CHE1503-001 2016 4 B PDF

DEPARTMENT OF CHEMISTRY
Laboratory Manual for
CHE1503
FIRST YEAR
CHEMISTRY PRACTICAL
S DUBE
UNIVERSITY OF SOUTH AFRICA,

PRETORIA
© 2015 University of South Africa
All rights reserved
Printed and published by the

University of South Africa
Muckleneuk, Pretoria
CHE1503/1/2016
60158697
InDesign
PR_Tour_Style
CONTENTS
Page
INTRODUCTIONv
GENERAL INFORMATIONviii
LABORATORY SAFETY RULESix
LABORATORY EQUIPMENTx
1 TITRATION PRACTICALS 1
Experiment 1: S tandardisation of sodium hydroxide stock solution with
potassium hydrogen phthalate5
Experiment 2: Determination of the acid content of vinegar11
Experiment 3: S tandardisation of sodium thiosulphate solution with
potassium iodate18
Experiment 4: Determination of the available chlorine in a commercial bleach23
Experiment 5: Standardisation of potassium permanganate using
sodium oxalate29
Experiment 6: D
etermination of the composition of a ferrous salt with
standard potassium permanganate34
2 INORGANIC CHEMISTRY PRACTICALS 39

Experiment 1: Classification of chemical reactions40
Experiment 2: Investigation of some precipitation reactions48
3 PHYSICAL CHEMISTRY PRACTICALS 55

Experiment 1: Enthalpy of fusion of ice56
Experiment 2: P
roperties of systems in chemical equilibrium –
Le Chatelier’s principle63
4 ORGANIC CHEMISTRY PRACTICAL 71

Experiment 1: Ester formation: the synthesis of acetylsalicylic acid (aspirin)72
...........
iii CH E1503/1
I nt r o d u c t i o n
INTRODUCTION
This is the laboratory manual for CHE1503.
Purpose of the module

The purpose of CHE1503, which is a composite practical module, is to equip
you with basic hands-on laboratory skills and techniques associated with some
of the theoretical concepts covered in the modules CHE1501 and CHE1502.
The prescribed practical experiments give you the opportunity to practically
demonstrate general chemistry theory. You will be trained to solve problems
individually, and to develop critical thinking skills.
Module structure
CHE1503 consists of the following four main practical sessions:
•• Titrimetry (analytical chemistry)
•• Physical Chemistry
•• Inorganic Chemistry
•• Organic Chemistry
To complete the module successfully, you must carry out all the experiments
in each session.
•• The Titrimetry session extends over 4 days, and you will carry out 6
experiments.
•• You will carry out 2 experiments during the Physical Chemistry session.
•• You will carry out 2 experiments during the Inorganic Chemistry session.
•• You will carry out 1 experiment during the Organic Chemistry session.
You will also have a session on safety and laboratory waste management.
How to use the laboratory manual

Your laboratory time is very limited, so please prepare for every experiment
in advance. This means that you need to read and understand each experi-
ment before the laboratory session. This reduces errors and will allow you to
carry out the experiments with understanding and efficiency. Each laboratory
experiment includes a pre-lab activity. Please do all the pre-lab activities at
home. Remember to take all the necessary precautionary measures! You need
to submit the activities before you will be allowed to start any practical work.
Your laboratory report sheets are attached at the end of each experiment.
You must complete and submit these at the end of each experiment. The
laboratory report sheets included in this manual are samples, so do not detach
them. You will receive the report sheets you need to use when you complete
each experiment.
...........
v CH E1503/1
INTRODUCTION
CHE1503 PRACTICAL SCHEDULE

A: Titrations
EXPERIMENT OR ACTIVITY NUMBER TITLE
Day 1 Welcome address Laboratory aspects

Introductory talk Aspects of titrations and the concept
Exp 1 of standardisation
Standardisation of sodium hydroxide
stock solution with potassium hydro-
gen phthalate
DAY 2 Pre-lab talk Quantitative analysis using titrimetry

Exp 2 Determination of the acid content of
Exp 3 vinegar
Standardisation of sodium thiosul-
phate solution with potassium iodate
DAY 3 Pre-lab talk Redox titrations

Exp 4 Determination of the available chlorine
Exp 5 in a commercial bleach
Standardisation of potassium perman-
ganate using sodium oxalate
DAY 4 Pre-lab talk Determination of the composition of

Exp 6 a ferrous salt with standard potassium
permanganate
DAY 5 CHE1502 discussion class Discussion class and submission of out-

standing reports
...........
vi
B: Specials
[NB: Specials refers to Organic, Physical, Inorganic Chemistry related experi-

ments as well as the Safety and Laboratory Waste Management activities.]
Group # Monday Tuesday Wednesday Thursday Friday
4 Organic Inorganic Physical Lecture Report

Chemistry Chemistry Chemistry CHE1502 writing
Experiment 1: Experiment 1: Experiment 1: and sub-
Ester forma- Classification Enthalpy of fu- mission
tion: the of chemical sion of ice
synthesis of reactions Experiment
acetylsalicylic Experiment 2: Properties
acid (aspirin) 2: Investiga- of systems
tion of some in chemical
precipitation equilibrium –
reactions Le Chatelier’s
principle
5 Inorganic Physical Organic Lecture Report

and sub-
mission
6 Physical Organic Inorganic Lecture Report

and sub-
mission
...........
vii CH E1503/1
INTRODUCTION
General information
(1) Time: The practical work will begin at 08:00 and end at 16:00. There will
be a lunch break between 12:00 and 13:00. No students will be allowed
in the laboratory during the lunch break and before 08:00 or after 16:00.
(2) Venue: Chemistry Department, Eureka Building, Florida Campus, Corner
of Christiaan de Wet Road and Pioneer Avenue, Florida, Johannesburg.
(3) Equipment: You will be assigned a locker which contains the glassware
for the experiments. You must check to see if you have all the equipment,
and sign a receipt for it. At the end of the practical session you must clean,
dry and return your glassware. Your demonstrator must check your locker
in order for you to obtain credit for returning the glassware.
(4) Laboratory notebook: You will receive an orange book. Use this as your
laboratory notebook. As you proceed with your experimental work, make
sure that you enter all data into your notebook. Amounts weighed and
volumes of reagents measured must be clearly stated in the laboratory
work. The laboratory notebook does not have to be neat, but it must
be readable. If you do not keep a notebook, you are at a risk of losing
marks. Do not scribble results, observations, or weighing data on pieces
of a paper or your lab coat!
(5) Reporting: Enter all results and calculations onto the laboratory report
sheet, and submit this for marking at the end of the experiment or when
your lecturer asks you to do so.
(6) Assessment criteria: The final mark for the practical examination will be
calculated from the weighted average of all six titration experiments plus a
contribution from the physical chemistry, organic chemistry and inorganic
chemistry experiments. There will be a session on safety and laboratory
waste management, and you will also be assessed on that.
You must attend all the practical sessions. If you miss one practical session,
you will automatically fail CHE1503.
In order to pass, you must obtain a minimum weighted average of 50% for
all the experiments.
...........
viii
Laboratory safety rules

Safety in the laboratory is extremely important. Please obey these safety rules:
(1) Know where the safety equipment is kept. This refers to fire extinguishers,
first aid kits, eye wash bottles and waste containers.
(2) Never work alone in a laboratory.
(3) You may not work in a laboratory outside scheduled hours unless the
lecturer in charge has given you permission to do so.
(4) Wear safety glasses when working in the laboratory.
(5) Tie or clip your hair back if it is long or hangs in your face.
(6) Report all accidents, however small, to the lecturer in charge immediately.
(7) If you accidentally spill materials on the bench or floor, wipe up the spill
immediately and wash the area thoroughly.
(8) Wear closed shoes in the laboratory.
(9) Wear clothes that cover your torso and legs to the knee.
(10) Do not smoke, eat or drink in the laboratory.
(11) Never taste chemicals or allow them to come into contact with your body.
(12) Do not smell a chemical by holding it close to your nose.
(13) You may not conduct unauthorised experiments. If you wish to try some-
thing new, obtain permission from the lecturer.
(14) When you are heating liquids in a test tube, do not point the test tube
towards yourself or towards anybody else.
(15) When you are diluting acids, pour the strong acid into water slowly and
stir constantly. NEVER POUR WATER INTO A STRONG ACID.
(16) Do not pipette solutions by mouth.
(17) Dilute strong concentrated acids and bases carefully before emptying
them into the sink (dispose of organic wastes in the appropriate organic
solvent containers).
(18) Do not play or joke around in the laboratory.
(19) Use a fume hood for experiments involving noxious fumes.
(20) Do not use faulty equipment. Return it to the staff member in charge.
(21) Remove broken glassware and paper from sinks.
(22) Dispose of broken glassware in designed glass bins and not in ordinary
paper bins.
(23) Consult a demonstrator before you use any electrical equipment or instru-
ment for the first time.
(24) Wash your hands and apparatus you have used before you leave the
laboratory.
...........
ix CH E1503/1
INTRODUCTION
Laboratory equipment
Crucible tongs Ring support
Utility clamp
Clay triangle
Ring stand
Forceps
Bunsen burner Buret clamp Wire gauze

(Tirrill type)
Spatula
Test tube holder

Wing top
(flame spreader)
Watch glass
Evaporating dish Pneumatic trough
...........
x
Beaker Erienmeyer flask Florence flask
Wide mouth bottle Wash bottle

Test tube brush
Test tube
Ignition tube
Graduated cylinder
Buret Graduated Volumetric Pasteur Medicine Thistle

pipet pipet pipet dropper top
Thermometer
Test tube rack

Crucible and cover Funnel Deflagration spoon
...........
xi CH E1503/1
INTRODUCTION
...........
xii
T I T R AT I O N P R A C T I C A L S
...........
1 CH E1503/1
T I T R AT I O N PR AC T I C AL S:
Titration procedure
1. Background
Read the sections dealing with the use of the pipette and burette in your manual.
Before you perform the titrations yourself, the supervisor will demonstrate to
you how to use the volumetric glassware properly. The supervisor will also
demonstrate the difference between a rough titration and an accurate titration.
2. Preparation of glassware
(a) Make sure that all glassware used in the experiment is clean, and not
greasy. There must be no droplets of water sticking 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.
NEVER POUR EXCESS SOLUTION BACK INTO THE STOCK BOTTLE.
4. Filling the burette with aqueous solution, e.g. dilute (0.1 M)

sodium hydroxide
(a) Rinse the burette and a small funnel twice with 10 mL of the aqueous
standard solution.
(b) Clamp the burette and fill it with dilute sodium hydroxide using a small
funnel till close to the zero mark. Remove the funnel immediately after
use. (To avoid spillage, when you are filling the burette, make sure that
air can escape from it. You can do this by placing a paper clip or a piece
of clean paper between the funnel and the burette.)
(c) Drain a few millilitres 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. You might have to shake the air bubble out
while the solution is running out.
(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.
...........
2

5. Transfer of aqueous solution, e.G. Potassium hydrogen phthalate

solution, to the conical flask
(a) Pour about 5 mL of the aqueous potassium hydrogen phthalate solution
into a clean beaker. Using this solution, rinse the pipette twice.
(b) If there is any solution left in the beaker, discard it and refill the beaker
with as much fresh aqueous potassium hydrogen phthalate solution as
you need for the actual transfer.
(c) Pipette 25 mL of aqueous potassium hydrogen phthalate solution into a

conical flask.
•• Use a pipette-filler to fill the pipette to above the mark.
•• Remove the bulb and use your index finger to bring the level of liquid
to the line on the pipette. You may also adjust the volume using the
pipette pump. 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.
(d) Using a wash bottle with distilled water, flush down the droplets of the
aqueous sodium hydroxide solution remaining on the inside wall of the
flask.
6. Titration
(a) Titration technique
(1) Hold and control the burette tap with your left
hand, and at the same time swirl the conical flask
with your right hand. (If you are left-handed, the
opposite applies.) Refer to the diagram on the left.
(2) 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 learn how to split a drop so that you can add
half a drop near the end point.
(3) Perform one rough titration followed by three
accurate titrations. (This should be carefully
demonstrated.)
(b) Rough titration
...........
3 CH E1503/1
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:
(1) Add 1 or 2 drops of phenolphthalein indicator solution to the aqueous

potassium hydrogen phthalate solution in the conical flask. Swirl the flask.
Note the colour.
(2) Place the conical flask on a white tile.
(3) Record the initial reading of the burette in the table on your laboratory
notebook and report sheet.
(4) From the burette, add the dilute sodium hydroxide solution, 1 mL at a
time, to the conical flask. Swirl the flask carefully after each addition.
Don’t swirl too vigorously!
(5) Stop the titration when the first faint pink colour appears and holds for
about 30 s. 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 approximately where 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.
Steps:
(1) Clean the conical flask with tap water, and then rinse it with distilled water.
(2) Using the bulb pipette, transfer 25 mL of the potassium hydrogen phthalate
solution to the conical flask. Add a few drops of indicator and place the
conical flask on the white tile.
(3) From the burette, add a large volume of dilute sodium hydroxide, 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.
(4) Now add dilute sodium hydroxide drop by drop, ensuring that you rinse
down with distilled water, all splashes on the inner walls of the flask.
Continue titrating until the indicator starts to change to a faint pink colour
permanently. Swirl the flask carefully after each addition.
(5) Record your final burette reading (to 0.02 mL) on your laboratory note-
book and report sheet.
Repeat the accurate titration once more. Three accurate titration volumes must
be within 0.10 mL. If not, repeat the titration as many times as you need to.
...........
4
EXPERIMENT
1 1
Standardisation of sodium hydroxide

1
stock solution with potassium hydrogen

phthalate
Introduction
The equation for the titration reaction is:
KH(C8H4O4) + NaOH → NaK(C8H4O4) + H2O
AIM
The aim of this experiment is for you to prepare your own stock solution of
NaOH and standardise it using a primary standard such as potassium hydro-
gen phthalate. You will have to calculate the exact concentration in moles
per litre of your NaOH stock solution. The molecular mass of KHC8H4O4 is
204.23 g mol-1.
Reagents: A.R. potassium hydrogen phthalate

0.1 M NaOH solution
phenolphthalein indicator solution
Procedure
(a) Calculate the mass of A.R. potassium hydrogen phthalate needed to pre-
pare a 0.1 M solution in a 250 mL volumetric flask. Ask a demonstrator
to check your calculations.
(b) Weigh by difference the potassium hydrogen phthalate, as supplied in a

glass vial, accurately to the nearest 0.1 mg (0.0001 g or 4 decimal places).
The procedure is as follows:
•• Zero a 4-place balance and weigh the weighing bottle and solid.
Record the value.
•• Transfer the solid into the funnel, placed into a suitable volumetric flask.
...........
5 CH E1503/1
•• Zero the 4-place balance (or check whether it is zeroed) and weigh
the “empty” bottle and residue. Record the value.
•• The amount of solid transferred into the volumetric flask is the difference
between the two recorded values.
(c) Half-fill the volumetric flask with deionized water and close it with a
stopper. Swirl the solution, without the solution touching the stopper, to
dissolve the solute.
(d) When all the solute has dissolved, make the solution up to the mark with
deionized water. Shake to mix well.
(e) Fill the burette with 0.1 M sodium hydroxide solution that has been
provided. (Refer to page 15 of this manual for notes on how to fill the
burette. It is critical to ensure that the burette is filled correctly, and that
it does not have an air pocket trapped in the tip.)
(f) Pipette a 25 mL aliquot of potassium hydrogen phthalate into each of

three 250 mL conical flasks. (Refer to page 16 of this manual for notes
on how to pipette.)
(g) Add 4 to 6 drops of phenolphthalein solution to the flask, carry out a

rough titration (see page 17) with your approximately 0.1 M NaOH stock
solution.
(h) Repeat the titration until you obtain three consistent results – in other
words, the individual titrations should not differ by more than 0.1 mL.
Note: Save the NaOH stock solution for Experiment 2.
...........
6
E XPERIMENT 1: Standardisation of sodium hydroxide stock solution with p otassium hydrogen phthalate
TITRATIONS - EXPERIMENT 1
PRE–LAB SHEET
Fill in this sheet before you come to the practical, and have it signed by
the demonstrator.
Surname: …………………………. First names: …………………...........…....……
Student No.: ……………………….. Group No.: …………………...........…...……..
Title of experiment: …………………………………………………………………………
(1) In the table below, list the apparatus and chemicals required for this
experiment.
Apparatus required Chemicals required
(2) Answer the following questions.
(a) Why should you never heat a volumetric flask, or add a hot solu-
tion to a volumetric flask?
(b) What is a standard solution?
(3) To how many decimal places should you report the volume (in mL) con-
tained in a 250 mL volumetric flask?
...........
7 CH E1503/1
(4) What is the molarity of a solution made by dissolving 5.25 g of potassium

hydrogen phthalate in distilled water and making it up to 250 mL with
distilled water in a volumetric flask?
(5) If 16.41 mL of aqueous NaOH is required to neutralise 20 mL of potas-

sium hydrogen phthalate solution described in question 4 above, what is
the molarity of the aqueous sodium hydroxide? Show your calculations
as required below:
(a) Write the reaction equation for the titration.
(b) Calculate the number of moles of KHC8H4O4 used in the titration.
(c) Using the balance reaction equation, find the number of moles
of NaOH that reacted.
(d) Calculate the molarity of the NaOH solution.
...........
8
E XPERIMENT 1: Standardisation of sodium hydroxide stock solution with p otassium hydrogen phthalate
TITRATIONS – EXPERIMENT 1
the demonstrator.
Experimental data
Mass of potassium hydrogen phthalate dissolved
Volume of potassium hydrogen phthalate pipetted
Mass of sodium hydroxide dissolved
(1) Calculate the molarity (mol L-1) of potassium hydrogen phthalate.
Results
Burette reading Rough titration Accurate titration
1st 2nd 3rd
Final reading (mL)
Initial reading (mL)
Volume added
Average volume of aqueous sodium hydrogen added
...........
9 CH E1503/1
Calculations
(a) Write the chemical equation for the reaction between aqueous
sodium hydroxide solution and potassium hydrogen phthalate.
Calculate the molarity of sodium hydroxide solution. (Use THE pre-lab SHEET
as a guide.)
...........
10
EXPERIMENT
2 2
Determination of the acid content of

2
vinegar
Introduction
Vinegar is essentially an aqueous solution of acetic acid, which is a carboxylic

acid. The acid has one ionisable proton, the hydrogen from the –OH group,
and it is a weak acid, with pKa value of 1.75 x 10 -5 at 25 °C. The total acid
content of vinegar can be determined by titration with a standard base such
as sodium hydroxide, using phenolphthalein as the indicator. The principal
acidic constituent is acetic acid. Although other acids are also present, the
results are reported in terms of acetic acid, which normally ranges between
4 and 6% (w/v).
The equation for the titration reaction is:
CH3COOH + NaOH → CH3COONa + H2O
The molecular mass of acetic acid is 60.05 g mol-1. Since the information on
the vinegar bottle label gives the concentration of acetic acid in w/v %, you
have to convert a concentration of acetic acid in mol/L to that in mass of acetic
acid per 100 mL of vinegar.
AIM
The aim of this experiment is to determine the number of g of acetic acid per
100 mL of the unknown vinegar sample.
Reagents: unknown vinegar sample
ca. 0.1 M NaOH standard solution (from Experiment 2)
phenolphthalein indicator solution
Procedure
Work individually
(a) Pipette 25 mL of your unknown vinegar solution into a 250 mL volumetric

flask and dilute to the mark with deionized water. Shake to mix well.
...........
11 CH E1503/1
(b) Fill the burette with your standardised sodium hydroxide solution from
Experiment 1, ensuring that there is no air pocket in the burette tip.
(c) Pipette a 25 mL aliquot of the diluted vinegar solution into each of three
250 mL conical flasks.
(d) Dilute each aliquot with an equal volume of deionized water. Then add
4 to 6 drops of phenolphthalein indicator.
(e) Titrate with your standardised NaOH solution from Experiment 1. The
end point is the first permanent pink colour.
(f) Repeat the titration until you obtain three consistent results – in other
words, the individual titrations should not differ by more than 0.1 mL.
NOTE: SEE EXPERIMENT 6 AND PREPARE YOUR POTASSIUM PERMAN-

GANATE SOLUTION TWO DAYS BEFORE YOU NEED IT. POTASSIUM
PERMANGANATE DOES NOT DISSOLVE EASILY.
...........
12
E XPER I M EN T 2: D e te r m i n at i o n o f t h e a c i d co nte nt o f v i n e g a r
PRE–LAB SHEET
the demonstrator.
experiment.
(2) In an experiment similar to the one you are about to perform, a student
found that the molarity of acetic acid in a vinegar was 0.640 mol/L.
(a) Calculate the acetic acid in g/L.
(b) What is the concentration of acetic acid in g per 100 mL of vinegar?
...........
13 CH E1503/1
(c) What, therefore, is the weight by volume percentage (w/v %) of

acetic acid in the vinegar?
(d) Is the product information on the label correct if the label states
that the vinegar is 4 w/v %?
...........
14
Laboratory report sheet
You must submit this report sheet before you leave the lab.
Experimental data and results
(1) Information about the vinegar investigated
(i) Brand name of vinegar
(ii) Concentration of acetic acid in the vinegar according to the label
(2) Data concerning the diluted vinegar
Volume of vinegar used to prepare solution
Volume of diluted vinegar
(3) Titration data
Volume of diluted vinegar used in the titration
Molarity of NaOH (aq) used in the titration
...........
15 CH E1503/1
1st 2nd 3rd
Final reading (mL)
Volume added
Average volume of aqueous sodium hydrogen added
Reaction equation for the titration
Calculations
(a) From the titration results, calculate the number of moles of NaOH required
to neutralise the acetic acid in the 25 mL of vinegar.
(b) Calculate the number of moles of acetic acid in the 25 mL of diluted

vinegar used in the titration.
(c) Find the molarity of acetic acid in the diluted vinegar.
...........
16
(d) What is the dilution factor used in preparing the diluted vinegar from the
original vinegar?
(e) Calculate the molarity of acetic acid in the original vinegar.
(e) Express the concentration of acetic acid in the vinegar in
(i) g/L
(ii) g/100 mL
(f) What, therefore, is the weight by volume percentage (w/v %) of acetic

acid in the vinegar?
...........
17 CH E1503/1
EXPERIMENT
3 3
Standardisation of sodium thiosulphate

3
solution with potassium iodate
Introduction
Sodium thiosulphate is not of ultra-high purity, and hence does not qualify to
be used as a primary standard in titrations. It should therefore be standardised
against a primary standard, potassium iodate (KIO3), in order to determine
its accurate concentration. The standardisation involves two redox equations
described below:
2S2O32–+ I2 → S4O62- + 2I-
IO3- + 5I- + 6H+ → 3I2 + 3H2O
In the second equation IO3- plays an oxidative role, where I- ions are oxidised
to I2 under acidic conditions, causing the solution to turn a brownish colour.
The iodine produced is then titrated with Na2S2O3 solution, using starch as an
indicator. The starch indicator is not added until the brownish colour, due to
iodine, has changed to pale yellow. When the starch is added to the solution,
the yellow colour changes to blue-black. The end point in the titration is reached
when a drop of the thiosulphate causes the solution to become colourless.
AIM
The aim of this experiment is to determine the actual concentration of the

thiosulfate solution (in mol/L) using potassium iodate as a standard. The mo-
lecular mass of KIO3 is 214 g mol-1.
Reagents: KIO3 (A.R.)
20 g Kl (iodate free) (for use in Experiments 3 and 5)
1 M HCI solution
0.1 M Na2S2O3 stock solution
Starch indicator solution
...........
18
E XPER I M EN T 3: St a n d a r d is ati o n o f s o d iu m t h i o su lp h ate s o lu t i o n w i t h p o t assiu m i o d ate
Procedure
(a) Calculate the mass of A.R. KIO3 needed to prepare a 0.016 M solution in
a 250 mL volumetric flask. Ask a demonstrator to check your calculations.
(b) Following the procedure given in Experiment 1, weigh by difference the

KIO3, as supplied in the glass vial, accurately to the nearest 0.1 mg. (Use
a 4-place balance.)
(c) Transfer the weighed KIO3 into a 250 mL volumetric flask, dissolve it, and
then make to the mark with deionized water. Shake to mix well.
(d) Fill the burette with 0.1 M Na2S2O3 stock solution, ensuring that there is
no air pocket in the burette tip.
(e) Pipette a 25 mL aliquot of the KIO3 solution into each of three 250 mL
conical flasks.
(f) Treat each aliquot individually from this point. Weigh 2 g Kl into a weigh-
ing beaker and add it to the conical flask, followed by 10 mL of 1 M HCI.
(g) Immediately titrate the liberated iodine with the 0.1 M Na2S2O3 stock
solution. When the colour of the solution becomes pale yellow, dilute
to 100 mL with deionized water and add 3 to 5 drops of starch indica-
tor solution. Continue the titration until the colour changes from blue to
colourless.
...........
19 CH E1503/1
Title of experiment: Standardisation of sodium thiosulfate solution with

potassium iodate
Experimental data
Mass of potassium iodate weighed
Volume of volumetric flask
Volume of potassium iodate solution pipetted
Thiosulfate solution No.
(a) Calculate the mass needed to prepare a 0.016 M solution in 250 mL.
(b) What is the actual molarity of the potassium that you have prepared?
...........
20
E XPER I M EN T 3: St a n d a r d is ati o n o f s o d iu m t h i o su lp h ate s o lu t i o n w i t h p o t assiu m i o d ate
Results
Volume of thiosulfate solution from titration
1st 2nd 3rd
Final reading (mL)
Volume added
Average volume of aqueous thiosulfate added ……………………....……….........
Calculations
(c) Write the chemical equation that describes the reaction involved in this
titration.
(d) Calculate the molarity of sodium thiosulfate.
(e) Describe the colour changes that take place during this experiment. What
is the colour at the end point?
(f) Explain why you added 2 g of KI into the conical flask before titrating.
...........
21 CH E1503/1
(g) Why is it important to also add 10 mL of 1 M HCl into the conical flask?
...........
22
EXPERIMENT
4 4
Determination of the available chlorine in

4
a commercial bleach
Introduction
Commercial bleach usually contains sodium hypochlorite, which is the active

constituent responsible for the bleaching action. When a bleach is treated with
hydrochloric acid, chlorine is liberated. An iodometric method may be used
to determine the amount of hypochlorite present in the bleach. The result is
normally reported as available chlorine. Available chlorine refers to the chlo-
rine which is liberated by the action of dilute acids.
A measured amount of a solution of the bleach sample is treated with an excess

of KI in acidic solution. The sodium hypochlorite in the bleach oxidises the
iodine ions. The liberated iodine will then be determined by titration with a
standard thiosulphate solution according to equation (3) below.
The equations for the reactions are:
OCl- + Cl- + 2H+ → Cl2 + H2O (1)
OCl- + 2I- + 2H+ → I2 + H2O + Cl- (2)
I2 + 2S2O32- → 2I- + S4O62- (3)
AIM
The aim of this experiment is to calculate the number of g of CI2 in a 100 ml

sample.
The molecular mass of chlorine is 70.91 g mol -1.
Solutions: Unknown bleach sample (ca. 70 mL)

1 M HCL solution
1 M NaOH solution
10 g KI (from Experiment 3)
M Na2S2O3 standardised (from Experiment 3)
Starch indicator solution
...........
23 CH E1503/1
Procedure
Work individually
(a) Pipette 25 mL of the unknown bleach solution into a 250 mL volumetric

flask. Add 2 mL of 1 M NaOH and dilute to the mark with deionized
water.
(b) Fill in the burette with 0.1 M Na2S2O3 standardised solution (from Experi-
ment 3), ensuring that the burette tip is free of an air pocket.
(c) Pipette a 25 ml aliquot of the diluted bleach solution into a 250 mL coni-
cal flask.
(d) Add 2 g Kl and 20 mL of 1 M HCI.
(e) Immediately titrate the liberated iodine with standard 0.1 M Na2S2O3 solu-
tion. When the colour becomes a pale yellow, add 3 to 5 drops of starch
indicator solution. Continue the titration until the colour changes from
blue to colourless. (If the titre is not reasonable, calculate on the basis
of the titration the dilution which must be made of the initial unknown
bleach solution in order to obtain a reasonable titre.)
(f) Repeat the titration procedure to obtain three consistent titres.
...........
24
E XPER I M EN T 4: D e te r m i n at i o n o f t h e av a i l a b l e c h l o r i n e i n a co m m e rc i a l b l e a ch
PRE–LAB SHEET
the demonstrator.
experiment.
(2) Consider the reaction of sodium hypochlorite with iodine. Which species
is oxidised and which is reduced? (Give the oxidation numbers of the
atoms to illustrate your answer.)
(3) Describe the colour changes that take place during this experiment. What
is the colour at the end point?
...........
25 CH E1503/1
(4) Why is hydrochloric acid added to the dilute bleach and iodine in the
conical flask?
(5) Explain why hydrochloric acid can be added using a measuring cylinder
and not necessarily a pipette.
(6) What is the role of starch in this titration? Why is it added near the end
point of the titration, and not at the beginning?
...........
26
E XPER I M EN T 4: D e te r m i n at i o n o f t h e av a i l a b l e c h l o r i n e i n a co m m e rc i a l b l e a ch
Results of the titration
Concentration of aqueous sodium thiosulphate ………………………………….....
Volume of dilute bleach solution used ……………………………………………......
Results
1st 2nd 3rd
Final reading (mL)
Volume added
Average volume of aqueous sodium thiosulphate added …………………...........
Calculations
(1). Calculate the amount (in moles) of sodium thiosulphate that reacted in
the titration.
(2) Calculate the amount (in moles) of I2 (aq) reduced by the aqueous sodium
thiosulphate.
...........
27 CH E1503/1
(3) Calculate the amount (in moles) of NaOCl in 25 mL of the diluted bleach.
(4) Calculate the concentration of NaOCl in mol/L in the diluted bleach

solution.
(5) Calculate the concentration of NaOCl in the original liquid bleach.
...........
28
EXPERIMENT
5 5
Standardisation of potassium
5
permanganate using sodium oxalate
Introduction
Sodium oxalate is a reducing agent. The oxalate ions can be oxidised to carbon
dioxide. We can use potassium permanganate in an acidic environment as an
oxidising agent. The equation for the titration reaction is:
5C2O42- + 2MnO4 - + 16H+ → 10CO2 + 2 Mn2+ + 8H2O
Because the initial reaction is slow we will have to heat the acidified oxalate
solution before adding potassium permanganate. This titration does not require
an indicator since the permanganate ion is intensely purple in colour and the
manganese (II) ion is almost colourless. Thus endpoints can easily be observed.
The first slight excess of the permanganate imparts a slight pink colour to the
solution, indicating that the oxalate has been completely consumed. In this
experiment sodium oxalate is the primary standard which we use for stand-
ardising potassium permanganate. The molecular mass of sodium oxalate
(Na2C2O4) is 134 g mol-1. The molecular mass of KMnO4 is 158.04 g mol-1.
AIM
The aim of the experiment is to determine the concentration of an aqueous

solution of potassium permanganate solution using a standard solution of
sodium oxalate.
Reagents: KMnO4
1 g primary standard Na2C2O4
0.9 M H2SO4
...........
29 CH E1503/1
Caution!
Potassium permanganate is a strong oxidising agent, and therefore danger-

ous. Take care when handling the solution. Button your lab coat, because if
you get any of the solution on your clothing it will leave a permanent stain.
Also, stains on your hands remain for a long time. Try not to spill any solu-
tion when transferring it into the burette. If you do spill some, wipe it up
immediately.
Procedure
Work individually
(a) Prepare an approximately 0.02 M KMnO4 solution in a 500 ml volumetric

flask, using the special (Milli-Q) water provided. Ask a demonstrator to
check your calculations.
(b) Pre-weigh 0.17 to 0.20 g Na2C2O4 into a small beaker on a toploader bal-
ance (2 decimals). Accurately weigh the small beaker and Na2C2O4 on an
analytical balance (4 decimals).
(c) Transfer the Na2C2O4 to a 400 mL beaker and re-weigh the small beaker.
(d) Dissolve the Na2C2O4 in 125 mL 0.9 M H2SO4 by stirring with a glass
stirring rod.
(e) Heat to 80 to 90 °C, and titrate with the KMnO4, stirring vigorously with
the glass stirring rod. The reagent should be introduced slowly so that the
pink colour is discharged before further additions are made. (See notes 1
and 2.)
(f) If the solution temperature drops below 60 °C, reheat the solution.
(g) The end point is the first persistent pink colour. (See notes at the end.)
(h) Titrate 2 or more Na2C2O4 samples to obtain 3 consistent values for the
titration.
(i) Determine the end point blank by titrating equal volumes of water and
sulphuric acid (125 mL H2O and 125 ml H2SO4). This value should be
deducted from each titre.
Notes: 1. Any KMnO4 splashed on the sides of the titration vessel should
be washed down immediately with a stream of water.
2. If KMnO4 is added too rapidly, some MnO2 will be produced in

addition to Mn2+. Evidence of MnO2 formation is a faint brown
discolouration of the solution. The presence of the precipitate is
not a serious problem, as long as sufficient oxalate remains to
reduce the MnO2 to Mn2+; the titration is temporarily discontinued
until the solution clears. The solution must be free of MnO2 at the
equivalence point.
...........
30
E XPER I M EN T 5: St a n d a r d is at i o n o f p o t assiu m p e r m a n g a n ate u si n g s o d iu m ox a l ate
3. To measure the volume of KMnO4, take the surface of the liquid
as a point of reference. Alternatively, provide sufficient backlight-
ing to permit reading of the meniscus in the usual way.
...........
31 CH E1503/1
experiment.
(2) This experiment involves the reaction between oxalate ions and perman-
ganate ions. What type of reaction is this?
(3) Why do you have to warm the oxalate solution before performing the
titration?
(4) How is the end point of this titration determined?
...........
32
E XPER I M EN T 5: St a n d a r d is at i o n o f p o t assiu m p e r m a n g a n ate u si n g s o d iu m ox a l ate
(5) Write half-equations for this reaction and give the overall balanced equa-
tion for the reaction.
(i) Oxidation half-reaction
(ii) Reduction half-reaction
(iii) Overall reaction equation
(6) Calculate the molarity of potassium permanganate.
...........
33 CH E1503/1
EXPERIMENT
6 6
Determination of the composition of

6
a ferrous salt with standard potassium

permanganate
Introduction
Potassium permanganate is a strong oxidising agent that is used in the deter-

mination of ferrous ion in various samples. The Fe2+ is oxidised to Fe3+ in
the process as described by the equation for the titration reaction:
5Fe2+ + MnO4 - + 8H+ → 5Fe3+ + Mn2+ + 4H2O
The titration does not require an indicator since the end point can easily be
detected when the purple permanganate ion changes to the colourless man-
ganese (II) ion.
AIM
The objective of this experiment is to calculate the percentage of ferrous sulphate

in the impure sample, given that the molecular mass of FeSO4 is 151.91 g mol-1.
Note: Ferrous solutions are not air stable, and will oxidise on standing. The
stock ferrous solution should be used on the same day that it is prepared.
Reagents: 10 g ferrous salt unknown
2 M H2SO4 reagent
H3PO4 reagent
0.02 M KMnO4 standard solution
Procedure
Work individually
(a) Weigh by difference the approximately 7 g of supplied impure ferrous

sulphate sample accurately on a 4-place balance. Transfer it into a 250 mL
volumetric flask. Immediately add 5 ml of 2 M H2SO4 solution to prevent
...........
34
EXPERIMENT 6: Determination of the composition of a ferrous salt with standard potassium permanganate
hydrolysis. (Pour it through a funnel into the flask.) Allow it to dissolve

and make to the mark with deionized water.
(b) Place 25 mL aliquots of this stock solution into each of three 250 mL
conical flasks.
(c) Add 10 mL of 2 M H2SO4 and 1 mL H3PO4 and titrate with standard 0.02
M KMnO4 solution. One drop of the permanganate standard solution in
excess of the equivalent amount of ferrous ion will produce a permanent
pink colour which indicates the end point of the titration.
Note: Permanganate solutions should not be allowed to stand in burettes any

longer than necessary because decomposition to MnO2 may occur. Freshly
formed MnO2 can be removed from burettes and glassware with a solution
of acidified FeSO4.
At the end of the experiment, use the remaining ferrous sulphate solution
to clean the burette.
...........
35 CH E1503/1
Experiment 6: Laboratory report sheet
Title of experiment: Determination of the composition of a ferrous salt

with standard KMnO4
Experimental data
Mass of iron (II) sulphate weighed ……………………..................................………
Volume of volumetric flask …………………………… ………………………………...
Volume of iron (II) sulphate solution pipetted ....................................................
Concentration of standard permanganate solution ………………………...………
Mass of KMnO4 (weighed in Experiment 6) …………………………………….......
Results
Volume of KMnO4 solution from titration
1st 2nd 3rd
Final reading (mL)
Volume added
Average volume of potassium permanganate added .........................................
Calculations
(a) Write half-equations (oxidation and reduction) for this reaction, and give
an overall balanced equation for the reaction.
...........
36
EXPERIMENT 6: Determination of the composition of a ferrous salt with standard potassium permanganate
(b) Calculate the molarity of FeSO4.
(c) Calculate the percentage of ferrous sulphate in the impure sample.
(d) Explain why the ferrous sulphate solution should be freshly prepared
and used on the same day.
(e) Why is it important to also add 10 mL of 2 M H2SO4 into the conical

flask?
...........
37 CH E1503/1
I N O R G AN I C CH E M IS T RY PR AC T I C AL S:
...........
38
INORGANIC CHEMISTRY PRAC TICALS
...........
39 CH E1503/1

EXPERIMENT
7 1
7 Classification of chemical reactions
Introduction
A chemical reaction is a process in which the reacting substances rearrange

their atoms and electrons into a new pattern, creating new substances that
are the reaction products. All chemical reactions have one characteristic
in common: they always occur so as to increase the stability of the chemical
system. In other words, the reaction products are always more stable than the
reactants. The difference between one reaction and another lies in the details
of the atom and electron rearrangements. A group of different reactions that
have similar reactant-to-product rearrangement details are conveniently col-
lected together into a class of reaction. Some common classes of reaction
are described below.
(1) Combination: The reaction of two substances to form one substance.
C(s) + O(g) → CO2(g)
2Na(s) + Cl2(g) → 2NaCl(s)
MgO(s) + H2O(l) → Mg(OH)2(s)
SO3(g) + H2O(l) → H2SO4(l)
(2) Thermal decomposition: Thermal decomposition occurs when a

substance is heated to a temperature high enough to make it unstable
and cause it to break apart into two or more smaller molecules or
fragments.
2HgO(s) → 2Hg(l) + O2(g)

heat
Ca(HCO3)2(s) → CaCO3(s) + H2O(l) + CO2(g)

heat
Mg(OH)2(s) → MgO(s) + H2O(l)

heat
...........
40
E XPER I M EN T 1: Cl assi f i c at i o n o f c h e m i c a l r e a c t i o ns
(3) Combustion: The rapid reaction of a compound with oxygen. All com-
bustion reactions are also combination reactions.
2Ca(s) + O2(g) → 2CaO(s)
S(s) + O2(g) → SO2(g)
(4) Single replacement: The replacement of an element in a compound by

another element originally in elemental form.
Mg(s) + 2AgNO3(aq) → Mg(NO3)2(aq) + 2Ag(s)
Ca(s) + 2HCl(aq) → CaCl2(aq) + H2(g)
(5) Double displacement (also called metathesis): An exchange of positive

and negative ion partners by two compounds (most commonly involving
two ionic compounds) in aqueous solution. This class of reaction may
be subdivided into precipitation reactions and acid–base neutralisation
reactions. All double displacement reactions may be represented by an
equation of the type:
AB + CD → AD + CB
AgNO3(aq) + NaCl(aq) →AgCl(s) + NaNO3(aq)
(Precipitation reaction. Observation: a precipitate forms.)
K2CO3(aq) + 2HNO3(aq) → 2KNO3(aq) + H2O(l) + CO2(g)
(Acid–base neutralisation followed by decomposition. Observation: a gas is

produced. Note that H2CO3 decomposes to H2O(l) + CO2(g).)
H2SO4(aq) + 2KOH(aq) → K2SO4(aq) + 2H2O(l)
(Acid–base neutralisation. Observation: heat is produced.)
(6) Oxidation–Reduction (Redox): These reactions involve a transfer of va-

lence electrons from one atom to another, resulting in changes in oxida-
tion number of the reacting compounds. Oxidation corresponds to an
increase in oxidation number, while reduction corresponds to a decrease
in oxidation number. Oxidation and reduction always occur together,
hence the name “redox”. To identify a redox reaction, you simply need
to see if there has been a change in oxidation number of the atoms of
the reacting compounds in going to products.
H2(g) + Cl2(g) → 2HCl(g)

ox. No.: 0 0 +1–1
(The oxidation number of hydrogen atoms increased, while that of chlorine

atoms decreased.)
Some of the examples of reactions given under other classes of reactions are
also redox reactions. Verify that the following are redox reactions:
...........
41 CH E1503/1
•• The first two reactions given under combination reactions

•• All the reactions given under combustion and single replacement
In this experiment you will run several reactions and attempt to classify them.
Remember that some reactions may fall under more than one class.
AIM
The aim of this experiment is to classify several chemical reactions.
Procedure
Note:
•• You will work individually.
•• Make observations of the reactants/products before, during, and after the
reaction. Record these directly on your report sheet immediately after
each experiment.
•• Upon completion of the reaction, add the resulting mixture to the container
labelled “Expt 1 – Waste”.
•• Caution: Do not point a test tube towards yourself or any other person.
Reaction 1:
Pour about 2 mL of 0.1 M barium chloride into a test tube and add about 2
mL of 0.1 M sodium sulphate.
Reaction 2:
Add a spatula tip of zinc metal powder to a clean test tube, and then add about
2 mL of 6 M HC1. During the reaction, stopper the test tube with your thumb
for a couple of minutes and insert a lighted splint. (Do not point the test tube
towards yourself or any other person.)
Reaction 3:
Pour about 2 mL of 1 M sodium carbonate into a test tube and add about 2 ml
of 2 M hydrochloric acid. During the reaction, stopper the test tube with your
thumb for a couple of minutes and insert a lighted splint into the gas evolved.
Repeat the experiment. This time, collect some of the gas with a clean dropper
and bubble it into 1 mL of lime water in a small test tube.
Reaction 4:
(a) Pour 20 mL of 0.25 M copper (II) sulphate into a 100 mL beaker. Add
30 mL of 1 M sodium hydroxide and record your observations. Save the
reaction mixture for the next step.
(b) Heat the beaker and contents from step 4a on a hotplate. Stir with a glass
rod until there is no further change. Use the reaction mixture in the next
step.
...........
42
(c) Allow the new precipitate formed in step 4b to settle. Discard the super-
natant solution, and add 25 mL of 1 M sulphuric acid to the precipitate
and stir. Save the reaction mixture for the next step.
Pour about 5 mL of the solution from step 4c into a clean test tube. Add a
spatula tip of zinc metal powder, shake the test tube and observe. Note that
two different reactions occur in this step. Observe and identify the reactions.
You may test for any gas evolved.
...........
43 CH E1503/1
INORGANIC CHEMISTRY SPECIALS – EXPERIMENT 1
PRE–LAB SHEET
the demonstrator.
experiment.
(2) Balance each of the following reactions and then classify each one ac-
cording to one or more of the six classes discussed in the introduction.
(a ……….Mg(s) + …….HCl(aq) → …….MgCl2(aq) + ……H2(g)

Classification:
(b) ……….P4O10(s) +……..C(s) → ………P4(s) + …..CO(g)

Classification:
(c) ……….AgNO3(aq) + ….NaBr(aq) → …….AgBr(s) + ……NaNO3(aq)

Classification:
(d) ……….Cl2(aq) + …….KBr(aq) → ……..Br2(aq) + …….KCl(aq)

Classification:
(e) ……….SO3(g) → ……..O2(g) + …….SO2(g)

Classification:
(f) ……….Ba(OH)2(aq) + …H2SO4 (aq) → ……BaSO4(s) + …..H2O(l)

Classification
...........
44
For each of the reactions performed, write a balanced reaction equation. Note
significant observations before, during and after the reaction (colour, precipitate,
gas evolution, heat evolution, and colour change). Classify the reaction into
one or more of the categories discussed in the introduction.
Reaction 1
Observations
Before the reaction
During the reaction
After the reaction
Reaction equation:
(net ionic)
Classification:
Reaction 2
Observations
Before the reaction
During the reaction
After the reaction
Reaction equation:
Classification:
...........
45 CH E1503/1
Reaction 3
Observations
Before the reaction
During the reaction
After the reaction
Reaction equation:
Classification:
Reaction 4a
Observations
Before the reaction
During the reaction
After the reaction
Reaction equation:
Classification:
Reaction 4b
Observations
Before the reaction
During the reaction
After the reaction
Reaction equation:
Classification:
...........
46
Reaction 4c
Observations
Before the reaction
During the reaction
After the reaction
Reaction equation:
Classification:
Reaction 4d
Observations
Before the reaction
During the reaction
After the reaction
Reaction equation:
Classification:
...........
47 CH E1503/1
EXPERIMENT
8 2
Investigation of some precipitation

8
reactions
Introduction
In this experiment you will apply your knowledge of the solubility rules. In
the first section you will decide which aqueous solutions to use in order to
prepare precipitates of certain insoluble compounds. In the second section you
are asked to identify certain unknown aqueous solutions; here you may also
use your knowledge about the characteristic colours of certain aqueous ions.
AIM
The aim of this experiment is to

•• prepare precipitates of some insoluble compounds
•• identify aqueous solutions of certain salts
Procedure
You will work individually.
Part A. Preparation of precipitates
(1) You are provided with the following aqueous solutions:
(1) barium chloride or barium nitrate (7) silver nitrate
(2) calcium chloride or calcium nitrate (8) sodium chloride
(3) copper (II) sulphate (9) sodium hydroxide
(4) lead (II) acetate or lead (II) nitrate (10) sodium phosphate
(5) magnesium chloride or magnesium nitrate (11) sodium sulphate
(6) potassium iodide (12) sodium

carbonate
The concentration of all these solutions is 0.1 M.
...........
48
E XPER I M EN T 2: I nve s t i g at i o n o f s o m e p r e c i p i t at i o n r e a c t i o ns
(2) From these solutions, select those that you need to prepare the following
precipitates. Use about 1 mL (20 drops) of each solution. Take care not
to contaminate the solutions provided, and use clean test tubes. Do not
interchange the droppers!
Precipitates to prepare:
(a) lead (II) iodide (b) copper (II) hydroxide
(c) calcium phosphate (d) silver chloride
(e) barium sulphate (f) magnesium carbonate
Enter all your data, observations and results in table 2.1 of your report sheet.
Note: Dispose of all reaction mixtures in the labelled waste container.
Part B. Identification of unknown solutions
(1) Each of five bottles, labelled A, B, C, D and E, contain 0.1 M aqueous

solutions of one of the following salts:
•• potassium iodide
•• sodium sulphate
•• ammonium nitrate
•• nickel (II) chloride
•• copper (II) nitrate
(2) Identify which one of the above solutions is in each bottle by carrying
out the tests given in table 2.2 of the report sheet. Use about half a mL
of each solution, and use a fresh sample of solution for each test.
Complete table 2.2 by entering all your observations in the spaces pro-
vided. If a test is negative, indicate this clearly – in other words, do not
leave a blank space in the table.
Note: Dispose of all test solutions and reaction mixtures in the “Waste Solu-
tions” container.
...........
49 CH E1503/1
PRE–LAB SHEET
the demonstrator.
experiment.
(2) Indicate the solubility in water of each of the following groups of compounds:
Substances Solubility
Salts of the alkali metals
Hydroxides
Chlorides
Carbonate
Sulphates
Nitrate
...........
50
(3) How would you test for the presence of the following ions in aqueous
solution of an unknown salt?
Ion Brief description of test Observations if test is

positive
I-
Reaction equation to account for observation:
CO32-
Ag+
Ba2+
(4) Indicate the characteristic colour of each of the following aqueous ions:
Ion Colour when Ion Colour when

aqueous aqueous
Copper (II) Nickel (II)
Iron (II) Chromate (VI)
Iron (III) Barium
Permanganate Cobalt (II)
Chromium (III) Dichromate (VI)
Silver Sodium
Ammonium Potassium
...........
51 CH E1503/1
PART A: Preparation of precipitates
Complete table 2.1 below by filling in the names of the solutions used to pre-
pare the named precipitate. Record the colour of each precipitate.
Table 2.1: solutions and colour of precipitate
Name of precipitate Solutions used Colour of precipitate
Lead (II) iodide
Copper (II) hydroxide
Calcium phosphate
Silver chloride
Barium sulphate
Magnesium carbonate
PART B: Identification of unknown solutions A, B, C, D and E
Fill in the information that is missing from table 2.2. State clearly what was
observed, e.g. “A white precipitate was formed,” or “there was no visible
change”. Do not leave a blank space for a negative test.
...........
52
Table 2.2: Tests on unknown solutions A, B, C, D and E
Unknown Record of the Test 1: Test 2: Test 3:

sample colour of the Add 1 mL of Add 1 mL Add 1 mL of
solution AgNO3 to 1 mL of BaCl2 or Pb(NO3)2 or
of unknown Ba(NO3)2 Pb(C2H3O2)2
to 1 mL of to 1 mL of
unknown unknown
Based on your observations recorded in table 2.2, identify each salt solution
and give a brief explanation for your choice in table 2.3 below.
Table 2.3: Identification of unknown solutions
Solution Identification Explanation
...........
53 CH E1503/1
...........
54
PHYSICAL CHEMISTRY PRAC TICALS
...........
55 CH E1503/1
EXPERIMENT
9 1
9 Enthalpy of fusion of ice
Introduction
The enthalpy of fusion is the energy needed to melt 1 mol of a substance; it

has the units J/mol (or kJ/mol). During a change of state, in this case from solid
to liquid, the temperature of a pure substance remains constant.
In this experiment, ice at 0 °C is added to a known mass of water. Since heat

flows from a warmer body to a cooler body, the ice will absorb heat from the
water and some ice will melt. Once the temperature of the mixture reaches
0 °C, the mass of liquid water is measured again. The additional mass comes
from melted ice. The heat of fusion of the ice can then be determined, using
the mass of ice melted together with the initial temperature and mass of water.
The process takes place in a calorimeter, which is a well insulated container,

so that there is no heat flow between the calorimeter contents and the sur-
roundings: heat flow in the calorimeter is only between the water and the
ice. The heat energy lost by the water must therefore be equal to the heat
energy gained by the ice.
The heat energy lost by the water depends on its mass, its specific heat capac-
ity, and the temperature change. It is given by the formula
q = m x c x ∆T
where q = heat (J),

m = mass (g),
c = specific heat capacity (J °C g-1),
∆T = temperature change = Tfinal – Tinitial (°C).
Note: We assume that the heat lost or absorbed by the calorimeter itself is
negligible.
AIM
The aim of the experiment is to determine the enthalpy of fusion of water.
...........
56
E XPER I M EN T 1: Ent h a lpy o f f u si o n o f i ce
Procedure
Work in pairs.
(1) Collect a digital thermometer and the simple calorimeter (400 mL beaker
with two nested polystyrene coffee cups plus stirrer and lid). Clean and
dry the polystyrene cups. Insert the nested cups in the 400 mL beaker
(see Fig. 1.1). Find the mass of the empty calorimeter with stirrer and lid
(use a top-pan balance), and record this in Table 1.1 of the Report sheet.
Digital
thermometer Stirrer
Lid
Two nested
polystyrene
Mixture
Beaker
Figure 1.1: Simple calorimeter used to find the enthalpy of fusion of ice
(2) With a measuring cylinder, add about 70 mL of distilled water to the
calorimeter, cover with the lid and insert the stirrer. Determine the mass
of the calorimeter with the water and stirrer and lid, and record this in
Table 1.1 of the report sheet.
(3) Stir the water in the calorimeter and record its temperature in Table 1.1.
(4) Collect about 40 g of ice in a small beaker. The ice should have become
a little wet. This indicates that it has started melting, and that its tempera-
ture is 0 °C. Carefully pat the ice dry with some tissue paper, and add it
to the calorimeter. Cover with the lid.
(5) Regularly stir the contents of the calorimeter, and allow to equilibrate
at 0 °C. Some ice should remain in the calorimeter. If no ice remains,
add some more to the calorimeter, stir and allow to equilibrate at 0 °C.
(Make sure that the ice added is at 0 °C – see step 4.) Record this final
temperature in Table 1.1.
(6) Determine the mass of a 250 mL beaker on the top-pan balance and
record this in Table 1.1.
(7) Carefully pour the water from the calorimeter into the beaker from step
6, holding back the ice that has remained. Determine the mass of the 250
mL beaker with water and record this in Table 1.1.
(8) Repeat the experiment to give you a total of two trials.
(9) Calculate the enthalpy of fusion of ice by following the steps indicated in
the report sheet.
...........
57 CH E1503/1
PH YSI C AL CH E M IS T RY PR AC T I C AL S:
PHYSICAL CHEMISTRY SPECIALS – EXPERIMENT 1
PRE–LAB SHEET
the demonstrator.
experiment.
(2) In an experiment similar to that described in the procedure, the following
data were collected:
Initial mass of water in the calorimeter: 70.89 g
Initial temperature of the water in the calorimeter: 17.6 °C
Final mass of water in the calorimeter: 86.48 g
Final temperature in the calorimeter: 0.0 °C
(a) Find the mass of ice that melted.
(b) Calculate the number of mol of ice melted.
...........
58
(c) What was the change in temperature of the initial mass of water
in the calorimeter?
(d) Calculate the energy released by the initial mass of water. (The
specific heat capacity of water is 4.184 J g–1 °C–1.)
(e) What was the energy absorbed by the ice that melted?
(f) Calculate the energy required to melt 1 mol of ice.
...........
59 CH E1503/1
Results and calculations
Enter all your data in Table 1.1 below, and perform the calculations given in
the different steps in this table. Show your calculations.
Table 1.1: Experimental data and calculations
Trial 1 Trial 2
(1) Mass of empty calorimeter

+ lid + stirrer
(2) Mass of calorimeter + water

+ lid + stirrer
(3)
Initial mass of water in
calorimeter
(4) Initial temperature of water
(5) Final temperature of water

+ excess ice
(6)
Mass of empty 250 mL
beaker
(7) Mass of 250 mL beaker + fi-

nal volume of water from the
calorimeter
(8) Final mass of calorimeter
(9) Mass of ice that melted
(10) No. of mol of ice that melted
(11) Change in temperature of

initial water
...........
60
(12) Energy released by initial

mass of water
(13) Energy absorbed by the ice

that melted
(14) Energy required to melt 1

mol of ice
(15) Average energy required to

melt 1 mol of ice
Questions
(1) Write a thermochemical equation for the melting of ice (include the energy
term!)
(2) The accepted value for the enthalpy of fusion of water is 6.01 kJ/mol.
Compare this with your average experimental value, and calculate the
percentage difference between the two. (Express this as a percentage of
the accepted value.)
(3) Comment on the accuracy of your average experimental value.
...........
61 CH E1503/1
(4)
Find below possible experimental errors. Would they have given a higher
or a lower value than the accepted value, or would this have remained
unchanged?
Experimental error Higher / lower / unchanged
Calorimeter was not perfectly insulated.
Heat lost or absorbed by calorimeter itself is …
...........
62
EXPERIMENT
10 2
Properties of systems in chemical

10
equilibrium – Le Chatelier’s principle
Introduction
When working in the laboratory one often makes observations that at first sight
are surprising and hard to explain. One might add a reagent to a solution and
obtain a precipitate – but the addition of more of the reagent to the precipitate
causes it to dissolve. A red solution might turn yellow on addition of a reagent,
while subsequent addition of another reagent brings back the original colour
of the solution. In this experiment we will examine and attempt to explain
several observations of this sort. Chemical systems exist in a dynamic equilib-
rium, where both forward and backward reactions occur simultaneously, but
the concentration of the reactants and products remains constant over time.
If one disturbs the equilibrium by changing the concentration of a reactant

or product, or by changing temperature, the reaction may shift to the left or
the right, producing the kinds of effects mentioned before. The effects of
concentration and temperature changes on systems in equilibrium are often
summarised by Le Chatelier’s principle, which states that:
If a system in equilibrium is altered by the change of some condition, chemical

reaction occurs to shift the equilibrium composition in a way that attempts to
reduce that change of condition.
This principle explains the effects that will be encountered in this experiment.
The application of Le Chatelier’s principle will be studied in the following

equilibria:
Part A. The solubility equilibrium of Ca(OH)2
Part B Equilibrium involving an acid–base indicator, bromothymol blue
Part C The equilibrium of Ni2+ and NH3 with Ni(NH3)62+
Part D The equilibrium of Co2+ and Cl- with CoCI42-

...........
63 CH E1503/1
AIM
The aim of this experiment is to study Le Chatelier’s principle using different

chemical equilibria.
Procedure
Work individually.
To avoid overcrowding, you can start with any part of the procedure.
Caution:
•• Take care when handling the solutions used in this experiment.
•• Do not use your finger as a stopper when mixing any of the solutions.
•• Wash your hands before you leave the lab.
•• Wash all apparatus immediately after use.
•• Solutions of ammonia, hydrochloric acid and NaOH (supplied in small
bottles) can cause chemical burns as well as ruin your clothing.
•• If you spill any solution, wash the contaminated area thoroughly and
report the incident immediately to the demonstrator.
Part A: The solubility equilibrium of Ca(OH)2
(1) Using a 10 mL measuring cylinder, pour 5 mL of 6 M NaOH into a thick

test tube.
(2) Rinse the measuring cylinder. Then add 5 mL of 1 M Ca(NO3)2 to the

same test tube.
(3) Stir the mixture with a stirring rod. A white precipitate should be present.
(4) Use the filter paper and funnel provided to filter the mixture into another
test tube. The filtration is slow, so start Part B while you wait.
(5) Wash the precipitate with 5 mL distilled water.
(6) Remove the precipitate with a metal spatula. Suspend this solid in 10 mL
of distilled water in a third thick test tube.
(7) Add 2 mL of 6 M HCl and stir the contents of the test tube. Record your
observation.
(8) Add 5 mL of 6M NaOH. Record your observation.
Part B. The equilibrium involving an acid–base indicator, bromothymol blue
(1) Mark each of two small beakers with an identification letter (A for acid
and B for base).
(2) Add 10 mL of distilled water and 4 drops of 6 M HCl to the beaker marked
A. Swirl to mix the contents.
...........
64
E XPER I M EN T 2: Pr o p e r ti e s o f s y s te ms i n c h e m i c a l e q u i li b r iu m – l e ch ate li e r ’s p r i n c i p l e
(3) Add 10 mL of distilled water and 4 drops of 6 M NaOH to the beaker

marked B. Swirl to mix the contents.
(4) Add 1 mL of distilled water to a clean test tube. Then add 4 drops of the
indicator solution, and record the colour of the solution.
(5) Add 2 drops of the dilute acid solution (A) to the solution from step 4.
Shake the test tube gently and record the colour of the resulting solution.
(6) Now add 4 drops of the dilute base solution (B) to the solution from step 5.
Shake the test tube gently and record the colour of the resulting solution.
(7) Add 8 more drops of the dilute acid solution (A) to the solution from step
6. Shake the test tube gently and record the colour of the solution.
(8) Discard the solutions by pouring them down the sink, and flush with
water.
Note: Typical indicators are aqueous solutions of weak acids that can be
represented as Hln(aq). The equilibrium of bromothymol blue in water may
thus be written as:
Hln(aq) + H2O(1) « H3O+(aq) + In-(aq)
Part C: The equilibrium of Ni2+ and NH3 with Ni(NH3)62+
(1) Work under the fume hood.
(2) Add 3 mL of 0.1 M Ni(NO3)2 to a clean test tube. Record the colour.
(3) Add 6 M NH3 a drop at a time until the colour changes and intensifies.
Record the colour.
(4) Add 6 M HCl a drop at a time until the colour changes again. Record the
colour.
Part D: The equilibrium of Co2+ and Cl- with CoCl42-
(1) Add 10 drops of 0.1 M Co(NO3)2 to a clean test tube. Record the colour.
(2) Add 20 drops of concentrated HCl (do not use the 6 M HCl). Mix by
shaking the test tube gently. Record the colour.
(3) Add 10 drops of distilled water. Shake the test tube gently. Record the
colour.
(4) Place the test tube in a beaker of boiling water (ask the demonstrator for
help). Wait three minutes. Record the colour.
(5) Cool the test tube in a beaker of cold water. Record the colour.
...........
65 CH E1503/1
PRE–LAB SHEET
the demonstrator.
experiment.
(2) Consider the hypothetical reaction which is at equilibrium:
A(aq) + B(s) ⇆ C(aq) + D(aq) ∆H<0
Indicate whether the concentration of the reactant A, [A], will increase, de-
crease or remain unchanged under the following changes effected upon the
equilibrium.
Change [A] Increase/Decrease/Unchanged
(1) A catalyst is added.
(2) Some C is removed from the

system.
(3) Some D is added to the system.
(4) The system is cooled.
(5) Some B is added to the system.
...........
66
Partner’s name and student NO.: .......................................................................
Observations and questions
PART A: The solubility equilibrium of Ca(OH)2
(1) Write the equilibrium equation for the partial dissolution of Ca(OH)2 in
water:
(2) Enter your observations in the table below:
Step No. Observation
Step 2: Formation of precipitate
Step 7: Addition of excess HCl
Step 8: Addition of excess NaOH
(3) Write an (equilibrium) equation for each step in the table above which
explains the observations made.
Step No. (Equilibrium) Equation
Step 2: Formation of precipitate
Step 7: Addition of excess HCl
Step 8: Addition of excess NaOH
...........
67 CH E1503/1
PART B: The equilibrium involving an acid–base indicator, bromothymol blue
Step 4: Colour of bromothymol blue

in water
Step 5: Colour after addition of dilute

HCl

NaOH
Step 7: Colour after further addition

of dilute HCl
(2) Refer to the equilibrium equation given under the procedure. Based on
your observations in 1 above, state the colour of HIn(aq) and that of In-(aq).
Colour of HIn(aq)
Colour of In-(aq)
PART C: The equilibrium of Ni2+ and Ni(NH3) with Ni(NH3)62+
Step 2: Colour of Ni(NO3)2

NH3
Step 4: Colour after addition of di-

lute HCl
(2) When NH3 is added to an aqueous solution containing Ni2+, the complex
ion Ni(NH3)62+ forms:
Ni2+(aq) + 6NH3(aq) ⇆ Ni(NH3)62+(aq)
Based on your observations in 1 above, state the colour of Ni(NH3)62+(aq).
Colour of Ni(NH3)62+(aq)
...........
68
(3) Given that NH3(aq) + H+(aq) “ NH4+(aq), explain your observations using Le
Chatelier’s principle:
PART D: The equilibrium of Co2+ and Cl- with CoCl42-
Step 2: Colour of aq Co(NO3)2

solution
Step 3: Colour after addition of conc.

HCl
Step 4: Colour after addition of H2O
Step 5: Colour after heating
Step 6: Colour after cooling
(2) Refer to the equilibrium equation given under the procedure. Based on
your observations under 1 above, state the colour of Co2+(aq) and that of
CoCl42-(aq), and state whether the formation of CoCl42-(aq) is endothermic
or exothermic.
Colour of Co2+(aq)
Colour of CoCl42-(aq)
Formation of CoCl42-(aq) is: endothermic/exothermic (circle one)
...........
69 CH E1503/1
O R G AN I C CH E M IS T RY PR AC T I C AL :
...........
70
ORGANIC CHEMISTRY PRAC TICAL
...........
71 CH E1503/1
EXPERIMENT
11 1
Ester formation: the synthesis of

11
acetylsalicylic acid (aspirin)
Introduction
Carboxylic acid reacts with alcohol in the presence of an acid catalyst to

form an ester. For example
H
RCOOH + R1OH ROOR1 + H2O
When a carboxylic acid reacts with an alcohol or a phenol, the major organic
products are an ester and water as the condensate. The esterification reac-
tion is slow, and equilibrium between the products and reactants is reached
during the reaction.
Another method for ester formation is the reaction of a carboxylic acid de-
rivative, such as an acid chloride or an acid anhydride, with an alcohol. Such
reactions are rapid and essentially irreversible, particularly when catalysed
by a strong acid.
Salicylic acid, or o-hydroxybenzoic acid, reacts with acetic anhydride in the

presence of concentrated sulphuric acid to produce acetylsalicylic acid, or
aspirin, according to the following reaction scheme:
The salicylic acid molecule contains both the phenol and the carboxylic acid
functional group. Therefore, it can form esters by acting as a phenol in a re-
action with a carboxylic acid or acting as a carboxylic acid upon treatment
with an alcohol.
...........
72
E XPER I M EN T 1: E s te r f o r m at i o n: t h e s y nt h e sis o f a ce t y ls a li c y li c a ci d (asp i r i n)
Acetylsalicylic acid, or aspirin, is formed by the reaction of salicylic acid

with the more reactive acetic anhydride in a rapid, irreversible reaction. The
excess acetic anhydride is then decomposed with water to form acetic acid.
Acetylsalicylic acid precipitates from the water solution, since it has limited
solubility in water (0.25 g/100 mL) and can be isolated by filtration of the solid.
In the experiment, the percentage yield of the product must be determined.

The percentage yield of the product is given by the following equation:
The actual yield of the product is the mass of pure aspirin isolated in the
experiment after the recrystallisation process.
To determine the theoretical yield, it is necessary to balance the chemical

reaction and then determine the limiting reactant. To determine the limiting
reagent, calculate the number of moles of aspirin that can be produced from
the starting amounts of each reactant. The moles of aspirin produced from
the limiting reactant are converted to the mass of aspirin. The mass of aspirin
obtained from theory is called the theoretical yield.
AIM
The aim of this experiment is to synthesise aspirin from salicylic acid and acetic
anhydride, purify it through recrystallisation and determine its melting point.
Experimental procedure
Place approximately 2 g of salicylic acid in a clean, dry 125 mL Erlenmeyer

flask. The exact mass of salicylic acid must be recorded. In a fume hood,
carefully add acetic anhydride (4 mL, 4.32 g) in such a way as to wash down
any material adhering to the sides of the mouth of the flask. Add 5 drops of
concentrated sulphuric acid to the reaction mixture in the flask. Heat the
reaction flask for 5 minutes in a large beaker of water heated to 85 to 90 oC.
Remove the flask from the water bath and slowly add 10 mL of iced distilled
water into the flask to decompose the excess acetic anhydride. The excess
acetic anhydride decomposes vigorously, causing the contents of the flask
to come to the boil. Caution: hot acid vapours are produced.
Cool the flask in an ice water bath for about 5 minutes. Once crystals form,
add 20 mL of distilled water and place the flask in an ice water bath until
crystallisation is complete.
The crystallisation process can be accelerated by scratching the wall of the

flask at the surface of the solution with a glass rod. If the solid in the flask
forms lumps, break up the lumps with the glass rod.
...........
73 CH E1503/1
Collect the product by filtration using a Buckner funnel and filter paper. Wash
the solid aspirin with 10 mL of cold water and allow the product to air dry.
Record the mass of the crude product.
Purify the product by recrystallisation from toluene and record the melting
point of the pure product.
Recrystallisation
When a crystalline solid is prepared in a typical laboratory experiment, the
solid is normally contaminated with some impurities. The purification of solids
is accomplished by recrystallisation from an appropriate solvent. The recrystal-
lisation procedure consists of the following steps:
•• Select a suitable solvent. The substance should be very soluble in a solvent at
high temperature, and only slightly or sparingly soluble at room temperature.
•• Heat the solvent to its boiling point.
•• Dissolve the substance in the minimum amount of the hot solvent.
•• Filter the hot solution by means of a hot filtration process to remove insoluble
impurities, if any are present.
•• Allow the hot solution to slowly cool to room temperature until crystallisation
is complete.
•• If crystals do not form, the crystallisation process can be accelerated by
scratching the wall of the flask at the surface of the solution with a glass rod.
•• Filter the cold mixture by suction and rinse the crystals with the smallest
amount possible of cold solvent.
•• Dry the crystals.
Recrystallisation of acetylsalicylic acid (aspirin) from toluene

•• In a fume hood, heat 20 mL of toluene to boiling in a beaker on a hotplate.
•• Transfer the crude acetylsalicylic acid to an Erlenmeyer flask and add 10
mL of hot toluene.
•• Heat the mixture to boiling, stirring all the while.
•• Add small amounts of hot toluene to dissolve the product while it is heating.
•• Once all the acetylsalicylic acid has dissolved, cover the mouth of the flask
with a watch glass. If impurities are observed, filter the hot solution by means
of a hot filtration process to remove the insoluble impurities.
•• Allow the reaction mixture to stand at room temperature until crystallisation
of the pure product is complete.
•• Filter the crystals by suction using a Buchner funnel. Wash the crystals with
5 mL of cold toluene.
•• Carefully remove the filter paper and the pure aspirin product from the
funnel, and dry it in an oven at 95 oC for 20 minutes.
•• Record the mass of the dry pure products.
Determine the melting point of the pure aspirin product, and record the melt-
ing point as a temperature range.
...........
74
ORGANIC CHEMISTRY SPECIALS – EXPERIMENT 1
Partner’s name and student No.: ........................................................................
Mass of salicylic acid used in

experiment
Molecular mass of salicylic acid
Moles of salicylic acid
Moles of aspirin produced from

salicylic acid
Mass of acetic anhydride used in

experiment
Molecular mass of acetic anhydride
Moles of acetic anhydride
Moles of aspirin produced from

acetic anhydride
Name of the limiting reagent
Molecular mass of aspirin
Theoretical mass of aspirin
Mass of crude aspirin
Actual mass of pure aspirin, after

recrystallisation
Percentage yield of pure aspirin
Melting point of aspirin
...........
75 CH E1503/1
Appearance of pure aspirin
Questions
(1) Describe in detail a mechanism for the acid catalysed esterification reac-
tion between salicylic acid and acetic anhydride.
(2) Why is concentrated H2SO4 used as the catalyst in esterification reactions?
Could dilute H2SO4 be used as a catalyst for the esterification reaction?
Give reasons for your answer.
(3) Explain why diethyl ether is not suitable as a solvent for recrystallisation.
(4) Explain why ethyl acetate should not be used as a solvent for the recrys-
tallisation of alcohols, especially in the present of traces of acid.
...........
76
(5) Why are boiling chips or bumping granules used when boiling liquids?
(6) Provide a definition for the melting point of a solid.
(7) Pure organic compounds have sharp melting points. Explain how impur-
ties influence the melting point of a solid.
FINAL MARK:
...........
77 CH E1503/1

CHE1503-001 2016 4 B PDF

Uploaded by

Copyright:

Available Formats

CHE1503-001 2016 4 B PDF

Uploaded by

Document Information

Original Title

Copyright

Available Formats

Share this document

Share or Embed Document

Sharing Options

Did you find this document useful?

Is this content inappropriate?

Copyright:

Available Formats

CHE1503-001 2016 4 B PDF

Uploaded by

Copyright:

Available Formats

DEPARTMENT OF CHEMISTRY

Laboratory Manual for

UNIVERSITY OF SOUTH AFRICA,

All rights reserved

Printed and published by the

LABORATORY SAFETY RULESix

2 INORGANIC CHEMISTRY PRACTICALS 39

3 PHYSICAL CHEMISTRY PRACTICALS 55

4 ORGANIC CHEMISTRY PRACTICAL 71

This is the laboratory manual for CHE1503.

Purpose of the module

How to use the laboratory manual

CHE1503 PRACTICAL SCHEDULE

EXPERIMENT OR ACTIVITY NUMBER TITLE

Day 1 Welcome address Laboratory aspects

DAY 2 Pre-lab talk Quantitative analysis using titrimetry

DAY 3 Pre-lab talk Redox titrations

DAY 4 Pre-lab talk Determination of the composition of

DAY 5 CHE1502 discussion class Discussion class and submission of out-

[NB: Specials refers to Organic, Physical, Inorganic Chemistry related experi-

Group # Monday Tuesday Wednesday Thursday Friday

4 Organic Inorganic Physical Lecture Report

5 Inorganic Physical Organic Lecture Report

6 Physical Organic Inorganic Lecture Report

Laboratory safety rules

Crucible tongs Ring support

Bunsen burner Buret clamp Wire gauze

Test tube holder

Beaker Erienmeyer flask Florence flask

Wide mouth bottle Wash bottle

Buret Graduated Volumetric Pasteur Medicine Thistle

Test tube rack

3. Collection of solutions to be used in the experiment

NEVER POUR EXCESS SOLUTION BACK INTO THE STOCK BOTTLE.

4. Filling the burette with aqueous solution, e.g. dilute (0.1 M)

5. Transfer of aqueous solution, e.G. Potassium hydrogen phthalate

(c) Pipette 25 mL of aqueous potassium hydrogen phthalate solution into a

(a) Titration technique

(2) Rinse down the sides of the conical flask with

A rough titration is normally performed as a time-saving procedure if sufficient

(1) Add 1 or 2 drops of phenolphthalein indicator solution to the aqueous

(c) Accurate titration

Standardisation of sodium hydroxide

stock solution with potassium hydrogen

KH(C8H4O4) + NaOH → NaK(C8H4O4) + H2O

Reagents: A.R. potassium hydrogen phthalate

(b) Weigh by difference the potassium hydrogen phthalate, as supplied in a

(f) Pipette a 25 mL aliquot of potassium hydrogen phthalate into each of

(g) Add 4 to 6 drops of phenolphthalein solution to the flask, carry out a

Note: Save the NaOH stock solution for Experiment 2.

Surname: …………………………. First names: …………………...........…....……

Student No.: ……………………….. Group No.: …………………...........…...……..

Title of experiment: …………………………………………………………………………

Apparatus required Chemicals required

(2) Answer the following questions.

(b) What is a standard solution?

(4) What is the molarity of a solution made by dissolving 5.25 g of potassium

(5) If 16.41 mL of aqueous NaOH is required to neutralise 20 mL of potas-

(a) Write the reaction equation for the titration.

LABORATORY SAFETY RULESix

4. Filling the burette with aqueous solution, e.g. dilute (0.1 M)

5. Transfer of aqueous solution, e.G. Potassium hydrogen phthalate

(c) Pipette 25 mL of aqueous potassium hydrogen phthalate solution into a

(2) Rinse down the sides of the conical flask with

(b) Weigh by difference the potassium hydrogen phthalate, as supplied in a

(f) Pipette a 25 mL aliquot of potassium hydrogen phthalate into each of

(g) Add 4 to 6 drops of phenolphthalein solution to the flask, carry out a

(4) What is the molarity of a solution made by dissolving 5.25 g of potassium

(5) If 16.41 mL of aqueous NaOH is required to neutralise 20 mL of potas-

(b) Calculate the number of moles of KHC8H4O4 used in the titration.

(a) Pipette 25 mL of your unknown vinegar solution into a 250 mL volumetric

(b) What is the concentration of acetic acid in g per 100 mL of vinegar?

(c) What, therefore, is the weight by volume percentage (w/v %) of

(b) Calculate the number of moles of acetic acid in the 25 mL of diluted

(f) What, therefore, is the weight by volume percentage (w/v %) of acetic

(b) Following the procedure given in Experiment 1, weigh by difference the