Notes on Pharm114L MT

Experiment No. 1 Hydrogen Peroxide

Formula: H2O2
MW: 34.02
It was discovered by L.J Thenard (1818) and he designated it as “oxygenated water”. He prepared it by the action of hydrochloric acid
on barium peroxide. Strong solutions are used as hair (6% solution) and fabric bleaches. They are particularly desirable because of the
harmless nature of the reaction products. Solutions are said to be in certain “volume strength” (ie 3% is a 10 volume peroxide).
Laboratory Preparation: Because of the difficulties in filtering the large volumes of precipitate formed when an official 3% peroxide is
made in small quantities that gives one tenth the strength of the official.
Pharmaceutical preparations and uses:
1. Hydrogen Peroxide Solution (Liquor Hydrogenii Peroxidi, Hydrogen Dioxide Solution) USP XIII
 Physical Properties
 An aqueous solution containing NLT 2.5 g and NMT 3.5 g of H2O2 in 100 ml
 It is a colorless liquid, odorless or having an odor resembling that of the ozone
 A trace of free acid and acetanilide increase its stability by catalytically retarding its decomposition
*Acetanilid – stabilizer in the preparation of Hydrogen Peroxide
Types of stabilizer:
Acids – employed to decrease the pH of the preparation to become stable (ie phenylphosphonic acid, nitrates,
pyrophosphates)
Complexing agents – used to chelate trace amounts of polyvalent metals making them unavailable to catalyse
decomposition (ie EDTA)
Adsorbents – used to remove impurities from hydrogen peroxide (ie alumina, silica)

 When exposed to the air at ordinary temperatures or when heated on a water-bath at a temperature not exceeding
60oC the solution loses chiefly water (thus the solution may be concentrated so as to contain 50% by volume of
hydrogen peroxide) and when rapidly heated, it frequently decomposes suddenly
When heated it decomposes to form water and oxygen
2H2O2 --> 2H2O + O2↑
 Must be practically free from any impurities (arsenic, barium and heavy metals)
 Pure hydrogen peroxide (100%) syrupy liquid having specific gravity of 1.4631
 It may be separated with very little decomposition from its aqueous solution by fractional distillation under reduced
pressure
 At ordinary temperatures, it is miscible in all proportions with water, alcohol and ether, it is more soluble in ether than in
water (therefore extracted from its aqueous solution by shaking two liquids through separatory funnel)

 Chemical Properties
 It is a feeble acid that enters readily into double decomposition to form peroxidates which easily become hydrated and
appear as crystalline precipitates
Ba (OH)2 + H2O2 ↔ 2H2O + BaO2
BaO2 + 8H2O ↔ BaO2. 8H2O
 Uses
 Antiseptic because of the active liberation of oxygen when it comes in contact with organic material (ie pus or blood).
The foaming caused by the liberation of O2 mechanically cleanses wounds by dislodging fixed bacteria, particles or dirt.
This mechanical action rather than its chemical antisepsis is its important function since the period of contact of oxygen
with the bacteria is too short to bring about an effective oxidizing action, and H 2O2 is only feebly antiseptic
 3% of the undiluted solution is also used in treating Vincent’s stomatitis used as a mouthwash several times daily
*continued use may cause “hairy tongue” or hyperthrophied filiform papillae which disappears on discontinuation of use
 Antidote for cyanide and phosphorous poisoning through oxidation of the poisonous materials to more or less harmless
oxidation products
 Acts as reducing agent where silver iodide is reduced with a rapid evolution of oxygen, potassium permanganate in
sulfuric acid is rapidly changed to manganese sulfate, potassium sulfate and oxygen
Ag2O + H2O2 --> 2Ag + H2O + O2 ↑
2KMnO4 + 3H2SO4 + 5H2O2 --> K2SO4 + 2MnSO4 + 8H2O + 5O2 ↑

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  Official tests for Identity
1. 1 ml of hydrogen dioxide is shaken with 10ml of distilled water containing 1 drop diluted sulfuric acid and then 2ml of ether
and a drop of potassium dichromate TS
Result: Evanescent blue color in the aqueous layer
Equation: K2Cr2O7 + H2SO4 --> H2Cr2O7 + K2SO4
*dichromic acid reacts with hydrogen dioxide to form perchromic acid (blue color that is more soluble in ether than in water)

 Storage requirements
The synthesized product must be maintained in 25-35oC to avoid decompositions and explosions, since the following re considered
exothermic.
a. Decomposes violently into water and oxygen if heated (60-100oC)
b. deteriorates upon standing and during contact with oxidizing and reducing agents
c. evaporates rapidly when exposed to air

Experiment No. 2 Boric Acid

Formula: H3BO3
MW: 61.84
Other name: boracic acid, orthoboric acid, Sal Sedativum Hombergi, acidum boricum, borofax
Obtained by William Homberg by heating borax with copperas, later prepared thru the action of sulfuric acid. It was identified as Sal
Sedativum Hombergi.
 Physical properties
 Acts as a tribasic acid. However, because it dissociates to such a small extent, it is a very weak acid that is actually used
in water solution as an eye wash. Pure boric acid is a colorless, odorless, white powder or transparent crystals with a
slightly oily feeling that slowly decomposes with heat at about 340°F (171°C).
 Boric acid loses water as it is heated, changing first into metaboric acid (HBO2) and then into pyroboric acid (H 2B4O7)
and eventually to boric oxide (B2O3). The three acids can be thought of as hydrates of boric oxide (B2O3). Orthoboric acid
is fairly soluble in water (especially hot water), alcohol, and glycerine.
 3 Forms:
a. Colorless, odorless, pearly scales having smoot feel
b. Six sided triclinic crystals
c. White odorless powder which is unctuous to touch
* all forms are stable in air, scale and crystalline are suitable in preparing aqueous solutions
 USP Descriptive terms of Solubility
Solubility in water Parts of water required to
dissolve 1 part of organic solvent
Very soluble <1
Freely soluble 1-10
Soluble 10-30
Sparingly soluble 30-100
Slightly soluble 100-1000
Very slightly soluble 1000-10,000
Practically insoluble/Insoluble >10,000

Boric acid is
Soluble in water and alcohol (18ml); Freely soluble in glycerin, boiling water and boiling alcohol (4-6ml)
 Weak acid: pKa= 9.19 therefore hard to titrate with NaOH
 Esterified with glycol, mannitol and cathecol
 When heated, produces various products

 Uses
 Boric acid has wide applications in our daily life. The most important uses of Boric acid is as a source of B 2O3 in glasses and
other vitreous products, fiberglass, heat-resistant borosilicate glasses, ceramic glazes, porcelain, ceramics, crockery,

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 enamels, artificial gemstones, and sealing and optical glasses. Boric acid has other applications like insecticide for
cockroaches, black carpet beetles and as an fungicide on citrus fruits.
 In the medical field, boric acid has extensive use in mouthwashes, nasal sprays, and eye-hygiene formulations. Boric acid can
also be used as a fire-retardant in some occasions. Other important applications include preservatives for natural products
such as wood and natural fibers.
 Assay
Purpose: To determine the percentage of purity in a given amount of the boric acid.
Process:
1 gram of boric acid is taken in conical flask and dissolved in distilled water, add glycerin and phenolphthalein TS as indicator
titrated against 1M NaOH until a faint pink color is produced.
Principle:
Boric acid is a local infective. It is very weak acid and hence it can be titrated with glycerin, glyceryl-boric acid is formed which
behaves as a strong acid and can be titrated against sodium hydroxide and phenolphthalein as indicator.

 Dosage forms boric acid is prepared: Dusting powders, solution, suppository, ointment, eyewash

Experiment No. 3 Sodium acetate

Formula: CH3COONa.3H2O
MW: 136.09
 Physical Properties
 Colorless, transparent monoclinic prisms or as a granular, crystalline powder. It is odorless or has a faint acetous odor
and has a cooling saline taste. When exposed to dry, warm air, the salt effloresces to change to a powder from loss of
water of crystallization). Its density is 1.45.
 1 gram is soluble in about 0.8 ml of water, 19ml of alcohol at 25oC. It is insoluble in ether
 Chemical Properties
 When heated to about 58oC, the salt begins to liquefy and at 120oC it becomes hard and anhydrous. At higher
temperatures, it decomposes, emitting inflammable vapors and leaving residue of sodium carbonate and carbon.
2CH3COONa.3H2O + 4O2 --> Na2CO3 + 9H2O + 3CO2 ↑
The residue gives positive tests for sodium, is alkaline to litmus paper and effervesces with acids (carbonates)
Sodium acetate gives all of the tests characteristics of acetates:
Acidification of sodium acetate or its solution causes the evolution of an acetic acid odor, particularly if the mixture is
warmed.
2CH3COONa + H2SO4 ↔ 2CH3COOH + Na2SO4
If sodium acetate is warmed with sulfuric acid and ethyl alcohol the acid is esterified to form ethyl acetate which
possesses a characteristic odor. The acid is formed first according to equation, and then the esterification takes place.
H2SO4
2CH3COOH + C2H3OH ----------> CH3COOC2H3 + H2O
Ferric chloride TS added to solutions of acetate causes the formation of a deep red color due to ferric acetate. This color
is destroyed by mineral acids.
FeCl3 + 3CH3COONa ↔ (CH3COO)3Fe + 3NaCl
 Laboratory preparation: The product should be dried in a current of air at a temperature not exceeding 30 oC.
3Pb(C2H3O2)2.3H2O + 3Na2CO3.H2O + 7H2O --> (PbCO3)2.Pb(OH)2↓ + 6NaC2H3O2.3H2O + CO2↑
 Pharmaceutical preparation and uses
1. Sodium Acetate (Sodii Acetas), NF VIII
When rendered anhydrous by drying at 120oC, contains NLT 99% of CH3COONa. Sodium acetate when orally administered is
absorbed and easily oxidized in the tissues to sodium bicarbonate. Its physiological action is reflected in the fact that it causes a
hypertonic condition of the extracellular fluid that attracts water from the cells into the extracellular fluid. The ‘salt effect’
results in a diuretic action, since the kidneys regulate the electrolyte concentration of the body fluids by excreting water in
varying amount of salts. At the same time the formation of bicarbonate tends to relieve systemic acidosis and lessen the acidity
of the urine. Has particular value as a diuretic and in the treatment of cystitis and diseases of the urinary tract associated with
highly acid urine.

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 2. Theobromine and sodium acetate (Theobromina et sodii acetas) USP XIII
Sodium acetate is the solubilizer of theobromine by forming a water-soluble double salt. Used as diuretics which are of
particular value in cardiac edema.
* Theobromine + sodium acetate (solubilizes theobromine by forming water soluble double salt) that is effective in cardiac edema
with 0.5 grams as the dose.
*Exhibit a longer duration of action and less side effects than theophylline salts.

3. Theophylline and sodium acetate (Theophylline et sodii acetas) USP XIII

A better diuretic than theobromine
*Theophylline + sodium acetate (solubilizes theobromine by forming water soluble double salt) that is effective as diuretic with 0.2
grams as the dose.

 Definition of terms
Efflorescence – refers to the loss water (or solvent) of crystallization from a hydrated or solvated salt to the atmosphere on
exposure to air.
Diuretic – substance that promotes the production of urine.
Types of diuretic (acts on the kidneys’ nephron with several parts that differentiates the types):
Loop diuretics – act on the Loop of Henle Thiazide diuretics – act on the distal convoluted tubule
Carbonic anhydrase inhibitors – act on proximal convoluted tubule Potassium-sparing diuretic – act on distal convoluted tubule
Osmotic diuretic – act on collecting duct

 Correlation
Mechanism of action of sodium acetate as a diuretic: The cation, Na+ of sodium acetate is introduced into the body fluids.
When taken orally, sodium acetate is easily oxidized in the tissues to sodium bicarbonate causing a hypertonic concentration of
the extracellular fluid attracting water from cells to the ECF, hence a “salt effect”.
Sodium acetate is of particular value in cystitis: cystitis is the inflammation of the bladder as a result of urine infection. When
sodium acetate is taken orally, it is readily converted to sodium bicarbonate which lessens the acidity of urine cystitis is
associated with highly acid urine.

Experiment No. 4 Sodium citrate

Formula: Na3C6H5O7
MW: 136.09
 Physical Properties
 Occurs in colorless, monoclinic crystals or as white, odorless, crystalline powder having a cool saline test. The salt slowly
effloresces on exposure to dry air. One gram dissolves in 1.5ml of water at 25oC and 0.6ml of boiling water. It is insoluble
in alcohol.
 Chemical Properties
 When heated to 100oC it begins to water and at about 150oC becomes anhydrous. At read heat it carbonizes, emitting
inflammable gases having a pungent acid odor and leaves a black residue of carbon and sodium carbonate.
2Na3C6H5O7.2H2O + 9O2 ---> 3Na2CO3 + 9CO2↑ + 9H2O
It is a salt of a strong base and a relatively weak acid and hydrolyzes sufficiently to impart a slight alkalinity to its aqueous
solutions.
Test for identity:
1. Excess of calcium chloride TS is added to a cold, neutral solution of sodium citrate, no precipitate is produced.
However, when the solution is heated, a white granular precipitate of calcium citrate settles out. The precipitate is
insoluble in sodium hydroxide TS but dissolves immediately in diluted hydrochloric acid due to the formation of water-
soluble citric acid and calcium chloride.
2. If potassium permanganate TS is added to a hot solution of sodium citrate, to which has been added one-tenth of its
volume of mercuric sulfate TS (Denige’s reagent), a white precipitate is produced.

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 3. When ignited, it behaves in the manner characteristic of almost all metallic salts of organic acids, in that at first chars
and burns, and then upon continued heating yields a residue of sodium carbonate which effervesces with acids and
imparts the yellow sodium color to a non-luminous flame.
 Pharmaceutical Preparations and Uses
1. Orally
- Ingested into the body and oxidized in the tissues to sodium bicarbonate (not as rapid as that taking place in acetates). Its
therapeutic value depends then on this alkalinization and hence it is used to relieve mild acidosis and promotes diuresis.
2. Parenterally
- Capable of shortening the coagulation time of the blood, although in contradiction to its anticoagulant action on blood in
vitro.
3. In-vitro (controlled environment outside of a living organism)
- When added to a freshly drawn blood, it prevents the coagulation of blood over relatively long period of time. This might
be due to the inactivation of blood calcium as dissociated calcium citrate is utilized in making blood-transfusions, wherein
the blood is drawn into a flask containing a suitable amount of sodium citrate. The drawn blood may be then kept for
some time, or may be used immediately without the danger of clotting. The citration of blood is usually carried out by
using a 2.5% sodium citrate solution in the proportion of 10ml to 100ml of the donor’s blood. It is necessary that citrated
blood be stored at body temperature and it should be used as soon as possible.
4. Pharmaceutically
- Used to prevent discoloration of various preparations such as glycerites of phenol and tannic acid.

*Sequestering agent- a substance that removes ions from a solution system by forming a ring which does not have chemical reactions
with the ion which is removed
Types:
Inorganic polyphosphates – best sequestering agents and also aids in cleansing, however hydrolyzes at high temperature thereby
losing effectivity (ie sodium tripolyphosphate, sodium hexametaphosphate
Aminocarboxylic acids – mostly used sequestering agents, intended for metal ions and stable at alkaline conditions (ie EDTA)
Organophosphonic acids – effective but expensive (ie ethylenediaminetetramethylene phosphoric acid)
Oxalates and hydrocarboxylic acids – excellent sequesterant for iron, ineffective for calcium and magnesium (ie Citrates)

Experiment No. 5 Sodium phosphate

Formula: Na2HPO4.7H2O
MW: 268.09
 Physical properties
 Occurs as colorless or white granular salt that has unpleasant saline taste having a specific gravity of 1.524 at 16 oC. It
easily effloresces in air, losing 5 molecules of water from the initial 12 molecules of water of hydration. One gram
dissolves in 4ml of water at 25oC and it is very slightly soluble in alcohol.
 Chemical properties
 When the salt is heated to 40oC, it fuses to a colorless liquid. At 100oC it becomes anhydrous and at 300oC it is converted
to pyrophosphate.
NaH2PO4 ↔ NaPO3 + H2O
2Na2HPO4↔ Na4P2O7 + H2O
An aqueous solution of disodium hydrogen phosphate is alkaline to litmus paper and to phenolphthalein test solution.
This is occasioned by hydrolysis (the tendency of the hydrogen ion of the water to combine with the monohydrogen
phosphate ion to form dihydrogen phosphate ion. The alkalinity of course is due to the presence of hydroxide ion.
HPO4 ꓿ + H2O ↔ H2PO4− + OH−
*many of the incompatibilities of this salt are due to insoluble salt formation. Insoluble salts are readily formed with
silver, barium, ferric and lead salts.
*the presence of ammonia salts will also cause the formation of tertiary barium phosphate

 Definition of terms
Exsiccation – process that leads to the loss of moisture (dehydrate).

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  Preparation
 High temperature must be avoided at the beginning of exsiccation since it may cause the salt to dissolve in its own water
of hydration making it difficult to expel traces of water from the hard cake residue left upon evaporation.
*5 grams of crystals to effloresce (several days in warm air: 25-30OC). In oven, 110OC is required. Salt ceases to lose its
weight.
 The exsiccated sodium phosphate is used in the preparation of effervescent sodium phosphate.
 Effervescent Sodium Phosphate- contains 20% exsiccated sodium phosphate, sodium bicarbonate, citric acid, tartaric
acid. It is used as laxative with improved taste due to carbonation of sodium carbonate and organic acids.
*It is powdered and stored in a well-close container.

 Pharmacological use
Saline Laxative
Mechanism of action: Draws a large amount of water from the body into the intestines which in turn increases the
pressure on the intestinal walls and stimulates the movement of bowel contents.
Dose: 2-4g in a glass og hot water, an hour before breakfast (to have soft stool within an hour)
Precaution: Prolonged use can lead to dehydration.
Examples: Magnesium sulfate, sodium phosphate, sodium biphosphate

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