODEL QUESTION PAPERS
D. PHARM. EXAMINATION
(PART – I)
12. PHARMACEUTICAL CHEMISTRY – I
[Time: 3 Hours]
Maximum : 80 Marks
Answer FIVE Questions

All questions carry EQUAL marks
Write chemical equations wherever necessary
1. (a) List the official compounds of calcium and mention their use. Give the
preparation, properties, use and assay of Iodine. (4+6) = 10
(b) Give an account on Biological effects of radiation and storage of Radio

Pharmaceuticals. (6)
2. Describe the principle of the limit tests of
(a) Lead (Dithizone method)
(b) Sulphate
(c) Iron (8 + 4 + 4)
3. Give the identification tests for the following radicals.
(a) Iodide
(b) Nitrate
(c) Carbonate
(d) Potassium
(e) Copper
(f) Aluminium
(g) Barium
(h) Zinc (8  2 = 16)
4. (a) Give an account on the sources of impurities in the Pharmacopoeial compounds.
(b) Discuss the methods used for the quality control. (10 + 6)
88
5. Write notes on :
(a) Pharmaceutical Buffers
(b) Antacids
(c) Saline Cathartics (5 + 6 + 5)
6. Give the principle of assay of the following:
(a) Borax
(b) Sodium Chloride
(c) Magnesium Sulphate
(d) Potassium Iodide
7. Outline the preparation of the following compounds.
(a) Chlorinated Lime
(b) Ammonium chloride
(c) Antimony Potassium tartrate
(d) Ferrous Sulphate (44 = 16)
8. Write briefly on :
(a) Oral electrolyte powder.
(b) Official mercury compounds
(c) Protective and adsorbent (5 + 6 + 5)
89
(PART – I)
[Time : 3 Hours]
Maximum : 80 Marks
1. (a) Give the preparation and chemical properties of ‘Boric Acid’..
(b) Explain the electrolytic process of manufacturing ‘Sodium Hydroxide’.
(c) Give the storage condition for
(i) Strong solution of ammonia.
(ii) Sodium hydroxide.
(d) Write a note on “Official buffers”. 4  4 = 16
2. (a) What are ‘Anti-Oxidants’? Give the preparation, properties and use of ‘Sodium
Meta bisulphite’.
(b) What are Antacids? Outline the preparation of ‘Aluminium Hydroxide Gel’.
(c) Explain the principle of assay of ‘Magnesium Tri Silicate’. (6 + 5 + 5)
3. Write notes on the following:
(a) Light Kaolin
(b) Talc
(c) Magnesium Sulphate
(d) Zinc Stearate 4  4 = 16
4. Explain the preparation, assay, storage condition and use of the following:
(a) Hydrogen peroxide
(b) Chlorinade lime 2  8 = 16
5. Explain the principle of assay of
(a) Iodine
(b) Ammoniated Mercury
(c) Zinc Sulphate
90
(d) Sodium Chloride 4  4 = 16
6. Give an account on :
(a) Precipitated Sulphur
(b) Dicalcium Phosphate
(c) Nitrous Oxide
(d) Antimony Potassium Tartrate 4  4 = 16
7. Write notes on :
(a) Storage of Radio-active pharmaceuticals
(b) Oral Rehydration Salts
(c) Radio-opaque contrast media
(d) Limit test for ‘Chloride’ (44 = 16)
8. (a) Outline the important sources of impurities in inorganic drugs.
(b) Describe the principle of limit test for heavy metals.
(c) Write down the tests for identification of following ions:
(i) Iron
(ii) Calcium (8 + 4 + 4)
91
(PART – I)
[Time : 3 Hours]
Maximum : 80 Marks
1. (a) Explain the term Radio activity and Radio Isotopes.

(4)
(b) Discuss the methods for measurement of Radio activity.

(6)
(c) Write the applications of Radio isotopes. (6)
2. Describe the method of preparation and medicinal uses of

(44 = 16)
(a) Yellow Mercuric Oxide
(b) Sodium bicarbonate
(c) Calcium hydroxide
(d) Potassium Iodide
3. Give the principle involved in the assay of (44 = 16)
(a) Ferrous Sulphate
(b) Ammonium Chloride
(c) Calcium Gluconate
(d) Iodine
4. (a) Give the reason for the following (42 = 8)
(i) Ammonia is used in the limit test for Iron.
(ii) Polyhydric alcohol is used in the assay of Boric acid.
(iii) The use of Lead acetate cotton wool in the limit test for Arsenic.
(iv) Thioglycollic Acid is added to the Ferric sulphate solution.

92
(b) Write the properties, storage conditions and medicinal uses of
42=8
(i) Oxygen
(ii) Ammonia
(iii) Bentonite
(iv) Epsom salt
5. What are dental products?

Write method of preparation and properties of (16)
(a) Calcium Carbonate
(b) Sodium Fluoride
(c) Zinc Chloride
(d) Dicalcium phosphate
6. Write notes on : (28 = 16)
(a) Sulphur and its compound.
(b) Protectives and adsorbent.
7. Give the method of preparation, properties and uses of (44 = 16)
(a) Silver nitrate
(b) Chlorinated lime
(c) Boric Acid
(d) Hydrogen Peroxide
8. (a) Explain the importance of quality control for drugs and pharmaceutical
substances. (10)
(b) Give the important test for the identification of (3  2 = 6)
(i) Chloride
(ii) Lead
(iii) Calcium
93

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D.

PHARM (PART-I) SYLLABUS FOR PHARMACEUTICAL CHEMISTRY - I

1) General discussions on the following inorganic compounds including important

b) Antioxidants-Hypophosphorous acid, Sulphur dioxide, Sodium bisulphite,

i) Acidifying agents - Dilute hydrochloric acid

ii) Antacid - Sodium bicarbonate, aluminium hydroxidegel, aluminium

iii) Protectives and Adsorbent - Bismuth subcarbonate, Kaolin.

iv) Saline cathartics, Sodium Pottassium tartate and magnesium sulphate,

i) Protectives, Zinc Oxide, calamine, Zinc stearate, Titanium dioxide,

ii) Antimicrobials and Astringents-Hydrogen peroxide*, Potassium .

iii) Sulphur and its compounds Sublimed sulphur, precipitated sulphur,

iv) Astringents: Alum and Zinc Sulphate.

f. Inhalants - Oxygen, Carbon dioxide, Nitrous oxide.

g. Respiratory stimulants - Ammonium carbonate. Expectorants and Emetics -

1) Antidotes - Sodium nitrite

2) Major Intra and Extracellular eletrolytes.

a) Electrolytes used for replacement therapy-Sodium chloride and its

b) Physiological acid base balance and electrolytes used, sodium acetate,

c) Combination of oral electrolyte powders and solutions.

5) Quality control of Drugs and Pharmaceuticals importance of quality control,

6) Identification tests for cations and anions as per Indian Pharmacopoeia.

2. Lowry-Bronsted Theory (Proton Concept)

STRONG AMMONIA SOLUTION

SODIUM META BISULPHITE

DILUTE HYDROCHLORIC ACID I.P

ALUMINIUM HYDROXIDE GEL

Preparation (Commercial Method)

1. They are generally insoluble.

LIGHT KAOLIN I.P.

SODIUM POTASSIUM TARTRATE

K2CO3 + Na2CO3 + 2H2SO4 → K2SO4 + Na2SO4 + 2CO2 + 2H2O

N – CH2 – CH2 - N Use :

Assay : By Complexometric Method

SULPHUR AND ITS COMPOUNDS

Dental Caries (Tooth decay)

ANTIMONY POTASSIUM TARTRATE

% Dextrose % NaCl m. eq/lit Available volume (ml)

5 0.11 18.8 250, 500 & 1000

5 0.20 34.2 250, 500 & 1000

5 0.225 38.5 250, 500 & 1000

Use : Fluid, nutrient & electrolyte replenisher.

5 0.3 51.3 500 & 1000

10 0.3 51.3 500 & 1000

15 0.45 76.9 150 & 500

20 0.45 76.9 250 & 500

POTASSIUM CHLORIDE (KCl)

18. PHYSIOLOGICAL ACID – BASE BALANCE

ELECTROLYTES USED TO BALANCE PHYSIOLOGICAL ACIDS AND BASES

POTASSIUM ACETATE (CH3COOK)

Incompatibility: It is incompatible with acids, silver, mercury and iron salts.

SODIUM BICARBONATE INJECTION

AMMONIUM CHLORIDE (NH4Cl)

AMMONIUM CHLORIDE INJECTION

COMBINATION OF ORAL ELECTROLYTE POWDERS AND SOLUTIONS

These combination products can be divided into two groups: 1) Fluid

Ringer’s Injection, U.S.P.

Sodium Chloride 8.6 g

Lactated Ringer’s Injection, USP

Oral Rehydration Salts I.P.