AIRFORCE INSTITUTE OF TECHNOLOGY

KADUNA
FACULTY OF SCIENCE
DEPARTMENT OF CHEMISTRY

100 LEVEL CHEMISTRY LABORATORY

MANUAL (CHM 108)
 PREFACE

The writing of this manual was embarked upon in order to provide a simple, interesting, easy
to follow instruction manual for thy students undertaking a chemistry programme leading to
bachelor degree in their different fields.

Each experiment is preceded by a background/introduction section which provides the student

with enough information to enable him/her understand the principles on which the experiment
is based

The procedure gives stepwise directives for carrying out the experiment. Both procedure and
background/introduction should be carefully studied before the scheduled laboratory period,
so that mistakes are minimized and time most effectively utilized.

In view of the current economic situation, the experiments have been designed to minimize

wastage of chemicals and to utilize equipment that is easily available in the laboratory. Most
of the experiments can be completed in a three (3) hours laboratory period, with efficient
organization. Those experiments that are longer can easily be discontinued at a convenient
point after three (3) hours and completed in a subsequent period.

At the end of most experiments are a number of questions. The instructor may assign some of
these questions to be answered and submitted along with the report.

All experimental work must be recorded directly into notebook, which must be submitted as at
when instructed and all un-submitted reports will be scored zero.

This manual is written on the assumption that the students are acquainted with the basic
principle of analytical chemistry. Correlation of the experiment with the lectures is highly
recommended, as this will make the experiments more relevant to the course and more exciting
for the students.
 Table of Contents

INTRODUCTION.............................................................................................. 4
CHEMISTRY LABORATORY SAFETY MEASURES AND DATA HANDLING ................. 4
LABORATORY TECHNIQUES ................................................................................. 5
LABORATORY LOGBOOK REPORTING ................................................................... 5
EMERGENCY PROCEDURE IN CASE OF ACCIDENT ................................................. 8
GLASSWARE ....................................................................................................... 9
BASIC LABORATORY TECHNIQUES ..................................................................... 10
ORGANIC CHEMISTRY............................................................................... 12
EXPERIMENT 1 ............................................................................................. 13
SOLUBILITY TESTS FOR CERTAIN ORGANIC COMPOUNDS ................................... 13
EXPERIMENT 2 ............................................................................................. 14
TESTS FOR FUNCTIONAL GROUPS I .................................................................... 14
EXPERIMENT 3 ............................................................................................. 17
TESTS FOR FUNCTIONAL GROUPS II ................................................................... 17
EXPERIMENT 4 ............................................................................................. 20
DETERMINATION OF THE AMOUNT OF ASPIRIN IN ASPIRIN TABLETS .................. 20
EXPERIMENT 5 ............................................................................................. 22
QUANTITATIVE ANALYSIS ................................................................................ 22
 INTRODUCTION

CHEMISTRY LABORATORY SAFETY MEASURES AND DATA HANDLING

The most important events in the laboratory are safety and the right to know the physical and
chemical hazards present in the laboratory. Follow instructions as stated in the laboratory
manual and be careful with all laboratory fluids and equipment. Before starting the experiment,
carefully read safety manuals that describe how to use chemicals and precautions to be taken
while working in the laboratory. It is very important to note that not all safety measures and
precautions are addressed here. Hence, your biggest source of prevention of any hazard is to
ASK QUESTIONS where you are not sure about what to do.

!!!PLEASE DO NOT DISOBEY LABORATORY RULES. IT

MIGHT END UP FATAL!!!!

The students must follow the following instructions:

1. Instructors, laboratory technologist, laboratory assistants, students and other personnel
that work in the laboratory MUST wear laboratory coats and approved goggles at all
times when in the laboratory.
2. It is advisable to wear long sleeve shirts, long pants and shoes. Shorts, midriff tops and
sandals are not allowed.
3. Long hair is to be tied and well tucked away. It is a fire hazard when let loose or flying.
4. Students are not allowed to work in the laboratory alone.
5. Horseplay or other pranks are prohibited in the laboratory.
6. Smoking, eating, drinking or applying makeup is not allowed inside the laboratory.
7. The laboratory will provide label containers for hazardous waste. Read the label very
well and dispose the waste appropriately. At no time should organic or toxic wastes
such as mercury, lead, chromium be dumped down the drain.
8. Ask when in doubt about proper disposal of waste.
9. Laboratory instructors are in-charge of all emergencies. Follow instructions as directed.
10. All laboratory users should learn how to locate the following materials: safety shower,
eyewash, blankets, fire extinguishers, first aid kit, and fire alarm.
10. Laboratory users should notify the laboratory instructors of any fire or injury.
11. Turn off all gas jets (Bunsen burner) if it is the source of the fire.

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12. Many common reagents, for example, alcohols, acetone, and especially ether, are
highly flammable. Do not use them anywhere near open flames.
13. All laboratory users should learn how to use the fire extinguisher.

LABORATORY TECHNIQUES
1. Use proper utensils such as crucible tongs to hold or move hot items.
2. Make sure there are no flammable materials near you when lightning a burner.
3. Add boiling chips to liquids before heating them up. This will help to prevent
bumping or boil over.
4. Place test tubes in a slanting position away from yourself and others when heating
liquids. Heat liquids at the surface of the liquid.
5. Do not heat up a closed system.
6. Heat all substances that emit noxious fumes under the fume cupboard.
7. Use funnel to transfer liquids into a narrow neck container.
8. Use a bulb or pump to pipette a liquid. Never use your mouth.
9. Avoid smelling anything unless instructed to do so. While sniffing, gently waffle the
material towards your nose when allowed to do so.
10. Do not return excess reagent to its original container.
11. Do not experiment with the chemicals in the laboratory except those that you are
scheduled to use.
12. Do not use your pipette or spatula to remove samples from the stock container. Use
the one provided by the laboratory technologist.
13. Correctly label test tubes or other containers indicating their contents.
14. Strong acids and bases should be added to water and not vice versa.

LABORATORY LOGBOOK REPORTING

One of your goals in this laboratory course should be to learn to keep proper records of your
work. Your laboratory reports will be based on the data in your notebook, and the more
complete the data are, the more likely it is that you will be able to prepare a good report. Writing
is ubiquitous in the sciences, and students primarily develop their writing skills through
laboratory reports. As a scientist-in-training, you ultimately need to learn how to make a
reasoned and articulate argument that is persuasive and based on scientific evidence; the
foundation of that argument needs to be grounded in data that are presented in an organized
and thorough manner. The laboratory report communicates to others the results and conclusions

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you obtained in performing an experiment. You should explain why the experiment was
performed, how the experiment was performed, what results were obtained, how the results
were analysed, and what conclusions were reached.
Data is primarily presented in the result section in the form of tables and figures.
Discrepancies and unexpected results can be accounted for only by referring to complete
records of your work. In a broader sense, a notebook is essential in any research laboratory
where it may be necessary to review data months or years after they were taken; hence full
details are necessary. You will be required to keep your laboratory records in a hard--‐cover,
bound notebook (available for purchase in the General Studies Department). The notebook
should contain all experimental data and pertinent observations recorded.

The following are the requirements for your notebook.

• Each day's work should be dated. The project being performed should be indicated
clearly.
• Be careful to avoid mistakes; mistakes should be crossed out with a single line but
remain legible.
• The notes must be neat and orderly enough for someone else to follow them.
• Use tables to organize data whenever possible.
• The following should be included in the laboratory notebook: all experimental data,
such as masses, burette readings, temperature, etc.
• Notable occurrences (especially phase or colour changes).
• Full details of a procedure need to be recorded; each step should be as concise as
possible.
• All answers to the questions following each experiment.
• Unless otherwise stated, report all experiments in the following pattern:

i. Title and Date of Experiment

ii. Aim of Experiment

iii. Apparatus and Chemicals

iv. Procedure/Methodology

S/N Tests Observation Inference

v. Result

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 vi. Discussion and Solutions to Questions

vii. Conclusion

Title Page
Name: ______________________. Matric. No.: ________________________
Experiment or Period: ____________ Date: ________________
Lab instructor (s): ________________________

Title: The title should summarize as specifically as possible the subject of the lab.

Introduction / Background: In this section you need to introduce the lab and include all
background information pertaining to the lab. This is where you will reorganize the notes that
you have been given in class into a well thought-out paragraph. Define any new or unusual
terms. In the last section of the introduction, clearly lay out the problems that you will be
researching.

Purpose: A single concise statement of the major objective(s) of the lab that answers one of
the following: what question or questions is this lab exercise designed to answer? Or what is
the lab exercise designed to show or prove? Or what hypothesis is the lab exercise trying to
prove or discover? (Note: To make a hypothesis you must be able to provide support for that
hypothesis, based upon your knowledge or literature research. A hypothesis should be an
educated prediction!)

Procedure: This section includes a description of what you did. This should not be a verbatim
copy of the instruction in the lab manual. You do not report any result in this section. Explain
what you give clearly enough for other people to follow your directions to repeat the
experiment. A step-by-step format is the best approach. It should include the definitions of key
terms and anything else necessary to understand exactly what was done.

Results: Calculations based on the data are presented in this section. You need to report all the
calculations that you did. You need to provide the formula used to compute results. Be sure to
identify any possible sources of error.

Discussion: This is the most important part of the lab, as it is where you interpret your
observation and results. For each conclusion you should discuss its significance and whether
or not it seems reasonable. In addition, be sure that you answer any questions that we ask in

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the laboratory instructions. You should infer conclusions from your data. For each completion,
you should provide evidence from your data. Be sure to include a simple calculation of each
type used. Give explanation for and implications of any relationships observed. (When
interpreting a graph infer conclusions based upon the slope of the line or lines).

Support your ideas with specific quantitative reference to the results of your analyses. How do
your observations lead to the conclusions reached? Were the relationships what you expected
from the underlying physical principles? If a conclusion does not seem reasonable, can you
find any error in your procedure which could have affected your results? For each conclusion
you should discuss its significance. Address any interesting questions you may have had as you
were working through the lab exercises. In addition, be sure that you answer any questions that
were asked in the laboratory instructions. Can you make any generalizations? Why or why not?

Conclusion: Summarize your results, the main points of a discussion and how they relate to
your stated purpose of the lab.

You are to restate all the conclusions that were made in the discussion section. No discussion
or explanation or speculation should occur in this section! (Do not use the words “because” or
“since” or “therefore”). It is a good idea to conclude how the main points of the discussion are
connected in order to demonstrate the overall significance of your findings and the concept you
learnt.

EMERGENCY PROCEDURE IN CASE OF ACCIDENT

Chemicals in the eyes - Flush with large amounts of cold tap (clean) water, next bathe the eyes
with 5% boric acid if the accident involved a base or 5% sodium bicarbonate if the
accident involved an acid.
Clothing on fire - Do not run, avoid inhalation of flames. Apply wet coats or wet towels. A
carbon dioxide extinguisher may be used with caution.
Cuts - If serious, stop the flow of blood, go to physician at once. If minor, wash the wound,
remove any pieces of glass and apply a disinfectant and sterile bandage.
Chemicals on skin - Flush off with large amounts of water, remove any contaminated clothing,
neutralize- if acids with 5% sodium bicarbonate -if bases with 5% boric acid -if bromine
with glycerol. After removal of chemical treat as for a burn.

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Swallowing of chemicals - Immediately drink several glasses of clean water and cause the
patient to vomit by tickling the back of the throat. Repeat process and go to physician
at once.
Burns- if extensive - GO TO PHYSICIAN AT ONCE. Keep patient warm and quiet and
give him/her water to drink. If minor- cover with burn ointment. If blisters develop see
physician.
Inhalation of fumes - Remove patient to fresh air. Keep warm and quiet. If breathing has
stopped, start artificial respiration immediately.
Fainting - lower patients head and raise feet. Pass ammonia vapours beneath the nostrils; do
not administer liquids while patient is unconscious.
Incompatible Chemical Mixtures - Some chemicals shouldn't be mixed together. In fact
these chemicals shouldn't even be stored in each other on the chance that an accident could
occur or the chemicals could react. Be sure to keep incompatibilities in mind when reusing
containers to store other chemicals. Here are some examples of mixtures to avoid:
• Acids with cyanide salts or cyanide solution. Generates highly toxic hydrogen cyanide
gas.
• Acids with sulfide salts or sulfide solutions. Generates highly toxic hydrogen sulfide
gas
• Acids with bleach. Generates highly toxic chlorine gas.
• Oxidizing acids (e.g nitric acid, perchloric acid) with combustible materials (e.g paper,
achohols, and other common solvents). May result in fire.
• Solid oxidizers (e.g. Permanganates, iodates, nitrate) with combustible materials (e.g
paper, alcohols, other common solvents). May result in fire.
• Hydrides (e.g., sodium hydride) with water. May form flammable hydrogen gas.

GLASSWARE
Once you have signed out the equipment in your locker, you are responsible for them until you
check out at the end of the session. Keep your lockers locked when not in use. You will be
charged for any broken or lost equipment.

Your notebook must be initialed at the end of each practical before you leave the laboratory.
This will be the only evidence that you have performed experiments should we need one.

Checking In and Checking Out

During your first regular practical period, you will be assigned a locker if available and you
will be given a list of equipment that should be in the locker. Bring along a padlock with key.

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Check the items in the locker against the list and make a checkmark ( ) against every item
present. Make a list of any missing items and collect them from the technical assistants in the
laboratory. If any item is unavailable, make a cross-mark (x) against it in the list. Then fill out
and sign the check-in form and submit to the laboratory assistant.
You are now responsible for those items in your locker. Keep them clean and lock your locker
whenever it is not use.
During your last practical period for the session, the contents of your locker will be checked
against your check-in list. The laboratory instructor or assistant, will place a checkmark (√)
against all item present and a cross-mark (´) against all missing or broken items. You will be
charged for any missing or broken item. When the checkout is completed, the instructor will
sign the check-out column. The instructor will retain your check-in/check-out list.
TAKE YOUR PADLOCK AND KEY AWAY WITH YOU.
All check-out must be completed before the start of the semester exams. Any locker not
checked out by the starting of the exams will be broken and you will pay the cost of repair. In
addition, you will be charged for all missing and broken items.
NOTE: It is important to be properly checked out so your clearance with the department at the
end of the session will be smooth and fast.

Replacement of Broken and Lost Equipment

Each time you need additional equipment sign a check out slip, when you return the equipment,
the slip is returned to you to discard it. Any item not return is listed on the back of your check-
in list and you will be charged for it. Any replacements will also be listed at the back of your
check-in list and you will be charged accordingly.

BASIC LABORATORY TECHNIQUES

Chemistry is an experimental science. It depends upon careful observation and the use of good
laboratory techniques. In this experiment, you will become familiar with some basic operations
that will help you throughout this course. Your success as well as your safety in future
experiments will depend upon your mastering these fundamental operations. Because every
measurement made in the laboratory is really an approximation, it is important that the numbers
you record reflect the accuracy of the device you use to make the measurement. Our system of
weights and measures, the metric system, was originally based mainly upon fundamental
properties of one of the world's most abundant substance, water. Conversions within the metric
system are quite simple once you have committed them to memory. Recently, scientists have

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started to use a briefer version of the metric system of units in which the basic units for length,
mass, and time are the meter, the kilogram, and the second. This system of units, known as the
International System of Units, is commonly referred to as the SI system and is preferred in
scientific work. Conversions within the metric system are quite easy if you remember the
definitions for the prefixes and use dimensional analysis in problem solving.

Important definitions to note:

Standard solution: a standard solution is one of which the concentration (molarity) and
therefore the number of moles per litre is known. The unit of concentration is moles per
dm3 (1 litre).
Molar solution: a molar solution of a substance is one which contains the gram molecular
weight (one mole) of the substance per dm3 of solution.
Indicators: indicators are organic or chemical substances which change colour as pH changes.
The colour changes of some indicators are given below:

Indicator pH range Acid colour Alkaline colour

Cresol red 0.2 – 1.8 Red Blue
Bromophenol Blue 2.8 – 4.6 Yellow Violet-blue
Methyl orange 3.1 – 4.4 Red Orange
Methyl red 4.2 – 6.3 Red Yellow
Bromothymol Blue 6.0 – 7.6 Yellow Blue
Phenolphthalein 8.2 – 10.0 Colourless Red

Choice of an indicator
To titrate:
i. A weak acid against a strong base, use phenolphthalein.
ii. A weak base against a strong acid, use methyl orange or methyl red
iii. A strong acid against a strong base, use any of the above indicators.

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ORGANIC CHEMISTRY
Organic chemistry is the study of the structure, properties, composition, reactions and
preparation of organic compounds which contain carbon in covalent bonding with hydrogen
and a number of other elements (e.g. nitrogen, oxygen).

Qualitative Organic Analysis

Qualitative Organic analysis is the step-wise and systematic study of the behaviour of an
unknown organic compound leading to its identification. The procedures described in this
manual, enables the students to identify the functional groups and to place any unknown
organic substance given into its appropriate chemical class. You are not expected to give the
specific names of any organic compounds you are provided with.

The following steps are employed in the identification of an unknown organic compound:
1. Preliminary tests.
2. Solubility tests.
3. Elemental analysis
4. Functional group tests (confirmatory tests).

For the purpose of these practicals, we will restrict ourselves to solubility tests and tests for
functional groups.

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 EXPERIMENT 1

SOLUBILITY TESTS FOR CERTAIN ORGANIC COMPOUNDS

Introduction
Solubility tests are very important because they narrow your choice of functional groups to a
few possibilities. Small amounts of your compound are tested for solubility in water, 5% HCl,
5% NaHCO3, 5% NaOH and concentrated H2SO4. This information reveals whether the
compound contains a nitrogen, oxygen or sulphur that can be protonated.

Method
a) Place a small piece of your unknown about 0.1g in a small test tube, add about 1cm3
distilled water and shake. Does it dissolve? If yes, go on but if no, proceed to b (ii).
b) (i) Test the solution with indicator paper (or red and blue litmus), by placing a glass
rod inside the solution and spotting it on the indicator paper. Record any colour
changes and inferences. If acidic, then your unknown is an acid or phenol. If
basic, it is an amine. If neutral then your unknown is a low molecular weight
compound either aldehydes, ketones, alcohols, esters, or amides.
(ii) If not soluble in water, decant (pour off) the water and add 1cm3 5% NaOH to
the same solid and shake. If the solid does not dissolve, proceed to c.
c) If it dissolves, then your compound is acidic. Pour out the solution, rinse the tube and
take another small amount of unknown, add about 1cm3 saturated HCO-3 and shake. If
it dissolves your unknown is a carboxylic acid. If it is insoluble, your unknown is a
phenol.
d) If your unknown was insoluble in 5% NaOH, decant the base, rinse the solid with a
little water, pour off the water and add about 1cm3 5% HCl to the solid and shake.
If it dissolves, your unknown is an amine. If it is insoluble, your compound is neutral and may
belong to one of the following: aldehydes, ketones, alcohols, esters, amides, aromatic nitro
compounds. With the solubility tests, you can eliminate certain functional groups and narrow
the possibilities for your unknown.

Questions
1. Define qualitative organic analysis.
2. List preliminary tests carried out in order to identify an unknown organic compound.
3. State the common solvents used in solubility tests of organic compounds

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 EXPERIMENT 2

TESTS FOR FUNCTIONAL GROUPS I

Introduction
Functional groups are specific groupings of atoms within molecules that have their own
characteristic properties, regardless of the other atoms present in a molecule. Common
examples are alcohols, amines, esters, carboxylic acids and ketones. There are 3 classes of
functional groups.
1. Acidic – phenols, carboxylic acids.
2. Basic – amines.
3. Neutral – alcohols, esters.

1. Test for Phenols

Most phenols are crystalline solids; notable exceptions are m-cresol and o-bromophenol. The
monohydric phenols generally have characteristic odours. Their solubility in water increases
with the number of hydroxyl groups in the molecule.

i. Iron (III) Chloride

To 1.0.ml of the solution suspected to be phenol add 3 drops of 1% iron (III) chloride
solution. Occasionally, the colour produced is not permanent; hence care should be
taken to watch the solution closely on the addition of the drop of ferric chloride.
The production of a colour, which may be purple, blue or green with ferric chloride
solution is typical of phenol and enols; but is not definitive as many phenols do not
develop any colour in the presence of iron (III) chloride. If no coloration is obtained,
confirmatory test is recommended which requires substitution of absolute ethanol or
methanol for water as solvent in the above experiment.
ii. Sodium Bicarbonate
Phenols do not usually liberate carbon dioxide from 5% sodium bicarbonate solution.
They will dissolve however, in sodium hydroxide solution.

Method
Add 0.1g of the substance to 1ml of 5% sodium hydroxide, stir and observe whether the
materials dissolve and/or a colorization is produced (e.g. a brown colorization).

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iii. Bromine Water
Many phenols, (with the exception of those with strong reducing properties) yield
crystalline bromination products. Dissolve or suspend 0.25g of the compound in 10ml
of dilute hydrochloric acid or water, and add bromine water drop-wise until de-
colorization occurs. This process is slow and a white precipitate of the bromo-phenol
may form.

2. Tests for Carboxylic Acids

Carboxylic acids are compounds which contain the carboxyl functional group (COOH), which
is a combination of the Carbonyl (C=C) group and the hydroxyl (OH) group and hence the
name carboxyl.

i. Action upon Sodium Bicarbonate Solution

Place 1ml of 5% sodium bicarbonate solution in a small beaker introduce the pure acid
sample, (1 drop or a little of the finely powered solid).
Evolution of carbon dioxide indicates the presence of an acid.
Test the solution so obtained for unsaturation by adding cold 1% potassium
permanganate solution, a drop at a time. The immediate disappearance of the purple
colour and the formation of a brown turbidity indicate the presence of a double bond.
Test a small quantity of the aqueous solution or extract of the carboxylic acid with
litmus or with universal indicator paper.

ii. Ester formation

When an organic acid is heated with a primary or secondary alcohol, especially in the
presence of a little mineral acid as a catalyst, an ester is formed. The process is known
as esterification.
Examples of esters are: Ethyl formate, n-pentyl acetate, ethyl butyrate

Method
Warm 1ml/1.0gm (if solid) of the sample with 2ml of absolute ethanol and 1ml of concentrated
sulphuric acid for 2 minutes, cool and pour cautiously into 5ml of 5% sodium carbonate
solution in a beaker, and smell immediately. An acid usually yields a sweet, fruity smell of an
ester.

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Questions
1. Write the balanced symbol state equations for the conversion of ethyne to ethanol.
2. Explain how to distinguish ethyne from ethane?
3. Give the structural formula of propan-1-ol and indicate the alkyl group.
4. Mention three industrial uses of alcohols.

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 EXPERIMENT 3

TESTS FOR FUNCTIONAL GROUPS II

Objective: To test for functional groups in given organic compounds.

1. Test for Aldehydes and Ketones

Aldehydes and Ketones contain the carbonyl group (C=O). If one of the two groups attached
to the carbonyl atom is hydrogen atom, the compounds are aldehydes. The aldehyde group is -
CHO. The following reactions are characteristics of aliphatic aldehydes

i. Reduction of Benedict’s solution.

Aldehydes will reduce alkaline cupric sulphate to cuprous oxide.

Reagent
Dissolve 173g of sodium citrate and 100g of sodium carbonate in about 800ml of warm water.
Dissolve 17.3g copper sulphate in about 100ml of water. Make up to 150ml pour the first
solution into a 2 litre conical flask and slowly add the copper sulphate solution with stirring.
Make up to 1 litre with distilled water.

Method
Add 5 drops of the test solution to 2ml of Benedict’s reagent; mix and place in a boiling water
bath for 5 minutes. Observe for brick-red colouration.

a. Test with Schiff’s reagent

(Funchsin aldehyde Reagent)
Schiff’s reagent is a dilute solution of Funchsin hydrochloride (p-rosaniline) a dye stuff in
coloured magenta, which on treatment with sulphur dioxide, forms a colourless substance.
When this colourless reagent is treated with an aldehyde, a new colourless to near pink coloured
compound is formed and the solution changes from colourless to pink coloured compound.

b. Action of dilute sodium hydroxide

Aldehydes and very few ketones react with sodium hydroxide solution to yield a yellow
coloured compound with a characteristic pungent odour (due to orotonaldehyde produced by
way of the aldo).

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Reagent
10 - 20% NaOH

Method
To 2 or 3 drops of sample, add 3 to 4ml of 10-20% sodium hydroxide.
Warm and observe the formation of a yellow aldehyde resin and the accompanying peculiar
odour.

c. Sodium Bisulphate test

Aldehydes react with saturated aqueous sodium bisulphate to form while crystalline addition
products. These addition compounds may readily be reconverted to carbonyl compounds by
treatment with acids or alkali. Thus bisulphate addition compounds may be used to separate
aldehydes from mixtures of other compounds.

Reagent
Prepare a saturated sodium bisulphate solution.

Method
To 5ml of saturated sodium bisulphate solution, add 2ml of the sample. Shake thoroughly and
observe the rise in temperature. Filter the crystalline precipitate, wash it with a little cold
alcohol, followed by ether, and allow it to dry.
Treat a small quality of the bisulphate addition compounds with 5ml of 10% sodium carbonate
solution, and note the odour. Repeat with 5ml of dilute hydrochloric acid.

Reaction Characteristic of Ketones

Ketones unlike aldehydes, do not:
i. reduce ammonical silver nitrate solution;
ii. reduce Fehling’s solution;
iii. react with Schiff’s reagent and
iv. yield resins with strong sodium hydroxide solution.

Most of the reactions of ketones are shared with aldehydes, and they involve substitution of
amides at the carbonyl ends.

C=O + H2N ® C=N + H2O

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Examples
i. Hydroxylamine (NH2OH), which will form oxime.
ii. Hydrazine to yield hydrazine compounds.
iii. 2,4-Dinitrophenyl-hydrazine – to yield 2, 4-dinitrophenyl-hydrazone compounds.

These crystals are almost insoluble in water because of their high molecular weight, hence very
good for the detection and characterization of carbonyl compounds.

Method
Add 2 drops (or 0.05-0.1g of the substance to be tested) to 3ml of the 2,4-dinitrophenyl-
hydrazine reagent and shake. A crystalline precipitate indicates the presence of a carbonyl
compound.

Reagent
Suspend 10g of 2, 4-dinitrophenyl-hydrazine in 199ml of methanol.
Add continuously and slowly 4.0ml of concentrated sulphuric acid. The mixture becomes warm
and the solid dissolves completely.

Questions
1. Name any 5 polar organic compounds.
2. Explain the method to distinguish between aldehydes and ketones in the lab?
3. List 2 reagents used to test for saturation and state their observed colours.

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 EXPERIMENT 4

DETERMINATION OF THE AMOUNT OF ASPIRIN IN ASPIRIN TABLETS

Introduction
Aspirin (acetylsalicylic acid) is a pain reliever and reduce fever act as antipyretic with a molar
mass of 180g. It is used for different elements such as aches, fever due to colds tension,
rheumatism arthritis. Aspirin tablets consist of pure aspirin and binder. The amount of pure
aspirin should be specified on the label, however sometimes there is a need to check it. As
aspirin has an acidic property the titration of aspirin tablets with standard na0h solution
provides a means of determining the number of milligrams of pure aspirin per tablet. Aspirin
is acetylsalicylic acid having the following structural formula:

Apparatus / Reagents
a. Burette
b. Conical flask
c. Standard NaOH solution- about 100cm3 (record the concentration)
d. Two tablets of aspirin.

Procedure
1. Rinse a burette twice with a few cm3 of standard NaOH solution, and then fill it above
the zero mark with the same solution and drain to the mark, making sure the burette tip
is full.
2. Dissolve one table of aspirin in about 50cm3 of distilled water in 250cm3 conical flask.
3. Heat the solution to about 900°C to help the aspirin to dissolve, as it is only slightly
soluble in cold water. The solution does not completely clear as the binder is insoluble,
but it does not affect your determination.
4. Cool the solution by placing the flask under running cold water. Add three drops of
phenolphthalein indicator and titrate with the standard NaOH solution given, swirling
the flask to ensure good mixing until the first appearance of a permanent pink colour.

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Note: After standing for several minutes, the pink colour may disappear due to a secondary
reaction.
5. Repeat the determination once more using the second table of aspirin.
6. Calculate the weight of aspirin in mg per tablet.

Questions
1. Vinegar contains acetic acid, CH3COOH. Titration of 5.00g of vinegar with 0.100 M
NaOH requires 33.0cm3 to reach the equivalence point.
a. What is the weight percentage of CH3COOH in vinegar?
b. If the vinegar has a density of 1.005gcm-3, what is the molarity of CH3COOH in
vinegar?
2. The approximate concentration of hydrochloric acid, HCl, in the stomach (stomach
acid) is 0.17M. Calculate the mass of the following antacids required to neutralize
50cm3 of stomach acid.
a. Bicarbonate of soda NaHCO3
b. Aluminium hydroxide, Al(OH)3
3. State what could be responsible for the disappearance of the pink colour of the mixture
on standing as indicated in item 4 of Procedure above.
4. Give a feasible reason why it was not insisted that you carried out more than two
determinations here, as this is contrary to the usual practice. What precaution would
you need to take here in order for your results to be reliable?

Assignment
List as many fruits and or natural foods and drinks that are acidic.

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 EXPERIMENT 5

QUANTITATIVE ANALYSIS

Objective: To determine the concentration, volume or number of moles of one of the reactants
involved in a reaction given that of other.

Introduction
Chemical analysis may be either quantitative or qualitative. Quantitative analysis, as the name
implies, involves the determination of the quantities of known components in a mixture, or of
known elements in a compound while qualitative analysis is used to determine the identity of
the components of a mixture or the identity of elements in a compound. Numerous quantitative
analytical procedures are routinely used in chemistry. They include, volumetric, gravimetric,
spectrophotometric and chromatographic methods. For the purpose of this experiment, we will
focus on volumetric analysis.

Strong acid versus strong base titration

A monoprotic acid (HCl or HNO3) will be titrated with a solution of NaOH of known
concentration. You are provided with 0.1M HCl and NaOH solution of unknown concentration.

Procedure
a. Pipette 25cm3 of the base into a conical flask. Add two drops of methyl orange
indicator. Place the acid solution into the burette and titrate it against the base until you notice
a colour change. Hold the conical flask over a white tile or filter paper while titrating. This will
enable you to detect the change once it occurs. Repeat the experiment three times and record
your readings.

Weak acid versus strong base titration

Procedure
b. Repeat the experiment with 0.1M acetic acid, using phenolphthalein as the indicator.

Questions:
1. Write a balanced symbol state equation for the reaction.
2. Calculate the molarity of the basic solution.
3. Calculate the concentration, in grams, of the acid solution.

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