MEWAR INTERNATIONAL

UNIVERSITY (MIU),
MASAKA, NASARAWA
STATE.

DEPARTMENT
OF
INDUSTRIAL CHEMISTRY
EXPERIMENTAL CHEMISTRY
PRACTICAL MANUAL
CHM 107

Dr. IMOISI CHINYERE

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 OBJECTIVE OF THE COURSE

It is hoped that by the end of these series of practical exercises, the students should be able to:

✓ Handle confidently, the analytical balance in routine work in Chemistry

✓ Prepare a standard solution of any given reagent
✓ Carryout a simple preparation of chemical compounds
✓ Carry out elementary quantitative analysis of a given compound
✓ Carryout measurement of pH using pH indicator, paper and pH meter
✓ Carry out chromatography separation technique
✓ Prepare acetyl salicylic acid (aspirin) from salicylic acid
✓ Analysis of tea

GENERAL INSTRUCTION

Each student must provide himself/herself with the following:

1. A white laboratory coats

2. Practical manual
3. A practical science workbook
4. A calculator.

ORGANIZATION OF PRACTICAL PERIODS:

A normal laboratory period is two hours. A student is expected to complete the experimental
work and submit the report within that period.

The students will be divided into groups with a group leader. The group leader will
collect the apparatus needed for the experiment at the beginning of the practical period and
return same at the end of the period.

You are advised to take your laboratory work very serious and also you are advised to
keep your practical notebook if it get lost, it is your fault. Therefore, you should make sure that
at the end of practical period you hand over your practical notebook to your class representative
who will in turn submit to your instructor and will be returned to you in the laboratory through
your class representative for the next practical class after it has been marked. There should be
no account you take your practical notebook home except on the permission of your instructor
only.
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 For easy identification of your practical notebook the following information of the
student should be boldly written on the front page of the notebook and the space provided
inside your notebook for same.

DEPARTMENT:
NAME:
MATRICULATION NO.:
CLASS NO.:
GROUP:
SAFETY REGULATIONS IN THE LABORATORY

Laboratory safety is one of our major concern. For the protection of everyone involved in the
laboratory exercise, the following rules must be strictly followed:

1. Eating, drinking or smoking are forbidden in the lab. except in a case of emergency.
Note that tap water on benches in the lab are not fit for drinking.
2. Running or any hurried physical activity, pranks and practical jokes can cause serious
injury and therefore strictly forbidden.
3. In preparing acid solution, always add acid to water, (A-W) in a slow stream. in the
otherwise, the heat evolved becomes so great that it converts some of the water to
steam, the steam then causes drops of the acid to escape from the mixture which would
causes bodily harm.
4. Burns caused by acid, flush with sodium hydroxide. If it is cause by an alkaline, flush
with lemon juice
5. The tapping of gas from a compressed gas cylinder must be done under the supervision
of the instructor or technologist.
6. Do not go into laboratory without permission.
7. Never take anything from the lab without permission
8. Never interfere with equipment or chemicals
9. Long hair must be tied and cardigans etc. should not be allowed to hang freely.
10. When heating things, use small amounts, and watch very carefully, what you are doing
all the time.
11. Make sure you know exactly what you are supposed to do, if in doubt, ask your
instructor.
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12. All students must wear white laboratory coats to all practical classes, this is strongly
advisable, put it on in the lab; wear safety glasses at when it is recommended in
experiment description. Student must not go barefooted in the laboratory.
13. If any chemical spilled on work bench, cleaned and washed with water so that other
student who touch such place are not hurt.
14. Do not sit on laboratory benches or put your lab. coats, bags and cases etc. on the bench.
15. Chemical must be extremely handled with care since many are poisonous, dangerously
reactive or explosive. Do not test chemical with your tongue.
16. When a substance is to be identified by smell, the vapour should be wafted towards the
nose and sniffed carefully do not look into the open end of a test tube or reaction vessel,
and never point it at another person, because it could be dangerous.
17. Broken or cracked glassware should be carefully cleared and dumped inside a waste-
bin.
18. Never use bare hands to handle hot beakers or crucible; use proper size tongs for the
purpose.
19. In the case of an accident:
a) Remain calm and immediately ask for assistance from your supervisor.
b) Report all injuries to your supervisor
c) Seek medical treatment even from a minor lab. injury.
20. The following first aid measures must be applied:
a) For chemicals in the eye, hold the eye open and flash with water (preferably
using a rubber hose attached to a water tap), continue for at least five minutes.
b) For chemicals spilled on skin, flush with large volumes of water for at least
five minutes.
21. All students must know the location of the first aid box, fire extinguishers and buckets
and also how to use the.
22. Common causes of laboratory accidents:
a) Most lab. accidents are cut from chipped glassware and from broken glass
tubing or thermometers.
b) Burns from concentrated acids and boiling solution
c) Fire (a serious hazard in any lab.) is usually caused by careless handling of
organic solvents and chemicals. Solvents must not be heated using a Bunsen
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 flame nor used in the vicinity of a flame, always use water bath in a case of fire
outbreak, call for fire extinguisher.
23. It is always better to filter a solution while it is still hot
24. Heating over water is preferred to avoid decrepitation.
25. The four major danger in the laboratory are:
1. Cuts and burns 2. Electric shock 3. Fires and explosions and 4. Poisoning

CARE OF THE LABORATORY:

1. All apparatus must be clean and benches must be kept tidy and free of any apparatus
which is not required for immediate use.
2. Reagent bottles must be corked properly and put back in their proper places after used
for their stopper not be interchanged
3. No solid material e.g. pieces of paper or glassware should be dropped into the sink, as
these will block the drainage system, their rightful place is the waste-bin
4. Common reagent must be used at their locations; on no account should they be carried
to private benches
5. If any reagent is spilled on the bench or floor it must be thoroughly washed with plenty
of water and the affected part wiped dry
6. Do not ever pour back unused reagent into the reagent bottle containing the stock
7. Burettes and pipettes must be kept in an inverted position in their stand when not in use
8. Graduated glassware must not be heated or filled with hot or cold liquids. These are
calibrated at room temperature and should be used under such conditions.
9. Above all ask your instructor/technologist/laboratory assistant questions wherever you
are in doubt.

GENERAL LABORATORY PROCEDURE

In carrying out an experiment in the laboratory a summary of work done should be reported
generally in the following order:

i. Title: e.g. acid base titration

ii. Aim: e.g. standardization of sodium hydroxide using standard hydrochloric acid.
iii. Apparatus: a list of non-consumable materials used such e.g. glassware.
iv. Material: list of consumable materials used such as reagents.

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 v. Method or Procedure: the details of how the practical work carried out. This should
be in a reported speech.
vi. Observation: all the changes observed during the course of the reaction or experiment
e.g. changes in color, odour, or taste.
vii. Results: the raw result obtained directly form the experiment.
viii. Calculations: any calculation required for the experiment
ix. Discussion: discussion based on the experiment
x. Conclusion: a final statement of the result and inference on the experiment.

Note that variation of this format exists depending on the nature of the experiment. For
example, a table form is used in qualitative and quantitative analysis. Your instructor will tell
you when a table form is more appropriate. The format is Test/Observation/inference.

LABORATORY NOTE BOOKS

You are provided with note books in which to write up the results of your experiments.
At the end of every practical class, submit your notebooks to your supervisor for assessment.

VOLUMETRIC ANALYSIS

Volumetric analysis involves accurate measurement of volumes of liquid or solutions.

Though one or two weighing may be involved.

STANDARD SOLUTION: A standard solution is the solution whose concentration (i.e. the
number of grammes of mole per litre) is accurately known. Any kind of unit weight or
volume may be used, but most commonly used is the grammes per litre.

STOCK SOLUTION: To save time and space in the laboratory, solutions that are routinely
used is purchased or prepared at a standardized concentrated form called stock solution. That
is a stock solution is a solution that is diluted to some lower concentration for actual use.

DILUTE SOLUTION: Solvent, e.g. water is added to the concentrated solution to achieve
the molarity desired for a particular solution. The process of adding more solvent to a solution
is called dilute while the solution is called a dilute solution.

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NORMAL SOLUTION: A normal solution of a substance is one which contains the gramme
equivalent weight of the substance per litre of solution. It should be noted that for a given
substance the equivalent weight depends on the reaction in which it is taking part.

MOLAR SOLUTION: A molar solution of a substance is one which contains the gram-
molecular weight of the substance per dm3 of solution.

MOLARITY (M): it is the number of moles of solute per dm3 of a solution.

M= Conc. in gramme per dm3

Mass of 1mole of the solution
M= number of mole of solute
1dm3 of solution
INDICATORS: Indicators are organic substance which changes colour as the PH changes.
An indicator shows a wide range of colour in a solution depends on the value of the PH of the
solution. It is used to indicate the degree of alkalinity or acidity of a solution.

The colour changes of some common indicators are given below:

S/N INDICATOR PH ACID ALKALIN NEUTRAL

RANGE COLOUR COLOUR
1 Methyl Orange 3.10-4.4 Red Yellow Orange
(pinkish)
2. Methyl red 4.2-6.3 Red Yellow Purple
3. Phenolphthalein 8.2-10.0 Colourless Red Pink
4. Bromophenol blue 2.8-4.6 Yellow Violet blue
5. Bromothymol blue 6.0-7.6 Yellow Blue
6. Litmus 5.6-7.6 Red Blue Purple
7 Congo red 3.0-5.0 Blue Red

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H+ (aq)/moldm-3 pH CONDITIONS

1.0 0

10-1 1 strongly acidic

10-2 2

10-3 3

10-4 4 weakly acidic

10-5 5

10-6 6 very weakly acidic

10-7 7 neutral

10-8 8 very weakly alkaline

10-9 9

10-10 10 weakly alkaline

10-11 11

10-12 12 very alkaline

10-13 13

10-14 14

LITMUS SOLUTION AND LITMUS PAPER

Litmus solution is a coloured dye. It is extracted from certain plants of the mosses and lichen
species. Litmus paper are made by dipping strips of white blotting paper into litmus solution.
The paper is then dried, cut into narrow strips and bound up into booklets. There are two major
colours of litmus viz: - Red litmus and Blue litmus.

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 QUANTITATIVE ANALYSIS:

There are two types of Classical Quantitative Analysis namely: Gravimetry and Titrations.

Quantitative Classical Chemical Analysis

Gravimetry Titration

Acid-base Precipitation complexometric Redox

TITRATION:

There are four types of titrations:

1. Acid-base titrations
2. Complexometric titrations
3. Precipitation titrations
4. Redox titrations:

Titration is the process by which a solution of a standard reagent of known molarity reacts
with another solution of unknown molarity but known volume. Using the known molarity
and volume of the solutions and the equation of the reaction, the unknown quantity
(concentration or volume) can then be calculated. When a neutralization reaction is carried
out in a quantitative way, the procedure is called an acid-base titration. Titration helps us
to achieved the chemical analysis of certain substances in solution. The following are
necessary in order to achieved a successful titration:

i. Volume must be accurately measured

ii. The standard solutions must react completely with one another
iii. The reaction between the two solutions must be fast
iv. The end-point must be easily detectable

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 ➢ Direct Titration: A reaction between the analyte (the substance whose concentration
or quantity is to be determine. i.e. the unknown solution) and the titrant (known
solution).
➢ Indirect Titration: The analyte forms a compound with the species that reacts with
the titrant.
➢ Back Titration: A known excess of titrant is added to the analyte. The excess of titrant
is titrated with a standard solution. It is used when the molar concentration of an excess
reaction is known but the need exists to determine the strength or concentration of an
analyte. A back titration may also be called an indirect titration
▪ It is done when the reaction occurs very slowly
▪ When the acid or (more commonly) base is an insoluble salt e.g. calcium
carbonate
▪ When direct titration endpoint would be hard to discern e.g. weak acid and weak
base titration.

Two steps are typically followed in a back titration to measure the amount
consumed by the analyte and to calculate the excess quantity:

1. The volatile analyte is permitted to react with an excess reagent

2. A titration is conducted on the remaining quantity of the know solution.

CHOICE OF AN INDICATOR IN TITRATING

i. A weak acid against a strong base, use phenolphthalein
ii. A weak base against a strong acid use methyl orange/methyl red
iii. A strong acid against a strong base use any of the above indicator.

most indicators used in the analysis are weak organic acid or base.

CALCULATION OF MOLARITY OF UNKNOWN SOLUTION USING THE

RELATION;

MaVa/MbVb = na/nb

Ma = Molarity of acid

Mb = Molarity of base

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Va = Volume of acid

Vb = Volume of base

na, nb = Number of moles of reactions a and b respectively as obtained from the stochiometric
equation.

CONCENTRATION (C) of the unknown solution can be calculated with the expression:
Conc (g/dm3) = Molarity X Molar Mass

FORMAT FOR REPORTING VOLUMETRIC WORK

Students should use the format below for presenting the results of their volumetric work

1. Title of Experiment
2. Molarity Calculated for the Standard Solution
3. Procedures:
i. Solution in burette
ii. Volume of Solution in pipette (state the pipette size)
iii. Indicator used
iv. End Point (colour change)
4. Titration Readings

Burette reading (cm3) 1st 2nd 3rd Average volume of

acid used
Final burette reading (cm3)
Initial burette reading (cm3)
Volume of acid used
(differences)
Average readings calculated to within ± 0.10cm3 in range.

5. Calculation
i. Reaction equation (s)
ii. Molarity of the unknown solution using the molarity formula earlier stated
iii. Concentration of the unknown solution using the concentration formula stated
above
iv. Any other quantities required such as the percentage purity of a given sample
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END POINT: The end point, also known as the equivalence point is very important in
volumetric analysis. The endpoint is the point at which exactly equivalent quantities of the
reactants are present. At the point, the total number of moles of the other reactant, that is, the
exact mole ratio required by the balanced chemical equation of the reaction is achieved.
Indicators enable us to detect the end point of a titration.

QUESTIONS:

1. Make a list of all the pieces of apparatus found in your laboratory. Compare your list
of apparatus with those of other students. Carefully rewrite your list, arranging the
items in an alphabetical order?
2. Draw or sketch each piece of apparatus in your laboratory and write a few sentences to
describe the important features and use of the apparatus
3. List the four major dangers in the laboratory?
4. Write short notes on possible cause and prevention of accidents by these methods
5. What should you do in case of any accident in your laboratory?

EXPERIMENT I:

TITRATION BETWEEN ACIDS AND BASES USING STANDARD SOLUTION

A): Titration of a standard acid against a base of unknown concentration

Given: Two solutions are provided, one of them is sodium hydroxide and the other is hydrogen
chloride whose concentration is 0.15M.

PROCEDURE:

STEP I: Rinse a clean burette with distilled water then rinse it again with a few milliliters of
the acid. Clamp it to a retort stand and fill it slightly above the zero mark with the acid. Adjust
the level of the liquid to the zero mark.

STEPII: Clean a 25cm3 pipette and rinse it with a few milliliters of the base. Use it to transfer
a known volume of the base (25cm3) into a conical flask.

STEP III: Add one or two drops of colourless phenolphthalein solution to the base and place
the flask on a piece of white tile (or filter paper) below the burette. Note the colour.

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STEP IV: Allow about 2cm3 of the hydrogen chloride to run into the flask and swirl gently.
Continue to add the acid in small quantities at a time, swirling the flask to ensure proper mixing
of the solutions, until the solution just becomes colourless.

STEP V: Repeat the titration at least twice.

Assuming that the titration values are given on the table below

Burette reading (cm3) 1st Rough 2nd 3rd Average volume of

acid used
Final burette reading (cm3) 22.80 41.3 22.80
Initial burette reading (cm3) 0.00 22.80 0.00
Volume of acid used
(differences)

Find the following

QUESTIONS:

I. Find the average volume of hydrogen chloride acid used.

II. Write the balance equation for the reaction (HCl + NaOH → NaCl + H2O)
III. Calculate the molarity of the base
IV. What is the concentration (strength) of the base in g/dm3?
V. What are the precautions.

SOLUTION:

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B): Titration of unknown concentration against a standard base solution

Given: Two solution A and B. Solution A is tetraoxosulphate (VI) acid of unknown

concentration and solution B is base which is a 0.039M sodium hydroxide. Methyl orange
indicator

Assuming that the titration values are given on the table below

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 Burette reading (cm3) Rough 2nd 3rd Average volume of
acid used
Final burette reading (cm3) 23.80 21.30 19.10
Initial burette reading (cm3) 0.00 1..80 0.00
Volume of acid used
(differences)
Find the following:

I. What is the volume of the tetraoxosulphate (VI) acid used?

II. Write a balance equation for the reaction
III. Calculate the molar concentration of the base
IV. Calculate the molarity of the acid
V. What is the concentration (strength) of the acid in g/dm3?
VI. State the percussions

SOLUTION:

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C): To compare the volume of standard hydrogen chloride required to neutralize a given
volume of sodium trioxocarbonate (IV) solution when (a) methyl orange and (b)
phenolphthalein are used respectively as indicator

Given: 0.1M solution of standard hydrogen chloride acid and a solution of sodium
trioxocarbonate (IV). Methyl orange and phenolphthalein indicator are used.

Procedure: Titrate the acid against the base. First of all, use methyl orange as indicator, then
repeat the set of titrations using phenolphthalein as indicator.

Tabulate your result.

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Assuming that the titration values are given on the table below when methyl orange indicator
was used

Burette reading (cm3) 1st 2nd 3rd Average volume of

acid used
Final burette reading (cm3) 25.80 24.45 26.80
Initial burette reading (cm3) 0.00 0.00 1.15
Volume of acid used
(differences)

Assuming that the titration values are given on the table below when phenolphthalein indicator
was used

Burette reading (cm3) 1st 2nd 3rd Average volume of

acid used
Final burette reading (cm3) 11.23 13.39 27.00
Initial burette reading (cm3) 0.00 1.15 13.39
Volume of acid used
(differences)
QUESTIONS:

I. Write equation for each of the reaction

II. What is the molarity of the trioxocarbonate (IV) solution when methyl orange indicator
is used?
III. Calculate the strength of the trioxocarbonate (IV) solution when methyl orange
indicator used?
IV. Compare the volume of acid required to neutralize 25cm3 portion of the sodium
trioxocarbonate (IV) solution in each of the titrations
V. How do you explain your observation in question 4 above?
VI. State the precautions

SOLUTION:

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17
D): A is a solution containing 6.00g/dm3 of trioxonitrate (V) (HNO3) acid. B is a solution
of hydrogen sodium trioxocarbonate (IV) (Na2CO3.XH2O), containing 4.00g/dm3 of the
trioxocarbonate (IV).

Procedure: Put solution A into the burette and titrate 25cm3 or 20cm3 portion of B using
methyl orange as indicator.

Record the volume of your pipette and tabulate your burette readings.

Assuming that the titration values are given on the table below

Burette reading (cm3) 1st Rough 2nd 3rd Average volume of

acid used
Final burette reading (cm3) 23.70 45.30 23.70
Initial burette reading (cm3) 0.00 23.70 0.00

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Volume of acid used 23.70 21.60 23.70
(differences)
Find the following

QUESTIONS:

I. Calculate the average volume of the acid used

II. Write the equation of the reaction
III. The molarity of B
IV. Calculate the number of molecules(X) of the water of crystallization in Na2CO3.XH2O.
V. The percentage by mass of water of crystallization in Na2CO3.XH2O.
(H = 1.0, C=12.0, N=14.0, O= 16.0 Na=23.0)
SOLUTION:

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 EXPERIMENT II:

USE OF THE ANALYTICAL BALANCE

INTRODUCTION: One of the most common operations in practical chemistry is weighing.

Weighing (determination of mass) is carried out with the aid of a weighing balance. All
balances operate on the same principle: comparing the mass of the unknown with a known
mass.

EXERCISE:

a. The instructor in charge will demonstrate the use of the two-pan beam balance.
b. Each group of students shall be provided with a number of solid objects of unknown
mass.
c. Working in turns, each group member shall weigh the samples provided for the group
d. Recording of results: for each object weighed, all masses used to balance the mass of
the objects weighed shall be tabulated. An example is shown below
e. Presentation of the experimental result: Title and date of the experiment

S/N Example: Unknown Sample Number Masses (g)

1. X1 12.000
2. X2 9.000
3. X3 3.000
4. X4 0.200
5. X5 0.010
Total Masses (g)

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QUESTION: weigh all the mass and calculate the total masses and the average mass

SOLUTION:

S/N Unknown Sample Number Masses (g)

1. X1
2. X2
3. X3
4. X4
5. X5
Total Masses (g)

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 EXPERIMENT III:

PREPARATION OF STANDARD SOLUTIONS

INTRODUCTION

Commercial acids are usually bought from manufacturers in highly concentrated forms
therefore there is need to reduce the concentrations of the commercial acids for daily laboratory
use. Certain basic information is necessary to enable one to reduce the concentrations of a
commercial acids. The information is supplied by the manufacturer written on the labels pasted
on the bottles. This information must be looked at before accepting any commercial acid into
the stock room. These facts are:

1. The percentage of the pure acid in the commercial acid. These acids are not 100% pure
acid. They contain some amount of impurities and water.
2. The specific gravity or density of the acid. For example, the figures mostly seen on the
bottles are shown below

S/N ACID % OF PURE RELATIVE DENSITY

ACID
1. HCl 32% - 36% 1.18g.cm-3
2. H2SO4 96% - 98% 1.84 or 1.86gcm-3
3. HNO3 65% - 72% 1.42gcm-3
4. CH3COOH 99% - 99.5% 1.047 – 1. 052g.cm-3

Bench acids are usually 2moldm-3 in strength. Standard acids of various molarities e.g.
1moldm-3, 0.1mol.dm-3, 0.02moldm-3 0.05moldm-3 etc. are frequently used for acid-base
titrations. Note that the molar mass of the acid must be known.

In preparing stock solutions unlike alkalis and salt which can be weigh, the problem is that it
is not possible to weigh acid solutions due to experimental difficulties and the fact that they
are not usually one hundred percent pure and their specific gravities are not 1gcm-3.

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1A): what volume of commercial H2SO4 must be dissolved in 1dm3 of water in order to get
0.5moldm-3 H2SO4? The relative density and percentage purity of the commercial acid are
1.84gcm-3 and 96% respectively.

Solution:

EQUIPMENT:

1. Measuring cylinder
2. Beaker
3. 1000ml of volumetric flask
4. Distilled water

1 mole of H2SO4 is 98g dissolved in 1dm3 water = 1moldm-3

0.5 moles of H2SO4 i.e. 49g dissolved in 1dm3 water = 0.5moldm-3

In order to prepare a 0.5moldm-3 H2SO4. 49g of the acid are required per 1dm3 of water.

The % purity of the acid is 98%. That means 98 parts of pure H2SO4 are in 100 parts of
commercial acid

∴ 49 parts of pure H2SO4 are in 100 X 49

98
= 50 parts of commercial acid

The relative density of the acid is 1.84gcm-3, that means 1.84 parts of pure H2SO4 are in 1cm3
of commercial acid

∴ 1 part of pure H2SO4 is in 1/1.84

50 parts of pure H2SO4 are in 1 X 50 cm3

1.84
= 27.2cm3/dm3

OR. (0.5moldm-3 of H2SO4/Relative density/% purity) X 100

= (0.5X98/1.84/98) X 100 = 27.2cm3 dm-3

27.2cm3/dm3 of the commercial acid will have to be measured out and dissolved in 1dm3 of
distilled water to get a 0.5moldm-3 H2SO4.
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 Usually several volumes of this bench acid are needed to go around the entire class.

If 10dm3 of this are needed to go around the class. Therefore, 27.2cm3/dm3 X 10cm2 = 272cm3
(i.e. 0.272dm3) of the commercial acid is dissolved in 10dm3 of water. On the other hand, if a
250cm3 volumetric flack is to be used for the preparation of the 0.5moldm-3 H2SO4 to be used
on a small scale, then one quarter of 27.2cm3 (27.2cm3/4) = 6.8cm3 of the commercial acid
must be dissolved in the 250cm3 flask.

Reasons: 1000cm3 (1dm3) of water require 27.2cm3

250cm3 of water will require 27.2 X 250

1000 1
i.e. 27.2/4 = 6.8cm3 or 27.2 X 0.25 = 6.8cm3

Note that the concentration of the solution is exactly 0.5moldm-3 as the concentration is a little
different. To calculate the exactly concentration of your solution from the masses you used to
prepare your solution:

m = n X M = CVM

n= CV

C = n/V = m/M/V

C = concentration

C = n/V

Label your solution to avoid confusion include the solute formula, the exact concentration of
your solution prepared, date, and your name.

Alternatively: C1V1 = C2V2 equation is used if the molar concentration of the commercial
stock acid is known against the relative density and the percentage by mass. As shown below:

Substance Conc. (moldm-3) % by mass Relative density

Conc. H2SO4 acid 18 98 1.84
Conc. HCl 12 36 1.18

B): Preparation of 0.5mol.dm-3 of H2SO4 in 1dm3 flask from commercial H2SO4.

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SOLUTION:

C1 = 18 given

V1 = volume of commercial acid requires

C2 = 0.5mol.dm-3

V2 = 1000cm3 (1dm3)

∴ (18) (V1) = (0.5) (1000)

V1 = 0.5 X 1000/18

= 27.8cm3/dm3

Note that the value obtained is very close with the first method

C): Preparation of 0.5molar solution of H2SO4 in 1dm3 flask from commercial H2SO4.

EQUIPMENT:

1. Measuring cylinder
2. Beaker
3. 1000ml of volumetric flask
4. Distilled water

PROCEDURES:

Step 1.

Wash the glassware (pipette, beaker, measuring cylinder and 1000ml of volumetric flask) with
distilled water and dry in oven.

Step 2.

1ml = 1.00 cm3 = 0.001dm3

Calculate the amount by volume of the commercial acid needed to be dissolved in 1dm 3 of
distilled water.

From the calculation above, 27.2cm3/dm3 of the commercial acid will have to be measured out
and dissolved in 1dm3 of distilled water to get a 0.5moldm-3 H2SO4.

26
Step 3.

➢ Take 500ml of distilled water in 1000ml (1dm3) of volumetric flask

➢ Carefully measure out 27.2cm3/dm3 H2SO4 with measuring cylinder in 500ml distilled
water
➢ Make up with dilled water up to mark of 1000ml volumetric flask.

The solution in the 1000ml of volumetric flask is 0.5 molar solution of H2SO4.

2): what volume of commercial HCl must be dissolved in 1dm3 of water in order to get
0.15mol.dm-3 HCl? The relative density and percentage purity of the commercial acid are
1.18gcm-3 and 36% respectively.

Solution:

1 mole of HCl is 36.5 dissolved in 1dm3 water = 1mol.dm-3

0.15moles of HCl i.e. 5.5g dissolved in 1dm3 water = 0.15mol.dm-3

In order to prepare a 0.15mol.dm-3 HCl 5.5g of the acid are required per 1dm3 of water.

The % purity of the acid is 36%. That means 36 parts of pure HCl are in 100 parts of
commercial acid

∴ 5.5 parts of pure H2SO4 are in 100 X 5.5

36.5
= 15.1 parts of commercial acid

The relative density of the acid is 1.18gcm-3, that means 1.18 parts of pure HCl are in 1cm3 of
commercial acid

∴ 1 part of pure HCl is in 1/1.18

15.1 parts of pure HCl are in 1 X 15.1 cm3

1.18
= 12.8cm3/dm3

12.8cm3/dm3 of the commercial acid will have to be measured out and dissolved in 1dm3 of
distilled water to get a 0.15mol.dm-3 HCl.

27
 EXPERIMENT IV

PREPARATION OF STANDARD ALKALI SOLUTIONS

INTRODUCTION: In preparing alkali solutions, unlike acidic solutions there are no much
difficulties in the sense that most alkalis are in solid form, they can be weighed directly by
using a chemical balance, electric balance or triple beam balance except ammonium hydroxide
i.e. ammonia in water (aqua ammonia) which is a colourless liquid.

Procedure:

i. calculate the mass of the alkali that will be needed to prepare the required standard
solution per dm3.
ii. Clean a graduated flask, wash well with water and then with distilled water.
iii. Weigh your watch-glass and record the mass
iv. Put the calculated amount of the solute on a watch-glass and weigh the watch-glass and
the contents and record the mass
v. Subtract the mass of watch-glass from the mass of watch-glass + the content to obtain
the accurate mass of the solute.
vi. Put the measured solute in a beaker add distilled water and keep steering with a glass
rod until the solute completely dissolved, rinse the glass rod into the beaker to ensure
that no solution is remaining on the glass rod.
vii. Using funnel transfer the solution into a graduated flask, rinse the beaker into the flask.
viii. Then add distilled water and shake the flask
ix. Add more distilled water to mark up to the mark of the flask and shake thoroughly.
x. The bottom of the water meniscus must be on the graduation mark. If your liquid level
exceeds the line, your solution is of unknown concentration and cannot be used.

Note: if a large group is being prepared for multiply that mass by number of dm3 of solution
required

Precaution:

i. ensure that during and after the process of dissolving the solute, no portion is lost either
by drop or drops splashing out.

28
 ii. Follow the simple method of pouring a solution into a flask or aspirator by carefully
using glass rod and funnel to avoid loss
iii. Ensure that the glass material used in dissolving the solute and the funnel used are
rinsed.
iv. Some alkalis e.g NaOH is corrosive and can cause chemical burns. Do not touch NaOH.
v. Wear safety goggles and gloves
vi. If you get NaOH on your skin, immediately rinse with a large volume of water.

A): Preparation of 2mol.dm-3 NaOH solution

Solution

Molar Mass of NaOH = 40g

1 mol.dm-3 NaOH contains 40g/dm3

2 mol.dm-3 NaOH will contain 2x40g = 80g/dm3

Therefore, 80g of NaOH will be dissolved in 1dm3 of distilled water

For 10dm3 solution 10x80g = 800g of NaOH will be dissolved in 10dm3

How many gramme of NaOH will be needed for 500cm3

1000cm3 = 1dm3

80g is needed for 1dm3

Therefore, 80g/dm3/2 = 40g

For 500cm3 = 40g

For 250cm3 = 20g

Note that sometimes the concentration of the solution is not exactly 2moldm-3 as the weight
mass, there may be a little different, hence always calculate the concentration of the solution.
To calculate the exactly concentration of your solution from the masses you used to prepare
your solution:

m = n X M = CVM

n= CV
29
C = n/V = m/M/V

C = concentration

C = 80/40/1 = 2mol/dm3

Label your solution to avoid confusion include the solute formula, the exact concentration of
your solution prepared, date, and your name.

B): Preparation of 0.05 moldm-3 washing soda (Na2CO3.10H2O)

Solution: Molar Mass 106 + 180 = 286g

0.05 moldm-3 will contain 0.05 x 286g/dm3 = 14.3 g/dm3

Therefore, 14.3g of Na2CO3.10H2O will be dissolved in 1dm-3 of distilled water.

-For 25dm3 solution the mass of the solute required = 25x14.3 = 357.5g will be needed for
25dm3.

-For 250cm3 solution. The mass of the solute needed = 14.3/4 = 3.6g/250cm3

i.e. 3.6g of the solute will be dissolved in 250cm3 of distilled water

NB. 1000cm3 = 1dm3

EXERCISES:

1. Calculate the volumes of commercial HNO3 fuming, that would be needed to prepare:
a. 2mol.dm-3 solution per dm3
b. 0.2mol.dm-3 solution per 10dm3
c. 0.05 mol.dm-3 solution per 500cm3
d. 0.03 mol.dm-3 solution per 250cm3

Given that the relative density of the acid is 1.42gcm-3 and the percentage w/w is 72%

2. Calculate the volumes of commercial HCl fuming, that would be needed to prepare:
a. 2mol.dm-3 solution per dm3
b. 0.2mol.dm-3 solution per 10dm3
c. 0.05 mol.dm-3 solution per 500cm3
d. 0.03 mol.dm-3 solution per 250cm3

30
Given that the relative density of the acid is 1.18gcm-3 and the percentage w/w is 36%

3. If the concentration in mol.dm-3 of glacial ethanoic acid is 19, the specific gravity is
1.05 and its percent w/w is 99.5%. calculate the molar concentration of a 20cm3 of the
commercial acid if it is dissolved in
a. 1dm3 b. 250cm3 c. 3.3dm3
4. What is the molar concentration of 2 mol.dm-3 H2SO4 when a dm3 of it is diluted to
100dm3?
5. What mass of Na2CO3.10H2O would be needed to prepare
i. 0.1mol.dm-3 solution
ii. 2 mol.dm-3 solutions for 5dm3
iii. 0.05mol.dm-3 solution for 200 students with 150cm3 each

31
 EXPERIMENT V

INTRODUCTION TO IODOMETRIC AND IODIMETRIC TITRATIONS

At the end of this section you will be able to identify the type of samples, standard solution,
indicator and reactions involved in iodometric and iodimetric titrations

Quantitative Classical Chemical Analysis

Gravimetry Titration

Acid-base Precipitation Complexometrc Redox

Permanganimetric Dichromatometric Titrations involving Iodine (I2)

Iodimetry

Iodometry

Iodimetric Titration of Copper

Permanganimetric and dichromatometric: are redox titrations. The difference between both
is the titrant. In permanganimetric methods the titrant is potassium permanganate (KMnO4)
Why in dichromatometric methods the titrant is potassium dichromate (K2Cr2O7).

Gravimetry is not widely use. Titrations are more fast and they are widely use in chemical
laboratories. There are four types of titrations: acid-base, complexometric, precipitation and
redox.

REDOX TITRATIONS
32
Iodine can be involved in redox titration in two ways: iodometric and iodimetric.

IODIMETRY TITRATION: When iodine titrant (standard solution of iodine I2) is titrated
directly with a reducing agents (Analyte) such as Na2S2O3 or active metals, the method is called
Iodimetry.

that is in iodimetry titration, the analyte is a reducing agent and the titrant is iodine. The
reducing agent is the substance that reduces species. In this case, the reducing analyte reduces
iodine to iodide that is one of the products. These are direct titrations, consequently, there is
only one step reaction between the analyte and the titrant.
Analyte + Titrant (iodine I2) → product (iodide I-)
unknown know
EXAMPLE I: Quantification of Ascorbic Acid (Vitamin C)
Iodine rapidly oxidizes ascorbic acid, C6H8O6, to produce dehydroascorbic acid, (C6H6O6).
C6H8O6 + I2 → C6H6O6 + 2I- + 2H+
IODOMETRY:
In this titration, the iodine (I2) is produced when an oxidizing analyte e.g. KIO3, KMnO4 or
K2Cr2O7 is added to excess I- (iodide e.g. KI).
Then the iodine (I2) produced is usually titrated with standard thiosulfate solution.
Iodometry is not a direct titration because it involves two steps reactions:
• analyte + I- (iodide) → I2 (unknown)
• I2 + titrant (standard thiosulfate) → product Known
Example 2: Quantification of Copper or Potassium
2Cu2+ + 4I- → 2CuI + I2
I2 + 2S2O32- → 2I- + S4O62-
Cu is the analyte of unknown concentration
sodium thiosulfate (Titrant-standard solutions) is the known concentration
Iodimetric titrations:
a) A reducing analyte
b) One step reaction
c) Standard solution is Iodine (I2)
Iodometric titrations:
a) An oxidizing analyte

33
b) Two step reactions
c) Standard solution is Sodium thiosulfate

INDICATOR FOR IODIMETRY AND IODOMETRY TITRATION:

Soluble starch is the indicator used in both case. The indicator is added prior to the end-point
in the titration process just when the brown colour of the iodine solution or liberated iodine
changed to pale yellow, giving a blue-black colouration unto the mixture in the conical flask.
As the reaction proceeds, the iodine would be consumed by the reducing agent from the burette.
At the end-point when there is no more iodine, the solution turns to colourless.
Note:
1. starch is not added at the beginning of the titration because it forms a water-soluble
complex with iodine and there is the possibility of absorption of some of the iodine on
the starch.
2. since iodine solution attacks rubber, if the solution has to be in a burette, the burette
must be one with glass stop-cock and not the Mohr`s burette.
3. An analytical or electrical balance should not be used to weigh iodine except with a
rough balance on a watch glass because iodine vapour attacks metals, thereby
interfering with the sensitivity of the balance.

APPLICATONS OF IODIMETRY AND IODOMETRY:

1. Determination of Copper in an ore
2. Analysis of hydrogen peroxide
3. Determination of Lead
4. Determination of available chlorine in bleaching powder
5. Determination of iron (III)
6. Determination of tin
7. Determination of iodides
A): Standardization of Na2S2O3 solution with iodine.
Principles: sodium thiosulfate Na2S2O3 contains five molecules of water of crystallization, it
is hydrated, hence is it not a primarily standard as it results of this water molecules it contains,
its efflorescent and the exact amount of water it contains is not certain. It can be standardized
by a solution of iodine dissolved in potassium iodide.
34
SOLUTION:
STEP I. calculate the masses of I and 2Na2S2O3. 5H2O per 1dm3
I2 + 2Na2S2O3. 5H2O → 2I- + S4062-
Molar Mass (2x127g) (2x248g)
254g 496g
Molar Ratio 1 : 2
∴ I2 = 0.05 Na2S2O3 = 0.1
254 X0.05 248X0.1
12.7g/dm3 24.8g/dm3
12.7g/1000dm3 24.8g/1000dm3
4 4
∴ 3.175g/250cm3 6.2g/250cm3

STEP II
PROCEDURE:
1. Weigh between 3.1g and 3.2g of iodine (I2) in a stoppered glass weighing bottle.
2. Weigh separately 20g of potassium iodide and dissolve it in about 100cm3 of distilled
water
3. Dissolve the iodine in the potassium iodine solution and make up to the mark (250cm3)
with distilled water.
4. Weigh 6.2g of Na2S2O3 and dissolve in the recently boiled water and make up to the
mark with the boiled water.
Note that Boiled water is used because of the CO2 dissolved in water and bacteria action
which cause the slow decomposition of Na2S2O3
STEP III
TITRATION:
• After the preparation, add two to three drops of chloroform or 10mg of mercury(II)
iodide per cm3 to check the effects.
1. Measure 20cm3 or 25cm3 portion of the standard iodine solution with pipette into a
conical flask.
2. Put the Na2S2O3 in a burette and titrate with 20cm3 or 25cm3 portion of the standard
iodine solution and note the average titre value.
35
 3. Add 2cm3 (2 or 3 drops) of starch indicator, when the solution turns yellow,
continue the titration until the blue-black colouration is discharged at end point.
4. Note your readings and calculate the average titre value
STEP IV
CALCULATIONS/RESULTS
The mass of iodine dissolved in 250cm3 = 3.18g
Volume of pipette = 20cm3
Let’s take the average titre value = 19.60cm3
Molar Conc. of iodine = n/v = m/M/V
1000cm3 = 1dm3
250cm3 = 4dm3
∴ 3.18/254/250
= 0.00005mol.cm-3 = 0.00005 x 1000 = 0.05mol
1000cm3 of iodine contain 0.05mole
20cm3 of iodine contain = 0.05 x 20 x 1
1000 1
= 0.001mol

∴ 20cm3 of iodine contain 0.001 moles

Molar Conc. of Na2S2O3 = m/M/V
= 6.2
496
250
= 0.00005mol.cm = 0.00005 x 1000 = 0.05mol.dm-3
3

1000cm3 of Na2S2O3 contain 0.05 moles

20cm3 of I2 = 19.6cm3 of S2O32-
1000cm3 Na2S2O3 = 0.05 x 20 x 2 mole
1000 1 1
= 0.002mol

19.6cm3 Na2S2O3 contain = 0.05 x 20 x 2 x 1000

1000 1 1 19.6

∴ 19.6cm3 Na2S2O3 = 0.102mol.dm-3 S2O32-

B): Estimation of copper in CuSO4 by the use of standard iodine solution and Na2S2O3.
STEP I

36
PRINCIPLES: Copper (II) ion reacts with the iodide ion to form Copper (I) iodide with the
liberation of iodine which is titrated with Na2S2O3 solution.
2Cu2+ + 4I- → 2CuI(aq) + I2
I2 + 2S2O32- → S4O62- + 2I-
2S2O32- : I2 : 2Cu2+
2mole 1mole 2mole
0.10 0.05 0.10
2Na2S2O3.5H2O : I2 : CuSO4 5H20
Molar Mass (2 x 248g) 254g (2 x 249g)
496 254 498
0.1x 248 0.05x254 0.1 x 249
24.8g/dm3 12.7g/dm3 24.9g/dm3
6.2g/250cm3 3.175g/250cm3 6.22g/250cm3
STEP II
PROCEDURE:
1. Weigh between 3.1g or 3.2g of iodine in a well stoppered glass weighing bottle.
2. Weigh separately 20g of potassium iodide and dissolve it in about 100cm3 of distilled
water
3. Dissolve the iodine in the potassium iodine solution and make up to the mark (250cm3)
with distilled water.
4. Prepare approximately 0.1mol/dm3 solution of Na2S2O3 and CuSO4. Weigh 6.2g of
Na2S2O3 and dissolve in 250cm3 volumetric flask and 6.225g of CuSO4 in another
250cm3 of volumetric flask.
STEP III
TITRATION:
1. Measure 20cm3 or 25cm3 portion of the CuSO4 solution with pipette into a three
conical flask.
2. Add Na2CO3 solution to each flask until a slight blush-green precipitate of basic
Copper (II) trioxocarbonate (IV) is formed.
2CuSO4 + 2Na2CO3 → CuO.CuCO3 + 2Na2SO4 +
CO2
Na2CO3 is added because Cu2+(aq) is acidic due to hydrolysis.
37
 3. The mixture in the flask is then acidified by adding ethanoic acid drop by drop until
the precipitate dissolves and a clear blue solution is obtained.
The ethanoic acid set free the cu2+ ions which then react with the iodide ions to liberate iodine.
4. pipette 20cm3 of 10% potassium iodide to the Cu2+(aq) in each flask and titrate the
liberated iodine with Na2S2O3 in the burette.
5. Titrate the Na2S2O3 against 20cm3 of the 0.05 mol/dm3 standard iodine solution.

STEP IV
RESULT/CALCULATION:
a. Molar Conc. of iodine solution = 0.05mol.dm-3
Volume of iodine solution used = 20cm3
Let’s take the average litre value of Na2S2O3 solution = 17.35cm3
b. Volume of CuSO4 solution = 20cm3
Average volume of Na2S2O3 solution = 19.69 cm3
CiVi = ns
CsVs ns
Let molar conc. of iodine solution be Ci
Volume of iodine solution be Vi
Molar conc. of Na2S2O3 solution be Cs
Volume of Na2S2O3 solution be Vs
Molar Ratio of I to Na2S2O3 = 1 : 2
∴ CiVi = 1
CsVs 2
(0.05) (20) = 1
Cs x 17.35 2

Cs = 0.05 x 20 x 2 = 0.115mol.dm-3
17.35

Molar ratio of S2O2- : Cu2+ = 1 : 1

Ccu. Vcu = ns
Cs. Vs ns
Ccu (20) = 1
(0.115)(19.69) 1

Ccu = (0.115)(19.69) = 0.113mol/dm3

38
 20
Conc. of CuSO4 in g/dm3 = 0.113 x 249
= 28.14g/dm3
CuSO4(aq) → Cu2+ + SO42+
1mole 1mole 1mole
Mass conc. of Cu2+ ions = 0.113 x 63.5
= 7.18g/dm3
% of Cu2+ in the sample = 7.18 x 100 = 25.499%
28.14 1

39
 EXPERIMENT VI
MEASUREMENT OF pH
The pH value of a solution is a measure of the concentration of hydrogen ions in the solution.
The Sorensen’s method, pH is defined as
pH = - Log10 [H+] = Log10 1/[H+].
According to the definition of pH, we have pH = - Log10 [H+] = -Log [10-7] i.e. pH = 7
This is the pH of pure water, which defines our standard of pH for a neutral solution.
If we add hydrogen ions to water, e.g. by pouring in hydrochloric acid, so that the
hydrogen ion concentration increases to 0.1mol dm-3 at equilibrium then. pH = - log (10-1) =1.
This shows that the pH of an acidic solution is less than 7.
On the other hand, if we pour alkali into water, the water equilibrium will shift to the left
in order to “Mop Up” the added hydroxide ions. That is, the concentration of hydrogen ions
will decrease. If we assume that in an alkali like sodium hydroxide. Solution the concentration
of hydroxide ions is 0.1mol dm-3 (10-1 moldm-3) we shall have (H+(aq)] x [10-1 Moldm-3] = 10-
14
moldm-3. So [H+ (aq)] = 10-13 mol dm-3 and pH = 13. This shows that the PH of an alkaline
solution is more than 7.

HOW pH VARIES WITH HYDROGEN ION CONCENTRATION

pH values are measured with figures ranging from 0 to 14. On this scale, the pH of a neutral
solution e.g. pure water is 7. pH value below 7 indicate acidity increasing down wards while
pH values above 7 indicate alkalinity increasing upw

ards.
H+ (aq) / mol dm-3 pH CONDITIONS

1.0 0

10-1 1 strongly (lightly) acidic

10-2 2

10-3 3

10-4 4 weakly acidic

40
 10-5 5

10-6 6 very weakly acidic

10-7 7 neutral

10-8 8 very weakly basic

10-9 9

10-10 10 weakly basic

10-11 11

10-12 12 very basic

10-13 13

10-14 14

pH SCALE

(H+)/ mol dm3

10-1 10-2 10-3 10-4 10-5 10-6 10-7 10-8 10-9 10-10 10-11 10-12 10-13 10-14

0 1 2 3 4 5 6 7 8 9 10 11 12 13 14

Increasing Increasing
Acidity
Alkalinity
Strongly mildly neutral mildly strongly
Acidic acidic alkaline alkaline
CALCULATIONS

Example I: find the pH in which the hydrogen ion, H+ concentration is 6.38 x10-6 moldm-3

solve

pH = - log10 [H+]
41
 = - log10 6.38 + 6

= - 0.805 + 6

= 5.195 = 5.2

2. Calculate

1. The pH of a solution 0.020m in H+

2. The pH of a solution 2.5 x 10-3 m in 0H-

Solve

(1) (H+) =0.020m = 2.0 x 10-2 m

pH = - log10 (H+) = - log (2.0 x 10-2) = - (0.3 – 2.0) = 1.7

2. By definition (H+) x (0H-) = 10-14

∴ H+ = 10-14 / (OH-)

= 10-14 = 4.0 x 10-12 ∴ pH = - log10 (4. 0 x 10-12) = - (0.6-12.0) =11.4

1.5 x 10-3

A) DETERMINATION OF pH OF VARIOUS SOLUTIONS USING pH PAPER,

UNIVERSAL INDICATOR AND pH METER
AIM: To find the pH of
1. Dilute HCl
2. Dilute solution of NaOH
3. Dilute solution of acetic (ethanoic) acid
4. Lemon juice
5. Water
6. Dilute solution of sodium bicarbonate (NaHCO3)
By using (A) pH paper (B) universal indicator solution.

42
REQUIREMENTS: Test tube, test tube stand, dropper, white glazed tile, pH paper or
universal indicator solution, pH paper, pH meter, distilled water and solution of given samples.

(I) USING pH PAPER

PROCEDURE:
i. Take six clean and dry test tubes
ii. Label the test tubes as A, B, C, D, E, and F and place them in order in a test tube stand.
iii. Take 10ml of each given sample in the test tubes,
iv. Place a small piece of pH paper (about 2cm) on a white glazed tile.
v. With the help of dropper, transfer 1 to 2 drops of dil. HCl from test tube A on the pH
paper. Observe the colour developed on pH paper and compare it with the colours in
the chart on the cover of the pH paper booklet.
vi. Repeat the same procedure for other samples and note their pH in the observation table.
RESULT:
OBSERVATION TABLE:

S/N SAMPLE COLOUR APPROXIMATE

PRODUCED pH
1 Dil. HCl Red 1
2. Dil. Solution of NaOH Purple 14
3. Dil. Solution of CH3COOH Yellow 6
4. Lemon juice Orange 2
5. Water Green 7
6. Dil. Solution of NaHCO3 Blue 9

(2) BY USING UNIVERSAL INDICATOR:

PROCEDURE:
i. Take six clean and dry test tubes
ii. Label the test tubes as A, B, C, D, E, and F and place them in order in a test tube stand.
iii. Take 10ml of each given sample in the test tubes,

43
 iv. Add 2 drops of BDH (British Drug House) universal indicator with the help of a
dropper to each test tube. Observe carefully the colour in each test tube and match it
with pH paper booklet or pH chat.

RESULT:
OBSERVATION TABLE:
S/N SAMPLE COLOUR APPROXIMATE
PRODUCED pH
1 Dil. HCl Red 1
2. Dil. Solution of NaOH Purple 14
3. Dil. Solution of CH3COOH Yellow 6
4. Lemon juice Orange 2
5. Water Green 7
6. Dil. Solution of NaHCO3 Blue 9
INFERENCE:
1. Acid samples with pH less than 7
2. Basic samples with pH greater than 7
3. Neutral samples with pH = 7

(3). USING A DIGITAL pH METER

pH meter can be small handheld or a larger stationary pH meter
Part of A pH Meter Include
a. The meter which allow the electrode to be easily move down into a beaker for the
sample to be tested
b. The arm
c. The electrode
The electrode of the pH meter needs to be stored properly, cap in a moist solution to prevent it
from drying out. The electrode must be rinsed using distilled water after used for each sample
solution.
STEP 1.
The pH meter must be calibrated using standard buffer solution of pH 4, pH 7 and pH 10.
44
Prepare Standard Buffer Solution: dissolve one tablet of pH 4 in 100ml of distilled water,
repeat same for pH 7 and pH 10.
Note that your pH meter has procedure for calibration, to calibrate your pH meter you will
need to know and follow proper procedures
In the process of calibration using the standard of pH 7 once the standard is calibrated remove
the pH 7 sample and rinsed the electrode with a distilled water, repeat the process using
standard of pH 4 and pH 10 when the pH standards are calibrated rinsed off the electrode with
distilled water. Note that the PH meter must be calibration each time, to ensure sample accurate
measurement using three different pH standards to provide a wide range of accuracy.
STEP 2.
Place the unknown sample solution beneath the electrode by slowing lowering the arm of the
electrode until it finally submerge in the solution. Take the reading from the pH meter and
record it, once the reading is complete remove your sample, once again rinsed the electrode
with distilled water repeat for another sample etc.
After your experiment, rinse the electrode with distilled water, replace the electrode protected
cap.

45
 PART 2.
EXPERIMENTAL VII
PAPER CHROMATOGRAPHY
PURPOSE/GOAL:
Students will be able to:
• Gain understanding of the purpose of chromatography.
• Measure and graph pigment separation.
• Use evidence gathered from the chromatograms to support their conclusions about which
suspects can be excluded from suspicion based on evidence.
• Understand that the separation of dye molecules in chromatography is a physical property of
the dye and movement of the dye is unique for each different dye molecule.
• Defend their conclusions about the dyes based on the evidence that they gathered.
What is Chromatography?
Chromatography is a laboratory method that is widely used for the separation, identification,
and determination of chemical components of a complex mixture. More specifically,
chromatography separates compounds based on differences in their structure, size, and/or
composition. Analytical chemist uses chromatography to conduct qualitative analysis (identify
the components) and quantitative analysis (determine the concentration) of unknown
substances. No other separation method is as powerful and generally applicable as
chromatography.

How Does Chromatography Work? There are numerous different chromatography

techniques; however, they all use a stationary phase and mobile phase. The part that stays in
one place is called the stationary phase, and the part that moves is called the mobile phase.
Components of a mixture are carried through the stationary phase by a flow of a gaseous or
liquid mobile phase. Each sample will migrate through the stationary phase at a different rate.
PAPER CHROMATOGRAPHY: uses paper strips or sheets as the adsorbent stationary
phase through which a solution flows and that is used specially to separate amino acids.
USING PAPER CHROMATOGRAPHY: In paper chromatography, a small amount of the
substance to be analyzed (analyte) is placed on a strip of paper (the stationary phase) above the
46
level of the solvent (mobile phase). In this activity, you will be using ink as the analyte and
alcohol as the solvent.
As the alcohol moves up the paper, the dye molecules from the ink mixture will move with it.
If they are more strongly attracted to the alcohol molecules (mobile phase) than to the paper
molecules (stationary phase), the dyes will continue to move up the paper. If the dye molecules
are more strongly attracted to the paper than the alcohol, they will move more slowly than the
alcohol or not at all. If two or more dyes have been mixed to form ink, then they may move at
different rates as the alcohol moves up the paper. If this happens, they will separate out as
different bands of color and can be identified by analyzing the paper chromatograms. Each
paper chromatogram displays a unique pattern formed by the separation of the visible bands of
dyes.
Note: Different mixtures of ink are specific for each brand of pen.
Retention Factors: After running the chromatogram, each separated band can be assigned a
Retention Factor (Rf) which is characteristic of each specific dye(s). The Rf is a ratio of the
distance the band travels to the distance the solvent (alcohol) travels. The Rf is calculated by
dividing the band distance by the solvent distance. This ratio should be a constant that is
characteristic of the dye(s) in a particular spot under a particular set of chromatographic
conditions (i.e. paper chromatogram, alcohol solvent, etc.).
Retention Factor (Rf) = Distance Traveled by Band ÷ Distance Traveled by Solvent
Each component of the mixture will move at definite distance on the paper in proportion to the
distance that the solvent moves. This ratio, Rf = distance component moves ÷ distance solution
moves, can be calculated for each component to aid in identification. Rf values are dependent
upon the paper, the solvent, and the amount of sample used.
(A):
Separation of components from a mixture of red and blue inks by paper chromatography
Chromatography is one of the most important separation technique and it is extensively used
for the separation of mixture of deep components it was first employed by a Russian scientist
Mikhail Tsvet.
MATERIALS:
• Pencil
• Ruler
• Test tubes or chromatography glass chamber “culture tubes” (20 X 150 mm) in test tube rack
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• Strips of chromatography paper (1 x 16 cm)
• thread
• set of black ink pens labeled “A”, “B”, “C”.
• Paper towels
• Colored pencils
• Wash bottle with rubbing alcohol
PROCEDURE:
• Take a strip of chromatography paper
• Draw a line with a pencil of about 2cm from one end to the other that is the starting
line (stationary phase)
• Draw another lengthwise from the center of the paper and mark the point the two
lines intercepted
• Take the ink with toothpick, put a drop of the ink at the point of interception on the
paper
• Allow it to dry in open air, put another drop on the same spot
• Take a thread and hang the paper on it, Suspend the paper vertically in the
chromatography chamber containing the solvent (ethanol) and make sure the
starting line is about 2cm above the solvent
• Study for some time, notice the rising solvent and the components of the ink
• After the solvent has stop risen, note the various bands.
• Calculate the retention factor for each band

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 EXPERIMENT VIII
PREPARATION OF ASPIRIN (ACETYL SALICYLIC ACID) FROM SALICYLIC
ACID
Salicylic acid contains a phenolic group when acetylated it gives its acetyl derivative. Phenols
are known to be irritating. The Bayer Company replaced the phenol group with an ester group.
This esterified compound (acetylsalicylic acid, also known as aspirin) was shown to be much
less irritating than salicylic acid.
Aspirin is an effective analgesic (pain reliever), antipyretic (fever reducer) and anti-
inflammatory agent and is one of the most widely used non-prescription drugs.

O COOH
COOH C CH3
+ O → + CH3CO2H
OH C CH3 ethanoic
acid
Salicylic acid O Aspirin OCOCH3 mol.
Wt. 60
C7H6O3 Acetic anhydride or C9H8O4
mol. Wt. 138 ethanolic (CH3CO)2O
mol. Wt. 102

MATERIALS REQUIRED:
Salicylic acid, ethanoic anhydride, ice, 50% ferric chloride, conc. H2SO4, sodium hydrogen
trioxocarbonate (IV) solution.
APPARATUS: Glass rod, 250ml beaker, 100ml conical flask, stirrer, thermometer, Bunsen
burner

PROCEDURE
PART I: Preparation of Aspirin

1. Weigh out about 9.7 gram (0.07mol) of salicylic acid on a piece of weighing paper. To
do this, first weigh a piece of weighing paper. Place some salicylic acid on the weighing
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 paper and weigh again. Add or remove solid until you have about 9.7gram of it on the
paper. Record the mass of the weighing paper plus the solid. Subtract to determine the
mass of the salicylic acid. Place this solid into a 100-ml Erlenmeyer flask
2. In the hood, measure out 13.2ml (0.14mol) of acetic anhydride in a small graduated
cylinder and add it to the flask. From this point on, keep your flask under the hood,
because it now contains acetic anhydride (the vapors of acetic anhydride are very
irritating).
3. Add 10 drops of concentrated (85%) sulphuric acid. This will be the catalyst for the
reaction, stir the mixture for thorough mixing.
4. Heat at 60OC for 15 minutes with occasional stirring.
5. Pour the reaction mixture in a 250ml of beaker and stir vigorously
6. Wash down the remaining with a little water
7. Continue stirring till the smell of ethanoic anhydride disappears. Observe the smell by
dipping a glass rod in the solution and smell the end.
8. To speed up decomposition of the unreacted ethanoic anhydride, if necessary. In the
hood, set up a ring stand and set a hot plate/magnetic stirrer on the base of the ring
stand. Put some water in a glass crystallization dish and set this on the hot plate – this
will be your hot water bath. Put your reaction flask in the water bath, and secure it in
place with a utility clamp attached to the ring stand.
9. Start heating the reaction, and turn on the magnetic stirrer or. Once the water bath starts
boiling, start timing the reaction. When the mixture has been allowed to react at 100°C
(the temperature of boiling water) for 15 minutes, you can consider the reaction to be
complete.
10. When there is no more smell of ethanoic anhydride, cool the solution in ice water and
filter the precipitate formed with filter paper.
11. Wash or rinse the precipitate with deionized water, dry the residue. The mass of this
residue (Aspirin) is your actual yield.
QUESTIONS:
i. Write out the balanced equation for the reaction between salicylic acid and
ethanoic anhydride.
ii. Determine the theoretical yield and calculate the percentage yield of the crude
product. Yield= 10.7g. %yield = actual yield X 100
Theoretical yield .
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 iii. Find a suitable solvent for crystallisation and recrystallise 2g of the crude
product.
iv. Dry and determine the melting points of the crude and purity products. The
product melt with decomposition at 135O-137OC.
v. According to your results from IV of this experiment, what can you say about
the purity of your aspirin?
vi. If you measured the melting point of the solid product from this experiment
and obtained a melting range of 122-128 °C, what does this tell you?
vii. Explaine how conc. H2SO4 catalyses the speed of the reaction salicylic acid
and ethanoic anhydride
viii. Why is ethanoic anhydride preferred in this reaction?
ix. Aspirin that has been stored for a long time may give a vinegar-like odor and
give a purple color with FeCl3. What reaction would cause this to happen?
Part 2: Recrystallization of Aspirin
1. Set aside a small amount of the crude aspirin you obtained in step 11 – you will test its
purity later. (You will need enough to test its melting point and to test its reactivity with
FeCl3.)
2. Transfer the rest of the crude aspirin to a 50-mL Erlenmeyer flask. Add 4 ml of ethanol
and warm the flask on a hot plate until all of the solid dissolves. Immediately remove
the flask from the heat and slowly add 13 ml of cold water. Crystals should form. Chill
this solution in an ice-water bath, and collect the crystals using vacuum filtration.
Carefully lift the filter paper with the crystals on it and place it on a clean watch glass.
Leave this aspirin in your drawer to dry until the next laboratory period.
3. At the following laboratory period (when your aspirin is dry), weigh the aspirin on a
piece of weighing paper or a weighing boat. (You will need to scrape it off of the filter
paper.)
Part 3: Purity of Aspirin.
1. Using a melting point apparatus, determine the melting point of your crude aspirin and
your recrystallized aspirin. (In order to get a meaningful result for the melting point
determination, the solids must be dry.) The melting point should be recorded as a range
– the first reading is the temperature at which the sample starts to liquefy, and the

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 second reading is taken when the sample is completely melted. The melting point of
pure aspirin is 135°C – 137°C and the melting point of salicylic acid is 158°C.
Comment on the purity of your aspirin based on its melting point.

Perform the following tests:

For the FeCl3 test, the samples do not have to be dry. To do the test, get 4 test tubes. Place
1 mL of ethanol and 2 drops of FeCl3 solution in each tube. Add a few crystals of salicylic
acid to one test tube. Add a few crystals of your crude aspirin product to the second tube.
In the third tube, place a few crystals of the recrystallized aspirin. Don’t add anything else
to the fourth tube – it will be your “blank”. Shake each of the tubes and record your
observations.

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