Chemistry Ah Pa

CFE Advanced Higher Chemistry
Practical Activities
1.
Preparation of Standard 0.1 mol l-1 Oxalic Acid Solution
2.
Standardisation of Approximately 0.1 mol l-1 Sodium Hydroxide Solution
3.
Determination of Ethanoic Acid Content of Vinegar
4.
Preparation of Potassium Trioxalatoferrate (III)
5.
Colorimetric Determination of Manganese in Steel
12
6.
Complexometric Determination of Nickel using EDTA
15
7.
Gravimetric Determination of Water in Hydrated

Barium Chloride
18
8.
Determination of Nickel using Dimethylglyoxime
20
9.
Preparation of Cyclohexene
23
10.
Identification by Derivative Formation
25
11.
Preparation of Benzoic Acid by hydrolysis of Ethyl

Benzoate
28
12.
Preparation of Aspirin
31
13.
Aspirin Determination
34
14.
Thin-layer Chromatography of Aspirin
37
page 1
Writing a Report on an experiment n Chemistry

This advice is designed to help you write a Report to meet the performance criteria of Outcome 3.
You must have played an active part n setting up the experiment and collecting results.
When writing your experimental Report avoid the use of the words 'I' and 'We'. Always use past
tense in writing Reports. Write your Report using the following headings and pay attention to the
advice under each heading.
It is useful to structure your Report under specific headings to avoid missing out important sections.
Title
Use the title in the Student Instruction Sheets.
Introduction
A brief statement of the aim(s) of the experiment.
A brief description of the background theory of the experiment.
Procedure
Write a brief description of how the experiment was carried out.
Do not put in too much detail, just sufficient so that anyone reading your Report would know what
you did rather than be able to repeat the experiment exactly. You should give the following
information as appropriate:
labelled diagram or description of the apparatus, instruments used

measurements taken or observations made
comments on safety.
page 2
Results
Include in this section all measurements and observations you make during the experiment as well
as your analysed results which you should present in an appropriate format.
Readings or observations should be recorded using the following, as appropriate:
a table with correct headings and appropriate units

a table with readings/observations entered correctly
a statement of results.
Readings or observations should be analysed/presented using the following, as appropriate:
a
a
a
a
a
a
a
table with suitable headings and units

table with ascending or descending independent variable
table showing appropriate computations
correct calculation
graph with independent and dependent variables plotted on horizontal axes respectively
graph with suitable scales and axes labelled with quantities and units
graph with data correctly plotted with a line or curve of best fit.
Discussion
In your discussion you should review your experimental results and draw appropriate conclusions.
You should also evaluate your experimental Procedures with some justification.
Conclusions should use evidence from the experiment and relate back to the aim of the experiment.
At least one of the following should be included:
the overall pattern to readings

the trends in analysed information or results
the connection between variables
an analysis of the observations
the findings from completed calculations.
Evaluation of the experimental Procedures should make reference to one of the following:
effectiveness of Procedures
control of variables
limitations of equipment
possible improvements
possible sources of error.
page 3
PA 1 - Preparation of Standard 0.1 mol l-1 Oxalic Acid Solution
Introduction
A primary standard is a reagent that is extremely pure, stable and has a high molecular weight .
Oxalic acid is a suitable primary standards for the titration of bases.
Oxalic acid:
(COOH)2 .2H2O - formula mass 126
For 250 cm3 of 0.1 mol l-1 oxalic acid solution, the mass required
=
126 x 0.1 x 0.25 = 3.15 g
Chemicals and Apparatus

Oxalic acid dihydrate (AR)
Balance (accurate to 0.01 g)
Specimen tube (or weighing bottle)
Beaker (250 cm3)
Standard flask (250 cm3)
Wash bottle/distilled water
Dropping pipette
Procedure
1.
Weigh accurately by difference pure oxalic acid dihydrate (about 3.15 g) into a clean, dry
250 cm3 beaker.
2.
Add about 50 cm3 distilled water, stir to dissolve and pour into a clean 250 cm3 standard
flask.
3.
Wash out the beaker using distilled water, adding all washings to the flask.
4.
Make up to the calibration mark with distilled water.
5.
Stopper the flask and shake well to mix.
Report
First mass of specimen tube + oxalic acid
= 26.09 g
Second mass of specimen tube + oxalic acid
= 22.91 g
Hence, the mass of oxalic acid used
= 3.18 g
i.e.
= 3.18
126
the number of moles present
Therefore the concentration of the solution
0.0252
0.25
= 0.0252
= 0.101 mol l-1
page 4
PA 2 - Standardisation of Approximately 0.1 mol l-1 Sodium Hydroxide Solution
Introduction
Solid sodium hydroxide, like pellets, is unsuitable for preparing a primary standard. It absorbs
moisture from the air. It also reacts with carbon dioxide forming sodium carbonate.
A secondary standard is a standard that is prepared in the laboratory for a specific analysis. It is
usually standardized against a primary standard. Oxalic acid can be used to standardise a sodium
hydroxide solution.
Equation for the reaction i.e.
2NaOH +
2 moles :
(COOH)2 . 2H2O (COONa)2 + 4H2O

1 mole

Standard oxalic acid solution (approximately 0.1 mol l-1)( from PA1)
Sodium hydroxide solution (approximately 0.1 mol l-1)
Phenolphthalein indicator
Pipette (20 or 25 cm3)
Conical flask (100 cm3)
Burette (50 cm3)
Procedure
1.
Pipette the sodium hydroxide solution (20 cm3) into a conical flask and add 2 or 3 drops of
phenolphthalein solution.
2.
Rinse and fill a burette with the oxalic acid solution, and note the reading on the scale.
3.
Add acid to the contents of the conical flask until the indicator just begins to change.
4.
Continue adding acid 1 cm at a time until the solution is permanently colourless, i.e., the
end-point has been reached. (Rough titre).
5.
Note the burette reading.
6.
Repeat several times, adding the acid dropwise as the end-point is approached.
Three readings should be obtained which agree within 0.1 cm3.
page 5
Report
First burette
reading/cm3
Second burette
reading/cm3
Difference/cm3
Trial
0.55
10.55
10.00
10.55
20.20
9.65
20.20
29.90
9.70
29.90
39.50
9.60
Average titre:
9.65
Number of moles of oxalic acid used
= 0.101 x 9.65 x 10-3

= 9.15 x 10-4
From the balanced equation

number of moles of sodium hydroxide reacting
= 9.75 x 10-4 x 2
= 1.95 x 10-3
Therefore, molarity of the sodium hydroxide
-3
= 1.95 x 10-3
20 x 10
= 0.098 mol l-1
page 6
PA 3 - Determination of Ethanoic Acid Content of Vinegar
Introduction
Vinegar is mainly composed of water and ethanoic acid. The concentration of ethanoic acid in
vinegar may be found by titrating a diluted solution of vinegar with standard sodium hydroxide
solution.
The equation for the reaction is NaOH + CH3 COOH CH3 COONa + H2O
i.e.
1 mole : 1 mole
This is a weak acid/strong base titration, and so phenolphthalein indicator is used. At the end-point,
the indicator changes colour from pink to colourless.

Vinegar
Standard flask (100 cm3)
Standard sodium hydroxide solution (approximately 0.1 mol l-1)(from PA2)
Phenolphthalein indicator
Balance (accurate to 0.01 g)
Pipette (20 or 25 cm3)
Burette (50 cm3)
Conical flask (100 cm3)
Wash bottle/distilled water
Dropping pipette
Procedure
1.
Weigh out accurately about 20 g of vinegar into a 100 cm3 standard flask.
2.
Make up to the calibration mark with distilled water and shake.
3.
Titrate 20 cm3 portions of this solution with standard 0.1 mol l-1 sodium hydroxide solution
(using phenolphthalein as indicator) until three concordant results are obtained (within 0.1
cm3).
page 7
Report
Why is the vinegar diluted?
Outline the correct procedure for bringing the solution in the volumetric flask precisely to the 100
cm3 mark.
Outline the procedure used in preparing the burette so that it is ready for the first titration.
Why is phenolphthalein used as the indicator in this titration?
Why is a rough titration carried out?
Why are three accurate titrations carried out?
Calculate the percentage (w/v) of ethanoic acid in the vinegar sample.
Sample calculation
Mass of vinegar used
= 19.98 g
Average titre for 20 cm3 of diluted vinegar
= 31.90 cm3
of 0.10 M NaOH
Number of moles of NaOH used
= 0.10 x 31.90 x 10-3

= 3.19 x 10-3
From the equation

Number of moles of CH3COOH in 20 cm3
= 3.19 x 10-3
Therefore, the number of moles in 100 cm3
= 3.19 x 10-3 x 5
= 1.595 x 10-2
i.e.
= 1.595 x 10-2 x 60
= 9.57 x 10-1g
the mass of CH3COOH present
(1 mole of CH3COOH weighs 60 g)
Therefore, the percentage of ethanoic acid present in vinegar

-1
= 9.57 x 10
19.98
100
1
= 4.8%
page 8
PA 4 - Preparation of Potassium Trioxaloferrate(III)
Introduction
Potassium trioxalatoferrate(III) contains the complex ion, [Fe(C2O4)3]3-, in which three oxalate ions
bind to an iron(III) ion in an octahedral arrangement. The oxalate ions behave as ligands.
Potassium trioxalatoferrate(III) can be prepared from ammonium iron(II) sulphate. A solution of the
latter is first treated with oxalic acid to form a precipitate of iron(II) oxalate and ammonium
hydrogensulfate solution. The iron(II) oxalate is isolated from the mixture and on reaction with
hydrogen peroxide and potassium oxalate, potassium trioxalatoferrate(III) and a precipitate of
iron(III) hydroxide are produced. On further treatment with oxalic acid, the iron(III) hydroxide
reacts to form more potassium trioxalatoferrate(III):
2Fe(OH)3 + 3H2C2O4 + 3K2C2O4 2K3[Fe(C2O4)3] + 6H2O
On cooling, crystals of hydrated potassium trioxalatoferrate(III), 2K3[Fe(C2O4)3].3H2O, separate
from the reaction mixture.

100cm3 glass beakers
balance (accurate to 0.01 g)
hot plate
glass stirring rod
25cm3 measuring cylinder
thermometer
dropper
glass filter funnel
filter papers
100cm3 crystallising basin
clock glass
hydrated ammonium iron(III) sulphate

oxalic acid solution
potassium oxalate solution
dilute sulphuric acid
'20 volume' hydrogen peroxide
deionised water
ethanol
COSSH
Wear eye protection and if any chemical splashes on your skin wash it off immediately.
Hydrated ammonium lron(II) sulphate may be harmful if ingested and may irritate the eyes. Wear
gloves.
Oxalic acid solution, potassium oxalate solution and the product, potassium trioxalatoferrate(III),
are all harmful by ingestion and are irritating to the eyes and skin. Wear gloves.
'20 volume' hydrogen peroxide is irritating to the eyes and skin. Wear gloves.
Ethanol is volatile, highly flammable, irritating to the eyes and intoxicating if inhaled or ingested.
Dilute sulphuric add is corrosive. Wear gloves.
page 9
Procedure
1.
Weigh a 100cm3 glass beaker and to it, add approximately 5g of hydrated ammonium
iron(II) sulphate, (NH4)2Fe(SO4)2.6H2O. Reweigh the beaker and its contents.
2.
Add approximately 15cm3 of deionised water and 1cm3 of dilute sulfuric acid to the
ammonium iron(II) sulphate. Warm the mixture to dissolve the solid.
3.
Once the ammonium iron(II) sulphate has dissolved, add 25cm3 of oxalic acid solution.
4.
Place the beaker on a hot plate and slowly heat the mixture with stirring until it boils.
5.
Remove the beaker from the heat and allow the precipitate of iron(II) oxalate to settle to
the bottom of the beaker.
6.
Decant off the liquid and add about 50cm3 of hot deionised water to the precipitate. Stir the
mixture and after the precipitate has settled once more, decant off the liquid.
7.
Add 10cm3 of potassium oxalate solution to the washed precipitate and heat the mixture to
about 40C.
8.
To this mixture, add slowly with Continuous stirring, 20cm3 of 20 volume hydrogen peroxide
solution. Keep the temperature close to 40C during the addition of the hydrogen peroxide.
9.
Heat the mixture nearly to boiling and add oxalic acid solution, dropwise with stirring, until
the brown precipitate of iron(III) hydroxide dissolves. Take care not to add too much oxalic
acid.
During the addition of the oxalic acid, keep the reaction mixture near to boiling.
10.
Filter the hot solution through a fluted filter paper into a crystallising basin.
11.
Add 25cm3 of ethanol to the filtrate and if any crystals form, redissolve them by gentle
heating.
12.
Cover the solution with a filter paper and set it aside in a dark cupboard for crystallisation to
take place.
13.
Filter off the crystals and wash them with a 1:1 mixture of ethanol and water.
14.
Weigh a clock glass and transfer the crystals to it. Cover the crystals with a filter paper and
leave them to dry at room temperature in a dark cupboard.
15.
Once dry, reweigh the crystals and clock glass.
16.
Calculate the percentage yield of hydrated potassium trioxalatoferrate(III)

K3[Fe(C2O4)3].3H2O.
page 10
Report
In your Report you may also wish to address the following points:
(a)
The 'Introduction' could include:
(b)
an explanation of how the oxalate ion can act as a ligand

a drawing of the trioxalatoferrate(III) ion to illustrate its shape
equations for the reactions involved in the preparation of potassium trioxalatoferrate(III).
In the 'Procedure' section you could include:
(c)
mention of the colour changes you observed in the preparation of potassium

trioxalatoferrate(III).
In the 'Discussion' section you could:
offer reasons for the fact that the yield of hydrated potassium trioxalatoferrate(III) is less
than 100%
explain the role that the hydrogen peroxide plays in the preparation of potassium
trioxalatoferrate(III).
page 11
PA5 - Colorimetric Determination of Manganese In Steel
Introduction
Colorimetry is an analytical technique used to determine the concentrations of coloured substances
in solution. It relies on the fact that a coloured substance absorbs light of a colour complementary
to its own and furthermore, the amount of light it absorbs (absorbance) is proportional to its
concentration.
Colorimetry is particularly suited to the determination of manganese in steel because the
manganese can be converted into permanganate ions which are coloured. The conversion is
achieved in two stages. Using nitric acid, the manganese is first oxidised to manganese(I1) ions
which are then oxidised to permanganate ions by the more powerful oxidising agent, potassium
periodate.

standard flasks (50 cm3 and 100 cm3)
50 cm3 burette
colorimeter
540 nm filter
optically matched cuvettes
balance (accurate to 0.001g)
glass beakers (50 cm3 and 250 cm3)
Bunsen burner, heating mat and tripod
measuring cylinders (50 cm3 and 10 cm3)
clock glass
filter funnel
tweezers
wash bottle
dropper
wire cutters
steel paper clips

0.0010 mol l-1 acidified potassium permanganate
2 mol l-1 nitric acid
85 % phosphoric acid
acidified potassium periodate solution
potassium persulfate
propanone
deionised water
anti-bumping granules
COSSH
The acidified 0.0010 mol l-1 potassium permanganate is harmful if ingested and irritates the eyes
and skin, Wear gloves.
Both 2 mol l-1 nitric acid and its vapour are corrosive and toxic causing severe burns to the eyes,
digestive and respiratory systems and in contact with the skin. Wear gloves.
85% phosphoric acid is corrosive; it burns and irritates the eyes and skin. A systemic irritant if
inhaled and if swallowed, causes serious internal injury. Wear gloves.
Acidified potassium periodate solution is harmful if swallowed and is an irritant to the eyes, skin and
respiratory system. It is also corrosive. Wear gloves.
Potassium persulfate is harmful if swallowed or inhaled as a dust. It irritates the eyes, skin and
respiratory system causing dermatitis and possible allergic reactions. Wear gloves.
Propanone is volatile and highly flammable and is harmful if swallowed. The vapour irritates the
eyes, skin and lungs and is narcotic in high concentrations. Wear gloves.
page 12
Procedure
Part A - Calibration graph
1.
Rinse the burette, including the tip, with 0.0010 mol l-1 acidified potassium permanganate
and fill it with the same solution.
2.
Run 2cm3 of the permanganate solution into a 50 cm3 standard flask and make up to the
graduation mark with deionised water. Use a dropper for the final centimetre.
3.
Stopper the flask and invert it several times to ensure the contents are completely mixed.
4.
Rinse a cuvette with some of this solution and fill it.
5.
Using the colorimeter (fitted with a 540nm filter) measure the absorbance of the solution in
the cuvette.
6.
Repeat steps two to five with 4, 6, 8, 10, 12 and 14 cm3 of the permanganate stock solution
in the burette.
7.
Plot a calibration graph of 'absorbance' against concentration of 'potassium permanganate.

Your teacher/lecturer will provide you with the accurate concentration of the potassium
permanganate stock solution.
Part B - Conversion of manganese to permanganate

Carry out the following Procedure in duplicate.
1.
Degrease a steel paper clip by swirling it with a little propanone in a small beaker. Using
tweezers, remove the paper clip and leave it to dry for about a minute or so on a paper
towel.
2.
Cut up the paper clip into small pieces.
3.
Weigh accurately about 0.2g of the paper clip pieces and transfer them to a 250cm3 glass
beaker.
4.
Add approximately 40 cm3 of 2 mol l-1 nitric acid to the beaker and cover it with a clock
glass.
5.
Heat the mixture cautiously, in a fume cupboard, until the reaction begins. Continue heating
gently to maintain the reaction, but remove the source of heat if it becomes too vigorous.
6.
Once the steel has dissolved, allow the solution Lo cool a little. Add a couple of antibumping granules and then boil the solution until no more brown fumes are given off.
7.
After the solution has cooled considerably - no more than 'hand hot' - add about 5 cm3 of
85% phosphoric acid, approximately O.2g of potassium persulfate and a couple of fresh
anti-bumping granules. Boil the mixture for about 5 minutes.
8.
To this solution, add approximately 15 cm3 of acidified potassium periodate solution plus a
couple of fresh anti-bumping granules and then gently boil the mixture. The solution should
start to turn pink. Continue gentle boiling until the intensity of the pink colour remains
page 13
constant. This should take about 5 minutes.

9.
Allow the pink solution to cool to room temperature and then transfer it to a 100 cm3
standard flask leaving the anti-bumping granules in the beaker.
10.
Rinse the beaker with a little deionised water and add the rinsings (but not the anti-bumping
granules) to the flask. Repeat this Procedure until you are within about a centimetre of the
graduation mark on the flask.
11.
Using a dropper, make up the solution to the graduation mark with deionised water.
12.
13.
Using a colorimeter fitted with a 540 nm filter, measure the absorbance of the solution.
14.
Use your calibration graph to convert the absorbance to a permanganate concentration and
then calculate the percentage by mass of manganese in the steel paper clip.
Report
(a)
(b)
an explanation of the technique of colorimetric analysis and its relevance in this experiment
equations for the oxidation reactions taking place in the conversion of manganese to
permanagante ions.
In the 'Discussion' section you could include comment on:
the reason for using a 520 nm filter in the colorimeter

the need to use optically matched cuvettes
the necessity of preparing a calibration graph
the need to wait until the intensity of the pink colour in the solution remains constant before
going on to measure its absorbance
the precision of the technique given that you have two estimates of the percentage
manganese in
page 14
PA 6 - Complexometric Determination of Nickel using EDTA
Introduction
Since ethylenediaminetetraacetic acid - commonly abbreviated to EDTA - forms stable complexes
with most metal ions, it is widely used to determine metals in what are known as complexometric
titrations. EDTA is a tetracarboxylic acid and can be represented as H4Y. In alkaline conditions,
EDTA exists as Y4- ions:
The Y4- ions form 1:1 complexes with metal ions. For example, Ni2+
ions bind with them to form the complex, NiY2- which has the
octahedral structure shown opposite.
2-
The end-point of an EDTA complexometric titration can be detected

by means of a metal ion indicator - an organic dye which changes
colour when it binds with metal ions. For it to be suitable in an EDTA
titration, the indicator must bind less strongly with metal ions than
does EDTA.

100 cm3 standard flask
250 cm3 conical flasks
20 cm3 pipette
50 cm3 burette
weighing bottle
25 cm3 measuring cylinder
pipette filler
filter funnel
white tile
wash bottle
glass stirring rod
dropper
hydrated nickel(II) sulfate

(NiSO4.6H2O)
0.10 mol l-1 EDTA solution
1 mol l-1 ammonium chloride
murexide indicator
0.88 aqueous ammonia
deionised water
COSSH
Hydrated nickel(II) sulfate is harmful by ingestion and inhalation, It irritates the eyes and skin.
Continued skin contact can cause dermatitis. Avoid raising a dust. Wear gloves.
EDTA is only toxic if ingested in large quantities.
0.85 aqueous ammonia is toxic if inhaled in high concentrations or if swallowed. The solution and
vapour irritate the eyes. The solution burns the skin and swallowing causes internal damage. Wear
goggles and gloves and handle in a fume cupboard.
1 mol l-1 ammonium chloride is harmful and irritates the eyes.
Murexide is harmful by ingestion and if inhaled as a dust. It may irritate the eyes.
Nickel(EDTA) complex - limited information is available on its toxicity. Its high stability and water
page 15
solubility will almost certainly give rise to low toxicity.
Procedure
Part A
1. Calculate the theoretical percentage by mass of nickel in NiSO4.6H2O.
Part B
1.
Transfer approximately 2.6 g of hydrated nickel(II) sulfate to a weighing bottle and weigh
the bottle and contents.
2.
Add about 25 cm3of deionised water to a 100 cm3 beaker and transfer the bulk of the nickel
salt to the water.
3.
Reweigh the bottle with any remaining salt.
4.
Stir the solution in the beaker until the solid has dissolved.
5.
Transfer the solution to a 100 cm3 standard flask.
6.
Rinse the beaker with a little deionised water and add the rinsings to the flask. Repeat this
Procedure until you are within about a centimetre of the graduation mark on the flask.
7.
8.
Stopper the flask and invert it several times to ensure the contents are thoroughly mixed.
9.
Rinse the burrette, including the tip, with 0.10 mol l-1 EDTA and fill it with the same solution
10.
Rinse the 20 cm3 pipette with a little of the nickel salt solution and pipette 20 cm3 of it into a
conical flask. Dilute the solution to about l00cm with deionised water.
11.
Add murexide indicator (approximately 0.05 g) to the diluted nickel salt solution together
with approximately 10 cm3 of ammonium chloride solution.
12.
Titrate the mixture with the EDTA solution and after the addition of about 15 cm3 of EDTA
make the solution alkaline by adding approximately 10 cm3 of 0.88 aqueous ammonia.
13.
Continue the titration to the end-point which is shown by the first appearance of a blueviolet colour. Detection of the end-point can be very difficult, so use this as a trial run. Keep
the titrated solution to help you detect the end-points in subsequent titrations.
14.
Repeat the titrations until two concordant results are obtained.
15.
Calculate the percentage by mass of nickel in your sample of hydrated nickel(II) sulfate
using the accurate concentration of the EDTA solution provided by your teacher/lecturer.
16.
For one of your determinations, calculate the percentage error and hence the absolute error
in the percentage of nickel in NiSO4.6H2O. Your teacher/lecturer will provide you with the
page 16
error in the concentration of the EDTA solution.
Report
(a)
(b)
an explanation of how EDTA can act as a ligand

an equation for the reaction between nickel(II) ions and Y' ions
the calculation of the theoretical percentage by mass of nickel in NiSO4.6H2O.
identify the major factors contributing to the error in the percentage of nickel in the salt
comment on whether the difference in your two estimates of the percentage nickel is
covered by the calculated experimental error
comment on the accuracy of the technique given that you have calculated the theoretical
percentage of nickel in NiSO4.6H2O
offer a reason for any difference between the experimental and theoretical values
give reasons why murexide is suitable as an indicator in a Ni2+/EDTA titration.
page 17
PA 7 - Gravimetric Determination of Water in Hydrated Barium Chloride
Introduction
Gravimetric analysis can be used to determine the number of moles of water molecules of
crystallisation per mole of hydrated barium chloride i.e. the value of n in BaCl2.nH2O. This can be
achieved by comparing the mass of a sample of the hydrated salt with the mass of the anhydrous
salt obtained on beating to constant mass.

silica or porcelain crucible and lid
tripod
pipe-clay triangle
Bunsen burner and heating mat
desiccator
tongs
hydrated barium chloride
COSSH
Wear eye protection and it any chemical splashes on your skin wash it off immediately.
Barium chloride is harmful by inhalation and by ingestion or skin contact. Wear gloves.
Hydrated barium chloride is crystalline, but the anhydrous salt that is produced is powdery. Avoid
raising a dust.
Procedure
1.
Place the empty crucible and lid on the pipe-clay triangle and heat them for about 10
minutes using a blue Bunsen flame. Heating should be gentle at first.
2.
Allow the crucible and lid to cool briefly before transferring them, using clean tongs, to the
desiccator.
3.
After cooling to room temperature, weigh the empty crucible and lid.
4.
Add 2-3 g of hydrated barium chloride to the crucible. Replace the lid and reweigh.
5.
Place the crucible back on the pipe-clay triangle with the lid partially covering the contents.
Heat gently for about 2 minutes and then strongly for 10- 15 minutes.
6.
Allow the crucible to cool briefly before transferring it to the desiccator.
7.
Reweigh the covered crucible and contents once they have cooled to room temperature.
8.
Heat the crucible and contents to constant mass i.e. reheat for about 4 minutes, cool in the
desiccator and reweigh until two successive readings are within 0.002 g of each other.
9.
Calculate the value of n in BaCl2.nH2O.
page 18
Report
(a)
(b)
an explanation of gravimetric analysis and its relevance in this experiment

an equation for the reaction taking place in the determination
an explanation of the meaning of the term 'heating to constant mass.
give the reason for using a blue flame rather than a yellow flame when heating the crucible
explain why the barium chloride had to be heated to 'constant mass
explain the need to wait until the crucible is cool before it is weighed
comment on the precision of the technique given that you have two estimates of n
comment on the accuracy of the technique given that the true value of n is integral
offer a reason for any difference in your value of n and the true value
comment on the accuracy of gravimetric analysis compared with volumetric analysis.
page 19
PA 8 - Determination of Nickel using Dimethylglyoxime
Introduction
Nickel(II) ions form a precipitate with dimethylglyoxime (butanedione dioxime) in the presence of a
slight excess of ammonia.
Ni2+ + 2 C4 H8O2N2 Ni (C4H7O2N2)2 + 2H+
Structural formulae (i)
Dimethylglyoxime
(ii) Nickel (II) dimethylglyoximate
An alcoholic solution of dimethyglyoxime (DMG) is used as the precipitating reagent during the
experiment because DMG is only slightly soluble in water (0.063 g in 100 ml at 25C).
The nickel dimethylglyoximate is a precipitate that is very bulky in character. Therefore, the sample
weight used in the analysis must be carefully controlled to allow more convenient handling of the
precipitate during transferral to the filtering crucible. A slow increase in the concentration of
ammonia in the solution causes the pH to rise slowly and results in the gradual precipitation of the
complex. The result is the formation of a more dense, easily handled precipitate.
Once the filtrate has been collected and dried, the nickel content of the solution is calculated
stoichiometrically from the weight of the precipitate.
page 20

Stirring rod with rubber 'policeman
Sintered-glass crucible (porosity 3)
Buchner flask and adapter
Filter pump
400 cm3 beaker
Steam bath
Desiccator
Measuring cylinders
0.1 mol l-1 dimethylglyoxime in ethanol
2 mol l-1 ammonia solution
AR nickel salt
Procedure
1.
Weigh accurately the nickel salt (about 0.4 g) and dissolve in distilled water (20 cm3) in a
400 cm3 beaker.
2.
Add 2 mol l-1 hydrochloric acid (20 cm3) and dilute with distilled water to about 200 cm3.
3.
Heat the solution to 70 - 80 C and add 0.1 mol l-1 dimethylglyoxime in ethanol (50 cm3); 5
cm3 for every 10 mg of Ni2+ is required, giving a slight excess.
4.
Add 2 mol l-1 ammonia solution dropwise, with constant stirring, until a permanent red
precipitate is obtained. Add a further 5 cm3 ammonia to provide a slight excess. The total
volume of ammonia should be approximately 30 cm3
5.
Heat on a steam bath for half an hour and when the precipitate has settled test the
supernatant liquid for complete precipitation by adding a few drops of the dimethylglyoxime
and ammonia solutions.
6.
Allow the precipitate to cool slowly to room temperature.
7.
Dry the sintered-glass crucible in an oven at 120 C, allow to cool and weigh.
8.
Set up the filtration apparatus and transfer the precipitate to the crucible as described in
experiment B2.
9.
Wash the precipitate with several portions of distilled water and dry in an oven at 120 C for
about one hour.
10.
Allow to cool in a desiccator and weigh.
11.
Repeat the drying to constant mass.
page 21
Report
(Salt used was NiCl2.6H2O)
First mass of weighing bottle + Ni2+ salt
= 12.9604 g
Second mass of weighing bottle + Ni2+ salt
= 12.5848 g
Mass of Ni2+ salt
= 0.3756 g
Mass of sintered-glass crucible
= 13.7733 g
Mass of sintered-glass crucible + precipitate
= 14.2283 g
Mass of Nickel(II) dimethylglyoximate
= 0.4550 g
Calculation
From the equation,
One mole of nickel ions gives one mole of Nickel(II) dimethylglyoximate
i.e.
58.7 g Ni
288.7 g Ni (C4H7O8N2)2
Mass of Ni2+ ions in precipitate
58.7
= 0.4550 x 288.7
= 0.0925 g
hence % of Ni2+ in original sample
0.0925
0.3756
x 100
= 24.6%
Theoretically, pure NiCl2.6H2O contains
58.7
237.7
x 100
= 24.7% Ni2+
page 22
PA 9 - Preparation of Cyclohexene
Introduction
Cyclohexene can be prepared by dehydrating cyclohexanol using concentrated phosphoric acid. The
product can be separated from the reaction mixture by distillation and after purification, it can be
weighed and the percentage yield calculated.

50 cm3 round-bottomed flasks
cork ring
condenser
still head
receiver adapter
thermometer adapter
thermometer
heating mantle
250 cm3 separating funnel
clamp stands and clamps
50 cm3 conical flask
test tube and rack
dropper
cyclohexanol
85 % phosphoric acid
saturated sodium chloride solution
anhydrous calcium chloride
bromine solution
COSSH
Cyclohexanol and its vapour are harmful to the eyes, lungs and skin and if swallowed. It irritates
and is absorbed through the skin. It is flammable and is a suspected carcinogen. Wear gloves.
85 % phosphoric acid is corrosive, it burns and irritates the skin and eyes. It is a systemic irritant if
inhaled and if swallowed, causes serious internal injury. Wear gloves
Anhydrous calcium chloride irritates the eyes, lungs and skin. Wear gloves.
Cyclohexene is highly flammable and its vapour is moderately toxic to the eyes, skin and respiratory
system. It is harmful if swallowed. Wear gloves. At the end of the experiment, dispose of the
cyclohexene since it may form unstable peroxides if it is stored.
Bromine solution causes burns and is toxic. Wear gloves. If any splashes on the skin, wash it off
with sodium thiosulfate solution.
Procedure
1.
Weigh a 50 cm3 round-bottomed flask supported on a cork ring. To the flask, add about 20g
of cyclohexanol and reweigh the flask and its contents.
2.
To the cyclohexanol, add dropwise with swirling approximately 8 cm3 85 % phosphoric acid.
3.
Add a few anti-bumping granules to the reaction mixture and set up the apparatus for
distillation. Gently heat the mixture for about 15 minutes - do not allow it to boil. Raise the
temperature and distil the mixture very slowly, collecting the liquid which comes over
between 70 and 90 C.
page 23
4.
Wash the distillation apparatus and leave it to dry.
5.
Pour the distillate into a separating funnel and add about an equal volume of saturated
sodium chloride solution. Stopper the funnel and shake the contents vigorously. (Sodium
chloride solution is used rather than water because it is more dense and will separate from
the cyclohexene more rapidly)
6.
Clamp the separating funnel and allow the two layers to separate.
7.
Remove the stopper from the funnel and run off the lower aqueous layer into a beaker and
dispose of it down the sink.
8.
Run the top layer (the crude alkene) into a small conical flask and add a few pieces of
anhydrous calcium chloride. Stopper the flask and shake the mixture for a few minutes until
the liquid is clear.
9.
Weigh a dry 50 cm3 round-bottomed flask in which to collect the pure cyclohexene.
10.
Decant the alkene into another dry 50 cm3 round-bottomed flask and add a few antibumping granules. Distil the alkene very slowly collecting the liquid which comes over
between 81 and 85 C in the preweighed flask.
11.
Weigh the flask and product.
12.
Carry out a test to show that the product is unsaturated.
13.
Calculate the percentage yield of cyclohexene.
Report
(a)
In the 'Introduction' you could include:
(b)
an equation (using structural formulae) for the dehydration of cyclohexanol.

The 'Procedure' section could include:
(c)
a labelled diagram of the assembled apparatus used for the initial distillation.
offer reasons for the fact that the yield of cyclohexene is less than 100%
explain why concentrated phosphoric acid was used to dehydrate the alcohol rather than
concentrated sulphuric acid
explain why distillation is a suitable technique in this case to separate the product from the
reaction mixture
explain the purpose of shaking the crude cyclohexene with saturated sodium chloride
solution
explain why anhydrous calcium chloride was added to the cyclohexene.
page 24
PA 10 - Identification by Derivative Formation
Introduction
Even if the homologous series to which an organic liquid belongs has been established, it can still
be difficult to identify the liquid from its boiling point. To overcome this problem, the liquid can be
converted into a solid derivative. By comparing the melting point of the derivative with those of
known derivatives, it is then possible to identify the organic liquid.
In this experiment, an unknown ketone is converted into a derivative by condensing it with
2,4-dinitrophenythydrazine:
The derivative, known as a 2,4-dinitrophenylhydrazone, is purified by recrystallisation before its

melting point is determined.

test tube and rack
stopper to fit test tube
dropper
Hirsch funnel and flask
glass filter funnel
hot plate
filter papers
oven
capillary tube
thermometer
melting point apparatus
water pump
watch glass
unknown ketone
Bradys reagent (2,4-dinilrophenylhydrazine
solution)
ethanol
anti-humping granules
COSSH
The ketone used is volatile and highly flammable and is harmful if swallowed. The vapour irritates
the eyes, skin and lungs and is narcotic in high concentrations. Wear gloves.
Bradys reagent contains 2,4-dinitrophenylhydrazine which is toxic by ingestion and by skin
absorption. Bradys reagent also contains methanol which is volatile and highly flammable. It is
toxic by ingestion, inhalation and by skin absorption. High concentrations may damage the cerebral
nervous system and impair vision. Bradys reagent also contains sulfuric add which is irritating to
page 25
the eyes and Skin. Wear gloves.

No information is available on the toxicity of the ketone-2,4-dinitrophenylhydrazone but analogy
would suggest that its toxicity is similar to that of 2,4-dinitrophenylhydrazine itself. It should be
handled in the same way as Bradys reagent.
Procedure
1.
Add about 10 cm3 of 2,4-dinitrophenylhydrazine solution to the test tube followed by

approximately 10 drops of the unknown ketone. Stopper the test tube and invert it several
times to ensure complete mixing.
2.
Set up the Hirsch funnel and flask for filtration and connect the side arm of the flask to the
water pump. Place a small filter paper in the funnel and wet it with a few drops of ethanol.
Turn on the water tap and the suction from the pump will ensure that the filter paper
adheres firmly to the perforated bed of the funnel.
3.
Filter off the precipitate at the water pump.
4.
Transfer the precipitate to a conical flask and add a small volume of the solvent, ethanol
(about 10 cm3).
5.
Add a few anti-bumping granules to the mixture and heat it gently on the hot plate until the
precipitate dissolves. Do not boil the solution. If noticeable amounts of solid remain, add a
little more ethanol.
6.
Filter the warm solution into a conical flask through a pre-heated fluted filter paper and
funnel.
7.
Set aside the conical flask until the solution has cooled to room temperature and
crystallisation has occurred.
8.
Using the Hirsch funnel and flask, filter the crystals at the water pump using the filtrate to
wash out and remove the remaining crystals from the flask.
9.
Wash the crystals with a little ethanol and transfer them to a watch glass. Dry the crystals in
an oven at a temperature of about 50 - 60 C.
10.
Using the melting point apparatus, determine the melting point of the crystals. To get an
accurate value of the melting point it is Important to raise the temperature very slowly about 2 C per minute.
11.
Compare the melting point with those in the following table and hence identify the ketone.
Ketone
Ketone
m.p. of 2,4-dnp *
derivative / C
propanone
128
pentan-3-one
156
butanone
115
hexan-2-one
107
pentan-2-one
141
cyclohexanone
162
page 26
* 2,4-dnp represents 2,4-dinitrophenylhtdrazinde
Report
(a)
(b)
an explanation of why it is difficult to identify an organic liquid from its boiling point even
when the homologous series is known
an equation (using structural formulae) for the condensation reaction between a ketone and
2,4-dinitrophenylhydrazine
an explanation of how a compound is purified by the process of recrystallisation.
comment on the purity of your sample of the 2,4-dinitrophenylhydrazone

explain why the warm solution of the 2,4-dinitrophenylhydra2one was filtered through a hot
rather than a cold filter paper and funnel
explain whether a rapid rise in temperature in the melting point apparatus would lead to an
overestimation or underestimation of the melting point of the sample.
page 27
PA 11 - Preparation of Benzoic Acid by Hydrolysis of Ethyl Benzoate -
Introduction
Benzoic acid can be prepared by the alkaline hydrolysis of the ester, ethyl benzoate:
If sodium hydroxide is used, then the residual solution will contain sodium benzoate. Insoluble
benzoic acid can be displaced from this solution by acidification. It can then be filtered off and
purified by recrystallisation from water. The percentage yield of benzoic acid can be calculated and
its melting point determined.

100cm3 round-bottomed flask
cork ring
condenser
heating mantle
Buchner funnel and flask
100cm3 measuring cylinder
glass filter funnel
capillary tube
thermometer
water pump
oven
hot plate
filter papers
250 cm3 glass beakers
clock glass
glass stirring rod
dropper
ethyl benzoate
2 mol l-1 sodium hydroxide
5 mol l-1 hydrochloric acid
blue litmus paper or pH paper
deionised water
COSSH
Wear eye protection and if any chemical splashes on your skin wash t off immediately.
Ethyl benzoate is of low volatility and flammability. It irritates the eyes and is harmful if ingested in
quantity.
2mol l-1 sodium hydroxide is corrosive to the eyes and skin. Gloves and goggles should be worn.
5 mol l-1 hydrochloric acid is irritating to the eyes, lungs and skin and if swallowed. Wear gloves
The product, benzoic acid is of low volatility and flammability. It may be harmful if ingested an
quantity.
Only a small amount of ethanol is produced in the reaction. it is volatile, highly flammable, irritating
to the eyes and intoxicating if inhaled or ingested.
page 28
Procedure
1.
Weigh the 100 cm3 round-bottomed flask supported on a cork ring. To the flask, add about
5 g of ethyl benzoate and reweigh the flask and its contents.
2.
To the ethyl benzoate, add approximately 50 cm3 of 2 mol l-1sodium hydroxide and a few
anti-bumping granules.
3.
Set up the apparatus for heating under reflux. Using a heating mantle, reflux the reaction
mixture until all oily drops of the ester have disappeared. This may take 45-60 minutes.
4.
Allow the apparatus to cool and then transfer the reaction mixture to a 250 cm3 beaker.
5.
Slowly and with stirring, add 5 mol l-1 hydrochloric acid to the reaction mixture to precipitate
out the benzoic acid. Continue adding the acid until no more precipitation takes place and
the mixture turns acidic - test with blue litmus paper or pH paper. (About 30 cm3 of acid will
be required)
6.
Allow the mixture to cool to room temperature and filter off the precipitate at the water
pump and wash the crude benzoic acid with a small volume of water.
7.
Transfer the crude benzoic acid to a 250 cm3 beaker and recrystallise it from about 100 cm3
of water.
8.
Filter off the crystals of benzoic acid at the water pump and wash them with a small volume
of water. Allow air to be drawn through the crystals for a few minutes in order to partially
dry them.
9.
Weigh a clock glass and transfer the crystals to it. Dry the crystals in an oven at about 70 C
and then reweigh the clock glass and crystals.
10.
Determine the melting point of the benzoic acid.
11.
Calculate the percentage yield of benzoic acid.
page 29
Report
(a)
(b)
equations (using structural formulae) for the alkaline hydrolysis of ethyl benzoate and the
displacement of benzoic acid from the sodium benzoate solution.
The 'Procedure' section could include:
(c)
labelled diagram of the assembled apparatus used in hydrolysing the ester.

offer reasons for the fact that the yield of benzoic acid is less than 100%
explain how the yield of benzoic acid would have been affected had the hydrolysis of ethyl
benzoate been catalysed by hydrochloric acid rather than sodium hydroxide
comment on the purity of your sample of benzoic acid given that the accepted value for its
melting point is 121 C.
page 30
PA 12 - Preparation of Aspirin
Introduction
Aspirin is an analgesic (pain-killing), anti-inflammatory and anti-pyretic (fever-reducing) drug. It is
an ester and can be prepared by the condensation reaction between 2-hydroxybenzoic acid (or
salicylic acid) and ethanoic anhydride:
2-hydroxybenzoic acid
ethanoic anhydride
After purification by recrystallisation, the product can be weighed and the percentage yield
determined. The purity of the final sample can be checked by determining us melting point.

50 cm3 conical flask
measuring cylinders (10 cm3, 50 cm3)
250 cm3 glass beakers
thermometers
dropper
hot plate
glass stirring rod
Buchner funnel and flask
water pump
filter papers
clock glass
oven
capillary tube
2-hydroxybcnzoic acid
ethanoic anhydride
85% phosphoric acid
ethanol
anti - bumping granules
deionised water
ice
COSSH
2-hydroxybenzoic acid is harmful by ingestion, causing nausea, vomiting, etc. It is also a severe
skin and eye irritant. Wear gloves.
Ethanoic anhydride is corrosive. The liquid irritates and burns the eyes and skin severely while
the vapour irritates the respiratory system and may cause bronchial and lung injury. lt is also
flammable. Wear gloves and handle in a fume cupboard.
85% phosphoric acid is corrosive: it burns and irritates the skin and eyes. lt is a systemic irritant
if inhaled and if swallowed, causes serious internal injury. Wear gloves.
page 31
Procedure
1.
Weigh a 50 cm3 conical flask and to it, add about 5 g of 2-hydroxybenzoic acid. Reweigh the
flask and its contents.
2.
In a fume cupboard, add 10 cm3 of ethanoic anhydride from a measuring cylinder, to the
2-hydroxybenzoic acid. During the addition, swirl the contents of the flask to ensure
thorough mixing.
3.
Add 5 drops of phosphoric acid to the mixture, again with swirling.
4.
Place the flask on a hot plate (in the fume cupboard) and heat the mixture to about 85 C.
Hold it at this temperature for about 10 minutes and constantly stir the mixture.
5.
Cool the mixture in an ice/water bath and then pour it into approximately 150 cm3 of cold
water contained in a 250 cm3 beaker.
6.
Filter off the precipitate at the water pump and wash it thoroughly with several portions of
cold water.
7.
Transfer the crude product to about 15 cm3 of ethanol in a 100 cm3 conical flask. Add a
couple of anti-bumping granules and heat the mixture gently on a hot plate until the solid
dissolves.
8.
Pour this solution into a 100 cm3 conical flask containing about 40 cm3 of water. If an oil
forms re-heat the mixture on the hot plate to dissolve it. If the oil still persists, add a few
drops of ethanol and re-heat the mixture.
9.
Set aside the mixture and allow it to cool to room temperature.
10.
Filter off the crystals of aspirin at the water pump and wash them with a small volume of
cold water. Allow air to be drawn through the crystals for a few minutes in order to partially
dry them.
11.
Weigh a clock glass and transfer the crystals to it. Dry the crystals in an oven at about 100
C and then reweigh the clock glass and crystals.
12.
Determine the melting point of the aspirin.
13.
Calculate the percentage yield of aspirin.
page 32
Report
(a)
(b)
an equation (using structural formulae) for the condensation reaction between 2hydroxybenzoic acid and ethanoic anhydride.
suggest why ethanoic anhydride is used rather than ethanoic acid in the preparation of
aspirin
offer reasons for the fact that the yield of aspirin is less than 100%
comment on the purity of your sample of aspirin given that the accepted value for its
melting point is 137 C.
page 33
PA 13 - Aspirin Determination
Aspirin has the following structural formula:
Since it is insoluble in water, aspirin has to be determined by a 'back titration' technique. This
involves treating a sample of accurately known mass with a definite amount of sodium hydroxide
i.e. the volume and concentration of the alkali must be accurately known. The alkali first catalyses
the hydrolysis of the aspirin to ethanoic and salicylic acids and then neutralises these acids. An
excess of alkali has to be used and the amount remaining after reaction is determined by titrating it
against a standard solution of sulphuric acid.

250 cm3 standard flasks
conical flasks (100 cm3 and 250 cm3)
25 cm3 pipette
50 cm3 burette
weighing bottle
hot plate (or Bunsen burner and tripod)
pipette filler
filter funnel
white tile
wash bottle
dropper
aspirin tablets
0.050 mol l-1 sulphuric acid
1.0 mol l-1 sodium hydroxide
phenolphthalein
deionised water
COSSH
0.050 mol l-1 sulphuric acid irritates the eyes and skin.
1.0 mol l-1 sodium hydroxide is corrosive to the eyes and skin. Gloves and goggles should be
worn.
Phenolphthalein indicator solution is highly flammable and irritating to the eyes because of its
ethanol content.
page 34
Procedure
1.
Add a definite number of aspirin tablets (about 1.5 g in mass) to the weighing bottle and
weigh the bottle and contents.
2.
Transfer the tablets to a large conical flask and reweigh the weighing bottle.
3.
Rinse the 25 cm3 pipette with 1.0 mol mol l-1 sodium hydroxide and pipette 25 cm3of this
solution into the flask containing the tablets.
4.
To the mixture in the flask, add approximately 25 cm3 of deionised water.
5.
Place the flask on the hotplate and simmer the mixture very gently for about 30 minutes.
6.
Allow the reaction mixture to cool before transferring it to the 250 cm3 standard flask.
7.
Rinse the comical flask with a little deionised water and add the rinsings to the standard
flask. Repeat this Procedure until you are within about a centimetre of the graduation mark
on the flask.
8.
9.
10.
Rinse the burette, including the tip, with 0.050 mol l-1 sulphuric acid and fill it with the same
solution.
11.
Rinse the 25 cm3 pipette with the 'standard flask' solution and pipette 25 cm3 of it into a 100
cm3 conical flask.
12.
Add a few drops of phenolphthalein indicator to the solution in the conical flask and titrate
to the end-point.
13.
Repeat the titrations until two concordant results are obtained.
14.
Calculate the mass of aspirin per tablet using the accurate concentrations of the sulphuric
acid and sodium hydroxide solutions provided by your teacher/lecturer.
15.
For one of your determinations, calculate the percentage error and hence the absolute error
in the mass of aspirin per tablet. Your teacher/lecturer will provide you with the errors in the
concentrations of the sulphuric acid and sodium hydroxide solutions.
page 35
Report
(a)
(b)
an explanation of the 'back titration' technique and its relevance in this experiment
equations for the reactions taking place in the determination.
identify the major factors contributing to the error in the mass of aspirin per tablet
comment on whether the difference in your two estimates of the mass of aspirin per tablet
is covered by the calculated experimental error
comment on how your result compares with the manufacture's specification and offer a
reason for any difference
explain why phenolphthalein is a suitable indicator for the titration (phenolphthalein has a
pH range of 8.3 - 10.0)
explain why only a few drops of phenolphthalein indicator are used in the titration
(phenolphthalein is a weak acid).
page 36
PA 14 - Thin-layer Chromatography of Aspirin
Introduction
You have probably used a simple chromatography experiment as part of your earlier studies to
separate the dyes in a coloured ink. The same technique can be used to separate substances which
are not dyes but in such experiments the chromatogram must be developed to show up the various
different substances that have been separated.
Chromatography techniques are used a great deal in industry because they can be controlled very
precisely and use very small amounts of substance. In this activity you investigate the purity and
identity of your laboratory prepared aspirin samples using thin-layer chromatography (tlc). In this
activity all the substances are white or colourless so you will need to develop the plate before you
can see what has happened.
Thin-layer chromatography is a powerful tool for determining if two compounds are identical. A spot
of the compound being investigated is placed on a chromatography plate, and a spot of a pure
manufactured sample of the same substance is placed next to it. The plate is then allowed to stand
in a suitable solvent, which travels up the plate. If the compound to be identified leaves exactly the
same pattern on the chromatography plate as the known pure compound it is reasonable to
conclude that they are the same. However, if extra spots are observed as well as the characteristic
pattern of the known compound, then impurities are likely to be present in the sample.
In this experiment both crude and recrystallised samples of aspirin are compared with
a known sample of aspirin.

Aspirin samples from PA 13
Commercial aspirin
Ethanol
Dichloromethane
Ethyl ethanoate
Thin layer chromatography plates
Chromatography tank
Capillary tubes
Spatula
Test tubes
UV lamp
COSSH
Dichloromethane is harmful by inhalation. Avoid breathing vapour and avoid contact with skin
and eyes.
Ethanol is flammable.
Ethyl ethanoate is volatile, highly flammable and the vapour may irritate the eyes and respiratory
system. Avoid breathing the vapour and avoid contact with the eyes. Keep away from flames.
Iodine
Short wave UV may cause skin cancer and eye damage. Do not observe directly. The viewer
should be screened from direct radiation.
page 37
page 38
Procedure
1.
Make sure that you do not touch the surface of the tlc plate with your fingers during this
activity. Handle the plate only by the edges and use tweezers if possible.
2.
Take a tlc plate and using a pencil (not a biro or felt tip pen) lightly draw a line across the
plate about 1 cm from the bottom. Mark three equally spaced points on this line.
3.
Place small amounts (about 1/3 of a spatula measure) of your crude aspirin, your
recrystallised aspirin and the commercial sample of aspirin in three separate testtubes.
Label the test-tubes so that you know which is which.
4.
Make up 5 cm3 of solvent by mixing equal volumes of ethanol and dichloromethane in a

test-tube. Add 1 cm3 of the solvent to each of the test-tubes to dissolve the samples. If
possible do this in a fume cupboard.
5.
Use capillary tubes to spot each of your three samples onto the tlc plate. Allow the spots to
dry and then repeat three more times. The spots should be about 12 mm in diameter.
6.
After all the spots are dry, place the tlc plate in the developing tank making sure that the
original pencil line is above the level of the developing solvent ethyl ethanoate. Put a lid
on the tank and allow to stand in a fume cupboard until the solvent front has risen to within
a few millimetres of the top of the plate.
7.
Remove the plate from the tank and quickly mark the position of the solvent front.
Solvent level
Rf value = a/b
a
Position for
initial spots
1 cm
Allow the plate to dry.
page 39
8.
Observe the plate under a short wavelength UV lamp and lightly mark with a pencil any
spots observed.
9.
Carefully place the plate in a jar or beaker containing a few iodine crystals. Put a cover on
the jar and warm gently on a steam bath until spots begin to appear. Do this in a fume
cupboard if possible.
Report
1.
Draw a diagram to show which spots appeared under UV light and which appear with iodine.
2.
Determine the Rf value of the samples using the expression

Rf = distance moved by sample/distance moved by solvent
3.
Write a short paragraph explaining why some substances move further up the tlc plate than
others and how the results are made visible.
4.
What conclusions can you draw about the nature of the three samples tested?
page 40

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CFE Advanced Higher Chemistry

Preparation of Standard 0.1 mol l-1 Oxalic Acid Solution

Standardisation of Approximately 0.1 mol l-1 Sodium Hydroxide Solution

Determination of Ethanoic Acid Content of Vinegar

Preparation of Potassium Trioxalatoferrate (III)

Colorimetric Determination of Manganese in Steel

Complexometric Determination of Nickel using EDTA

Gravimetric Determination of Water in Hydrated

Determination of Nickel using Dimethylglyoxime

Identification by Derivative Formation

Preparation of Benzoic Acid by hydrolysis of Ethyl

Thin-layer Chromatography of Aspirin

Writing a Report on an experiment n Chemistry

labelled diagram or description of the apparatus, instruments used

a table with correct headings and appropriate units

Readings or observations should be analysed/presented using the following, as appropriate:

table with suitable headings and units

the overall pattern to readings

PA 1 - Preparation of Standard 0.1 mol l-1 Oxalic Acid Solution

(COOH)2 .2H2O - formula mass 126

126 x 0.1 x 0.25 = 3.15 g

Chemicals and Apparatus

Make up to the calibration mark with distilled water.

Stopper the flask and shake well to mix.

Second mass of specimen tube + oxalic acid

Hence, the mass of oxalic acid used

the number of moles present

Therefore the concentration of the solution

PA 2 - Standardisation of Approximately 0.1 mol l-1 Sodium Hydroxide Solution

(COOH)2 . 2H2O (COONa)2 + 4H2O

Chemicals and Apparatus

Note the burette reading.

Number of moles of oxalic acid used

= 0.101 x 9.65 x 10-3

From the balanced equation

Therefore, molarity of the sodium hydroxide

= 0.098 mol l-1

PA 3 - Determination of Ethanoic Acid Content of Vinegar

Chemicals and Apparatus

Make up to the calibration mark with distilled water and shake.

Average titre for 20 cm3 of diluted vinegar

Number of moles of NaOH used

= 0.10 x 31.90 x 10-3

From the equation

Therefore, the number of moles in 100 cm3

the mass of CH3COOH present

(1 mole of CH3COOH weighs 60 g)

Therefore, the percentage of ethanoic acid present in vinegar

PA 4 - Preparation of Potassium Trioxaloferrate(III)

Chemicals and Apparatus

hydrated ammonium iron(III) sulphate

Once dry, reweigh the crystals and clock glass.

Calculate the percentage yield of hydrated potassium trioxalatoferrate(III)

The 'Introduction' could include:

an explanation of how the oxalate ion can act as a ligand

mention of the colour changes you observed in the preparation of potassium

PA5 - Colorimetric Determination of Manganese In Steel

Chemicals and Apparatus