CP 1: INVESTIGATE THE COMPOSITION OF INKS USING SIMPLE DISTILLATION AND PAPER

CHROMATOGRAPHY

SIMPLE DISTILLATION

AIM
To investigate the composition of inks using simple distillation and paper chromatography.

EQUIPMENT LIST
 250 cm3 beaker
 Quickfit Apparatus (including a condenser with rubber tubing, a fractionating column and
connectors)
 Round-bottomed or pear-shaped flask
 Bunsen burner
 Clamp and stand
 Cold water tap
 Thermometer

METHOD
1. Add a small volume of ink to a flask and connect the flask to a condenser (thermometer may also be
added). Connect the condenser to a tap and place a beaker at the end of the opening.
2. Using a Bunsen burner, heat the flask slowly so that the ink simmers. Be careful not to heat the flask
too strongly. Move the Bunsen burner away if it starts boiling vigorously.
3. Collect a sample of the distilled solvent. Turn the Bunsen burner off when finished.

KEY POINTS
 Condenser should be horizontal with water entering at the bottom and leaving at the top.
 The flask should not be heated too strongly as this could cause the water to boil over into the
beaker collecting the distillate.

DIAGRAM:

SAFETY PRECAUTIONS
 Turn off the gas or leave the Bunsen burner on orange
safety flame when not in use.
 Tie back long hair.
 Keep flammable substances away from the flame.
 Be careful of the glassware. Clean up any smashed glass
immediately.

ANALYSIS OF RESULTS
The temperature recorded on the thermometer can be used
to identify the solvent present in the ink by comparing it to
the boiling point of possible solvents.
PAPER CHROMATOGRAPHY

AIM
Investigate the composition of inks using simple distillation and paper chromatography.

EQUIPMENT LIST
 250 cm3 beaker
 Ruler and pencil
 Distilled water or suitable solvent
 Chromatography paper
 Pipette or capillary tube

CHEMICALS REQUIRED
 Distilled water or suitable solvent
 Ink mixture to be separated

METHOD
1. Use a pencil to draw a line across the chromatography paper, 2 cm from the bottom.
2. Use the pipette or capillary tube to add small dots of different inks to the line on the
chromatography paper. Make sure they are not placed too close together.
3. Place the paper in a beaker containing 1 cm3 of solvent and leave the solvent until it has
moved 2/3 of the way up the paper.
4. Remove the chromatogram from the solvent. Mark where the solvent reached by drawing a
horizontal line across the chromatography paper at this point.
5. Leave the chromatography paper until the solvent has dried.
6. Measure the distance travelled by the solvent front and the spots from the pencil line.

KEY POINTS
 Pencil should be used to draw the line on the chromatography paper as it is insoluble in the
solvent so it will not travel up the paper.
 Ink spots should be placed above the level of solvent in the beaker to prevent them
dissolving in the solvent and being washed away.
 The chromatography paper should be removed from the
solvent before the solvent front reaches the top to allow
the Rf values to be calculated. Spots with the same Rf
value for the same mobile and stationary phases are
likely to be the same substance

DIAGRAM:

SAFETY PRECAUTIONS
 Wear safety goggles and gloves when handling harmful
solvents.
 Use a well-ventilated lab or fume cupboard when using harmful solvents.
 Clear up any spillages or broken glassware immediately.

ANALYSIS OF RESULTS
 Calculate the Rf value of each ink spot using the formula:
 Rf = distance moved by substance ÷ distance moved by solvent.
 Compare Rf values and colours of each ink spot.

CP 2: INVESTIGATE THE CHANGE IN PH ON ADDING POWDERED CALCIUM HYDROXIDE OR

CALCIUM OXIDE TO A FIXED VOLUME OF DILUTE HYDROCHLORIC ACID

INVESTIGATING PH (NEUTRALISATION)

AIM
Investigate the change in pH on adding powdered calcium hydroxide or calcium oxide to a fixed
volume of dilute hydrochloric acid.

EQUIPMENT LIST
 25 cm3 measuring cylinder or volumetric pipette and pipette filler
 Beaker
 Glass rod
 Universal indicator or pH probe
 Spatula

CHEMICALS REQUIRED
 Hydrochloric acid
 Powdered calcium hydroxide or calcium oxide

METHOD
1. Using the measuring cylinder or volumetric pipette, add 25 cm3 of dilute hydrochloric acid to
a beaker.
2. Add a few drops of universal indicator. Compare the initial colour of the solution to a pH
colour chart and record the pH. Alternatively, a pH probe can be used.
3. Add calcium hydroxide or calcium oxide (one level spatula at a time) to the beaker, stirring
and recording the pH between additions.
4. Stop adding calcium hydroxide/calcium oxide when the pH remains constant.

KEY POINTS
 The equations for the reactions, depending on which base is used, are: CaO + 2HCl → CaCl2
+H2O Ca(OH)2 + 2HCl → CaCl2 + 2H2O
 A volumetric pipette offers greater accuracy than a measuring cylinder when measuring the
volume of hydrochloric acid.
 Stirring the solution before taking a pH reading ensures the reaction is
complete and that the pH is consistent throughout the mixture.
 Using a pH probe instead of universal indicator offers greater accuracy.

DIAGRAM:

SAFETY PRECAUTIONS
 Safety glasses must be worn.
 Hydrochloric acid is corrosive in high concentrations. Wash hands
immediately after any contact with the skin.
 Calcium hydroxide may cause skin and eye irritation so wear gloves and
safety goggles. Wash hands immediately after any contact with the skin.
 Clear up any spillages or broken glassware immediately.

ANALYSIS OF RESULTS
The starting pH and final pH can be recorded to investigate the effect of adding calcium
hydroxide/calcium oxide to hydrochloric acid.

CP 5: CARRY OUT AN ACCURATE ACID-ALKALI TITRATION, USING BURETTE, PIPETTE AND A

SUITABLE INDICATOR

ACID-ALKALI TITRATION

AIM
To carry out an accurate acid-alkali titration using a burette, pipette and a suitable indicator.

EQUIPMENT LIST
 50 cm3 burette
 25 cm3 pipette with pipette filler
 250 cm3 conical flask
 100 cm3 beaker
 Funnel
 White tile
 Burette clamp and stand

CHEMICALS REQUIRED
 Phenolphthalein indicator
 0.4 mol/dm3 hydrochloric acid
 Sodium hydroxide solution (unknown concentration)
 Deionised water

METHOD
1. Add exactly 25 cm3 of sodium hydroxide to a conical flask using a pipette and pipette filler.
Add a few drops of phenolphthalein indicator to the conical flask then place the conical flask on
a white tile.
2. Setup the burette in the clamp and stand. Close the tap and use a funnel to pour about 10
cm3 of hydrochloric acid into the burette.
3. Place a beaker under the burette and open the tap, allowing the tip of the burette to fill with
acid and displace any air bubbles.
4. Close the tap before the burette empties then use a funnel to fill the burette with acid.
Record the initial burette reading to the nearest 0.05 cm3.
5. Place the burette above the conical flask. Carry out a rough trial titration, adding the acid 1-2
cm3 at a time, swirling the conical flask constantly.
6. Close the burette tap as soon as the solution decolourises. Record the final burette volume
and calculate the volume of acid that has been added from the burette.
7. Rinse the conical flask with deionised water then add 25 cm3 of sodium hydroxide. Refill the
burette if necessary and record the initial volume of acid in the burette.
8. Using the rough titre as guidance, add the acid to the conical flask until within about 4 cm3 of
the rough titre volume. Add the acid drop by drop after this, swirling constantly until the
endpoint is reached. Record the final burette reading and use this value to calculate the titre
volume.
9. Repeat steps 7 and 8 until concordant titres are obtained (results within 0.1 cm3).
10. Use the concordant results to calculate the mean titre.

KEY POINTS
 The equation for this reaction is: HCl + NaOH → NaCl + H2O
 The white tile is used to make the colour change of
the indicator easier to see so the end point can be
identified.
 The conical flask is swirled to ensure all the
reactants are mixed together throughout the
experiment. This ensures an accurate end point is
obtained.
 The rough titre must not be used to calculate the
mean as it is not accurate enough.
 The indicator phenolphthalein is colourless in acids
and pink in alkalis.
 When reading the volume of acid in the burette, it
should be read at eye level from the bottom of the
meniscus (the curve of the liquid).
 The end point is the point at which the indicator
first changes colour.

DIAGRAM:

SAFETY PRECAUTIONS
Safety goggles must be worn at all times.
Fill the burette below eye level to prevent chemicals splashing into someone's face. This can be
achieved by placing the burette on the floor when it is being filled.
Sodium hydroxide is an irritant so avoid contact with the skin. If the skin comes into contact,
wash immediately.
Hydrochloric acid is corrosive. Although a low concentration is being used in this experiment,
treat with the same precautions as sodium hydroxide.
Take care when using fragile glassware like the burette and pipette. Clear up any broken glass
immediately.

ANALYSIS OF RESULTS
The results from each titre can be recorded in a table similar to the one below. More columns
may be added until 2 concordant results are obtained:

To determine the concentration of the sodium hydroxide used: HCl + NaOH → NaCl + H2O
From the equation above it is easy to identify that hydrochloric acid and sodium hydroxide react
in a 1:1 ratio. Therefore, to find the concentration of alkali:
1. Find the moles of HCl used by multiplying the mean titre of HCl (in dm3) by the
concentration. The 1:1 ratio can be used to find the number of moles of NaOH that reacted (this
will be the same as the number of moles of HCl).
2. Divide the moles of NaOH by the volume used (dm3).
3. This value is the concentration of NaOH. Round it to 3 significant figures.