Documente Academic
Documente Profesional
Documente Cultură
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.
BURETTE: A burette has an accuracy of 0.05 cm^3. The graduations are
after every 0.10 cm^3 but you can read up to an accuracy of 0.05 cm^3. So
the maximum accepted error in the titre is 0.10 cm^3 and that's how close
the two readings we pick should be.
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.
8. Independent on x-axis, dependent is y-axis. Independent is something you
are changing, depending is something you are measuring.
9. LABELLING!!!
10. Not more than 15 minutes on graph!!!
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.
Gas test
1. You should write the OBSERVATION of the confirmatory test whenever
needed. But to save time, you DO NOT need to perform it. Just use your
common sense of chemistry.
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.
2. Ammonia is pungent, very disturbing...sometimes they make you smell it.
YES, they do! Don't forget to use wet red litmus to test ammonia as well. Red
litmus turns into blue because ammonia is a base.
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.
4. You make get confused with droppers. It helps making marks on
them..whatever, don't use same dropper for two solutions. Believe me, it will
affect your results.
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.
7. Use rationally pipette, burette or measuring cylinder.
8. Quote from the syllabus:
"Candidates should normally record burette readings to the nearest
0.05 cm^3 and temperature readings to the nearest 0.5 C when
using thermometer calibrated in 1 C intervals, and to the nearest 0.1
C when the interval is 0.2 C"
9. Talking about errors, an example:
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.
Ex. If I measure a value of 50s using the same stopwatch as mentioned
before with the error 0.005s. Then,
Uncertainty = [(error)/(my measured value)]*100
= [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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Formula Test
Test 1
Heat the solid in a test tube with a
Bunsen burner.
It should decompose producing the
oxide and carbon dioxide. E.g.
Carbonate
CO3
2-
Hydrogencarbonate HCO3-
Sulphate (VI)
SO4
2-
Sulphite
SO32-
Chloride
Cl
Observations
Limewater should
turn from colourless
to cloudy in the
presence of carbon
dioxide due to
precipitation of
calcium carbonate.
Test 2
Add dilute HCl to the solid.
Test for the gas evolved using
limewater solution.
Vigorous
effervescence.
Limewater should
turn from colourless
to cloudy in the
presence of carbon
dioxide due to
precipitation of
calcium carbonate.
Test
Add calcium chloride to a
hydrogencarbonate solution.
No precipitate forms
since calcium
hydrogencarbonate is
soluble.
Test
Add barium chloride solution acidified
with dilute HCl to the test solution.
White precipitate of
barium sulphate
forms.
Test
Warm the sulphite with dilute HCl.
The solution turns
Test for gases using acidified potassium green.
dichromate(VI) solution (or paper)
Test 1
Add concentrated sulphuric acid to the
solid chloride.
Test 2
Add dilute nitric acid to a solution of a
chloride to acidify the solution. This
White precipitate of
eliminates any carbonates or sulphites. AgCl forms.
Add silver nitrate to the solution.
Add dilute ammonia solution.
Solid dissolves.
Test 1
Add concentrated sulphuric acid to the
solid bromide.
Bromide
Br-
Test 2'
Add dilute nitric acid to a solution of a
bromide to acidify the solution. This
Cream precipitate of
eliminates any carbonates or sulphites. AgBr forms.
Add silver nitrate to the solution.
Add concentrated ammonia solution.
Solid dissolves.
Test 1
Add concentrated sulphuric acid to the
solid iodide.
Iodide
Steamy brownish
acidic fumes are
seen.
Test 2
Add dilute nitric acid to a solution of a
iodide to acidify the solution. This
Yellow precipitate of
eliminates any carbonates or sulphites. AgI forms.
Add silver nitrate to the solution.
Solid is insoluble.
Test 1
Heat solid nitrate.
Nitrate
NO3-
Test 2
Boil nitrate solution with
aluminium/Devardas alloy, in sodium
hydroxide solution.
Test vapour with red litmus paper.
Ammonium
NH4+
Test
Warm ammonium compound with
NaOH.
Test vapours immediately using damp
red litmus paper.
NH
3
turns the litmus
paper blue.
Test
Dip nichrome wire in HCl.
Lithium
Li+
Test
Dip nichrome wire in HCl.
Sodium
Na+
A yellow flame is
seen.
K+
Magnesium
Mg2+
Test
Add NaOH solution to the magnesium
solid.
Test
Dip nichrome wire in HCl.
Ca2+
Calcium
Strontium
Barium
Tests of gases:
Name
Formula Test
Observations
Hydrogen
H2
Ignite gas.
Oxygen
O2
Carbon
dioxide
CO2
Ammonia
NH3
litmus paper.
Chlorine
Cl2
Test 1
Test for gas using damp
litmus paper (red or blue)
Test 2
Test for gas using moist
starch-iodide paper.
Test 3
The solution turns from colourless to
Pass gas through a solution of
orange.
a bromide.
Test 4
The solution turns from colourless to
Pass gas through a solution of brown (possibly with a black
an iodide.
precipitate, iodine).
Nitrogen
dioxide
Sulphur
dioxide
NO2
SO2
Test 1
Bubble gas through a solution The solution turns from orange to
of potassium dichromate (VI) green.
dissolved in sulphuric acid.
Test 2
Bubble gas through a solution The solution turns from purple to
of potassium manganate (VII) colourless.
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.
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.
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.
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 isnt really suitable.
Simple distillation:
To separate a volatile solvent from a mixture
Fractional distillation:
To separate mixtures of volatile liquids.
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 arent washed away / dont 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:
Ca2+
Sr2+
Ba2+
Hydroxide solubility:
If sodium hydroxide is added to a solution of a group 2 compound then a precipitate is likely.
Group 2 ion in solution Effect of adding a hydroxide solution
Mg2+
Ca2+
Sr2+
Ba2+
Effect of heat
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.
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.
Vigorous effervescence.
Limewater should turn from
colourless to cloudy in the
presence of carbon dioxide due to
precipitation of calcium carbonate.
Hydrogencarbonate HCO3-
Test
No precipitate forms since calcium
Add calcium chloride to a hydrogencarbonate
hydrogencarbonate is soluble.
solution.
Sulphate (VI)
SO42-
Test
Add barium chloride solution acidified with
dilute HCl to the test solution.
Sulphite
SO
Test
Warm the sulphite with dilute HCl.
Test for gases using acidified potassium
dichromate(VI) solution (or paper)
Test 1
Add concentrated sulphuric acid to the solid
chloride.
Chloride
Cl-
Bromide
Br-
23
Test 2
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
Add concentrated sulphuric acid to the solid
bromide.
Iodide
I-
Test 2'
Add dilute nitric acid to a solution of a
bromide to acidify the solution. This
eliminates any carbonates or sulphites.
Add silver nitrate to the solution.
Add concentrated ammonia solution.
Test 1
Add concentrated sulphuric acid to the solid
iodide.
Solid dissolves.
Test 2
Add dilute nitric acid to a solution of a iodide
to acidify the solution. This eliminates any
Yellow precipitate of AgI forms.
carbonates or sulphites.
Add silver nitrate to the solution.
Solid is insoluble.
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/Devardas Litmus paper turns blue in the
alloy, in sodium hydroxide solution.
presence of ammonia.
Test vapour with red litmus paper.
Ammonium
NH4+
Test
NH
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.
Lithium
Li+
Sodium
Na+
Test
Dip nichrome wire in HCl.
Potassium
K+
Magnesium
Mg2+
Test
Add NaOH solution to the magnesium solid.
Test
Dip nichrome wire in HCl.
Calcium
Ca2+
Test
Dip nichrome wire in HCl.
Strontium
Sr2+
Test
Dip nichrome wire in HCl.
Barium
Ba2+
b) Recognise the chemical tests for simple gases, to include hydrogen, oxygen,
carbon dioxide, ammonia, chlorine, nitrogen dioxide and sulphur dioxide
Tests
Name
Formula Test
Observations
Hydrogen
H2
Ignite gas.
Oxygen
O2
Carbon
dioxide
CO2
Ammonia
NH3
Test 1
Test for gas using damp litmus
Chlorine bleaches the litmus paper very quickly.
paper (red or blue)
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.
Nitrogen
dioxide
Sulphur
dioxide
NO2
Test 4
Pass gas through a solution of
an iodide.
Test 1
Bubble gas through a solution
of potassium dichromate (VI)
dissolved in sulphuric acid.
Test 2
Bubble gas through a solution
of potassium manganate (VII)
dissolved in sulphuric acid.
SO2
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.
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.
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.
Shake the flask vigorously and/or invert the flask 5 or 6 times to create a solution with
uniform concentration.
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.
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)
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).
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.
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).
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.
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 isnt really suitable.
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 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
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.
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
the crystals arent washed away / dont dissolve.
Transfer the crystals to a desiccator to dry. Drying between filter paper is sometimes
recommended, but it is a very poor method.
Organic tests
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
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
organic compounds listed in topic 2.2
Sulphate solubility
If a solution of any sulphate is added to a solution of a group 2 metal compound then a precipitate
is likely.
Mg2+
Ca2+
Sr2+
Ba2+
Hydroxide solubility
If sodium hydroxide is added to a solution of a group 2 compound then a precipitate is likely.
Group 2 ion in solution
Mg2+
Ca2+
Sr2+
Ba2+
Effect of heat
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
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.
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.
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
Chemistry 3B
Sulphate solubility
If a solution of any sulphate is added to a solution of a group 2 metal compound then a precipitate is
likely.
Group 2 ion in
solution
Mg2+
Ca2+
Sr2+
Ba2+
Hydroxide solubility
If sodium hydroxide is added to a solution of a group 2 compound then a precipitate is likely.
Group 2 ion in
solution
Mg2+
Ca2+
Sr2+
Ba2+
Effect of heat
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.
Specification
f) interpret quantitative and qualitative results.
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
tests
Ion
Formu
Test
la
Observations
Test 1
Heat the solid in a test tube with a Bunsen burner.
It should decompose producing the oxide and carbon
dioxide. E.g.
Carbonate
CO32-
Hydrogencarbona
HCO3te
Sulphate (VI)
Sulphite
Chloride
Bromide
Iodide
SO42-
2-
SO3
Cl-
Br-
I-
Vigorous effervescence.
Limewater should turn from colourless
to cloudy in the presence of carbon
dioxide due to precipitation of calcium
carbonate.
Test
Add calcium chloride to a hydrogencarbonate solution.
Test
Add barium chloride solution acidified with dilute HCl to
the test solution.
Test
Warm the sulphite with dilute HCl.
Test for gases using acidified potassium dichromate(VI)
solution (or paper)
Test 1
Add concentrated sulphuric acid to the solid chloride.
Test 2
Add dilute nitric acid to a solution of a chloride to acidify
the solution. This eliminates any carbonates or sulphites.
Add silver chloride to the solution.
Add dilute ammonia solution.
Test 1
Add concentrated sulphuric acid to the solid bromide.
Test 2'
Add dilute nitric acid to a solution of a bromide to acidify
the solution. This eliminates any carbonates or sulphites.
Add silver chloride to the solution.
Add concentrated ammonia solution.
Test 1
Add concentrated sulphuric acid to the solid iodide.
Solid dissolves.
Solid dissolves.
Test 2
Add dilute nitric acid to a solution of a iodide to acidify the
solution. This eliminates any carbonates or sulphites.
Yellow precipitate of AgI forms.
Add silver chloride to the solution.
Solid is insoluble.
Nitrate
NO3-
Test 2
Boil nitrate solution with aluminium/Devardas alloy, in
sodium hydroxide solution.
Test vapour with red litmus paper.
Ammonium
NH4+
NH
Test
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.
Lithium
Li+
Sodium
Na+
K+
Mg2+
Test
Add NaOH solution to the magnesium solid.
Calcium
Ca2+
Test
Strontium
Barium
Tests
Name
Formu
Test
la
Observations
Hydrogen
H2
Ignite gas.
Oxygen
O2
Carbon
dioxide
CO2
Ammonia
NH3
Test 1
Test for gas using damp litmus paper (red or Chlorine bleaches the litmus paper very quickly.
blue)
Chlorine
Cl2
Test 2
The paper turns blue-black.
Test for gas using moist starch-iodide paper.
Test 3
Pass gas through a solution of a bromide.
Test 4
Pass gas through a solution of an iodide.
Nitrogen
dioxide
Sulphur
dioxide
NO2
SO2
Test 1
Bubble gas through a solution of potassium The solution turns from orange to green.
dichromate (VI) dissolved in sulphuric acid.
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.
Make sure that the balance is clean and dry. Wipe it with a damp cloth.
Place the weighing bottle on the pan and tare 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.
When you have the required amount, write its value down immediately.
Replace on balance, and if the required amount is added, withdraw the mass.
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.
Add about 100cm3 of distilled water to the flask.
Stir the solution using a glass rod.
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.
Stopper the flask.
Shake the flask vigorously and/or invert the flask 5 or 6 times to dissolve the solid.
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.
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
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
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.
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 isnt really suitable.
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 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.
Organic tests
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)
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
5.31 4.18 T
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 (dil)HNO and 1moldm (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
CO O H
1
1
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
C
C H
C H
CO
CH
(1 )
(2 )
O H H
O
H
(b) H
(c)Structural formula for X?(c) H
X must be a secondary alcohol because ketone formed on oxidation carboxylic acid is not formed
(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
(3)(a)Write an ionic equation for the hydrolysis of 1-bromobutane by water
M a ss lo s s /g
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
50cm of 1moldm
2
Small pieces
3
3
50cm of 1moldm heated to
1 .0 0
E x p t.
80C
3 RT
One large
3
3
50cm of 1moldm
piece
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 , 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 theres 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)
Sulphur dioxide
Cation
Ammonium
SO2
NH4+
H+
Copper(II) Cu2+
Iron(II)
Fe2+
Iron(III)
Fe3+
Calcium
Ca2+
Magnesium
Mg2+
Aluminium
Al3+
Lead
Pb2+
Zinc
Zn2+
Anion
Carbonate pH>10
CO32
universal indicator
Hydrogen carbonate HCO3
pH 8-9
Chloride
Cl
Bromide
Br
Iodide
Nitrate
NO3
Sulphate
SO42
Sulphite
SO32
In excess, insoluble
In excess, insoluble
A little, brown ppt forms
A little, brown ppt forms
In excess, insoluble
In excess, insoluble
A little, milky suspension forms
A little, milky suspension forms
In excess, insoluble
In excess, insoluble
Distinguish Mg from Ca through flame test
A little, milky suspension forms
A little, milky suspension forms
In excess, insoluble
In excess, insoluble
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
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
A little, white ppt forms
A little, white ppt forms
In excess, dissolves giving colourless solution
In excess, dissolves giving colourless solution
Test
Add (dil)HCl(aq)
Pass gas through lime water, CO2 evolved turning lime water milky
Or add group II ions, white ppt or heat/add boiling water, no gas evolved
Add (dil)HCl(aq)
Pass gas through lime water, CO2 evolved turning lime water milky
Or add metal ions
no ppt but heating causes white ppt to form or Heat/add boiling water, CO2 evolved
Acidify with (dil)HNO3(aq)
Add AgNO3(aq)
Add (dil)NH3 to ppt
White ppt AgCl forms Ppt dissolves leaving colourless solution
Acidify with (dil)HNO3(aq)
Add AgNO3(aq)
Add (conc)NH3 to ppt
Cream ppt AgBr forms Ppt dissolves leaving colourless solution
Acidify with (dil)HNO3(aq)
Add AgNO3(aq)
Add (conc)NH3 to ppt
Yellow ppt AgBr forms Ppt insoluble
Add NaOH(aq) Add Devardas alloy (powdered Zn, Al)
Heat & hold moist red litmus at mouth of test tube
NH3 evolved, litmus paper red blue
Add Barium nitrate Ba(NO3)2(aq)/chloride BaCl2(aq) Add HCl(aq)
White ppt
Insoluble
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
Edexcel, a Pearson company, is the UKs 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
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Authorised by Roger Beard
Prepared by Sarah Harrison
All the material in this publication is copyright
Edexcel Limited 2008
Contents
Introduction
1.1 Activities
3.1 Accuracy
3.2 Errors
3.3 Calculations
3.4 Graphs
4 Activity d: Preparation
11
12
Reference section
13
13
Appearance
13
Flame tests
14
Heating
14
15
15
16
16
B Precipitates
17
17
Ammonia solution
18
18
19
19
C Organic compounds
20
Appearance
20
Solubility
20
Ignition
20
Chemical tests
21
D Spectroscopy
23
Mass spectrometry
23
Infrared spectroscopy
23
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.
User guide (Internal Assessment of Practical Skills) Edexcel AS/A GCE in Chemistry (8CH01/9CH01)
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1.1
Activities
At both AS and A2 Level the skills being assessed in the activities are:
a
(verification)
Qualitative observation
(14 marks)
Quantitative measurement
(14 marks)
Preparation
(12 marks)
1.2
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
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.
1.4
Students must follow the health and safety rules which normally operate in their chemistry
laboratories, including the following:
HazChem labels (eg flammable) should be read and appropriate precautions (eg keep
liquid away from flame) taken
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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2.1
Recording observations
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.
Possible change
Example of observation
a gas is evolved
tests on a gas
flame tests
yellow flame
a solid dissolves
a reaction is exothermic
a reaction is endothermic
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.
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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.
2.2
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
2,4dinitrophenylhydrazine. 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
2,4dinitrophenylhydrazine 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 2,4dinitrophenylhydrazine test.
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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.
Apparatus
Precision of reading
pipette
burette
measuring cylinder
balance
timers
thermometers
When students record readings they should include the appropriate number of decimal
places. For example a burette reading of exactly 24.7 cm3 should be recorded in a results
table as 24.70 cm3.
When titres have to be averaged, the mean should be expressed to either the nearest
0.05 cm3 or to the second decimal place. Eg if a student records four titres as listed below
the mean should be calculated as:
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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 H value may involve a weighing of 1.56 g and
a temperature rise of 7.5C. A student who calculates a value of H from these figures
may obtain a value of 195.6843 on a calculator but this should be finally recorded as 200
kJ mol1, although 196 kJ mol1 may also be acceptable.
A significant proportion of the marks awarded for a quantitative measurement activity will be
for accuracy. These marks will be awarded by comparing the students 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
The following points will apply.
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.
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.
8
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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 yaxis.
And the pre-determined quantity (eg volume of solution) on the xaxis.
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 21.0C and 39.0C are to be plotted there is
no need to begin the yaxis at 0. Rather it could be scaled from 20.0C to 40.0C.
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.
3.5
The instructions for carrying out a quantitative measurement activity will include the essential
points for the particular task. For example:
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
conical flasks and volumetric flasks should be rinsed out with distilled water
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
10
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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
solvent extraction
drying
Following some preparations students will be asked to calculate the maximum mass of product
and a percentage yield.
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11
12
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Reference section
blue
copper(II)
pale green
iron(II)
green
purple
manganate(VII)
brown
iron(III)
pink
manganese(II)
yellow
chromate(VI)
orange
dichromate(VI)
The colours of transition metal ions in dilute, aqueous solution are shown in the table
below.
Colour
Possible identity
blue
copper(II)
green
brown / yellow
iron(III)
pale pink
manganese(II)
yellow
chromate(VI)
orange
dichromate(VI)
purple
manganate(VII)
colourless
zinc(II)
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13
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.
Flame colour
Inference
yellow
sodium ion
lilac
potassium ion
yellow-red*
calcium ion
red*
pale green
barium ion
3 Heating
14
Possible source
carbon dioxide
oxygen
water
hydrated salts
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Gas
Observations
oxygen
carbon dioxide
ammonia
colourless gas which turns moist red litmus paper blue and
forms white smoke with hydrogen chloride
nitrogen dioxide
brown gas*
hydrogen
hydrogen chloride
chlorine
bromine
brown gas*
iodine
purple vapour
water vapour
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.
Action of acid
Possible source
carbonate
hydrogen evolved
a metal
chromate(VI) to dichromate(VI)
thiosulfate
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15
16
Inference
brown precipitate
chromium(III) to chromate(VI)
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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.
Students should assume that aqueous sodium hydroxide should be added until it is in
excess even if this is not explicitly stated in the instructions.
Observation on adding
excess dilute NaOH
Likely ion
green precipitate
precipitate dissolves to a
green solution
chromium(III)
precipitate is insoluble
manganese(II)
precipitate is insoluble
iron(II)
brown precipitate
precipitate is insoluble
iron(III)
green precipitate
precipitate is insoluble
nickel(II)
blue precipitate
precipitate is insoluble
copper(II)
white precipitate
precipitate dissolves to a
colourless solution
zinc(II)
white precipitate
precipitate is insoluble
magnesium, barium,
strontium, calcium
no precipitate
sodium, potassium
ammonium
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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.
Likely ion
green precipitate
chromium(III)
off-white precipitate
precipitate is insoluble
manganese(II)
precipitate insoluble
iron(II)
brown precipitate
precipitate insoluble
iron(III)
green precipitate
nickel(II)
blue precipitate
copper(II)
white precipitate
zinc(II)
white precipitate
precipitate is insoluble
magnesium
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.
Anion
Precipitate
colour
formula
sulfate
white
BaSO4
precipitate is insoluble
sulfite
white
BaSO3
precipitate dissolves
carbonate
white
BaCO3
If dilute hydrochloric acid is added to the anion solution before aqueous barium chloride
then only the sulfate will form as a precipitate.
18
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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.
Precipitate
colour
formula
dilute
concentrated
chloride
white
AgCl
soluble
bromide
cream
AgBr
soluble in excess
soluble
iodide
yellow
AgI
insoluble
insoluble
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.
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.
Halide
Observations on adding
concentrated H2SO4
Observed reaction
products
chloride
HCl
bromide
iodide
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C Organic compounds
Students will always be told if a compound, or mixture of compounds, to be identified is
organic. Often the molecular formula, or the number of carbon atoms in a molecule, of a
compound will be given. Chemical tests may be followed by spectroscopic information.
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
Solubility of compound
Possible identity
pH of
solution
Possible
identity
dissolve in water
above 7
amines
below 7
carboxylic
acids,
phenols
amines
dissolve in aqueous
alkali but may not
dissolve in water
3 Ignition
Igniting an organic unknown on a crucible lid may help in identifying it.
20
Observation
Possible inferences
no residue
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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.
Test
Observation
Inference
orange to green
solution
primary or secondary
alcohol, aldehyde
yellow solution is
decolorised
alkene
if white
precipitate also
formed
phenol
precipitate:
halogenoalkanes:
white
CCl
cream
CBr
yellow
CI
phosphorus(V) chloride
steamy fumes of
HCl that turn damp
blue litmus paper
red
OH group in alcohols
and carboxylic acids
2,4dinitrophenylhydrazine solution
orange precipitate
C=O group in
aldehydes and
ketones
aldehyde
silver mirror
aldehyde
effervescence
carboxylic acid
effervescence
(bubbles), sodium
dissolves, white
solid formed
alcohol, phenol or
carboxylic acid
ester smell, eg
glue-like
alcohol
(Tollens reagent)
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21
Test
Observation
Inference
orange precipitate
aromatic amine
pale yellow
precipitate
methyl ketone or
ethanal,
C CH3
O
methyl secondary
alcohol or ethanol
CH CH3
OH
22
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D Spectroscopy
Modern instrumentation plays a vital role in the characterisation and identification of
molecules and ions. The sections which follow will enable interpretation of the data likely to
be presented to students.
1 Mass spectrometry
Simplified mass spectra will be given which may be interpreted in two main ways.
1
The value of the compounds 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.
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.
1714sb130508S:\LT\PD\Support\GCE in Chemistry Intrnl Asst of Practical Skills User guide Issue 2.doc.1-28/1
User guide (Internal Assessment of Practical Skills) Edexcel AS/A GCE in Chemistry (8CH01/9CH01)
Issue 2 May 2008 Edexcel Limited 2008
23
May 2008
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