Pharmaceutical Inorganic Chemistry Laboratory
Centro Escolar University | BS Pharmacy – 1st Semester, A.Y. 2022-2023 | MJGM
• In semi-micro qualitative analysis, small
volumes in small test tubes are used.
• Small volumes of liquids are conveniently
removed from centrifuged solids with
capillary pipets
• Liquid regents are added with medicine
droppers.
• All equipment is washed thoroughly with a
detergent solution, rinsed thoroughly with
tap water, and finally rinsed with distilled
water.
• All equipment must be clean because
traces of impurities may interfere with
many qualitative tests.
• Ordinary medicine droppers deliver about
1mL per 20 drops.
• Capillary pipets, with small tips, deliver
approximately 1 mL per 40 drops.
• Chemical process where two aqueous
solutions are combined to produces an
insoluble product or salts known as
precipitate.
• A precipitation reaction occurs can be
determined by using the solubility rules for
common ionic solids, because not all
aqueous reaction form precipitates and
one must consult the solubility rules.
1. Alkali metal (Group IA) compounds are
soluble.
2. Ammonium (NH4+) compounds are
soluble.
3. Nitrates (NO3-), chlorates (CIO3-), and
perchlorates (CIO4-) are soluble.
4. Most hydroxides (OH-) are insoluble.
The exceptions are the alkali metal hydroxides
and Ba(OH)2, Ca(OH)2 is slightly soluble.
5. Most chlorides (CI-), bromides (Br) or
iodides (I-) are soluble. The exceptions
are those containing Ag+, Hg+2, and
Pb+2.
6. Carbonates (CO3-2), phosphates (PO4)
and sulfides (S-2) are insoluble.
7. Most sulfates (So4-2) are soluble.
CaSO4 and Ag2SO4 are slightly
soluble.
BaSo4, HgSO4, and PbSO4 are
insoluble.
Two types of test tubes are available for this
purpose:
1. Tapered test tubes with a capacity of
approximately 5mL and
2. The ordinary 10mL test tubes.
• The only advantage of the tapered type is
that by its structure it tends to magnify the
size of the precipitate it contains.
• It is then generally preferred to carry out
all precipitation in ordinary test tubes.
• When a precipitation reaction is carried
out, one must check for the completeness
of precipitation.
• This is done by centrifuging the reaction
mixture at full speed for approximately 1
minute, adding one drop of the
precipitating reagent to the clear solution,
and observing carefully to see whether
additional precipitate forms.
• Repeat the procedure until the addition of
a drop of the reagent; no precipitate s
formed in the layer of the solution.
• This marks the point when enough
reagents have been added.
• A large excess of the reagent should be
avoided since it may increase the solubility
of the precipitate or may form soluble
compounds containing complex ions and
may interfere with succeeding operations.
• Many precipitation reactions result in the
formation of colloidal particles, that are too
small to be separated from the liquid
Pharmaceutical Inorganic Chemistry Laboratory
Centro Escolar University | BS Pharmacy – 1st Semester, A.Y. 2022-2023 | MJGM
phase by filtration or by centrifuging the
mixture.
• Colloidal suspensions can usually be
coagulated by heating the mixture in a
water bath for a few minutes. This process
is called digestion.

True Solution – Size < 1nm

Colloidal Solution – Size between 1-100nm
Suspension Solution – Size > 100nm

• Is 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.
• Gravity filtration uses a glass funnel
with a stem and filter paper folded
using a basic technique or fluted type.
• The paper is folded in half, then folded
in quarters, and the tip of one corner is
torn off to allow for a snug fit in the
funnel cone.
• Open filter paper cone and line funnel.
• Tear off the corner. Fluted filter paper
is often better for gravity filtration with
organic solvents.
• A diagram of how to fold fluted filter
paper is shown below.
• In semi-micro procedures, the process of
filtration is replaced by the use of a
centrifuge.
• The centrifuge is a device by which a
centrifugal force produced by an electric
motor speed up the rate of settling of a
precipitate.
• Precipitate will usually settle, in a good
centrifuge, in less than a minute's time. A
balance tube containing a volume of water
equal to the volume of solution to be
centrifuged is always placed in the
centrifuge exactly opposite the solution.
• *An unbalanced load in the centrifuge will
cause severe vibration and damage the
centrifuge's bearings.
Pharmaceutical Inorganic Chemistry Laboratory
Centro Escolar University | BS Pharmacy – 1st Semester, A.Y. 2022-2023 | MJGM
Removal of Supernatant Liquid:
• ▪ After a mixture has been centrifuged, the
tube should be held at an angle so that the
liquid (centrifugate) can be easily drawn
into a capillary pipet.
• Supernatant is often used to describe a
clear solution above the precipitate.
However, the term centrifugate is more
descriptive in this case.
• Avoid disturbing the precipitate as the
liquid is withdrawn. At times, bits of
precipitate may be drawn into the capillary
pipet with the liquid.
• To prevent this, wind a very small piece of
cotton around the end of the capillary pipet
to serve as a filter.
• The clear centrifugate is usually
transferred to another test tube.
Washing of Precipitate
• After the removal of the centrifugate, the
precipitate is wet with the solution
containing ions of the centrifugate.
• The ions may cause interference in the
analysis of the precipitate and are usually
removed by washing.
• Washing is done by adding the required
amount of distilled water (about 5 drops)
mixing thoroughly with a stirring rod and
then centrifuged.
• The first wash liquid should be added to
the separated solution(centrifugate) by
means of a capillary pipet or micropipette.
• Usually a precipitate is washed twice, and
the second wash liquid is discarded.
Dissolving Precipitates
• it is possible that sometimes the volume of
the solvent suggested in the procedure
may not totally dissolve a given precipitate
or solid.
• In such cases, centrifuge, decant the
mixture, and save the solution.
• Then add more of the same solvent to the
precipitate or solid to see if it will not
dissolve some more.
• Repeat the process until no significant
results are obtained; then combine all the
solutions obtained.
• This method is often used to reduce
the volume of the solution. Heating a
solution contained in a test tube within
a water bath is a time-consuming
process.
Evaporation may be accomplished in two ways:
• The solution is placed in a small
evaporating dish or casserole and
heated gently until the liquid has been
reduced.
• Extreme caution must be exercised in
evaporating small amounts of liquid
since very little heat is required.
• Once the evaporating dish or
casserole becomes hot, it may remain
above the boiling point of water for
some time even after the flame has
been removed.
• The heat of the dish is sufficient to
complete the evaporation.
• It can be done from test tubes.
• The tube is held at an angle with the tip of
a very small flame directed at the upper
surface of the liquid. A stirring rod is
inserted into the test tube and rotated
constantly to break up bubbles of steam,
which may cause the solution to "bump"
out of the test tube.
• NEVER POINT A TEST TUBE TOWARDS
YOURSELF OR ANOTHER PERSON
WHILE EVAPORATION IS BEING DONE.
Heating Liquids
• A small test tube containing a solution or
mixture cannot be safely heated over a
direct flame, since "bumping" would cause
the loss of part or all of the liquid.
• The most satisfactory method of heating
solution in a test tube is in a water bath.
The beaker (can be used as a water bath)
Pharmaceutical Inorganic Chemistry Laboratory
Centro Escolar University | BS Pharmacy – 1st Semester, A.Y. 2022-2023 | MJGM
should be ¾ filled with water and heated response to the surface of the container. It
to simmering during the entire time of an can be either convex or concave.
analysis. • A convex meniscus will occur when the
molecules in your sample have a stronger
attraction to each other than to the
container.
• Whenever it is directed to make a • Conversely, a concave meniscus will
solution acid or alkaline, add from a occur when the molecules of the sample
graduated cylinder an amount of acid or are more attracted to those of the
alkaline solution less than what is needed
container than to themselves.
in order to neutralize the acid or alkali
known to be present in solution.
• Then add some more of the acid or alkali
drop by drop, at the same time stirring the
solution. With a piece of litmus paper on
a watch glass, test the solution for its
acidity or alkalinity as the case maybe. It
is not a good practice to put the litmus
paper into the solution. The solution may
be dropped by the use of a glass
• rod tip on the litmus paper on the watch
glass.
• DO NOT USE THE LITMUS PAPER
MORE THAN ONCE.
• To make a solution ammoniacal, add
NH3 solution or NH4OH, shaking it for a
• while until a distinct odor of the vapor is
perceptible.

Using the Pipette

MEASURING LIQUIDS
The volume of liquids is ordinarily measured using
a graduated cylinder.
Other volume-measuring devices are the pipet,
buret, and volumetric flask.
• When a liquid is held in a glass vessel, the
surface of the liquid curves.
• The curve is the meniscus and it is where
the height of the liquid is read.
• The meniscus is the curved upper surface
of a column of liquid which is produced in
1. Select the pipette that will deliver the
appropriate volume of liquid for your needs.
2. Always use both hands when operating the
pipette, one hand for the pipette pump(aspirator)
and the other hand to support the pipette.
3. When filling the pipette, keep the tip of the
pipette below the surface of the sample as the
sample is drawn into the pipette.
4. Fill the pipette.
5. To release the liquid in a volumetric pipette,
hold the pipette and allow liquid to drain.
Using the Volumetric Flask
1. Measure and add the solute for the solution.
2. Add enough solvent to dissolve the solute.
3. Continue to add solvent until you are near the
line marked on the volumetric flask.
Pharmaceutical Inorganic Chemistry Laboratory
Centro Escolar University | BS Pharmacy – 1st Semester, A.Y. 2022-2023 | MJGM
4. Use a pipette or dropper to fill the volumetric
flask, using the meniscus of the solution and the
line on the flask to determine your endpoint.
5. Seal the volumetric flask and invert it to
thoroughly mix the solution.
Using the Burette
1.Wash the burette with soap and water.
2.Wash the burette with the new solution.
3.Eliminate air bubble before use.
4.Fill the burette with the solution.
5.Drain the solution slowly by rotating the
stopcock.
MEASURING SOLIDS
▪ The mass of an object is determined by a
balance. In the laboratory, several types of
balances are used depending on the degree of
accuracy required.
▪ The balances available in the laboratory are the
platform balance, beam balance, and analytical
balance. Using the Top loading/Analytical
Balance
▪ With nothing on the pan, set it to zero by
pressing the "on" button.
▪ Place weighing bottle/paper, beaker, or vial on
balance and set to zero again.
▪ Use a clean spatula to transfer the sample into
the container slowly, until you reach the desired
mass.
Note: If you are using an analytical balance, close
all the doors before taking measurements
Using Double Pan/Beam Balance
▪ The beams are calibrated in grams.
▪ The upper beam is divided into ten major units
of 1 gram each.
▪ Each of these units is further divided into units of
1/10 of a gram.
▪ The lower beam is equal to 10 grams.
▪ The lower beam can be used to find the masses
of objects up to 200 grams.
▪ Each beam has a rider that is moved to the right
along the beam.
▪ The rider indicates the number of grams needed
to balance the object in the left pan.
Before using the balance, be sure that the pans
are empty and both riders are set to zero.
If the pointer does not read zero, slowly turn the
adjustment knob.
Procedure in using the balance;
1. Place the object to be weighed in the left pan.
2. Place the standard masses on the right pan.
3. Be sure that the pointer indicator should be at
zero, meaning, the left and right pans are
balanced.
4. Count the number of standard masses. It is
equivalent to the mass of the object weighed.
Using Triple Beam Balance
▪ The triple beam balance is a single-pan balance
with three beams calibrated in grams.
▪ The front beam or 100-gram beam is divided
into ten units of ten grams each.
▪ The middle or 500-gram beam is divided into
five units of 100 grams each.
▪ The back beam or 10-gram beam is divided into
10 major units of 1 gram each.
Procedure for using the balance:
1. Place the object to be weighed on the pan.
2. Move the rider on the middle beam notch by
notch until the horizontal pointer drops below
zero. Move the rider back to one notch.
3. Move the rider on the front beam notch by
notch until the pointer again drops below zero.
Move the rider back to one notch.
4. Slowly slide the rider along the back beam until
the pointer stops at the zero point.
5. The mass of the object is equal to the sum of
the readings on the three beams