Practical 1: Finding the Molar Volume of a Gas

The molar volume of any gas is the same at given conditions of pressure and temperature
(Avogadro’s law).
Method
1. Set up the equipment as shown in diagram below.
2. Measure out 30 cm3 (excess) of ethanoic acid into the conical flask.
3. Place 0.05g of the calcium carbonate marble chips to a test tube and weigh it accurately,
recording the combined mass of the test tube and calcium carbonate.
4. Pour the calcium carbonate into the conical flask containing the ethanoic acid and quickly
replace the bung.
5. Measure and record the volume of carbon dioxide gas produced using the gas syringe.
6. Reweigh the test tube and calculate the actual mass of calcium carbonate that was added to the
conical flask.
7. Repeat, increasing the mass of the marble chips by around 0.05g each time, up to a mass of
0.40g

Apparatus set-up

Key points
● Overall equation: CaCO3 + 2CH3COOH → Ca(CH3COO)2 + CO2 (g) + H2O

Don’t use too much CaCO3 so you don’t produce more gas than the measuring cylinder can fit.
● A weak acid is used so that the reaction is slower, meaning there is less gas loss between
adding the marble chips and attaching the bung.
● An alternative method could involve attaching marble chips on a string to the bung, sealing the
test tube with a bung, and then tipping the test tube so that the acid comes to the contact with the
marble chips. This could reduce the loss of gas.

Errors
● If using syringe, plunger may not be free moving. It may need a lubricant.
● CO2 is slightly soluble in water, so the exact volume is not measured.
● Some gas escapes in between the addition of marble chips and sealing the test tube.
● Bung may not be airtight.
● Transferring the solid. It is important to weigh the tube containing marble chips before the
addition and reweigh after the addition. This method is ‘ weighing by difference’ and ensures the
amount of CaCO3 that ends up in the reaction mixture is known.

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Practical 2: Determination of the Enthalpy Change of a Reaction using Hess’s Law

Introduction
Enthalpy change for the decomposition of potassium hydrogencarbonate cannot be measured
directly. The reaction needs heating, so the recorded ΔT is not exclusively due to the
decomposition of the starting material. Two reactions (both with measurable enthalpy changes)
can be combined to form a desired reaction and therefore the previously unmeasurable enthalpy
change can be calculated.

Hess’s law: The enthalpy change for a reaction is independent of the path taken

Method
1. Place approximately 3g of potassium carbonate into a test tube and weigh and record its mass.
2. Put a polystyrene cup in a 250 cm3 beaker for support and then pour 30 cm3 of 2 mol dm-3
hydrochloric acid into the cup.
3. Place a thermometer into the cup and record the start temperature of the liquid. Then add the
potassium carbonate and monitor the temperature of the solution, recording the highest
temperature reached.
4. Reweigh the test tube that contained potassium carbonate and calculate the mass transferred
into the polystyrene cup.
5. Repeat steps 1-4 using potassium hydrocarbonate but instead record the lowest temperature
reached.

Key Points
 Q = mcΔT, where m = mass of the solution, c = specific heat capacity, ΔT = change in
temperature.
 ∆H = Q/moles, where Q is in kJ. Include +/ − sign to specify whether the reaction is
exothermic or endothermic. If temperature increases it is exothermic. If temperature
decreases it is endothermic.
 This practical combines two neutralisation reactions:
1) K2CO3 + 2 HCl → 2 KCl + H2O + CO2
2) 2 KHCO3 + 2 HCl → 2KCl + 2H2O + 2CO2
 The desired reaction is: 2 KHCO3 → K2CO3 + CO2 + H2O. Therefore to find the enthalpy of
the desired reaction, measure the enthalpy change for (1) and (2) then calculate (∆H2) -
(∆H1).

Errors
 We assume the specific heat capacity of the solution to be that of water.
 Polystyrene is more insulating than glass, so less heat is lost.

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Practical 3: Titration to find the Concentration of a Solution of Hydrochloric Acid

Method
1) Set up the apparatus as shown below with 25 cm3 of the unknown solution of hydrochloric
acid in the conical flask and the burette filled with a known concentration of sodium
hydroxide solution.
2) Add a few drops of a suitable indicator.
○ Phenolphthalein is pink in basic solutions and colourless in acidic and neutral
solutions.
○ Methyl orange is yellow in basic solution, orange in neutral solution, and red in an
acidic solution.
3) First carry out a quick trial titration to find the approximate end-point. Note down the value
of this titre.
4) Carry out a more accurate titration, adding the titrant drop by drop when approaching the
end-point. ○ When titrating, wash down the walls of the conical flask with a bit of distilled
water from time to time. This will ensure that all the titrant ends up reacting with the analyte.
5) Repeat accurate titrations until you have at least two concordant (within 0.10 cm3 ) titres.
6) Find a mean titre using these concordant values.

Key Points
 Use a pipette filler to draw a little solution of your analyte into the pipette to rinse it.
 Calibrate the pipette by ensuring there are no air bubbles in the tip.
 Rinse and fill the burette with the solution of your titrant using a funnel.

Errors
 Allow the titrant enough time to drain down the walls of the burette before reading
the burette.
 Swirl the conical flask so it mixes properly with the analyte.
 Use a white tile to make the colour change more noticeable.
 Diluting your solutions may produce a reading with a smaller percentage error (i.e.
10 cm3 titre has a smaller percentage error than a 30 cm3 titre).
 Phenolphthalein used in this titration may turn colourless at the end point if you
leave the solution to stand. This because NaOH reacts with CO2 from the air to
form Na2CO3 .
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Practical 5: Investigating the Rates of Hydrolysis of Halogenoalkanes.

Method
1) Set up 3 test tubes, each with 1 cm3 of ethanol and two drops of a different haloalkane
(iodo/bromo/chloro alkanes) and label which is which.
2) Place the test tubes in a water bath (60 °C), along with 3 test tubes of 5 cm3 of 0.1 mol
dm−3 silver nitrate and leave them all to reach a constant temperature.
3) Quickly add the silver nitrate solution from one test tube to the first test tube containing a
haloalkane, and start the stopwatch.
4) Measure and record the time taken for the precipitates to form (this is a measure of the rate
of reaction).
5) Repeat steps 3 and 4 for the remaining 2 haloalkanes.

Key points
 This is a nucleophilic substitution reaction where water acts as the nucleophile (hydrolysis).
 Precipitation with Ag+

¨
 The variables you control should be either the nature of the halide (changing Cl, Br and I
within a particular haloalkane), or the type of alkane (primary, secondary, tertiary with one
type of halide). Only change a single variable

Errors
 Use water bath to control the temperature.
 Use lower temperatures to reduce the rate of reaction. This will make the time difference
between haloalkanes larger, giving a lower uncertainty.

Expected Results

Halogenalkane Result
Chloroalkane White precipitate forms slowly
Bromoalkane Cream precipitate forms faster than chloro
but slower than iodo
Iodoalkane Yellow precipitate forms quickly

These results reflect the relative carbon-halogen bond strengths. C-I is the weakest bond in this
series, so the reaction is the fastest.

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Practical 6: Chlorination of 2-methlypropan-2-ol with Concentrated Hydrochloric Acid

2-methylpropan-2-ol
The structure of this alcohol is shown. It is a tertiary alcohol as the -OH hydroxyl functional group is
bonded to a carbon which is bonded to 3 other carbon atoms

Method
1) Add 35 cm3 of concentrated HCl and 10 cm3 of the tertiary alcohol to a 250 cm3 conical
flask.
2) Put the rubber bung in and swirl the flask gently. Open the bung to release the pressure
from fumes from time to time. Repeat this regularly for 20 minutes.
3) Use a spatula to add 2-3 scoops of anhydrous CaCl 2 and shake. At this point, there should
be two distinct layers. ● In this case, the upper (organic) layer contains the desired product.
The lower layer is the aqueous layer.
4) Transfer the contents of the flask to separating funnel.
5) Allow the layers to separate and discard the lower (aqueous) layer. Close the tap, keep the
organic layer in the separatory funnel.
6) Add a solution of NaHCO3 to remove the unreacted HCl. Swirl gently. Stopper the
separating funnel and shake it. Invert the separatory funnel and open the tap to release the
pressure due to CO2 formed. Repeat twice.
7) Remove the stopper and run off the aqueous layer. Then, run the organic layer into a 50
cm3 conical flask. Add a spatula of anhydrous Na2SO4 which acts as a drying agent.
8) Swirl the contents and leave the flask to stand for a bit. Then decant the liquid into a 50
cm3 pear-shaped flask.
9) Distill to purify the product. The method for this is detailed in core practical 7

Key Points
 A weaker base is used to prevent hydrolysis of haloalkane. NaOH could react with the
product via nucleophilic substitution
 Equation: (CH3)3COH + HCl → (CH3 )3CCl + H2O.

Errors
 Some product is lost when transferring liquids between the vessels.

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Practical 7: Oxidation of Propan-1-ol to Produce Propanal and Propanoic Acid

The oxidation of propan-1-ol to propanal (aldehyde) requires distillation apparatus. To oxidise

propan-1-ol completely to propanoic acid (carboxylic acid), reflux apparatus is required.

Method
1) Measure 20 cm3 of acidified potassium dichromate solution into a pear-shaped flask. Cool
down the flask using an ice bath.
2) Add a few anti-bumping granules. These will prevent the formation of large gas bubbles
that cause violent boiling.
3) Add 1 cm3 of ethanol dropwise to the pear-shaped flask using a pipette. Stir to ensure
complete mixing.
4) Warm up the flask to room temperature.
5) Set up the reflux apparatus as shown below, placing the flask in a water bath.
6) Heat using the Bunsen burner for 5-10 minutes.
7) Allow some time for the apparatus to cool down. Afterwards, collect the product via
distillation using the equipment shown in the diagram below.
o In this set-up the propan-1-ol will be completely oxidised to propanoic acid.
o Use the thermometer to prevent the temperature from rising too high.
8) To preparing an aldehyde, conduct the same reaction under distillation conditions without
the reflux process.
o In this set-up the propan-1-ol will be oxidised to propanal. For both reactions, the
colour change occurs from orange (Cr2O7 2−) to green (Cr3+ ) as the potassium
dichromate solution is reduced.
Diagrams
b. Distillation

Reflux

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Practical 8: Analysis of Some Inorganic and Organic Unknowns

Inorganic Tests

a.Test for acid or base

● Use litmus paper
○ Blue litmus paper turns red = acid
○ Red litmus paper turns blue = base
● Use universal indicator and compare to a scale like the one below

b.Flame tests for Group I and Group II metal cations

Method:
o To clean the nichrome wire - dip the wire in a solution of concentrated HCl and then
into a Bunsen burner flame.
o Dip the wire into the unknown compound and carefully place it at the top of the blue
Bunsen burner flame.

Observe the colour:

 Li+ = red
 Na+ = orange/yellow
 K+ = lilac ○ Rb+ = red
 Cs+ = blue
 Mg2+ = no colour
 Ca2+ = brick-red
 Sr2+ = crimson red
 Ba2+ = Green
+
C. Test for NH4 ions
o Add aqueous NaOH and gently warm the mixture.
o The ammonia gas will turn moist pH indicator paper blue.
o Additionally, a pungent smell is given off.

d.Test for SO4 2− ions

o Add acidified barium chloride solution.
o White ppt forms (BaSO4 ).

Mixtures of anions When carrying out the above test, it may be useful to add some HNO 3 before
you add Ba2+ (aq).The carbonate anion also gives a white precipitate with barium cations, and
addition of acid will remove any carbonates present in the mixture. Then, the test for sulfates can
be conducted.

e. Halides
 Dissolve 2 spatulas of the unknown product in 10 cm3 of water.
 Then, add a few drops of dilute nitric acid and silver nitrate solution. Observe the colour of
any precipitate formed:
 Cl− forms a white ppt with silver nitrate which is soluble in dilute NH3 .
 Br− forms a cream ppt with silver nitrate which is soluble in concentrated
NH3 .
 I− forms yellow ppt with silver nitrate which is insoluble in NH3 .
 The colours are all quite similar, so the solubility test with ammonia is a good way to
confirm the identity of the halide ion present. Halides can also be tested for by reacting a
solid halide salt with conc. H2SO4 .
 Chloride produces steamy fumes of HCl.
 Bromide produces steamy fumes, brown vapour (HBr, Br2 , SO2 ).
 Iodide produces steamy fumes, purple vapours, black solid (I2 , HI, SO2 or even solid S).

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f. Metal cations
Testing for various metal cations using sodium hydroxide. Group I hydroxides are all soluble.

Metal Cation Add Some NaOH Add more NaOH

Mg 2+ White suspension n/a
Ca 2+ White suspension, but more n/a
soluble than Mg(OH)2
Sr2+ Ba2+ Soluble hydroxides. n/a
Zn2+ White ppt, Zn(OH)2 . Soluble Ppt dissolves, colourless
in NH3 , colourless solution, solution, Zn(OH)4 2−
Zn(NH3 )4 2+
Al 3+ White ppt, Al(OH)3 Ppt dissolves, colourless
solution, Al(OH)4 −
Ag + Dark brown ppt, Ag2O. Soluble Ppt doesn’t dissolve
in NH3 , colourless solution,
Ag(NH3)2 +
Cu 2+ Blue ppt, Cu(H2O)4 (OH)2 , Ppt doesn’t dissolve
soluble in excess NH3 to form
a deep blue solution,
Cu(NH3 )4 2+
Fe 2+ White/green ppt, slowly Ppt doesn’t dissolve
turning brown when exposed
to air (oxidation to Fe(OH)3 )
Fe 3+ Brown ppt, Fe(OH)3 Ppt doesn’t dissolve
Cr 3+ (Blue or Green) Blue-green ppt, Cr(H2O)3 Ppt dissolves, Cr(OH)6 3−
(OH)3 , soluble in NH3 , Cr(NH3 green solution.
)6 3+, violet solution
Co 2+ Blueish ppt, Co(H2O)4 (OH)2 . Ppt doesn’t dissolve
Slowly turns pink. The
precipitate dissolves in NH3 ,
Co(NH3 )6 2+, light brown
colour. Turns to dark brown
upon standing - slow oxidation
to Co(III).
Ni 2+ Green ppt, Ni(H2O)4 (OH)2 . Ppt doesn’t dissolve
Soluble in NH3 - blue solution,
Ni(NH3 )6 2+
Mn 2+ (Pale Pink) Off-white ppt, Mn(OH)2 turns Ppt doesn’t dissolve
brown upon exposure to air
(oxidation to MnO2 )

g. Transition metal colours

 MnO4 − = violet
 CrO4 2− = yellow (could be converted to orange Cr2O7 2− in acid and vice versa).
H. Test for bromide

 Add chlorine water to a solution of bromides

 Produces an orange solution if present.
 Some effervescence may be observed.

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Organic tests
a. Organic Haloalkanes
See core practical 5, hydrolysis followed by halide test.

a.1 Alkenes
● Add 10 drops of your compound to a test tube followed by 1 cm3 of bromine water and
shake.
● If there are any C=C bonds, the colour change occurs from orange to colourless.

a.2 Alcohols
Alcohols can be primary, secondary or tertiary. Primary and secondary alcohols can be oxidised to
aldehydes and ketones respectively but tertiary alcohols cannot be oxidised.
● Add 1 cm3 of your unknown compound to a pear shaped flask followed by 5 cm3 of
acidified potassium dichromate solution.
● Heat the mixture under distillation conditions so the product is collected.
● If there is a colour change from orange to green then the potassium dichromate has been
reduced meaning a primary or secondary alcohol is present, these will have formed
aldehydes and ketones respectively.

a.3 Tollen’s reagent or Fehling’s solution can then be used to determine if the alcohol was primary
or secondary.
● If there is no colour change, a tertiary alcohol was present.

a.4 Test for CO3 2- and HCO3 – ions

● Add aqueous acid.
● If CO3 2- or HCO3 - ions are present bubbles of CO2 gas will be observed.
● Use a delivery tube to pass the CO2 through limewater.
● The solution will turn cloudy due to formation of CaCO3 precipitate.

a.5 Carboxylic acid

● Add 1 cm3 each of the unknown substance and ethanol into a boiling tube and heat for 5
minutes in a beaker of boiling water.
● Add a few drops of sodium carbonate solution.
● If a carboxylic acid was present there will be a sweet ester smell.

a.6 Aldehydes and Ketones

Using Tollens’ solution
● Add 10 drops of the unknown compound to a test tube followed by 5 cm3 of ethanol, 5
cm3 of sodium hydroxide solution and warm in a water bath for 5-10 minutes.
● Then add 1 cm3 of dilute nitric acid solution and 10 drops of silver nitrate solution.

● Aldehydes give a positive test and a silver mirror is observed.

● Ketones cannot be oxidised, so no change observed Using Fehling’s reagent
● Add 1 cm3 of blue Fehling’s reagent to 10 drops of the unknown compound and warm the
mixture in a 60 °C water bath
● Aldehydes give a positive test and form a brick red precipitate.
● Ketones don’t react so the solution stays deep blue.

a.7 Iodoform reaction

● Warm with iodine and sodium hydroxide
● Yellow precipitate.
● Antiseptic smell (triiodomethane, iodoform).

● Positive test with methyl ketones (e.g. propanone), ethanal, ethanol, and methyl secondary
alcohols (e.g. propan-2-ol).

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a.8 Esterification test
● Gently warm an alcohol and a carboxylic acid in the presence of concentrated H2SO4
● Should produce a compound with a characteristic smell, (e.g. pineapples).

a.9 Solubility test:

● Compounds with groups that can form H-bonds may be soluble in water, (e.g. amines, alcohols,
carboxylic acids etc
● Some carboxylic acids may not be soluble in water, but may be soluble in alkaline solution (due
to formation of RCOO−).
● Same goes with amines. Some may not be soluble in water, but will be soluble in acidic solution
(e.g. formation of RNH3 + ).

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