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1. No unnecessary titrations. If you have done two that are close enough,
that's already sufficient. Remember close enough means two titres within
o.10 cm^3. Example 21.50 and 21.60 is fine, 22.75 and 22.80 is fine but
23.25 and 23.40 is not enough. In such cases, perform another titration.
Graphs
1. The scale needs your values to cover at least half of the page, mind it.
2. Sharp your pencil, use 2H pencil(not HB) for graphs if available. You can
get in a good stationary shop.
3. Double check before plotting, but be real quick. One mistake in plotting
and you may mess with the whole graph.
4. Line of best fit doesn't strictly mean line only, sometimes(rarely) it could
be a curve too.
5. Always draw a triangle for gradient. The bigger the traingle, the more
accurate is your gradient.
6. Ask me now if you don't know ideas about gradient and y-intercept clearly.
7. Always write by the axis, what it represents along with its unit.
9. LABELLING!!!
11. Even if graph is wrong, you won't lose *dherai* marks, just don't lose
hopes and work out on gradient and intercept stuffs, you will get method
markings. But never leave the questions, just fill the space even if you go
blank.
12. When they ask you to prove some relationship like T=kV or T is directly
proportional to V, write that since the graph is a straight line, the value of the
K is constant and therefore the relationship is true. DON'T FORGET IT!!!
13. If you don't have enough time, don't make all points. Make two or three
points and work out on other stuffs... Believe me, it helps if you are running
out of time.
1. There is a trick with aluminium and lead(II) ions. Both of them give same
observation with ammonia and sodium hydroxide. To distinguish them, you
need to add HCl . If precipitate forms, it is because of lead(II) ions, otherwise
it is aluminium ions. Lead chloride is insoluble.
Gas test
Example, when ZnCO3 is reacted with HCl, you know that a gas is released.
What could that be? Just think...it is CO2...Now what you need to write is
something like this(already given in the booklet) -"Colorless gas which turns
lime water milky"
Already given in the booklet, but remember NO2 is brown in color and to my
knowledge, it is very difficult to observe it. Common sense helps a lot.
Otherwise use a white paper or tile as background while observing.
3. If you are not familiar with the smells of gases, you can confuse colorless
gases which smell differently. H2S, for example, smells like rotten eggs while
SO2 smells like the smoke just after you burn a match.
General Tips
1. Read carefully the names of all solutions..otherwise you will have to suffer.
Sometimes you might have to start from the beginning, it will kill your
confidence as well as time. Unlike physics practical, you need to be very
fast...It is very unlikely to happen that you will finish before time.
2. Don't spend time washing burettes and all...do it real quick!!! Like 1
burette washing in 10 seconds.
3. If you think some solutions have been mixed or there is impurity or even if
your intuition says daal mey kuch kaaala hey, then ask them to replace it!
They will not scold you like Minnu mam.
5. If strong heating is directed, you should STRONG heat it, not just
warming...don't just write the observation fast.
6. Some examiners might be strict, they may not provide you chemicals
again until empty. Be careful in spending.
Error in any instrument is half of the smallest unit you can read on it. For
instance, the stopwatch we had in the lab had the smallest unit as a 0.01s so
the error in the readings read would be +/- 0.005s.
Now you can find the uncertainty using the following formula, it might give
you an understanding why it depends on the size of the value you measure.
= [0.005/50]*100
= 0.01 percent.
But it is much more complex due to human reaction time in stopwatchs. They
won't ask you, hopefully. :)
7. Lastly, even if the practical goes horrible(like with me), don't get your
hopes down. You can easily manage to get 'a' if you work good on P1 and P2.
I've seen students with 'U' on P3, still they managed to get overall 'a'. :)
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Chemistry Unit 3B notes
Tests of ions:
Test 1
Heat solid nitrate.
Oxygen gas is evolved
If group 1 solid (not Li) then will
that will relight a
decompose to give the nitrite and
Nitrate NO3- glowing splint.
oxygen.
Brown gas is seen
All other solid nitrates decompose to
(NO2). Oxygen gas is
give the metal oxide, nitrogen dioxide
also evolved and will
and oxygen.
relight a glowing
splint.
Test 2
Boil nitrate solution with Litmus paper turns
aluminium/Devarda’s alloy, in sodium blue in the presence
hydroxide solution. of ammonia.
Test vapour with red litmus paper.
Test NH
Warm ammonium compound with 3
Ammonium NH4+
NaOH. turns the litmus
Test vapours immediately using damp paper blue.
red litmus paper.
Test
Dip nichrome wire in HCl.
Tests of gases:
Volumetric analysis:
Volumetric analysis (titration) involves the reaction between two solutions. For one solution,
both the volume and the concentration are known; for the other, the volume only is known.
Apparatus used includes a burette, a pipette and a volumetric flask.
A solution for which concentration is accurately known. The concentration may have been
found by a previous titration or by weighing the solute and making a solution of known volume.
Such a solution is a primary standard solution.
How is a 250cm3 standard solution prepared?
Make sure that the balance is clean and dry. Wipe it with a damp cloth.
Place the weighing bottle on the pan and take the balance (i.e. re-zero it)
Take the bottle off the balance and add solid to it. This ensures that no spillages fall on
the pan.
Take the balance of the weighing bottle + solid and find the balance of solid by
subtraction.
Replace on balance, and if the required amount is added, withdraw the mass.
When you have the required amount, write its value down immediately.
Wash out a 250cm3 volumetric flask three times using pure water.
Transfer the solid to a 250cm3 volumetric flask using a funnel, and wash out the
weighing bottle into the flask through the funnel using distilled water.
Add about 100cm3 of distilled water to the flask.
Stir the solution using a glass rod until all the solid visibly dissolves into a solution.
Wash all remaining apparatus including the glass rod, funnel and transfer the rest of this
to the flask.
Make up to 250cm3 with distilled water so that the bottom of the meniscus just touches
the 250cm3 mark.
Attach a stopper to the flask.
Shake the flask vigorously and/or invert the flask 5 or 6 times to create a solution with
uniform concentration.
Concentration of solution = mass of solid used/molar mass of solid x 1000/250 (units
moldm-3)
A glass bulb pipette will deliver the volume stated on it within acceptable limits only.
Using a pipette filler, draw a little of the solution to be used into the pipette and use this
to rinse the pipette.
Fill the pipette to about 2-3cm3 above the mark. Pipette fillers are difficult to adjust
accurately, so quickly remove the filler and close the pipette with your forefinger (not
thumb). Release the solution until the bottom of the meniscus is on the mark.
Immediately transfer the pipette to the conical flask in which you will do the titration,
and allow the solution to dispense under gravity.
Using the burette:
Making sure that the tap is shut, add about 10-15cm3 of the appropriate solution to the
burette and rinse it out, not forgetting to open the tap and rinse the jet.
Close the tap and fill the burette. A small funnel should be used to add the solution but
be careful not to overfill the funnel.
Remove the funnel, because titrating with a funnel in the burette can lead to serious
error if a drop of liquid in the funnel stem falls into the burette during the titration.
Bring the meniscus on to the scale by opening the tap to allow solution to pass through
the burette. There is no particular reason to bring the meniscus exactly to the zero
mark.
Make sure that the burette is full to the tip of the jet.
After a suitable indicator has been added to the solution in the conical flask, swirl the
flask under the burette with one hand whilst adjusting the burette tap with your other
hand.
Add the solution in the burette to the conical flask slowly, swirling the flask all the time.
As the endpoint is approached, the indicator will change colour more slowly. The titrant
should be added drop by drop near to the endpoint.
Repeat the titration until you have three concordant titres, i.e. volumes that are similar.
This means within 0.2cm3 or better if you have been careful. Taking the mean of three
tires that differ by 1cm3 or more is no guarantee of an accurate answer.
Common indicators:
Methyl orange - yellow in alkali, red in acid & orange in neutral solutions(usually the end
point of a titration)
Phenolphthalein - pink in alkali, colourless in acid.
Weigh a spirit lamp (containing a liquid alcohol) using a balance accurate to 3 decimal
places. Record the mass measured.
Use a measuring cylinder to put 100 cm3 of distilled water into a small beaker and
clamps this at a fixed height above the spirit lamp (about 2 cm).
Record the initial temperature of the water using a thermometer.
Light the lamp using a burning splint.
Heat the water using the spirit lamp until the temperature has gone up by about 10C.
Stir the water with the thermometer the whole time.
Put a cap on the spirit to stop the alcohol burning. The lid stops also stops further
evaporation of the liquid alcohol.
Reweigh the spirit lamp and record the mass.
Calculate the enthalpy change.
Possible sources of error:
There may be heat loss due to the apparatus used and heat may have dissipated
through the insulating material --> should use a polystyrene cup and insulation like a lid.
The specific heat capacity and density of water are used (and not of HCl).
The masses of solid added to the acid are ignored.
It is assumed that the specific heat capacity of the polystyrene cup is negligible.
Some heat is lost when the hydrogen or carbon dioxide are evolved in the reactions.
Organic Procedures:
Heating under reflux - This allows reactions to occur slowly, over a long period of time, without
any loss of volatile liquid. The solvent evaporates and is condensed and returns to the flask.
To achieve this without loss of liquid, reaction mixtures are heated in a flask carrying a
vertical condenser.
This is heating under reflux; the solvent is condensed and returned to the flask, so the
mixture can be heated as long as desired.
To heat the round bottomed flask, either use a water bath, an oil bath or a heated plate
mantle. A Bunsen burner isn’t really suitable.
Simple distillation:
Re-crystallisation method:
1. Dissolve the solid in the minimum amount of boiling solvent. This ensures that the
solution is saturated with respect to the main solute but not with respect to the
impurities, which are present in much smaller amounts.
2. Filter the hot mixture through a preheated filter funnel. This removes insoluble
impurities. The hot funnel is necessary to prevent the solute crystallising and blocking
the funnel. Filtration under vacuum using a Buchner funnel is often preferred, because it
is fast.
3. Cool the hot filtrate, either to room temperature or, if necessary, in a bath of iced
water. Rapid cooling gives small crystals, slow cooling large ones. The large crystals are
often less pure.
4. Filter the cold mixture using a Buchner funnel.
5. Wash the crystals with a small amount of cold solvent. This removes any impurity
remaining on the surface of the crystals. A small amount of cold solvent is used so that
the crystals aren’t washed away / don’t dissolve.
6. Suck the crystals as dry as possible on the filter.
7. Transfer the crystals to a desiccator to dry. Drying between filter paper is sometimes
recommended, but it is a very poor method.
This is used to determine the purity of the re-crystallisation solid. Place small amount of the
solid in the sealed end of a capillary tube. Place in the melting point apparatus. A sharp melting
point over a small range shows purity, when compared with the set-book value of a higher
melting point, that indicates an impure solid.
Organic tests:
Sulphate solubility:
Hydroxide solubility:
Alkane: Burn /oxidise/combust them. They will burn with a yellow flame and form CO2
and H2O (limited supply of CO).
Alkene: A yellow, sootier flame is produced (due to the extra carbon and higher ratio of
carbon:hydrogen).
Alkene - Add to orange bromine water. The alkene will decolourise it.
Halogenalkane - Heat with sodium hydroxide solution. Acidify with dilute nitric acid and
then test with silver nitrate solution as with inorganic halides.
Alcohols or carboxylic acids containing C-OH - In a dry test tube (i.e. dry alcohol), add
PCl5. Misty fumes of HCl are produced, which turns blue litmus paper red.
Distinguishing between different classes of alcohol:
Primary - Add PCl5. Warm it with aqueous potassium dichromate (K2Cr2O7) and dilute H2SO4.
Misty fumes are given off and the colour changed from orange to green --> aldehyde.
Halogens are toxic and harmful by inhalation, although iodine is much less so than chlorine or
bromine, because it is a solid. Chlorine and bromine must always be used in a fume cupboard.
Liquid bromine causes serious burns an must be handled with gloves.
Ammonia is toxic. Concentrated ammonia solutions should be handled in the fume cupboard.
Concentrated mineral acids are corrosive. If spilt on the hands, washing with plenty of water is
usually enough, but advice must be sought. Acid in the eye requires immediate attention and
prompt professional medical attention.
Barium chloride solution and chromates and dichromates are extremely poisonous and so
should be used in the fume cupboard/should not be inhaled.
Sodium or potassium hydroxide or concentrated ammonia in the eye is extremely serious and
must always receive professional and immediate attention. Sodium hydroxide and other alkali
metal hydroxides are amongst the most damaging of all common substances to skin and other
tissue. Wear gloves, goggles and an apron when handling these solutions in high
concentrations.
General safety:
Tests
Ion Formula Test Observations
Test 1
Heat the solid in a test tube with a Bunsen
burner.
Limewater should turn from
It should decompose producing the oxide and colourless to cloudy in the
carbon dioxide. E.g. presence of carbon dioxide due to
precipitation of calcium carbonate.
Carbonate CO32-
Test for the gas using limewater solution.
Vigorous effervescence.
Test 2
Limewater should turn from
Add dilute HCl to the solid.
colourless to cloudy in the
Test for the gas evolved using limewater
presence of carbon dioxide due to
solution.
precipitation of calcium carbonate.
Test
No precipitate forms since calcium
Hydrogencarbonate HCO3- Add calcium chloride to a hydrogencarbonate
hydrogencarbonate is soluble.
solution.
Test
White precipitate of barium
Sulphate (VI) SO42- Add barium chloride solution acidified with
sulphate forms.
dilute HCl to the test solution.
Test
Warm the sulphite with dilute HCl.
Sulphite SO 3
2-
The solution turns green.
Test for gases using acidified potassium
dichromate(VI) solution (or paper)
Test 1
White steamy acidic fumes are
Add concentrated sulphuric acid to the solid
seen - HCl fumes.
chloride.
Test 2
Chloride Cl- Add dilute nitric acid to a solution of a chloride
to acidify the solution. This eliminates any
White precipitate of AgCl forms.
carbonates or sulphites.
Add silver nitrate to the solution.
Solid dissolves.
Add dilute ammonia solution.
Test 1
Purple acidic fumes are seen. The
Add concentrated sulphuric acid to the solid
mixture turns to a brown slurry.
iodide.
Test 2
Add dilute nitric acid to a solution of a iodide
Iodide I- to acidify the solution. This eliminates any
Yellow precipitate of AgI forms.
carbonates or sulphites.
Solid is insoluble.
Add silver nitrate to the solution.
Test 1
Heat solid nitrate.
If group 1 solid (not Li) then will decompose Oxygen gas is evolved that will
to give the nitrite and oxygen. relight a glowing splint.
Nitrate NO3- All other solid nitrates decompose to give the Brown gas is seen (NO2). Oxygen
metal oxide, nitrogen dioxide and oxygen. gas is also evolved and will relight
a glowing splint.
Test 2
Boil nitrate solution with aluminium/Devarda’s Litmus paper turns blue in the
alloy, in sodium hydroxide solution. presence of ammonia.
Test vapour with red litmus paper.
Test NH
Ammonium NH4+ Warm ammonium compound with NaOH. 3
Test vapours immediately using damp turns the litmus paper blue.
red litmus paper.
Test
Dip nichrome wire in HCl.
Test
Dip nichrome wire in HCl.
Test
Dip nichrome wire in HCl.
Test
Dip nichrome wire in HCl.
Tests
Name Formula Test Observations
Hydrogen H2 Ignite gas. Squeaky pop is heard.
Bubble gas through limewater A solution turns from colourless to cloudy. A white (milky)
Carbon
CO2 (saturated solution of calcium precipitate of calcium carbonate forms which is sparingly
dioxide
hydroxide) soluble.
Test 1
Test for gas using damp litmus
paper (red or blue) Chlorine bleaches the litmus paper very quickly.
Test 2
Test for gas using moist starch- The paper turns blue-black.
iodide paper.
Chlorine Cl2
Test 3
Pass gas through a solution of a The solution turns from colourless to orange.
bromide.
Test 4
The solution turns from colourless to brown (possibly with
Pass gas through a solution of
a black precipitate, iodine).
an iodide.
Nitrogen
NO2 Not many tests for this gas. The gas is brown.
dioxide
Test 1
Bubble gas through a solution
The solution turns from orange to green.
of potassium dichromate (VI)
dissolved in sulphuric acid.
Sulphur
SO2
dioxide
Test 2
Bubble gas through a solution
The solution turns from purple to colourless.
of potassium manganate (VII)
dissolved in sulphuric acid.
Volumetric analysis (titration) involves the reaction between two solutions. For one solution, both
the volume and the concentration are known; for the other, the volume only is known. Apparatus
A solution for which concentration is accurately known. The concentration may have been found by
a previous titration or by weighing the solute and making a solution of known volume. Such a
Place the weighing bottle on the pan and take the balance (i.e. re-zero it)
Take the bottle off the balance and add solid to it. This ensures that no spillages fall on the
pan.
Take the balance of the weighing bottle + solid and find the balance of solid by subtraction.
Replace on balance, and if the required amount is added, withdraw the mass.
When you have the required amount, write its value down immediately.
Wash out a 250cm3 volumetric flask three times using pure water.
Transfer the solid to a 250cm3 volumetric flask using a funnel, and wash out the weighing
bottle into the flask through the funnel using distilled water.
Stir the solution using a glass rod until all the solid visibly dissolves into a solution.
Wash all remaining apparatus including the glass rod, funnel and transfer the rest of this to
the flask.
Make up to 250cm3 with distilled water so that the bottom of the meniscus just touches
Shake the flask vigorously and/or invert the flask 5 or 6 times to create a solution with
uniform concentration.
moldm-3)
Using the pipette
A glass bulb pipette will deliver the volume stated on it within acceptable limits only.
Using a pipette filler, draw a little of the solution to be used into the pipette and use this to
Fill the pipette to about 2-3cm3 above the mark. Pipette fillers are difficult to adjust
accurately, so quickly remove the filler and close the pipette with your forefinger (not thumb).
Release the solution until the bottom of the meniscus is on the mark.
Immediately transfer the pipette to the conical flask in which you will do the titration, and
burette and rinse it out, not forgetting to open the tap and rinse the jet.
Close the tap and fill the burette. A small funnel should be used to add the solution but be
Remove the funnel, because titrating with a funnel in the burette can lead to serious error
if a drop of liquid in the funnel stem falls into the burette during the titration.
Bring the meniscus on to the scale by opening the tap to allow solution to pass through the
burette. There is no particular reason to bring the meniscus exactly to the zero mark.
Make sure that the burette is full to the tip of the jet.
After a suitable indicator has been added to the solution in the conical flask, swirl the flask
under the burette with one hand whilst adjusting the burette tap with your other hand.
Add the solution in the burette to the conical flask slowly, swirling the flask all the time.
As the endpoint is approached, the indicator will change colour more slowly. The titrant
Repeat the titration until you have three concordant titres, i.e. volumes that are similar.
This means within 0.2cm3 or better if you have been careful. Taking the mean of three tires
Common indicators
Methyl orange - yellow in alkali, red in acid & orange in neutral solutions(usually the end
point of a titration)
Weigh a spirit lamp (containing a liquid alcohol) using a balance accurate to 3 decimal
Use a measuring cylinder to put 100 cm3 of distilled water into a small beaker and clamps
Heat the water using the spirit lamp until the temperature has gone up by about 10C. Stir
Put a cap on the spirit to stop the alcohol burning. The lid stops also stops further
the insulating material --> should use a polystyrene cup and insulation like a lid.
The specific heat capacity and density of water are used (and not of HCl).
It is assumed that the specific heat capacity of the polystyrene cup is negligible.
Some heat is lost when the hydrogen or carbon dioxide are evolved in the reactions.
d) Describe the techniques used in simple organic preparations such as
distillation and heating under reflux
Heating under reflux - This allows reactions to occur slowly, over a long period of time, without any
loss of volatile liquid. The solvent evaporates and is condensed and returns to the flask.
To achieve this without loss of liquid, reaction mixtures are heated in a flask carrying a
vertical condenser.
This is heating under reflux; the solvent is condensed and returned to the flask, so the
To heat the round bottomed flask, either use a water bath, an oil bath or a heated plate
Simple distillation
Simple distillation is used where a volatile component has to be separated from a mixture,
the other components of the mixture being very much volatile or non-volatile.
The fraction that boils is collected within the temperature range of the fraction. (normally 1
The condenser cools the fraction so it distils and is collected in the receiving flask.
Fractional distillation
impurities. The choice of solvent is important. The substance must be easily soluble in the
boiling solvent and much less soluble at room temperature. This ensures the smallest possible
Re-Crystallisation Method
Dissolve the solid in the minimum amount of boiling solvent. This ensures that the solution
is saturated with respect to the main solute but not with respect to the impurities, which
Filter the hot mixture through a preheated filter funnel. This removes insoluble impurities.
The hot funnel is necessary to prevent the solute crystallising and blocking the funnel.
Filtration under vacuum using a Buchner funnel is often preferred, because it is fast.
Cool the hot filtrate, either to room temperature or, if necessary, in a bath of iced water.
Rapid cooling gives small crystals, slow cooling large ones. The large crystals are often
less pure.
Wash the crystals with a small amount of cold solvent. This removes any impurity
remaining on the surface of the crystals. A small amount of cold solvent is used so that
Transfer the crystals to a desiccator to dry. Drying between filter paper is sometimes
This is used to determine the purity of the re-crystallisation solid. Place small amount of the solid
in the sealed end of a capillary tube. Place in the melting point apparatus. A sharp melting point
over a small range shows purity, when compared with the set-book value of a higher melting point,
Organic tests
Halogenoalkane – Add NaOH, ethanol as solvent. Shake and warm for 3 minutes. Cool and
add nitric acid + silver nitrate. --> white = chloride; cream = bromide; yellow = iodide. -->
e) recall and interpret details of the chemistry of the elements and compounds
listed in Units 1 and 2 of this specification
this includes the chemistry of Groups 1, 2 and 7 and the chemistry associated with the
If a solution of any sulphate is added to a solution of a group 2 metal compound then a precipitate
is likely.
Hydroxide solubility
Sodium and potassium carbonates No effect (except water of crystallisation may be given off)
Group 2 nitrates - Oxide, brown fumes of nitrogen dioxide and oxygen formed.
Alkane: Burn /oxidise/combust them. They will burn with a yellow flame and form CO2 and
Alkene: A yellow, sootier flame is produced (due to the extra carbon and higher ratio of
carbon:hydrogen).
Alkene - Add to orange bromine water. The alkene will decolourise it.
Halogenalkane - Heat with sodium hydroxide solution. Acidify with dilute nitric acid and
Alcohols or carboxylic acids containing C-OH - In a dry test tube (i.e. dry alcohol), add
PCl5. Misty fumes of HCl are produced, which turns blue litmus paper red.
Primary - Add PCl5. Warm it with aqueous potassium dichromate (K2Cr2O7) and dilute H2SO4.
Misty fumes are given off and the colour changed from orange to green --> aldehyde.
calculations.
g) devise and plan simple experiments based on the chemistry and techniques
summarised in a to e above Normally the last question on the paper. It will ask
you to identify certain compounds from four. E.g. titrations, how to make a
standard solution, how to titrate, identify QCO3 when heating it where Q is a
group 2 metal ion.
Halogens are toxic and harmful by inhalation, although iodine is much less so than chlorine or
bromine, because it is a solid. Chlorine and bromine must always be used in a fume cupboard.
Ammonia is toxic. Concentrated ammonia solutions should be handled in the fume cupboard.
Concentrated mineral acids are corrosive. If spilt on the hands, washing with plenty of water is
usually enough, but advice must be sought. Acid in the eye requires immediate attention and
Barium chloride solution and chromates and dichromates are extremely poisonous and so should
Sodium or potassium hydroxide or concentrated ammonia in the eye is extremely serious and must
always receive professional and immediate attention. Sodium hydroxide and other alkali metal
hydroxides are amongst the most damaging of all common substances to skin and other tissue.
Wear gloves, goggles and an apron when handling these solutions in high concentrations.
General safety
Toxic/carcinogenic – use gloves, fume cupboard
Hydroxide solubility
If sodium hydroxide is added to a solution of a group 2 compound then a precipitate is likely.
Group 2 ion in
Effect of adding a hydroxide solution
solution
Lithium and all group 2 nitrates Nitrogen dioxide and oxygen evolved
g) devise and plan simple experiments based on the chemistry and techniques summarised in a to e above
Normally the last question on the paper. It will ask you to identify certain compounds from four. E.g.
titrations, how to make a standard solution, how to titrate, identify QCO3 when heating it where Q is a
group 2 metal ion.
h) evaluate error in quantitative experiments see Appendix I for material available to assist centres in
teaching this area Percentage error = absolute uncertainty/actual value x 100%
j) comment on safety aspects of experiments based on supplied data or recall of the chemistry of the
compounds listed in Units l and 2. Safety considerations should relate to specific experiments not be of a
general nature it will be assumed that students wear eye protection during all practical work.
Halogens are toxic and harmful by inhalation, although iodine is much less so than chlorine or bromine,
because it is a solid. Chlorine and bromine must always be used in a fume cupboard. Liquid bromine
causes serious burns an must be handled with gloves.
Ammonia is toxic. Concentrated ammonia solutions should be handled in the fume cupboard.
Concentrated mineral acids are corrosive. If spilt on the hands, washing with plenty of water is usually
enough, but advice must be sought. Acid in the eye requires immediate attention and prompt professional
medical attention.
Barium chloride solution and chromates and dichromates are extremely poisonous and so should be used
in the fume cupboard/should not be inhaled.
Sodium or potassium hydroxide or concentrated ammonia in the eye is extremely serious and must always
receive professional and immediate attention. Sodium hydroxide and other alkali metal hydroxides are
amongst the most damaging of all common substances to skin and other tissue. Wear gloves, goggles and
an apron when handling these solutions in high concentrations.
General safety
• Toxic/carcinogenic – use gloves, fume cupboard
• Flammable – Water baths, no naked fumes.
• Harmful gases – Use fume cupboard
• Corrosive – wear goggles/gloves
• Spillage of concentrated acid – wash with plenty of water.
tests
Formu
Ion Test Observations
la
Test 1
Heat the solid in a test tube with a Bunsen burner.
Limewater should turn from colourless
It should decompose producing the oxide and carbon to cloudy in the presence of carbon
dioxide. E.g. dioxide due to precipitation of calcium
carbonate.
Carbonate CO32-
Test for the gas using limewater solution.
Vigorous effervescence.
Test 2 Limewater should turn from colourless
Add dilute HCl to the solid. to cloudy in the presence of carbon
Test for the gas evolved using limewater solution. dioxide due to precipitation of calcium
carbonate.
Test
White precipitate of barium sulphate
Sulphate (VI) SO42- Add barium chloride solution acidified with dilute HCl to
forms.
the test solution.
Test
2- Warm the sulphite with dilute HCl.
Sulphite SO3 The solution turns green.
Test for gases using acidified potassium dichromate(VI)
solution (or paper)
Test 2
Chloride Cl-
Add dilute nitric acid to a solution of a chloride to acidify
the solution. This eliminates any carbonates or sulphites. White precipitate of AgCl forms.
Add silver chloride to the solution.
Add dilute ammonia solution. Solid dissolves.
Test 1
Steamy brownish acidic fumes are seen.
Add concentrated sulphuric acid to the solid bromide.
Test 2'
Bromide Br-
Add dilute nitric acid to a solution of a bromide to acidify
the solution. This eliminates any carbonates or sulphites. Cream precipitate of AgBr forms.
Add silver chloride to the solution.
Add concentrated ammonia solution. Solid dissolves.
Test 1
Heat solid nitrate.
If group 1 solid (not Li) then will decompose to give the Oxygen gas is evolved that will relight a
nitrite and oxygen. glowing splint.
Nitrate NO3- All other solid nitrates decompose to give the metal oxide, Brown gas is seen (NO2). Oxygen gas is
nitrogen dioxide and oxygen. also evolved and will relight a glowing
splint.
Test 2
Boil nitrate solution with aluminium/Devarda’s alloy, in Litmus paper turns blue in the presence
sodium hydroxide solution. of ammonia.
Test vapour with red litmus paper.
NH
Test
Ammonium NH4+ 3
Warm ammonium compound with NaOH.
turns the litmus paper blue.
Test vapours immediately using damp red litmus paper.
Test
Dip nichrome wire in HCl.
Test
Dip nichrome wire in HCl.
Test
Dip nichrome wire in HCl.
Test
Dip nichrome wire in HCl.
Test
Dip nichrome wire in HCl.
Tests
Formu
Name Test Observations
la
Ammonia NH3 Test for gas using damp red litmus paper. Litmus paper turns blue.
Test 1
Test for gas using damp litmus paper (red or Chlorine bleaches the litmus paper very quickly.
blue)
Test 2
The paper turns blue-black.
Test for gas using moist starch-iodide paper.
Chlorine Cl2
Test 3
The solution turns from colourless to orange.
Pass gas through a solution of a bromide.
Test 1
Bubble gas through a solution of potassium The solution turns from orange to green.
dichromate (VI) dissolved in sulphuric acid.
Sulphur
SO2
dioxide
Test 2
Bubble gas through a solution of potassium The solution turns from purple to colourless.
manganate (VII) dissolved in sulphuric acid.
Volumetric analysis
Volumetric analysis (titration) involves the reaction between two solutions. For one solution, both the
volume and the concentration are known; for the other, the volume only is known. Apparatus used
includes a burette, a pipette and a volumetric flask.
Common indicators
• Methyl orange - yellow in alkali, red in acid (orange at end point)
• Phenolphthalein - pink in alkali, colourless in acid.
Simple distillation
To separate a volatile solvent from a mixture
• Simple distillation is used where a volatile component has to be separated from a mixture, the
other components of the mixture being very much volatile or non-volatile.
• The mixture is heated.
• The fraction that boils is collected within the temperature range of the fraction. (normally 1 or 2
degrees before the boiling temperature)
• The condenser cools the fraction so it distils and is collected in the receiving flask.
Fractional distillation
To separate mixtures of volatile liquids.
• Re-crystallisation - Used to purify a solid material by removing both soluble and insoluble
impurities. The choice of solvent is important. The substance must be easily soluble in the boiling
solvent and much less soluble at room temperature. This ensures the smallest possible loss of
material, although some loss is inevitable with this technique.
Re-crystallisation method
1. Dissolve the solid in the minimum amount of boiling solvent. This ensures that the solution is
saturated with respect to the main solute but not with respect to the impurities, which are present
in much smaller amounts.
2. Filter the hot mixture through a preheated filter funnel. This removes insoluble impurities. The hot
funnel is necessary to prevent the solute crystallising and blocking the funnel. Filtration under
vacuum using a Buchner funnel is often preferred, because it is fast.
3. Cool the hot filtrate, either to room temperature or, if necessary, in a bath of iced water. Rapid
cooling gives small crystals, slow cooling large ones. The large crystals are often less pure.
4. Filter the cold mixture using a Buchner funnel.
5. Wash the crystals with a small amount of cold solvent. This removes any impurity remaining on the
surface of the crystals. A small amount of cold solvent is used so that the crystals aren’t washed
away / don’t dissolve.
6. Suck the crystals as dry as possible on the filter.
7. Transfer the crystals to a desiccator to dry. Drying between filter paper is sometimes
recommended, but it is a very poor method.
Organic tests
• Collect 10 cm³ of the samples.
• Test the samples in the following order
• Alkenes – bromine water --> decolourises --> alkene
• Alcohols – Spatula of solid PCl5. Test fumes with damp litmus paper --> litmus red? White fumes
near ammonia? --> alcohol
• Halogenoalkane – Add NaOH, ethanol as solvent. Shake and warm for 3 minutes. Cool and add
nitric acid + silver nitrate. --> white = chloride; cream = bromide; yellow = iodide. --> Confirm with
ammonia
• Alkane, the substance left is the alkane.
Techniques
Separating insoluble impurities from a soluble substance (Removing sand and impurities from salt solution)
(1)Reason for heating the mixture but then taking the flame away
(1)provide Ea, exothermic/prevent reaction getting out of control
Separating mixtures of similar compounds in solution (Separating dyes present in a sample of ink)
Chromatogram Chromatography Different components of the dye spread out at different rates
Using a square sheet of filter paper, spots of dye solutions are put along the baseline
The filter paper is coiled into a cylinder and placed in a tank containing a small volume of solvent
The lid is replaced on the tank, solvent rises up the filter paper
When the solvent nearly reaches the top of the filter paper, the filter paper is removed and position
of solvent marked.
Dyes A & B are either pure substances or a mixture of dyes not separated with the solvent used
Dye C is composed of A & B as the spots correspond
Colourless substances can be separated and seen by spraying/dipping the filter paper into a
locating agent which colours the spots produced
Mixture Compound
- Proportions of the different elements can be varied - Different elements have to be present in fixed proportions
- Properties are those of the elements making it up - Properties different from properties of elements making it up
- Elements can be separated by simple methods - Difficult to separate into the elements which make it up
- No energy gained or lost when the mixture is made - Energy usually given out/taken in when compound is formed
Sub-atomic particles Protons, neutrons and electrons which makes up the atom
Particle An atom, molecule, ion, electron or any identifiable particle RTP Room temperature and pressure
Electron A negatively charged particle, with negligible mass occupying the outer regions of all atoms
Immiscible Unable to mix, dissolve in each other, to form a homogenous mixture Miscible Soluble in each other
(aq) Substance dissolved in water to form an aqueous solution
State symbols Physical state of the reactants at RT Aqueous(aq)
Solvent Substance in which other substances are dissolved
Solute Substance dissolved in another substance(solvent)to form a solution
Chemical species Collection of particles Distilled water Water that has been purified by distillation
Ion When number of protons and electrons are different
Atom The smallest part of an element that can exist on its own
Molecule 2 or more atoms bonded together
Element A pure substance which can’t be split up by chemical
reaction
Compound Combination of elements in fixed proportions via
synthesis
In formation of a compound from ions the charges balance out
Physical properties: Mt, Bt, hardness
• Compounds ending in –ate –ite contain oxygen, greater proportion of oxygen in the compound ending in –ate
Sodium sulphate Na2SO4 Sodium sulphite Na2SO3
• Compounds with prefix per– contain extra oxygen
Sodium oxide Na2O Sodium peroxide Na2O2
• Compounds with prefix thio– contain a sulphur atom in place of an oxygen atom
Sodium sulphate Na2SO4 Sodium thiosulphate Na2S2O3
Metalloid Element which has properties between metals and nonmetals
- Ions in an ionic compound are tightly held together in a regular lattice, lattice energy is required to break it up and melt the substance
A metal high in the reactivity series has stable ores and the metal can be obtained only by electrolysis
A metal middle in the reactivity series doesn’t form stable ores and can be extracted by reduction reactions (often with carbon)
A metal low in the reactivity series, if present in unstable ores can be extracted by heating
Decomposition Splitting up of a compound (Thermal decomposition - decomposition of a compound by heating)
Combustion is the reaction of a substance with oxygen, total mass of products is greater than the mass of the substance burned,
difference being the mass of oxygen combined
Sublimation of an element/compound is a transition from solid to gas with no intermediate stage
When a change of state takes place the temperature remains constant despite a continuing supply of energy. Latent heat is the energy
which is not being used to raise the temperature and supplies particles with the extra energy they require as the state changes(given out
when the reverse changes take place)
Fe(s) + CuSO4(aq) FeSO4(aq) + Cu(s) Blue solution turns colourless and brown copper is deposited
A displacement reaction where a more reactive metal replaces a less reactive metal in a compound
Electrolysis of HCl(aq): 2HCl(aq) Cl2(g) + H2(g) Cathode: 2H+(aq) + 2e– H2(g) Anode: 2Cl –(aq)Cl2(g)+2e–
Heat
Ammonium chloride NH4Cl(s) NH3(g) + HCl(g)
Cool
A stopper from a bottle of (conc)NH3(aq) held near a stopper from a bottle of (conc)HCl acid gives a dense white smoke of NH4Cl
Synthetic Pathways(Series of reactions built up to convert one functional group into another)
• Reactions of functional groups assumed to be the same whether molecules are simple or complicated
• Synthesis of the product molecule possible because in any reaction of a functional group a product is formed capable of conversion
into other molecules
– 5.31 × 4.18 × ΔT
mass of G used (g) –1 Would the result for ∆H be more accurate if the temperature of the solution were known to 3dp?
∆H = kJ mol Yes, temperature would then be known to a comparable precision to the other factors in the equation
Plan an experiment to investigate concentration on rate of a reaction Mg(s) + 2HCl(aq) → MgCl (aq) + H (g)
2 2
• Apparatus diagram/description/addition of Mg to acid in appropriate container
• Weigh Mg/cut measured length and measure volume of acid, measure volume of H with time/time how long it takes for Mg to
2
’dissolve’ • repeat with different concentration(s) HCl • repeat with same mass/length Mg and same volume HCl
• one axis labelled concentration/volume H and other axis time/t axis changed to 1/t
2
if measured volume H at least two curves showing increasing rate with conc
2
if measured time to dissolve Mg one line showing time decreasing with conc or 1/t increasing with conc
• Acid irritant so wear gloves or hydrogen explosive - no naked flame or Build up of pressure in syringe - attach plunger with string
– –
(NH ) CO reacts with both 1moldm ³(dil)HNO and 1moldm ³(dil)KOH in the ratio 1:2
42 3 3
Devise an experiment to determine which of the two reactions is the more exothermic
• Prepare solutions of known concentration of the solid
• Suggestion of apparatus used e.g. lagged calorimeter or low mass polystyrene cup • Use same volume of each solution
• Measure maximum temperature change • Improve reliability of results, repeat experiment • Possible sources of error identified
• Reaction with the greater temperature change is the more exothermic • Since ammonia evolved use a fume cupboard
M = Group 1 M CO (s) + 2HCl(aq) → 2MCl(aq)+CO (g)+H O(l)
2 3 2 2
Plan an experiment, results of which used to calculate the relative
molecular mass of the carbonate and identify M
3
At temp of experiment 1 mole of CO occupies a volume of 24dm
2 G a s s y rin g e
Relative atomic mass: Li = 7, C = 12, O = 16, Na = 23, K = 39, Rb = 85,
Cs = 133
• Add M CO + acid and stopper flask/use suspended test tube in large flask
2 3
• Mass of M CO and (final)vol of CO /when effervescence stops record volume of gas in syringe
2 3 2
• Explain conversion volume of CO to moles by correct use of 24
2
• Use of moles M CO = mass M CO ¸ M M CO to find M • Hence find identity of M
2 3 2 3 r 2 3 r
• Escape of gas before bung replaced/solid did not all react/CO soluble in acid • Eye protection-acid hazard
2
• Should not affect identification since even if M is slightly wrong it will still correspond to nearest Group 1 metal atomic mass
r
–1
Plan an experiment to identify an acidic compound, molar mass for an acid estimated to be 88 ± 2 g mol
What simple test would allow butenoic acid to be distinguished from the other two? Devise a plan based upon a quantitative
experiment that would allow the other two to be distinguished
–1 –1 CO O H
CH = CH CH COOH 86 g mol CH CH CH COOH 88 g mol –1
2 2 3 2 2 HC O O H 90 g mol
3 structures proposed for this acid
Alkene detected using bromine water, only 1 would show decolourisation
Fixed mass of acid, Standard named alkali, Controlled method of addition, To an identified end point of a named suitable indicator,
Calculation of mole ratio
(1)A sample of NaCl was thought to contain an impurity of Ba(NO3)2 A student suggested a flame test
(a)(i)Suggest why a flame test on the mixture would not be a satisfactory way of detecting the presence of barium ions in the sample
(i) • yellow/stronger/persistent Na flame • Obscures/Ba flame NOT “makes it difficult to distinguish between the two colours”
(ii)Suggest a reagent that could be used to produce a ppt of a barium compound from a solution of the sample
(ii) • (conc)H SO (solution) of any soluble sulphate (MgSO , (NH )2SO , Na SO )
2 4 4 4 4 2 4
(2)(a)X(has OH group)decolourised cold potassium manganate(VII) acidified with (dil)H SO acid, structure of X suggested by this?
2 4
(a)carbon double bond
(b)Complete oxidation of X with potassium dichromate(VI) solution and (dil)H2SO4 acid produces Y C H O structure for Y?
4 6
H H H H H H H
C C C C H C H 2 C H CO CH 3 (1 ) C C C C H (2 )
(b) H O H (c)Structural formula for X?(c) H O H H
X must be a secondary alcohol because ketone formed on oxidation carboxylic acid is not formed
+ –
(3)(a)Write an ionic equation for the hydrolysis of 1-bromobutane by water (a)CH H Br + H O → C H OH + H + Br
4 9 2 4 9
(b)Suggest why ethanol was used in the experiment (b)Solvent/silver nitrate solution in water and bromobutane immiscible
(c)Suggest a reason for the use of a water bath (c)Reaction slow at RT/increases rate/flammable
(4)Describe tests you would use to distinguish between the following pairs of compounds including results
(a)NaNO and ammonium nitrate NH NO (a) Flame test, sodium salt gives yellow colour, ammonium salt gives no colour
3 4 3
(5)(a)1-bromobutane Bt102 °C may be prepared by the reaction C H OH + NaBr + H SO → C H Br + NaHSO + H O
4 9 2 4 4 9 4 2
(a)Describe how you would use distillation apparatus to give a sample of pure 1-bromobutane
(a)Heat mixture(slowly), collect only distillate produced at around 102 °C at Bt of 1-bromobutane
(b)Suggest 2 reasons why the actual yield was much lower than the max yield
(b)side reactions, reaction incomplete, product lost in purification/transfers
2 .0 0
(6)CaCO (s) + 2HCl(aq) → CaCl (aq) + H O(l) + CO (g)
3 2 2 2
Experiment CaCO HCl acid
3
1 .5 0
1 RT Small pieces 3 –3
M a ss lo s s /g
50cm of 1moldm
2 Small pieces 3 –3
50cm of 1moldm heated to 1 .0 0 E x p t. 1
80°C
3 RT One large 3 –3
piece 50cm of 1moldm
0 .5 0
4 RT Small pieces 3 –3
50cm of 2moldm
(a)(i)Explain why there is a loss in mass as the reaction proceeds
(i)CO (g) evolved 5 10 15
2
T im e /m in
(ii)Explain the shape of the curve drawn for Experiment 1 Results of Experiment 1
(ii)Reaction(fast at first then)slows down/gives off less CO per
2
min when line is horizontal, the reaction has finished/after 6 or 7
minutes/when 1 g of CO lost
2
(b)Draw curves on the graph to represent the results you would expect for Experiments 2, 3 and 4. Label the curves 2, 3 and 4
(b)Experiment 2 steeper than 1 and same mass loss Experiment 3 less steep than 1 and same mass loss/reaction incomplete
Experiment 4 steeper than 1 and horizontal at twice mass loss
(7)Suggest one appropriate safety precaution that should be taken as ethanedioic acid is toxic (7)Safety pipette filler
2+ 2+
(8)In an experiment to find ∆Η, zinc CuSO4(aq) in a plastic cup Zn(s) + Cu (aq) → Zn (aq) + Cu(s)
Suggest reasons why a series of temp readings is taken rather than simply initial and final readings
(8) Reason 1 Any fluctuations in temperature smoothed out / minimises reading error/allows line of best fit to be drawn
Reason 2 Able to allow for cooling effect/able to calculate more accurate temperature change/need to find highest temperature
Another Test List (If you find above one hard to read)
Flame test
1 Clean end of platinum/nichrome wire with(conc)HCl, burning off impurities in a roaring bunsen flame until there’s no persistent flame colouration
2 Moisten the end of the clean wire with (conc)HCl and then dip into the sample to be tested
3 Hold the sample at the edge of a roaring bunsen flame
Lithium Carmine red Calcium Brick red
Sodium Yellow Strontium Crimson
Potassium Lilac Barium Apple green
Gas Test
Ammonia NH3 Pungent smell, Moist litmus paper red blue, (conc)HCl at mouth of bottle, white smoke forms
Carbon dioxide CO2 Pass through lime water, turning lime water milky
CaCO3(s) + H2O(l) + CO2(g) Ca(HCO3)2(aq)
Limewater CO2 test Ca(OH)2(aq) + CO2(g) CaCO3(s) White ppt + H2O(l)
Chlorine Cl2 Swimming pool smell, moist litmus paper blue red bleached
Hydrogen H2 Lighted splint, burns with squeaky pop
Hydrogen chloride HCl Moist litmus paper blue red
Nitrogen(IV)oxide NO2 Brown gas, acrid smell, moist litmus paper blue red
Oxygen O2 Glowing splint, relights
Water vapour H2O White anhydrous copper(II) sulphate white blue CuSO4(s) + 5H2O(l) CuSO4.5H2O(s)
Or dry blue cobalt chloride paper blue pink
Sulphur dioxide SO2 Acrid smell, moist litmus paper blue red
Or potassium dichromate(VI) solution/paper from orange green
Cation Test Add NaOH(aq) Add NH4OH(aq)
Ammonium NH4+ • Heat, ammonia evolved, moist litmus paper red blue
H+ • Moist litmus paper blue red
• Add a carbonate, pass gas through lime water, CO2 evolved turning lime water milky
Copper(II) Cu2+ • A little, blue ppt forms • A little, blue ppt forms
• In excess, insoluble • In excess, dissolves and a dark blue solution forms
Iron(II) Fe2+ • A little, green ppt forms • A little, green ppt forms
• In excess, insoluble • In excess, insoluble
Iron(III) Fe3+ • A little, brown ppt forms • A little, brown ppt forms
• In excess, insoluble • In excess, insoluble
Calcium Ca2+ • A little, milky suspension forms • A little, milky suspension forms
• In excess, insoluble • In excess, insoluble
Distinguish Mg from Ca through flame test
Magnesium Mg2+ • A little, milky suspension forms • A little, milky suspension forms
• In excess, insoluble • In excess, insoluble
Aluminium Al3+ • A little, white ppt forms • A little, white ppt forms
• In excess, dissolves giving colourless solution • In excess, insoluble
No ppt with (dil)H2SO4/cold(dil)HCl/(dil)KI/(dil)Na2S Sodium sulphide
Lead Pb2+ • A little, white ppt forms • A little, white ppt forms
• In excess, dissolves giving colourless solution • In excess, insoluble
White ppt with (dil)H2SO4 White ppt with cold(dil)HCl
Yellow ppt with (dil)KI Black ppt with (dil)Na2S Sodium sulphide
Zinc Zn2+ • A little, white ppt forms • A little, white ppt forms
• In excess, dissolves giving colourless solution • In excess, dissolves giving colourless solution
Anion Test
Carbonate pH>10 CO32– Add (dil)HCl(aq) Pass gas through lime water, CO2 evolved turning lime water milky
universal indicator Or add group II ions, white ppt or heat/add boiling water, no gas evolved
Hydrogen carbonate HCO3– Add (dil)HCl(aq) Pass gas through lime water, CO2 evolved turning lime water milky
pH 8-9 Or add metal ions no ppt but heating causes white ppt to form or Heat/add boiling water, CO2 evolved
Chloride Cl– Acidify with (dil)HNO3(aq) Add AgNO3(aq) Add (dil)NH3 to ppt
White ppt AgCl forms Ppt dissolves leaving colourless solution
Bromide Br– Acidify with (dil)HNO3(aq) Add AgNO3(aq) Add (conc)NH3 to ppt
Cream ppt AgBr forms Ppt dissolves leaving colourless solution
Iodide I– Acidify with (dil)HNO3(aq) Add AgNO3(aq) Add (conc)NH3 to ppt
Yellow ppt AgBr forms Ppt insoluble
Nitrate NO3– Add NaOH(aq) Add Devarda’s alloy (powdered Zn, Al) Heat & hold moist red litmus at mouth of test tube
NH3 evolved, litmus paper red blue
Sulphate SO42– Add Barium nitrate Ba(NO3)2(aq)/chloride BaCl2(aq) Add HCl(aq)
White ppt Insoluble
Sulphite SO32– Add Barium nitrate Ba(NO3)2(aq)/chloride BaCl2(aq) Add HCl(aq)
White ppt Dissolves
Or add (dil)HCl(aq) Heat
SO2 evolved turning potassium dichromate(VI) solution/paper from orange green
Practical List
1. Make a salt and calculate the percentage yield (hydrated nickel sulfate)
2. make a salt and calculate the percentage yield (ammonium iron(II) sulfate)
3. carry out and interpret results of simple test tube reactions
4. measuring some enthalpy changes
5. finding the enthalpy of combustion of an alcohol
6. finding an enthalpy change that cannot be measured directly
7. reaction of alkanes
8. reaction of alkenes
9. experiment to find the effect of electrostatic force on jets of liquid
10. solubility of simple molecules in different solvents
11. thermal decomposition of group 2 nitrates and carbonates
12. flame tests on compounds of group 1 and 2
13. simple acid-base titrations
14. oxidation of metal and non-metallic elements and ions by halogens
15. disproportion reactions with cold and hot alkali
16. iodine/thiosulfate titration and the determination of purity of potassium iodate(V)
17. reactions between halogens and halide ions/some reactions of the halides
18. factors that influence the rate of chemical reactions
19. effect of temperature, pressure and concentrations on equilibrium
20. reactions of alcohols
21. preparation of organic liquid (reflux and distillation)
22. preparation of a halogenoalkane from an alcohol
23. reactions of the halogenoalkanes.
GCE
Chemistry
User guide
Issue 2
May 2008
Edexcel, a Pearson company, is the UK’s largest awarding body, offering academic
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This includes the ability to provide detailed performance data to teachers and
students which helps to raise attainment.
This specification is Issue 2. Key changes are sidelined. We will inform centres of any
changes to this issue. The latest issue can be found on the Edexcel website:
www.edexcel.org.uk
References to third party material made in this specification are made in good faith.
Edexcel does not endorse, approve or accept responsibility for the content of
materials, which may be subject to change, or any opinions expressed therein.
(Material may include textbooks, journals, magazines and other publications and
websites.)
Introduction 1
1 — The scheme of assessment 3
1.1 Activities 3
1.2 Conditions under which assessments are to be carried out 3
1.3 Materials allowed when carrying out assessment activities 4
1.4 Health and safety 4
4 — Activity d: Preparation 11
5 — Activity c+d: Multi-stage experiment 12
Reference section 13
A — Inorganic compounds and elements 13
1 Appearance 13
2 Flame tests 14
3 Heating 14
4 Recognition and identification of common gases 15
5 Action of dilute acids 15
6 Tests for oxidizing and reducing agents 16
7 Hydrogen peroxide solution 16
B — Precipitates 17
1 Sodium hydroxide solution 17
2 Ammonia solution 18
3 Barium chloride solution 18
4 Silver nitrate solution 19
5 Concentrated sulfuric acid 19
C — Organic compounds 20
1 Appearance 20
2 Solubility 20
3 Ignition 20
4 Chemical tests 21
D — Spectroscopy 23
1 Mass spectrometry 23
2 Infrared spectroscopy 23
3 Nuclear magnetic resonance (nmr) 23
Introduction
This User guide has been written for students to help them in preparing for the tasks that are
part of the internal assessment of practical skills. Teachers may also find this information
helpful when preparing students for the assessment activities. The material contained in the
booklet does not extend the specification content, but aims to help students to succeed in the
assessment activities by:
• explaining in more depth what is required in carrying out the activities, making
observations and measurements with appropriate precision and recording these
methodically
• advising them how to interpret, explain, evaluate and communicate the results of the
activities clearly and logically using the relevant chemical knowledge, understanding and
appropriate specialist vocabulary.
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1 — The scheme of assessment
1.1 Activities
At both AS and A2 Level the skills being assessed in the activities are:
a General practical competence (GPC) (verification)
b Qualitative observation (14 marks)
c Quantitative measurement (14 marks)
d Preparation (12 marks)
The maximum mark available at both AS and A2 Level is 40.
Students will have their practical skills assessed by carrying out the assessment activities on a
number of occasions throughout the course. The assessment activities are set by Edexcel.
For activity a, the teacher is required to confirm that students have completed a range of
practicals over the whole year and developed their laboratory skills. Students must have
carried out at least five practicals in class. The practicals that the students complete must
cover the three areas of physical, organic and inorganic chemistry. These five practicals can
be either core practicals, or suitable alternatives.
The marks for activities b, c and d are awarded following the teacher’s application of the
mark schemes that accompany each assessed activity. Students need only carry out one
exercise for each of activities b, c and d. However they may carry out more than one. In this
case, only the highest mark for each activity will count towards the final mark out of 50.
At A2 there is the option of completing a multi-stage experiment at A2, which consists of
activities c and d together in a longer practical, which is worth 26 marks.
Teachers have the option of marking these activities or having them marked by Edexcel.
The practical assessment activities must be carried out under controlled conditions that
guarantee that students produce individual work. This includes those activities that involve
the processing of results. Students must not consult with each other during the activities.
Some activities can be completed in a laboratory session of approximately one hour. When an
activity has to be carried over to a following session students must not remove any materials,
including results and instruction sheets, from the laboratory. Instead, these must be collected
by the teacher and reissued at the beginning of the next session when the activity is to be
completed.
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1.3 Materials allowed when carrying out assessment activities
Each activity has a cover sheet and a student brief giving full instructions for carrying out the
activity and the questions based on it.
During the activity students must not refer to books and notes although the data booklet is
required for some exercises. This User guide must not be used as a reference when carrying
out the internal assessment tasks.
Students must follow the health and safety rules which normally operate in their chemistry
laboratories, including the following:
• eye protection must always be worn
• laboratory coats must be worn when appropriate
• plastic gloves must be worn when supplied for a particular exercise
• all substances should be regarded as being potentially toxic and hazardous
• HazChem labels (eg flammable) should be read and appropriate precautions (eg 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 students to do
so, and then this should be done only with great care.
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2 — Activity b: Qualitative observation
Activity b will be assessed by tasks that include a number of tests to be carried out, usually on
a test tube scale. The instructions for each test will include details on quantities to be used,
whether heat is required and whether excess reagent should be added. The reagents used for
the tests will be limited to those included in the specification. Similarly, unknowns will be
limited to compounds containing the ions, elements and organic compounds with the
functional groups listed in the specification. As part of a task to identify an organic unknown,
spectroscopic data may be included for students to analyse. Other physical data such as
melting temperatures may also be given.
These qualitative observation tasks will change each year.
After a student has carried out each test, as instructed in the task, they must communicate
the results by giving a brief description of what has been observed. Possible changes that can
occur during tests are listed below, along with examples of what students should write in the
observation boxes.
There are a number of common mistakes which students make when recording their
observations. The following should be avoided.
• Referring to ‘layers’ in test tubes. Almost certainly the presence of layers is due to
inadequate mixing of the reagents. The exception to this is when an organic liquid is mixed
with an aqueous solution, or with water, in which case ‘layers’ may be a valid observation.
• Describing colours with elaborate adjectives such as brown-black or blue-green. Marks are
awarded for simple descriptions of the colours of solutions and precipitates, such as black
or blue, even if there is a trace of a second colour.
• Stating that a gas is evolved without making an observation such as bubbles or
effervescence.
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• Using clear instead of colourless for a solution. All solutions are clear even if coloured, eg
copper sulfate solution is clear but coloured blue, whereas sodium sulfate solution is
colourless.
The purpose of asking students to make inferences from their observations is to test their
knowledge, understanding and evaluation of the chemistry which leads to the observations.
Activities include asking students to identify precipitates or gases formed in a test and which
are recorded as an observation. Also, students could be asked to identify the unknown
compound following a series of tests.
In some cases the test may be enough to enable students to suggest the identity of a
particular ion or functional group, but in others a number of possibilities may exist as a result
of a single test.
Example 1
The addition of aqueous ammonia to an inorganic compound produces a green precipitate. The
inference from this test alone should be iron(II) hydroxide, chromium(III) hydroxide or
nickel(II) hydroxide.
Example 2
In an organic analysis, a compound produces an orange precipitate with
2,4−dinitrophenylhydrazine. The expected inference would be that the unknown compound is
an aldehyde, ketone or carbonyl compound. If a following test shows that the compound is an
aldehyde then the inference still stands, as this was valid on the basis of the
2,4−dinitrophenylhydrazine test. If more is known about the compound, for example its
molecular formula and the fact that it cannot be oxidised, then it may be that the compound
can be identified as a result of the 2,4−dinitrophenylhydrazine test.
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3 — Activity c: Quantitative measurement
Activity c will be assessed through tasks that involve using apparatus to make measurements
and to process the results, to draw conclusions and evaluate the procedure.
Quantitative activities could involve:
• a volumetric analysis task
• a simple thermochemistry task
• a task to follow the rate of a reaction.
3.1 Accuracy
Unless an activity instructs students differently, they should assume that readings from
equipment and apparatus should be made with the following precision.
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• Students should try to obtain at least two titres within 0.20 cm3, or better, of each other
and average these to obtain a mean titre. Students should make it clear which titres have
been used to obtain a mean.
• A final result should only be given to the same number of significant figures as is suggested
in the exercise. For example a task to find a ΔH value may involve a weighing of 1.56 g and
a temperature rise of 7.5°C. A student who calculates a value of ΔH from these figures
may obtain a value of 195.6843 on a calculator but this should be finally recorded as 200
kJ mol−1, although 196 kJ mol−1 may also be acceptable.
• Units should always be included with a quantitative result.
A significant proportion of the marks awarded for a quantitative measurement activity will be
for accuracy. These marks will be awarded by comparing the student’s results with an
expected value.
3.2 Errors
Students should appreciate that any piece of equipment (burette, pipette, thermometer,
balance) used in a quantitative exercise has an uncertainty associated with its use. Even if the
equipment is used carefully, the uncertainty leads to an error in the reading and in the final
result.
Eg a balance has an uncertainty of 0.01 g when read to the second decimal place. A reading of
2.64 g recorded in an experiment has an error of:
0.01
× 100% = 0.38%
2.64
2 Students should:
• calculate the error involved in using a particular piece of equipment and state what effect
this has on the overall accuracy of the activity
• understand that the percentage error would be affected by the magnitude of the quantity
being measured. There will be a greater error in weighing a mass of 2.64 g than in
weighing 8.64 g using the same balance.
3 Only a simple treatment of errors is needed and students will not be asked to combine
errors.
3.3 Calculations
Usually calculations will be structured. Students will be taken/guided through a series of steps
leading to a final answer. Since most of the marks for these steps will be for use of a correct
method, rather than for the numerical answer, it is important that students include their
workings even if these seem to be trivial. Marks cannot be awarded for an incorrect answer
without workings, but a correct method followed by an incorrect answer can often receive
credit. Units, if appropriate, should always be included with a quantitative result.
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3.4 Graphs
For some activities students will need to treat their readings graphically.
The following are some useful points for students to consider when drawing graphs.
• Put the dependent variable, the quantity being measured (eg temperature), on the y−axis.
And the pre-determined quantity (eg volume of solution) on the x−axis.
• Choose the scales so that the results are spread out as far apart as the size of the grid
allows, but this should not be at the expense of using a sensible scale, eg using 1 cm on
the axis to represent 3 or 4 units might spread the readings better than using 1 cm to
represent 5 units, but the scale would be hard to read.
• The origin (0,0) does not need to be included on either scale if it is not relevant,
• For example if temperature readings between 21.0°C and 39.0°C are to be plotted there is
no need to begin the y−axis at 0. Rather it could be scaled from 20.0°C to 40.0°C.
• Clearly label the axes with the quantity being plotted (eg time) and its units
(eg minutes).
• Join the points plotted with a continuous straight line or smooth curve. Since the 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.
The instructions for carrying out a quantitative measurement activity will include the essential
points for the particular task. For example:
• which chemicals to use
• the quantities needed
• the sequence of steps in the method
• the readings to be taken.
The assessment activities will assume that students have developed a range of routine
practical skills in their course leading up to the exercise. Instructions may not, therefore,
include every step needed to gain accurate readings.
Examples of normal laboratory procedures which may not be referred to in the instructions
include:
• burettes, pipettes and measuring cylinders should be rinsed with the solution they are to
contain
• a pipette filler should always be used with a pipette
• conical flasks and volumetric flasks should be rinsed out with distilled water
• a burette should be read at eye level
• a thermometer bulb must be held in the centre of a solution when temperature readings
are taken
• care should be taken not to lose drops of a solution when thermometers or stirring rods are
removed from it
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• containers may need to be labelled if this has not already been done
• care should be taken as to where apparatus is placed on the bench, eg temperature
measurements should not be taken in apparatus standing next to a Bunsen burner, in a
patch of sunlight or in a strong draught.
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4 — Activity d: Preparation
Activity d is assessed through tasks in which students follow a procedure to prepare and, in
some cases, purify an inorganic or organic compound. Marks are awarded for the student's
ability to follow laboratory procedures and to use apparatus competently and safely.
Preparations can include some of the following laboratory procedures:
• distillation
• heating under reflux
• filtration, including under reduced pressure
• purification by washing in a separating funnel
• solvent extraction
• drying
• boiling and melting temperature determination
• crystallization and recrystallization.
Following some preparations students will be asked to calculate the maximum mass of product
and a percentage yield.
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5 — Activity c+d: Multi-stage experiment
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Reference section
1 Appearance
• The colours of transition metal ions in dilute, aqueous solution are shown in the table
below.
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2 Flame tests
• To carry out a flame test, a clean nichrome wire is used to mix a sample of a solid with
one drop of concentrated hydrochloric acid. The wire is held in progressively hotter
parts of a non-luminous Bunsen flame.
3 Heating
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4 Recognition and identification of common gases
Gas Observations
oxygen colourless gas which relights a glowing splint
carbon dioxide colourless gas which gives a white precipitate with
limewater (calcium hydroxide solution)
ammonia colourless gas which turns moist red litmus paper blue and
forms white smoke with hydrogen chloride
nitrogen dioxide brown gas*
hydrogen colourless gas which ignites with a ‘pop’
hydrogen chloride steamy fumes on exposure to moist air, acidic and forms
white smoke with ammonia
chlorine pale green gas which bleaches moist litmus paper
bromine brown gas*
iodine purple vapour
water vapour turns blue cobalt chloride paper pink
• When dilute sulfuric or hydrochloric acid is added to a substance a gas may be evolved
or there may be a colour change in the solution.
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6 Tests for oxidizing and reducing agents
Aqueous hydrogen peroxide (H2O2) can act as both an oxidizing and a reducing agent often
with the evolution of oxygen, although this may be unreliable.
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B — Precipitates
When two aqueous solutions are mixed together and an insoluble compound is formed this is
known as a precipitate not a suspension. The observation that a precipitate is formed should
always be accompanied by the colour of the precipitate, even if this is white. Some reagents
should be added until they are in excess. This may result in a precipitate forming then
dissolving in excess reagent.
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2 Ammonia solution
• Dilute aqueous ammonia (NH3), when added to a solution containing a cation, will form
the same hydroxide precipitate as dilute sodium hydroxide solution, eg Mn(OH)2. Excess
aqueous ammonia may dissolve the precipitate to form a complex ion, eg
[Cu(NH3)4(H2O)2]2+.
• Students should assume that aqueous ammonia must be added until it is in excess.
• Aqueous barium chloride forms precipitates of insoluble barium salts with a number of
anions but is usually used as the test for the sulfate, SO42−, ion. Aqueous barium
chloride is usually used with dilute hydrochloric acid.
If dilute hydrochloric acid is added to the anion solution before aqueous barium chloride
then only the sulfate will form as a precipitate.
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4 Silver nitrate solution
• Aqueous silver nitrate is commonly used to test for the presence of halide ions in
solution. Anions which would interfere with the test (eg carbonate) are removed by
adding dilute nitric acid before the aqueous silver nitrate.
• The identity of a halide may be confirmed by the addition of aqueous ammonia, (NH3),
both dilute and concentrated.
• Silver halides which dissolve in ammonia do so to form a colourless solution of the
complex ion, [Ag(NH3)2]+.
• When a few drops of concentrated sulfuric acid (H2SO4) are added to a solid halide the
observed reaction products may be used to identify the particular halide ion present.
This is a potentially hazardous reaction.
• It must be carried out on a small scale and in a fume cupboard.
• The products in brackets will not be observed since they are colourless gases. The
halide ion may be identified without the need to test for these gases. No attempt
should ever be made to detect these gases by smell.
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C — Organic compounds
1 Appearance
Simple organic compounds are usually colourless liquids or white solids. It is unlikely that
appearance alone will provide firm evidence for identification.
2 Solubility
3 Ignition
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4 Chemical tests
The details of how these tests are to be carried out will be included in the instructions to
students in the assessment activities.
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Test Observation Inference
sodium nitrite and dilute hydrochloric orange precipitate aromatic amine
acid followed by an alkaline solution
of phenol in ice-cold conditions
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D — Spectroscopy
1 Mass spectrometry
Simplified mass spectra will be given which may be interpreted in two main ways.
1 The value of the compound’s relative molar mass may be obtained from the m/e value of
M+, the molecular ion. This will have the highest value of m/e. This need not necessarily
be the ‘base’ peak, which is simply the most abundant ion. Questions will be set in such a
way that students will not be confused by the presence of a line due to the (M + 1) ion.
2 The fragmentation pattern of the spectrum gives useful information about the structure of
the molecule. For example, a peak at m/e 29 is likely to be due to the presence of a C2H5
group in the molecule. Students are reminded that, when asked, they should give
displayed structures for fragments, which must carry a positive charge also.
2 Infrared spectroscopy
This is a very powerful non-destructive technique which provides information regarding the
nature of covalent bonds within the molecule.
Students should look at the most intense absorptions to quickly gain structural clues. Table 1
provides sufficient details to enable the principal bands to be assigned. Students should
remember that absorption frequency is affected by the chemical environment and that
absorption may take place outside the range given.
The connection between structures should be recognised. For instance, an alcohol [O-H]
stretch will be accompanied by a [C-O] stretch.
Please see the Data booklet for specific IR spectroscopy data.
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