Objective : To prepare a standard solution of sodium carbonate and use it to standardize a given solution of dilute hydrochloric
acid.
Introduction : Anhydrous sodium carbonate is a suitable chemical for preparing a standard solution (as a primary standard). The
molarity of the given hydrochloric acid can be found by titrating it against the standard sodium carbonate solution
prepared.
The equation for the complete neutralization of sodium carbonate with dilute hydrochloric acid is
Na2CO3(aq) + 2HCl(aq) → 2NaCl(aq) + CO2(g) + H2O(l)
Apparatus :
Procedure : 1. Weight out about 1.3 g of anhydrous sodium carbonate accurately using the method of “weighing by
difference”.
2. Transfer the weighed carbonate to a beaker and add about 100 cm3 of distilled water to dissolve it completely.
3. After dissolving, transfer the solution to a 250.00 cm3 volumetric flask. Rinse the beaker thoroughly and
transfer all the washes into the volumetric flask. Remember not to overshoot the graduation mark of the flask.
4. Make up the solution to the mark on the neck by adding water.
5. Pipette 25.00 cm3 of sodium carbonate solution to a clean conical flask.
6. Add 2 drops of methyl orange indicator to the carbonate solution.
7. Titrate the carbonate solution with the given dilute hydrochloric acid until the colour of solution just changes
from yellow to orange.
8. Repeat the titration two times.
Calculation : Calculate the molarity of the sodium carbonate solution prepared and the molarity of the hydrochloric acid.
Results :
Objective : To prepare a standard solution of ethane-1,2-dioic acid (oxalic acid) and use it to standardize a solution of
potassium permanganate.
Optional Activity
Standardization of Hydrogen peroxide solution used the standardized potassium permanaganate solution.
Introduction : Permanganate ion, MnO4-(aq), is a strong oxidant. Since permanganate ion is intensely coloured and its
reduction product, Mn2+(aq), is almost colourless, a self-indicating titration is possible. The addition of the first drop
of permanganate solution in excess imparts a pink colour to the solution.
Potassium permanganate does not oxides oxalates in cold solution. A temperature of about 70ºC is necessary
to cause the reaction to occur rapidly.
Formula mass of ethane-1,2-dioic acid (H2C2O4·2H2O) is 126. A 0.05 M solution of ethane-1,2-dioic acid is to
be prepared by weighing out about 1.5 g of the acid and made up to 250.0 cm3 of solution on a standard volumetric
flask.
Optional Activity
Potassium permanganate KMnO4(aq) also reacts with hydrogen peroxide H2O2(aq) to form colourless products.
Therefore, the concentration of a H2O2(aq) solution can also be determined by titrating it against the potassium
permanaganate solution just standardized.
Apparatus :
1. Weigh out accurately about 1.5 g ethane-1,2-dioic acid, dissolve in water and make up to 250.00 cm3.
2. Pipette 25.00 cm3, using a pipette filler, of the prepared solution into a conical flask. Add about 25 cm3 of 3 M
H2SO4 and heat the mixture on a tripod to about 60ºC (The temperature can be estimated by using your
fingers. Swirl the flask for about 10 seconds, if the side of the flask is still just too hot to be touched, the
temperature of the liquid is approximately correct.)
3. Titrate with the potassium permanganate solution till a permanent pink coloration is observed. Heat the
solution occasionally to maintain the temperature at 60ºC, after the addition of every 5 cm3 of KMnO4(aq).
Swirl the flask continuously throughout titration.
4. Repeat the titration for two times.
Optional Activity
Design a procedure to standardize a solution of hydrogen peroxide using the potassium permanganate solution just
standardized. Note : Heating is not required in this reaction.
Calculation : Calculate the concentration of the potassium permanganate solution in molarity (M) and in gdm-3.
Optional Activity
Calculate the concentration of the hydrogen peroxide solution provided.
Results :
Questions : 1. Ethane-1,2-dioic acid is used as the primary standard in the titration. What is primary standard ? What criteria
a chemical need to fulfill to be a good primary standard. Other than the ethane-1,2dioic acid and anhydrous
calcium carbonate, give an example of primary standard for each of the following :
i. acid
ii. base
iii. oxidizing agent
iv. reducing agent
2. Why is it that potassium permanganate is used as a titrant in ACIDIC MEDIUM?
3. In the above titration, what conditions should be maintained?
4. Close observation of the solution during the titration may reveal the evolution of small gas bubbles. What gas
or gases are formed?
5. Dichromate ion is also a strong oxidant. Do you think that dichromate titrations could also be self-indicating?
Half-reaction of dichromate is:
Cr2O72-(aq) + 14H+(aq) + 6e- → 2Cr3+(aq) + 7H2O(l)
orange green
6. For the titration between potassium permanaganate and hydrogen peroxide, write a balanced equation for the
reaction. Which chemical acts as a reducing agent and which acts as an oxidizing agent in the reaction, explain
your answer briefly.
Experiment : 3
Introduction : Sodium chlorate(I) (sodium hypochlorite) forms the basis of most commercial bleaches. The amount of this
active ingredient available can be estimated by the following method.
In this analysis, the sodium chlorate(I) is allowed to react with an excess of potassium iodide solution in the
presence of acid, liberating iodine, which is then titrated against standard sodium thiosulphate solution. The
reactions involved are:
Chemicals : Commercial bleach (2 brands), 1 M KI, dilute H2SO4, 0.050 M Na2S2O3, starch indicator (freshly prepared)
Procedure : 1. Pipette 10.00 cm3 of the bleach into a clean 250.00 cm3 volumetric flask. Make up to the mark using water.
2. Pipette 25.00 cm3 of this solution into a conical flask, add to it 10 cm3 of 1 M potassium iodide solution and 10
cm3 of dilute sulphuric(VI) acid.
[Hazard Warning: Bench dilute sulphuric(VI) acid is corrosive.]
3. Titrate this against the standard sodium thiosulphate solution. Add 1cm3 of freshly prepared starch indicator
when the reaction mixture turns light brown and continue to titrate to the end-point. Repeat your titration once.
4. Repeat steps (1) to (3) with another brand of bleach.
Brand A
Trade Name: _______________ Manufacturer: _______________ Price: __________ Volume : __________
Brand B
Trade Name: _______________ Manufacturer: _______________ Price: __________ Volume : __________
Questions : 1. According to your results, which of the two brands of bleach is a better buy?
2. Why should potassium iodide be present in excess?
3. What is the function of the dilute sulphuric(VI) acid ?
4. Bleaching solution may deteriorate for two main reasons. One is the attack by carbon dioxide in air according
to the equation:
2ClO-(aq) + CO2(aq) → CO32-(aq) + Cl2(aq)
What is the other possible reason?
5. The starch indicator should not be added too early. Why?
Experiment : 4
Introduction : Aspirin is an analgesic and antipyretic drug. Analgesics are drugs which relieve pain. O
Antipyretics are drugs which lower body temperature. C CH3
O O
The main constituent of aspirin tablets is 2-ethanoylhydroxybenzoic acid (acetyl-salicylic
H C C
acid, CH3COOC6H4COOH, m.m. 180.0). Aspirin passes unchanged through the acidic C C OH
conditions in the stomach but is hydrolysed to ethanoate (acetate) ions and C C
2-hydroxybenzoate (salicylate) ions by the alkaline juices in the intestines. H C H
Salicylates lower body temperature rapidly and effectively in feverish patients H
(antipyretic action), but have little effect if the temperature is normal. They are also mild
analgesics, relieving certain types of pain such as headaches and rheumatism.
Although the toxic dose from salicylates is relatively large, their uncontrolled use could be dangerous. Single
doses of 5 to 10 grams of salicylate have caused death in adults; and 12 grams taken over a period of twenty-four
hours produces symptoms of poisoning.
Pharmaceutical manufacturers are required by law to state on the packaging the amount of each active
ingredient in their products. In this experiment a consumer survey on the amount of the active ingredient (2-
ethanoyloxybenzoic acid, or o-acetylsalicylic acid) in different commercial brands of aspirin tablets is carried out,
to see whether the manufacturers' claims are justified.
2-ethanoyloxybenzoic acid can be readily hydrolysed, using a known excess of sodium hydroxide, into the
sodium salts of two weak acids, ethanoic acid and 2-hydroxybenzoic acid. The excess amount of sodium hydroxide
is then estimated by a back titration with standard sulphuric(VI) acid. The equation for the hydrolysis reaction is:
Phenol red (pH range 6.8 – 8.4) is most suitable for this titration due to the presence of the salts of two weak
acids, though phenolphthalein is also satisfactory for the present purpose.
Chemicals : standard 0.5M NaOH, H2SO4 (about 0.05 M), a standard sodium carbonate solution, 2 brands of aspirin tablets,
phenol red indicator, methyl orange indicator,
Procedure : [Hazard Warning: 0.5 M sodium hydroxide and 0.05 M sulphuric(VI) acid are irritant.]
Do the Step 1 and 2 of Part II first.
Part II – Analysis of aspirin tablets of 2 brands (Pair up with another student and each member choose a brand).
1. Weigh accurately two aspirin tablets into a 250 cm3 conical flask.
2. Initiate the hydrolysis of the aspirin by adding 50.00 cm3 of 0.5 M sodium hydroxide from a pipette, diluting
with 25 cm3 of water. Warm the flask gently for ten minutes to complete the hydrolysis. Cool down the flask
thoroughly.
3. After cooling, transfer the reaction mixture with washings to a 250 cm3 volumetric flask. Dilute to the mark
with distilled water. Shake the flask to mix well.
4. Titrate 25.00 cm3 aliquots of the diluted reaction mixture with the standard sulphuric(VI) acid provided, using
phenol red as indicator until the colour changes from red to orange.
5. Repeat the titration
6. Calculate the mass of 2-ethanoyloxybenzoic acid in each tablet and compare the results with the
manufacturer's specification.
Questions : 1. What is back titration ? When should it be used instead of direct titration ?
2. Determine which brand of aspirin gives the best value for money.
Experiment : 5
Introduction : The enthalpies of reaction between calcium and hydrochloric acid calcium carbonate and hydrochloric acid are
determined experimentally. By mean of an energy cycle, the enthalpy of formation of calcium carbonate can then
be calculated. The following data will be needed :
1. Weigh out accurately about 2 g of dry powdered calcium carbonate directly into a clean dry plastic cup.
2. Place about 50 cm3 of the hydrochloric acid in a measuring cylinder. Record its temperature every 15 seconds.
At exactly the second minute, pour the acid on the carbonate in the plastic cup, cover the cup with the cover
provided.
3. Stir gently with the thermometer and record the temperature every 15 seconds until the sixth minute.
4. Tabulate your results.
5. Plot the graph of temperature of the liquid against time.
6. Calculate the no. of mole of limiting reagent used and the amount of heat evolved, hence the molar heat of
reaction between calcium carbonate and dilute hydrochloric acid.
Introduction : This experiment enables an approximate determination of the enthalpy change of hydration of copper(II)
sulphate(VI) to be calculated using Hess's law. The enthalpy changes when known masses of anhydrous copper(II)
sulphate(VI) and copper(II) sulphate(VI)-5-water crystals are respectively dissolved in the same quantity of water
are measured. From this, the molar enthalpy changes are calculated in each case.
Apparatus : Polystyrene foam cup, -10 – 110 ºC thermometer, 100 cm3 measuring cylinder, 400 cm3 beaker, cotton wool
Repeat part A using 8.0 g of anhydrous copper(II) sulphate(VI) instead of the hydrated salt. [Hazard
Warning: Anhydrous copper(II) sulphate(VI) is harmful.]
Introduction : Breaking or formation of intermolecular hydrogen bonds between molecules in liquids would cause an
enthalpy change when the liquids are mixed. This experiment is to investigate such enthalpy changes and to
measure approximate strengths of hydrogen bonds formed between molecules of ethanol and those between
molecules of trichloromethane and ethyl ethanoate using simple calorimetric methods.
Apparatus : 10 cm3 and 25 cm3 measuring cylinders, 50 cm3 beaker, 250 cm3 beaker, -10 – 110 °C thermometer, cotton wool
Procedure : [Hazard Warning: Ethanol, cyclohexane and ethyl ethanoate are flammable, trichloromethane is harmful, and
tetrachloromethane is toxic.]
1. Using a measuring cylinder, add 5 cm3 of ethanol into an insulated 50 cm3 beaker. Measure the
temperature of the liquid.
2. Then add 20 cm3 of cyclohexane to the ethanol in the beaker, mix well and record the lowest temperature
attained.
3. From the temperature drop estimate the hydrogen bond strength (in kJmol-1) in ethanol.
B. To measure the strength of hydrogen bonds formed between molecules of ethyl ethanoate and
trichloromethane
[Hazard Warning: Mixtures of trichloromethane and propanone have been known to explode on standing.
The solvent residues from this experiment should not be disposed of into a container in which propanone is
present.]
1. Measure 5 cm3 of ethyl ethanoate into an insulated 50cm3 beaker. Record its temperature.
2. Add to this 20 cm3 of trichloromethane and mix well. Record the highest temperature attained.
3. From the temperature change estimate the strength of the hydrogen bond formed between molecules of
ethyl ethanoate and trichloromethane.
N.B. Actually either ethyl ethanoate or trichloromethane can be in excess.
Questions : A. To measure the strength of hydrogen bond formed between ethanol molecules
1. Why should the beaker be insulated?
2. Is the mixing process endothermic or exothermic?
3. Account for the temperature change.
4. Explain why cyclohexane has to be used in excess in this experiment.
B. To measure the strength of hydrogen bonds formed between molecules of ethyl ethanoate and
trichloromethane
1. Is the mixing process exothermic or endothermic?
2. Account for the temperature change.
3. Explain why it does not matter which liquid is used in excess.
Experiment : 8
Title : The Methanal Clock Reaction – A Study of the Factors Affecting the Rate of a Chemical Reaction
Introduction : The reactions between methanal and hydrogensulphate(IV) ion can be represented as:
In the overall reaction, hydrogensulphate(IV) ion is consumed. When its concentration drops to a certain level,
the pH rises sharply, and a pink colour will be observed if phenolphthalein indicator is present. By measuring the
time taken for the colour of the solution to turn pink under different conditions, factors which determine the rate of
the reaction can be studied.
Chemicals : 200 cm3 Solution A (0.3 M methanal), 200 cm3 solution B (0.2 M with respect to sodium hydrogensulphate(IV)
and 0.05 M with respect to sodium sulphate(IV) with a little phenolphthalein added)
Apparatus : burette, boiling tube, stop watch, -10 – 110 °C thermometer, 250 cm3 beaker
Procedure : [Note : Use 3 different burettes to measure the volume of solution A, solution B and water. Deliver the amount of
the solution required to test-tube or boiling tube, then mix the solutions in one batch.]
A. Effect of dilution
1. Mix the following amounts of water with 5 cm3 of solution A in a boiling tube, then add 5 cm3 of solution
B to each and stir vigorously. Record the time for the pink colour to form.
1. Mix the given amounts of solution A and water in a boiling tube as listed in the table below and then add
5 cm3 of solution B. Record the time taken for the solution to turn pink.
C. Effect of temperature
1. Prepare a solution of 20 cm3 of water and 10 cm3 of solution A in a boiling tube. Put 10 cm3 of solution B
into another test-tube.
2. Immerse the boiling tube and the test tube in the hot water bath with the following temperature for 2
minutes.
3. Mix the two solutions and record the maximum temperature of the solution attained and the time taken for
it to turn pink.
Approximate 25 30 35 40 45
temperature / ºC
Maximum
temperature reached
/ ºC
Time /s
N.B. In plotting a graph, usually, the independent variable is plotted as x and the dependent variable is plotted
as y.
Questions : A. Effect of dilution
1. What effect does the amount of water have on the rate of the reaction as indicated in your graph?
C. Effect of temperature
1. What effect does temperature have on the rate of the reaction as indicated in your graph?
Experiment : 9
Title : Determination of order of rate of disproportionation of sodium thiosulphate in acidic medium by initial rate
method.
Introduction : In acidic medium, thiosulphate ion disproportionate (an element undergoes oxidation and reduction at the same
time) to sulphur and sulphur dioxide according to the following equation.
The formation of sulphur precipitate will turn the mixture cloudy. If a paper with a cross is placed under the
flask of reaction mixture, the cross will be masked by the sulphur precipitate gradually. By assuming that the
concentration of the reactants, rate of disproportionation and the amount required to mask the cross are all constant
in the due course of the reaction. A rate equation can be formulated as
Rate0 = k[H+(aq)]0x[S2O32-(aq)]0y
1 + s 2- y
t = k’ [H (aq)]0 [S2O3 (aq)]0
By keeping the concentration of the acid in large excess the equation can be further simplified as
1 2- y
t = k’’[S2O3 (aq)]0
1
ln t = ln k’’ + y ln [S2O32-(aq)]0
1
By plotting a graph of ln t vs ln [S2O32-(aq)]0 , the order of reaction with respect to thiosulphate ion would be
determined.
Chemicals :
Apparatus :
Experiment : 10
Title : To Determine the Activation Energy of the Reaction between Bromide Ion and Bromate(V) Ion in Acid Solution
Introduction : During a reaction, bonds are first broken, and others are then formed. Energy is required to break certain
bonds and start this process, no matter the overall reaction is exothermic or endothermic. Particles will not always
react when they collide because they may not possess sufficient energy for the appropriate bonds to break.
A reaction will only occur if the colliding particles possess more than a certain minimum amount of energy known
as the activation energy, EA.
Using the kinetic theory and probability theory, Maxwell and Boltzmann showed that the fraction of molecules
with energy greater than EA Jmol-1 was given by e-EA/RT where R is the gas constant, T is the absolute temperature
and e is the exponential function.
This suggests that at a given temperature: Reaction rate α e-EA/RT. But as k, the rate constant for a reaction, is a
measure of the reaction rate, we can write
k α e-EA/RT
k = A e-EA/RT
In acidic solution, the reaction between bromide ion and bromate(V) ion can be represented by
The progress of the reaction may be followed by adding a fixed amount of phenol together with some methyl
red indicator. The bromine produced during the reaction reacts very rapidly with phenol (forming tribromophenol).
Once all the phenol is consumed, any further bromine bleaches the indicator immediately. So, the time for the
reaction to proceed to a given point may be determined.
1
k α time for methyl red to be bleached
constant
k= t
constant
ln ( t ) = ln A + ln e-EA/RT
1 EA
ln (constant) + ln t = ln A - RT
EA
ln t = [ln A - ln (constant)] - RT
1 1 EA
so a graph of ln t against T has a gradient of - R .
Chemicals : 50 cm3 solution A (0.083 M with respect to KBr and 0.017 M with respect to KBrO3), 25 cm3 0.5 M H2SO4, 50 cm3
0.01 M phenol solution, methyl red indicator
Apparatus : Beaker, boiling tube, stop watch, two -10 – 110 °C thermometers, burette
Procedure : [Hazard Warning: 0.5 M sulphuric(VI) acid is irritant, and phenol is toxic.]
1. Place 10.0 cm3 of 0.01 M phenol solution, 10.0 cm3 solution A and 2 drops of methyl red indicator into a
boiling tube.
2. Place 5.0 cm3 of 0.5 M sulphuric(VI) acid into a second boiling tube.
3. Place both boiling tubes into a beaker of water which is maintained at about 30°C. Allow the contents of the
tubes to reach the temperature of the water bath.
4. Pour the content of the first boiling tube into the sulphuric(IV) acid, and at the same time start the stop watch.
Swirl well for 5 seconds.
5. Keep the second boiling tube in the water bath throughout the experiment. Record the time (t) taken when the
red colour fade.
6. Record also the temperature (T), to the nearest degree, of the reaction mixture at the end of the experiment.
7. Repeat steps (1) to (6), maintaining the reaction temperature at about 35 °C, 40 °C, 45 °C and 50 °C.
Result :
Temperature
Experiment Time t / s 1 T / ºC T/K 1/T / K-1
ln t
1
2
3
4
5
Questions : 1. Give an equation for the reaction between phenol and bromine.
2. What is the use of methyl red in this experiment?
3. Should the time be taken when the methyl red starts to fade or when the methyl red becomes colourless ?
Why?
3. Based on your results, is it advisable to perform the experiment at high temperatures such as 80 °C?
4. Why is it not necessary to know how far the main reaction has proceeded at the point where the methyl red is
decolorized ?
5. The Arrhenius equation can be represented as:
k = A e-EA/RT
(a) Can 1/t substitute k in this equation? Why?
(b) Derive an equation relating ln k and 1/T.
6. Explain why the reaction rate can be affected by temperature.
Experiment : 11
Objective : The purpose of this experiment is to find out how a system in equilibrium responds to a change in concentration of
components in the mixture.
Introduction : Equilibrium I
Iron(III) ions and thiocyanate ions react in solution to produce thiocyanatoiron(III), a complex ion, according to the
equation :
Fe3+(aq) + SCN-(aq) d Fe(SCN)2+(aq)
pale colourless blood-red
yellow
Equilibrium II
Bromine molecules and water molecules react in solution to produce hydrogen ions, bromide ions and
hydrobromous acid (hydrobromic (I) acid) molecules, according to the equation :
Br2(aq) + H2O(l) d H+(aq) + Br-(aq) + HOBr(aq)
yellow colourless colourless colourless colourless
brown
Equilibrium III
Dichromate(VI) ions and water molecules react in solution to produce chromate(VI) ions and hydrogen ions,
according to the equation :
Cr2O72-(aq) + H2O(l) d 2CrO42-(aq) + 2H+(aq)
orange yellow
Equilibrium IV
Bismuth trichloride molecules and water molecules react in solution to produce bismuth oxychloride precipitate
and hydrochloric acid, according to the equation :
BiCl3(aq) + H2O(l) d BiOCl(s) + 2HCl(aq)
colourless white
precipitate
Chemicals : water, 0.01 M KSCN, 0.01 M FeCl3, 1M FeCl3, 1M NH4Cl, Br2(aq), H2SO4(aq), NaOH(aq), K2Cr2O7(aq), BiCl3(aq)
Apparatus : safety spectacles, 4 test-tubes and test-tube rack, 2 teat-pipettes, spatula, glass stirring rod
Procedure :
Equilibria Reagent A Reagent B Reagent C Reagent D
I 0.01M FeCl3(aq) 0.01M KSCN(aq) 1M NH4Cl(aq) 1M FeCl3(aq)
II Br2(aq) H2O(l) H2SO4(aq) NaOH(aq)
III K2Cr2O7(aq) H2O(l) H2SO4(aq) NaOH(aq)
IV BiCl3(aq) H2O(l) H2SO4(aq) NaOH(aq)
Objective : To find the equilibrium constant by titration for the reaction : Ag+(aq) + Fe2+(aq) d Fe3+(aq) + Ag(s)
Introduction :
Chemicals :
Apparatus :
Procedure : 1. Prepare a sample of reaction mixture by adding together 70.00 cm3 each of 0.100M iron(II) sulphate and
0.100M silver nitrate solutions in a 250 cm3 conical flask.
2. Stopper the flask tightly and leave them to stand overnight.
3. Carefully pipette out into a conical flask 25.00 cm3 of the supernatant solution above the silver precipitate.
4. Titrate the 25.00 cm3 sample of solution with 0.0500 M standard potassium thiocyanate solution. When all
Ag+(aq) ions have been removed, thiocyanate ions react with iron(III) ions (also present in the equilibrium
mixture) to give a blood red color which acts as an indicator.
5. Repeat the titration and calculate Kc for this reaction.
Results :
Questions : 1. Write an equation for the reaction between silver(I) ion and thiocyanate ion.
2. Write an equation to account for the formation of the blood red color at the end point.
3. Why was it necessary to stopper the conical flask containing 25 cm3 of iron(II) sulphate and silver nitrate
solution tightly?
4. Why is it necessary to leave the solutions to stand overnight?
5. Suggest sources of error for this experiment
Experiment : 13
Chemicals :
Apparatus :
Procedure : 1. Put approximately 10 cm3 portions of the different buffer solutions, in numerical order, in 8 test tubes in a
rack.
2. Add 3 drops of universal indicator to each tube and shake to mix.
3. Add 5.0 cm3 of 0.2 M ethanoic acid and 5 cm3 of 0.1 M NaOH solution using burettes, into a clean, dry test
tube to produce a half-neutralized acid solution. Add 3 drops of universal indicator. Determine the
approximate pH of this solution by comparing with the colour set.
4. Determine the dissociation constant for the acid.
Questions : The pH for a half-neutralized acid equals pKa. Account for this.
Experiment : 14
Objective : To determine the proportions of sodium carbonate and sodium hydroxide in a mixture solution using Double
indicator method.
The neutralization of a strong alkali by means of a strong acid can be followed by the used of indicator.
Sodium hydrogen carbonate solution is definitely alkaline to it. If acid is added to a mixture of sodium hydroxide
and sodium carbonate in solution, using phenolphthalein as indicator, then the pink colour of the indicator is
discharged when reactions I and II are completed. If methyl orange is now added and a further quantity of acid is
also added, the amount required will be that necessary to complete reaction III. But 1 mole of sodium hydrogen
carbonate formed from one mole of sodium carbonate and hence the amounts of acid required for reactions II and
III will be the same.
Suppose the volume of acid needed to reach end-point as indicated by the phenolphthalein is x cm3 and the
additional volume of acid to reach the end point as indicated by the methyl orange is y cm3 . Then the volume of
acid reacting with sodium hydroxide is x - y cm3.
Chemicals :
Apparatus :
Procedure : Pipette 25.00 cm3 of the mixture solution into a conical flask. Add two drops of phenolphthalein indicator. Titrate
with the given standard hydrochloric acid (0.100M) until the pink colour is just discharged. Note the burette
reading and add a few drops of methyl orange and a further quantity of acid until the yellow colour of the methyl
orange changes to orange.
Repeat the above procedure 3 times more.
Results :
Questions : 1. What is the mean volume of the titrant with phenolphthalein indicator. (x cm3)
2. What is the mean volume of the titrant with methyl orange indicator. (y cm3)
3. Calculate the concentration of the solution with respect to sodium carbonate and sodium hydroxide. Give your
answer in molarity and gdm-3.
Experiment : 15
Introduction : The voltage across an electrochemical cell is affected by the pH of electrolyte in which electrodes are immersed in.
By measuring the voltage across two reference electrodes immersed in buffer solutions with different pH, a
calibration graph can be constructed with the pH vs the voltage (V) across the 2 electrodes.
Using the calibration curve obtained, the voltmeter calibrated functions as a pH meter to trace the change in pH in
the course of an acid-base titration. Consequently, titration curve can be constructed to determine the end point of
the titration.
Chemicals : 0.2M standard hydrochloric acid, 0.2 M sodium hydroxide, 0.2 M ethanoic acid, 0.2 M ammonia solution, buffer
solutions with pH = 2.2, 4.2, 5.9, 8.0, 10.0, 12.0, copper(II) sulphate solution
Apparatus : Burette, Pipette, Retort stand & clamp, Magnetic stirrer, magnetic bar & remover, DC 3 V and connecting wires,
Antimony electrode, copper electrode, digital multimeter, crocodile clips, Wash bottle, Salt bridge–use filter paper
strips
1. Calibrate the voltmeter by using the buffer solutions provided, with the pH = 2.2, 4.2, 5.9, 8.0, 10.0, 12.0.
Construct a calibration curve using the voltage measured as the vertical axis against the pH of the buffer
solutions as the horizontal axis.
1. Pipette 25.00 cm3 of 0.2 M (approximate) sodium hydroxide solution into a beaker.
2. Set up the apparatus as demonstrated. Set the magnetic stirrer in motion.
3. Run in from a burette, 5.00 cm3 of 0.2 M (accurate) hydrochloric acid. Determine the voltage of the cell.
4. Continual add 5.00 cm3 portions of acid, taking the voltage reading after each addition, until a total of
20 cm3 has been added. Then add the acid in 1.00 cm3 portions until a total of 30.00 cm3 has been added.
Then revert to 5.00 cm3 portions until a total of 40.00 cm3 has been added, determining the voltage
throughout.
5. Obtain the pH values of the solutions from the calibration graph. Plot the titration curve of the pH of the
solution (vertical axis) against the volume of hydrochloric acid added.
1. With the original calibration curve, repeat the titration using 0.2 M (approximate) ammonia solution
instead of sodium hydroxide solution and construction of titration curve to determine the concentration of
ammonia solution provided.
Wash the burette and refill the burette with the 0.2M (approximate) ethanoic acid provided for Part IV and
V.
1. With the original calibration curve, repeat the titration using the 0.2 M (approximate) ammonia provided
and construction of titration curve to determine the concentration of ethanoic acid provided by assuming
that the concentration of ammonia determined in Part III is accurate.
1. With the original calibration curve, repeat the titration using 0.2 M (approximate) sodium hydroxide
solutions and construction of titration curve to determine the concentration of ethanoic acid provided
again by assuming that the concentration of sodium hydroxide determined in Part II is accurate.
Calculation : Part II : Use the titration curve to determine the accurate concentration of the sodium hydroxide solution provided.
Part III: Use the titration curve to determine the accurate concentration of the ammonia solution provided.
Part IV: Use the titration curve to determine the accurate concentration of the ethanoic acid provided.
Part V: Use the titration curve to determine the accurate concentration of the ethanoic acid provided again.
Questions : 1. What differences can be observed among the three titration curve obtained ? Explain the differences briefly.
2. Compare and comment on the concentrations of ethanoic acid determined in Part IV and Part V.
Experiment : 16
Introduction : Vanadium has a range of oxidation states from 0 to +5. The following experiments are designed to identify the
colours of vanadium solutions for the various oxidation states, the ease with which the oxidation states can be
formed and the stability of the vanadium compounds made.
Chemicals : Ammonium metavanadate, 0.1 M FeSO4, 0.1 M Fe2(SO4)3, 0.1 M KI, 0.1 M KBr, 0.1 M I2 in KI, aqueous SO2,
copper powder, zinc powder, dilute H2SO4, 0.05M Na2S2O3(aq)
Apparatus : Bunsen burner, 8 test tubes and rack, filter funnel, filter paper, stoppers
Procedure : [Hazard Warning: Ammonium metavanadate is toxic, iron(III) sulphate(VI) is irritant, and bench dilute
sulphuric(VI) acid is corrosive.]
1. Dissolve a small spatula of ammonium metavanadate in 60 cm3 of dilute sulphuric(VI) acid to make a V(V)
solution in a conical flask.
2. Transfer 10 cm3 of the solution to a test tube and stopper it for later use.
3. Add a little zinc powder to the remaining solution in the conical flask with constant swirling and warming to
reduced V(V) to Vanadium compounds with lower oxidation states. When the solution turns blue, filter 10 cm3
of the solution to a test tube and stopper it for later use.
4. Repeat the heating and filtering procedure for the green and violet solutions.
N.B. Extra zinc powder should only be added when most of the zinc powder in the solution have been
dissolved.
The violet solution can be air oxidized, keep it away from air.
Make a large copy of Table 1 on your raw data sheet. Using the chart of Eo values and the colour of vanadium
containing ions at different oxidation states, predict the likely experimental result when substances are mixed
as in the table. This should cover the expected oxidation state of vanadium in the final solution and the likely
observations.
(Be careful about the mixing of coloured solutions even without chemical reactions. A blue and yellow
solution can give a green one on mixing. If iodine is present, the colour of other products can only be seen if
the iodine is converted to colourless iodide ions by sodium thiosulphate or removed in a solution of 1,1,1-
trichloroethane.)
3. Test them out by performing the actual experiments. Record the results also in the table.
Table 1
Substances to be mixed Prediction Experimental Result
V(V) + FeSO4(aq)
V(V) + KI
V(V) + SO2(aq)
V(V) + Cu
V(V) + Zn
V(IV) + V(II)
V(V) + V(III)
V(IV) + V(III)
V(IV) + Fe2(SO4)3
V(III) + Fe2(SO4)3
V(IV) + KI
V(V) + KBr
V(III) + I2
V(IV) + I2
Title : The variation of boiling point with composition for a binary liquid mixture
Objective : The purpose of this experiment is to construct boiling-point / composition curves for mixtures of two different
liquids.
Introduction : Works in groups of 3, each member choose one of the following binary mixture
You measure the boiling-points of these mixtures at various compositions and construct boiling-point composition
curves from your results. For simplicity, you plot volume composition rather than mole fraction - the curves have
the same general shape.
Share your data with your members in the group and plot a boiling point composition curve showing the liquid
composition curve only for each of the binary mixture.
Chemicals : trichloromethane CHCl3, methyl ethanoate CH3CO2CH3, ethanol C2H5OH, cyclohexane, C6H12
propan-1-ol, CH3CH2CH2OH, propan-2-ol, CH3CH(OH)CH3
Apparatus : safety spectacles, quick-fit apparatus, thermometer, 0-100 °C, ± 0.1 °C, anti-bumping granules, Bunsen burner,
gauze and tripod
Procedure :
1. Set up a suitable assembly for reflux, with the flask positioned over a tripod and gauze. It is important that the
thermometer is positioned so that it will dip into the liquid mixture but it must not touch the walls of the flask.
2. Choose one of the three systems shown and ensure that the other students in your group investigate the other
systems. In the remaining procedure steps we refer to the components of each system as A or B, as shown.
3. Transfer 10.0 cm3 of A from the burette to the pear-shaped flask containing a small spatula measure of anti-
bumping granules. Heat the flask gently until the liquid just begins to boil.
4. Record the boiling-point of A.
5. Turn off the Bunsen burner and allow the apparatus to cool for about two minutes.
6. Measure 2.0 cm3 of liquid B from the burette into a test-tube and pour this liquid down the condenser into the
pear-shaped flask.
7. Reheat the flask gently until the liquid mixture just boils and record its boiling-point.
8. Repeat stages 5, 6 and 7 with further additions of 2 cm3 portions of component B until a total of 10 cm3 of B
has been added.
9. Allow the apparatus to cool and ask your teacher how you can safely dispose of the mixture.
10. Repeat the experiment from step 3, this time starting with 10 cm3 of liquid B in the flask and adding 2 cm3 of
component A after each boiling point determination until a total of 8 cm3 of A has been added.
11. Plot a graph of boiling-point (y-axis) against percentage composition by volume (x-axis).
12. Collect the results for the other two systems from your members and plot the results in exactly the same way.
Results :
Volume of 10 10 10 10 10 10 0 2 4 6 8
Component A / cm3
Volume of 0 2 4 6 8 10 10 10 10 10 10
Component B / cm3
Volume % of
Component A
Boiling point / ºC
Questions : 1. For each boiling-point/composition curve, sketch an approximate vapour pressure composition curve showing
both liquid composition curve and vapour composition curve.
2. Study the vapour pressure curves and classify each mixture as ideal or as showing positive or negative
deviations from ideality.
Experiment : 18
Objective : The purpose of this experiment is to determine the value of the distribution coefficient for the equilibrium that
exists when ammonia is distributed between water and 1,1,1-trichloroethane.
Introduction : In this experiment you shake some ammonia solution with 1,1,1-trichloroethane (relative density 1.34) to establish
equilibrium, and then determine the concentration of ammonia in each solvent by titration. This enables you to
calculate the distribution coefficient, KD.
[NH3(aq)]
KD = [NH ]
3(tce)
Chemicals : 50 cm3 ammonia solution 1M NH3, 1,1,1-trichloroethane CH3CCl3, methyl orange indicator solution,
hydrochloric acid 0.010M HCl (standardized), hydrochloric acid, 0.50 M HCl (standardized)
Apparatus : safety spectacles, measuring cylinder, separating funnel 150 cm3, 2 beakers 100 cm3, pipette 10 cm3 and safety
filler, 2 conical flasks 150 cm3, wash-bottle of distilled water, white tile, burette 50 cm3 and stand
Results :
Introduction : A mixture of unknown amino acids can be separated and identified by means of paper chromatography. The
positions of the amino acids in the chromatogram can be detected by spraying with ninhydrin, which reacts with α-
amino acids to yield highly coloured products.
Chemicals : 2% ammonia, propan-2-ol, aluminium foil, ninhydrin spray (2% solution of ninhydrin in ethanol), separate
solutions of 0.05 M glycine, tyrosine, leucine, and aspartic acid in 1.5 % HCl in 4 test tubes, an unknown
containing one to four of the above amino acids at a concentration of about 0.05 M each in 1.5 % HCl
Procedure : 1. Mix 10 cm3 of 2 % ammonia solution with 20 cm3 of propan-2-ol in a clean, 500 cm3 beaker, and cover tightly
with a piece of aluminium foil. This would be used as the solvent for the experiment. [Hazard Warning:
Propan-2-ol is flammable.]
2. On a clean sheet of chromatography paper with size about 12 cm by 22 cm, mark a light pencil line parallel to
the bottom and about 1.5 cm away (Figure 1). Along this line mark ten light crosses ("×") at intervals of about
2 cm. Label each cross as shown in Figure 1. ("U" represents the unknown amino acid mixture.)
3. Using capillary tubes, place a small amount of each appropriate solution on its two positions along the line on
the chromatography paper. Avoid getting the spot on the paper larger than about 2 mm in diameter. Let the
paper dry for a few minutes in air. Add a second portion of the unknown to one of its two positions, to make
certain that sufficient quantities of each component of the unknown will be present for good visual observation
when the paper is developed.
4. Roll the paper into a cylindrical form. Staple the ends together in such a fashion that they do not touch each
other (Figure 2). Otherwise the solvent will flow more rapidly at that point and form an uneven solvent front.
5. When the spots on the cylindrical paper are dry (it may be necessary to place the paper in an oven at about
100°C for a short time), place it carefully in the beaker of solvent, and cover carefully and tightly with the
aluminium foil. Make sure that the paper does not touch the wall of the beaker.
Let the solvent rise up the paper for at least 1.5 hours. If the time is shorter, the components may not be
sufficiently separated for easy identification. Remove the paper and place it upside down on the desk top to
dry. When most of the solvent has evaporated, open the cylinder by tearing it apart where it was stapled and
hang it in a fume cupboard. Spray the paper lightly but completely with a solution of ninhydrin, and leave the
paper in the fume cupboard until the spray solution is dry.
[Hazard Warning: The ninhydrin solution should be kept off the body because it reacts with proteins in the
skin to form a rather long-lasting purple discoloration. The teacher should ensure that students wear laboratory
gowns, gloves and safety spectacles in carrying the experiment.]
Place the paper in an oven at 100°–110°C for about 10 minutes, or until all the spots have developed.
8. Circle each spot with a pencil, and measure the distance each spot traveled (use the centre of the spot for
measurement). Measure the distance the solvent traveled at each position, and calculate the Rf values for each
amino acid. Determine the composition of the unknown by visual comparison of spot colours and by
comparing the Rf values.