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2.4 Experiment for First Semester

Experiment 1

Topic: Volumetric analysis - Stoichiometry

Purpose: To determine the exact concentration of a monobasic acid, HX

Question:

You are provided with a monobasic acid, HX, with a concentration in the range of
0.500 mol dm-3 to 1.00 mol dm-3. You are required to plan and carry out an experiment to
determine the exact concentration of the HX solution provided.

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Experiment 2

Topic: Volumetric analysis - Acid base and redox

Purpose: To determine the mass of sodium ethanedioate used to prepare a solution containing
sodium ethanedioate and hydrated ethanedioic acid

Materials:
· KA 1 is a solution containing hydrated ethanedioic acid, H2C2O4.2H2O, and sodium
ethanedioate
· KA 2 is a solution containing 3.50 g potassium manganate(VII) per dm3
· KA 3 is a solution containing 1.70 g hydroxide ions per dm3
· KA 4 is 1.00 mol dm-3 sulphuric acid
· Phenolphthalein is used as an indicator

Procedure:
(a) Pipette 25.0 cm3 KA 1 into a titration flask. Add two or three drops of phenolphthalein
and titrate this solution with KA 3. Record your readings in the table below.
Repeat the titration at least two times to achieve accurate results.

Results:
(b) Record your titration readings in the table below.

Accurate
Titration number Rough
First Second
Final reading/cm3
Initial reading/cm3
Volume of KA 3/cm3

(i) Calculate your average titre value showing the suitable titre values that you use.
(ii) 25.0 cm3 of KA 1 required ……… cm3 of KA 3 for a complete reaction.

(c) Pipette 25.0 cm3 of KA 1 into a titration flask. Then add 25 cm3 of KA 4. Heat this
solution to about 60 °C, and titrate the solution with KA 2 until a faint pink colour
persists in the solution.
Repeat the titration at least two times to achieve accurate results.

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Results:
(d) Record your titration readings in the table below.

Accurate
Titration number Rough
First Second
Final reading/cm3
Initial reading/cm3
Volume of KA 2/cm3

(i) Calculate your average titre value showing the suitable titre values that you use.
(ii) 25.0 cm3 of KA 1 required ……… cm3 of KA 2 for a complete reaction.

Questions:
(e) Calculate the concentration, in mol dm-3, of hydrated ethanedioic acid in KA 1 solution.
(f) Calculate the mass of ethanedioate ions, C2O42-, in 1.00 dm3 of KA 1.
(g) Calculate the concentration, in mol dm-3, of ethanedioate ions which originated from the
sodium ethanedioate salt.
(h) Calculate the mass of sodium ethanedioate present in 1.00 dm3 of solution KA 1.
(i) Calculate the percentage of sodium ethanedioate in solution KA 1.
(j) Why was solution KA 4 added to solution KA 1 before the titration?

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Experiment 3

Topic: Volumetric analysis - Purity and stoichiometry

Purpose: To determine the purity of a sample of sodium sulphite

Materials:
· KA 1 is 0.050 mol dm-3 aqueous iodine
· KA 2 is 0.100 mol dm-3 aqueous sodium thiosulphate
· KA 3 is a solution containing 24.00 g of anhydrous sodium sulphite, Na2SO3, per dm3
· KA 4 is 2.00 g sodium hydrogencarbonate
· Starch is used as an indicator

Introduction:
The sulphite ion can be oxidised quantitatively to the sulphate ion by iodine in the presence of
the hydrogen carbonate ion.

SO32 - + I2 + H2O SO42 - + 2HI

2HI + 2HCO3- 2I - + 2H2O + 2CO2

If a solution of sodium sulphite is added to an excess of a standard solution of iodine, the excess
iodine in the resulting solution can be titrated with a standard solution of sodium thiosulphate.
Hence the concentration of sodium sulphite can be determined.

Procedure:
(a) Pipette 50.0 cm3 of KA 1 into a titration flask. Using another pipette, place 25.0 cm3 of
KA 3 slowly into the titration flask containing KA 1 and shake. Add 2.00 g of KA 4 and
shake the flask again. Titrate the resulting solution with KA 2 using starch as indicator.
Repeat the titration as many times as you think necessary to achieve accurate results.

Results:
(b) Record your titration readings in the table below.

Accurate
Titration number Rough
First Second
3
Final reading/cm
Initial reading/cm3
Volume of KA 2/cm3

(i) Calculate your average titre value showing the suitable titre values that you used.
(ii) 50.0 cm3 of KA 1 required ……… cm3 of KA 2 for a complete reaction.

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Questions:
(c) Write a balanced equation for the reaction between iodine and the thiosulphate ion.
(d) Calculate the volume of I2 that did not react with the sulphite ions.
(e) Using your answer to (d), calculate the volume of I2 that reacted with the sulphite ions.
(f) Using your answer to (e),
(i) calculate the concentration, in mol dm-3, of the sulphite ions in solution KA 3,
(ii) calculate the mass of Na2SO3 present in 250 cm3 of KA 3.

(g) Using your answer to (f)(ii), calculate the percentage purity of Na2SO3 that you used.

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Experiment 4

Topic: Reaction kinetics

Purpose: To determine the effect of temperature on the reaction rate

Materials:
· KA 1 is 0.150 mol dm-3 potassium iodide solution
· KA 2 is 0.5% starch solution
· KA 3 is 0.050 mol dm-3 sodium thiosulphate solution
· KA 4 is 0.100 mol dm-3 hydrogen peroxide solution
· KA 5 is 0.100 mol dm-3 sulphuric acid

Procedure:
(a) Pipette 25.0 cm3 of KA 1 into a conical flask. By means of a measuring cylinder, add
10 cm3 of KA 2 and 25 cm3 of distilled water to the solution. Then run in 10.00 cm3 of
KA 3 from the burette. Record the temperature of the mixture in the table below.
Using a measuring cylinder, place 50 cm3 of KA 4 and 20 cm3 of KA 5 into a beaker.
Transfer this mixture quickly into the conical flask above and immediately start the
stopwatch. Swirl the conical flask regularly and record the time when the mixture turns
blue. Note the time taken to the nearest second. If no colour appears after two minutes,
repeat the procedure.
Repeat the experiment at the following temperatures:
(i) 10 °C below room temperature;
(ii) 10 °C above the room temperature and;
(iii) 20 °C above the room temperature.

Results:
(b) Record and complete your readings in the table below.

Mixture 1 2 3 4
Volume of KA 1/cm3 25.0 25.0 25.0 25.0
3
Volume of KA 2/cm 10 10 10 10
Volume of distilled water/cm3 25 25 25 25
Volume of KA 3/cm3 10.00 10.00 10.00 10.00
Volume of KA 4/cm3 50 50 50 50
Volume of KA 5/cm3 20 20 20 20
Temperature, T/°C
Time, t/s
1 -1
/s
t

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Questions:
(c) Why does the mixture in (a) turn blue?
1
(d) Plot a graph of against T.
t
(e) From your graph, what could be the effect of temperature on the reaction rate?
(f) Using your graph,
(i) compare the rate of reaction at 30 °C with the rate of reaction at 40 °C,
(ii) give an explanation for your answer.

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Experiment 5

Topic: Equilibrium and solubility

Purpose: To determine the solubility product, Ksp, of MX2 and enthalpy change of solution,
ΔH sol

Materials:
· KA 1 is 0.100 mol dm–3 of M 2+ ion
· KA 2 is 0.500 mol dm–3 of X - ion

Introduction:
A compound MX2, which is slightly soluble in water, is formed when two solutions, one
containing M 2+ ions and the other X - ions, are mixed together. The compound will be
2
precipitated at the temperature of reaction when the value of the product [ M 2+ ][ X - ] is greater
than the value of the solubility product, Ksp, of the compound and a saturated solution is formed.
The chemical equilibrium of the compound in the saturated solution is represented by
MX2(s) M 2+ (aq) + 2X - (aq)

Procedure:
(a) Transfer 12.00 cm3 of KA 1 from a burette into a boiling tube. Place thermometer in the
boiling tube and titrate solution KA 1 with KA 2 from a second burette until the first
appearance of the white precipitate. Record the temperature of the first appearance of the
white precipitate and the volume of KA 2 used in the table provided.
(b) Transfer 12.00 cm3 of KA 1 from a burette into a boiling tube. Place a thermometer in the
boiling tube and from the second burette run 7.00 cm3 of KA 2 into it. Stir the saturated
solution gently with the thermometer. Leave the boiling tube for a few minutes until the
reaction has reached equilibrium.
Then place the boiling tube in a hot water bath at 75 °C – 80 °C. Stir the saturated
solution until all the precipitate has dissolved. Do not remove the thermometer from
the solution.
Remove the boiling tube from the hot water bath and continue to stir the solution gently
with the thermometer until the first appearance of white precipitate is observed. Record
the temperature of the first appearance of the white precipitate in the table provided.
Wash and clean the thermometer for the next experiment. Repeat the experiment with
different volumes of KA 2 as shown in the table provided.

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Results:
(c) Record and complete your readings in the table below.

Temperature of the Solubility

Experiment Volume of Volume of
first appearance of product, Ksp /
number KA 1/cm3 KA 2/cm3
precipitate/°C mol3 dm-9
1 12.00
2 12.00 7.00
3 12.00 9.00
4 12.00 11.00
5 12.00 13.00

Questions:
(d) Calculate the solubility product, Ksp, of compound MX2 at each temperature recorded.
Record your results in the table above.
(e) Plot a graph of solubility product, Ksp, of compound MX2 against temperature.
(f) Use your graph to determine the solubility product of compound MX2 at 50 °C.
(g) The relationship between solubility product, Ksp, of a compound and temperature, T, in
Kelvin is given by the equation
DH 1
log10 K sp = - · + constant
2.303R T

(i) From the results obtained in (d), tabulate the data to plot a graph of log10 K sp against
1
and calculate the enthalpy change of solution, ΔH sol for the reaction
T

MX 2 (s) M 2+ (aq) + 2 X - (aq)

(ii) Is the reaction exothermic or endothermic? Explain your answer.

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