PRACTICAL CHEMISTRY

Introduction

Scientific subjects are, by their nature, experimental. It is accordingly important that

an assessment of a student’s knowledge and understanding of Chemistry should
contain a component relating to practical work and experimental skills. This booklet
has been produced to help students preparing for and taking practical Examinations.
The material contained in this booklet does not extend the curriculum specification
content. Rather it seeks to help the candidate succeed in practical examination by
explaining in more depth what is required of him or her in carrying out the exercises,
making observations and measurements with appropriate precision and recording
these methodically. This booklet advices candidate on how he or she should
interpret, explain, evaluate and communicate the results of the exercises clearly and
logically using relevant chemical knowledge and understanding and using
appropriate specialist vocabulary.

1.1APPARATUS IN A CHEMISTRY LABORATORY

1.2 SPECIAL LABORATORY APPARATUS AND TECHNIQUES

(a) USING THE BURETTE

A burette is used to deliver solution in precisely measured, variable volumes.

Burettes are used primarily for titration, to deliver one reactant until the precise end
point of the reaction is reached. To fill a burette, close the stopcock at the bottom
and use a funnel. You may need to lift up on the funnel slightly, to allow the solution
to flow in freely.
You can also fill a burette using a disposable transfer pipette. This works better than
a funnel for the small, 10 mL burettes. Be sure the transfer pipette is dry or
conditioned with the titrant, so the concentration of solution will not be changed.

Before titrating, condition the burette with titrant solution and check that the burette
is flowing freely. To condition a piece of glassware, rinse it so that all surfaces are
coated with solution, then drain. Conditioning two or three times will insure that a
stray drop of water does not change the concentration of titrant.
Rinse the tip of the burette with water from a wash bottle and dry it carefully. After a
minute, check for solution on the tip to see if your burette is leaking. The tip should
be clean and dry before you take an initial volume reading.
When your burette is conditioned and filled, with no air bubbles or leaks, take an
initial volume reading. A burette-reading card with a black rectangle can help you to
take a more accurate reading. Read the bottom of the meniscus. Be sure your eye is
at the level of meniscus, not above or below. Reading from an angle, rather than
straight on, results in a parallax error.

Deliver solution to the titration flask by turning the stopcock. The solution should be
delivered quickly until a couple of mL from the endpoint. The endpoint should be
approached slowly, a drop at a time. Use a wash bottle to rinse the tip of the burette
and the sides of the flask. Your TA can show you how to deliver a partial drop of
solution, when near the endpoint.

(b) Volumetric (measuring) Flasks

Erlenmeyer flasks and beakers are used for mixing, transporting, and reacting, but
not for accurate measurements. The volumes stamped on the sides are approximate
and accurate to within about 5%.
 (c) Graduated Cylinders
Graduated cylinders are useful for measuring liquid volumes to within about 1%.
They are for general-purpose use, but not for quantitative analysis.

If greater accuracy is needed, use a pipette or volumetric flask.

(d) Pipette
A pipette is used to measure small amounts of solution very accurately. A pipette
bulb is used to draw solution into the pipette.
Start by squeezing the bulb in your preferred hand. Then place the bulb on the flat
end of the pipette.
Place the tip of the pipette in the solution and release your grip on the bulb to pull
solution into the pipette. Draw solution in above the mark on the neck of the pipette.
If the volume of the pipette is larger than the volume of the pipette bulb, you may
need to remove the bulb from the pipette and squeeze it and replace it on the
pipette a second time, to fill the pipette volume completely.
Quickly, remove the pipette bulb and put your index finger on the end of the pipette.
Gently release the seal made by your finger until the level of the solution meniscus
exactly lines up with the mark on the pipette. Practice this with water until you are
able to use the pipette and bulb consistently and accurately.

(e) Volumetric Flask

A volumetric flask is used to make up a solution of fixed volume very accurately. This
volumetric flask measures 500 mL ± 0.2 mL. This is a relative uncertainty of 4 x 10 -4
or 400 parts per million.

To make up a solution, first dissolve the solid material completely, in less water than
required to fill the flask to the mark.

After the solid is completely dissolved, very carefully fill the flask to the 500 mL mark.
Move your eye to the level of the mark on the neck of the flask and line it up so that
the circle around the neck looks like a line, not an ellipse. Then add distilled water a
drop at a time until the bottom of the meniscus lines up exactly with the mark on the
neck of the flask. Take care that no drops of liquid are in the neck of the flask above
the mark.
After the final dilution, remember to mix your solution thoroughly, by inverting the
flask and shaking.

(f) Analytical Balance

An analytical balance measures masses to within 0.0001 g. Use these balances when
you need this high degree of precision.
Turn the balance on by pressing the control bar. The display lights up for several
seconds, then resets to 0.0000.
Place creased, small weighing paper on the balance pan.
Close the sliding glass doors. Wait for the green dot on the left to go out. This is the
stability indicator light, indicating that the weight is stable.
Press the control bar to cancel out the weight of the container or paper. The display
will again read 0.0000. Carefully add the substance to be weighed up to the desired
mass. Do not attempt to reach a particular mass exactly. Before recording the mass,
close the glass doors and wait until the stability detector lamp goes out. Record mass
of solid.
Don't pick up tare containers with bare hands since your fingerprints add mass. Use
tongs to prevent this.

Don't lean on the bench while weighing.

Do record the mass of your container, if you will need it later.

Do check the level indicator bubble before weighing. The two rear balance feet serve
as levelling screws. Use the brush provided to clean spills in the weighing chamber.
Discard any disposable tare containers or weighing paper, in the nearest
wastebasket.

(g) Calorimetry
Calorimetry is used to determine the heat released or absorbed in a chemical
reaction. The calorimeters shown here can determine the heat of a solution reaction
at constant (atmospheric) pressure. The calorimeter is a double Styrofoam cup fitted
with a plastic top in which there is a hole for a thermometer.

(It's crude, but very effective!) Key techniques for obtaining accurate results are
starting with a dry calorimeter, measuring solution volumes precisely, and
determining change in temperature accurately.

(h) Using a Calorimeter

Solutions volumes should be carefully measured with a graduated cylinder. Add
solution completely, to a dry calorimeter. Don't forget to add the spin bar each time!
Set up the calorimeter with the thermometer (0° to 50°C, graduated every 0.1°C)
supported from a stand so that the bulb does not touch the bottom of the cup. Note
that the thermometer used for calorimetry differs from the less accurate one in your
glassware drawer. Clamp the calorimeter so that it rests on the stirrer. Be careful not
to turn on the heat or you will melt the Styrofoam.
The change in temperature is determined by measuring the initial temperature, T 1, of
the reactants, and the maximum temperature, T2, of the contents of the calorimeter
during the exothermic reaction. Use a magnifying glass to measure temperature
values precisely.
Interpolate between the divisions of the thermometer and record temperatures to +/-
0.01 °C. See your lab manual for a discussion of how to determine accurately the
change in temperature from your graph of temperature vs. time.

(i) Top-loading Balance

Use a top loading balance to weigh solid material when a precision of 0.1 g is
adequate. For more accurate mass measurements or small amounts, use an
analytical balance.

Using a Top-loading Balance

Check if the balance is turned on. If not, press the on/off button and wait until the
display reads 0.0 g. Place a container or large, creased weighing paper on the
balance pan. Push tare button to zero the balance. Carefully add substance to the
container or paper. Record the mass. Use the brush provided to clean any spills.
Discard any disposable tare containers or weighing paper in the nearest wastebasket.

GENERAL EXPERIMENTAL PROCESSES

Quantitative Transfer
Quantitative Transfer simply means that all the material to be transferred from one
place to another must make the trip. For example, every particle of solid must be
transferred from the weighing paper to the (clean) beaker.
This can be done be carefully tipping the creased weighing paper to pour the solid
into the beaker. Tapping the paper with a spatula will knock particles into the beaker.
Finally, the paper should be rinsed into the beaker, to remove all traces of the solid.

Transferring a Solution or Mixture

If you are transferring a solution or heterogeneous mixture to another vessel, rinse
the container with solvent to be sure the transfer is quantitative. The rinsing should
be transferred to the second vessel along with the rest of the mixture or solution.

Titration
A titration is a method of analysis that will allow you to determine the precise
endpoint of a reaction and therefore the precise quantity of reactant in the titration
flask. A burette is used to deliver the second reactant to the flask and an indicator or
pH Meter is used to detect the endpoint of the reaction.

COMMON LABORATORY EXPERIMENTAL PROCEDURES

1. BUNSEN BURNER
(i) Close the air hole and turn the gas tap full on. Light the gas and hold a piece of
wire in different parts of the flame, moving it from the bottom to the top. Note the
hottest place in the flame. Open the air hole. Again hold the wire in the flame,
moving from the bottom to the top. Note the hottest place in the flame. Compare the
two flames and note which has the hottest point.
(ii) Close the air hole. Hold a test-tube with its bottom end just above the flame.
Carbon deposits on the glass. To test whether unburned carbon gives the yellow
colour to the flame, sprinkle powdered charcoal into the flame to see if this gives the
same effect.
(iii) Open the air hole again. Note whether carbon deposits on a test-tube held in this
flame. Air mixing with the gas helps it to burn more rapidly and efficiently. To test
what is in the cooler inner cone hold a splint of wood in the flame so that it passes
through the inner cone. Note which part of the splint burns. Hold a piece of glass
tubing with one end in the inner cone then ignite the gas that comes out of the other
end.
(iv) Investigate a candle flame and the flame of a spirit lamp in a similar way. Find
the hottest part of the flame. Test for unburned carbon particles in the flame. Look
for an inner cone of unburned gases.

IDENTIFICATION OF PURE SUBSTANCES

2. Melting points, mp, of naphthalene

(i) Put a very small amount of naphthalene in a capillary tube sealed at one end. You
can pull out the capillary tube from heated glass tubing. Use a rubber band to attach
the capillary tube, sealed end down, to a thermometer. Heat a thermometer and
capillary tube in a beaker of water on a tripod. Use the thermometer to stir the water
but do not let water enter the capillary tube. Slowly raise the temperature of the
water. Note the temperature of the naphthalene when it melts. Let it cool and note
the temperature when the naphthalene solidifies Calculate the average of these two
values.
(ii) Use a clean test-tube and thermometer to repeat the experiment using stearic
acid, mp 69o, or use any other substance, mp < 100oC.

3. Impurities affect the melting point of a substance

Mix stearic acid with the naphthalene, thus making the naphthalene impure. Look for
changes in the melting point. Impurities lower the melting point.

4. Boiling point of water

We can identify a pure substance from its melting point or boiling point. Put water in
a test-tube and hold a thermometer with the bulb just under the water. Add boiling
chips to prevent bumping. Bring the water to the boil with a very small flame and
read the thermometer. Note any change in the reading if the thermometer touches
the bottom of the test-tube.

5. Boiling point of inflammable liquids

(i) Use a different method of heating inflammable liquids, e.g. ethanol, bp 78.4 oC and
acetone, bp 56oC. Put 2 cm of the inflammable liquid in a test-tube. Put the test-tube
in an empty beaker. Put a thermometer into the test-tube with the bulb in the liquid.
Boil water in an electric jug or on an electrical hot plate. Pour the hot water into the
beaker so that the level is higher than the inflammable liquid in the test-tube. Stir the
inflammable liquid gently with the thermometer and read the thermometer when the
inflammable liquid boils.
(ii) Use a very small test-tube or seal one end of a piece of glass tubing, 8 cm length
and 3 cm external diameter. Put the inflammable liquid into this tube. Put a capillary
tube, sealed at one end, into the inflammable liquid with the sealed end up and the
open end down in the inflammable liquid. Use a rubber band to attach the tube
containing inflammable and capillary tube to the bulb of a thermometer. Hold the
apparatus in a beaker of water and heat gently with a Bunsen burner flame. When
the temperature rises, bubbles slowly come out of the capillary tube. At the boiling
point the bubbles suddenly come out as a steady stream. Read the temperature. Let
the water cool and read the temperature again when the steady stream of bubbles
ceases. Calculate the boiling point as the average of the two readings.

6. Pressure affects the boiling point

Put water in a sidearm test-tube or in a round-bottom flask with a 2-hole stopper.
Insert a thermometer through a hole in the stopper so that the bulb of the
thermometer reaches, but does not touch, the bottom of the test-tube or flask. Add
boiling chips to prevent bumping. Boil the water and read the temperature on the
thermometer. Stop heating. Connect a water pump to the sidearm or to the second
hole of the 2-hole stopper. When the water stops boiling, turn on the water pump to
reduce the pressure. Read the temperature, heat to boiling and read the temperature
again.

7(a). Solubility in water

Test different salts taken to show that each has a different solubility in water. Take 5
g samples and try to dissolve each in 15 mL of water in a test-tube. Attach the
stopper then shake each test-tube vigorously for the same time to show that
solubility is a characteristic of a particular substance, e.g. sugar, common salt,
potassium nitrate, calcium sulphate. The solubility of a salt is usually expressed as
the number of grams able to dissolve in 100 g water at 20oC, e.g. ammonium chloride
37.2 g, barium chloride 35.7 g, calcium chloride 42.7 g, copper sulphate 20.7 g, lead
nitrate 54.4 g, magnesium sulphate 25.2 g, potassium chloride 34.0 g, potassium
iodide 144.0 g, sodium bicarbonate 9.6 g, sodium chloride 36.0 g, sodium hydroxide
109.0 g, sodium nitrate 87.5 g.

(b) Solubility of a substance in water at a given temperature

Put about 50 cm3 of water in a beaker and add baking powder, sodium bicarbonate,
gradually while stirring. Potassium sulphate is an alternative substance. Make a
saturated solution by stirring until no more solute will dissolve. Read the temperature
of the saturated solution. Weigh a clean evaporating dish, w1. Add some clear
saturated solution and weigh again, w2. Carefully evaporate the solution in the
evaporating dish to dryness and weigh again, w3. The mass of the sodium
bicarbonate dissolved = w3 - w1. The mass of water = w2 - w1 - w3. Calculate the
solubility of the sodium bicarbonate as g per 100 g water at room temperature.

Temperature/OC 0 10 20 30 40 50 60
Solubility(g/ 6.9 8.2 9.6 11.1 12.7 14.5 16.4
100g of water)

8(a) Solubility and particle size

To show that small particles dissolve faster than the large particles, add 4 g of coarse
able salt to one test-tube half filled with water, and 4 g of fine table salt to a second
test-tube containing the same amount of water or use whole and crushed copper
sulphate crystals. Stir or shake both tubes equally and simultaneously. Pause after
every few seconds to observe the amount of undissolved salt left in each tube.

(b) Solubility and solvents

(i) Fill two test-tubes one third full with (a) water and (b) methylated spirits. To each
test-tube add 1 g sodium chloride, attach a stopper and shake. Sodium chloride
dissolves readily in water but not so readily in methylated spirits.
(ii) Fill two test-tubes one third full with (a) 88g water and (b) a solution of 1 g
potassium iodide in 5 mL water. To each test-tube add iodine crystals, attach a
stopper and shake. Sodium chloride dissolves readily in water but not so readily in
alcohol

DETERMINATION OF DENSITY
9(a) Density of a solid
The density of a solid is the ratio of mass to volume. We can find the density of a
regular solid with a balance and ruler. We can find the volume of an insoluble
irregular solid with a measuring cylinder. Half fill a graduated cylinder with water.
Read the volume, immerse the solid in the water and read the volume again. The
difference in the two readings is the volume of the solid.

(b) Density of a liquid

Weigh a small container, fill with liquid and weigh again. Transfer the liquid to a
measuring cylinder. Find the density by dividing the mass of the liquid by the volume.

Heat of fusion and vaporization

10(a) Separate by sublimation

Separate iodine from a mixture of crystals of iodine and sodium chloride. Heat the
mixture in an evaporating dish with a funnel placed over it. The iodine sublimes on to
the cool sides of the funnel.

SEPARATION OF MIXTURES

(b) Separate by distillation

Put 10 mL ink in a flat bottom conical flask. Add boiling chips to prevent bumping. Fit
a stopper with a delivery tube reaching half way down a collecting test-tube or an U-
tube, in a beaker of water. Heat the ink with a Bunsen burner flame. Drops of a
colourless liquid appear in the collecting tube. Identify the liquid as water by its
action of turning white anhydrous copper sulphate to blue hydrated copper sulphate.
Do not allow ink to froth up or splash into the delivery tube.

(c) Separate salt and sand

Prepare a mixture of salt and sand. Put about 2 mL of the mixture in a test-tube. Add
5 mL water and shake until all the salt has dissolved. Pour the contents of the tube
into a filter paper in a funnel over an evaporating basin. Wash the test-tube with
water and add this to the filter paper. The sand will remain on the filter paper and
may be dried and collected. The salt can be recovered from the filtrate by warming
the evaporation basin to drive off the water.

(d) Solvent extraction of oil from nuts

Put groundnuts (peanuts) or pieces of chopped coconut into a mortar. Add 20 mL of
acetone or methylated spirits. Grind the nuts in the solvent as finely as possible. Pour
off the liquid into a test-tube and filter into an evaporating basin. Warm the
evaporating basin for 10 minutes. The solvent evaporates leaving the oil extracted
from the nuts.

(e) Separate two immiscible liquids of different density

Use a separating funnel or make a separating funnel with a piece of wide tubing
fitted with a stopper, tube and rubber tube with a clip. Shake the mixture thoroughly
in a closed container then run it into the separating funnel. Wait until a clear
boundary appears between the two liquids and then run off the denser layer into a
beaker below.

11(b). HEATING AND BURNING DIFFERENT SUBSTANCES

Substances that gain mass when heated.

Clean 25 cm of magnesium ribbon and cut into 1 cm pieces. Weigh a crucible plus lid,
put the pieces of magnesium ribbon in the crucible and weigh again. Put the crucible
on a pipe clay triangle supported on a tripod. Heat very gently then strongly. Hold
the crucible lid in a pair of tongs close to the crucible. The magnesium ribbon darkens
just before it begins to melt. At the first sign of burning, place the lid on the crucible
and remove the Bunsen burner. Every 4 seconds, raise the lid to allow more air to
enter but do not allow any white magnesium oxide smoke to escape. When the
magnesium stops burning on raising the lid, remove the lid. Heat the crucible again
strongly but still hold the crucible lid in a pair of tongs close to the crucible in case
the magnesium starts to burn again. Leave the crucible to cool. When cool, weigh the
crucible plus lid plus contents. Calculate the increase in mass of the magnesium.

(b) Substances that lose mass when heated

(i) Weigh a test-tube containing 1 cm potassium permanganate crystals and a 1 cm
plug of cotton wool at the mouth to prevent loss of any solid during heating. Heat the
test-tube and cotton wool and weigh it again. Note any change in the potassium
permanganate crystals. Note any loss in mass due to the loss of water of
crystallization.
(ii) Weigh a test-tube containing 1 cm copper carbonate and a 1 cm plug of cotton
wool at the mouth to prevent loss of any solid during heating. Heat the test-tube and
cotton wool and weigh it again. Note any change in the copper carbonate. Note any
loss in mass.

(b) Substances that neither gain nor lose mass when heated
Weigh a test-tube containing 1 cm dry zinc oxide and a 1 cm plug of cotton wool at
the mouth to prevent loss of any solid during heating. Heat the test-tube and cotton
wool and weigh it again. Note any change in the zinc oxide. Note any loss in mass.

(c) Effect of heat on copper sulphate crystals

Crush blue copper sulphate crystals and put them into a dry test-tube to a depth of 4
cm. Heat the tube gently. Note whether vapour collects on the cooler parts, change
of colour from blue to white, and any liquid collecting in the receiving tube. Identity
of the liquid by measuring the boiling point. When all the copper sulphate crystals
have changed to white and the tube has cooled, hold the tube in your hand and pour
the liquid back on to the white crystals. Note whether the blue colour restored and if
any heat is given back.

Blue copper sulphate crystals + heat -> white, anhydrous copper sulphate + water.
This is a reversible change.

12.PREPARING, COLLECTING AND TESTING GASES

(b) Hydrogen
Be careful! A dangerous explosion may occur if you use any vessel bigger than a
small test-tube when igniting the gas, particularly if it is mixed with air.
Never dry hydrogen gas with concentrated sulphuric acid!
(i) Place a few pieces of granulated zinc or zinc foil from the casing of an old dry cell
in a boiling tube; add 2 drops of copper sulphate solution. An alternative to the thistle
funnel at A is a syringe as shown at B. Pour enough 1 M sulphuric acid down the
thistle funnel on to the zinc to cover the bottom of the funnel tube. Discard the first
two or three test tubes of hydrogen, as they will contain displaced air. Collect test
tubes of the gas and stopper them. Test the third test-tube of gas by holding a
lighted taper or splint over the mouth as soon as you take out the stopper. Pure
hydrogen burns with a quiet "pop" sound.
(ii) Alternatively, add sulphuric acid from a syringe. Gas cannot escape through the
syringe so you do not need to cover the tube of the syringe with acid.
(iii) Hydrogen burns in air to form water vapour. When hydrogen ignites in a dry test-
tube, note any vapour or mist on the sides of the test-tube.
(iv) Investigate whether hydrogen is lighter than air by "pouring" the gas into a test-
tube held either above the first tube or below it. Use a lighted taper to investigate
where the hydrogen has gone.
(v) Blow soap bubbles by holding the delivery tube of the apparatus in detergent or
soap solution. The hydrogen bubbles will rise into the air, showing the low density of
hydrogen gas.

(b) Oxygen
(i) Prepare oxygen safely by decomposition of hydrogen peroxide solution. Put 20 mL
hydrogen peroxide into a 100 mL bottle. Fix a delivery tube to the bottle. Add two
spatulas of manganese dioxide and oxygen bubbles off for collection.
(ii) Oxygen is colourless and has no smell. To test whether the test-tube contains
oxygen, light a splint of dry wood, blow out the flame leaving a glowing splint then
put the glowing splint in a test-tube of oxygen. The glowing splint bursts into flame.
This experiment is called the glowing splint test.
(iii) Use an L-shape piece of nichrome wire with a shield to fit on the top to protect
your hand. Fix steel wool into a loop in the lower end of the Nichrome wire. Heat the
steel wool to red hot in a Bunsen burner flame then inserts it quickly into a test-tube
of oxygen.
(iv) Fix a small piece of charcoal into the loop in the lower end of the Nichrome wire.
Ignite the charcoal in the Bunsen burner flame and then insert it quickly into another
test-tube of oxygen.
(v) Dip the loop in the lower end of the Nichrome wire into sulphur powder. Ignite the
sulphur powder in a Bunsen burner flame and then insert it quickly into another test-
tube of oxygen.

(c) Hydrogen chloride

Put rock salt, sodium chloride, into a 100 mL filtering flask. Coarse rock salt causes
less frothing than the fine salt. Carefully add concentrated sulphuric acid down the
thistle funnel. You can collect hydrogen chloride gas by upward displacement of air,
as in the diagram.
(i) Collect four test tubes of the gas and cork them. Remove the cork from one of
these test tubes under water. Note the solubility of hydrogen chloride.
(ii) Hold a piece of cotton wool soaked in ammonium hydroxide at the mouth of a
test-tube of hydrogen chloride.
(iii) Shake a test-tube of the gas with water to obtain a solution of hydrogen chloride.
Test the solution with an acid/base indicator. Put a piece of magnesium ribbon in the
solution. Collect any gas formed and test for hydrogen with the glowing splint test.

(d) Ammonia
(i) Put a mixture of calcium hydroxide and ammonium chloride into a test-tube to a
depth of 4 cm. Fill a U-tube with lumps of calcium oxide mixed with cotton wool. The
cotton wool is to prevent blocking of the tube. Gently heat the test-tube. The calcium
oxide dries the ammonia gas. Test whether the receiver test-tube is full by holding a
piece of red litmus paper at the opening. Collect test tubes of ammonia and cork
them. The method of collection illustrates that ammonia gas is lighter than air.
(ii) Fill a flask with ammonia. Fit a cork and tube into the flask as shown. The tube
should have been drawn out into a jet. Warm the flask gently to expand the gas and
then hold the flask upside down with the tube in the water. Water will spray into the
flask from the jet.

(e) Carbon dioxide

Many reactions can be used to produce carbon dioxide gas. Marble chips or other
carbonate rock treated with dilute acid provides a good source. The gas is not too
soluble to be collected by water displacement, as shown above for the preparation of
hydrogen. Alternatively, carbon dioxide can be collected by displacing air from dry
bottles. To test if the bottle is full, lower a lighted splint or taper into the top of the
jar. If the flame is extinguished at the entrance as at (ii), then the jar is full. Put a
cardboard cover over the top to prevent diffusion of the gas. Check the density of the
carbon dioxide by pouring" the gas into another bottle either above or below the first
bottle. Find where the gas is by testing with a lighted splint. Note: The presence of
carbon dioxide can be confirmed by the fact that limewater becomes "milky" when
the gas is Passed through it.

(f) Cooking and carbon dioxide

The purpose of baking powder or soda in cooking is to produce tiny bubbles of carbon
dioxide. This expands the pastry, cake or dough, making it light and pleasant to eat.
Yeast cells do the same thing in bread making, though this takes longer. Baking
powder, or sodium bicarbonate, NHCO3, reacts with an acid such as lactic acid from
sour milk to produce carbon dioxide. Commercial "baking powders" often contain a
solid acid, which only reacts with the sodium bicarbonate when moist.
(i) Put baking powder into water. Note whether carbon dioxide gas forms. Note
whether carbon dioxide forms when you put sodium bicarbonate into water. Add
baking powder in a test-tube with vinegar or lemon juice (acetic acid). Note whether
carbon dioxide forms.
(ii) Make a sugar solution and half fill a jar with this solution. Add a spoonful of yeast
and leave to stand for 2 days. Construct a bubbler to fit on the top of the jar. Note
whether the yeast forms a gas. Note whether carbon dioxide gas collects in the upper
part of the jar.

12(a) RUSTING
Take 7 test tubes and 11 clean nails. Prepare the tubes as shown below:
Tube 1: Put 2 clean nails in the test-tube and half cover them with distilled water.
These nails are in contact with air and water and form the control experiment.
Tube 2: Put a few pieces of anhydrous calcium chloride or silica gel in the bottom of a
dry test-tube, and also two nails. Put a plug of cotton wool in the top of the tube.
These nails are in contact with air, but not moisture.
Tube 3: Boil water for several minutes to expel dissolved air and pour into the test-
tube whilst hot. Put 2 nails in the water. Put a little Vaseline or a few drops of olive oil
on the surface of the hot water. The Vaseline will melt and form an airtight layer,
solidifying as the water-cools. These nails are in contact with water but not air.
Tube 4: Half cover 2 nails with water containing a little common salt dissolved in it.
These nails are in contact with air, water and salt.
Tube 5: Wrap a piece of zinc foil round part of a nail. Put the nail in the test-tube and
almost cover with tap water.
Tube 6: Wrap a piece of tin foil round part of the nail. Put the nail in the test-tube and
add tap water as you did for tube 5.
Tube 7: Wrap a piece of copper wire round a nail and put it in the test-tube exactly
like tubes 5 and 6. Stand these 7 test tubes in a rack and leave for several days. Note
the conditions for rusting and which metal, (zinc, copper or tin), is best at preventing
rusting.

(b) INCREASE IN MASS OF IRON DURING RUSTING

Counterbalance a piece of iron on a knife-edge, using a brass weight or stone. Leave
in moist air or on a window ledge for a few days and note the effect of the rust on the
longer arm of the lever. During rusting, metallic ion changes to Fe (OH) 3.xH2O.

(c) WHAT COMBINES WITH IRON DURING RUSTING

Moisten the inside of a test-tube with water, sprinkle into it a spatula measure of iron
filings and rotate it horizontally so that the filings spread and adhere to the walls.
Alternatively, push a small plug of moistened iron wool to the bottom of the tube.
Invert the test-tube in a beaker about one third full of water. Use the beaker lip to
support the tube. The water levels inside and outside the tube should be the same
and the level should be marked on the tube. Leave the tube in this position for a few
days. The iron will rust and the water level will rise up inside the tube, finally
becoming steady. Again add water to the beaker until the levels inside and outside
the tube are the same and mark the new level. It will be seen that one fifth of the air
volume has been used up, suggesting that oxygen has been used up in the rusting of
iron. The residual gas does not support combustion of a lighted splint.

13 COLOURED EXTRACTS FROM FLOWERS AS INDICATORS OF ACIDS AND

BASES
(a) Extract coloured substances from plants
Select brightly coloured flowers, such as the purple and red bougainvillaea, or
coloured leaves. Squeeze or grind one of the coloured flowers or leaves in a mortar
with a mixture made of 2 mL acetone and 2 mL ethanol. By this means the colouring
matter will be extracted into the solvent. Filter and collect the filtrate. Repeat this
experiment with one or two other flower colours. Keep these coloured solutions for
use as "indicators" in the next experiment.

(b) Plant extracts to indicate whether a substance is acidic or basic

(i) Put a spot of the coloured flower extract on to a filter paper and leave to dry. Put
one drop of lemon juice on to the spot then note any change of colour. Repeat the
experiment with other fruit juices and vinegar. They are acidic substances. Note any
colour change with dilute hydrochloric acid. Different colours suggest that some
substances are more acidic than others.
(ii) Put some of the original filtrate on to another piece of filter paper. When dry, note
the colours given by sodium bicarbonate solution, washing soda, limewater and a
dilute solution of sodium hydroxide. These are alkaline, or basic, substances. Note
whether they all give the same colour: Plant extracts can act as indicators to test
whether a substance is acidic or basic.
(iii) Add a few drops of sodium bicarbonate solution to 1 mL of flower extract
indicator in a test-tube. Then add lemon juice and note any colour change.
(iv) Repeat the experiment with limewater and indicator followed by dilute
hydrochloric acid. Note any colour change. Note whether you can get back the
original colour by adding more limewater. Note how many times you can change the
indicator colour before the test-tube is full.
(v) Litmus, an extract of lichens, is another plant indicator. An acidic solution turns
blue litmus red. An alkaline solution turns red litmus blue.
(v) Universal Indicator can be in the form of a solution or dried on filter paper.
Universal indicator not only indicates whether a substance is acidic or basic but also
how acidic it is. Investigate the effect of Universal Indicator on the solutions above.
To avoid using the name of a colour to indicate acidity, we use a scale of numbers
from 0 to 14 called the pH scale. We can use the pH scale to express the degree of
acidity. Acid solutions have a pH value less than 7. Alkaline or basic solutions have a
pH value greater than 7. Solutions with a pH value of 7 are neither acidic nor basic,
they are neutral.
On the bottle or packet of Universal indicator, a colour chart shows the colour and the
pH value associated with this colour as follows:
(a) Colour (b) pH (c) Acid/Base
(a) Red (b) 1-3 (c) very acidic
(a) Orange (b) 4-5 (c) weak acid
(a) Yellow (b) 6 (c) very weak acid
(a) Green (b) 7 (c) neutral
(a) Blue (b) 8 (c) very weak base
(a) Indigo (b) 9-10 (c) weak base
(a) Violet (b) 11- 14 (c) very basic
Use 2 drops of Universal Indicator to 10 mL of solution to be tested. Test the pH value
of lemon juice, vinegar, sodium bicarbonate solution, washing soda, lime water,
sodium hydroxide solution, tap water, distilled water.

14. CRYSTALS
(a) Crystal growth
Sodium thiosulphate crystals grow rapidly from a super-saturated aqueous solution.
The formula for the crystals is Na2S2O3.10H2O. On heating, these crystals dissolve in
some of their water of crystallization. Put 3 cm of sodium thiosulphate crystals in a
test-tube. Add 2 drops of water. Heat gently until all the crystals have dissolved. They
appear to "melt". Leave to cool. Crystals may not form unless you drop a tiny seed
crystal of sodium thiosulphate into the solution. Then crystal growth commences and
spreads rapidly through the whole solution. Watch the growth from one centre. Hold
the tube in the hand while crystallization occurs.

(b) Crystals of naphthalene grow from the melt

Put a little naphthalene on a glass slide. Hold over a flame until the crystals melt. Put
a cover slip over the liquid and allow to cool. Watch the crystals grow using a hand
lens. Sometimes crystals will grow from several points simultaneously to make
boundaries where they meet. Draw the shape of the boundary between the forming
crystals and the melt. View the crystals through Polaroid filters.

(c) Grow large crystals

(i) Use a 0.5 - 0.8 cm long seed crystal to start growing large crystals. Make seed
crystals by slow evaporation of 30 mL of saturated solution in a glass dish. Dry a
selected seed crystal. Tie a piece of clean cotton around it without touching the seed
crystal with your hands because impurities easily affect the size and shape of the
crystal. Hang the seed crystal 5 cm from the base of the container with a bent wire.
Fill a jar (with a screw-on lid) with a solution of the salt less than saturation strength
before you put the seed crystal in position. If little crystals grow on the surface of the
seed crystal, then screw on the lid of the jar to make the little crystals dissolve.
Prevent crystals growing on the sides of a crystallizing dish by rubbing Vaseline
round the upper inside rim. Evaporation may be increased by sitting the crystal
growing jar on a tin with a 5 watt bulb mounted inside it. An air flow over the solution
surface given by a fan will also hasten crystal growth. You can preserve large crystals
by painting with a clear varnish.
(ii) You can also support the seed crystal at the end of a glass tube. Heat a 3 mm
bore piece of glass tubing in a flame until the end softens sufficiently to squeeze with
pliers to make a smaller hole. When the glass tubing cools, drop seed crystals on its
end until one catches in the smaller hole. Keep this crystal in place by dropping other
crystals on it. Support the glass tubing vertically so that the seed crystal at the end is
immersed in the solution of the salt. The seed crystal should then grow. Turn the
crystal regularly so that growth on all faces is equal.

15. DIFFUSION
(a) Diffusion of heavy carbon dioxide gas upwards
(i) Fill a jar with carbon dioxide and invert it over a similar jar full of air. After a few
moments separate the jars, pour a little lime water in the lower one and shake it. The
lime water will turn milky indicating that the carbon dioxide has fallen into the lower
jar because it is the heavier gas.
(ii) Repeat the experiment with the carbon dioxide in the lower jar and invert a jar of
air on top of it. If the jars are left for about 5 minutes carbon dioxide will be carried
into the upper jar by diffusion; in the same way air will be carried into the lower jar.
The lime water test will show the presence of carbon dioxide in the upper jar.

(b) Diffusion rates of ammonia and hydrogen chloride gases

The long glass tube should be horizontal. Corks should fit at both ends. Using a pair
of tongs or tweezers, dip a piece of cotton wool into concentrated hydrochloric acid
and another piece into concentrated ammonium hydroxide. Drain off excess liquid.
As nearly as possible at the same time, put the ammonia cotton wool at one end of
the tube and the acid cotton wool at the other. Close the ends of the tube with corks.
After a while, look carefully for a white ring which will form where the ammonia gas
and the hydrogen chloride gas meet after diffusing through the air towards each
other. Ammonia is the less dense gas and the white ring of ammonium chloride
should form nearer to the hydrogen chloride end than from the ammonia end of the
tube.

(c) Diffusion of liquids

(i) Place a crystal of potassium dichromate, potassium dichromate (VI), or ammonium
dichromate at the bottom of a beaker of water. To do this, put a glass tube into the
beaker of water so that it touches the bottom, then to drop the crystal down the
tube. Close the top of the tube with your finger and remove the tube gently, leaving
the crystal in the beaker. The colour of the dissolving crystal will spread throughout
the water in quite a short time.
(ii) Fill a very small open bottle with a strong solution of potassium permanganate,
potassium manganate (VII). Place this in a larger jar. Fill the larger jar very carefully
by pouring water down the side until the water level is above the top of the small
bottle. Leave this for a few days. The potassium permanganate solution diffuses
evenly through the water.

(d) Size of a molecule

We select an oil molecule because it has a density less than the density of water. Oil
floats on the surface and does not dissolve in the water. If the water has a large
enough surface area, we assumed that thin oil will spread out in a layer one molecule
thick called a monomolecular layer and not form little "hills" of molecules. If we know
the original volume of oil and the surface area that it forms, then we can calculate
the thickness of a monomolecular layer dividing the volume by the area. Use a tray
with area > 30 cm2 so as not to restrict the oil film. Sprinkle the surface of the water
with a very fine light powder, e.g. talc powder. When you put oil on the water, it
pushes the powder aside so you can easily see the area covered by the oil. Pour thin
petroleum distillate oil into a burette. Find the volume of fifty drops by running oil
from the burette drop by drop and counting the drops. Allow one more drop to fall on
a piece of plastic. Touch the oil drop with the point of a glass rod and then touch the
prepared water surface. The oil spreads out. Measure the approximate area over
which it spreads. Estimate what fraction of oil was removed by the glass point by
using the glass point to remove successive fractions from the drop until it has been
used up. The volume of oil put on the water can be calculated and an estimate made
of the thickness of the oil layer, about 10-6 mm. This is an approximate dimension of a
single molecule of the oil.

16. ELECTRICITY
(a) Solids that conduct electricity
The source of the DC supply can be dry cells in series giving 6 volts. The bulb, which
should be low power, indicates when the current is flowing. The electrodes may be
carbon or steel, perhaps mounted in a wooden support, cork or rubber stopper so as
to keep the electrodes a constant distance apart.

(i) Test the conductivity of solids by making a good contact between the surface of
the solid and the two electrodes. The surface of the solid must first be cleaned. All
metals conduct electricity. Carbon conducts electricity. Note whether non-metallic
solids, e.g. plastics, naphthalene, wax, sugar, sodium chloride and sulphur, conduct
electricity.
(ii) Glass can be a conductor. Heat a glass rod until it becomes very hot and begins to
soften. Test the hot, soft part with the conductivity apparatus. When molten, glass is
a good conductor of electricity.

(b) LIQUIDS THAT CONDUCT ELECTRICITY

(i) First test liquids obtained by melting substances. Melt the following substances,
but heat very gently and cautiously because otherwise they may ignite and burn:
sulphur, wax, naphthalene, polyethylene material, tin, lead and, if available, a low
melting point salt such as lead bromide, m.p. 488oC, or potassium iodide, m.p.
682oC . Test the conductivity of the melt by dipping in the electrodes and waiting a
few moments for the electrodes to reach the same temperature. This ensures that
the electrodes are in contact with the liquid and not the solidified melt. Scrape and
clean the electrodes between each test.
(ii) Test ethanol, or methylated spirits, acetone, carbon (IV) chloride, vinegar, sugar
solution, copper (II) sulphate solution, sodium chloride solution, and other substances
dissolved in water. Clean and dry the electrodes between each test.
(iii) Test pure distilled water for conductivity. Put the electrodes into a beaker of
distilled water. The bulb does not light up so pure water does not conduct electricity.
Very gradually stir small crystals of common salt into the water. Note any changes to
the bulb as the salt dissolves. Classify substances into the following groups: (a) those
which conduct electricity in the solid state and those which do not; (b) those which
conduct in the liquid state and those which do not; (c) those which conduct when
dissolved in water and those which do not

(c) ELECTROLYSIS OF LEAD BROMIDE

There are very few suitable low melting point salts. Lead bromide has a low melting
point and makes an interesting electrolysis experiment. Potassium bromide may
have too high a melting point, 682oC, to melt easily. The lead bromide is melted in a
100 mL hard glass beaker, or in a crucible. The carbon electrodes are supported by a
strip of wood with two holes bored 2 cm apart for the electrodes. Connect crocodile
clips to the rods and complete the circuit with a torch bulb, to indicate when a
current is flowing, and a 12-volt torch battery or cells wired in series. The electrodes
can be labelled positive and negative. The only ions present in this melt are the
bromide and lead ions. Bromine is readily seen coming off at the positive electrode,
which is the anode. The fact that bromine appears only at the positive electrode
helps in the understanding of the existence of a negative bromide ion. Lead has both
a lower melting point and a greater density than lead bromide and therefore appears
as a melt at the bottom of the beaker. The small globule of lead, which accumulates
at the negative electrode, the cathode, can be seen after about 10 minutes of
electrolysis. Decant off the molten lead bromide carefully into another crucible. The
electric current has split up crystalline lead bromide into bromine gas and lead metal.

(d) ELECTROLYSIS
In aqueous solutions there are usually four ions present, two from the water and two
from the dissolved salt. The products will be gaseous, or metals which are deposited
on the negative electrode. It is composed of an open cylinder of glass approximately
8 cm high and 2.5 cm in diameter. A small bottle of similar size with the bottom cut
off would do just as well. The cylinder has a 2-hole rubber stopper carrying two
carbon electrodes with connecting leads to a battery, or DC supply of 4 to 6 volts. If
cork is used, this must be made leak proof by covering the whole of the bottom
surface round the electrodes and the glass edge with Faraday's wax or a similar soft
wax. The electrodes may be carbon rods from a dry cell or pencil leads. The alloy
supports for the coiled filament in electric light bulbs have also been found suitable
for electrodes. The electrodes should project about 2 cm into the cylinder and also 2
cm below for attaching the leads to the battery. Pencil leads are brittle, and if they
are used it is better to fix the electrodes in the following way. Solder a piece of stout
copper wire to a 4 cm length of braided copper screening wire. Drill two holes in the
rubber stopper with a 1 mm drill. Insert the copper wire into the hole from above and
pull it right through the stopper until the screening wire is also pulled a little way into
the hole. Into the core of this screening wire insert the pencil lead securely. Then pull
the screening wire with the lead further into the stopper so that the lead electrode is
firmly held in the stopper. The excess copper wire is cut off. This procedure is
repeated with the other electrode. The solution is placed in the glass cylinder. The
two small tubes are then filled with the solution, and carefully inverted over the
electrodes. The electrodes are connected to a safe DC supply with a small bulb in
series. Increase the voltage until the bulb lights, showing that a current is flowing.
When this happens, cut out the bulb from the circuit by closing the switch, as shown.
This will allow a larger current to flow. The tubes collect any gas given off and the
properties of the gas should be tested. Using carbon electrodes, the following results
will be found.

(d) ELECTROLYSIS OF WATER

Pure water does not conduct electricity. For this reason 2 or 3 mL of dilute sulphuric
acid or dilute sodium sulphate solution is added to the water in the electrolysis cell.
Connect the cell to the DC supply and watch for bubbles of gas at both electrodes. If
none appear, add a little more acid or sodium sulphate solution. After 5 to 10 minutes
there should be enough hydrogen and oxygen gas for testing. Predict at which
electrode each gas will appear.

(e) Electrolysis of solutions of ionic salts

Most ionic salts can be used satisfactorily in electrolysis. Concentrations of 1M or less
are suitable. Potassium iodide gives iodine at the anode and hydrogen gas at the
cathode. Zinc sulphate gives a spongy mass of zinc at the cathode, oxygen gas at the
anode. Lead acetate deposits lead on the cathode and oxygen gas is produced at the
anode. If the lead acetate solution is cloudy, add a few drops of acetic acid. Sodium
chloride gives hydrogen gas at the cathode and chlorine gas at the anode. Copper
sulphate deposits copper at the cathode and oxygen gas is produced at the anode.

17. COMMON REACTIONS

(a) DISPLACEMENT OF COPPER FROM AQUEOUS SOLUTION OF COPPER IONS
(i) A metal higher in the activity order can displace copper metal from a solution of
copper ions. Put 10 mL of molar copper sulphate solution in a small beaker. Clean
magnesium ribbon and cut into 0.5 cm pieces. Add these pieces to the copper
sulphate solution one at a time. The reaction can be vigorous! Copper metal deposits
and the blue colour gradually disappear as the magnesium displaces the copper ion.
Note any heat given out by the reaction. When the solution is colourless, decant the
solution from the red copper powder at the bottom of the beaker. Collect the copper
and dry it.
Mg(s) + Cu2+(aq) -> Mg2+(aq) + Cu(s)
(ii) Repeat the experiment by attempting to displace copper metal using powdered
zinc and iron metal. Note the comparative activity of the metals.

(b) REACTION OF SODIUM WITH WATER

(i) A very safe way of demonstrating the reaction of sodium and water is to drop a
very small piece of sodium into a swimming pool.
(ii) Pour a 2 cm layer of kerosene on to the surface of water in a test-tube. Drop a 3
mm diameter piece of sodium into the kerosene. Be careful! Sodium sinks in the
kerosene and float in the water. Adjust the layer of kerosene to be shallow enough to
allow the top of the sodium to protrude above the surface. This reaction between
sodium and the water is much slower than if the sodium had been dropped directly
on to the water. You can watch the reaction through a hand lens held at the side, but
never at the top. Sodium metal is lighter than water but heavier than kerosene. A
small area of the sodium suddenly reacts causing a stream of bubbles to appear. The
stream of bubbles at one side causes movement. The irregular shape of the sodium
changes to a sphere. The sodium melts because the reaction gives off heat. Note any
variations in light refraction and reflection below the sodium that indicates something
dissolving in the water. Slight smoke where the hot sodium is above the kerosene
level suggests a slight reaction with air. Test the gas bubbles for oxygen or hydrogen.

(c) DISPLACEMENT OF HYDROGEN FROM ACIDS BY METALS

(i) Pour 5 cm of the acids in the table below into test-tubes. Place a piece of metal foil
in each test-tube. Note the formation of hydrogen and compare the different rates at
which the bubbles are formed.
Rate of formation of hydrogen gas - very rapid, rapid, slight, very slight, none
Metal (b) 3M hydrochloric acid (c) 3M sulphuric acid
Magnesium (b) Very rapid (c) Rapid
Aluminium (b) Slight (c) None
Zinc (b) Moderate (c) Slight
Iron (b) Very slight (c) Very slight
Tin (b) None (c) None
Lead (b) None (c) None
Copper (b) None (c) None
(ii) Recover the zinc after the reaction has ceased. Evaporate the solution to leave
zinc sulphate crystals. Dissolve the colourless zinc sulphate crystals in water and put
two carbon electrodes (central poles of dry cell batteries) in the solution. Connect the
electrodes to a 6-volt or 12 volt DC supply. Zinc forms rapidly on the cathode.

(d) PREPARE SULPHUR DIOXIDE

Do the following preparations in a fume cupboard.
(i) Prepare sulphur dioxide by burning sulphur in air. Put powdered sulphur in a
porcelain jar; ignite it and collecting the gas formed in a funnel. Aspirate the gas into
a bottle containing water.
(ii) Prepare sulphur dioxide in a generator which allows dilute sulphuric or
hydrochloric acid to drip slowly on to sodium sulphate. The acid is contained in a
thistle funnel and a tap controls the flow on to sodium sulphite in a suitable flask. The
sulphur dioxide produced can be collected in gas jars covered with cardboard discs,
which have central holes for the delivery tube.

(e) REDUCTION OF POTASSIUM PERMANGANATE WITH SULFUR DIOXIDE

(i) Add 10 mL of 0.1M solution of potassium permanganate and 10 mL 3M solution of
dilute sulphuric acid to 200 mL of water containing sulphur dioxide. The solution will
gradually become colourless as the sulphur dioxide reacts with the permanganate.
The experiment can be continued further by stirring in a 0.25M solution of barium
chloride when the solution will become "milky" due to the formation of barium
sulphate.
(ii) The generator used in experiment 2.75B is a convenient piece of apparatus for
giving a continuous supply of sulphur dioxide for bleaching Bowers and other plants.
The gas from the generator is passed through a jar containing the plant, and excess
gas is absorbed in water. The colour of the bleached plant can easily be regenerated
by placing the plant in a solution of hydrogen peroxide. This experiment could be
used as an introduction to the processes of reduction and oxidation.
(f) REACTION OF MAGNESIUM WITH CARBON DIOXIDE
Fill a gas jar with carbon dioxide as described in experiment 2.38. Hold a piece of
clean magnesium ribbon in a pair of tongs; ignite the magnesium with a Bunsen
burner flame and plunge it into the carbon dioxide gas. The magnesium continues to
burn. If the magnesium is taking oxygen from the carbon dioxide for burning then
you would find carbon in the gas jar. Look for carbon specks in the gas jar. To make
the carbon more visible, you can add drops of sulphuric acid to remove the
magnesium oxide and any unburnt magnesium.

(g) TITRATION OF ACIDS AND BASES

Measure exactly 20 drops of a dilute acid such as vinegar and put these into a test-
tube. Add one drop of indicator; either methyl orange or phenolphthalein is
satisfactory. To this mixture of acid and indicator, add a dilute base drop by drop,
and count the drops. Within experimental error, it will always take the same number
of drops to neutralize the 20 drops of acid provided that the same dropper is used. A
teat pipette makes a satisfactory dropper. If the concentration of the acid is known,
the concentration of the base can be estimated by comparing the numbers of drops
of acid and drops of base that just react.

(h) MAKE SOAP FROM FATS

Soap can be made from many oils and fats. The reaction is a double displacement
involving a strong base such as sodium hydroxide and fats. (a) Obtain animal fat
from a butcher. Boil this fat in water and the oil will separate on the surface. When
cold, the fat will solidify and it can be separated from the water. Melt the fat again
and strain through several layers of cloth. (b) Weigh this fat and then weigh out
about one third as much sodium hydroxide pellets. Take care not to touch either the
solid sodium hydroxide or the solution, because it is very caustic. Heat the fat in an
iron saucepan or dish and, when it is molten, slowly add the sodium hydroxide
solution with continuous stirring. Heat with a small flame to avoid boiling over. Allow
the fat and the sodium hydroxide to boil for 30 minutes. Stir the mixture frequently.
(c) The next stage is to weigh out common salt, sodium chloride; about twice the
weight of sodium hydroxide used in (b) is needed. After the 30 minutes boiling, stir
this salt well into the mixture. Then allow to cool. The soap separates as a layer at
the top. Separate this soap from the liquid below, melt and pour into matchboxes
where it will solidify again as small bars of soap.

17. ENERGY FROM CHEMICAL REACTIONS

The following group of reactions involve ions in aqueous solution. When the water
containing the reacting ions becomes hotter, then we have gained this heat and we
can make it do work for us. During the reaction the ions have lost this heat, which we
have gained. On the other hand, when the water containing the ions becomes colder,
it is the ions which have gained the energy and the water has lost an equivalent
amount.
(a) REACTIONS THAT GIVE OUT HEAT ENERGY
Be careful! The reaction is vigorous so do not do the experiment in a stoppered
bottle!
(i) Put white anhydrous copper sulphate powder to a depth of about 1 cm in a test-
tube. Hold a thermometer with the bulb in the powder. Add water drop by drop.
Record the changes of the thermometer reading.
(ii) Put about 10 mL of strong aqueous copper sulphate solution into a wide test-tube
or small beaker. Support a thermometer with the bulb in the solution. Add
magnesium powder, or ribbon, a little at a time until the blue colour disappears. Note
any changes in the thermometer reading.
(iii) To a little water in a wide test-tube, add concentrated sulphuric acid, drop by
drop, down the side of the tube. Stir gently with a thermometer after the addition of
each drop. Note any changes in the thermometer reading.

(b) REACTIONS THAT TAKE IN HEAT ENERGY

Put 10 mL of water in a test-tube. Read the temperature of the water. Dissolve about
2 g of potassium nitrate in the water. The temperature should fall through 90 oC. This
means that, in the process of dissolving in the water, the particles have absorbed
energy. This energy has been taken from the surrounding water in the form of heat.
A similar result can be obtained by using potassium chloride instead.

(c) HEAT OF A NEUTRALIZATION REACTION

Dissolve 40 g of sodium hydroxide pellets in water and make up to 500 mL. This is a
2M solution Also prepare 500 mL of a 2M hydrochloric acid solution. Leave the
solutions to cool to room temperature. Note the actual temperature of the solutions
when cool. Then add the acid to the base quite rapidly and stir with a thermometer.
Note the maximum temperature reached. The increase of temperature should be
about 13oC.
(iii) Since the volume of water has been doubled by adding one solution to the other,
the final solution contains 1 mole of OH- (aq) ions which reacted with 1 mole of H+(aq)
ions to form 1 mole of water molecules. We must assume that the specific heat of
this moderately weak solution is the same as that of water.

(d) HEAT OF A COPPER DISPLACEMENT REACTION

(i) Put 25 mL 0.2 M copper sulphate solution in a 100 mL polythene fitted with a 1-
hole stopper and thermometer. Replace the stopper, invert the bottle and shake it
gently. Record the temperature of this solution. Turn the bottle the right way up,
remove the stopper and add 0.5 g of zinc dust. The quantity of zinc powder is in
excess to ensure that all the copper sulphate is used up in the reaction, so some zinc
will remain when the reaction stops. Replace the stopper, invert the bottle, and shake
gently. Record the highest temperature reached. Calculate the rise of temperature.
This rise of temperature in not affected by the volume of 0.2 M copper sulphate used
for the experiment. For a 1 M solution, multiply the rise in temperature by 5 (5 X
0.2M = 1.0 M). The reactants lost energy to the solution. The temperature change is
usually between 9oC and 10oC.
Zn(s) + Cu2+(aq) --> Zn2+(aq) + Cu(s)
(ii) Repeat the experiment with 0.5 g of iron powder or iron filings. This amount is
again an excess so that all the copper sulphate will be used up in the reaction. The
temperature change is usually between 6oC and 7oC.

(e) ELECTRICAL ENERGY FROM CHEMICAL REACTIONS - ELECTROCHEMICAL

CELLS
In the preceding experiment zinc metal became zinc ions and copper ions became
copper metal due to transfer of electrons from zinc metal to the copper ion. To
get electrical energy these electrons must flow in an external conductor from the zinc
to copper. The potential or voltage will reflect the greater activity of zinc over copper.
The current flowing will depend on the extent and rate of the reaction.
2.84 Electrical energy from the displacement of copper by zinc
Put concentrated copper sulphate solution in a beaker. Connect copper foil to the
positive terminal of a 5 V voltmeter. Connect zinc foil to the negative terminal. Dip
the two metals briefly into the copper sulphate solution. Note any changes in the
voltmeter reading. Note the maximum reading. Note any changes at the copper foil
and the zinc foil. The voltage falls to zero after a short time because copper
deposited on the zinc and caused the reaction to stop.
18. RATE OF REACTION
(a) SIZE OF PARTICLES AND RATE OF REACTION
Marble chips can be broken up with a hammer and graded into 3 or 4 sizes: (a)
coarse powder; (b) pieces about half the size of a rice grain; (c) pieces as large as
rice grains; and (d) the original lumps of marble chips. Place four 100 X 16 mm test
tubes in a stand. Weigh approximately 2 g of each grade, size, of marble chips and
put the four grades separately into each of the four tubes. Obtain four balloons and
blow them up several times to stretch them. Put 5 mL of bench hydrochloric acid into
each of the four balloons and slip the mouth of the balloon over the top of the tube
without letting any acid into the tube. When each balloon is in place, tip the acid into
each test-tube at the same time and observe which balloon is the fastest and the
slowest to be blown up. The smallest should give the carbon dioxide in the shortest
time. Instead of using marble chips you can use granulated zinc. Do not use metals in
powder form because the reaction may be too vigorous and even cause an explosion.
Be careful! This reaction produces hydrogen gas! Instead of collecting the gas in a
balloon or plastic bag, a more accurate method would be to collect the gas in a
burette inverted over water and compare the volume of gas given off in unit time for
each grade of marble chips. Another accurate method is to stand a conical flask
containing the marble chips and acid on a balance and record the loss in mass every
half minute. Carbon dioxide is a heavy gas and most balances will enable the loss in
mass to be found as the gas escapes.

(b) CONCENTRATION AND RATE OF REACTION

The reaction between sodium thiosulphate and hydrochloric acid can take a
noticeable time. Sulphur is produced during the reaction making the solution cloudy.
The rate of reaction can be found by finding the time taken to reach a certain degree
of cloudiness in the solution. The degree of cloudiness in this case may be defined as
the point at which a black cross marked below the reaction vessel can no longer be
seen by looking through the solution from above. In this experiment the
concentration of sodium thiosulphate is made variable, whilst the concentration of
acid is kept constant. Sodium thiosulphate may be bought as "hypo" which is used in
photography. Make up 500 mL of aqueous solution containing 20 g sodium
thiosulphate. 2 M hydrochloric acid is also needed. Bench dilute acid is usually of this
strength. Using a measuring cylinder, put 50 mL of thiosulphate solution into a 100
mL beaker. Place the beaker on a black cross marked on a sheet of paper. Add 5 mL
of the acid and note the time given by the second hand of a clock. Stir the acid into
the solution. Note the time when the cross is no longer visible through the sulphur in
the solution. Repeat the experiment with a smaller concentration of thiosulphate.
Take 40 mL of thiosulphate solution and add 10 mL of distilled water. Stir and then
add 5 mL of acid as before. The time for the cross to become invisible should be
greater than for the last experiment. Repeat the experiment using 30 mL, 20 mL and
10 mL of this sulphate mixed with 20 mL, 30 mL and 40 mL of distilled water. Plot
concentration of the thiosulphate solution against time taken for the reaction.
Concentration values may be taken as the volume of the original thiosulphate
solution used. Since I/time, reciprocal of time, is the measure of the rate of the
reaction, plot thiosulphate concentrations against I/time. The equation for the
reaction can be written as:
Na2S2O3 (aq) + 2HCl(aq) --> H2O (l) + SO2 (g) + S(s)

(c) TEMPERATURE AND RATE OF A REACTION

Use the reaction in experiment 2.92 to investigate the effect of temperature. Put 10
mL of sodium thiosulphate solution into the 100 mL beaker and stir in 40 mL of
water. Use this concentration for the series of experiments with the temperature of
the solution as the variable. Add 5 mL of acid as before and record the initial time
and the temperature of the solution. Record the final time when the black cross
below the beaker is no longer visible. Repeat the experiment, each time warming the
thiosulphate solution to just over 30oC

(c) CATAL YSTS AND RATE OF REACTION

The variable in this reaction is the substance used as a catalyst in the decomposition
of an aqueous solution of hydrogen peroxide. Set up the burette filled with water as
in a standard water displacement experiment. 2 mL of 20-volume hydrogen peroxide
will give enough oxygen almost to fill the burette. Weigh out 1 g each of copper (II)
oxide, nickel oxide, manganese (lV) oxide and zinc oxide. Put 50 mL of water in the
flask and add 2 mL of hydrogen peroxide solution. Add the 1 g of copper oxide.
Immediately insert the bung with the delivery tube into the flask. Time the volume of
oxygen given off at intervals of 15 seconds. Plot the volume of oxygen produced
every 15 seconds against the time of the reaction. Repeat the experiment using the
other oxides as catalysts. Plot a graph for each experiment. Manganese (IV) oxide is
usually used as a catalyst in this reaction. The catalyst is not used up during the
reaction. A catalyst may slow down a reaction as well as speed it up.

19. BREAKDOWN OF STARCH TO SUGAR

FEHLING'S TEST FOR REDUCING SUGARS
Starch can be recognized by the deep blue colour which develops when it is in
contact with iodine solution. This is a very sensitive test. Sugar does not react with
iodine, but sugar will reduce copper (II) in Fehling's solution to red copper (I) oxide,
and this is also a sensitive test. Starch does not react with Fehling's solution. Saliva
contains enzyme catalysts, which convert starch to sugar. This experiment
investigates the progress of this reaction. Put about 10 mL of dilute starch solution
into a test-tube. Add to this 1 mL of saliva and stir this into the starch solution.
Record the time of adding the saliva. At 5-minute intervals, remove 2 or 3 drops by
means of a dropper and put them on a clean white tile, taking care to keep them
from running into each other. The dropper must be washed well between each test.
Put a little iodine solution on each drop. The decreasing intensity of the blue colour
indicates that starch is being used up. Test for increasing amounts of sugar at the
same time as testing for starch. To do this, put 2 or 3 drops of the reaction mixture
into a small test-tube. Add 3 mL of Fehling's solution and warm this mixture almost to
boiling point. The test should show that the amount of sugar is increasing. The
enzyme in the saliva is therefore slowly breaking starch down into sugar, which is a
smaller molecule. In a previous experiment yeast was used to break down sugar into
ethanol, which is an even smaller molecule. Living yeast, which is a variety of fungus,
produces enzymes which act as catalysts in the conversion:
C6H12O6 -> 2C2H5OH + 2CO2

20. BREAKDOWN OF ETHANOL TO ETHENE (ETHYLENE)

Absorb ethanol on to cotton wool or asbestos wool and push this to the bottom of a
hard glass test-tube. In the middle of the test-tube pack small pieces of unglazed
porcelain. Fit a delivery tube to collect ethene gas over water. Have 3 test-tubes
ready to collect ethene. First heat the porous pot strongly and then gently warm the
cotton wool to produce ethanol vapour. This vapour will break down over the hot
porous pot to produce ethene gas and water vapour. The ethene is insoluble in water,
unlike ethanol, and will collect in the test-tubes. Test the 3 samples by: (a) burning
ethene; (b) shaking with a few drops of dilute potassium permanganate solution
made alkaline with sodium carbonate solution, the colour should disappear; (c)
shaking with a little bromine water, the colour again disappears. Disconnect the
delivery tube when you stop heating to avoid a suck back of water onto the hot
porous pot.
20. BREAKDOWN OF POLYMERS
Usually the smallest molecules are gaseous or liquid at room temperature and the
large molecules are solids. Perspex and polystyrene are solid polymers, which can be
broken down to smaller molecules by heat. Put pieces of Perspex or polystyrene in a
hard glass test-tube. Connect a delivery tube as 2.97 From large molecules to small
molecules A Perspex or polystyrene B receiving tube c cold water D a liquid collects.
The collecting test-tube must be cooled thoroughly with cold water, as the fumes are
harmful. Gently heat the test-tube containing the Perspex. The polymer will melt and
give off vapours, which are collected in the receiving tube. Heating must be carefully
controlled to enable all the fumes to be condensed in the receiving tube. A liquid is
obtained. This suggests that the polymer has been broken down by heat to smaller
molecules. The liquid does not return to the solid state unless a catalyst is used. The
specific catalysts are not usually available in school laboratories.

GENERAL EXAMINATION REQUIREMENTS

Apparatus List

This list given below has been drawn up in order to give guidance to schools
concerning the apparatus that is expected to be generally available per student for
examination purposes. The list is not intended to be exhaustive: in particular, items
(such as Bunsen burners, tripods) that are commonly regarded as standard
equipment in a chemical laboratory are not included in this list.

One burette, 50 cm3

A measuring cylinder, 50 cm³ or 25 cm³
A filter funnel
One pipette, 25cm3
Two conical flasks within the range 150cm3 0r 250cm3
A beaker, squat form with lip: 250 cm³
A thermometer, -10°C to + 110°C at 1 °C
A polystyrene or other plastic beaker of approximate capacity 150 cm³
Clocks (or wall-clock) to measure to an accuracy of about 1s. (Where clocks are
specified, candidates may use their own wristwatch if they prefer)
Wash bottle
Test tubes (some of which should be Pyrex or hard glass). Approximately
125 mm x 16 mm
Boiling tubes, approximately 150 mm x 25 mm
Stirring rod

ACCURACY

Unless a question instructs candidates differently they should assume that readings
from equipment and apparatus ought to be made with the following precision:

 Burette readings should be to the nearest 0.05 cm3

  Weighings should be made to 0.01 g or 0.001 g depending on the precision of
the balance
 0 to 1000C thermometers should be read to the nearest 0.50C and 0 to 500C
thermometers to the nearest 0.20C
 Timers will normally be read to the nearest second.

It is important that when candidates record reading they include the appropriate
number of decimal places. For example a burette reading of exactly 24.7 cm 3 should
be recorded in a results table as 24.70cm3. A temperature of reading of exactly 350C
should be recorded as 35.50C.

When titres have to be averaged, it is important that the mean is expressed to either
the nearest 0.05cm3 or to the second decimal point. For example, if a candidate
records four different titres as listed below, the mean can be worked out.

26.50cm3 26.25cm3 26.60cm3 26.65cm3

The candidate is expected to ignore the second titre and average the remaining
three

26.50 + 26.60 + 26.65 = 26.583 this should be recorded as 26.60cm3

3

(to the nearest 0.05cm3)

In general, a final should always be given to the same number of significant figures
as is suggested in the exercise.
A significant proportion of marks for quantitative exercise will be awarded for
accuracy. The marks will be awarded by comparing the candidate’s results with the
teacher’s reports.

CALCULATIONS
Usually calculations will be structured. Candidates will be led through a series of
steps leading to a final value. Since most of the marks for these steps will be for a
correct method rather than the numerical answer, it is important that candidates
include their working even if this seems to be trivial. No marks can be awarded for an
incorrect answer without working but a correct method followed by an incorrect
answer will receive credit.

GRAPHS
Some exercises in practical chemistry will require candidates to treat their readings
graphically. The question will however instruct the candidate which axes to use for
each quantity being plotted. Some useful points for candidates to keep in mind when
constructing graphs are listed below.
 Candidates will normally be instructed to put the dependent variable, the
quantity being measured e.g. temperature on the y- axis. The predetermined
quantity e.g. volume will be on the x-axis.
 The scales should be chosen so that the results are spread out as far apart as
the size of the grid allows but not at the expense of using a sensible scale. For
example using 1cm to represent 3 units might spread the readings better than
using 1 cm to represent 4 units but the scale may be difficult to read. It is
always advisable ton use even scales.
  The origin (0,0) need not necessarily be included on either scale if it is not
relevant. For example if temperature readings between 210C and 280C are
plotted, there is no need to begin the axes at zero.
 The axes must be clearly labelled with the quantity being plotted e.g. mass
and its units e.g. kilograms
 The points plotted may be joined with a straight line or a smooth curve. Since
readings are all subject to experimental error, the line drawn may not
necessarily pass through every point. Points should never be joined by a
series of short straight lines.

Doing a Titration
Begin by preparing your burette, as described on the burette page. Your burette
should be conditioned and filled with titrant solution. You should check for air bubbles
and leaks, before proceeding with the titration.
Take an initial volume reading and record it in your notebook. Before beginning a
titration, you should always calculate the expected endpoint volume.
Prepare the solution to be analysed by placing it in a clean Erlenmeyer flask or
beaker. If your sample is a solid, make sure it is completely dissolved. Put a magnetic
stirrer in the flask and add indicator. Use the burette to deliver a stream of titrant to
within a couple of mL of your expected endpoint. You will see the indicator change
colour when the titrant hits the solution in the flask, but the colour change disappears
upon stirring.
Approach the endpoint more slowly and watch the colour of your flask carefully. Use
a wash bottle to rinse the sides of the flask and the tip of the burette; to be sure all
titrant is mixed in the flask.
As you approach the endpoint, you may need to add a partial drop of titrant. You can
do this with a rapid spin of a Teflon stopcock or by partially opening the stopcock and
rinsing the partial drop into the flask with a wash bottle. Ask your TA to demonstrate
these techniques for you, in the lab.
Make sure you know what the endpoint should look like. For phenolphthalein, the
endpoint is the first permanent pale pink. The pale pink fades in 10 to 20 minutes.

If you think you might have reached the endpoint, you can record the volume reading
and add another partial drop. Sometimes it is easier to tell when you have gone past
the endpoint.
When you have reached the endpoint, read the final volume in the burette and
record it in your notebook.
Subtract the initial volume to determine the amount of titrant delivered. Use this, the
concentration of the titrant, and the stoichiometry of the titration reaction to
calculate the number of moles of reactant in your analyte solution.

Indicators
An indicator is a substance used in titrations, which has one colour in the presence of
an excess of one reagent and a different colour in the presence of an excess of the
other. Examples of indicators include;
(i) Methyl orange
(ii) Phenolphthalein
(iii) Methyl red
(iv) Bromothymol blue
The pH scale

A much more useful measure of the strength of an acid solution was worked out by
the Danish biochemist S. Sorensen. He worked in the laboratories of the Carlsberg
breweries and was interested in checking the acidity of beer. The scale he
introduced was the pH scale. The scale runs from 1 to 14, and the following general
rules apply.

Rules for the pH scale:

a. Acid have a pH less than 7,
b. The more acidic a solution, the lower the pH.
c. Neutral substances, such as pure water, have a pH of 7,
d. Alkalis have a pH greater than 7,
e. The more alkaline a solution, the higher the pH.
The pH of a solution can be measured in several ways. Universal indicator papers
that are sensitive over the full range of values can be used. Some colour changes of
common indicators are shown below.

Indicator colour changes

Indicator Colour change PH Type of acid-

Acid to alkali base titration
Methyl orange Red to yellow 3.5 Strong acid –
strong or weak
base
Litmus Red to blue 6.0 Strong acid –
strong or weak
base
Bromothymol blue Yellow to blue 7.0 Strong acid –
strong or weak
base
Phenolphthalein Colourless to red 9.5 Strong base-
strong or weak
acid

Candidates may be asked to carry out exercises involving:

 Simple quantitative experiments involving the measurement of volumes:

 Speeds of reaction.
 Measurement of temperature based on a thermometer with 10C graduations.
 Problems of an investigatory nature, possibly including suitable organic
compounds.
 Filtration.
 Identification of ions and gasses as specified in the curriculum.

HEALTH AND SAFETY

Candidates must follow the health and Safety policy normally operates in their
laboratories when carrying out the practical Examination. Eye protection must
always be worn. Laboratory overalls are recommended. All substances should be
regarded as being potentially toxic and hazardous. Hazard labels (e.g. flammable)
should be read and appropriate precautions (e.g. keep liquid away from flame) taken.
All substances spilled on the skin should be rinsed off immediately. Chemicals must
never be tasted Gases and vapours should never be smelt unless the question
instructs the candidates to do so and then only with great care.

2.0 QUANTITATIVE ANALYSIS

2.1 Molar solutions and volumetric analysis.

Amount of substance
In quantitative analysis, it is important to measure the amounts or moles of reacting
substances accurately. To do that, we must use values of relative atomic masses
expressed on a periodic table. If we are given the mass of a compound, we can
determine the number of moles.

The first step is to calculate the mass of one mole of the compound by summing up
the relative atomic masses of the constituent atoms. E.g. 1 mole of calcium
carbonate (CaCO3) will have a mass of 40 + 12 + 48 = 100g

10g of CaCO3 will contain 10/100 = 0.1moles

2.2 concentration of a solution

It is very useful to be know exactly how much of a dissolved substance is present

in a solution of particular concentration or volume of a solution. So we need a
standard way of comparing the concentrations of solutions. The concentration of
a solution is determined from the number of moles of solute dissolved in one litre
(1dm3) of solution.

If one mole of a solute is dissolved in water and the volume of the solution made up
to 1litre (1dm3), this solution in known as a molar solution or 1M solution. If two
moles are dissolved in 1litre (1dm3), the resulting solution is 2M and so on.
 MOLES VOLUME (CM3) CONCENTRATION
DISSOLVED (M)
1 1000 1M
1 500 2M
1 250 4M
1 2000 0.5M

You need to be able to calculate

(i) The number of moles or mass of substance in an aqueous solution of

given volume and concentration

(ii) The concentration of an aqueous solution given the amount of

substance and volume of water.

(iii) Use the equation: molarity of Z = moles of Z / volume in dm 3

Remember: moles Z = mass Z / formula mass of Z

Concentration can also be expressed directly in grams per litre (1dm 3). 9.8g of
H2SO4 can be expressed either as 0.1M or 9.8g/dm3

Molarity (M) = g/dm3 / formula mass

Example 1: 5.95g of potassium bromide were dissolved in 400cm 3 of water.

Calculate its molarity. [Ar values: K = 39, Br = 80]

Moles = mass / formula mass, (KBr = 39 + 80 = 119)

mol KBr = 5.95/119 = 0.05 mol

400 cm3 = 400/1000 = 0.4 dm3

molarity = moles of solute / volume of solution

molarity of KBr solution = 0.05/0.4 = 0.125M

2.3 Volumetric calculations (acid-alkali titrations)

Chemical Equations

These balancing numbers have an additional meaning where these amount

calculations are concerned. The balancing numbers give the numbers of moles
present for each chemical involved in the reaction.
For example, sodium chloride may be prepared by the reaction of sodium hydroxide
and hydrochloric acid, according to the following equation -

NaOH (aq) + HCl (aq) NaCl (aq) + H2O (l)

The equation specifies what amounts of sodium hydroxide and hydrochloric acid will
react together and what amounts of products are produced.

1NaOH (aq) + 1HCl (aq) 1NaCl (aq) + 1H2O (l)

This equation states that 1 mol of sodium hydroxide and 1 mol of hydrochloric acid
will react together to give of 1 mol sodium chloride and of 1 mol water.

The ratio of NaOH: HCl: NaCl: H2O is 1: 1: 1: 1.

What this means is that if the amount of any one of the components in the above
reaction is known then the others may be worked out from the ratio above.

Or, if the masses of chemicals reacting together are known then amounts can be
calculated and the balancing numbers deduced from the amounts reacting together.

2.4 Titration Experiment

Titrations can be used to find the concentration of an acid or alkali from the
relative volumes used and the concentration of one of the two reactants.

Titration involves the neutralisation of an acid with an alkali or a soluble

carbonate. Since both reactants and products are colourless, an indicator is used
to find the neutralisation point or end point i.e. the point at which the acid has
been neutralised. This process is done in three stages.

(i) The acid is poured into the burette. A known volume of the alkali is
transferred using a pipette into four separate conical flasks. Two or
three drops of suitable indicator are added to each of the conical
flasks.
(ii) The acid is run into the flask until the indicator just changes colour. The
difference between the initial and final burette readings gives the
volume of the acid used commonly known as the titre. The first
titration usually gives and approximate end point and is treated as the
trial.
(iii) The experiment is repeated for each of the other conical flask, to try to
obtain the end point accurately. This is usually done by running out the
acid to a point one unit away from the trial, the going drop-by-drop
until an accurate end point is obtained. The volume of the acid
required for each change is read off and recorded in a table similar to
the one below.

PROCEDURE DURING TITRATION

 Titrations require continuous shaking of the conical flask and its contents.
  Check the quantity of the pipette as indicated on the bulb of the pipette
and remember to record it in the appropriate place.
 As you release the liquid from a pipette into a conical flask, one should
not blow out the last drop remaining in the jet.
 Before you take any reading from the burette after filling it, first allow the
solution to run out to fill the tap and jet of the burette, and then you begin
taking your readings.
 Always write the reading immediately you take them.
 When completing the table of results, you will be expected to complete all
columns as accurately as the as the limits of the apparatus can allow e.g.
burette used is usually read to the nearest read to the nearest 0.05 cm 3,
pipette is accurate to 0.05 cm 3 (1 drop).
 Use minimum amount of indicator possible (2 – 3 drops) and recognize the
end point has been reached e.g. when the colour just changes.
 Show the values that can be averaged to obtain an acceptable value for
use in calculations (only those values within 0.2 cm 3 should be averaged).
 Attempt to work out the questions from the first principles and not use the
formula method, which has its own limitations.

GENERAL NOTES FOR QUALITATIVE

AND QUANTITIVE ANALYSIS
Indicators
An indicator is a substance used in titrations, which has one colour in the
presence of an excess of one reagent and a different colour in the presence
of an excess of the other. Examples of indicators include;
(v) Methyl orange
(vi) Phenolphthalein
(vii) Methyl red
(viii) Bromothymol blue

Indicator colour changes

Indicator Colour change PH Type of acid-

Acid to alkali base titration
Methyl orange Red to yellow 3.5 Strong acid –
strong or weak
base
Litmus Red to blue 6.0 Strong acid –
strong or weak
base
Bromothymol blue Yellow to blue 7.0 Strong acid –
strong or weak
base
Phenolphthalein Colourless to red 9.5 Strong base-
strong or weak
acid
Candidates may be asked to carry out exercises involving:

 Simple quantitative experiments involving the measurement of

volumes:
 Speeds of reaction.
 Measurement of temperature based on a thermometer with 1 0C
graduations.
 Problems of an investigatory nature, possibly including suitable organic
compounds.
 Filtration.
 Identification of ions and gasses as specified in the curriculum.

QUALITATIVE ANALYSIS

Qualitative analysis is mainly about identification of substances. No emphasis

is laid on amount or quantity. In qualitative analysis exercises, candidates
should use approximately 1cm depth of a solution (1-2cm 3) for each test and
add reagents slowly, ensuring good mixing, until no further change is seen.
Candidates should indicate at what stage a change occurs, writing any
deductions alongside the observations on which they are based. Answers
should include details of colour changes and precipitates formed and the
names and chemical tests for any gases evolved.

Marks for deductions or conclusions can only be gained if the appropriate

observations are recorded.

QUALITATIVE ANALYSIS NOTES

TABLE 1:TESTING FOR GASES

TEST FOR TEST METHOD OBSERVATIONS TEST CHEMISTRY

Hydrogen gas H2 Lighted splint Squeaky pop 2H2(g) + O2(g)
sound (might see 2H2O(l) + energy
condensation on
test tube)
Carbon dioxide Bubble into Turns cloudy - Ca(OH)2(aq) +
gas CO2 limewater fine milky white CO2(g)
(aqueous calcium precipitate of CaCO3(s) +
hydroxide calcium H2O(l)
solution) carbonate
Oxygen gas O2 Glowing splint re-ignites it - C(in wood) + O2(g)
flame CO2(g)
Hydrogen (i) Damp blue (i) Litmus turns (i) Litmus turns
chloride gas HCl litmus or red, red,
(ii) Drop of silver
nitrate on the end (ii) White (ii) White
of a glass rod precipitate with precipitate with
 silver nitrate silver nitrate
Sulphur dioxide Freshly made Paper changes The dichromate
gas SO2 potassium from orange to (VI) ion, Cr2O72-(aq)
dichromate (VI) green is reduced to the
paper green Cr3+(aq) ion
Ammonia gas NH3 Strong pungent (i) Litmus turns (i) Only common
odour, (i) red blue, (ii) white alkaline gas and
litmus, (ii) fumes clouds with HCl (ii) forms fine
conc. fumes. ammonium
hydrochloric acid chloride crystals
with HCl
Chlorine gas Cl2 (i) blue litmus, (ii) pungent green (i) non-metal, is
[test (ii) on its drop silver nitrate gas, (i) litmus acid in aqueous
own is no good, on the end of a turns red and solution and a
could be HCl] glass rod then is bleached powerful
white, (ii) white oxidising agent,
precipitate (ii) forms chloride
ion in water
Nitrogen(IV) No simple Reddish- brown Strong oxidising
oxide (or nitrogen relatively gas agent
dioxide) NO2 unambiguous test
Water vapour H20 (i) White (i) turns from (i) Blue hydrated
anhydrous white to blue, (ii) copper(II) crystals
copper(II) turns from blue or solution
sulphate, (ii) dry to pink formed, (ii)
blue cobalt hydrated cobalt
chloride paper ion formed
[Co(H2O)6]2+
Hydrogen (i)Smell (i)‘Bad eggs’
sulphide (ii)Burning splint (ii)Gas burns-
(iii)Lead (II) sulphur deposits
ethanoate paper (iii)Turns brown-
black

TABLE 2: TEST FOR ANIONS

TEST FOR TEST OBSERVATIONS TEST CHEMISTRY

METHOD
Carbonate ion add any Fizzing - carbonate/hydrogen
CO32- (or dilute strong colourless gas - carbonate + acid
hydrogen acid to the turns limewater salt + water + carbon
carbonate HCO3-) suspected milky cloudy dioxide, then white
carbonate - precipitate with
 if colourless limewater.
gas given
off, test with
limewater
Sulphate To a solution White Ba2+(aq) + SO42-(aq)
ion (SO42-) of the precipitate of BaSO4(s)
suspected barium sulphate any soluble barium salt
sulphate + any soluble sulphate
add dilute barium sulphate
hydrochloric
acid and a
few drops of
barium
chloride or
nitrate
solution
Sulphite ion SO32- (i) Add (i) Choking (i) Sulphite salt +
dilute sulphur dioxide hydrochloric acid
hydrochloric gas formed, (ii) chloride salt + sulphur
acid to the the dichromate dioxide, (ii) the sulphur
suspected paper turns dioxide reduces the
sulphite, (ii) from orange to dichromate (VI) to
test any gas green chromium (III). Note:
evolved with sulphites do not give
fresh ppt. with acidified
potassium barium chloride/nitrate
dichromate because sulphites
(VI) paper dissolve in acids.
Chloride ion Add dilute White Ag+(aq) + Cl-(aq)
Cl- nitric acid precipitate of AgCl(s). Any soluble silver
and silver silver chloride salt + any soluble
nitrate soluble in dilute chloride silver
solution. ammonia. chloride precipitate.

TEST FOR TEST OBSERVATIONS TEST CHEMISTRY

METHOD
Bromide ion Add dilute Cream (i) Ag+(aq) + Br-(aq)
Br- nitric acid precipitate of AgBr(s) any soluble silver
and silver silver bromide, salt + any soluble
nitrate partially soluble bromide silver
solution in dilute bromide precipitate
ammonia
Iodide ion I- (i) Add (i) Yellow (i) Ag+(aq) + I-(aq) AgI(s)
dilute precipitate of any soluble silver salt +
nitric acid silver iodide any soluble iodide
and silver insoluble in silver iodide precipitate,
 nitrate dilute ammonia, (ii) Insoluble lead (II)
solution, (ii) a yellow iodide formed, Pb2+(aq) +
OR (ii) Add precipitate 2I-(aq) PbI2(s)
lead(II) forms
nitrate
solution
Nitrate ion boil the fumes of the aluminium powder
NO3- suspected ammoniaproduc is a powerful reducing
nitrate ed, which turns agent and converts the
with red litmus blue. nitrate ion, NO3-, into
sodium ammonia gas, NH3
hydroxide
solution
and fine
aluminium
powder
Hydroxide ion ie an (i) litmus (i) turns litmus (i) pH meter gives a
alkali OH- or blue, (ii) if value of more than 7,
(ii) add strongly alkaline the higher the pH
ammoniu ammonia should number the stronger the
m salt be released. alkali, the higher the
OH- concentration, (ii)
ammonia gas is
evolved: NH4+(aq) + OH-
(aq) NH3(g) + H2O(l)

TABLE 3: TESTS FOR CATIONS

TEST FOR With aqueous Test with TEST CHEMISTRY

sodium hydroxide aqueous
ammonia
White ppt. White ppt. Mg2+(aq) + 2OH-(aq)
Magnesium(Mg2 insoluble in insoluble in Mg (OH)2(s)
+) excess excess white ppt. The pp
t. is not soluble in
excess of NH3 or
NaOH. You could
distinguish Mg2+
from Ca2+ with a
flame test
Calcium (Ca2+) White ppt. No ppt. or very Ca2+(aq) + 2OH-(aq)
insoluble in slight white ppt Ca(OH)2(s)
excess insoluble in white ppt. The
 excess ppt. is not soluble
in excess of NH3
or NaOH.

Aluminium(Al3+) White ppt. White ppt. Aluminium

soluble in excess insoluble in ion:Al3+ +3OH-
giving a excess Al(OH)3(s) in
colourless excess NaOH
solution forms soluble
(Al(OH)4-)
Zinc (Zn2+) White ppt. White ppt. Zinc ion: Zn2+(aq)
soluble in excess soluble in excess + 2OH-(aq)
giving a giving a Zn(OH)2(s) white
colourless colourless ppt. The ppt.
solution solution dissolves in both
excess sodium
hydroxide and
ammonia to give
a clear colourless
solution.
Lead (Pb2+) White ppt. White ppt.
soluble in excess insoluble in
giving a excess
colourless
solution
Iron(II) (Fe2+) Green ppt. Green ppt. iron(II) ion: Fe2+(aq)
insoluble in insoluble in + 2OH-(aq)
excess excess Fe(OH)2(s) dark
green ppt. The
ppt. is not soluble
in excess of NH3
or NaOH.
Iron (III) (Fe3+) Red-brown ppt Red-brown ppt iron(III) ion: Fe3+
-
insoluble in insoluble in (aq) + 3OH (aq)
excess excess Fe(OH)3(s) brown
ppt.* The ppt. is
not soluble in
excess of NH3 or
NaOH.
Copper (Cu2+) Light blue ppt. Light blue ppt.
insoluble in soluble in excess
excess giving a deep-
blue solution

TABLE 4: ORGANIC TESTS

TEST FOR TEST METHOD OBSERVATIONS TEST CHEMISTRY

ALKENE or bubble gas the orange/brown R2C=CR2 + Br2
alkyne any other through, or add bromine, BrR2C-CR2Br
non-aromatic liquid to, a decolourises, as a Colourless
unsaturated solution of saturated
hydrocarbons bromine in colourless
hexane or water organic bromo-
compound is
formed
(saturated
alkanes give no
fast reaction with
bromine)
Hydroxy group R- Mix it with a few Litmus turns red R-OH + CH3COCl
OH in alcohols (in drops of ethanoyl and a white CH3COOR + HCl
'dry' conditions) chloride, test precipitate with An ester and
fumes with litmus silver nitrate, if hydrogen
and silver nitrate the mixture is chloride are
poured into water formed
you may detect a
'pleasant' ester
odour, can test
for HCl but water
and amines
produce it too!
Carboxylic acids Mix with water Fizzing, RCOOH +
RCOOH and add a little colourless gas NaHCO3
sodium gives white RCOONa +
hydrogencarbona precipitate with H2O + CO2
te solid or limewater
solution

TABLE 5: MISCELLANEOUS TESTS

TEST FOR TEST METHOD OBSERVATIONS TEST CHEMISTRY

Lead (II) ion Add potassium Yellow precipitate Pb2+(aq) +2I-(aq)
iodide solution PbI2(s) lead(II)
yellow precipitate iodide ppt.
Metal Carbonates Sometimes Copper (II)
heating a metal carbonate
carbonate copper(II) oxide +
strongly to carbon dioxide:
decompose it CuCO3(s)
provides some CuO(s) + CO2(g)
clues to its
identity. Adding [green]
 acid CO2 and
the colour of the [black] +
resulting solution [colourless gas,
(e.g. blue Cu2+(aq), test with
may also provide limewater, white
clues. The metal precipitate]
ion solution might
also give a flame zinc carbonate
colour or a zinc oxide +
hydroxide carbon dioxide
precipitate with
sodium hydroxide ZnCO3(s)
e.g. copper. ZnO(s) + CO2(g)

[White]
[Yellow hot, white
cold] +[colourless
gas, test with
limewater, white
precipitate]

Hydrogen ion H+ (i) litmus or (i) litmus turns (i) PH meter gives
or H3O+ universal red, variety of a value of less
indicator or pH colours with than 7, the lower
meter, (ii) add a universal the pH number
little sodium indicator. strong - the stronger the
hydrogen red, weak - acid, the higher
carbonate yellow/orange, (ii) the H+
powder fizzing with any concentration, (ii)
carbonate - test HCO3-(aq) + H+(aq)
for CO2 as above H2O(l) + CO2(g)
Ammonium ion no smell at first, Smelly ammonia Ammonia gas is
NH4+ add COLD sodium evolved and red evolved: NH4+(aq)
hydroxide litmus turns blue + OH-(aq)
solution to the NH3(g) + H2O(l)
suspected
ammonium salt
and test any gas
with red litmus

TABLE 6. FLAME TESTS

A tungsten wire loop is first dipped into some concentrated hydrochloric acid
to dissolve any oxides and hence clean the wire. It is then dipped into salt
powder and introduced into a colourless Bunsen burner flame. The colour is
then observed and inferences made.
Metal ion Symbol Flame colour
Lithium Li+ Scarlet
Sodium Na+ Yellow
Potassium K+ Lilac
Calcium Ca2+ Brick red
Strontium Sr2+ Crimson
Barium Ba2+ Apple green

TABLE 7: HEAT ANALYSIS

Observation on heating Conclusion

Water vapour / steam evolved, turning Crystals contain water of

cobalt chloride paper pink crystallization, or the solid is a
hydroxide which decomposes
Colourless gas evolved which relights a Oxygen from a nitrate of potassium
glowing splint or sodium

Brown gas evolved and a glowing splint Nitrogen dioxide and oxygen from the
relights decomposition of a nitrate

Gas given off which turns limewater Carbon dioxide from the
cloudy decomposition of a carbonate

Pungent gas evolved which turns acid Sulphur dioxide from the
dichromate paper from orange to green decomposition of a sulphate

Sublimate forms on cool part of the Likely to be an ammonium salt.

tube (Ammonia may also be detected with
moist red litmus: it turns it blue.)

Residue turns yellow when hot and then Zinc oxide, which may have been
white again when cold formed by the decomposition of
another zinc compound

Residue which is red when hot and Led (II) oxide, which may have been
yellow when cold formed by the decomposition of
another lead compound

TABLE 8: SOLUBLE AND INSOLUBLE SALTS

 Soluble Insoluble
Bases The alkalis: sodium and All other metal oxides and hydroxides
potassium hydroxides;
calcium hydroxide, which
is slightly soluble;
ammonia.

Salts All nitrates

All chlorides Silver chloride and lead chloride (lead
except chloride is soluble in hot water)
Barium sulphate and lead sulphate;
calcium sulphate is slightly soluble
All sulphates
except All other carbonates

Carbonates of Sodium and

potassium

TABLE 9: GENERAL PRELIMINARY TESTS

COLOUR POSSIBLE IONS IN

SALT
Blue Copper(II)
Pale green Iron(II)
Green Copper(II)
Brown Iron(III)

TABLE 10 : IGNITION ANALYSIS

Candidates may be asked to heat an unknown alone in an ignition tube. The

colour changes or the identity of any gases evolved may provide evidence as
to the identity of the unknown.

COLOUR CHANGE POSSIBLE HYDRATED SALT

Blue to white Copper (II) sulphate
Blue to black Copper (II) nitrate
Pale green to brown Iron (II) salts
TABLE 10: RESIDUE WHEN HOT AND COLD
Residue remaining after ignition may have a different colour when hot and
cold

APPEARANCE OF RESIDUE POSSIBLE IDENTITY

HOT COLD
White Yellow Zinc Oxide
Yellow Red Lead(II)Oxide
Brown Black Iron (III)Oxide
Sublimes - Ammonium salt

TABLE 11: HEATING A SOLID

Gases or vapours may be evolved during heating of the solid

GAS OR VAPOUR POSSIBLE SOURCE
Carbon dioxide Carbonates of metals other than
Group 1 or Hydrogen carbonates of
group 1
Ammonia Ammonium salts
Oxygen alone Group 1 nitrates
Oxygen and nitrogen dioxide Nitrates (other than Na or K)
Hydrogen chloride Hydrated chloride or ammonium
chloride
Water Hydrated salts

TABLE 12: SOLUBILITY

The patterns of solubility for various types of salts

Soluble Insoluble
Salts
Sodium salts All are soluble None
Potassium salts All are soluble None
Ammonium salts All are soluble None
Chlorides Most are soluble Silver chloride, lead (II)
 chloride
Nitrates All are soluble None
Sulphates Most are soluble Barium sulphate, lead (II)
sulphate, calcium sulphate
Ethanoates All are soluble None
Carbonates Sodium, potassium and Most are insoluble
ammonium carbonates

KEY

Ppt = precipitate

Sol = solution

Insol = insoluble

Xs = excess
Dil = dilute

1.HYDROGEN CHLORIDE

Physical Properties

Colour Colourless
Odour Pungent odour
Poisonous
Density Heavier than air.
compared to air
(heavier or
lighter)

Chemical Properties

Solubility in Very soluble in water. It

water reacts with water to form
hydrochloric acid.
Burning Does not support
combustion
Moist pH paper Acidic reaction
Red rose petals No reaction
Specific test It will fume in moist air

Footnotes:

 Dilute hydrochloric acid is one of the three common dilute acids used
in the laboratory.
 Concentrated hydrochloric acid is used in the manufacture of many
chemicals.

2.CARBON DIOXIDE

Physical Properties

Colour Colourless
Odour Odourless
Density Heavier than air
compared to air
 (heavier or
lighter)

Chemical Properties

Solubility in Fairly soluble in water. It

water reacts with water to form a
weak acid called carbonic
acid.
Burning Does not support
combustion.
Moist pH paper Shows a weak acidic
reaction (around pH6)
Red rose petals No change
Specific test Turns lime water "cloudy"

Footnotes:

 Makes up 0.04% of the gases in the air. Rainwater is slightly acidic

because carbon dioxide dissolves in it.
 Needed by green plants during photosynthesis.
 Product of respiration in living things.
 Product of combustion
 Is one of the "greenhouse" gases present in the atmosphere.
 Used in fire extinguishers since it is heavier than air and forms a
"blanket" around the fire. This prevents combustion since carbon
dioxide does not support it and the presence of carbon dioxide stops
oxygen reaching the combustible material.

3.CHLORINE GAS

Physical Properties

Colour Greenish-yellow
Odour Pungent odour
Poisonous
Density Heavier than air
compared to air
(heavier or
lighter)
Chemical Properties

Solubility in Soluble in water. Most of it

water reacts with water to form
acids.
Burning Does not support
combustion.
Moist pH paper Shows a strong acidic
reaction
Red rose petals Would bleach and lose
their colour
Specific test None

Footnotes:

 One of the "family" of halogen gases (iodine and bromine are in the
same family)
 Used in water purification.
 Used to make bleaching powder, disinfectants and antiseptics
 Also used to make some explosives, poison gases and pesticides.

4.HYDROGEN CHLORIDE GAS

Physical Properties

Colour Colourless
Odour Pungent odour
Poisonous
Density Heavier than air.
compared to air
(heavier or
lighter)

Chemical Properties

Solubility in Very soluble in water. It

water reacts with water to form
hydrochloric acid.
 Burning Does not support
combustion
Moist pH paper Acidic reaction
Red rose petals No reaction
Specific test It will fume in moist air

Footnotes:

 Dilute hydrochloric acid is one of the three common dilute acids used
in the laboratory.
 Concentrated hydrochloric acid is used in the manufacture of many
chemicals.

5.HYDROGEN GAS

Physical Properties

Colour Colourless
Odour Odourless
Density Lighter than air. Can
compared to air escape through the
(heavier or atmosphere into space.
lighter)

Chemical Properties

Solubility in Insoluble
water
Burning Explodes when a burning
match is placed into it.
Reacts with oxygen gas to
form water.
Moist pH paper No reaction
Red rose petals No reaction
Specific test A lighted match will
produce a "squeak" sound.
This is a small explosion.

Footnotes:
  The lightest gas known.
 Once used in airships but replaced by helium which is not explosive.
 Used to make ammonia which is needed in the manufacture of
fertilizers and explosives.

6.NITROGEN

Physical Properties

Colour Colourless
Odour Odourless
Density Same as air
compared to air
(heavier or
lighter)

Chemical Properties

Solubility in Slightly soluble

water
Burning Does not support
combustion
Moist pH paper No reaction
Red rose petals No reaction
Specific test None

Footnotes:

 Makes up around 79% of the gases in the air.

 Used to make ammonia gas, which in turn is used to make explosives
and fertilizers.
 Used in light bulbs and thermometers because it is not reactive.
 Also used as the atmosphere in rooms where explosives are stored.

7.OXYGEN
Physical Properties

Colour Colourless
Odour Odourless
Density Slightly heavier than air
compared to air
(heavier or
lighter)

Chemical Properties

Solubility in Slightly soluble in water

water
Burning Oxygen gas is needed for
burning or combustion.
Something that burns in air
will burn five times more
ferociously in pure oxygen
gas.
Moist pH paper No change
Red rose petals No change
Specific test A glowing match or
wooden spill will relight
when placed in oxygen
gas.

Footnotes:

 Makes up 20% of the gases in the air.

 Needed by the majority of living organisms for respiration

Is produced by green plants as a by-product of photosynthesis.

8.SULPHUR DIOXIDE GAS

Physical Properties
 Colour Colourless
Odour Pungent odour
Density Heavier than air
compared to air
(heavier or
lighter)

Chemical Properties

Solubility in Soluble. It reacts with

water water to form a strong
acid.
Burning Does not support
combustion
Moist pH paper Acidic reaction
Red rose petals Are bleached and lose their
colour
Specific test None

Footnotes:

 It is used as a bleaching agent.

 It is one of the gases responsible for air pollution.