Measuring mass by weighing by

Measuring volumes
difference

Method Method
1. Measure the mass on 2 d.p balance of a 1. Check the scale on the glassware you are
weighing bottle with the required using.
quantity of solid in it.
2. Get eye level to the meniscus.
2. Empty mass into reaction vessel/flask
3. Take a reading from the bottom of the
3. Reweigh the empty weighing bottle meniscus.
4. Subtract the mass 4. Record the
of the empty measurement to
weighing bottle the correct
from the first read- number of d.p.
ing to give exact ie a burette.
of mass actually reading should
added. taken to the
nearest 0.05 cm3.

Measuring Gas Volumes

delivery tube
Collecting under water measuring
conical flask cylinder
Method
1. Set up the apparatus as shown. reaction
mixture
2. Using a measuring cylinder, add
10.0cm3 of the 1.00 mol dm–3 sulfuric
acid (an excess) to the 250 cm3
conical flask.
Errors

3. Weigh by difference about 0.10g of • Some gas may escape before the stopper/

unknown metal. bung is replaced.→replace as quick as pos-

sible
4. Record the exact mass of unknown
metal. • If the gas released is CO2 or SO2 it may dis-
solve in the water so the true amount is not
5. Remove the stopper, add the calculated.→use a gas syring instead.
unknown metal to the flask and
quickly replace the stopper.

6. Collect the gas and record the final Calculation

volume of hydrogen. • n(gas) = v(gas) / 24,000 (assume RTP).
Measuring Gas Volumes

Collecting using a gas syringe

Method
1. Set up the apparatus as shown in the
diagram, using a 250 cm3 conical flask
and a 100cm3 gas syringe

2. Support the gas syringe using a clamp

and stand.

3. Add the reactants and replace the

bung as quickly as possible.
Errors
4. Record either the volume of gas pro-
• Some gas may escape before the stopper/
duced at regular intervals (ie every 10
seconds) or the final volume of gas bung is replaced → replace the bung as
produced. quick as possible or place the solid in a small
vial inside the conical flask. Once the gas
syringe is attached shake the flask to knock
over the vial and mix the contents.

Preparing a standard solution

Method
Errors
1. Weigh a known mass of solid using a mass
• Some of the weighed solid may not be
balance (work out if given data)
transferred from the weighing boat →
2. Dissolve in 100cm3 of water in a beaker. weigh by difference.
Use a glass rod to stir to help dissolve the
• Take care not to spill any
solid.
solid or solution during
3. Add to a 250cm3 volumetric flask transfer.
using a funnel
• Volumetric flask needs to
4. Rinse beaker glass rod and funnel and be inverted sufficiently to
add washings to the flask ensure the concentration
is even.
5. Make up to the mark with distilled water
(bottom of meniscus on the mark) using a
pipette.

6. Stopper the flask and invert several times

to mix.
Titration

Method
1. Rinse the pipette with the substance to go in it (often alkali).

2. Pipette 25 cm3 of the required solution into the 250 cm3 conical
flask.

3. Touch the surface of solution with pipette (to ensure correct

amount is added).
4. The burette should be rinsed out with substance that will be put in
it before being filled between 0 to 5 cm3.

5. Make sure the jet space in the burette is filled with the solution
and air bubbles are removed.
6. Take an initial burette reading.
7. Add 3-5 drops of indicator to the conical flask and place on a white tile.
8. Add solution from burette whilst swirling the mixture and add drop-wise at end point
9. Take a final burette reading.
10. Repeat until get 2 concordant results (within 01 cm3)

Titration

Points to consider
• 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 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. This would give a lower titre volume.
• 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.

• 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.
• Results should be clearly recorded in a table. They should be recorded in full (i.e. both initial
and final readings) to 2dp (0.05 cm3)
• To work out an average titre results, only make an average of the concordant titre results.
Qualitative Ion Tests

Anion Method Positive result Equation

• Place 1cm3 of unknown

solution into a test tube CO32-(aq) + 2H+(aq) → CO2(g) +
CO32- fizzing/bubbling
• Add a few drops of acid, eg H2O(l)
HNO3

• Place 1cm3 of unknown

solution into a test tube white
SO42- Ba2+(aq) + SO42-(aq) → BaSO4(s)
• Add a few drops of either precipitate
BaCl2(aq) or BaNO3(aq)

• Place 1cm3 of unknown Cl- white ppt

Ag+(aq) + Cl-(aq) → AgCl(s)
solution into a test tube (soluble in dil.
• Add a few drops of AgNO3 NH3)
(aq) Br- cream ppt
X-
(soluble in conc. Ag (aq) + Br (aq) → AgBr(s)
+ -
• Add dilute NH3(aq) to see if
the ppt dissolves NH3)
• Add conc. NH3(aq) to see if I- yellow ppt
Ag+(aq) + I-(aq) → AgI(s)
the ppt dissolves. (insoluble in NH3)

Qualitative Ion Tests

Cation Method Positive result Equation

• Place 1cm3 of unknown
solution into a test tube.
• Add about 10 drops of NaOH(aq).
• Shake the mixture. Damp red NH4+(aq) + OH-(aq) → NH3(g) +
NH4+ • Warm the mixture in the test tube gently H2O(l)
litmus turns blue
using a water bath.
• Test the fumes released from the mixture by
holding a piece of damp red litmus paper
in the mouth of the test tube.

Fe2+ Green ppt Fe2+(aq) + 2OH-(aq) → Fe(OH)2(s)

• Place 1cm3 of unknown solution Orange/brown

Fe3+ Fe3+(aq) + 3OH-(aq) → Fe(OH)3(s)
into a test tube. ppt

Mn2+ • Add about 10 drops of NaOH Pale brown ppt Mn2+(aq) + 2OH-(aq) → Mn(OH)2(s)
(aq) mixing well.
Cu2+ Blue ppt Cu2+(aq) + 2OH-(aq) → Cu(OH)2(s)
• Continue to add NaOH(aq)
dropwise with gentle shaking, Grey/green ppt Cr3+ + 3OH- → Cr(OH)3
until in excess dissolves to give
Cr3+ dark green [Cr(H2O)6]3+ + 6OH- → [Cr(OH)6]3- +
solution 6H2O
Determine Enthalpy Changes - Calorimetric method

Method
1. Wash the equipment (cup and pipettes etc) with the solu-
tions to be used and dry the cup after washing.
2. Place the polystyrene cup in a beaker for insulation and
support.
3. Using a measuring cylinder measure out the desired volume
of solution and transfer to insulated cup.
4. Place the thermometer into the solution and measure the
initial temperatures of the solution or both solutions if 2 are
used.
5. Do this every minute for 2-3 minutes
6. At minute 3 transfer the second reagent (either a 2nd solu-
tion or a solid) to the cup.
7. Stir the mixture to ensure that all of the solution is at the
same temperature.
8. Record the temperature to the nearest 0.5oC every minute
after addition for several minutes

Determine Enthalpy Changes - Calorimetric method

Errors Calculaiton
• energy lost to (or less common gained q = mc∆t
from) the surroundings → insulate / use a
n = m/Mr or n = c x v / 1000
lid.
• experiment not carried out under ∆H = q/n
standard conditions
• the specific heat capacity of solution is
approximated. The method assumes all Points to consider
solutions have the heat capacity of water. Extrapolation can
• we ignore any energy absorbed by the be used to the
apparatus. determine the
maximum
• the reaction or dissolving may be incom-
temperature in
plete or slow.
order to determine
• the density of solution is taken to be the the temperature
same as water change.

Remember to describe more energy being released as more negative or more exothermic rather
than just increases and energy absorbed as less negative or less exothermic.
Determine Enthalpy Changes - Using a Spirit Burner

Method
1. Using a measuring cylinder add
100cm3 of water at room temperature
(not direct from the tap) to the cop-
per can/beaker.
2. Using a balance weigh the spirit
burner, including the cap, as
accurately as possible and record the
mass in a Results Table.
3. Arrange the heat of combustion
apparatus, as shown in the diagram below. Adjust the height of the calorimeter so that the
base of your beaker should be about 3cm above the wick of the burner
4. Take the temperature of the water before you start heating and record it in your results table
to the nearest 0.5°C.
5. Slowly and continuously stir the water in the can and watch the thermometer. When the tem-
perature has risen by about 20 °C, extinguish the flame and immediately replace the cap.
Continue stirring and record the maximum temperature of the water.
6. Re-weigh the spirit burner and cap and record the mass.

Determine Enthalpy Changes - Using a Spirit Burner

Errors Calculaiton
• energy lost to (or less common gained q = mc∆t
from) the surroundings → insulate and try
n = m/Mr or n = c x v / 1000
to reduce drafts.
• experiment not carried out under ∆H = q/n
standard conditions
• energy absorbed by the apparatus is
ignored Points to consider
• incomplete combustion may have If asked about incorrect weighing of the fuel
occurred. then heat for twice as long so a larger mass of
fuel is burnt and the percentage error is
• a layer of soot may form on the outside of
reduced
the beaker due to incomplete
combustion and absorb heat energy. Any thermometer reading needs to be to 1
• evaporation of the fuel may occur after decimal place to the nearest 0.5oC
weighing.

Remember to describe more energy being released as more negative or more exothermic rather
than just increases and energy absorbed as less negative or less exothermic.
Equilibria

Method
1. Mix known concentrations and volumes of reactants and/or products in a beaker.

2. Leave for a period of time to allow to reach equilibria.

3. Analyse a sample of the equilibrium mixture (usually by titration) in order to determine the
equilibrium no. of moles of one of the reactants/products.

4. Use this no. of moles to work out the equilibrium moles of the remaining reactants and
products.

Purification of an organic liquid

Method
1. Place the impure liquid into a separating
Separating funnel
funnel
2. If acid impurities may be present add Less dense liquid
(Na2CO3(aq)) or (NaHCO3(aq)).
More dense liquid
3. Shake and occasionally release the stopper
to reduce the pressure from the CO2 Stopcock
produced.
4. Allow the layers to separate in the funnel
and then run and discard the aqueous layer.
5. Run the organic layer into a clean, dry
Points to consider
conical flask and add a drying agent such
The layer with the lower density will be the
as anhydrous CaCl2(s) or anhydrous MgSO4
upper layer. This is usually the organic layer.
(s) slowly while swirling the conical flask until
Anything with a density of less than
the drying agent stops clumping.
1.00gcm-3 is less dense than water so would
6. Decant (pour off) the organic liquid or filter it be the upper layer.
into a round bottomed flask. If you are given densities then make sure
7. Distil to collect the pure product. you state whether the organic layer that
you are keeping is the upper or lower layer
Distillation

Distillation has two main uses

1. To separate an organic product from the rest of the mixture. The distillate is
collected at the approximate boiling point of the desired liquid
2. During the purification of an organic liquid distillation is used after the organic liquid has been
using a separating funnel

Points to note
• The water goes in the bottom of the condenser
to go against gravity. This allows more efficient
cooling and prevents back flow of water.
• The bulb of the thermometer should be
opposite the opening to the condenser to
measure the correct boiling point
• Don’t draw lines between the flask and the
condenser. It should be clear that there is a
path through which gases can flow.
• A water bath or electric heater should be used
to heat the mixture if there are flammable
substances present.

Reflux

Reflux is used when organic reaction mixtures need to be heated for

long periods of time. The condenser prevents organic vapours from
escaping by condensing them back to liquids.

Points to note
• The water goes in the bottom of the condenser to go against
gravity. This allows more efficient cooling and prevents back
flow of water.
• Never seal the end of the condenser as the build of gas
pressure could cause an explosion.
• Anti-bumping granules are added to the flask in both distillation
and reflux to prevent vigorous, uneven boiling by making small
bubbles form instead of large bubbles.
• Don’t draw lines between the flask and the condenser. It
should be clear that there is a path through which gases can
flow.
• The condenser must have outer tube of water that is sealed at
the top and bottom.
Measuring rate of reaction—Continuous monitoring

The continuous monitoring method involves following one experiment over time and recording
the changes in concentration at regular time intervals.

Typical method
• Measure 50 cm3 of the 1.0 mold dm-3 hydrochloric acid
and add to the conical flask.
• Set up the gas syringe.
• Weigh 0.20g of magnesium.
• Add the magnesium to the conical flask, quickly
place the bung into the conical flask and start the
stopwatch.
Errors
• Record the volume of hydrogen gas collected every
Some gas may have been lost
15 seconds for 3 minutes.
before replacing the bung

The gradient represent the rate of reaction. The gradient is steepest at the start as the rate or
reaction is fastest due to the high concentration of reactants. The rate drops as the reactants
start to get used up and their concentration decreases. The graph will eventually level off and
become horizontal with a gradient of 0 when the reaction has stopped.

Measuring rate of reaction—Continuous monitoring

The initial rate of reaction of a reaction can be

determined by finding the gradient of the a
concentration-time graph when t = 0. This can be
useful as we know the concentration of the reactants
at the start of the experiment.

In reactions where there are several reactants, if the

concentration of one of the reactant is kept in a large
excess then that reactant will appear not to affect
rate and will be pseudo-zero order. This is because its
concentration stays virtually constant and does not
affect rate.

• If half-lives are constant then the order is 1st order.

• If half-lives rapidly increase then the order is 2nd
order.
• The half-life of a first-order reaction is independent
of the concentration and is constant.
Measuring rate of reaction—Initial rates method

• The initial rates method determines the rate at the very start of the reaction when t = 0
• The initial rate can be found by drawing a concentration-time graph, drawing a tangent at
t = 0 and calculating it’s gradient.
• If the experiment is carried out several times, each time varying the concentration of one
reactant whilst keeping the other reactants constant, working out each initial rate, then you
can determine the order reaction with respect to the reactant.

Clock reactions
Clock reactions are a more convenient way of measuring the initial rate of reaction using a single
measurement.
The time taken, t, for a specific visual change in the reaction to occur is measured.
These changes could be a colour change or the formation of a precipitate.
The clock reaction depends on the major assumption that there is no significant change in the
rate of reaction between the start of the reaction and the time when the measurement is taken.

In clock reactions there are often two successive

reactions and an end point is achieved when one limited The initial rate is proportional to 1/t.
reactant runs out, resulting in a sudden change.

Measuring rate of reaction—Initial rates method

The iodine clock experiment is a common clock experiment. Limitations

Typical method The initial rate measured
• For each experiment, measure out required volumes of the during a clock reaction is an
potassium iodide, sodium thiosulphate, starch and estimate as it is based on the
water using either pipettes, measuring cylinders or burettes assumption that the rate of
into a small conical flask/boiling tube. reaction is constant.
• Measure the required volume of hydrogen peroxided into As the reaction progresses,
a boiling tube the concentration of the
reactants decreases.
• Pour the hydrogen peroxide from
Therefore, when the time
the boiling tube into the conical
measured for the rate of
flask and immediately start the
reaction to occur is short then
stopwatch. Stir the mixture
there is a higher chance that
• Time unit the first hint of blue/black colour appears. the initial rate calculated will
be closer to the true value. As
the time taken for the
Errors
reaction to occur increases
Timing of the appearance of the blue colour could be
the value is the initial rate will
inaccurate so an average value of the time recorded by two
become less accurate.
student could be used.
Measuring rate of reaction—Possible methods and some examples

• Measurement of change in volume of a gas

This works if there is a change in the number of moles of gas in the reaction. Using a gas syringe is a
common way of following this.
(CH3)2C=CH2(g) + HI(g) → (CH3)3CI(g)

HCOOH(aq) + Br2(aq) → 2H+(aq) + 2Br - (aq) + CO2(g)

Measurement of change of mass

This works if there is a gas produced which is allowed to escape. Works better with heavy gasses such
as CO2.
HCOOH(aq) + Br2(aq) → 2H+(aq) + 2Br - (aq) + CO2(g)

• Titrating samples of reaction mixture with acid, alkali, sodium thiosulphate etc.
Small samples are removed from the reaction mixture (quenched (which stops the reaction and then
titrated with a suitable reagent.
HCOOCH3(aq) + NaOH(aq) → HCOONa(aq)) + CH3OH(aq) The NaOH could be titrated with acid.

BrO3-(aq) + 5Br-(aq) + 6H+(aq) → 3Br2(aq) + 3H2O(l) The H+ could be titrated with alkali

CH3COCH3(aq) + I2(aq) → CH3COCH2I(aq) + H+(aq) + I-(aq) The I2 could be titrated with

sodium thiosulphate

Measuring rate of reaction—Possible methods and some examples

• Colorimetry
If one of the reactants or products is coloured then colorimetry can be used to measure the change in
colour of the reacting mixtures
H2O2(aq) + 2I- (aq) + 2H+(aq) → 2H2O(l) + I2(aq) The I2 produced is a brown colour.

• Measuring change in electrical conductivity

Can be used if there di a change in the number of ions in the reaction mixture.
HCOOH(aq) + Br2(aq) → 2H+(aq) + 2Br - (aq) + CO2(g)

• Measurement of optical acitvity

If there is a change in the optical activity through the reaction this could be followed in a polarimeter.
CH3CHBrCH3(l) + OH−(aq) → CH3CH(OH)CH3 (l) + Br−(aq)

Module 1 questions on rates of reaction could involve plotting graphs. Make sure that axis are la-
belled including units and points are plotted accurately. Draw a line/curve of best fit.

The equations given to the possible methods for determining the rate of reaction are examples
and DO NOT need to be learnt
Measuring pH with a pH meter

pH meters can be used to monitor the pH during an acid-base titration in order to construct a pH
curve

Method Calibration
1. Transfer 25cm3 of acid to a coni- pH meters can lose accuracy on
cal flask with a pipette. storage so need to be calibrated
2. Measure the initial pH of the before use. This is achieved by
acid with a pH meter. measuring the known pH of a
3. Add alkali in small amounts buffer solution. The probe is
(2cm3) noting the volume add- placed in a set buffer (often pH4)
ed. and a calibration button/setting
4. Stir the mixture for that pH is pressed. Sometimes
this is repeated with a second
5. Measure and record the pH to 2
buffer at a different pH.
d.p.
6. Repeat steps 3-5 but when ap-
proaching the endpoint add in
smaller volumes of alkali.
7. Add until alkali in excess

Redox titrations including those involving Fe2+/MnO4–

The redox reaction between iron (II) ions, Fe2+(aq) and mangante (VII) ions, MnO4-, in acid conditions is used
as a basis for a redox titration.

MnO4-(aq) + 8H+(aq) + 5Fe2+(aq) → Mn2+(aq) + 4H2O(l) + 5Fe3+(aq)

purple colourless

This titration is self indicating because of the significant colour change from reactant to product.

Choosing the acid End Point

Only use dilute sulfuric acid for The potassium manganate(VII) solution is usually run in from a
managanate titrations Fe2+ titrations. burette. At first, it turns colourless as it reacts. The end point is
• Insufficient volumes of H2SO4 or the first trace of permanent pink in the solution showing a tiny
using a weak acid will mean the so- excess of manganate(VII) ions.
lution is not acidic enough and
MnO2 will be produced instead of
Method for amount of Fe in iron tablets
Mn2+.
1. Accurately weigh 2 iron tablets.
• It cannot be conc HCl as the Cl- ions
2. Grind up the tablets in a mortar and pestle before dissolv-
would be oxidised to Cl2 by MnO4-.
ing them in sulfuric acid.
• It cannot be nitric acid as it is an
3. Transfer to a 100 cm3 volumetric flask and make up to 100
oxidising agent and would oxidises
cm3 using more sulfuric acid
Fe2+ to Fe3+
4. Titrate 10.0 cm3 portions of the solution with KMnO4
Redox titrations including those involving I2/S2O32-

This titration can be used to determine the concentration of an oxidising agent, which oxidises iodide ions to
iodine molecules.
The amount of iodine produced as a result of oxidation taking place is determined from titration against a
known quantity of sodium thiosulfate solution.

2S2O32– (aq) + I2 (aq) → 2I–(aq) + S4O62– (aq)

Thiosulfate/Iodine titrations
1. Add a standard solution of Na2S2O3 to the burette
2. Prepare a solution of the oxidising agent to be analysed.
3. Using a pipette, add this solution to the conical flask.
4. Then add an excess of potassium iodide. The oxidising agent reacts with iodine ions to produce iodine,
which turns the solution a yellow-brown colour.
5. Titrate this solution with the Na2S2O3(aq).
6. During the titration, the iodine is reduced back to I – ions and the brown colour fades quite gradually,
making it difficult to decide on an end point. T
7. This problem is solved by using starch indicator. When the end point is being approached, the iodine
colour has faded enough to become a pale straw colour, a small amount of starch indicator is added.
A deep blue-black colour forms. As more sodium thiosulfate is added, the blue-black colour fades.
8. The end point will be when the blue-black colour disappears and all the iodine will have just reacted.

Electrochemical Cells

Method Method
• Clean the zinc and copper foils/electrodes • If one or both of the half cells do not contain a
with emery before use conducting metal, we must use an inert platinum
• Place the copper strip into a 100 cm3 beaker electrode.
with about 50 cm3 of 1 mol dm–3 CuSO4 solution. • Set up a copper half cell using a similar
• Place the zinc strip into a 100 cm3 beaker with arrangement to the previous one.
about 50 cm3 of 1 mol dm–3 ZnSO4 solution. • Combine it with a Fe2+/Fe3+ half-cell with a
• Use a strip of filter paper soaked in saturated platinum electrode. This half cell should have a
potassium nitrate solution for the salt bridge mixture of acidified 1.0 mol dm-3 iron(II) sulphate
• Connect the Cu(s)|Cu2+ (aq) and Zn(s)|Zn2+ solution (1.0 mol dm-3 Fe2+(aq) ions) & an equal
(aq) half- cells by connecting the metals using volume of 0.5 mol dm-3 iron(III) sulphate solution
the crocodile clips and leads provided to the (1.0 mol dm-3 Fe3+(aq) ions) as the electrolyte.
Electrochemical Cells

Note
In the electrode system containing two solutions it is necessary to use a platinum electrode and both ion
solutions must be of a 1mol dm–3 concentration so [Fe2+] = 1mol dm–3 and [Fe3+] = 1mol dm–3

Salt Bridge Platinum Electrode

The salt bridge is used to connect up the circuit. The If the half equation for the half cell does not
involve a conducting metal, a platinum elec-
free moving ions conduct the charge.
trode is used because it is unreactive and can
A salt bridge is usually made from a piece of filter conduct electricity
paper (or material) soaked in a salt solution, usually
Potassium Nitrate.
Drawing a cell diagram using two half cells
It can also be a glass U tube containing a salt solution
• includes labels for electrodes, solution
plugged with cotton wool.
concentrations all at 1 mol dm-3, gases at
The salt should be unreactive with the electrodes and 101kPa and temp at 298K (ie include ALL
electrode solutions. standard conditions).
E.g. potassium chloride would not be suitable for
• Ensure it is a complete circuit with use of
copper systems because chloride ions can form com-
labelled salt bridge and voltmeter.
plexes with copper ions.
A wire is not used because the metal wire would set up • Show that the beakers contain a solution
its own electrode system with the solutions. an ensure that the electrodes and salt
bridge are in contact with the solution.

Purification of an organic solid

Step Reason
1. Dissolve the impure compound in a minimum An appropriate solvent is one which will dissolve both
volume of hot (near boiling) solvent. compound and impurities when hot and one in
which the compound itself does not dissolve well
when cold. The minimum volume is used to obtain
saturated solution and to enable crystallisation on
cooling
2. Cool the solution (by inserting beaker in ice) Crystals will reform but soluble impurities will remain in
solution form because they are present in small quan-
tities so solution is not saturated. Ice will
increase the yield of crystals
3. Filter under reduced pressure to separate out The water pump connected to the Buchner flask
crystals reduces the pressure and speeds up the filtration.
4 Wash the crystals with distilled water To remove soluble impurities.

5. Dry the crystals between absorbent paper

Purification of an organic solid

Filtration under reduced pressure Reasons for loss of yield in the

purification process
Filter paper
• Crystals lost when filtering or washing
Buchner Funnel
• Some product stays in solution after
recrystallisation
• Other side reactions occurring

If the crystals are not dried properly the

mass will be larger than expected
To Vacuum Pump which can lead to a percentage yield
Buchner Flask
>100% .

Checking the purity of an organic solvent

Melting point
• One way of testing for the degree of purity is to
determine the melting “point”, or melting range,
• Comparing an experimentally determined melt-
ing point value with one quoted in a data
source will verify the degree of purity.
• Pure compounds should have a narrow melting
point close to the known value.
• If impurities are present (and this can include
solvent from the recrystallisation process) the
melting point will be lowered and the sample will
melt over a range of several degrees Celsius.

Melting point can be measured in an electronic

melting point machine or by using a practical set up
where the capillary tube is strapped to a thermometer
immersed in some heating oil. In both cases a small
amount of the sample is put into a capillary tube. The
tube is heated up and is heated slowly near the
melting point
Checking the purity of an organic solvent

Melting point
• One way of testing for the degree of purity is to
determine the melting “point”, or melting range,
• Comparing an experimentally determined melt-
ing point value with one quoted in a data
source will verify the degree of purity.
• Pure compounds should have a narrow melting
point close to the known value.
• If impurities are present (and this can include
solvent from the recrystallisation process) the
melting point will be lowered and the sample will
melt over a range of several degrees Celsius.

Melting point can be measured in an electronic

melting point machine or by using a practical set up
where the capillary tube is strapped to a thermometer
immersed in some heating oil. In both cases a small
amount of the sample is put into a capillary tube. The
tube is heated up and is heated slowly near the
melting point

Checking the purity of an organic solvent

Thin Layer Chromatography Spectroscopy (NMR/IR)

Run a TLC and calculate the Rf value. Run an NMR or IR and compare with the
Compare to known data. It should have a spectra of a known sample. Spectra should
similar Rf value. contain the same/very similar peaks and not
have any additional peaks.
Rf value = distance moved by sample
distance moved by the solvent
Tests for organic functional groups

Alkenes Carbonyls
Method Method
Add bromine water and shake Add 2,4-DNP (Brady’s reagent)
Observation
Alkenes should decolourise the bromine water Observation
(colourless to orange). An orange precipitate is formed with both
aldehydes and ketones

Identification
Aldehydes
• The melting point of the crystal formed can be
Method
used to help identify which carbonyl was used.
Add Tollen’s Reagent (aqueous ammonia and
silver nitrate) and heat gently. • Take the melting point of orange crystals
Observation product from 2,4-DNP.
With aldehydes, a silver mirror forms. Ketones
• Compare melting point with known values in
result in no change.
database.

Other points to consider

Carboxylic Acids
Method Use 2,4-DNP to identify if the compound is a
Add carbonate ions (eg Na2CO3(aq)) carbonyl. Then to differentiate an aldehyde from
Observation a ketone use Tollen’s reagent.
Fizzing/bubbling/effervescence if a carboxylic
acid is present.

Tests for organic functional groups

Haloalkanes Water is a poor nucleophile but it can react

Method slowly with haloalkanes in a substitution
• In a test tube add silver nitrate to each haloalkane. reaction
• Without delay, put all three test tubes simultaneously in
a hot water bath. The quicker the precipitate is formed, the
faster the substitution reaction and the more
reactive the haloalkane
Comparing the rate of hydrolysis of haloalkanes
reaction
CH3CH2I + H2O → CH3CH2OH + I- + H+
Hydrolysis is defined as the splitting of a molecule (in
this case a haloalkane) by a reaction with Ag+(aq) + I-(aq) → AgI(s)
water The iodoalkane forms a precipitate with the
CH3CH2X + H2O → CH3CH2OH + X-- + H+ silver nitrate first as the C-I bond is weakest
and so it hydrolyses the quickest.
Aqueous silver nitrate is added to a haloalkane and
the halide leaving group combines with a
silver ion to form a SILVER HALIDE AgI (s) - yellow precipitate
The precipitate only forms when the halide ion has left AgBr(s) – cream precipitate forms faster
the haloalkane and so the rate of formation of the
precipitate can be used to compare the reactivity of AgCl(s) – white precipitate
the different haloalkanes.
Tests for organic functional groups

Primary alcohols/secondary alcohols/aldehydes

Method Observations
Add Cr2O72-(aq) and H+(aq) ions and heat Orange to green

Phenol • Phenols are very weakly acidic. They are weaker

Method acids than carboxylic acids.
Determine the pH using a pH meter or indicator
AND add carbonate ions (eg Na2CO3(aq)) • Only carboxylic acids will react with sodium
carbonate as a phenol is not strong enough an
Observations acid to react.
The pH is that of a weak acid (ie pH 4 to 5) and • Both phenols and carboxylic acids will react with
does not fizz/bubble when the carbonate is sodium hydroxide.
added.

Points to consider
Phenol will also decolourise Br2(aq) (and produce
a white precipitate) at room temp and with out a The sodium phenoxide compound is more
catalyst but this is not often used as a test for soluble than the original phenol. So the solid
phenol to avoid confusion with the alkenes. phenol dissolves on addition of NaOH

Tests for organic functional groups

Functional Group Reagent Observation

Alkene Br2 Orange to colourless

Carboxylic acid Na2CO3 (aq) Bubbles/fizzing

Silver Mirror
Tollens (ammoniacal AgNO3)
Aldehyde AND
Orange/yellow ppt (can be used
Brady’s reagent OR 2,4 DNP
to identify with mp)
No observable reaction (no silver
Tollens (ammoniacal AgNO3)
mirror)
Ketone
AND
Orange/yellow ppt (can be used
Brady’s reagent OR 2,4 DNP
to identify with mp)
Test pH and add Na2CO3 pH of weak acid (4 to 5) but does
not fizz
Phenol or or

Br2 Orange solution to white ppt

Haloalkane H2O and AgNO3 in ethanol See AgX ppt and rate of hydrolysis

Primary/Secondary alcohol AND

Cr2O72- / H+ and heat Orange to green
aldehyde