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Index |
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|
1. |
Soloutions |
|
|
2. |
Determination
of solubility of inorganic compound |
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3.
|
Double
displacement method |
|
|
4. |
Prepare
and dispense vanishing cream |
|
|
5. |
Density |
|
|
6. |
Density
of water at different temperature using pycnometer |
|
|
7. |
Preparation
of toothpaste |
|
|
8. |
Prepartion & dispensing of castor
oil emulsion |
|
|
9. |
Preparation of simple syrup |
|
|
10. |
Identification of particle size by sieve
method |
|
|
11. |
Preparation of
ACP Powder |
|
Safety Precautionary Measures of Laboratory:-
There
are some safety measures of lab listed here
- Always wear lab coats and
Gloves while using any hazardous chemical or substance.
- Never do unauthorized experiments.
- Never work alone in laboratory.
- Keep your lab space clean and
organized.
- Do not leave an on-going
experiment unattended.
- Always inform your instructor
if you break a thermometer. Do not clean mercury yourself!!
- Never taste anything. Never
pipette by mouth; use a bulb.
- Never use open flames in
laboratory unless instructed by TA.
- Check your glassware for cracks
and chips each time you use it. Cracks could cause the glassware to fail
during use and cause serious injury to you or lab mates.
- Maintain unobstructed access to
all exits, fire extinguishers, electrical panels, emergency showers, and
eye washes.
- Do not use corridors for
storage or ork areas.
- Do not store heavy items above
table height. Any overhead storage of supplies on top of cabinets should
be limited to lightweight items only. Also, remember that a 36"
diameter area around all fire sprinkler heads must be kept clear at all
times.
- Areas containing lasers,
biohazards, radioisotopes, and carcinogens should be posted accordingly.
However, do not post areas unnecessarily and be sure that the labels are
removed when the hazards are no longer present.
- Be careful when lifting heavy
objects. Only shop staff may operate forklifts or cranes.
- Clean your lab bench and
equipment, and lock the door before you leave the laboratory.
·
.png)
·
Biohazard
symbol (black and yellow)
Symbol for biological
hazard.
Danger radiation zone
warning sign
Nitrile gloves
Solubility
Definition:
The amount of substance(Solute) that dissolves in a unit volume of a
liquid substance(Solvent) to form a homogenous saturated solution under
specified conditions of temperature and pressure. This phenomenon is known is Solubility.
Solubility of a compound in a particular solvent is defined as the
concentration of solute (compound) in a saturated solution at a certain
temperature.
it may be defined as a the continuous interaction of two or more
compound to form homogenous molecular dispersion the basis of solute and
solvent present in the solution.
Role:
Solubility is an
important phenomenon in pharmaceutical sciences it plays very effective and
prominent role in the form ulations of dosage
forms.
CLASSIFICATION:
it can be classified
in three categories.
1) Saturated
solution: Saturated solution
is the one in which the substances (solute) is in equillibirium with solid
phase at a particular temperature.in these types of solution ,the solute is
completely in the soluble state
2) Unsaturated
solution : it is the solution which containing the less
amount of solute than the saturated solution at a particular temperature.
3) Supersaturated
solution: A supersaturated
solution is one that contains more substance than required for the preparation
of the saturated solution at a definite temperature. solubility of the solute is enhanced by
changing the physical parameters.
Solubility may be
expressed in aconcise form by J.W.Gibb,
it is useful for relating the effect of variables on solubilty like
temperature, pressure,concentration etc.upon the various phases such as
solid,liquid and gaseous.
F=C-P+2
Where F is degree of freedom in the system,
C is the number of components and
P
represents the number of bases
this equation is
known as Gibb's phase rule or equation.
Iceßà waterßà
Vapor
In this example
component (C) = 1 and the number of
phases (P) =3
Expression of solubility: Many terms are used for the expression othif
solubility.when quantitative data are available,solubility may be expressed in
many ways like molarity,molality,normality,mole fraction and percent
solution.ln pharmaceutical sciences solubility can be expressed in the
following terms.
(a) % w/w ( weight by weight )
(b) % w/v
( weight by volume)
(c) %
v/v ( volume by volume)
Solubility of the Drugs is expressed in
various units in the merck index.
|
Term |
Parts of solvent required for 1 part of
solute |
|
Very soluble |
Less than 1 part |
|
Freely Soluble |
1 to 10 parts |
|
Soluble |
10 to 30 parts |
|
Sparingly Soluble |
30 to 100 parts |
|
Slightly Soluble |
100 to 1000 parts |
|
Very slightly soluble |
1000 to 10,000 parts |
|
Practically insoluble |
More than 10,000 parts |
Factors affecting solubility:
Many factors are' affecti..g solubility of
substances in solvents viz.
• Temperature
• Concentration
• Types of solute and solvent
• pH
• Partical size
• Molecular structure
• Common ion effect
• Combined effect of solvent and pH
• Effect of wetting agent or surfactant
• Effect of non electolytes.
Determination of solubility:
For determination of
solubility of a solid in liquids,it can be divided into two steps
1) Preparation
of saturated solution:
Saturated solution
can be prepared by three methods.all three methods are employed for the preparation of saturated soultion in
practice but second method is more preferable than the first and third methods
because this method is fast and easy to prepare the saturated solution.
a) In first method,the substance
is added in the solvent slowly at a praticu(ar temperature and solute is not
added more than the saturation.
b) The second method is based on
the effect of temperature,as solubility increases with increases in
temperature.if the soulbility is to studied at 25°C,then the solvent is to be
heated at 300 to 350C with excess amount of solute.The amount of solute
required is more higher temperature for the preparation of saturated
solution.when this solution is cooled at the study temperature (25°C) the
excess amount of solute is separated out in the solution.it can be separated by
the filtration.the filtration solution is considered as saturated soution at
the study temperature.
c) The third method is same as
second method but is slightly different from the second,as in this method
excess amount of the solute is added in solvent at the study temperature and
shaken with continuous stirring or by wrist action shaker for few hours or left
the container for 24 hour saturation. With occadonal shaking and removing
excess amount of solute by filtration.This solution is known as saturated
solution.
2) Analysis of saturated
solution:
The anaylsis of
saturated solution depends on the nature of the substance (solute) and accuracy
of analysis.Many methods have been employed for the determination of solubility.
a) Evaporation method: This method is suitable for those substance
which do not decompose at a slightly higher (10-20°C) temperature than the
boiling point of a solvent.In this method a suitable volume of the saturated
solution of the solute in the solvent at the study temperature is weighed in a
porcelain dish and the solvent is evaporated till dryness.it is heated to
achieve a final volume in an oven to a constant weight.Thus,the amount of the
solid present in the solution can be calculated.
b) Volumetric method: This method is suitable for determination of
solubility of acids and bases by titration.In this method a fixed volume of
solution is treated with a suitable reagent using an indicator and
determination amount of the solute present in the solution.This method is
suitable for the determination of solubility in the solvent
c)
Gravimetric method: This method is suitable to those substances which react with reagent in
solution and gives sparingly soluble product.In this method, a known quantity
of solution is taken and added suitable reagent to precipitate the substance
completely into form of new compounds or salts form. Filter the precipitate and
remove the solvent if necessary wash the precipitate using purified water and
then dry tin e precipitate.weighed amount of precipitate is to be dried in
porcelin dish to get qa constant weight.By this method solubility can be
calculated as the number of grams of solute in 100g of the solvent.
d) Instrumental methods: All these methods are very sensitive and
suitable for determination of solubility in fractions or in
microns.Instrumental methods are very popular for the determination of
solubility due to its ease of working and simplicity.
a) UV-spectrophotometer method
b) High performance liquid chromatography
(HPLC)
c) Thin layer chromatography(TLC)
d) Gas chromatography (GC) e) Many
Experiment #1 Soloutions
Isotonic sol:
Isotonic solution are those solutions that
have same concentration of salts as the normal concentration of body and blood.
Apparatus:
·
Weighing balance
·
Liquid
·
Beaker
·
Watch glass
·
Stirrer
Chemicals:
·
Sodium Choride (NaCl)
·
Water
Procedure:
Weigh accurately 0.9g of salt
in watch glass and transfer into a volumetric flask then add small amount of
water stir it until it dissolves.
Now make the volume up to 100ml , note the
solution is clear.
Uses:
·
For prevention of dehydration.
·
For electrolyte replacement.
·
For flushing of wounds.
Experiment #2
Determination of solubility of in organic
compounds
Solubility:
‘’The
number of grams of solute dissolved in 100ml of solvent’’
·
According to IUPAC definition:
‘’Solubility is
analytical composition of saturated solution expressed as a proportion of
designed solute in designated solvent’’.
·
Solubility may be stated in units of
concentration, molarity, mole friction, mole ratio and other units.
·
The extent of stability of substance in
specific solvent is measured as concentration when adding more solute.
· Purpose:
To study method of
preparation of solubility and have understanding of the familiar saturated
solutions.
· Apparatus:
·
Thermometer
·
Procelain dishes and watch glasses
·
Beaker
·
Pipette
·
Hot plate
·
Chemicals:
·
Pure inorganic salts (KCl, NaCl etc).
·
Distilled water.
· Procedure:
·
Clean all glassware using detergent solution
and chromic acid solution.
·
Wash two to three times using purified water.
·
Take 50ml of distilled water in a beaker
(100ml)
·
Add some amount of salt like potassium
chloride or sodium chloride in distilled water and stir using glass rod or by
electric motor driven shaker.
·
Increase the temperature to 85 degree with
continuous stirring.
·
Maintain the temperature for few minutes than
cool down the solution.
·
Take sample at 80 degree using pipette with a
piece of paper, tied at the tip of the pipette so that the insoluble salt can
be removed.
·
Remove the piece of filter paper from the tip
of pipette and transfer 10ml of this solution in weighed porcelain dish or
water glass.
·
Allow the temperature to fall down slowly to
70, 60, 50, 40,30 degree Celsius and then to room temperature.
·
At each temperature take sample of solution
and repeat the step 7 and 8.
·
Evaporate the solution of each porcelain dish
or watch glass using direct heat or on the water bath
·
Dry the solution till constant weight.
·
Take weight of the dish using double pan
balance or chemical balance and calculate weight of the powder.
· Observations and Calculations:
·
NaCl:
·
Weight of empty china dish = W1 =
·
Weight of residue of NaCl = W2 =
·
Actual weight of NaCl = W2 – W1 =
·
Saturated NaCl =
·
30ml of solvent in which NaCl is dissolved =
·
In 30ml of solvent NaCl =
·
In 100ml of solvent NaCl =
·
KCl:
·
Weight of empty china dish =
·
Weight of KCl residue =
·
Total weight of KCl =
·
30ml of solvent in which KCl is dissolved =
·
In 30ml of solvent =
·
In 100ml solvent =
·
Result:
Solubility of the given
salt at room temperature (considering the saturated solution at room
temperature) =
Plot the graph
between solubility and temperature the graph will show a smooth curve without
any break.
Experiment # 3
Preparation of precipitation by double
displacement method
Precipitation:
A
chemical reaction that involves in the formation of an insoluble product is
called precipitation.The reactant are soluble but the product form would be
insoluble and separated out.
Apparatus:
Beaker, stirrers, weighing balance
Chemicals:
NaCl (sodium
chloride), Silver nitrate, H2O
Chemical Reaction:
NaCl + AgNO3 >
NaNO3 + AgCl2
Procedure:
Make a solution of NaOH and AgNO3 in water.
Add a few drops of NaCl solution in the reacting flask and a few drops of AgNO3
and observed a immediate cloudness that indicate the formation of precipitation
of AgCl2 forms.
Results:
Precipitate
of AgCl2 forms.
Eperiment
#4
Prepare And Dispense vanishing cream
Apparatus
Pastle and mortar,
water bath, stirrer, beaker.
Ingredients
Stearic acid…… 20g
KOH……………… 1.4g
Glycerine……….. 4g
Water…………….. qs
Perfume…………. Qs
Procedureweight given or standard amount of stearic acid in a beaker
and heat it in water bath at 70 C until it melts dissolve rest of the
ingredients in standard amount of water with continuous stirring. Gently heat
water or aquous phase at 70 C. Add water phase in oil phase with continuous
stirring cool it to 45 C and add perfume in it after that dispense in a
suitable dispensing bottle.
Uses:
. used for oily skin.
Experiment #5
Density
Definition “The
mass per unit volume at a constant temperature
and pressure is termed as density”#
Density
is a derived quantity.
It is the
characteristic property of a substance that the density of a substance is the
relationship between the mass of substance and how much space it takes up
(volume).
Formula and Unit:
The density can be determined
by:
Density = weight/volume
The unit of density in CGS is gram per
centimeter cube (g/cm).
Other Terms For Representation:
Number of terms are used to represent the mass or
weight of equal volume of different substances:
·
Absolute density
·
Apparent density
·
Relative density
·
Specific density
Absolute Density:
Absolute density is the ratio
of mass of a substance to volume of substance at specific temperature.(mass of
any substance is reffered as the weight of substance at a specific temperature)
absolute density =
mass in grams (in vaccum)/volume in milliliters
Apparent Density:
Apparent density is the ratio
of mass of a substance in air to the volume of the substance at specific
temperature.
Apparent density = mass in grams(in air)/ volume in milliliters
Relative Density:
Relative density is an expression which exhibits mass of 1ml
of a standard substances such as water at a specific temperature, relative to
water at 4 degree Celsius.
Specific Density:
Specific density may be defined as
the ratio of mass of substance to the
mass of an equal volume of another substance taken as standards
Specific density = Ws/v = Ws
Ww/v Ww
Where as weight of
substance, Ww weight of equal volume of water and V volume in milliliter.
INSTRUMENTS USED TO MEASURE DENSITY
Specific gravity may be determind by using
various types of methods using different types of equipment like
·
Pycnometer
·
Density bottle (specific gravity bottles).
Experiment
#6
Determine
the density of water at different
temperature using pycnometer:
Apparatus
·
Pycnometer
·
Thermometer
·
Beaker
·
Water bath
·
Weighting balance
Chemicals:
·
Distilled water
·
Chromatic acid solution
·
Acetone
Procedure:
Clean the pycnometer using chromic acid
solution and then rise with purified water. Rinse it again using acetone and
let it dry.
Weigh the dry pycnometer first then
fill the pycnometer with distilled water and weigh it again.
After maintaining different
temperatures (37, 42, 55, 68, 75, 85 and 95 degree Celsius ) by uing water
bath, repeat the experiment three times.
Observations:
·
Volume of pycnometer = V ml
·
Weight of empty and dry pycnometer = W1 g
·
Weight of pycnometer with water = W2 g
·
Weight of water in pycnometer = W2 – W1 g
|
Calculations:
Density of water at room temperature:
Density = weight of water at room temp
(W2-W1) / volume of pycnometer (V)
Result:
Report the result on the bases of
calculation of density (density of water decreases with increasing temperature)
It is important in case of water. Density
of water is highest i.e 1.0 at 4 degree Celsius , while increases in
temperature (above 4 degree) and decreasing (below 4 degree) of temperature of
water, density decreases.
What is a paste?
A thick soft
substance produced by mixing liquid with dry substances
Toothpaste:
Toothpaste is a paste used with a toothbrush as an accessory to clean and maintain
the aesthetics and health of teeth. Toothpaste is used to
promote oral hygiene:
it serves as an abrasive that aids in removing the dental
plaque and food from the teeth, assists in suppressing halitosis,
and delivers active ingredients (most commonly fluoride) to
help prevent tooth decay (dental caries)
and gum disease (gingivitis). Salt and sodium bicarbonate (baking
soda) are among materials that can be substituted for commercial toothpaste.
Toothpaste is not intended to be swallowed due to the fluoride content, but is
generally not very harmful if accidentally swallowed in small amounts; however,
one should seek medical attention after swallowing abnormally large amounts.
Experiment
#7
Preparation
of toohpaste
Apparatus:
·
Pestle
and mortar
·
Beaker
·
Stirrer
·
Spatula
·
Weighing
balance
Ingredients:
1.
Sodium
fluoride -2g
2.
Methyl
paraben -0.5g
3.
Sodium
alginate -3.5g
4.
Calcium
carbonate -2g
5.
Sorbital
and peppermint -2 drops
6. Water -100ml
(q/s)
Procedure:
Weigh all the
ingredients in 31.75ml of water add methyl paraben, sodium alginate, calcium
carbonate and sodium lauryl sulphate . Now make dispersion of sodium fluoride
in 10ml of water. add it to the above base and mix both the solutions and add 2
drops of sorbitol and peppermint as a flovouring agent.
Role of ingredients:
1.
Sodium
fluoride : source of fluorine
2.
Methyl
paralen : as preservative
3.
Sodium
alginate : thickening agent
4.
Calcium
caebonate : source of calcium and gives strength
5.
Peppermint
: flavour
6.
Sorbital
: flavour
Experiment
# 08
Preparation & Dispensing of Castor Oil
Emulsion
Apparatus
:
● Pestle and mortar
● Water bath
● Stirrer
● Beaker
Ingredients
:
Caster oil --------- 8ml
Gum acasia -------2g
Purified water ----- qs
Dilution Test :
● Purified water --- 60ml
Procedure
: Take
dispensing bottle with 60 ml of water in it.Wiegh 2g of gum acasia . Triturate
with 4 ml of water in mortar and pestle.triturate it in one direction , this form a mucilage. Now take 8 ml caster
oil and pour it into mucilage deep by deep with continous trituration in one
direction until a creaming paste is formed and electrating sound is produced
then add remaining water for dilution . Pour the emulsion in bottle and make up
volume upto 60 ml.
Experiment
#09
Preparation
of simple syrup
Chemicals
:
Sucrose
Distilled water
Apparatus
:
Weighing balance
Beaker
Stirrer
Procedure
:
Take 5g of sucrose in a
beaker. Properly mixed sucrose in a beaker in sufficient quantity of water.
After proper mixing finely makeup the volume with 100 ml of water.
Uses
:
It can be formulated into medicated syrup.
Experiment #10
Identification
of particle size by sieve method
Apparatus
:
Different sieve
Weighing balance
Spatula
Chemicals
:
Talcum powder
Procedure
:
Take 50g of powder though weighing balance then by
using different sieve like Mesh No 20,14,16 and pour the powder on mesh.
Desired particle size of powders can be achieved, large the mesh number smaller
the be the particle size and vice versa.
Experiment # 11
Preparation of ACP Powder
Definition of Powder
Fine,
dry particles produced by the grinding, crushing, or disintegration of a solid
substance are called powder.
ACP Powder
The powder form of Aspirin, Caffeine and Paracetamol together is known as ACP powder.
Theory
ACP powder is a dry bulk solid
composed of a fine and dry particles which are produce by the grinding, crushing, or disintegration of
solid form of Aspirin, Caffeine and paracetamol together. They can be intended for internal
as well as external use. ACP is widely used due to its therapeutic properties.
Apparatus
·
Weighting balance
·
Spatula
·
Beaker
·
Pestle and Motor
Standard formulae
·
Aspirin 250mg +
·
Paracetamol 130mg +
·
Caffeine 20mg
+
Ø Total
·
ACP = 400mg
Procedure
·
Weight all the ingredient one by one according
to the amount needed.
·
Mix them together according to geometrical
mixing .
·
Packed the mixed particles substance in a
paper sheet.
·
Now labeled it
Role of Ingredients
Aspirin
Aspirin is well recognized as an effective anti-platelet drug
for secondary prevention in subjects at high risk of cardiovascular events.
It prevent cancer diseases.
Caffeine
Caffeine
ingestion can delay fatigue during exercise, but the mechanisms remain elusive.
This study was designed to test the hypothesis that blockade of central nervous
system (CNS) .
Paracetamol
Paracetamol (acetaminophen) has been shown to be an
effective analgesic for the treatment
of moderate pain where it is chiefly indicated.
Uses
Relieving headache , muscle aches, and other minor
aches and pain. It is also used to reduce fever. It may also be used for other
conditions as determined by your doctor.
Acetaminophen/aspirin/caffeine
powder packet is an analgesic and antipyretic combination. It works by blocking
substances in the body that cause pain and inflammation. Caffeine constricts
blood vessels, which helps to relieve headaches.
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