COLLEGE OF SCIENCE, ENGINEERING AND TECHNOLOGY

Department of Chemistry

Chemistry I (Practical)

Practical Manual for

CHE1PRA

Compiled by TR Mashile

Revised January 2015

UNIVERSITY OF SOUTH AFRICA

FLORIDA
© 2015 University of South Africa

All rights reserved

Printed and published by the

University of South Africa
Muckleneuk, Pretoria

CHE1PRA/1/2016

60158719

InDesign

PR_Tour_Style
 CONTENTS

 Page

A: LABORATORY RULES AND SAFETY1

1: INTRODUCTION2
2: LABORATORY RULES3
3: SAFETY IN THE CHEMICAL LABORATORY4
3.1 General4
3.2 Protective clothing and equipment 4
3.3 Fume hoods 6
3.4 Handling of glassware 6
3.5 Handling of chemicals 7
3.6 Chemical contamination 7
3.7 Chemical hazard symbols 7
3.8 More hazard symbols and their meanings 9
3.9 No eating, drinking or smoking in the laboratory 12
3.10 Hand washing 12
3.11 Chemical spills 12
3.12 Fire safety 12
4: BASIC FIRST AID14
4.1 Cuts14
4.2 Thermal burns 14
4.3 Chemical burns 15
4.4 Ingestion of chemicals 15
4.5 Inhalation of chemicals 15
5: GOOD MANNERS IN THE LABORATORY17
6: CARE AND MAINTENANCE OF LABORATORY GLASSWARE18
6.1 General handling of glassware 18
6.2 Heating and cooling 19
6.3 Vacuum and pressure use 20
6.4 Ground-glass joints 20
6.5 Sintered glassware 20
6.6 Volumetric glassware 21
7: APPARATUS22
8: LABORATORY TECHNIQUES24
8.1 Mass measurement 24
8.2 Filtration25
8.3 Decanting27

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CO N T EN T S

B: PRACTICAL WORK29
9: PREPARATION OF IONIC COMPOUNDS30
9.1 Introduction30
9.2 Experiment 1 31
10: QUALITATIVE ANALYSIS33
10.1 Experiment 2 33
11: QUANTITAVE ANALYSIS36
11.1 Gravimetry36
11.2 Experiment 3 37
11.3 Volumetry/titrimetry38
11.3.1 Terminology38
11.3.2 Methods for the standardisation of solutions 39
11.3.3 Acid–base indicators 42
11.3.4 Techniques used in titrations 42
11.3.5 Experiment 4 44
11.3.6 Experiment 5 47
11.3.7 Experiment 6 49

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 A
LABORATORY RULES AND SAFETY

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1 1

1 Introduction

In your report book which will be given to you during the course of the
practicals there is a form for each experiment. At the end of each practical,
you must complete a report. Hand in all the completed reports before you
leave on the last day.

Do not hesitate to ask the lecturer if you need help during a practical or
while completing a report.

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 2 2

2 Laboratory rules

(1) Do not perform unauthorised experiments. This includes variations of

prescribed experiments.
(2) To reduce the risk of chemicals entering your system through your mouth
and lungs, do not smoke, eat, drink or chew chewing gum in the laboratory.
(3) Always wear a lab coat, dust coat or overall when working in the laboratory.
(4) Do not engage in horseplay or other careless behaviour in the laboratory,
and do not bring other people not registered for this course into the
laboratory with you.
(5) Plan your work to minimise time when you are standing around doing
nothing. You may only leave the laboratory at the end of the practical
session.
(6) Work as quietly as possible.
(7) Keep your workstation tidy at all times. Wipe up any spilt chemicals and
water with a cloth immediately.
(8) Throw away used matches, paper and broken glass in the designated bin
for that particular type of waste.
(9) Hand broken glassware (burettes, pipettes, volumetric flasks and measuring
cylinders) kept for stocktaking purposes to the lecturer.
(10) Place bookcases in front of the benches, not between them.
(11) Buy your spatulas from the laboratory assistant, and keep them in a safe
place when you are not using them in the laboratory.
(12) To avoid contamination, do not introduce any object into a reagent bottle.
(13) Use a spatula to take reagent from a bottle – do not tip reagent from the
bottle. Wipe up any spilt reagent immediately.
(14) Once you have used a reagent, put it back immediately, as other people
will also need it.
(15) Always keep the stopper of a reagent bottle in your hand. NEVER place
the stopper on the bench, since it could accidentally be used for the
wrong bottle.
(16) If you have taken out too much reagent, do not return the excess to the
bottle. Either discard it or give it to a student who needs it for his or her
experiment.
(17) NEVER heat measuring cylinders, volumetric flasks and bottles.
(18) Do not move the balance, and check the level of the balance.
(19) Keep balances tidy. Switch off the balance after using it.
(20) Leave your workstation and apparatus clean and tidy when you leave
the laboratory.
(21) Close the windows when you leave the laboratory.

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3 3

3 Safety in the chemical laboratory

3.1 GENERAL
Rules on their own cannot guarantee safety. Safety is the result of the correct
attitude and behaviour. Each one of you must always be on the lookout for
potential dangerous situations and practices and report them so that they can
be rectified immediately and permanently.

The safety issues I will be discussing below apply to everybody in the laboratory.

No visitor may work in the laboratory without written permission from the
head of the Department of Chemistry.

No one may work alone in a laboratory outside the normal working hours
without permission from the lecturer.

3.2 PROTECTIVE CLOTHING AND EQUIPMENT

Personal protective equipment includes safety glasses, face shields, special
clothing such as splash-proof aprons, and gloves. This equipment helps prevent
contact with objects or spilt chemicals that could cause burns or chemical
contamination.

Safety glasses and face shields protect your eyes and face from contact with
splashed or spilt chemicals.

Special clothing such as splash-proof aprons protects your body.

Gloves protect your hands. Some gloves prevent chemical contamination, while
others help prevent burns from hot objects. Certain chemicals can damage
some types of gloves, causing them to fail.

Each person working in the laboratory must have the following safety equipment:
•• Dust coat/lab coat/overall
•• Safety glasses
•• Gloves

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Safety glasses
You must wear approved safety glasses or prescription glasses.
•• when you are working with the following substances:
þþ bromine or volatile bromine compounds
þþ ammonia
þþ maleic acid anhydride
þþ phthalic acid anhydride
þþ concentrated and strong acids
þþ strong bases
þþ acid chlorides
þþ all irritant substances

•• and/or when you are

þþ distilling flammable and irritant substances under atmospheric conditions
þþ opening a high-pressure gas cylinder
þþ using mechanical motors to pulverise material
þþ performing any action that could involve splashing liquid
þþ igniting liquids or gases for fluoride or sulphur determinations
þþ pouring a liquid boiling mixture into a container or preparing a boiling
mixture
þþ handling an ultraviolet source
þþ working in a fume hood

Dust coat/lab coat/overall

You must wear a knee-length cotton dust coat or lab coat or an overall when
you are working in the laboratory.

Your coat or overall must be neat and clean. Wash it regularly. Mend any tears
and holes to ensure that the coat or overall protects you and your clothing.

Keep your coat or overall buttoned up while you are working, and do not roll
up the sleeves.

In some laboratories you may take off your coat or overall when you are writing
or performing calculations at a desk.

Gloves
Leather gloves: You must wear leather gloves when you are handling cylinders
or heavy objects. Do not wear leather gloves when you are handling chemicals.

Cotton (terry towelling) gloves: You must wear cotton gloves when you are
handling hot or cold materials.

Insulated gloves (College of science, engineering and technology thermal

gloves): You must wear insulated gloves when you are handling cryogenic
materials, i.e. dry ice (solid CO2) or liquid nitrogen.

Plastic or rubber gloves: You must wear plastic or rubber gloves when you
are handling corrosive chemicals such as acids, bases and phenols.

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Latex gloves (surgical gloves): These offer general protection when you are
working with samples and chemicals.

Shoes
It is not compulsory to wear safety shoes in the laboratory. However, if you
wear ordinary shoes, these should have a flat heel and be closed. Closed
leather shoes offer the best protection.

Jewellery
Do not wear rings in the laboratory, as chemicals could get under the rings
and cause severe burns.

Tongs
Use suitable tongs when you are handling hot products or apparatus.

3.3 FUME HOODS

Always handle dangerous and poisonous gases and materials in a fume hood
to prevent the gases and vapours from entering the laboratory. Always handle
CCI4, CS2, H2S and benzene in a fume hood, especially if you are bubbling or
filtering these substances.

To prevent gases and vapours from escaping out of the fume hood, do not
open the hood door too wide.

3.4 HANDLING OF GLASSWARE

•• Never force glass. It cannot stretch, and it can bend only slightly.
•• Normally, when force is exerted on glass, it breaks and splinters, with painful
consequences for the person handling it.
•• Fire polish all sharp edges of glassware and glass tubing with a Bunsen burner.
•• Heat glassware gradually. Don’t put cool glassware on a hot surface or object
such as hot wire gauze. If glassware is not heated correctly, it may shatter.
•• Place hot glassware on insulated pads, not on cold counter tops, otherwise
the hot glassware could burn the counter top and/or shatter.
•• Hot glassware looks the same as cold glassware. Use holders or insulated
gloves to pick up hot glassware – do not use your hands. Fingertip burns
can be very painful. To find out whether glassware is hot, hold your hand a
short distance away from it. If it is hot you will be able to feel the heat coming
from it without being burnt.
•• Glassware that has been dropped may develop invisible small cracks and
stress points. Avoid using glassware that has been scratched or dropped,
as it may break the next time it is used.
•• If you break glassware, pick up all the pieces immediately and put them
in the container for broken glassware. Use a dust pan and brush to clean
up broken glassware.
•• All broken glassware must be placed in the special containers provided.
•• Never clamp glassware between metal surfaces. Always cover metal surfaces
with cork, rubber or another elastic type of material.

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•• If you are carrying more than two pieces of glassware or sample bottles,
carry them in a suitable container. If you are carrying a bottle by the neck,
support the bottle by keeping one hand 3: underneath
S a f e t y i n t h eit.c h e m i c a l l a b o r ato r y
•• Use a suction bulb or similar device to draw liquids into pipettes. Do not
pipette by mouth! A mouthful of toxic chemicals may kill you.

3.5 HANDLING OF CHEMICALS

Only use chemicals for the prescribed purposes. Do not give chemicals to
anybody for any other purpose. No laboratory chemicals may be used for
human consumption.

Many laboratory chemicals are hazardous. Some are flammable or corrosive,

while others are toxic (poisonous). Pay careful attention to the labels on
chemicals, as these will indicate whether the chemicals are hazardous.

Flammable chemicals can cause fires, and corrosive chemicals, such as acids,
can burn you. Store chemicals in their proper locations, and only take as
much as you need for your tests. Leaving excess chemicals lying around in a
laboratory creates unnecessary hazards.

Sample chemicals can also be hazardous. Make sure they are labelled properly.

3.6 CHEMICAL CONTAMINATION

Chemical contamination occurs when you are exposed to a hazardous chemical
that is released into a work space. It can be caused by chemical spills, equipment
failure, or in a number of other ways. You can cause chemical contamination by
following unsafe work practices such as handling equipment with contaminated
gloves.

3.7 CHEMICAL HAZARD SYMBOLS

There are many hazardous reagents in the laboratory, and these are classified
into different groups according to the hazards that they pose.

Below are some chemical hazard symbols and their meaning. (All these symbols
are printed in black on an orange background.)

Symbol Explanation

Explosive
(Chemicals that explode)

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Symbol Explanation

Oxidising
(Chemicals that react exothermally with other
chemicals)

Flammable
(Chemicals that have an extremely low flash
point and boiling point, and gases that catch
fire in contact with air OR chemicals that may
catch fire in contact with air, only need brief
contact with an ignition sources, have a very
low flash point or evolve highly flammable
gases in contact with water.)

Toxic
(Chemicals that at very low levels cause
damage to health OR chemicals that at low
levels cause damage to health)

Harmful
(Chemicals that may cause damage to health)

Corrosive
(Chemicals that may destroy living tissue on
contact)

Dangerous for the environment

(Chemicals that may present an immediate or
delayed danger to one or more components of
the environment)

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3.8 MORE HAZARD SYMBOLS AND THEIR MEANINGS AND THEIR

COLOUR CODING

Symbol Explanation Colour coding

Explosive substances Black on orange

Hazard: Substances that may explode background
under particular conditions
Example: Ammonium dichromate
Caution: Avoid shock, friction, sparks
and heat

Flammable gas Black on red

Hazard: Gas which will ignite on background
contact with a source of
ignition
Examples: Butane, propane
Caution: Avoid formation of flammable
gas–air mixtures, and keep
away from sources of ignition

Non-flammable, non-toxic gas Black on green

background

Toxic gas Black on white

background

Oxidising gas Black on yellow

background

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Symbol Explanation Colour coding

Flammable liquid Black on white

* flashpoint below –18 °C background
* flashpoint between –18 °C and 23 °C
* flashpoint from 23 °C to 61 °C
Examples: Acetone, benzene, diethyl
ether
Caution: Keep away from open fires,
sources of heat and sparks

Flammable solid Black on red/

white striped
background

Spontaneously combustible substance Black on divided

Hazard: Substances that can white/red
spontaneously combust on contact with background
air (oxygen)
Examples: Phosphorus, sodium
Caution: Avoid contact with air
(oxygen)

Substance sensitive to moisture Black on dark

Hazard: Chemicals that readily form blue background
flammable gases on contact
with water
Examples: Lithium, sodium borohydride
Caution: Avoid contact with moisture
or water

Oxidising agent Black on yellow

Hazard: Oxidising substances can background
ignite combustible material
or worsen existing fires, and
thus make fire-fighting more
difficult
Examples: Potassium permanganate,
sodium peroxide
Caution: Keep away from combustible
material

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Symbol Explanation Colour coding

Toxic substance Black on white

Hazard: Substances that are very background
hazardous to health when
inhaled or swallowed or come
into contact with the skin;
they may even lead to death
Examples: Arsenic trioxide, mercury (II)
chloride
Caution: Avoid contact with the human
body and immediately consult
a doctor in cases of serious
illness

Harmful substance Black on white

Hazard: When taken up by the body background
these substances cause slight
damage
Examples: Pyridine, trichloroethylene
Caution: Avoid contact with the human
body, including inhalation of
the vapours; consult a doctor
in cases of illness

Irritating substance
Hazard: Substances that may have an
irritant effect on skin, eyes
and respiratory organs
Examples: Ammonia solution, benzyl
chloride
Caution: Do not breathe vapours and
avoid contact with skin and
eyes

Corrosive substance Black on white/

Hazard: Living tissue as well as black divided
equipment is destroyed on background
contact with these chemicals
Examples: Bromine, sulphuric acid,
hydrochloric acid, sodium
hydroxide
Caution: Do not breathe in vapours
and avoid contact with
skin, eyes and clothing.
Wear appropriate protective
clothing.

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3.9 NO EATING, DRINKING OR SMOKING IN THE LABORATORY

Eating: You may not take any food into any of the laboratories.

Drinking: You may not take any drinks (e.g. coffee, tea or cool drinks) into
the laboratory.
You may not use laboratory glassware to drink out of.

Smoking: You may not smoke in any of the laboratories or the laboratory store.

3.10 HAND WASHING

Hand washing is very important. Wash your hands thoroughly as often as
needed. Unless you are specifically instructed to do so, do not use solvents.
Some solvents can penetrate your skin and transport (carry) toxic chemicals
into your body.

3.11 CHEMICAL SPILLS

Follow the procedures described below in the case of chemical spills up to a
volume of one litre. In the event of a bigger spill, notify the lecturer.

Acid spills
(1) Apply neutraliser (sodium hydrogen carbonate) around the edge of the spill.
(2) Mix thoroughly until fizzing and evolution of gas ceases. You may have
to add water to the mixture to complete the reaction. Neutraliser has a
tendency to absorb acid before fully neutralising it.
(3) Check mixing with indicator paper to make sure the acid has been
neutralised.
(4) Transfer the mixture to a plastic bag, tie it closed, and give it to the lecturer.

Solvent spills
(1) Apply activated charcoal or cat litter around the edge of the spill.
(2) Mix thoroughly until the material is dry and no evidence of solvent remains.
(3) Transfer the absorbed solvent to a plastic bag, tie it closed, and hand it
to the lecturer.

3.12 FIRE SAFETY

Every laboratory user must be able to identify the types of fires that can occur
in a laboratory, and must know the procedures for dealing with various types
of fires.

Small fires
(1) Extinguishable within 1 to 2 minutes.
(2) Cover the fire with an inverted beaker or wet paper towels. If this fails,
use a fire extinguisher.
(3) To use the fire extinguisher, think of the word PASS:
P – pull out the pin.

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A – aim the hose at the base of the fire.

S – squeeze the handle.
S – sweep the hose back and forth.

Large fires
(1) Remain calm.
(2) Activate alarm.
(3) Call the fire department (the numbers are displayed in the lab).
(4) Switch off all equipment.
(5) Assemble all your belongings if possible.
(6) Close windows.
(7) Close the door behind you as you exit the room on your way out of the
building.
(8) Assist anyone who has been injured.
(9) Exit the building as quickly as possible.

Person on fire
(1) The rescuer should (by force, if necessary) make the victim STOP, DROP
and ROLL.
(2) Use a fire blanket to smother the flames engulfing the person.
(3) Call the emergency services.

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4 4

4 Basic first aid

Everyone is under obligation to help another person who is injured or ill.

You need to know and be able to apply simple first aid techniques to give
life support and other care and develop safety awareness habits that promote
general laboratory safety.
If possible, always wash your hands before and after giving first aid to reduce
the risk of infection and transmission of disease. If possible, wear latex gloves
while giving first aid.

4.1 CUTS
Small cuts
Clean the area with soap and water and place a clean dressing over the wound.
Significant bleeding
(1) Call the emergency services immediately.
(2) Calm and reassure the injured person.
(3) Lay the injured person down. This will reduce the chance of fainting.
(4) Do not remove any impaled objects from the injured person.
(5) Put direct pressure on the wound with a sterile bandage or a clean cloth.
(6) If direct pressure does not control the bleeding, elevate the wound above
the heart if possible.
(7) If bleeding is severe, raise the injured person’s legs about 30 cm, and
cover him or her with a blanket.

4.2 THERMAL BURNS

First-degree burns
These burns are characterised by pain, redness and swelling. An example is
a mild steam burn.
(1) Run cool water over the burn or soak it in cool water for at least 5 minutes.
(2) Cover the burn with a sterile bandage or a clean cloth.
(3) Do not apply ointments, sprays or salves.

Second- and third-degree burns

These burns are characterised by red or mottled skin with blisters (second
degree) and white or charred skin (third degree).
(1) If the victim is on fire, put the fire out.
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(2) Call the emergency services.

(3) Do not remove any burnt clothing unless it comes off easily.
(4) Cover burns with dry, sterile or clean bandaging.
(5) Do not apply ointments, sprays or salves.

4.3 CHEMICAL BURNS

Wear gloves and safety glasses to protect yourself if you are attempting to assist
someone covered in chemicals.

On skin
(1) Remove the victim’s clothes and shoes – don’t let modesty stand in the way.
(2) Rinse the area with large quantities of water for at least 15 minutes.
(3) Do not apply burn ointments or sprays to affected areas.
(4) Cover with dry, clean or sterile material.
(5) If large areas of the victim’s body are affected, call emergency services.

In eyes
(1) You may have to force the victim’s eyelids open so that you can wash
effectively behind the eyelids.
(2) Be sure to wash from the nose outwards towards the ear. This will avoid
washing chemicals back into the eye or into the unaffected eye.
(3) Wash the victim’s eyes and eyelids with water for a minimum of 15 minutes.
(4) If the victim wears contact lenses, remove these as soon as possible to
rinse eyes of any harmful chemicals.
(5) Cover both the victim’s eyes with clean or sterile gauze.
(6) Call emergency services.

4.4 INGESTION OF CHEMICALS

(1) Call emergency services.
(2) If the victim is awake and able to swallow, give them water or milk to
drink. If the victim vomits, stop administering fluids.
(3) If the victim is unconscious, turn their head to the left or place them
onto their left side. Be prepared to start CPR, but be cautious about
exposing yourself to chemical poisoning via mouth-to-mouth resuscitation.
If available, use a mouth-to-mask resuscitator.

4.5 INHALATION OF CHEMICALS

Evacuate the area, move the victim into fresh air, and call the emergency
services.

If the victim is not breathing

(1) Perform CPR until the emergency services arrive.
(2) Try to avoid exposure to chemical poisoning via mouth-to-mouth
resuscitation. If a mouth-to-mask resuscitator is available, use it.

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If the victim is breathing

(1) Loosen the victim’s clothing and maintain the airway.
(2) Lay the victim flat on their back. Place one of your hands under their
neck and lift.
(3) With the heel of your other hand on the victim’s forehead, rotate or lift
the victim’s head backwards into maximum extension.
(4) If you need to open the airway further, gently push the victim’s lower jaw
into a jutting-out position.

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5 5

5 Good manners in the laboratory

•• Never insert your personal pipette into community reagent bottles.

•• Several students share laboratory reagents. Leave the reagents in their
assigned area unless you are instructed to take them to your bench.
•• Always hold bottle stoppers in your hand. Never put them down on the
bench top.
•• Try not to take too much reagent out of the bottle. However, if you do take
too much, never return the excess reagent to the bottle.
•• Some liquids may be disposed of by pouring them down the sink. However,
others (such as most organic solvents) may not. Ask before you pour anything
down the sink.
•• Discard solids in designated waste containers. Do not dispose of them
down the sink.
•• Always clean up your lab bench and make sure the equipment is ready for
the next class.

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6 6

Care and maintenance of laboratory

6

glassware

To obtain the maximum life and performance from glassware, you must handle
it properly.

You should find the following notes useful both if you are a new user and if
you are experienced and just need to be reminded of the correct procedures.

6.1 GENERAL HANDLING OF GLASSWARE

•• Wear appropriate clothing, such as a lab coat, face mask and gloves when
conducting any laboratory activity.
•• Always examine glassware before you use it. Do not use glassware that
is scratched, chipped, cracked or etched. Defects of this kind weaken the
glass, and it will tend to break more easily.
•• When you are stirring solutions in glass vessels, do not use unprotected
stirring rods, as these may cause scratches. Use a “policeman” or a coated
stirrer.
•• Wash or soak glassware promptly after use to avoid the formation of hard,
dried residues.
•• Do not lift or carry glass vessels by the neck, rim or side arm. Place one
hand under the base as support.
•• Never force hoses onto glass side arms. Instead, lubricate and ease them
on gently. (Most glassware such as condensers and filter flasks are supplied
with detachable plastic hose connectors to allow easy and safe attachment
of rubber tubing, etc.) Wear protective gloves.
•• Never force bungs and stoppers into the necks of glass vessels. Be sure to
select the correct size.
•• Although Pyrex glass is highly resistant to chemical attack, do not use it
when working with hydrofluoric acid, hot phosphoric acid or hot alkalis.
•• Do not mix sulphuric acid and water in measuring cylinders. The heat of
reaction can cause base failure.
•• Lubricate ground-glass joints with laboratory grease before use.
•• Keep all volumetric glassware perfectly clean and grease free. Dirt, and
especially grease, can affect the shape of the meniscus and so impair
accuracy.
•• Many volumetric items, such as flasks and burettes, have narrow necks.
When you are filling these items, always use a funnel to avoid spillage.

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•• Always hold glassware items vertically (upright) when you are reading the
meniscus. To avoid parallax errors, the meniscus should be at eye level.
•• Do not use a funnel to fill the burette.
•• Never pipette by mouth. Always use purpose designed pipette filler.
•• Never apply direct heat to any item of volumetric glassware.

6.2 HEATING AND COOLING

•• If you are using electrical heating equipment, ensure that it is in good
condition, and follow the manufacturer’s instructions.
•• If you are using a Bunsen burner for heating, employ a soft flame and use
wire gauze to prevent localised heating.
•• Heat vessels containing liquids slowly to avoid bumping and splattering of
the solution.
•• To prevent thermal shock and possible failure, always cool glassware slowly,
and avoid draughts.
•• Never heat glassware that is scratched, chipped, cracked or etched. These
defects reduce the thermal strength of the glassware, making it more prone
to breakage.
•• When you are autoclaving Pyrex bottles with screw caps, always loosen
the caps. If you autoclave Pyrex bottles with the cap tightly closed, the
bottles may break.
•• Pyrex borosilicate glass is completely microwave safe. However, as with any
microwave vessel, be sure it holds a microwave absorbing material such as
water before placing it in the oven. Note that fitments such as plastic screw
caps may not necessarily be microwave safe.
•• Do not put hot glassware on a cold, damp surface. Although Pyrex can
withstand extreme temperature, sudden temperature changes may cause
the vessel to break. Similarly, do not put cold glassware onto hot surfaces.
Warm up gently.

•• To heat a test tube over a flame, grasp the tube with a test tube holder and
move the tube back and forth through the flame at an the angle, as shown
in the figure. Be careful not to point the tube at anyone, including yourself,
while it is being heated.
•• Take great care when heating liquids which have a high viscosity. Viscous
liquids can act as thermal insulators and can cause “hot spots” or even
thermal breakage of the glassware. This is particularly important with media
solutions, as the viscosity usually increases considerably during preparation.
•• Stir the solution regularly to assist even distribution of heat. If you are using
a magnetic stirrer, set the speed to ensure adequate agitation of the whole
liquid.

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•• Check the stirring action regularly to ensure that it remains adequate as the
viscosity of the solution increases.
•• Heat vessels gradually and avoid very rapid boil-up rates.
•• Do not use glass vessels with thick walls, such as Pyrex Heavy Duty Ware,
or standard beakers or flasks which have a capacity of 5 litres or greater.
•• For personal safety, consider placing the hotplate on a tray. This will help
contain any spillages in the event of a breakage.

6.3 VACUUM AND PRESSURE USE

•• Because working conditions can vary enormously, glassware cannot be
guaranteed against breakage when it is used under vacuum or pressure.
•• The use of positive pressures with glassware is particularly hazardous, and
should be avoided if at all possible.
•• Always use adequate safety screens and/or a protective cage.
•• Avoid stresses caused by over tightening clamps. Support glassware gently
where possible.
•• Under no circumstances use glassware which is scratched, chipped or
etched. Its strength will be seriously impaired.
•• Never subject glassware to sudden pressure changes. Always apply and
release pressure gradients and vacuums gradually.
•• Do not use flat-bottomed vessels, such as Erlenmeyer flasks, under vacuum,
as they are likely to implode. However, it is safe to use vessels with specially
thickened walls, such Bucher filter flasks and desiccators, under vacuum.

6.4 GROUND-GLASS JOINTS

Always lubricate joints with a laboratory grease to prevent seizure. Alternatively,
use PTFE joint sleeves. If joints do seize, however, then try the following:
•• Always wear protective gloves and a face mask.
•• Carefully rock the cone in its socket.
•• Try penetrating oil.
•• If the use of high temperature is permissible, in other words, if no volatile
liquids are present, then warm the socket, not the cone, under a running
stream of hot water from the tap.

6.5 SINTERED GLASSWARE

•• Never subject sintered ware to differential pressures exceeding 100 kN/
m2 (15 psi).
•• Avoid subjecting sintered ware to sudden temperature changes or to
direct flame (the thermal endurance is less than standard Pyrex or Quickfit
products.)
•• Always heat sintered glassware very gradually, and also cool it gently.

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6.6 VOLUMETRIC GLASSWARE

•• Keep all volumetric glassware perfectly clean and grease free. Dirt, and
especially grease, can affect the shape of the meniscus and so impair
accuracy.
•• Discard items with chipped or damaged jets, as these pose a safety hazard.
Also, damaged jets could affect delivery times and impair accuracy.
•• Many volumetric items, such as flasks and burettes, have narrow necks.
When filling these items, always use a funnel to avoid spillage.
•• Hold all items vertically (upright) when you are reading the meniscus. To
avoid parallax errors, the meniscus should be at eye level.
•• Do not use scratched or chipped items.
•• Never pipette by mouth. Always use a purpose-designed pipette filler.
•• Never apply direct heat to any item of volumetric glassware.

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7 7

7 Apparatus

Beaker
Erlenmeyer flask
Pipette
Volumetric flask

Buchner flask
Buchner funnel
Funnel

Burette

Bunsen burner Wire gauze

Clay triangle

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22
 7: A p p a r at u s

Crucible tongs

Crucible with lid Evaporating dish

Watch glass

Measuring cylinder
Test tube

Spatula
Water bottle
Test tube rack with test tubes

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8 8

8 Laboratory techniques

8.1 MASS MEASUREMENT

The automatic analytical balance
This balance can determine a mass of approximately 150 g with a sensitivity
of approximately 0.0001 g.

Procedure for mass measurement

(1) Check the water level at the back, and set the balance if necessary.
(2) Place the weighing boat in the
middle of the pan and close the
windows.
(3) Switch the balance on.
(4) Open the window and, using a
spatula, place the substance to
be weighed in the weighing boat.
(Take care not to spill anything
in the balance or on the pan.)
Approximately the required mass
is weighed.
(5) The actual mass can vary by 10%
from the mass that is required. For
example, let’s say that the required
mass is 0.5 g. 10% of 0.5 g is 0.05 g. The
weighed mass can then vary between 0.45 g
and 0.55 g.
(6) Close the window, and write down the mass to four decimals.
(7) Switch off the balance.
(8) Open the window and remove the weighing boat.
(9) Make sure that the balance is clean, and close the window.

Possible errors during mass measurements

The success of a qualitative analysis depends greatly on the accuracy of the
mass measurement. Here are some possible reasons for faults during mass
measurements:
(1) The weighing boat is not centred on the pan.
(2) Some of the sample has spilt on the pan.

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24
 8 : L a b o r ato r y te ch n i q u e s

(3) Air buoyancy due to an open window.

(4) The object is too warm.
(5) The substance that is weighed is hygroscopic or deliquescent.

8.2 FILTRATION
Gravity filtration
A precipitate can be separated from a solution by filtration. Fold the filter paper
as shown in the figure below. The filter paper must fit tightly into the funnel.
Add a little water to moisten the filter paper. Press the filter paper against the
side of the funnel.

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Vacuum filtration
Filtration speed is greatly increased if suction is applied to the filter paper.
Instead of using a glass funnel (conical funnel), you would use a Buchner funnel,
which has a perforated plate to support a filter paper. A rubber seal seals the
funnel to a heavy-walled side-arm vacuum filter flask. An aspirator attached to
the water tap supplies suction. This works well, but changes in water pressure
sometimes cause water to back up in the vacuum hose. To guard against this
backflow, another filter flask is inserted in the line as a trap, as you can see in
the figure below. This is especially important if you need the filtrate.

The filter paper must be well sealed to the perforated plate in the Buchner
funnel. To seal it, place the dry filter paper in the funnel and wet it well with
the solvent present in the solution to be filtered. If the solvent concerned
is ethanol, you can use water to wet the paper. Turn the pump on, and the
paper is pressed into place. During filtration the pump must stay turned on, as
otherwise water from the pump may drain back into the filtrate. When all the
material has been filtered, disconnect the pump from the flask while it is still
running. If any of the solid has not been transferred to the funnel, retrieve a
portion of the filtrate and use it for swilling the residue into the funnel. Wash
the solid free of filtrate by pouring a small portion of chilled fresh solvent into
the funnel while the pump is disconnected. Finally, the solid is drained as dry
as possible by suction from the pump.

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 8 : L a b o r ato r y te ch n i q u e s

8.3 DECANTING
Allow the precipitate to settle. Carefully pour the liquid from the precipitate
without disturbing the precipitate. Use a glass rod to regulate the flow direction.

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 B
PRACTICAL WORK

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9 9

9 Preparation of ionic compounds

9.1 INTRODUCTION
While preparing ionic compounds you will be making use of a variety of
reactions, namely precipitation, redox and acid–base reactions.

Precipitation reactions
Precipitation reactions include any chemical change in solution that results in
one or more insoluble products. For aqueous solution reactions the product
is insoluble in water. How do you know whether a precipitate will form? The
solubility rules set out in the table below make prediction easy. There are
exceptions to the solubility rules, but you will seldom be wrong if you apply
the rules.

Solubility rules for ionic compounds in water

(1) All lithium, sodium, potassium, and ammonium compounds are

generally soluble.
(2) All nitrates and acetates are generally soluble.
(3) All chlorides, bromides and iodides (halides) are soluble. However,
halide compounds containing lead(II), silver(I),and mercury(I) are
insoluble.
(4) All carbonates and phosphates are generally insoluble. Sodium,
potassium, lithium and ammonium carbohydrates and phosphates
are, however, soluble.
(5) Hydroxides and sulphides are generally insoluble. Sodium, potassium,
calcium and ammonium compounds are, however, soluble.

Oxidation-reduction reactions
Another important reaction type, oxidation-reduction, takes place because
of the transfer of negative charge (one or more electrons) from one reactant
to another (atoms, molecules, or ions). As a result of this transfer of electrons,
charges on atoms in the various reactions change.

The reaction of zinc metal with copper(II) ions is one example of

oxidation-reduction:
Zn (s) + Cu2+ (aq) → Zn2+ + (aq) + Cu (s)

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 9 : Pr e p a r at i o n o f i o n i c co m p o u n d s

Zinc metal atoms each donate two electrons to copper(II) ions. Consequently,
zinc atoms become zinc(II) ions and copper(II) ions become copper atoms.
Zinc is oxidised (increased positive change) and copper is reduced (decreased
positive charge) as a result of electron transfer.

Acid–base reactions
Acid–base neutralisation reactions are processes in which an acid reacts with
a base to yield water plus an ionic compound called a salt. Acids are defined
as compounds that produce W ions when dissolved in water, and bases
are compounds that produce OH ions when dissolved in water. Thus, the
driving force behind a neutralisation reaction is the production of the stable
covalent water modules by removal of H+ and OH- ions from solution.

The reaction between sulphuric acid (H2SO4) and ammonium hydroxide

(NH4OH) to yield water and ammonium sulphate is a typical example:
H2S04 (aq) → 2H+ (aq) + SO42- (aq)
2NH4OH (aq) → 2NH4+(aq) + 2OH- (aq)
H2SO4(aq) + 2NH4OH(aq) → (NH4)2SO4(s) + 2H2O

9.2 EXPERIMENT 1
Preparation of copper(I) chloride

Chemicals required

Bench chemicals Other chemicals

Deionized water (distilled water) Na2SO3(s) – sodium sulphite
CuC2.2H2O(s) – copper(II) chloride
dihydrate
0,001 M H2SO4 – dilute sulphuric acid

Apparatus

Weighing boat Bunsen burner Wash bottle

Tripod Filter paper Glass stirring rod
Buchner funnel Beakers (2) Measuring cylinder (50 ml/100 ml)
Spatula Wire gauze square

Method:
(1) Place 5 g Na2SO3(s) in a beaker.
(2) Add 30 ml distilled water and heat over a small flame while stirring till
the solution is clear. Be careful not to boil the water.
(3) Remove from the flame to cool down.
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(4) Place 6 g CuC2.2H2O(s) in a beaker.

(5) Add 20 ml distilled water and stir till the solution is clear.
(6) Add the Na2SO3 solution (prepared in steps 1and 2 above) drop by drop
while stirring.
(7) Add 20 ml 0.001 M H2SO4 and stir well.
(8) Filter the white crystals (CuCI) with a Buchner funnel.
(9) Wash the crystals 3 times with 10 ml 0.001 M H2SO4.
(10) Wash the crystals 3 times with 10 ml ethanol.
(11) Write your name on a sheet of paper, and attach the filter paper with the
crystals to it. Hand this in.

Reactions

2CuCl2(aq) + H2 O(/) + Na2SO3(aq) – Na2SO4(aq) + 2HCI(aq) + 2CuCI(s)

SO32- (aq) + 2 H+(aq) – SO2(g) + H2 O(/)

2CuC l2(aq) + S02(g) + 2H2O(/) – H2SO4(aq) + 2CuCI(s) + 2HCI(aq)

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10 10

10 Qualitative analysis

10.1 EXPERIMENT 2
Anion analysis
Discussion
You will receive a mixture in which a combination of any of the following
anions will be found:
CO32-, SO42-, Cl-, l-, NO3-
The anions are divided into four groups according to specific reactions.
Identification tests are then performed to identify the anions. The properties
are summarised in the following table:

GROUP EXAMPLES OF CHARACTERISTIC PROPERTIES

ANIONS
A CO32-; S2-; SO32- Forms a gaseous product with the addition
of HCI(d)
B PO43- ; SO42- Forms characteristic precipitates
Forms characteristic precipitates.
C Br-; Cl- ; I- Functional oxidation to the halogen forms a
characteristic colour in CS2.

Only the anions printed in bold will be tested for.

Chemicals required
Bench chemicals Other chemicals
Deionized water (distilled water) Mixture of salts containing certain anions
Dilute HCI Special bench regents
Concentrated HCI Ca(OH)2 or Ba(OH)2 solution (clear lime
Dilute HNO3 water)
Concentrated HNO3 BaCl2 solution
FeCl3 solution
CS2 liquid
AgNO3 solution

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Apparatus
Erlenmeyer flask Bunsen burner Wash bottle
Tripod Filter paper Glass stirring rod
Crucible tongs Beaker Measuring cylinder (50 ml/100 ml)
Spatula Wire gauze square Measuring cylinder (10 ml)
Matches Test tube holder

Experimental procedure

ANION
MIXTURE

If the sample is in powder form, dissolve it in 30 ml water.

Filter if necessary.
Pour 5 ml amounts of the solution into four test tubes.

Group A

Carbonate ion (CO32-)

Pour 5 ml saturated Ca(OH)2 or Ba(OH)2 into a test tube. (Filter the

solution if necessary – it must be clear.)
Add 2 ml HCI(d) to one of the first four test tubes. If a gas is evolved,
pour the gas over in the test tube with the Ca(OH)2 and shake.
A MILKY solution indicates the carbonate ion.
CO32- (aq) + 2HCl(aq) → CO2(g) + H2O(/) + 2CI- (aq))
CO2(g + Ca(OH)2(aq) → CaCO3(s) + H2O(/)

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 10 : Q u a li t at i ve a n a l y sis

Group B

Sulpate ion (SO42-)

Pour 5 ml HCl(d) to this part. Filter if necessary.

Add 3 drops BaCl2 solution to the clear solution.
A WHITE precipitate indicates the sulphate ion.
SO42- (aq)+BaCl2 (aq) → BaSO4(s) + 2Cl- (aq).

Group C

Iodide and chloride ions (I- and Cl-)

Divide the solution into two parts.

Iodide ion (I-) Chloride ion (CI-)

Add 1 ml FeCh and 1 ml CS2 to the If iodide is present, add If iodide is absent,
solution and shake well. 2 ml HNO3(c) to the solution add 1 drop AgNO3
and boil till the volume is solution to the
A PURPLE colour in the CS2 layer ± 3 ml. Any I- is oxidized to solution.
indicates the iodide ion. I2 that escapes as gases.
2I- (aq) + 2Fe3+(aq) → I2 (s)+ 2Fe+(aq) Add 1 drop AgNO3 solution
I2(s) + CS2(l) [12] CS2 to the remaining solution.
A WHITE precipitate indicates the chloride ion.
6 I- (aq)+8 HNO3(aq) → 3 I2(g) + NO(g) +4H2O+
6NO3- (aq)
Cl- + AgNO3 → (aq) AgCl(s) + NO3- (aq)

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11 11

11 Quantitative analysis

11.1 GRAVIMETRY

INTRODUCTION
In this type of analysis a balance is used to determine the actual composition
of a sample. The result is then given as a percentage or some other measure.

MASS MEASUREMENT
The automatic analytical balance
This balance can determine a mass of approximately 150 g with a sensitivity
of approximately 0.0001 g.

Procedure for mass measurement

(1) Check the water at the back and set the balance if necessary.
(2) Place the weighing boat in the middle of the pan and close the window.
(3) Switch the balance on by pressing down the beam in the front briefly
and then releasing it.
(4) Open the window and use a spatula to place the substance to be weighed
in the weighing boat. (Take care not to spill any of the substance on the
balance or on the pan.) Approximately the required mass is weighed.
(5) The actual mass can vary by 10% from the mass that is required. For
example, let’s say that the required mass is 0.5 g. 10% of 0.5 g is 0.05 g.
The weighed mass can then vary between 0.45 g and 0.55 g.
(6) Close the window and write down the mass to four decimals.
(7) Switch off the balance by lifting the beam.
(8) Open the window and remove the weighing boat.
(9) Make sure that the balance is clean and close the window.

Wait at your workstation until it is your turn to use the balance.

Possible errors during mass measurements

The success of a quantitative analysis depends greatly on the accuracy of the
mass measurement. Here are some possible reasons for faults during mass
measurements:
(1) The weighing boat is not centred on the pan.
(2) Some of the sample has spilt on the pan.
(3) Air buoyancy due to an open window.
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36
 11: Q u a nt i t at i ve a n a l y sis

(4) The object is too warm.

(5) The substance that is weighed is hygroscopic or deliquescent.

11.2 EXPERIMENT 3
Determination of the number of moles of crystal water in BaCl2.xH2O(s)

Chemicals required
BaCl2.xH2O(s)
Apparatus
Porcelain crucible (without lid)
Crucible tongs Spatula
Tripod Matches
Bunsen burner Porcelain tile
Silica triangle (or clay triangle) Large beaker and watch glass to cover it
with

Method
(1) Place a clean porcelain crucible on a clay triangle and heat vigorously for
approximately 5 minutes with a Bunsen burner.
(2) Cool the crucible off in the beaker covered with the watch glass. Only
handle the crucible with crucible tongs from now on.
(3) Determine the mass of the crucible.
(4) Weigh approximately 0.5 g of the BaCl2.xH2O(s) accurately in the crucible.
(5) Heat the crucible and the sample for approximately 10 minutes and place
these in the desiccator to cool down.
(6) Determine the mass of the crucible and the sample.
(7) Heat the crucible and the sample again for 5 minutes, cool them in the
desiccator, and determine their mass once again.
(8) If the mass differs by more than 2% from the previous mass, heat the
crucible and sample for a further 5 minutes, and cool and weigh them
again.
Tabulation of results

Mass of crucible and sample (g)

Mass of crucible and sample after 1st heating (g)
Mass of crucible and sample after 2nd heating (g)
Mass of crucible and sample after 3rd heating (g)
Mass of empty crucible (g)
Mass of sample BaCl2.xH2O(s) (g)
Mass of sample after heating (BaCl2) (g)
Mass of H2O expelled (g)

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Calculations

COMPOUND MASS (g) MOLE (mol) MOLE RATIO

BaCl2

H 2O

11.3 VOLUMETRY/TITRIMETRY

11.3.1 Terminology
Titrimetry – A group of analytical methods based on determining the quantity
of a reagent of known strength that is required to react completely with the
analyte.
Standard solution – A solution of which the concentration is accurately known.
Important requirements for a standard solution are the following:
(1) It must be sufficiently stable so that it is necessary to determine its
concentration only once;
(2) It must react fast with the substance whose concentration is being
determined, so that the time required between additions of reagent
is minimised;
(3) It must react more or less completely with the analyte so that
satisfactory end points are realised (give a clear end point for the
reaction in the titration process);
(4) It must undergo a selective reaction with the analyte that can be
described by a simple balanced equation.
Standardisation – The process through which the concentration of a solution
is determined.
Primary standard – A highly purified compound that serves as a reference
material in all volumetric and mass titrimetric methods. The accuracy of a
method is critically dependent on the properties of this compound.
Important requirements for a primary standard are:
(1) High purity. Established methods for confirming purity should be
available.
(2) Stability toward air. It must be stable under ambient conditions.
(3) Absence of hydrate water so that the composition of the solid does
not change with variations in relative humidity.
(4) Ready availability at modest cost.
(5) Reasonable solubility in the titration medium (usually water).
(6) Reasonably large molar mass so that the relative error associated
with weighing the standard is minimised.
Titration – The process in which controlled volumes of one reagent with
unknown concentration are added to another reagent with known concentration
or mass to give a clear end-point volume.
Molarity – The concentration of a solution expressed as the number of moles
of the solute dissolved in 1litre (ℓ) (1 dm3) of the solution.
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38
 11: Q u a nt i t at i ve a n a l y sis

n = n = n×1000 C = concentration (mol/litre or

C= mol.dm-3 or M)
V(liter) V(ml)/1000 V(ml)
n = number of mole (mol)
V = volume

In titrations, ml(cm3) are used as the unit of volume, while the unit for
concentration is the litre (dm3) according to the definition of concentration.
Thus: If you divide by volume in ml (cm3) you must multiply by 1000, and
if you multiply by volume in ml (cm3) you must divide by 1000 in order
to convert ml to ℓ (cm3 to dm3).

11.3.2 Methods for the standardisation of solutions

Primary standard method
The mass of the primary standard to be weighed must be calculated so that the
mass will use ± 25 ml (cm3) or 40 ml of the solution in the burette that must
be standardised. The volume used for the solution in the burette depends on
the mass of the primary standard that must be weighed. The pre-calculation
is first done for a volume of 25 ml, and if the mass of the primary standard
that must be weighed is less than 0.2 g, the pre-calculation is repeated for a
volume of 40 ml (40 cm3).

EXAMPLE

A must be standardised, and the primary

standard is B. The concentration of A must be
known approximately. The reaction involved
is as follows:

aA + bB → cC + dD

The mass of B must now be determined so

that it will use either ± 25 ml or 40 ml of A
in the titration.

CA=approximate concentration of A (M) (mol.dm-3

VA= volume with which you want to titrate (ml) (cm3)

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Approximately the calculated mass of B is now weighed accurately, transferred

to an Erlenmeyer flask with distilled water and titrated with A. Another two
masses are weighed accurately and titrated.
The exact mass of B and the titration value of A are now known.
The concentration of A is now calculated as follows:

Mass of B that will use

25ml (40ml) of A

MB= exact mass of B (g)

MB= molar mass of B (g.mol-1

VA = volume of titration (ml) (cm3)

25ml (40ml) of A that must be standardised

ADVANTAGES OF PRIMARY STANDARD METHOD

Since there is weighed three, weighing errors are eliminated.
DISADVANTAGE OF PRIMARY STANDARD METHOD
The weighing process is time consuming.
Standard solution method
A certain mass of the primary standard must be weighed and transferred to a
volumetric flask to prepare a solution of which the concentration is accurately
known. This concentration must be such that approximately equal volumes of
the two solutions are used in the titration.

EXAMPLE
A must be standardised, and the
primary standard is B.
The concentration of A must be
known approximately.
The reaction involved is the
following:
aA + bB → cC + dD
The mass of B must now be
determined so that a standard
solution can be prepared in a
volumetric flask so that equal
volumes in the titration will be used.
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40
 11: Q u a nt i t at i ve a n a l y sis

CA= approximate
concentration of A (M)
(mol.dm-3)

VB= volume of volumetric

flask (ml) (or cm3)

Approximately the calculated mass of B is now weighed accurately, transferred

to a volumetric flask, dissolved in distilled water and then filled up to the mark.
Three 25 ml aliquots are then titrated against A.

The exact mass of B in the volumetric flask and the titration values are now
known. From that the concentration of B is first calculated.

mB= exact mass of B weighed in volumetric flask (g)

VB= volume of volumetric flask (ml) (or cm3)

The concentration of A is now calculated as follows:

CB=concentration of B from first part (M)

(or mol.dm-3

VB=volume of pipette (ml) (or cm3)

VA= volume of titration (ml) (or cm3)

ADVANTAGE OF STANDARD SOLUTION METHOD

Triplicate titrations are quick, since aliquots are withdrawn with a pipette.

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DISADVANTAGE OF STANDARD SOLUTION METHOD

A weighing error can be made, since only one mass determination is done.

11.3.3 Acid–base indicators

This group of indicators shows a colour change when the acidity changes from
acid to alkaline or vice versa.
The choice of an indicator depends on
(1) the clarity of the colour change
(2) the pH of the solution when the end point of the reaction is reached

Na2CO3 against HCl NaOH against HCl

pH pH

Examples of titration curves

11.3.4 Techniques used in titrations

Preparing a standard solution

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42
 11: Q u a nt i t at i ve a n a l y sis

Using a pipette

Using the burette

Hold the Erlenmeyer flask and shake it with your right hand. Your left hand
goes across the burette to regulate the tap.
The end point is the first drop that brings about the desired colour change.

Follow these steps for a successful titration:

•• Wash everything with tap water. Rinse with a little distilled water. Using
a burette
•• Make sure that the apparatus is clean. It is especially important that the
burette is not greasy.
•• Rinse the container in which you fetch the solution beforehand with a little
of the solution.
•• Rinse the burette with a little of the solution that goes in it.
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•• Rinse everything else with distilled water only.

•• The first aliquot in the standard solution method is used to rinse the pipette,
and is then thrown away.

11.3.5 Experiment 4
Titration of a strong base with a strong acid
Aim
The aim of this experiment is to determine the concentration of an aqueous
sodium hydroxide solution.

Introduction
In the experiment you will determine the concentration of an aqueous sodium
hydroxide solution. This solution is titrated with a standard solution of dilute
hydrochloric acid and methyl red is used as the indicator.

Procedure
1. Background
Read the sections dealing with the use of the pipette and burette in your manual.
Before performing the titrations yourself, the supervisors will demonstrate to
you the proper use of the volumetric glassware. The difference between a
‘rough’ titration and an ‘accurate’ titration will also be demonstrated.

2. Preparation of glassware
(a) Make sure that all glassware used in the experiment is clean and not
greasy: no droplets of water should stick to the walls of the pipette and the
burette. If necessary, wash the glassware with soap or detergent solution.
(b) Rinse the glassware with tap water and then with distilled water.

3. Collection of solutions to be used in the experiment

Use clean 100 mL beakers. Label them clearly with the name of the solution.
Before you add the stock solution to your beaker make sure that the beaker is
dry, or rinse the beaker with a small quantity of the stock solution.

Note: NEVER pour excess solution back into the stock bottle.

4. Filling of the burette with aqueous hydrochloric acid

(a) Rinse the burette and a small funnel twice with some 10 mL of aqueous
hydrochloric acid.
(b) Clamp the burette and fill it with dilute hydrochloric acid till close to the
zero mark. Use a small funnel and remove it immediately after use. (Make
sure that air can escape from the burette when filling it.)
(c) Drain a few milliliters of the solution to make sure that there are no air
bubbles trapped in the jet below the tap. If the air bubble persists, slant
the burette at the sink and open the tap to allow some of the solution to
flow out with the air bubble.
(d) Take the initial burette reading to 0,01 ml. To avoid parallax error, your
eye should be level with the bottom of the meniscus when you take this
reading.
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5. Transfer of aqueous sodium hydroxide solution to the conical flask

(a) Pour about 5 mL of the aqueous sodium hydroxide solution into a clean
beaker.
Using this solution, rinse the pipette twice.
(b) Discard the solution left in the beaker (if any) and refill with enough fresh
aqueous sodium hydroxide solution needed for the actual transfer.
(c) Pipette 25 mL of aqueous sodium hydroxide solution into a conical flask:
•• Use a pipette-filler to fill the pipette above the mark.
•• Remove the bulb and use your index finger to bring the level of liquid to
the line on the pipette. Make sure that the lower curve of the meniscus
sits on the line.
•• Transfer the liquid to a clean conical flask. (Note: The conical flask
should have been rinsed with distilled water only).
•• Do not blow out the small amount of liquid that remains in the pipette.
•• Place the conical flask on a white tile.
•• Place the conical flask on a white tile.
(d) Using a wash bottle with distilled water, flush down the droplets of the
sodium hydroxide solution remaining on the inside wall of the flask.

6.Titration
(a) Titration technique
(i) Hold and control the burette tap with the left hand, at the same time
swirl the conical flask with the right hand. (If you are left-handed the
opposite applies). Refer to the diagram on the left.
(ii) Rinse down the sides of the conical flask with distilled water during
the titration. Learn how to control the tap to give you a drop at a time
and also how to split a drop so that you can add half a drop near
the end point.
(iii) Perform one rough titration followed by two accurate titrations. (This
should be carefully demonstrated).

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(b) Rough titration

A “rough” titration is normally performed as a time-saving procedure if sufficient
sample is available. The accurate titrations can then be performed much faster.
Steps:
(i) Add a few (1 or 2) drops of methyl red indicator solution to the
aqueous sodium hydroxide solution inside the conical flask. Swirl
the flask. Note the colour.
(ii) Place the conical flask on a white tile.
(iii) Record the initial reading of the burette in-the table of your report
sheet.
(iv) From the burette, add 1 mL portions of the dilute hydrochloric acid
at a time, to the conical flask. Swirl the flask carefully after each
addition, but not too vigorously!
(v) Stop the titration when the yellow colour has become orange and
record your final reading. At the endpoint of the titration the indicator
has just changed colour.
(c) Accurate Titration
From the rough titration you know where approximately the indicator changes
colour (i.e. where the end point is). Therefore now a large volume of the titrant
can be added all at once. Then a drop at a time is added close to the endpoint.
(i) Clean the conical flask with tap water and then rinse it with distilled
water.
(ii) Transfer 25 mL of the aqueous sodium hydroxide solution with the
bulb pipette to the conical flask. Add a few drops of indicator and
place it on the white tile.
(iii) From the burette add a large volume of dilute hydrochloric acid, i.e.
1 to 2 mL less than was needed for a colour change of the indicator
in the rough titration. Swirl the conical flask.
(iv) Now add dilute hydrochloric acid drop by drop, until the indicator
starts to get a permanent change in colour. Swirl the flask carefully
after each addition.
(v) Record your final reading of the burette (to 0.02 mL) in your Report
Sheet.
(vi) Repeat the accurate titration once more. Three accurate titrations
volumes must be within 0.10 ml. If not, repeat the titration-as many
times as, required.

Table of results

TITRATIONS
Rough 1 2 3
Volume NaOH (ml)
Final burette reading (ml)
Initial burette reading (ml)
Volume HCl (ml)
Average volume HCl (ml)

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11.3.6 Experiment 5
Standardisation of ± 0.1 M HCI with anhydrous Na2CO3 as primary standard

PRIMARY STANDARD METHOD

Special chemicals required Bench chemicals required

Na2CO3(s) - sodium carbonate Methyl orange indigo carmine
(anhydrous) indicator
± 0.1M HCI Deionized water (distilled water)

Apparatus
Weighing boat Burette
3 Erlenmeyer flasks Beaker
White porcelain tile Wash bottle
Spatula

Pre-calculation
A pre-calculation is done to determine the mass of Na2CO3 that will use
± 25 ml or ± 40 ml of the expected ± 0.1 M HCI solution.

VHCl = volume with which

you want to titrate (ml or cm3)

CHCl= approximate
concentration of HCl (M or
mol.dm-3)

Method
(1) Use a clean beaker (it need not be dry) to collect the HCI with which
you are going to titrate. Rinse the beaker with about 10 to 20 cm3 of the
HCI to get rid of any water. Take about 100 cm3 of the HCI solution in
the beaker. (Do not fill the beaker.)

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(2) Pour about 20 cm3 of the HCI into a clean burette and rinse the burette
with the HCI solution to get rid of any water.
(3) Fill the burette, making sure there are no air bubbles.
(4) Accurately weigh the calculated mass of Na2CO3.
(5) Transfer the Na2CO3 to an Erlenmeyer flask by emptying the weighing
boat. (The Erlenmeyer flask must be clean, but need not be dry.)
(6) Dissolve the Na2CO3 in a sufficient amount of distilled water.
(7) Add three drops of indicator and titrate with the HCI solution. Repeat
twice more.
Indicator: Methyl orange indigo carmine
Colour change: Green to grey to purple – end point is grey

Tabulation of results

TITRATIONS
1 2 3
Mass of Na2CO3 + weighing boat (g)
Mass of empty weighing boat (g)
Mass of Na2CO3 (g)
Final burette reading (ml)
Initial burette reading (ml)
Volume HCI (ml)
Concentration HCI (M)
Average concentration of HCI (M)

Calculations

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11.3.7 Experiment 6
Standardisation of ± 0.1 M NaOH with KHC8H4O4 as primary standard

STANDARD SOLUTION METHOD

Special chemicals required Bench chemicals required

KHC8H4O4 - potassium hydrogen Phenolphthalein indicator
phthalate (KHP) Deionized water (distilled water)
± 0.1 M NaOH

Apparatus
Weighing boat Burette
3 Erlenmeyer flasks Beaker
White porcelain tile 25 ml pipette and pipette pump (suction bulb)
Wash bottle 250 ml volumetric flask with stopper
Spatula

Theory
Potassium hydrogen phthalate is an acid salt. It contains an ionisable hydrogen
that can be transferred to a base in an acid–base reaction.

phthalic acide potassiumhydrogen phthalate

Precalculations

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Method
Accurately weigh the calculated mass of KHC8H4O4, and transfer it to a
volumetric flask. (Procedure to prepare a standard solution on page 35.)

Titrate three 25 ml aliquots with the NaOH solution. Add three drops of
indicator before titration. (Procedure for using a pipette on page 36.)

Indicator: Phenolphthalein

Colour change: Colourless to pink – end point is the first tinge of pink

Tabulation of results:

CONCENTRATION KHC8H4O4
Mass of KHC8H4O4 + weighing boat (g)
Mass of empty weighing boat (g)
Mass of KHC8H4O4 (g)
Concentration of KHC8H4O4 (M)

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TITRATIONS
1 2 3
Volume KHC8H4O4 (ml)
Final burette reading (ml)
Initial burette reading (ml)
Volume NaOH (ml)
Average volume NaOH (ml)
Average concentration of NaOH (M)

Calculations

Precalculations

VKHP = 250 ml
(Volume of volumetric flask)
VKHP = 25 ml (Volume of pipette)
VNaOH = volume of titration

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