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Unit_3_core_practical_reference

This practical guide provides essential information on core practicals for A-level chemistry, including safety measures, gas volume measurement techniques, and methods for determining enthalpy changes using Hess's Law. It outlines detailed experimental procedures for measuring gas volumes, heating substances in a crucible, and calculating enthalpy changes through calorimetric methods. The guide emphasizes the importance of accuracy, proper technique, and understanding potential errors in experiments.

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0% found this document useful (0 votes)
14 views24 pages

Unit_3_core_practical_reference

This practical guide provides essential information on core practicals for A-level chemistry, including safety measures, gas volume measurement techniques, and methods for determining enthalpy changes using Hess's Law. It outlines detailed experimental procedures for measuring gas volumes, heating substances in a crucible, and calculating enthalpy changes through calorimetric methods. The guide emphasizes the importance of accuracy, proper technique, and understanding potential errors in experiments.

Uploaded by

Yam Yam
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
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Reference material - Practical Guide International EDEXCEL

This guide includes details about the core practicals for A-level chemistry. It also contains information about
other experiments that often occur in A-level examinations. You may be asked to describe these experiments
in details or be asked about reasons for doing individual steps.
You may be asked about other unfamiliar experiments but these will be using the skills and techniques that
are described in the following experiments.

Safety and hazards


Irritant - dilute acid and alkalis- wear googles Hazardous substances in low
Corrosive- stronger acids and alkalis wear goggles concentrations or amounts
Flammable – keep away from naked flames will not pose the same risks as
Toxic – wear gloves- avoid skin contact- wash hands after use the pure substance.
Oxidising- Keep away from flammable / easily oxidised materials

Measuring gas volumes


Using a gas syringe Make sure you don’t leave gaps in
your diagram where gas could
Gas syringes can be used for a variety of escape
experiments where the volume of a gas
is measured, possibly to work out moles
of gas or to follow reaction rates.

Potential errors in using a gas


syringe •gas escapes before bung If drawing a gas syringe make
inserted •syringe sticks sure you draw it with some
• some gases like carbon dioxide or sulphur dioxide measurement markings on the
are soluble in water so the true amount of gas is not barrel to show measurements can
measured. be made.

Alternatively gas volumes can be measured


The volume of a gas depends on pressure
and temperature so when recording ‘over water’ with an up-turned measuring
volume it is important to note down the cylinder in a trough of water
temperature and pressure of the room.

Moles of gas can be calculated from gas


volume (and temperature and pressure)
using ideal gas equation PV = nRT or using
the molar gas volume (1mol gas =24dm3
at room temperature and pressure

CHSE/Unit 3- Alternative practical reference notes for core practical’s /2020 Page 1 of 24
Core Practical 1:Measure the molar volume of a gas
Detailed method

1. Measure 30 cm3 of 1 mol dm⁻3 ethanoic acid and transfer to a


conical flask.
2. Attach conical flask to gas syringe or use collection
over water method (see previous page)
3. Measure the mass of a weighing bottle with

Volume of CO2 in cm3


approximately 0.05 g of calcium carbonate
4. Add the calcium carbonate to the conical flask-
quickly resealing the bung so no gas escapes
5. Measure the final total volume of gas
6. Reweigh the empty weighing bottle test tube from step 3
7. Repeat the experiment several more times, increasing the mass of
calcium carbonate by about 0.05 g each time.

Mass of CaCO3 in g

Analysis
From the graph read the volume of CO2 given off with 0.25 g CaCO3
Work out the moles of CaCO3 in 0.25g = 0.25/100.1 = 2.5 x 10-
3 Assume the moles of CO2 = moles of CaCO3

Work out molar volume of CO2 = volume of CO2/ moles of CO2

Method for using a gas syringe to calculate the Mr of propanone


1. Extract 0.20 cm3 of propanone into a hypodermic syringe and then measure the mass of this syringe
2. using hand protection, remove a gas syringe from the oven and note the volume of air already in
the barrel – about 5 cm3.
3. inject the propanone through the self-seal cap into the barrel. The plunger will move straight away.
4. Put the gas syringe back into the oven.
5. Measure the mass of the empty hypodermic syringe immediately.
6. After a few minutes measure the volume of the gas in the gas syringe, record the temperature of the
oven shelf and the pressure of the room.

Example 1 : 0.150g of a volatile liquid was injected into a sealed gas syringe. The gas syringe was placed in an oven at
70oC at a pressure of 100kPa and a volume of 80cm3 was measured. Calculate the Mr of the volatile liquid (R = 8.31)
moles = PV/RT 100 kPa = 100 000 Pa
= 100 000 x 0.00008 / (8.31 x 343) 80 cm3 = 0.00008 m3
= 0.00281 mol
Mr = mass/moles
= 0.15 / 0.00281
= 53.4 g mol-1

CHSE/Unit 3- Alternative practical reference notes for core practical’s /2020 Page 2 of 24
Heating in a crucible This method could be used for measuring mass loss in various
thermal decomposition reactions and also for mass gain
when reacting magnesium in oxygen.

The lid improves the accuracy of the


The water of crystallisation in calcium sulfate crystals can be experiment as it prevents loss of
removed as water vapour by heating as shown in the following solid from the crucible but should be
equation. CaSO4.xH2O(s) → CaSO4(s) + xH2O(g) loose fitting to allow gas to escape.
Method.
•Weigh an empty clean dry crucible and lid .
•Add 2g of hydrated calcium sulfate to the crucible and weigh
again •Heat strongly with a Bunsen for a couple of minutes •Allow
to cool
•Weigh the crucible and contents again
•Heat crucible again and reweigh until you reach a constant mass (
do this to ensure reaction is complete).

Large amounts of hydrated calcium sulfate, such as 50g,


should not be used in this experiment as the decomposition
is likely to be incomplete. Small amounts of the solid , such as
0.100 g, should not be used in this
The crucible needs to be dry otherwise a wet crucible experiment as the percentage
would give an inaccurate result. It would cause mass loss to uncertainties in weighing will be
be too large as the water would be lost when heating. too high.

Example 2. 3.51 g of hydrated zinc sulfate were heated and 1.97 g of anhydrous zinc sulfate were
obtained. Use these data to calculate the value of the integer x in ZnSO4.xH2O
Calculate the mass of H2O = 3.51 – 1.97 = 1.54g

Calculate moles of = 1.97 Calculate moles of = 1.54


ZnSO4 161.5 H 2O 18
= 0.0122 =0.085
Calculate ratio of mole of = 0.0122 = 0.085
ZnSO4 to H2O 0.0122 0.0122
=1 =7
X=7

CHSE/Unit 3- Alternative practical reference notes for core practical’s /2020 Page 3 of 24
CORE PRACTICAL 2: To determine the enthalpy change of a reaction using Hess’s Law
Measuring the Enthalpy Change for a Reaction

Experimentally Calorimetric method This equation will only give the


energy for the actual quantities
For a reaction in solution we use the following equation used. Normally this value is
converted into the energy
energy change = mass of solution x heat capacity x temperature change
change per mole of one of the
Q (J) = m (g) x cp (J g-1K-1) x T ( K) reactants. (The enthalpy change
of reaction, H)

Calorimetric method

One type of experiment is one in which substances are mixed This could be a solid dissolving or reacting in
in an insulated container and the temperature rise measured. a solution or it could be two solutions
reacting together

General method
• washes the equipment (cup and pipettes etc) with the solutions to be used
• dry the cup after washing
• put polystyrene cup in a beaker for insulation and support
• Measure out desired volumes of solutions with volumetric pipettes and transfer
to insulated cup
• clamp thermometer into place making sure the thermometer bulb is immersed
in solution
• measure the initial temperatures of the solution or both solutions if 2 are used. Do
this every minute for 2-3 minutes
• At minute 3 transfer second reagent to cup. If a solid reagent is used then add
the solution to the cup first and then add the solid weighed out on a balance.
• If using a solid reagent then use ‘before and after’ weighing method
• stirs mixture (ensures that all of the solution is at the same temperature)
• Record temperature every minute after addition for several minutes

If the reaction is slow then the exact temperature rise can


be difficult to obtain as cooling occurs simultaneously with
the reaction

To counteract this we take readings at regular time intervals


and extrapolate the temperature curve/line back to the time
the reactants were added together.

We also take the temperature of the reactants for a few


minutes before they are added together to get a better average
temperature. If the two reactants are solutions then the
temperature of both solutions need to be measured before
addition and an average temperature is used.

Errors in this method Read question carefully. It


may be necessary to
• energy transfer from surroundings (usually loss)
describe:
• approximation in specific heat capacity of solution. The method assumes all
• Method
solutions have the heat capacity of water.
• Drawing of graph with
• neglecting the specific heat capacity of the calorimeter- we ignore any energy
extrapolation
absorbed by the apparatus.
• Description of the
• reaction or dissolving may be incomplete or slow.
calculation
• Density of solution is taken to be the same as water.

CHSE/Unit 3- Alternative practical reference notes for core practical’s /2020 Page 4 of 24
Calculating the enthalpy change of reaction, Hr from experimental data
The heat capacity of water is 4.18 J
General method g-1K-1. In any reaction where the
reactants are dissolved in water
1. Using q= m x cp x T calculate energy change for quantities used we assume that the heat capacity
is the same as pure water.
2. Work out the moles of the reactants used
3. Divide q by the number of moles of the reactant not in excess to give H Also assume that the solutions have
-1 -1 the density of water, which is 1g cm-
4. Add a sign and unit (divide by a thousand to convert Jmol to kJmol 3. Eg 25cm3 will weigh 25 g

Example 3. Calculate the enthalpy change of reaction for the reaction where 25.0cm3 of 0.20M
copper sulfate was reacted with 0.01mol (excess of zinc). The temperature increased 7.0 oC .

Step 1: Calculate the energy change for the amount of reactants in the calorimeter.

Q = m x cp x T Note the mass is the mass of the copper sulfate


Q = 25 x 4.18 x 7 solution only. Do not include mass of zinc powder.
Q = 731.5 J
Step 2 : calculate the number of moles of the reactant not in excess.

moles of CuSO4 = conc x vol If you are not told what is in excess, then you need to work
= 0.2 x 25/1000 out the moles of both reactants and work out using the
= 0.005 mol balanced equation which one is in excess.

Step 3 : calculate the enthalpy change per mole, H (the enthalpy change of
reaction) H = Q/ no of moles
= 731.5/0.005
= 146300 J mol-1
= 146 kJ mol-1 to 3 sf
Remember in these
Finally add in the sign to represent the energy change: if temp increases questions: sign, unit
the reaction is exothermic and is given a minus sign e.g. –146 kJ mol-1

Example 4. 25.0cm3 of 2.0 mol dm-3 HCl was neutralised by 25.0cm3 of 2.0 mol dm-3 NaOH. The
temperature increased 13.5oC. Calculate the enthalpy change per mole of HCl?
Step 1: Calculate the energy change for the amount of reactants in the test tube.
Q = m x cp x T
Note the mass equals the mass of acid + the
Q = 50 x 4.18 x13.5
mass of alkali, as they are both solutions.
Q = 2821.5 J

Step 2 : calculate the number of moles of the HCl.


moles of HCl = conc x vol
= 2 x 25/1000
= 0. 05 mol

Step 3 : calculate H the enthalpy change per mole which can be called the enthalpy change of neutralisation
H = Q/ no of moles
= 2821.5/0.05
Remember in these
= 56430 J mol-1 Exothermic and so is given a minus sign questions: sign, unit,
= -56.4 kJ mol-1 to 3 sf

CHSE/Unit 3- Alternative practical reference notes for core practical’s /2020 Page 5 of 24
Often Hess’s law cycles are used to measure the enthalpy change for a reaction that cannot be measured directly
by experiments. Instead alternative reactions are carried out that can be measured experimentally.

H reaction This Hess’s law is used to work out the


enthalpy change to form a hydrated salt from
CuSO4 (s) + 5H2O (l) CuSO4.5H2O (s) an anhydrous salt.

+ aq + aq This cannot be done experimentally because it


-66.1 kJ mol-1 +11kJ mol-1
is impossible to add the exact amount of water
CuSO4 (aq) without the solid dissolving and it is not easy
to measure the temperature change of a solid.

H reaction + 11kJmol-1 = -66.1 kJ mol-1 Instead both salts are dissolved in excess
H reaction= -66.1 - 11 water to form a solution of copper sulfate. The
-1 temperature changes can be measured for
= -77.1 kJ mol these reactions.

Detailed method for measuring enthalpy change of solution of anhydrous copper(II) sulfate
1. Weigh out between 3.90 g and 4.10 g of anhydrous copper(II) sulfate in a dry weighing bottle. The precise
mass should be recorded.
2. Using a volumetric pipette, place 25 cm3 of deionised water into a polystyrene cup and record its temperature at the
beginning (t=0), start the timer and then record the temperature again every minute, stirring the liquid continuously.
3. At the fourth minute, add the powdered anhydrous copper(II) sulfate rapidly to the water in the polystyrene cup
and continue to stir, but do not record the temperature.
4. Reweigh the empty weighing bottle
5. At the fifth minute and for every minute up to 15 minutes, stir and record the temperature of the solution in
the polystyrene cup.
6. Plot a graph of temperature (on the y-axis) against time. Draw two separate best fit lines; one, which joins the points
before the addition, and one, which joins the points after the addition, extrapolating both lines to the fourth minute.
7. Use your graph to determine the temperature change at the fourth minute, which theoretically should
have occurred immediately on addition of the solid.
8. Using q= m x cp x T calculate energy change
= 20 x 4.18 x T
9. Calculate Hsolution by dividing q by number of moles of anhydrous copper(II) sulfate in mass added

The above method is then repeated using hydrated copper sulfate. The two Hsolution can then be used to
calculate the H for the enthalpy change of forming a hydrated salt as in the example above

CHSE/Unit 3- Alternative practical reference notes for core practical’s /2020 Page 6 of 24
Measuring Enthalpies of Combustion using Flame Calorimetry

Enthalpies of combustion can be calculated by using calorimetry.


Generally the fuel is burnt and the flame is used to heat up water in
a metal cup.
Need to measure
• mass of spirit burner before and after
• Temperature change of water
• Volume of water in cup

Errors in this method


• energy losses from calorimeter
• Incomplete combustion of fuel
• Incomplete transfer of energy
• Evaporation of fuel after weighing
• Heat capacity of calorimeter not included
• Measurements not carried out under standard conditions as H 2O
is gas, not liquid, in this experiment

Example 5. Calculate the enthalpy change of combustion for the reaction where 0.65g of propan-1-ol
was completely combusted and used to heat up 150g of water from 20.1 to 45.5 oC
Step 1: Calculate the energy change used to heat up the water.

Q = m x cp x T
Note the mass in this equation is the mass of water in
Q = 150 x 4.18 x 25.4
the calorimeter and not the alcohol
Q = 15925.8 J

Step 2 : calculate the number of moles of alcohol combusted.

moles of propan-1-ol = mass/ Mr


= 0.65 / 60
= 0.01083 mol

Step 3 : calculate the enthalpy change per mole which is called cH (the enthalpy change of combustion)
H = Q/ no of moles
= 15925.8/0.01083
= 1470073 J mol-1
= 1470 kJ mol-1 to 3 sf
Remember in these
Finally add in the sign to represent the energy change: if temp increases
questions: sign, unit
the reaction is exothermic and is given a minus sign eg –1470 kJ mol-1

CHSE/Unit 3- Alternative practical reference notes for core practical’s /2020 Page 7 of 24
Core practical 3+4. Make up a volumetric solution and carry out a simple acid–base titration

Making a solution

• Weigh the sample bottle containing the required mass of Alternatively the known mass of solid
solid on a 2 dp balance in the weighing bottle could be
• Transfer to beaker transferred to beaker, washed and
• Reweigh empty sample bottle
washings added to the beaker.
• Record the difference in mass

• Add 100cm3 of distilled water to the beaker. Use a glass rod


to stir to help dissolve the solid.

•Sometimes the substance may not dissolve well in cold water


so the beaker and its contents could be heated gently until all
the solid had dissolved.
Remember to fill so the bottom of the
• Pour solution into a 250cm3 graduated flask via a funnel. meniscus sits on the line on the neck of
• Rinse beaker and funnel and add washings from the the flask. With dark liquids like potassium
beaker and glass rod to the volumetric flask. manganate it can be difficult to see the
• make up to the mark with distilled water using a meniscus.
dropping pipette for last few drops.
• Invert flask several times to ensure uniform solution. Shake the volumetric flask thoroughly
to ensure a uniform concentration

A graduated flask has one mark on the neck which the level to fill
to get the accurate volume. Do not heat or put hot solutions in
the volumetric flask because the heat would cause the flask to
expand and the volume would then be incorrect.

Measuring mass accurately:


In many experiments the best method for measuring mass is
1. Measure mass on 2 or 3d.p. balance of a weighing bottle
with the required quantity of solid in it
2. Empty mass into reaction vessel/flask
3. Reweigh the now empty weighing bottle
4. Subtract the mass of the empty weighing bottle from the
Graduated/volumetric flask first reading to give exact of mass actually added.

Dilutions

Diluting a solution
Using a volumetric pipette is more accurate
than a measuring cylinder because it has a
•Pipette 25cm3 of original solution into a 250cm3 smaller uncertainty
volumetric flask
•make up to the mark with distilled water using a Use a teat pipette to make up to the mark in
dropping pipette for last few drops. volumetric flask to ensure volume of solution
• Invert flask several times to ensure uniform solution. accurately measured and one doesn’t go
over the line

CHSE/Unit 3- Alternative practical reference notes for core practical’s /2020 Page 8 of 24
Titrations Core Practical 3+4: Make up a volumetric solution and carry out a simple acid–base titration

General Method
•rinse equipment (burette with acid, pipette with alkali, conical flask with distilled water)
•pipette 25 cm3 of alkali into conical flask
•touch surface of alkali with pipette ( to ensure correct amount is added)
•adds acid solution from burette
•make sure the jet space in the burette is filled with acid
•add a few drops of indicator and refer to colour change at end point
•phenolphthalein [pink (alkali) to colourless (acid): end point pink colour just disappears] [use if NaOH is used]
•methyl orange [yellow (alkali) to red (acid): end point orange] [use if HCl is used]
•use a white tile underneath the flask to help observe the colour change
•add acid to alkali whilst swirling the mixture and add acid drop wise at end point
•note burette reading before and after addition of acid
•repeats titration until at least 2 concordant results are obtained- two readings within 0.1 of each other

Titrations are done often to find out the concentration of


one substance by reacting it with another substance of
known concentration.
They are often done with neutralisation reactions, but can be
done with redox reactions. burette

One substance (generally the one we don’t know the


concentration) is put in the conical flask. It is measured
using a volumetric pipette. conical
The other substance is placed in the burette flask

However, the standard phrase: titrate solution A


with solution B means that A should be in the
conical flask and B should be in the burette.

A conical flask is used in preference to a beaker because


it is easier to swirl the mixture in a conical flask without
spilling the contents.
pipette

Detailed Method for Titration Make sure bottom of


Using the pipette meniscus is on line on
neck of pipette

•rinse pipette with substance to go in it (often alkali).


•pipette 25 cm3 of solution A into conical flask. The
volumetric pipette will have a mark on its neck to show
the level to fill to. The bottom of the meniscus should
sit on this line.
•touch surface of solution with pipette ( to ensure
correct amount is added). A small amount of solution
will be left in the pipette at this stage. The calibration
of the pipette will take into account this effect. It
should not be forced out.

CHSE/Unit 3- Alternative practical reference notes for core practical’s /2020 Page 9 of 24
Using the burette
The burette should be rinsed out with substance that will be
put in it. If it is not rinsed out the acid or alkali added may be
diluted by residual water in the burette or may react with
substances left from a previous titration. This would lead to
the concentration of the substance being lowered and a
larger titre being delivered.

Don’t leave the funnel in the burette because small drops of


liquid may fall from the funnel during the titration leading to
a false burette reading (would give a lower titre volume)

make sure the jet space in the burette is filled with the
solution and air bubbles are removed.

If the jet space in the burette is not filled properly prior to commencing
the titration it will lead to errors if it then fills during the titration, leading
to a larger than expected titre reading.

Read the bottom of the meniscus on the burette

This is reading 9.00cm3


Even though a burette has marking reading to 0.1cm3, the burette readings
should always be given to 2dp either ending in 0.00 or 0.05. 0.05cm3 is the
volume of 1 drop of solution delivered from a burette and so this is the
smallest difference in readings that can be measured. If the bottom of the
meniscus sits on a line it should end with a 0.00 as in the above example
9.00cm3. If the meniscus sits between two lines it should end 0.05. e.g. if the
bottom of the meniscus sits between the lines marked 9.1 and 9.2, you
should record 9.15

Adding indicator
Indicators are generally weak acids so only add a
Add a few drops of indicator and refer to colour few drops of them. If too much is added they will
change at end point affect the titration result
phenolphthalein Methyl orange
If acid is added from the burette the colour change would
Methyl orange is a suitable indicator for neutralisation
be pink (alkali) to colourless (acid): end point pink colour
reactions where strong acids are used.
just disappears [use with titrations using strong alkalis
It is red in acid and yellow in alkali. It is orange at the
e.g. NaOH ]
end point.

Methyl orange
Methyl orange Methyl orange
Alkali colour
phenolphthalein phenolphthalein acid end point acid colour
Alkali colour colour Use a white tile underneath the flask to
help observe the colour change

CHSE/Unit 3- Alternative practical reference notes for core practical’s /2020 Page 10 of 24
Add solution from burette whilst swirling the mixture and add drop-wise at end
point

Distilled water can be added to the conical flask during a titration to wash
the sides of the flask so that all the acid on the side is washed into the
reaction mixture to react with the alkali.
It does not affect the titration reading as water does not react with the
reagents or change the number of moles of acid added.

note burette reading before and after addition of solution


Only distilled water should be used to
repeats titration until at least 2 concordant results wash out conical flasks between
are obtained- two readings within 0.1 of each other titrations because it does not add any
extra moles of reagents
A single titration could be flawed. Repeating allows
for anomalous titres to be spotted and discounted
lf 2 or 3 values are within 0.10cm3 and
therefore concordant or close then we
Recording results can say results are accurate and
•Results should be clearly recorded in a table repeatable and the titration technique
•Result should be recorded in full (i.e. both initial and final readings) is good and consistent
•Record titre volumes to 2dp (0.05 cm3)

Working out average titre results


Only make an average of
Titration number 1 2 3
the concordant titre results

Initial burette reading (cm3 ) 0.50 2.50 1.55 Average titre = (24.50+ 24.40)/2
= 24.45
Final burette reading (cm3 ) 24.50 27.00 25.95

Titre (cm3 ) 24.00 24.50 24.40

Safety precautions
Common Titration Equations
Acids and alkalis are corrosive CH3CO2H + NaOH → CH3CO2-Na+ + H2O
(at low concentrations acids are irritants)
Wear eye protection and gloves H2SO4 + 2NaOH → Na2SO4 +2H2O
If spilled immediately wash affected parts after spillage HCl + NaOH → NaCl +H2O
NaHCO3 + HCl → NaCl + CO2 + H2O
If substance is unknown treat it as potentially toxic and
wear gloves. Na2CO3 + 2HCl →2NaCl + CO2 + H2O

Titrating mixtures
Testing batches If titrating a mixture to work out the concentration
In quality control it will be necessary to do titrations/testing of an active ingredient it is necessary to consider if
on several samples as the amount/concentration of the the mixture contains other substances that have acid
chemical being tested may vary between samples. base properties.
If they don’t have acid base properties we can
titrate with confidence.

CHSE/Unit 3- Alternative practical reference notes for core practical’s /2020 Page 11 of 24
Uncertainty
Readings and Measurements
Readings Measurements In general, if uncertainty is not indicated
the values found from a single the values taken as the on apparatus, the following assumptions
judgement when using a piece difference between the are made:
of equipment judgements of two values For an analogue scale-
(e.g. using a burette in a The uncertainty of a reading (one
titration) judgement) is at least ± 0.5 of the smallest
scale reading.
Calculating Apparatus Uncertainties
The uncertainty of a measurement (two
Each type of apparatus has a sensitivity uncertainty
judgements) is at least ± 1 of the smallest
•balance  0.001 g (if using a 3 d.p. balance) scale reading.
•volumetric flask  0.1 cm3 - If the apparatus has a digital scale, the
•25 cm3 pipette  0.1 cm3 uncertainty is  the resolution of the

•burette (start & end readings and end point )  0.15 cm3 apparatus in each measurement
Calculate the percentage error for each piece of equipment used by
Uncertainty of a measurement using
% uncertainty =  uncertainty x 100 a burette. If the burette used in the
Measurement made on apparatus titration had an uncertainty for each
reading of +/– 0.05 cm3 then during a
e.g. for burette titration two readings would be taken
% uncertainty = 0.15/average titre result x100 so the uncertainty on the titre volume
would be +/– 0.10 cm3 .
To calculate the maximum total percentage apparatus uncertainty in the
final result add all the individual equipment uncertainties together.

Reducing uncertainties in a titration To decrease the apparatus uncertainties


you can either decrease the sensitivity
Replacing measuring cylinders with pipettes or burettes which have uncertainty by using apparatus with a
lower apparatus uncertainty will lower the % uncertainty . greater resolution (finer scale divisions ) or
you can increase the size of the
To reduce the % uncertainty in a burette reading it is necessary to make measurement made.
the titre a larger volume. This could be done by: increasing the volume
and concentration of the substance in the conical flask or by decreasing
the concentration of the substance in the burette. If looking at a series of measurements in
an investigation, the experiments with
the smallest readings will have the
highest experimental uncertainties.
Reducing uncertainties in measuring mass
Using a balance that measures to more decimal places or using
a larger mass will reduce the % uncertainty in weighing a solid.

Weighing sample before and after addition and then calculating


difference will ensure a more accurate measurement of the
mass added.
If the %uncertainty due to the apparatus < percentage
Calculating the percentage difference between the actual difference between the actual value and the calculated
value and the calculated value value then there is a discrepancy in the result due to
other errors.
If we calculated an Mr of 203 and the real value is 214, then
the calculation is as follows: If the %uncertainty due to the apparatus > percentage
Calculate difference 214-203 = 11 difference between the actual value and the calculated
% = 11/214 x100 value then there is no discrepancy and all errors in the
=5.41% results can be explained by the sensitivity of the
equipment.

CHSE/Unit 3- Alternative practical reference notes for core practical’s /2020 Page 12 of 24
Core practical 5: Investigation of the rates of hydrolysis of some halogenoalkanes

Testing for halogenoalkanes method


• Arrange three test tubes in a row and add three drops of halogenoalkane in the sequence 1-chlorobutane,
1-bromobutane, 1-iodobutane.
• Add 4 cm3 of 0.02 M silver nitrate to each halogenoalkane.
• Without delay, put all three test tubes simultaneously in a hot water bath.
• Note the order in which precipitates appear

Comparing the rate of hydrolysis of halogenoalkanes reaction

Hydrolysis is defined as the splitting of a molecule ( in this case Water is a poor nucleophile but it can
a haloalkane) by a reaction with water react slowly with haloalkanes in a
substitution reaction
CH3CH2X + H2O → CH3CH2OH + X- + H+

Aqueous silver nitrate is added to a haloalkane and the halide CH3CH2I + H2O →CH3CH2OH + I- + H+
leaving group combines with a silver ion to form a SILVER
HALIDE PRECIPITATE. Ag+ (aq) + I-(aq) → AgI (s) - yellow precipitate
The precipitate only forms when the halide ion has left the The iodoalkane forms a precipitate with
haloalkane and so the rate of formation of the precipitate can the silver nitrate first as the C-I bond is
be used to compare the reactivity of the different haloalkanes. weakest and so it hydrolyses the quickest

The quicker the precipitate is formed, the faster the


AgI (s) - yellow precipitate
substitution reaction and the more reactive the haloalkane
AgBr(s) – cream precipitate forms faster
The rate of these substitution reactions depends on the strength of the AgCl(s) – white precipitate
C-X bond . The weaker the bond, the easier it is to break and the faster
the reaction.

CHSE/Unit 3- Alternative practical reference notes for core practical’s /2020 Page 13 of 24
Purifying an organic liquid

General method
• Put the distillate of impure product into a separating funnel
Sodium hydrogencarbonate will
• wash product by adding either
• sodium hydrogencarbonate solution , shaking neutralise any remaining reactant acid.
and releasing the pressure from CO2 produced.
Sodium chloride will help separate the
• Saturated sodium chloride solution
organic layer from the aqueous layer
•Allow the layers to separate in the funnel, and then run
and discard the aqueous layer. The layer with lower density will be the
upper layer. This is usually the organic layer
•Run the organic layer into a clean, dry conical flask and add
three spatula loads of drying agent (e.g. anhydrous sodium The drying agent should
sulphate, calcium chloride) to dry the organic liquid. When dry •be insoluble in the organic liquid
the organic liquid should appear clear. • not react with the organic liquid

• Carefully decant the liquid into the distillation flask Decant means carefully pour off
organic liquid leaving the drying agent
•Distill to collect pure product in the conical flask

Separating funnel

Distillation It’s important to be able to


draw and label this
In general used as separation technique to separate apparatus accurately. Don’t
thermometer draw lines between flask,
an organic product from its reacting mixture. Need to
adaptor and condenser.
collect the distillate of the approximate boiling point
range of the desired liquid.

Note the bulb of the thermometer should be Liebig condenser


at the T junction connecting to the
condenser to measure the correct boiling
point

Note the water goes in the bottom of the Water


condenser to go against gravity. This allows more out
efficient cooling and prevents back flow of water.
Round Water in
bottomed
flask
Electric heaters are often used to heat organic
Heat
chemicals. This is because organic chemicals are
normally highly flammable and could set on fire The collection flask can be
cooled in ice to help improve
with a naked flame.
yield of distillate

CHSE/Unit 3- Alternative practical reference notes for core practical’s /2020 Page 14 of 24
CORE PRACTICAL 6: Chlorination of 2-methylpropan-2-ol using concentrated hydrochloric acid

Detailed method for preparing and purifying a halogenoalkane from an alcohol


1. Measure 8 cm3 of 2-methylpropan-2-ol in a measuring cylinder and measure its mass.
2. Pour the 2-methylpropan-2-ol into a separating funnel, and reweigh the measuring cylinder to find
the mass of the 2-methylpropan-2-ol used.
3. In a fume cupboard, add 20 cm3 of concentrated hydrochloric acid to the separating funnel, in portions
of 3cm3. After each portion, stopper the flask and invert it several times . Open the tap when doing this
to release the pressure.
4. Allow the separating funnel to stand in the fume cupboard for about 20 minutes. Gently shake it at
intervals.
5. After 20 minutes, allow the layers to separate in the funnel. Open the tap and remove the lower
aqueous layer. Dispose of this layer.
6. Add sodium hydrogencarbonate solution in 2 cm3 portions to the separating funnel. This neutralises
any remaining acid. Shake the funnel after each addition, and release the pressure. Continue until no
more bubbles of CO2 are seen.
7. Allow the layers to separate in the funnel. Again remove and pour away the lower aqueous layer. Run
off the organic layer into a clean conical flask and add two spatulas of anhydrous sodium sulfate.
Stopper the flask, shake the contents and allow this to stand until the liquid becomes clear. This step
dries the organic liquid.
8. Decant the liquid into a weighed clean distillation flask.
9. Distil the liquid by holding a 250ml beaker half-full of boiled water around the flask using
standard distillation set up. Collect the liquid that distils in the range 47-53oC.
10. Measure the mass of the 2-chloro-2-methylpropane collected.

Detailed method for preparing and purifying Cyclohexene from cyclohexanol


OH
Conc
H3PO4 +H2O

a) Pour about 20 cm3 of cyclohexanol into a weighed 50 cm3 pear-shaped flask. Reweigh the flask and
record the mass of cyclohexanol.
b) Using a plastic graduated dropping pipette, carefully and with frequent shaking, add to the
flask approximately 8 cm3 of concentrated phosphoric acid.
c ) Add a few anti-bumping granules to the flask and assemble the distillation apparatus, so that the contents of
the flask may be distilled. Heat the flask gently, distilling over any liquid which boils below 100 °C.
d) Pour the distillate into a separating funnel and add 50 cm3 of saturated sodium chloride solution.
Shake the mixture and allow the two layers to separate.
e) run off the lower layer into a beaker and then transfer the upper layer, which contains the
crude cyclohexene, into a small conical flask.
f) Add a few lumps of anhydrous calcium chloride or anhydrous sodium sulfate(VI) or anhydrous
magnesium sulfate to the crude cyclohexene to remove water. Stopper the flask, shake the contents and
allow this to stand until the liquid becomes clear.
g) Decant the liquid into a clean, dry, weighed sample container.
h) Reweigh the container, calculate the mass of dry cyclohexene produced

CHSE/Unit 3- Alternative practical reference notes for core practical’s /2020 Page 15 of 24
Detailed Method for Preparing and Purifying an Ester
Propyl ethanoate can be made in the laboratory from propan-
1-ol and ethanoic acid.
The equation for the reaction is
CH3COOH + CH3CH2CH2OH → CH3COOCH2CH2CH3 + H2O
Procedure
1. Propan-1-ol (50 cm3) and ethanoic acid (50 cm3) are
mixed thoroughly in a 250 cm3 round-bottomed flask.
2. Concentrated sulfuric acid (10 cm3) is added drop by drop Sulfuric acid is a catalyst
to the mixture, keeping the contents of the flask well- Adding conc H2SO4 is an exothermic reaction- to
prevent uncontrolled boiling over add drop by drop
shaken and cooled in an ice-water bath. and cool

3. When the acid has all been added, a reflux condenser In reflux the reactant vapours of volatile compound are
is fitted to the flask and the mixture gently boiled over an condensed and returned to the reaction mixture. The
electric heating mantle for about 30 minutes. reaction is slow so it is heated for 30 minutes The
electric heating mantle allows for controlled heating
and stops flammable vapour lighting
4. The mixture is cooled, and the apparatus rearranged for
distillation. The crude ester (about 60 cm3) is distilled off. Sodium carbonate reacts with unreacted acid
5. The distillate is placed in a separating funnel and shaken and remaining catalyst still present after
with about half its volume of 30% sodium carbonate solution, distillation. The reaction produces CO2 so the
with the pressure being released at intervals. The lower pressure of gas needs to be released.
The upper layer is organic because it has a
aqueous layer is then discarded.
lower density than water

6. The crude ester is shaken in a separating funnel with


about half its volume of 50% calcium chloride solution, which
removes unreacted alcohol. The lower layer is discarded.
Calcium chloride is a drying agent. The liquid will
7. The ester is run into a clean, dry flask containing appear clear when dry.
some anhydrous calcium chloride and swirled.

8. The ester is filtered into a clean, dry flask, with a few anti- Anti-bumping granules are added to the prevent
bumping granules, and distilled. The fraction boiling vigorous, uneven boiling by making small
between 100°C and 103°C is collected. bubbles form instead of large bubbles

Measuring boiling point

Purity of liquid can be determined by measuring a boiling point. This can be


done in a distillation set up or by simply boiling a tube of the sample in an To get a correct measure of
heating oil bath. If the liquid is pure it will have the boiling point referred to in boiling point the thermometer
data books. If impure the boiling point tends to be higher than the pure liquid should be above the level of
the surface of the boiling
liquid and be measuring the
Pressure should be noted as changing pressure can change the boiling point
temperature of the saturated
of a liquid
vapour.

Measuring boiling point is not the most accurate method of identifying


a substance as several substances may have the same boiling point.

CHSE/Unit 3- Alternative practical reference notes for core practical’s /2020 Page 16 of 24
Core practical 7. Oxidation of an alcohol
Partial Oxidation of Primary Alcohols H O

Reaction: primary alcohol → aldehyde


Reagent: potassium dichromate (VI) solution and dilute sulfuric acid. HC

Conditions: (use a limited amount of dichromate) warm gently and distil


out the aldehyde as it forms: H
H

Ethanal

Observation: the orange


H H H H H O dichromate ion (Cr2O72-)
H C C C O H +[O] H C C C + H 2O reduces to the green Cr 3+ ion
SAFETY
H H H H H H
You must wear gloves when handling
OH + [O] O +H2O solid potassium dichromate(Vl) since it
is highly toxic and a category 2
CH3CH2CH2OH + [O] → CH3CH2CHO + H2O carcinogen; it is also an irritant. Avoid
inhaling any dust.
propan-1-ol propanal
Concentrated sulfuric acid is corrosive.

Detailed Method: The partial oxidation of propan-1-ol

This experiment uses a limited quantity of oxidising agent (0.01 mol) and the product is distilled from the
reaction mixture immediately it is formed. In this way we hope to achieve a partial oxidation of propan-1-ol.

• Place about 10 cm3 of dilute sulfuric acid in a flask and add about 3g of potassium dichromate(VI) and 2 or 3
anti-bumping granules. Shake the contents of the flask until solution is complete (do not warm).
• Add 1.5 cm3 of propan-1-ol in drops from a dropping pipette, shaking the flask so as to mix the contents,
and then assemble distillation apparatus as shown below
• Gently heat and slowly distil 2 cm3 of liquid into a test tube, taking care that none of the reaction
mixture splashes over.

Distillation It’s important to be able to


draw and label this
In general used as separation technique to separate an apparatus accurately. Don’t
thermometer draw lines between flask,
organic product from its reacting mixture. Need to
adaptor and condenser.
collect the distillate of the approximate boiling point
range of the desired liquid.

Note the bulb of the thermometer should be Liebig condenser


at the T junction connecting to the
condenser to measure the correct boiling
point

Note the water goes in the bottom of the Water


condenser to go against gravity. This allows more out
efficient cooling and prevents back flow of water.
Round Water in
bottomed
flask
Electric heaters are often used to heat organic
Heat
chemicals. This is because organic chemicals are
normally highly flammable and could set on fire
with a naked flame.

CHSE/Unit 3- Alternative practical reference notes for core practical’s /2020 Page 17 of 24
Reflux: Full Oxidation of Primary Alcohols
H H O

Reaction: primary alcohol → carboxylic acid


Reagent: potassium/sodium dichromate(VI) solution H C C C
and sulfuric acid
Conditions: use an excess of dichromate, and heat O H
H H
under reflux: (distil off product after the reaction
has finished) Propanoic acid

OH + 2[O] OH
+ H2 O Observation: the
orange dichromate
O
ion (Cr2O72-)
CH3CH2CH2OH + 2[O] → CH3CH2COOH + H2O reduces to the
propan-1-ol Propanoic acid green Cr 3+ ion

Detailed method
• Measure 5 cm3 of water into a boiling tube. Add 6 g of sodium dichromate(VI), shake and set aside to dissolve.
• Put about 1.5 cm3 propan-1-ol into a 50 cm3 round bottomed flask and add about 5 cm3 of water and two
or three anti-bumping granules. Put a condenser on the flask for reflux, as shown in figure below.
• Add 2 cm3 of concentrated sulfuric acid down the condenser in drops from a dropping pipette. While the
mixture is still warm, start to add your sodium dichromate(VI) solution down the condenser in drops from a
dropping pipette. The energy released from the reaction should make the mixture boil. Add the solution a
drop at a time so that the mixture continues to boil without any external heating.
• When all the sodium dichromate(VI) solution has been added, use a low Bunsen burner flame to keep
the mixture boiling for 10 minutes, not allowing any vapour to escape.
• At the end of that time remove the Bunsen burner and arrange the apparatus for distillation. Gently distil 2-
3 cm3 of liquid into a test tube.

Reflux
Reflux is used when heating organic reaction mixtures for long periods. The
condenser prevents organic vapours from escaping by condensing them Water out
back to liquids. The reactant vapours of volatile compound are condensed
and returned to the reaction mixture.
condenser
Never seal the end of the condenser as the build up of gas
pressure could cause the apparatus to explode. This is true of
any apparatus where volatile liquids are heated including the
distillation set up

Anti -bumping granules are added to the flask in both Water in


distillation and reflux to prevent vigorous, uneven boiling by
making small bubbles form instead of large bubbles

Round
It’s important to be able to draw and label this bottomed
flask
apparatus accurately.
• Don’t draw lines between flask and condenser.
• Don’t have top of condenser sealed
• Condenser must have outer tube for water that is sealed
Heat
at top and bottom
• Condenser must have two openings for water in and
out that are open

CHSE/Unit 3- Alternative practical reference notes for core practical’s /2020 Page 18 of 24
Fractional Distillation: In the laboratory
Fractional distillation is used
• Heat the flask, with a Bunsen burner or electric mantle
• This causes vapours of all the components in the to separate liquids with
mixture to be produced. different boiling points
• Vapours pass up the fractionating column.
• The vapour of the substance with the lower boiling point
reaches the top of the fractionating column first.
• The thermometer should be at or below the boiling
point of the most volatile substance.
• The vapours with higher boiling points condense
back into the flask.
• Only the most volatile vapour passes into the condenser.
• The condenser cools the vapours and condenses to
condenser
a liquid and is collected.
fractionating column

flask

CHSE/Unit 3- Alternative practical reference notes for core practical’s /2020 Page 19 of 24
CORE PRACTICAL 8 + 15: Analysis of some inorganic unknowns
Testing for cations
Flame tests
Method Lithium : Scarlet red
Use a nichrome wire ( nichrome is an unreactive metal Sodium : Yellow
and will not give out any flame colour) Potassium : lilac
Clean the wire by dipping in concentrated hydrochloric Rubidium : red
Caesium: blue
acid and then heating in Bunsen flame Magnesium: no flame colour (energy emitted of a
If the sample is not powdered then grind it up. wavelength outside visible spectrum)
Dip wire in solid and put in Bunsen flame and observe flame Calcium: brick red
Strontium: red
Barium: apple green

Method: adding dilute sodium hydroxide This test can be used


–3
a) Place about 10 drops of 0.1 mol dm metal ion solution in a test tube. on group 2 metal
–3
b) Add about 10 drops of 0.6 mol dm sodium hydroxide solution, mixing well. ions and transition
c) Continue to add sodium hydroxide solution, dropwise with gentle shaking, until in excess metal ions.

Results for Group 2


The results in this test are an application of the trend that group II hydroxides become more soluble down the group.

Magnesium hydroxide is classed as insoluble in water


and will appear as a white precipitate. A suspension of magnesium hydroxide in
water will appear slightly alkaline (pH 9) so
Simplest Ionic Equation for formation of Mg(OH)2 (s) some hydroxide ions must therefore have
Mg2+ (aq) + 2OH-(aq) → Mg(OH)2 (s). been produced by a very slight dissolving.

Calcium hydroxide is classed as partially soluble in water and


will appear as a white precipitate (it may need more sodium A suspension of calcium hydroxide in water will
hydroxide to be added before it appears compared to a appear more alkaline (pH 11) than magnesium
magnesium solution.) hydroxide as it is more soluble so there will be
Simplest Ionic Equation for formation of Ca(OH)2 (s) more hydroxide ions present in solution.

Ca2+ (aq) + 2OH-(aq) → Ca(OH)2 (s).


Strontium and barium salts will not form a hydroxide precipitate on addition of
sodium hydroxide due to their high solubility. The solutions will be highly alkaline

Testing for Ammonium ions (NH4+)


Results: alkaline
a) Place about 10 drops of 0.1 mol dm–3 ammonium chloride in a test tube.
ammonia gas is released
b) Add about 10 drops of 0.4 mol dm–3 sodium hydroxide solution. Shake the mixture.
which turns the red
c) Warm the mixture in the test tube gently using a water bath.
d) Test the fumes released from the mixture by holding a piece of damp red litmus paper blue
litmus paper in the mouth of the test tube.

CHSE/Unit 3- Alternative practical reference notes for core practical’s /2020 Page 20 of 24
CORE PRACTICAL 8+15: Analysis of some inorganic unknowns
Testing for anions: – Group 7 (halide ions), OH– , CO32– , SO42–

Testing for presence of a sulfate ion


BaCl2 solution acidified with hydrochloric acid is used as a reagent to test for
sulphate ions.
If acidified Barium Chloride is added to a solution that contains sulfate ions a white
precipitate of Barium Sulfate forms.

Other anions should give a negative


Simplest ionic equation
2+
Ba (aq) + SO42-(aq) → BaSO4 (s). result which is no precipitate
forming.

The hydrochloric acid is needed to react with carbonate impurities that are often found in salts
which would form a white Barium carbonate precipitate and so give a false result. You could not
used sulphuric acid because it contains sulphate ions and so would give a false positive result.

2HCl + Na CO → 2NaCl + H O + CO Fizzing due to CO2 would be observed if a carbonate was present.
2 3 2 2

Testing for presence of halide ions with silver nitrate. The role of nitric acid is to react with any
carbonates present to prevent formation of the
This reaction is used as a test to identify which halide ion is precipitate Ag2CO3. This would mask the
present. The test solution is made acidic with nitric acid, and desired observations
then Silver nitrate solution is added dropwise. 2 HNO3 + Na2CO3 → 2 NaNO3 + H2O + CO2

Fluorides produce no precipitate


Chlorides produce a white precipitate
Ag+(aq) + Cl- (aq) → AgCl(s)
Bromides produce a cream precipitate
Ag+(aq) + Br- (aq) → AgBr(s)
Iodides produce a pale yellow precipitate
Ag+(aq) + I- (aq) → AgI(s)

The silver halide precipitates can be treated with ammonia solution to help differentiate between
them if the colours look similar:

Silver chloride dissolves in dilute ammonia to form a complex ion


AgCl(s) + 2NH3(aq) →[Ag(NH3)2]+ (aq) + Cl- (aq)
Colourless solution
Silver bromide dissolves in concentrated ammonia to form a complex ion
AgBr(s) + 2NH3(aq) →[Ag(NH3)2]+ (aq) + Br - (aq)
Colourless solution
Silver iodide does not react with ammonia – it is too insoluble.

Testing for presence of carbonate ions


Add any dilute acid and observe effervescence.
Fizzing due to CO2 would
Bubble gas through limewater to test for CO2 – will turn limewater
be observed if a carbonate
cloudy 2HCl + Na2CO3 → 2NaCl + H2O + CO2 was present

Testing for presence of a hydroxide ions


Alkaline hydroxide ions will turn red litmus paper blue

CHSE/Unit 3- Alternative practical reference notes for core practical’s /2020 Page 21 of 24
Reactions of halide salts with concentrated sulfuric acid.
The halides show increasing power as reducing
Explanation of differing reducing power of
agents as one goes down the group. This can be
halides A reducing agent donates electrons.
clearly demonstrated in the various reactions of
The reducing power of the halides increases down group
the solid halides with concentrated sulfuric acid.
7 They have a greater tendency to donate electrons.
This is because as the ions get bigger it is easier for the outer
Know the equations and observations of electrons to be given away as the pull from the nucleus on
these reactions very well. them becomes smaller.

Fluoride and Chloride


F- and Cl- ions are not strong enough reducing agents to reduce the S in H2SO4. No
redox reactions occur. Only acid-base reactions occur.
NaF(s) + H2SO4(l) →NaHSO4(s) + HF(g) Observations:
These are acid –base reactions and not
White steamy fumes of HF are evolved. NaCl(s) +
redox reactions. H2SO4 plays the role
H2SO4(l) → NaHSO4(s) + HCl(g) Observations: White of an acid (proton donor).

steamy fumes of HCl are evolved.

Bromide
Br- ions are stronger reducing agents than Cl- and F- and after the initial acid-base reaction reduce the
sulfur in H2SO4 from +6 to + 4 in SO2
Observations: White steamy fumes of
Acid- base step: NaBr(s) + H2SO4(l) → NaHSO4(s) + HBr(g) HBr are evolved.
Red fumes of Bromine are also evolved
Redox step: 2HBr + H2SO4 → Br2(g) + SO2(g) + 2H2O(l)
and a colourless, acidic gas SO2
Ox ½ equation 2Br - → Br2 + 2e-

Re ½ equation H SO + 2 H+ + 2 e- → SO + 2 H O
2 4 2 2 Reduction product = sulfur dioxide
Note the H2SO4 plays the role of acid in the first step producing HBr and
then acts as an oxidising agent in the second redox step.

Iodide
I- ions are the strongest halide reducing agents. They can reduce the sulfur from +6 in
H2SO4 to + 4 in SO2, to 0 in S and -2 in H2S.

NaI(s) + H2SO4(l) → NaHSO4(s) + HI(g) Observations:


2HI + H2SO4 → I2(s) + SO2(g) + 2H2O(l) White steamy fumes of HI are evolved.
6HI + H2SO4 → 3 I2 + S (s) + 4 H2O (l) Black solid and purple fumes of Iodine are
8HI + H2SO4 →4I2(s) + H2S(g) + 4H2O(l) also evolved
A colourless, acidic gas SO2
A yellow solid of sulfur
Ox ½ equation 2I - → I2 + 2e-
H2S (Hydrogen sulfide), a gas with a bad egg smell.
Re ½ equation H2SO4 + 2 H+ + 2 e- → SO2 + 2 H2O

Re ½ equation H2SO4 + 6 H+ + 6 e- → S + 4 H2O Re ½ Reduction products = sulfur dioxide,


+ -
equation H2SO4 + 8 H + 8 e → H2S + 4 H2O sulfur and hydrogen sulfide

Note the H2SO4 plays the role of acid in the first step producing HI and
then acts as an oxidising agent in the three redox steps

Often in exam questions these redox reactions are


worked out after first making the half-equations

CHSE/Unit 3- Alternative practical reference notes for core practical’s /2020 Page 22 of 24
More on Insoluble salts and Precipitation reactions

Insoluble salts can be made by mixing appropriate solutions of ions so that a precipitate is
formed Barium nitrate (aq) + sodium sulfate (aq) → barium sulfate (s) + sodium nitrate (aq)
These are called precipitation reactions. A precipitate is a solid

There are some common rules for solubility of salts. No syllabus requires these to be learnt but a
good chemist does know them.
Soluble salts Insoluble salts
All sodium, potassium and ammonium salts
All nitrates
Most chlorides, bromides, iodides Silver, lead chlorides, bromides iodides
Most sulfates Lead, strontium and barium sulfate
Sodium, potassium and ammonium Most other carbonates
carbonates
Sodium, potassium and ammonium Most other hydroxides
hydroxides

When making an insoluble salt, normally the salt would be removed by filtration, washed with
distilled water to remove soluble impurities and then dried on filter paper

Filtration
Filter
residue paper
Filter
funnel

filtrate

This is gravitational filtration. Use


if small amounts of solid are
formed.

Writing Ionic equations for precipitation reactions

We usually write ionic equations to show precipitation Spectator ions are ions that are
reactions. Ionic equations only show the ions that are • Not changing state
reacting and leave out spectator ions. • Not changing oxidation number

Take full equation Ba(NO3)2 (aq) + Na2SO4 (aq) → BaSO4 (s) + 2 NaNO3 (aq)
- + 2- + -
Separate (aq) solutions into Ba2+(aq) + 2NO3 (aq) + 2Na (aq)+ SO4 (aq) → BaSO4(s) + 2 Na (aq)+ 2NO3 (aq)
ions

Cancel out spectator ions leaving Ba2+ (aq) + SO42-(aq) → BaSO4 (s).
the simplest ionic equation

CHSE/Unit 3- Alternative practical reference notes for core practical’s /2020 Page 23 of 24
CORE PRACTICAL 8+15: Analysis of some organic unknowns
Tests for alcohol, aldehyde, alkene and carboxylic acid
Functional group test for an Alkene
To 0.5 cm3 of bromine water in a test tube add a few drops of the unknown and shake.
Observation: alkenes should decolourise bromine water

Fehling’s solution Fehling's solution method


Reagent: Fehling’s solution containing blue Cu ions. 2+ Place 1 cm3 of Fehling's A into each of
Conditions: heat gently two boiling tubes, and then add
Fehling's B until the blue precipitate
Reaction: aldehydes only are oxidised by Fehling’s
redissolves. Add a few drops of the
Solution into a carboxylic acid and the copper (II)
unknown and leave in the water bath for
ions are reduced to copper(I) oxide .
a few minutes.
Observation: Aldehydes :Blue Cu 2+ ions in solution change to
a red precipitate of Cu2O. Ketones do not react
CH3CHO + 2Cu2+ + 2H2O → CH3COOH + Cu2O + 4H+

Summary of Identification of Functional Groups by test-tube reactions

Functional group Reagent Result

Alkene Bromine water Orange colour


decolourises
Alcohols PCl5 Misty fumes of HCl
produced
Alcohols Sodium metal Efferevesence due to H2
gas

Aldehyde Fehling’s solution Blue solution to red


precipitate

1o 2o alcohol and Sodium dichromate and Orange to green colour


aldehyde sulfuric acid change
chloroalkane Warm with silver nitrate Slow formation of white
precipitate of AgCl

CHSE/Unit 3- Alternative practical reference notes for core practical’s /2020 Page 24 of 24

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