Practical Paper 3 Notes

1 Make up a volumetric solution and carry out a simple acid–base titration

2 Measurement of an enthalpy change
3 Investigation of how the rate of a reaction changes with temperature
4 Carry out simple test-tube reactions to identify:
● cations – Group 2, NH4+
● anions – Group 7 (halide ions), OH–, CO32–, SO42

5 Distillation of a product from a reaction

6 Tests for alcohol, aldehyde, alkene and carboxylic acid
7 Measuring the rate of reaction:
● by an initial rate method
● by a continuous monitoring method

8 Measuring the EMF of an electrochemical cell

9 Investigate how pH changes when a weak acid reacts with a strong base and
when a strong acid reacts with a weak base
10 Preparation of:
● a pure organic solid and test of its purity
● a pure organic liquid

11 Carry out simple test-tube reactions to identify transition metal ions in

aqueous solution
12 Separation of species by thin-layer chromatography
General Safety Notes
- Wear goggles to prevent any chemicals from entering the eyes. Gloves may also
be necessary for those with sensitive skin. Harmful gases may touch the eye
which may cause damage.
General Evaluation Notes
- To ensure reliability, repeat the experiment 3 times. The more repeats there are
the more reliable the data is. It also allows anomalies to be identified.
- Check if the repeats are concordant. This will also show if it is more reliable
because by replicating the same experiment there hasn't shown significant
difference which may highlight it is an anomaly.
Practical 1 - Titration

Practical 2 - Enthalpy Change

The aim of this practical is to measure the enthalpy change using a simple
calorimeter.
Safety
Each student will use a fairly large amount of
copper sulfate(VI) and it has an environmental
warning. This is because Cu2+ ions are toxic to
plants, algae and a variety of other organisms
that reside within lakes and rivers, hence a
high concentration can have disastrous effects
on the ecosystem.

Waste will be an issue so solutions should be

collected, filtered and allowed to evaporate so
that copper sulfate(VI) can be recycle.

Copper (II) Sulfate is toxic therefore should be

kept away from the mouth at all times.
Brief practical instructions​:
- Place polyester cup in the glass beaker.
- Put in waters
- Place the lid on top
- Add the thermometer
- Measure at regular 1 minute interval change and tabulate.
- Add the substance that is being tested e.g copper anhydrous
Do not measure in the minute after the substance has been added.
- Measure from the next minute
- Continue measuring in constant intervals.

Side practical notes:

- A lower volume of water is used in hydrated copper sulphate as water is already
inside the crystal so a slightly lower volume is used so the total volume of water
is still the same.
- You can make anhydrous copper sulphate by heating up the hydrated copper
sulphate with a bunsen burner then store in a dessicator(a storage compartment
to prevent the reactant from reacting with water in the air).
Graphing Data:
Plot a graph of time
against
temperature.As you
can see here, you
extrapolate both lines
and you take the
difference in
temperature at the 4
minute point where
the substance was
added.

The graph of hydrated

copper sulphate
barely changed and
that is due to the copper already being hydrated so there should not be any expected
change in temperature due to it.

Calculations

Using q=mc∆t we can work out the enthalpy change of the reaction.

M is the mass of the water(Presume density to be ​1 g/cm³​)

C is the specific heat capacity of water (4.18J/g​°​K)
T is the change in temperature (As this is the change treat temperature in
kelvin same as in degrees)

Our example:
Q = Heat energy change in Joules
M = 24
C = 4.18
T = 8.4

So q = 24 x 4.18 x 8.4 = 108.72J

Evaluation of practical

Issues that can arise:

- The temperature keeps rising even after a minute. If this is the case then repeat
the experiment and make sure you have correctly timed it to a minute. It will
come down later on so a line of best should still be able to be be drawn.
 Practical 3 - Investigation of how the rate of a reaction changes with
temperature
The aim is to test if varying temperature affects the rate of reaction of sodium
thiosulphate and hydrochloric acid. The reaction between these two reactants gives a
sulphur precipitate. This can be used to tested to see how long it takes for this
precipitate to form a certain amount.

Safety
- Sulphur dioxide is produced in this reaction which is toxic and can affect people
with asthma. Ventilation should be in place to remove the sulphur dioxide.
- Use a stop bath with sodium carbonate and phenolphthalein to remove the
sulphur dioxide. The indicator is there to see when the stop bath needs replacing.
A fume cupboard would be useful to place this to so the sulphur dioxide can be
extracted.

Brief Instructions
- Place the sodium thiosulphate in a container with an X at the bottom and put the
container inside a water bath.
- Add 1ml of HCL and start the timer.
- Stop the timer when you stop seeing the cross
- measure the temperature now and record it.
- Repeat the steps above for varying temperature lower than 55.
Additional notes and precautions
- We take the averages of the temperature to give a more accurate reading to
cater for temperature fluctuations.
- You do not exceed 55C because at the precipitate may form instantly which is
hard to measure.
This shows the rate increasing as temperature increases. The secondary source shows
a similar sort of curved straight line rather than a full straight line.(Question: Why is it
increasing in a slightly exponential fashion at higher temperature?).
Arrhenius equation

k = 1/t
Calculation

Using the gradient number 41.04.

Because the gradient -Ea/R then you multiply it by R which is 4.18. -m =

-Ea/R so m can be taken as positive. -m as there is a negative correlation.

41.04 x 8.31 = 341J = 0.341kJ

The intercept is ln A. To remove the ln u ln A to the power of e(e^lnA) to

make it A.

A = e^intercept = e^-0.36052 = 0.0272

Evaluate

- Taking more repeats for teach temperatures could increase the reliability of the
experiment.
- A better way to conduct the experiment is using a cuvette to give a distinct end
point as the fading of the black cross is slightly subjective.
 Practical 4
Safety
Wear gloves when handling testing halide ions due to the concentrated sulfuric acid to
give you time to take off the glove so the acid does not corrode your skin.

Test Brief Practical Results Image

Instruction

NaOH to test group - Add the cation Barium -

2 elements in the tube Colourless
with NaOH Strontium -
dropwise then Calcium - Slight
add excess white precipitate
and shake. Magnesium -
white percipitate in
excess
(MgOH is the
most insoluble)

H2SO4 to test - Add h2so4 Barium - White ppt

group 2 elements dropwise into Strontium - White
the test tube ppt
and shake Calcium - slight
well. white ppt
Magnesium -
colourless
Barium sulphate is
insoluble

Test for ammonium - Add NaOH Forms ammonium

ions and warm the hydroxide which
mixture. turns the litmus
- Hold a damp paper blue as it is
litmus paper a base.
to the mouth
of the test
tube.

Test for hydroxide Use a damp - It turns damp

ions litmus(dampen with red litmus paper
deionized blue
water)paper and
 place it in the test
tube with solution or
in the petri dish with
a filter paper.

Test for carbonate 1) Add HCL to The limewater will

ions the carbonate become cloudy
compound due to the CO2
2) Put delivery produced
tube in which
is attached to
the limewater

Test for sulphate Add equal amounts Forms barium

ions of HCL and BaCl2 to sulphate which is
the sulphate a white precipitate
compound

Test for halide ion Add nitric acid to the Cl - White ppt,
in aqueous solution halide compound dilute ammonia
then add some causes it to go
ammonia then add colourless.
excess ammonia. Br- Cream ppt to
colourless in
excess ammonia
I - Yellow ppt and
ammonia causes
no change

Test for halide ions - Add conc They all undergo

in solid salts sulphuric acid effervescence
- Test with blue
litmus paper Bromine produces
- Test the brown gas
bromine ion produced solution
with turns deep
potassium brown/red. Filter
dichromate paper goes from
dipped filter orange to green
paper due to potassium
- Test the dichromate
iodine with a
filter paper Iodine - solution
with lead goes red/brown
nitrate instantly
solution Brown gas
produced. Lead
nitrate - turns blue
black from white
 Practical 5
To prepare cyclohexene by the dehydration of cyclohexanol and to distil the
cyclohexene from the reaction mixture.

A phosphoric acid catalyst will also be used

Brief practical overview

Add phosphoric acid​ drop by drop ​(as it is exothermic and you wouldnt want it to
overheat)​ to the cyclohexanol which is in a pear shaped flask. Swirling mixture as well
to allow for the catalyst to spread evenly. Add anti bumping granules which ​they will
prevent superheating of the liquid being distilled and they will cause a more controlled
boil​, eliminating the possibility that the liquid in the ​distillation flask​ will bump into the
condenser.
Put in the condenser to prevent vapour from escaping. Heat the mixture in the flask to
70C. Remove the condenser and attach it like a distiller. Boil it with a small blue flame
so the liquid doesn't start spitting. Distill all the product with a boiling point below 100.
Stop it when white fumes form ​because at this time mass is starting to be lost so the
percipitate.

Purification
Transfer impure cyclohexene to the separating funnel. Wash organic layer
with saturated solution of NaCl. Then add aqueous sodium carbonate and
wash then wash with water. Then separate out the mixture using the
separating funnel and remove the lower layer and then get another conical
flask to obtain the top layer.

Drying
Add calcium chloride to the mixture.

Testing
Use bromine water to test if it is an alkene. Positive will show
decolourisation.
Potassium dichromate will oxidise the alcohol and change colour from
orange to green.
 Practical 6

Aim: To test for alcohol, aldehyde, alkene and carboxylic acid

Safety - Carefully dispose products such as the sodium ethoxide which is

very basic therefore highly corrosive.

Testing Brief Practical Result Image

Outline
Alcohol Add sodium into Fizzing, you can
alcohol test tube use a lighted
splint to check it
is hydrogen as it
will give off a
squeaky
pop.​(This is a
really bad test as
any sort of base
even water with
sodium can give
off hydrogen)
Aldehyde Mix Fehling A Aldehyde will be
and Fehling B oxidised and the
and add to a test Cu2+ ions will be
tube with sodium reduced to Cu+
carbonate with ions in the
anti bumping copper oxide
granules. which produces
a brick red ppt
Alkene Add bromine Bromine water
water decolourises if
positive
Orange ->
Colourless
Carboxylic acid Add sodium Effervescence
carbonate to the
carboxylic acid
Halogenoalkane Add sodium Chlorine - White
hydroxide at 60C Bromine - cream
to ​allow for the Iodine - yellow
elimination
reaction. ​Add
dilute nitric acid
to ​remove
unwanted
anions.​ Then
add silver nitrate
 Practical 7
The aim is to test the rate of reaction of iodine with the change in
concentration of iodide ions

H2O2(aq) + 2H+(aq) + 2I– (aq) → I2(aq) + 2H2O(l)

2S2O3 2– (aq) + I2(aq) → 2I– (aq) + S4O6 2– (aq)

We will use starch as an indicator to test for the I- ions. It will turn blue
black.

Brief outline of practical

Prepare varying concentrations of potassium iodide by varying the amount of water and
potassium iodide and keep everything else the same.
Add the sodium thiosulphate at the end and start timer and stop the timer when it turns
blue black. Remember to keep stirring so all the content is evenly distributed.

Extra note: The hydrogen peroxide is the reagent controlling the time of the reaction and
the concentration stated above can be varied as required
Evaluation
Use a magnetic stirrer as this will ensure the stirring is constant and
prevents there from being a big change due to varying stirring speeds from
human stirring,

Practical 8
Aim: Measure the EMF of the Cell

Safety:
Propanone is flammable, keep away from open flame
Zinc sulphate and copper sulphate are harmful so if they touch your skin
rinse off immediately.

Brief outline of the experiment

Clean the piece of copper and zinc with emery paper and degrease the metal using
cotton and propanone. (
Place the rods in their respective solution (zinc with zinc sulphate and copper with
copper sulphate) both with the same concentration and volume in their beakers.
Place a salt bridge(NaCl) between the solutions

Additional notes: Voltmeter has high resistance so no current flows so max potential
difference can be measured.
Salt bridge is there to conduct the charge of the free moving ions to complete the circuit.
A wire would would make an electrode system with the solution.

Platinum is used as it conducts electricity and doesn’t react to the HCL. Using porous
platinum increases the surface area

The paper is filter paper. This is a convenient system to check the emf of
different metal samples as it can be easily changed.

Practical 9
Aim:​ Investigate the changes when a weak acid reacts with a strong base

Calibration Outline
Rinse the pH probe with deionized water and remove excess water. Place in varying
buffer solutions and record the pH and rinse each time. Plot pH reading of probe against
the pH of the buffer solution producing a calibration curve.

pH measurement of acid and alkali

Measure the pH of the acid using a probe attached and record every time you add alkali
in small proportions using the burette and stir constantly. When near end point add in
smaller increments. Keep adding until alkali is excess. Amount of alkali added in the x
axis and pH in the y-axis. Use the calibration curve to adjust your pH reading you
recorded.

Practical 10
Aim: Prepare an organic sample and test the purity

Brief instructions

Measure out the mass of salicylic acid and put it into a flask. Mix it with ethanoic
anhydride.
25 cm3 measuring cylinder boiling tube ethanol thermometer deionised or distilled
water in a wash bottle 250 cm3 beaker 100 cm3 conical flask stirring rod kettle
access to a digital mass balance (reading to 2 decimal places). Suggested method Part
1 Preparation a) Weigh out approximately 6.00 g of salicylic acid directly into a 100 cm
3 conical flask. b) Record the mass of salicylic acid used. c) Using a 10 cm 3 measuring
cylinder, add 10 cm 3 of ethanoic anhydride to the flask and swirl the contents. d) Add 5
drops of concentrated sulfuric acid to the flask and swirl the mixture in the flask for a few
minutes to ensure thorough mixing. e) Warm the flask for about 20 minutes in a 400 cm
3 beaker of hot water at approximately 60 °C. The temperature in the flask should not
be allowed to rise above 65 °C. f) Allow the flask to cool and pour its contents into 75
cm 3 of water in a beaker, stirring well to precipitate the solid. g) Filter off the aspirin
under reduced pressure, avoiding skin contact.

Collect the crude aspirin on a double thickness of filter paper and allow it to dry Part 2
Purification a) Using a 25 cm3 measuring cylinder, measure out 15 cm3 of ethanol into
a boiling tube. b) Prepare a beaker half-filled with hot water at a temperature of
approximately 75 °C. The safest way to do this is to use a kettle of boiling water and
add water from the kettle to cold water in the beaker until the temperature is at
approximately 75 °C. NB The boiling point of ethanol is 78 °C and the temperature of
the water in the beaker should not be allowed to go above this. c) Use a spatula to add
the crude aspirin to the boiling tube and place the tube in the beaker of hot water. Do
not scrape the filter paper. d) Stir the contents of the boiling tube until all of the aspirin
dissolves into the ethanol. e) Pour the hot solution containing dissolved aspirin into
approximately 40 cm3 of water in a 100 cm3 conical flask. If a solid separates at this
stage, gently warm the contents of the flask in the water bath until solution is complete.
You should avoid prolonged heating, since this will decompose the aspirin. f) Allow the
conical flask to cool slowly and white needles of aspirin should separate. g) If no
crystals have formed after the solution has cooled to room temperature, you may need
to scratch the insides of the flask with a glass stirring rod to obtain crystals. Cool the
whole mixture in an ice bath. h) Filter off the purified solid under reduced pressure and
allow it to dry on filter paper. i) Record the mass of the dry purified solid. Analysing the
effectiveness of this method of preparation of aspirin a) Calculate the theoretical yield of
aspirin which should be formed from 6.00 g of salicylic acid. b) Calculate the percentage
yield of aspirin from your experiment and comment on the reasons for the losses that
have occurred during the preparation and the purification of the solid. c) Calculate the
atom economy for the preparation of aspirin by this method. d) Consider the reasons
why the alternative preparative method which uses ethanoyl chloride rather than
ethanoic anhydride, is not favoured by industry even though this alternative method has
a higher atom economy.
To test the purity of an organic solid by measuring its melting point The purity of an
organic solid can be determined in part by measuring its melting point and comparing
the value with the known Data Book value of the melting point for that compound. A
pure dry solid will melt at a precise temperature whereas an impure solid will melt over a
range of temperatures which are lower than the melting point of the pure solid. Melting
point apparatus varies in type from the most simple using an oil bath to the more
sophisticated electrothermal devices. In every case, the same general principle applies
that the heating of a small quantity of the solid in a thin-walled melting point tube should
be undertaken slowly and with care. When melting occurs, the solid should collapse into
a liquid without any change in temperature and the way in which this occurs can give a
clue to the purity of the solid. Repeat measurements should be taken with further
samples of the organic solid to verify the reliability of the value obtained. The method
will not work if the solid decomposes on heating. Requirements You are provided with
the following: pure benzenecarboxylic acid other pure organic solids as desired by the
centre thermometer (0 °C to 250 °C range) melting point apparatus to include either:
an electrothermal melting point apparatus or oil bath (Thiele tube or small beaker
halffilled with mineral oil) tripod, gauze and Bunsen burner rubber ring to attach
melting point tube to thermometer (if needed) melting point tubes watch glass spatula.
a) Powder a sample of the organic solid by crushing it gently with a spatula onto the
surface of a filter paper. b) Fill three melting point tubes with the organic solid to a depth
of approximately 0.5 cm. c) Set up the melting point apparatus provided and mount one
of the melting point tubes ready for taking a measurement. d) Heat the apparatus gently
and observe the temperature at which the solid collapses into a liquid. The melting point
will be in the range 100 °C to 200 °C. e) Allow the melting point apparatus to cool and
repeat the measurement of the melting point of the solid with the other two samples. If
the first reading is taken as an approximate value, then the subsequent heating of the
other two samples can be done much more slowly as this approximate value is
approached. f) On the basis of the three measurements that you have taken, record the
melting point of the organic solid. g) Ask your teacher for the Data Book value of the
melting point for the solid that you have tested and compare this value with your own