Practical: 1
FILTRATION
Filtration, the technique used to separate solids from liquids, is the act of pouring a mixture onto
a membrane (filter paper) that allows the passage of liquid (the filtrate) and results in the collection
of the solid. Two filtration techniques are generally used in chemical separations in general chemistry
lab: "gravity" filtration and "vacuum" filtration.
Aim: To separate solid from liquid using gravity filtration.
Requirements: Funnel, filter paper, clamp, glass rod
Procedure: Gravity filtration uses a polyethylene or glass funnel with a stem and filter paper. Filter
paper can have pore sizes ranging from small to large to permit slow to fast filtering. The paper is
folded in half (Figure 1), then folded in quarters, and the tip of one corner is torn off to allow for a
snug fit in the funnel cone. (If the paper has been pre-weighed, the torn corner piece must be saved
to add to the post-filter weighing to avoid any errors.) The paper cone is fitted to the funnel so three
thicknesses of the paper line one-half of the cone and one thickness lines the opposite half (Figure
1). Now place the funnel into a beaker and wet the filter paper completely with the dominate solvent
or solvents in the mixture to be filtered. This step adheres the filter paper to the funnel walls
preventing solid from escaping. Then, support the funnel with a clamp or ring (if necessary) and
place a clean beaker beneath the funnel so the stem rests against the side of the beaker (this prevents
splattering).
Before filtering, allow most of the solid in the mixture to settle. Now pour the supernatant liquid (the
liquid standing over the solid in a mixture) through the filter first. This will allow the initial part of
the filtration to proceed faster and may prevent clogging of the filter by the solid. To prevent
splattering pour the liquid down a glass rod as shown in Figure 2.
Scrape the solid onto the filter with a rubber policeman or spatula. Rinse the spatula, glass rod and
beaker and pour the washings into the filter funnel. If the remaining solid residue is to be washed,
rinse with three small portions (a few milliliters each) of an appropriate solvent. If the solid is to be
saved, remove the filter paper carefully and place it on a watch glass to dry.
Observation: The solid is separated from liquid.
Result: The solid is separated from liquid. The weight of the solid…………….g.
Practical: 2
Aim: To separate solid from liquid using vacuum filtration.
Requirements: Buchner Funnel, side arm conical flask, filter paper, clamp, glass rod
Procedure:
Vacuum (or Suction) Filtration
Vacuum filtration uses a Buchner (pronounced "byook-ner") funnel and a water aspirator assembly.
A Buchner funnel is a flat bottomed, porous, circular porcelain bowl with a short stem. The stem is
fitted with a rubber stopper and inserted in the mouth of a side arm filter flask. Circular filter paper,
the same diameter as the bowl, is placed on the flat bottom and wetted with the appropriate solvent
to create a seal before starting the filtration.
The hose in the above figure is attaches the side arm of the filter flask to a vacuum aspirator/vacuum
pump. To filter a sample, turn on the aspirator and carry out the filtration in the same manner
described for gravity filtration. (Note: NEVER pry off the funnel if the system is under vacuum!
Water can flash back into the collection flask or the filter paper can be damaged resulting in the loss
of filtered solid.) Turn off the water aspirator before carefully removing the wet filter paper without
tearing.
Observation: The solid is separated from liquid.
Result: The solid is separated from liquid. The weight of the solid…………….g.
Practical: 3
(Crystallization)
Aim: Purification of the impure organic solid compound.
Requirements: Solvents, Bunsen burner, stands, evaporating dish, Petri dish, filter paper,beaker,
funnel.
Crystallization:
Crystallization is a process whereby solid crystals are formed from another phase, typicallya liquid
solution or melt.
Precipitation:
Precipitation is another word for crystallization but is most often used when crystallizationoccurs
very quickly through a chemical reaction.
Procedure:
1) Find out the solubility of organic compounds in various solvents.
2) Take some amount of solvent in the beaker and add impure organic solid compound till
the saturated point is reached.
3) Filter the solution to remove any insoluble impurity that is present.
4) Heat the solution and reduce its volume to one-third.
5) Filter the solution and separate it into an evaporating dish. And wait for crystallizationto
start. Or you can keep the evaporating dish in the water-containing trough to increase the
crystallization process. Cover it with the Petri dish.
6) After some time nearly half an hour, a pure form of organic solid compound crystal was
observed.
7) Separate the pure crystals by filtration, wash with a cold solvent to remove the impurities
on the surface, and dry.
Observation:
Solvent required to make saturated solution:
Shape of the crystals: ………………..
Colour of the crystals: ………………..
Weight of the crystals: ………………..
Result: The pure solid crystals of substance is obtained after crystallization.
Practical: 4
(Sublimation)
Aim: Purification of organic solid compound mixture through sublimation.
Requirements: Bunsen burner, stands, beaker, round bottom flask.
Sublimation: Certain organic solids on heating directly change from a solid to a vapor state without
passing through a liquid state. These substances are sublimable. This process is sublimation.
Procedure:
1. Place a mixture of 1 gm. of one of the sublimed substances and 5 gm. of any other organic
compound (e. g. benzoic acid and glucose) in a 250 ml beaker, covered with a round-
bottomed flask.
2. Filled with cold water, the beaker is placed on a sand bath or a very low flame.
3. The sublimed substance (i, e. the benzoic acid) will collect on the bottom of the cold
flask and the side walls of the beaker in pure, crystalline form.
4. Scrap the sample of sublimed material from the flask and beaker.
5. Collect in a small flask, weigh, and determine the M.P. of the pure substance.
Observation: M.P. of obtained crystal: ____________
M.P. of original sample: ____________
Difference in M.P.= _____________
Mass of the pure crystals: _____________
Result: The sublimed crystals are of and its melting point is__________.
Practical: 5
(Fractional Crystallization)
Aim: Purification of organic solid-solid compound.
Requirements: Solvents, Bunsen burner, stands, petri dish, test tube, filter paper, beaker.
Fractional crystallization is a method of refining substances based on differences in their solubility.
It fractionates via differences in crystallization (forming of crystals). If a mixture of two or more
substances in solution are allowed to crystallize, for example by allowing the temperature of the
solution to decrease or increase, the precipitate will contain more of the least soluble substance. The
proportion of components in the precipitate will depend on their solubility products.
Procedure:
The two acids differ in their solubilities in warm water (40°C). Cinnamic acid is insoluble in water
at this temperature and benzoic acid is soluble. And, therefore, these two acids can be separated by
fractional crystallization using warm water (40°C) as a solvent. A mixture of 2 g each of the above
acids is placed in a 100 ml beaker and 30 ml of warm water (40°C) is added to it. The mixture is
stirred for 5 minutes on a hot water bath. The temperature of the mixture is to be maintained at
40°C. The contents of the mixture are allowed to settle down and the supernatant liquid is filtered
while hot using a hot water funnel. The filtrate is collected in another beaker. The residue left in the
first beaker, is treated similarly with warm water four times and then the final residue is
recrystallized from boiling water. The product cinnamic acid hence obtained, is checked for purity
by melting point determination (i.e., 133°C). All the filtrates are combined in 250 ml beaker and is
concentrated down to 20 ml. On cooling, benzoic acid is crystallized out, which is further purified
by recrystallization from hot water. The purity of benzoic acid is also checked by melting point
determination (i.e., 121°C). In addition, the left cinnamic acid is recrystallized to get pure cinnamic
acid.
Observation:
M.P. of benzoic acid after crystallization:
M.P. of cinnamic acid after crystallization:
Result: The obtained crystals of benzoic acid and cinnamic acid are pure having melting
points ________and______, respectively.
Practical: 6
Aim: Purification of the liquid using simple distillation.
Requirements: Water, Boiling stones, Bunsen burner, clamps, Ring (support), stands, three-way
adapter, Distillation flask, condenser, water pipes, receiving flask, adapters, Thermometer.
Procedure:
1) Take liquid in the distillation flask. Add two boiling stones to the flask.
2) Clamp the distillation flask to a support stand. Adjust the height of the distillation flask so
that its position will be above the Bunsen burner flame.
3) Place the three-way adapter in the distillation flask. Place the thermometer pocket having
paraffin oil into the upper side of the three-way adapter and insert the thermometer so we
can measure temperature during distillation then place the condenser sidewise in the three-
way adapter with a support stand.
4) Connect water tubes with inlet and outlet of Condenser.
5) At last clamp the condenser outlet with receiving flask and check the full assembly
connected well.
6) Turn on the water through the condenser and start the Bunsen burner with low flame and
check the temperature in the thermometer.
7) Observe the temperature change as the vapor rises in the distillation apparatus and the
temperature of the vapor increases. Observe the boiling point boiling liquid. Wait for the
temperature to reach the liquid's boiling point and then collect the liquid till the
temperature remain at its boiling point.
8) Turn off the Bunsen burner and allow the glassware to cool before dismantling the
distillation apparatus.
Simple distillation diagram
Observation: Boiling point of liquid: _______________
Volume of collected liquid:____________
Result: The given liquid is ___________.
Practical: 7
(Simple Distillation)
Aim: Purification of the miscible organic liquid-liquid mixture using simple distillation.
Requirements: Water, Boiling stones, Bunsen burner, clamps, Ring (support), stands, three-way
adapter, Distillation flask, condenser, water pipes, receiving flask, adapters, Thermometer.
Procedure:
1) Take liquid-liquid mixtures in the distillation flask. Add two boiling stones to the flask.
2) Clamp the distillation flask to a support stand. Adjust the height of the distillation flask so
that its position will be above the Bunsen burner flame.
3) Place the three-way adapter in the distillation flask. Place the thermometer pocket having
paraffin oil into the upper side of the three-way adapter and insert the thermometer so we
can measure temperature during distillation then place the condenser sidewise in the three-
way adapter with a support stand.
4) Connect water tubes with inlet and outlet of Condenser.
5) At last clamp the condenser outlet with receiving flask and check the full assembly
connected well.
6) Turn on the water through the condenser and start the Bunsen burner with low flame and
check the temperature in the thermometer.
7) Observe the temperature change as the vapor rises in the distillation apparatus and the
temperature of the vapor increases. Observe the boiling point range of lower-temperature
boiling liquid and separate the first liquid at that temperature till the temperature does not
start increasing.
8) After separating the first liquid, change receiving flask to collect the second liquid. Wait
for the temperature to reach the second liquid's boiling point and then collect the second
liquid till the temperature remain at its boiling point.
9) Turn off the Bunsen burner and allow the glassware to cool before dismantling the
distillation apparatus.
Simple distillation diagram
Observation:
1. Volume of the given liquid mixture: _____________.
2. Boiling point of liquid 1: ____________.
3. Volume collected of liquid 1: _________.
4. Boiling point of liquid 2: ____________.
5. Volume collected of liquid 2: _________.
Result:
1. Liquid 1: Boiling point of liquid: Volume collected:
2. Liquid 2: Boiling point of liquid: Volume collected:
Practical: 8
(Fractional Distillation)
Aim: Purification of miscible organic liquid-liquid mixture using fractional distillation.
Requirements: Water, Boiling stones, Bunsen burner, clamps, Ring (support), stands,
Distillation flask, Fractional Column, condenser, receiving flask, adapters, Thermometer.
Procedure:
1) Fill the distilling flask with liquid-liquid mixtures. Add two boiling stones to the flask.
2) Clamp the distilling flask to a support stand. Adjust the height of the distilling flask and
connect it with the fractional column.
3) Place the thermometer into the adapter of the fractional column so we can measure the
temperature of distillation and clamp the fractional column with a condenser with a support
stand.
4) Condenser connects with the inlet and outlet water pipe.
5) In the last clamp condenser outlet with receiving flask and check full assembly is connected
well.
6) Turn on the water through the condenser and start the Bunsen burner with low flame
andcheck the temperature in the thermometer.
7) Observe the temperature change as the vapor rises in the distillation apparatus and the
temperature of the vapor increases. Observe the boiling point range and separate the first
liquid at that temperature.
8) After separating the first liquid collect from receiving flask and checking the second
liquid’s boiling point separate and collect.
9) Turn off the Bunsen burner and allow the glassware to cool before dismantling the
distillation apparatus.
Observation:
Boiling point of liquid, Vapor Temperature of liquids, Portion of collected liquid.
Result:
1. Liquid 1: Boiling point of liquid: Volume collected:
2. Liquid 2: Boiling point of liquid: Volume collected:
Practical: 9
(Determination of Boiling point)
Aim: Determination of the boiling point of the organic liquid-liquid mixture using a distillation
process.
Requirements: Water, Boiling chips, Bunsen burner, clamps, Ring (support), stands, Distillation
flask, condenser, receiving flask, adapters, Thermometer.
Procedure:
1) Take liquid-liquid mixtures in the distillation flask. Add two boiling chips to the flask.
2) Clamp the distillation flask to a support stand. Adjust the height of the distillation flask so
that its position will be above the Bunsen burner flame.
3) Place the three-way adapter in the distillation flask. Place the thermometer pocket into the
upper side of the three-way adapter and insert the thermometer so we can measure
temperature during distillation then place the condenser sidewise in the three-way adapter
with a support stand.
4) Connect water tubes with inlet and outlet of Condenser.
5) At last clamp the condenser outlet with receiving flask and check the full assembly
connected well.
6) Turn on the water through the condenser and start the Bunsen burner with low flame and
check the temperature in the thermometer.
7) Observe the temperature change as the vapor rises in the distillation apparatus and the
temperature of the vapor increases. Observe the temperature i.e., the boiling point of lower
temperature boiling liquid when the first liquid at that temperature starts going into the
collecting flask. Continue the separation till the temperature does not start increasing.
8) After separating the first liquid, change receiving flask to collect the second liquid. Wait
for the temperature to reach the second liquid's boiling point, note this temperature, and
collect the second liquid till the temperature remains at its boiling point.
9) Turn off the Bunsen burner and allow the glassware to cool before dismantling the
distillation apparatus.
Observation: Boiling point of liquid 1:
Boiling point of liquid 2:
Result:
1. Liquid 1: Boiling point of liquid: Volume collected:
2. Liquid 2: Boiling point of liquid: Volume collected:
Practical: 10
(Vacuum/reduced pressure Distillation)
Aim: Purification of a liquid through ditillation at reduced pressure.
Requirements: Water, Boiling stones, Bunsen burner, clamps, Ring (support), stands, Distillation
flask, Vacuum pump, vacuum adapter condenser, receiving flask.
Procedure:
1) Fill the distilling flask with the mixtures. Add two boiling stones to the flask.
2) Clamp the distilling flask to a support stand. Adjust the height of the distilling flask and
connect it to the condenser.
3) Clamp the distilling flask and condenser with the vacuum adapter with a support stand and
connectthe vacuum pump with the vacuum adapter.
4) Condenser connects with the inlet and outlet water pipe.
5) In the last clamp condenser outlet with receiving flask and check full assembly is connected
well.
6) Turn on water through the condenser and start the Bunsen burner with low flame and start
the vacuum pump with low pressure.
7) Observe the changes when temperature rises and risen vacuum pressure when vapor rises
inthe distillation apparatus at that time temperature is constant and up and down vacuum
pressure only and separate the first liquid from the mixture.
8) After separating the first liquid collect it from receiving flask and separating in the other
flask. And the same process collects the second liquid.
9) Turn off the Bunsen burner and vacuum pump and allow the glassware to cool before
dismantling the distillation apparatus.
Observation:
Reduced Pressure:________________.
Boiling point of liquid at Atmospheric pressure:__________.
Boiling point of liquid at reduced pressure: ___________.
Time for removal of the solvent:____________.
Result: The purification of liquid at reduced pressure save time and energy.
Practical: 11
(Melting Point)
Aim - To determine the melting point of a given solid substance.
Requirements – Given Solid Substance, Capillary Tube, Paraffin, Laboratory thermometer,
Melting point apparatus.
Theory- The change from solid to liquid state of a compound in heating is called melting, and
the temperature at which a solid melts in its pure form is called the melting point. Every pure
solid has melting point characteristics; therefore, the determination of melting point helps
identify the compound. The presence of impurities lowers the melting point of the solid. Thus,
the Melting point also serves as a criterion for the purity of a compound.
Procedure-
1. Take a fine capillary of length 5-6cm. Seal its one end by inserting the end of the
capillary tube horizontally into the extreme edge of a small, steady Bunsen flame for a
few seconds, rotating the capillary meanwhile.
2. Take a small quantity of the compound whose melting point is to be determined on a
porous plate and powder it with a spatula.
3. Introduce the powdered compound in the capillary tube by introducing the open end of
the capillary tube into the powdered compound and gently rotating it. Gently tap the
capillary tube against the porous plate so the compound sinks into the closed end.
Repeat the procedure of introducing and tapping three to four times.
4. Place the thermometer with the capillary tube in the melting point apparatus containing
at least two-thirds of its volume of liquid paraffin in such a way that the closed end of
the capillary remains below the surface of the Liquid paraffin.
5. Now start heating at 2 oC/min. and note down the temperature from time to time and
finally note down the temperature at which the compound starts melting and completely
melts.
Precaution-
1. The capillary tube is filled one third of its length.
2. The rate of heating should be controlled. It should be very slow near the melting point so
that the melting point can be recorded accurately.
Observation:
Melting point 1) ……………………oC
2) ……………………oC
Result:
The melting point of given substance is___________
