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CAPE CHEMISTRY

UNIT I
LAB MANUAL
Montego Bay Community College
Pre-University Sciences

Name:

Lab Section:

Lab Day: Lab Time:

Lab Lecturer:
Chemistry @ MBCC Pre-University Science Year 1

Table of Contents
General Safety Rules....................................................................................................................... 3
Working in the Laboratory.............................................................................................................. 5
The Laboratory Book ...................................................................................................................... 8
Skills Assessed ................................................................................................................................ 9
Acknowledgements ....................................................................................................................... 11
MODULE 1: FUNDAMENTALS IN CHEMISTRY .................................................................. 12
Experiment 1: Titration of Sodium Hydroxide with Sulphuric Acid ........................................... 12
Experiment 2: Standardisation of Sulphuric Acid with Sodium Carbonate ................................. 14
Experiment 3: Standardisation of Hydrochloric Acid with Borax................................................ 16
Experiment 4: Structure Bonding and Properties ......................................................................... 19
Experiment 5: Standardization of Potassium Permanganate with Ferrous Salts .......................... 23
Experiment 6: Standardization of Potassium Permanganate with Sodium Oxalate ..................... 25
Experiment 7: Testing for Oxidizing and Reducing Agents ......................................................... 27
Experiment 8: Finding the percentage of Fe2+ in Fe(NH4)2(SO4)2·xH2O and the value of x....... 29
Experiment 9: Displacement Reactions of Metals ........................................................................ 32
Experiment 10: The Principles of Iodine/Thiosulphate Titrations ............................................... 33
Experiment 11: Determination of the Heat of Neutralisation of HCl and NaOH ......................... 35
Experiment 12: Molar Enthalpy Change for the Displacement of Cu2+ by Zn ............................ 37
Experiment 13: Heat of Hydration of Copper (II) Sulphate (Approximate Method) ................... 40
Experiment 14: Planning and Designing I .................................................................................... 41
MODULE 2: KINETICS AND EQUILIBRIA............................................................................. 42
Experiment 16: Investigation of the Order of the Reaction of Iodine with Acetone .................... 42
Experiment 17: Principles of Chemical Equilibria I ..................................................................... 48
Experiment 18: Principles of Chemical Equilibria II ................................................................... 50
Experiment 20: Planning and Designing II ................................................................................... 54
Experiment 21: Planning and Designing III ................................................................................. 56
MODULE 3: CHEMISTRY OF THE ELEMENTS .................................................................... 57
Experiment 23: Flame Tests ......................................................................................................... 57
Experiment 24: Qualitative Analysis I – Test for Cations ............................................................ 58
Experiment 25: Qualitative Analysis II – Tests for Anions .......................................................... 61
Experiment 26: Qualitative Analysis III – Identification of Unknown Compounds .................... 64
Experiment 27: Planning and Designing IV ................................................................................. 69
WORKSHEETS ............................................................................................................................ 70
Worksheet 1: Molarity .............................................................................................................. 70
Worksheet 2: Titration Calculations ......................................................................................... 72
Worksheet 3: Redox Reactions ................................................................................................. 74
Worksheet 4: Redox Reactions II ............................................................................................. 75
Worksheet 5: Qualitative Identification of Compounds ........................................................... 77
Worksheet 6: Transition Metals ................................................................................................ 78
Appendix ....................................................................................................................................... 79

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Chemistry @ MBCC Pre-University Science Year 1

GENERAL SAFETY RULES


1. Safety glasses are to be worn at all times in the laboratory. There is always a possibility of
injury to the eyes when working with corrosive chemicals which may splatter, and when
working with apparatus under reduced pressure.
2. Never place your eyes over the opening of any chemical container. Do not point test tubes,
especially when being heated, at your neighbour.
3. If a chemical should get into your eye, immediately go to the eye wash area, hold head over
the eye wash station and flush eyes with liberal quantities of water. If other areas are
affected, wash with plenty of water as well and deactivate any possible residual chemical by
neutralization or other chemical means. Report the injury immediately to the lecturer or
lab technician!!
4. Exercise care in handling all reagents especially those known to be corrosive, e.g. nitric acid,
concentrated sulphuric acid, etc. Do not allow chemicals to touch skin.
5. Work in the fume hood when handling chemicals with toxic or obnoxious odours.
6. Clean up any spilled chemicals at once.
7. Leave balances clean.
8. Before heating a liquid to its boiling point always add a boiling chip. This applies to
reactions under reflux, distillation and recrystallisation.
9. DO NOT smoke, eat or drink in the laboratory.
10. No student may work in the laboratory unless a lecturer or lab technician is present.

Handling of Apparatus
1. Never apply any undue pressure or strain to any piece of glassware, e.g., when assembling
quick fit apparatus.
2. Never use cracked glassware as damaged glassware may collapse when heated.
3. Clean glassware as soon as possible after use, when most residues can be removed by
washing with detergent and water or with a common organic solvent like acetone.
4. Quick fit apparatus should be separated and washed immediately after use or the round glass
joints may tend to stick together and be very difficult to separate later on.

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Chemistry @ MBCC Pre-University Science Year 1

Fire Precautions
1. You should regard all organic liquids as flammable. Organic liquids must always be heated
carefully, using a water bath, a hot plate or a sand bath unless instructed otherwise.
2. Organic solvents should always be kept in closed containers and never in open beakers.
Containers containing organic solvent should be kept away from open flames.
3. Never pour flammable liquids for e.g. organic solvents such as acetone, ethanol or methanol
from one container into the other unless all flames are first extinguished.
4. Avoid using flames in the laboratory whenever possible. If flames have to be used you may
light a Bunsen burner after first after checking that your neighbours are not using flammable
solvents. Remember to extinguish the flame as soon as it is no longer required.
5. If a fire it is essential that you remain calm. Minor fires which may occur in beakers or
flasks can be usually be put out by covering the vessel with wire gauze in order to exclude
air.
Report any fires immediately to the lecturer or lab technician even after they have been
extinguished.
6. Familiarize yourself with the location and the operation of the nearest fire extinguisher.
7. Never heat a closed apparatus assembly even if it includes a condenser in the system. The
increase in pressure due to heating may cause the assembly to blow up or explode. If a flame
is being used, any liquid present in the system may be ignited.
8. All hair should be pinned back or tied back during laboratory activities. Hair is extremely
flammable especially when it contains lots of chemicals. Long synthetic hair is especially
flammable.

ALL ACCIDENTS, HOWEVER MINOR SHOULD BE REPORTED TO THE


LECTURER OR LABORTORY TECHNICIAN

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Chemistry @ MBCC Pre-University Science Year 1

WORKING IN THE LABORATORY


1. To ensure that the laboratory session is used for effective practical work, each student must
be prepared before coming to the lab session. Preparation for lab includes: a) reading through
the details of each experiment, b) being aware of all safety precautions and c) answering all
prelab questions. This will ensure in order to get a full understanding of what is expected and
what you are going to do.
2. Work carefully and steadily. Never rush, since this invariably produces errors and injuries.
3. Plan your work so that you can be flexible in your approach.
4. Leave supply chemicals and general equipment in their proper positions and in good order
for the next user.
5. DO NOT remove supply chemicals from the front of the room and carry them to your work
bench as this inconveniences other students and clutters your work area.
6. Clean up equipment as soon as you are finished working with it
7. Keep your work area clean and dry. Clean up any spillage immediately when they occur.
Provide yourself with a piece of cotton rag for this purpose.

Use of apparatus
A. Bunsen burner

The flame of a Bunsen burner can be adjusted by regulating the air intake. This will cause a
change from relatively cool luminous flame to a hot non-luminous flame with blue cone. The
hottest part of the flame is just above the top of the cone. Glassware should never be heated
directly, but gently at first to reduce the risk of breakage. The rubber tubing connections to
Bunsen burners should be checked frequently and replaced as soon as they show signs of
deteriorating. If this is not done, they will leak and the escaping gas will ignite (C06J manual,
2008-2009).

B. Balances

All balances must be carefully treated. In the laboratory, you will see two different balances. The
balances in the laboratory are for use in the preparative experiments as well as for rough initial
weighings for quantitative analysis. At no time must materials be weighed out directly on the
pans or on filter paper, and any material accidentally spilled on them must be wiped off

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Chemistry @ MBCC Pre-University Science Year 1

immediately. The balances in the room adjacent to B21 are analytical balances and give accurate
reading to the nearest ± 0.0001 and must be handled with care.
For the analytical balances;
• Keep level and on a firm foundation.
• When not in use, keep clean and in good order with the beam in the rest position
• Hot objects should never be weighed on it.
• When weighing, first set to zero.
• The object to be weighed should be placed in the centre of the pan.
• Use a suitable container (weighing bottle) for weighing to ensure protection from
chemicals.
• Never adjust or remove any part of the balance.
• If adjustment is required, call the lab technician.

C. Measuring cylinder
A measuring cylinder is used for limited accuracy of volume measurements of cold liquids. The
volume of liquid is obtained by observing the level of the bottom meniscus with the eye at the
same level and reading the calibration at that point.

D. Pipette
Transfer pipettes are designed to deliver accurately specified volumes of cold liquids under
standard conditions.
These conditions are as follows:

• Using the pipette filler rinse the pipette twice with the solution to be measured.
• Suck up the solution to above the mark using a pipette filler and NOT your mouth
• Let the solution run out slowly with the tip touching the neck of the flask or bottle until
the bottom of the meniscus just touches the mark with the pipette held vertically.
• Let the pipette discharge freely in a vertical position with the tip touching the inner
surface of the flask.
• When the meniscus stops moving, allow 15secs for drainage, with the pipette vertical and
its tip still touching the inside of the flask.

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Chemistry @ MBCC Pre-University Science Year 1

• Remove the pipette without dragging it against the wall of the flask.
• Never blow the liquid out of the pipette.

E. Burette
Burettes are designed to deliver accurately defined volumes of liquids. Before a burette is used,
its tap should be lightly greased. Solutions of caustic soda tend to cause burette taps to stick, and
if used, the burette must be washed immediately afterwards. In using the burette, it should first
be washed with distilled water and then with two 5ml portions of the solution being used. Any
excess droplets on the tip of the burette should be removed by wiping with paper towel. The
burette reading is taken at the level of the bottom of the meniscus- a black and white card held
behind the burette is sometimes useful in helping to see it distinctly.

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Chemistry @ MBCC Pre-University Science Year 1

THE LABORATORY BOOK


A good laboratory notebook and proper record-keeping is fundamental to good science. The
purpose of a lab book is to record what you do, as you do it and record all observations as you
perform the experiments.

General Guidelines for Laboratory Report


1. Lab reports should be written in ink. Labs written in pencil will not be accepted.
2. If using a book, leave at least two pages at the start for your table of contents. It is
recommended that you number the pages of your lab book and fill in your table of contents
as you go along.
3. DO NOT use whiteout in lab books. Any mistakes should be neatly crossed out, by drawing
a single line through it. Make the correct entry above or beside the crossed out mistake.
4. DO NOT remove an original page from the lab book. If the entire page is incorrect, draw a
single diagonal line through the page to indicate an omitted page.
5. Record all data and results (with units) directly into your notebook. DO NOT record data on
scrap paper, your hand, etc., to be transferred later.
6. If you need to add a graph to a book, paste your graph neatly on its own page. Do not fold
graph paper in book. Graphs should have a title, properly labelled axes and an appropriate
scale.
7. Each experiment or lab report should begin on a new page.
8. Write the title of the experiment, date, and your name at the top of each page.
9. NEVER skip a space for later additions. Complete labs before moving on to the next lab.
10. Be neat and thorough! Someone should be able to pick up your notebook twenty years from
now and be able to repeat your experiments. Record all procedures carried out and
observations made during experimental work including all modifications made to the lab.
Methods should be recorded in your own words using continuous prose.
11. For calculations, show the formula and a sample calculation. For multiple calculations of the
same type, use a table to report your results.
12. Summarize the key results and provide a conclusion. The conclusion should be a summary of
how things turned out and will refer to objective or aim.

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Chemistry @ MBCC Pre-University Science Year 1

SKILLS ASSESSED
Planning and Designing
1. Statement of hypothesis, clearly stated (based on the problem statement)
2. Aim clearly stated (relevant to the hypothesis)
3. Apparatus and Materials (relevant to the experiment)
4. Method/Procedure
- Steps to be followed in appropriate sequence. State how the apparatus and materials
will be used. The procedure must be written in logical sequence using appropriate
language (instructional)
5. Precautions to be taken
6. Treatment of variables
- Controlled variables
- Manipulated variables
- Dependent variables
7. Treatment of Data
- Type of data to be collected
- How data will be treated and possible calculations
8. Expected results and treatment (predict results)
- Prediction of observation that should be made based on the hypothesis that is being
tested.
- A statement of how these results will support the hypothesis must be written.
9. Limitations, source of error and any assumptions
- These comprise factors that could affect the results.

Analysis and Interpretation


1. Background Knowledge: This includes the theory on which the investigation is based. This
will be used in interpreting the observations or results.
2. Explanation: Background knowledge is used to fully explain the observation.
3. Conclusion/ Inference: This must be linked to the aim and hypothesis. The control (if
included) should be used in arriving at the inference or conclusion. Where appropriate, patterns
or relationships should be clearly stated.

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Chemistry @ MBCC Pre-University Science Year 1

4. Limitations and Assumptions: Limitations must be discussed. These are uncontrolled variables
and sources of error which may have affected the results obtained. Assumptions must be stated.

Measurement and Manipulation (M/M)


1. Assessment is based on the logical and correct use of each chemical apparatus used in the
experiment.
2. A written presentation of data recorded should show error associated with each apparatus for
e.g. if a 25 cm3 pipette has an error of ± 0.05 then the reported value for let’s say a titration
should be (25 ± 0.05) cm3.

Observation Recording and Reporting (ORR)

Assessment of ORR labs often involves the use of a written observations i.e. events that happen
during the experiment that are experienced through the senses. The best and easiest way to
represent information of this kind is to tabulate in the format shown below.
Test Observation Inference

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Chemistry @ MBCC Pre-University Science Year 1

ACKNOWLEDGEMENTS
This lab Manual is dedicated in the memory of Avian Miller

This laboratory manual is the compilation of activities from different resources. The following
resources must be acknowledged:
• UWI C06J Manual
• Chemistry in Context Laboratory Manual by Hill and Holman
• Nigel Saunders online (with permission obtained)
• Assignments in Practical Chemistry by T.E Rogers and B.C. Williams (1972)
• Avian Miller (MBCC lab manual)
• AQA (www.AQA.org.uk)
• OCR (www.ocr.org.uk)

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Chemistry @ MBCC Pre-University Science Year 1

MODULE 1: FUNDAMENTALS IN CHEMISTRY

Experiment 1: Titration of Sodium Hydroxide with Sulphuric Acid

Prelab Exercise
1. Suppose you prepare 500 ml of a solution of a 0.10M solution of some salt and then spill
some of the solution after preparing it. What happens to the concentration of the solution left
in the container?
2. A certain volume of a 0.50M solution contains 4.5g of a salt. What mass of the salt is present
in the same volume of a 2.50M solution?
3. 25.0 cm3 of a 0.10 moldm-3 solution of sodium carbonate was titrated against a solution of
hydrochloric acid of unknown concentration. 27.3 cm3 of the acid was required to reach the
endpoint. What was the concentration of the acid?

Aim
In this experiment, you will determine the concentration of an aqueous solution of sulphuric acid
of unknown concentration using standard sodium hydroxide.

Apparatus and Materials


Burette (50 cm3), pipette (25 cm3), pipette filler, conical flasks (250 cm3)
Sulphuric acid solution (unknown concentration), sodium hydroxide solution (0.125 M),
phenolphthalein indicator

Procedure
1. Rinse and fill the burette with the standard sodium hydroxide solution. Record the initial
burette reading. Burette readings must be to two decimal places.
2. Rinse the pipette with some of the sulphuric acid solution and carefully transfer 25cm3 of the
acid solution to a clean conical flask.
3. Add 2 drops of the phenolphthalein indicator to the contents of the flask and swirl.
4. Run sodium hydroxide from the burette into the flask, with swirling until the solution changes
from colourless to pale pink. Record the burette reading.
5. Repeat the titrations as many times as is necessary to obtain two concordant results (i.e. titre
volumes that agree within 0.10 cm3 of each other)

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Chemistry @ MBCC Pre-University Science Year 1

Results
Table 1: Volume of sodium hydroxide required to reach the endpoint

Total Volume (cm3) 1 2 3

Final Volume
Initial Volume

Total Volume used

Average Titre Volume

Calculations and Analysis


1. Write a balanced equation for the reaction between sodium hydroxide and sulphuric acid.
2. Calculate the number of moles of sodium hydroxide in the average titre volume.
3. Use the molar ratio of acid to alkali to calculate the number of moles of sulphuric acid in the
pipetted volume.
4. Hence, calculate the molar concentration of the sulphuric acid solution.
5. Calculate the mass concentration of the sulphuric acid solution.

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Chemistry @ MBCC Pre-University Science Year 1

Experiment 2: Standardisation of Sulphuric Acid with Sodium Carbonate

Prelab Exercise
1) Give TWO safety precautions you will need to follow for this lab.
2) When using the following equipment, state TWO errors which the student can make which
contribute to inconsistent titre readings in the:
a) Pipette
b) Burette
3) What colour is screened methyl orange indicator:
a) in a base eg. sodium carbonate?
b) in an acid eg. sulphuric acid?
4) What colour is the solution at the endpoint?

Aim
The purpose of this experiment is to determine the concentration of a solution of sulphuric acid
using a standard solution of sodium carbonate.

Apparatus and Materials


Burette (50.00 cm3), pipette (25.0 cm3), pipette filler, Erlenmeyer flasks (250 cm3), filter funnel
Sulphuric acid solution (unknown concentration), sodium carbonate solution (0.1 M), screened
methyl orange indicator

Procedure
1. Rinse and fill the burette with sulphuric acid solution. Record the initial burette reading.
2. Rinse the pipette with some of the sodium carbonate solution and carefully transfer 25cm3
aliquot of sodium carbonate solution to a clean Erlenmeyer flask.
3. Add 2 drops of the screened methyl orange indicator and swirl the flask.
4. Run sulphuric acid from the burette into the flask, with swirling until the appropriate colour
change is observed. At the endpoint the indicator will change from green to pale grey. Record
the burette reading to two decimal places.
5. Repeat the titrations as many times as is necessary to obtain two concordant results (i.e. titre
volumes that agree within 0.10 cm3 of each other).

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Chemistry @ MBCC Pre-University Science Year 1

Results
Table 1: Volume of acid required to reach the endpoint

Total Volume (cm3) 1 2 3

Final Volume
Initial Volume

Total Volume used

Average Titre Volume

Calculations and Analysis


1. Write a balanced equation for the reaction between sodium carbonate and sulphuric acid.
2. Calculate the number of moles of sodium carbonate in 25 cm3 of the standard solution.
3. Using the molar ratio of acid to alkali, calculate the number of moles of sulphuric acid in the
mean volume of acid used.
4. Hence, calculate the molar concentration of the sulphuric acid solution.
5. Calculate the mass concentration of the sulphuric acid solution.

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Chemistry @ MBCC Pre-University Science Year 1

Experiment 3: Standardisation of Hydrochloric Acid with Borax

Prelab Exercise
4.04g of Borax (Na2B4O7.10H2O) was dissolved in 25.0 ml distilled water. 19.38 ml of HCl were
required to titrate this borax solution.
a) Write TWO equations that illustrate the reactions occurring in Borax/HCl titration
b) Calculate the number of moles of hydroxide ions liberated in the reaction
c) Calculate the number of moles of HCl that was required to reach the endpoint
d) Hence, calculate the HCl concentration

Introduction
Borax or sodium tetraborate decahydrate (Na2B4O7.10H2O) can be used as a primary standard
since it does not decompose under normal storage, it is readily obtained in a very pure form
(99.999% purity), it reacts with a known stoichiometry and can be weighed and used directly. In
water, the salt dissociates as shown below:
Na2B4O7.10H2O → 2Na+ + B4O72- + 10H2O
and the tetraborate anion is hydrolysed:
B4O72-+ 7H2O → 4H3BO3+ 2OH-
The liberated hydroxide ions can then be titrated with a strong acid.

Safety Notes
During this experiment you will be working with a weak base and a strong acid. You must wear
eye protection at all times. In the event that any reagent used in this investigation comes in
contact with your skin or eyes, wash the affected area immediately with lots of water and notify
your instructor.

Aim
In this experiment you will use Borax to determine the concentration of hydrochloric acid
solution

Apparatus and Materials


Burette (50 cm3), pipette (25 cm3), beakers (50 cm3 and 100 cm3), conical flasks (250 cm3),
analytical balance

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Chemistry @ MBCC Pre-University Science Year 1

Borax, hydrochloric acid solution, methyl orange indicator

Procedure
1. Weigh out 0.3 g of borax into a clean, small 50 cm3 beaker using the rough (top-loading)
balance.
2. Take this beaker containing in the borax and your workbook into the balance room. Weigh the
beaker and the borax on the analytical balance and record the weight to the nearest 0.0001g as
W1.
3. Return to your bench and gently transfer the contents of the beaker into a clean, carefully
labelled 250 cm3 conical flask. DO NOT USE A SPATULA TO TRANSFER MATERIAL.
4. Weigh the 50 cm3 beaker again on the analytical balance, after you have transferred the borax.
Record this weight as W2. The difference between the two weights gives the accurate weight
(W3) of borax that was transferred to the conical flask.
5. Repeat steps 1-4 for the remaining two conical flasks. Label conical flasks clearly.
6. Add 25 cm3 of water to the borax in each of the flasks. Warm gently if needed to ensure that
the borax completely dissolves.
7. Allow the solution to cool to room temperature. Add one drop of methyl orange to each
conical flask.
8. Rinse and fill the burette with hydrochloric acid. Record the initial reading.
9. Titrate the contents of each conical flask against hydrochloric acid solution.

Results
Table 1: Mass of Borax used in titration
Mass (g) Flask 1 Flask 2 Flask 3
Mass of beaker + borax (W1)
Mass of beaker after transfer of borax (W2)
Mass of borax used (W3)

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Chemistry @ MBCC Pre-University Science Year 1

Table 2: Volume of hydrochloric acid required to reach the endpoint


Total Volume (cm3) Flask 1 Flask 2 Flask 3

Final Volume

Initial Volume
Total Volume used

Calculations and Analysis


Table 3: Results of borax-HCl titration
Flask 1 Flask 2 Flask 3
Mass of borax (g)
Molar mass of borax (g/mol)
Number of moles of tetraborate ion (mol)
Number of moles of OH- ions released (mol)
OH-: HCl mole ratio
Number of moles of HCl to reach endpoint (mol)
Concentration of HCl (mol/dm3)
Average concentration of HCl (mol/dm3)

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Chemistry @ MBCC Pre-University Science Year 1

Experiment 4: Structure Bonding and Properties

Prelab Exercise
1. What types of intermolecular forces are found in:
a) Water, b) Iodine, c) Graphite, d) Hexane?
2. Use suitable diagrams to illustrate the structure of:
a) Water, b) Iodine, c) Graphite, d) Hexane?

Introduction
Most of the physical and chemical properties of a substance can be related to the type of
bonding present in that substance. In this practical, you will investigate the properties such as
volatility and conductivity and try to explain these properties in terms of the bonding in the
substance involved.
Substances that are ionically bonded contain positive and negative ions. Substances that
are covalently bonded contain molecules. If these molecules contain atoms of different sorts,
they may be polar due to the unequal sharing of electrons between the different atoms. The
degree of polarity in a molecule, determined by the shape of the molecule and the relative
electronegativities of the atoms in it, has a great effect on the properties of the substance.

Aim
In this experiment you will be given some compounds and asked to determine the structure and
bonding present by investigating their physical properties.

Apparatus and Materials


Beakers (100 cm3), test-tubes, carbon electrodes, ammeter, 6 V battery, crocodile clips
Powdered graphite, iodine, calcium chloride, ethanol, hexane, distilled water, silver nitrate
solution, ethyl ethanoate, 1,1,1-trichloroethane.

Procedure
#1 Miscibility of liquids
Testing the miscibility of:
a) Water and ethanol
b) Water and hexane
c) Hexane and ethanol

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Chemistry @ MBCC Pre-University Science Year 1

Explain the results in terms of the polarities of the molecules in the different liquids.

#2 Solubility of iodine in liquids


a) Place a very small crystal of iodine in a test tube.
b) Add 2 ml distilled water, stopper and shake.
c) Repeat using ethanol as the solvent and finally hexane as the solvent.
Explain the relative solubility of iodine in the three solvents in terms of the particles present in
iodine and the forces of attraction holding particles together.
Suggest a reason for the differing colours of solutions of iodine in different solvents.

#3 Solubility of graphite in liquids


a) Place a very small amount of graphite in a test tube.
b) Add 2 ml distilled water, stopper and shake.
c) Repeat using ethanol as the solvent and finally hexane as the solvent.
Explain the relative solubility of graphite in the three solvents tested.

#4 Solubility of calcium chloride in liquids


a) Place a very small crystal of calcium chloride in a test tube.
b) Add 2 ml distilled water, stopper and shake.
c) Repeat using ethanol as the solvent and finally hexane as the solvent.
d) Solutions of calcium chloride are colourless, therefore, you will need to use silver nitrate to
decide how much calcium chloride has dissolved in each liquid. First, decant approximately 1 ml
the liquid into a test tube. Next, add 1 ml of silver nitrate solution to the decanted solution and
shake.
Explain the relative solubility of calcium chloride in the three solvents by looking at the
particles present in calcium chloride and the forces of attraction holding particles together.

#5 Volatility of iodine, graphite and calcium chloride


Heat the crystal of each solid in turn in a hard-glass test tube and judge their relative volatilities.
Explain the relative volatilities in terms of the particles they contain and the forces of
attraction between them.

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Chemistry @ MBCC Pre-University Science Year 1

#6 Conductivity
For each of the aqueous solutions of the solids given, connect a pair of carbon electrodes in
series with a 6V battery and a 100 mA ammeter. Dip the electrodes in the solution each time. If
the solid does not dissolve do not perform test. Test the conductivity of each of the pure solvents.
Explain the relative conductivities of the different solutions.

#7 The colour of iodine in solution


Test the colour of iodine in ethanol, ethyl ethanoate and 1,1,1-trichloroethane.
Suggest a reason for the differing colours of solutions of iodine in different solvents.

Results
Table 1: Miscibility of three different liquids (Procedure 1)
Mixture Miscibility
Water + Ethanol
Water + Hexane
Hexane + Ethanol

Table 2: Solubility of a given material in three different liquids (Procedures 2, 3 and 4)


Solubility
Compounds Hexane Ethanol Water
Iodine
Graphite
Calcium chloride
Addition of AgNO3 to the CaCl2 decant

Table 3: Volatility of three given solids (Procedure 5)


Mixture Volatility
Iodine
Graphite
Calcium chloride

Table 4: Conductivity of three given solids (Procedure 6)


Mixture Conductivity
Iodine
Graphite
Calcium chloride

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Chemistry @ MBCC Pre-University Science Year 1

Table 5: Colour of iodine in three given solvents (Procedure 7)


Mixture Colour of solution
Ethanol
Ethyl ethanoate
1,1,1-trichloroethane

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Chemistry @ MBCC Pre-University Science Year 1

Experiment 5: Standardisation of Potassium Permanganate with Ferrous Salts

Prelab Exercise
Please read the section on Preparation of Standard Solutions (Appendix B). Be prepared to
answer questions on this topic.

Aim
In this experiment you are asked to determine the concentration of a Potassium permanganate
solution using the iron (II) salt given.

Apparatus and Materials


Beaker (50 cm3 and 250 cm3), burette (50 cm3), pipette (10 cm3), volumetric flask (250 cm3),
Erlenmeyer flasks, analytical balance, top loading balance, measuring cylinder (250 cm3)
Iron (II) sulphate, sulphuric acid solution, potassium, permanganate solution

Procedure
1. Weigh out 0.0102 moles of ferrous sulphate into a clean, small 50 cm3 beaker using the rough
(top-loading) balance.
2. Take this beaker and your workbook into the balance room. Weigh the beaker and the ferrous
salt and record the weight to the nearest 0.0001g as W1.
3. Return to your bench and gently transfer the contents of the beaker into a 250 cm3 beaker. DO
NOT USE A SPATULA TO TRANSFER THE MATERIAL.
4. Weigh the 50 cm3 again using the analytical balance (W2). The difference between the two
weights gives the accurate weight of ferrous salt in your beaker.
5. Add 28-32 cm3 of dilute sulphuric acid into the 250 cm3 beaker and stir into solution. Place a
funnel in the neck of the volumetric flask.
6. Pour the solution down the rod, into the funnel in the volumetric flask. Wash the beaker and
the rod into the funnel and then wash the funnel into the flask.
7. Fill the flask to just below the line, stopper it and shake well. Allow the stoppered flask to
stand on the bench for a minute or two, remove the stopper and make up the solution to the line
by cautious addition of water. Stopper and shake well again.
8. Pipette three 10 cm3 aliquots of the Fe2+ solution into titration flasks; add 25 cm3of dilute
sulphuric acid from a measuring cylinder into each flask.

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Chemistry @ MBCC Pre-University Science Year 1

9. Rinse burette and fill with permanganate solution. Titrate each flask with permanganate
solution to a faint pink, permanent endpoint

Results and Calculations


Table 1: Preparation of Iron (II) solution
Mass of beaker + iron (II) salt (W1) (g)
Mass of empty beaker (W2) (g)
Mass of iron (II) salt (W3) (g)
Molar mass of iron (II) salt (g/mol)
Volume of iron (II) solution prepared (cm3)
Number of moles of Iron (II) salt in the prepared volume
Molarity of Iron (II) solution (mol/dm3)

Table 2: Volume of permanganate solution required to reach endpoint

Total Volume (cm3) 1 2 3

Final Volume
Initial Volume

Total Volume used

Average Titre Volume

Calculations and Analysis


1. Write an equation for the reaction between the permanganate ion and Fe2+.
2. Calculate the number of moles of iron (II) salt in the pipetted volume.
3. Calculate the number of moles of permanganate in the average titre volume.
4. What is the molarity of permanganate solution?
5. Express the concentration of the permanganate ion in solution as gdm-3.

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Chemistry @ MBCC Pre-University Science Year 1

Experiment 6: Standardisation of Potassium Permanganate with Sodium Oxalate

Prelab Questions
1. Write the balanced half equation to show oxidation of the oxalate ion (C2O42-) to carbon
dioxide (CO2).

2. Write the balanced half equation to show reduction of the permanganate ion (MnO 4-) to the
Mn2+ ion.

3. Write the overall balanced equation for the redox reaction occurring between the oxalate and
permanganate ion

Introduction
The soluble oxalate ion reacts with permanganate in acid solution to give carbon dioxide
and water. The reaction between the oxalate ion and the permanganate ion is very slow in the
cold but is self-catalyzed by the Mn2+. Heating the system to 600 C can sufficiently increase the
rate. 600 C can be estimated as the temperature at which the flask is just too hot to hold.

Aim
To determine the concentration of potassium permanganate using pure sodium oxalate

Apparatus and Materials


Sodium oxalate salt, Sulphuric acid solution, potassium permanganate solution
Beakers (250 cm3), burette (50 cm3), pipette (25 cm3), volumetric flasks (250 cm3), conical flasks
(125cm3), analytical balance, top-loading balance, measuring cylinder

Procedure
1. Prepare 250 cm3 of about 0.05M solution sodium oxalate of accurately known concentration

2. Pipette a 25 cm3 aliquot of this solution into the conical flask.

3. Add approximately 25 cm3 of acid of dilute Sulphuric acid using a measuring cylinder.

4. Heat the solution until it is just too hot to hold but do not boil. Titrate the hot solution with
permanganate until a faint pink colour that lasts for at least 30 seconds. If necessary the
solution should be reheated before the end point is reached.

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Chemistry @ MBCC Pre-University Science Year 1

Results and calculation


Determine the concentration of the permanganate as molar concentration and mass
concentration.

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Chemistry @ MBCC Pre-University Science Year 1

Experiment 7: Testing for Oxidizing and Reducing Agents

Prelab Questions
1. Define the following terms:
a) Oxidizing agent
b) Reducing agent
2. List at least two examples of:
a) An oxidizing agent
b) A reducing agent

Aim
To investigate redox reactions and classify reagents as oxidizing or reducing agents

Apparatus and Materials


Test tubes, test tube rock, teat dropper, beaker
Potassium permanganate, Hydrogen peroxide, Potassium iodide, Iron (III) chloride
Sodium sulphite, Potassium dichromate

Procedure
1. Perform the tests in the table below and note the colour of the reactants. Also note any colour
changes as a result of the reaction.
2. In the Inference section:
i) Write balanced redox equations for the reactions that occur
ii) Account for any colour change (reactions) that occur
iii) identify the oxidizing and reducing agents

TEST OBSERVATION INFERENCE


Permanganate ions and Sulphite ions
Pour sulphite solution into a test tube to a
depth of about 2 cm. Use a teat dropper
add one or two drops of permanganate and
observe
Dichromate ions and Hydrogen peroxide
Pour hydrogen peroxide into a test tube
to a depth of 2cm. Use a teat dropper to
add one or two drops of dichromate and
observe

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Chemistry @ MBCC Pre-University Science Year 1

TEST OBSERVATION INFERENCE


Hydrogen peroxide and Iodide ions
Pour potassium iodide solution into a test
tube to a depth of 2cm. Use a teat dropper
to add a few drops of hydrogen peroxide
to the test tube and observe.
Iron (III) ions and Iodide ions
Pour ferric chloride solution into a test
tube to a depth of about 2cm. Add about
3ml of potassium iodide to the test tube
drop by drop and observe the colour change
Sulphite ions and Aqueous Iodine
Pour sodium sulphite solution in
a test tube to a depth of about
2cm. Use a teat dropper to add iodine
solution drop by drop and observe any
colour change

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Chemistry @ MBCC Pre-University Science Year 1

Experiment 8: Finding the percentage of Fe2+ in Fe(NH4)2(SO4)2·xH2O and the value of x

Prelab Exercise
Sodium carbonate exists in hydrated form, Na2CO3.xH2O, in the solid state. 3.5 g of a sodium
carbonate sample was dissolved in water and the volume made up to 250 cm3. 25.0 cm3 of this
solution was titrated against 0.1 mol dm-3 HCl and 24.5 cm3 of the acid were required. Calculate
the value of x given the equation:
Na2CO3 + 2HCl → 2NaCl + CO2 + H2O

Introduction
The manganate (VII) ion, MnO4-, is a strong oxidizing agent. It accepts electrons easily, and is
reduced to colourless manganese (II) ions according to the half equation below:
MnO4-(aq) + 8H+(aq) + 5e- → Mn2+(aq) + 4 H2O(l)
The electrons are provided by reducing agents such as iron (II) salts:
Fe2+(aq) → Fe3+(aq) + e-
Overall equation:
MnO4-(aq) + 8H+(aq) + 5Fe2+(aq) → Mn2+(aq) + 4 H2O(l) + 5Fe3+(aq)
As a result manganate (VII) is added from a burette, to a solution of reducing agent and is
decolourised immediately. As soon as the reducing agent is used up, the next drop of manganate
(VII) is not decolourised, and so the solution in the conical flask goes pale pink. The endpoint of
the titration is the first appearance of this pale pink colour. Manganate is therefore self-indicating
and no other indicator is needed. The acid used to provide the H+(aq) is dilute sulphuric acid. This
should always be used in excess or else insoluble, brown MnO 2 will form.

Aim
You are asked to determine the percentage Fe2+ and to determine the amount of water of
crystallisation in the given iron (II) salt.

Apparatus and Materials


Burette (50 cm3), pipette (25 cm3), volumetric flask (250 cm3), beakers (50 cm3 and 100 cm3),
measuring cylinder (100 cm3), conical flasks (250 cm3), top loading (rough) balance, analytical
balance
Iron (II) salt, sulphuric acid, potassium permanganate (0.02 M)

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Chemistry @ MBCC Pre-University Science Year 1

Procedure
1. Weigh accurately between 9.5g and 10.5g of the iron (II) salt to the nearest 0.0001g.
2. Dissolve the salt in about 150 cm3 of water in a beaker. Transfer the solution to the
volumetric flask.
3. Make up the solution in the volumetric flask to the 250 cm3 mark and mix thoroughly.
4. Pour the solution into a clean beaker and pipette 25 cm3 into a conical flask.
5. Using a measuring cylinder, add 25 cm3 of dilute sulphuric acid to the conical flask
containing the iron (II) solution. Titrate against 0.02M KMnO4 from the burette.
6. Repeat steps 4 and 5 until two concordant titre readings are obtained.

Results and Calculations


Table 1: Weight of iron (II) salt
Weight of beaker + iron (II) salt (W1) (g)
Weight of empty beaker (W2) (g)
Weight of iron (II) salt (W3) (g)

Table 2: Volume of permanganate solution required to titrate 25 cm3 of iron (II) salt
solution

Total Volume (cm3) 1 2 3

Final Volume

Initial Volume

Total Volume used

Average Titre Volume

Calculations and Analysis


1. Calculate the average titre of KMnO4
2. Calculate the number of moles of KMnO4 used to reach the endpoint
3. Calculate the number of moles of Fe2+ in 25 cm3 of the solution and then the number of moles
of Fe2+ in your sample.
4. Calculate the mass of Fe2+ in your sample of crystals and then the percentage by mass of Fe2+
in them.

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Chemistry @ MBCC Pre-University Science Year 1

5. Calculate the mass of anhydrous Fe(NH4)2(SO4)2 present in your original sample of crystals
and then the mass of water in those crystals.
6. What is the value of x in Fe(NH4)2(SO4)2 ·xH2O?
7. Discuss the sources of error and their importance in the experiment. Suggest ways of reducing
these errors and improving the experiment.

More Practice Questions


1. The 0.2640 g of sodium oxalate is dissolved in a flask and requires 30.74 mL of potassium
permanganate (from a buret) to titrate it and cause it to turn pink (the end point). The equation
for this reaction is:
5Na2C2O4(aq) + 2KMnO4(aq) + 8H2SO4(aq) →2MnSO4(aq) + K2SO4(aq) + 5Na2SO4(aq) + 10 CO2(g)
+ 8 H2O(l)
(a) How many moles of sodium oxalate are present in the flask?
(b) How many moles of potassium permanganate have been titrated into the flask to reach the
end point?
(c) What is the molarity of the potassium permanganate?

2. A solution contains both iron (II) and iron (III) ions. A 50.0 mL sample of the solution is
titrated with 35.0 mL of 0.00280 M KMnO4, which oxidizes Fe2+ to Fe3+. The permangante
ion is reduced to manganese (II) ion. Another 50.0 mL sample of solution is treated with zinc
metal, which reduces all the Fe3+ to Fe2+. The resulting solution is again titrated with 0.00280
M KMnO4, this time 48.0 mL is required. What are the concentrations of Fe2+ and Fe3+ in the
solution?
5Fe2+ + 8H+ + MnO4¯ → 5 Fe3+ + Mn2+ + 4 H2O

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Chemistry @ MBCC Pre-University Science Year 1

Experiment 9: Displacement Reactions of Metals

Prelab Exercise
What would you observe if an iron nail was placed in beaker containing copper nitrate solution
and left for one week? Use equations (with appropriate state symbols) to illustrate your answer.

Aim
In this experiment you will be required to determine the reactivity order for four metals - A, B, C
and D.

Apparatus and Materials


Test-tubes, test-tube rack, spatula
0.2M nitrate solutions of metals A, B, C and D
Metals A, B, C and D

Procedure
1. Add 1cm3 of nitrate solute of A to each of three clearly labeled test-tubes.
2. Add metal B to the first test-tube, metal C to the second test-tube and metal D to the third test-
tube.
3. Record your results in a suitable table. Your table should include observations and inferences.
4. Repeat steps 1-3 for the nitrate solutions of B, C and D.

Discussion and Analysis


1. List the metals in order of most reactive to least reactive.
2. How did you determine the order off reactivity of the metals?

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Chemistry @ MBCC Pre-University Science Year 1

Experiment 10: The Principles of Iodine/Thiosulphate Titrations

Introduction
Thiosulphate ions are oxidized by iodine according to the following half equation:
2S2O32-(aq) → S4O62-(aq) + 2e-
In the iodine/thiosulphate reactions, the usual procedure is to run a standard solution of
thiosulphate ions from a burette into the iodine solution, with starch present to aid the detection
of the endpoint. In the presence of iodine starch forms a deep blue colour which disappears as the
iodine is removed. It is advisable to add the starch solution when most of the iodine has been
reduced as the reaction of the starch with iodine in high concentration is less readily reversed.
The major application of iodine/thiosulphate titrations is not the direct determination of the
concentration of solutions of iodine but as a general method for the determination of the
concentration of solutions of oxidizing agents. The technique is to add a known volume of the
oxidizing agent to an excess of acidified potassium iodide solution and determine the quantity of
iodine produced, using a standard thiosulphate solution.

Aim
In this experiment, you will investigate the principles of the iodine/thiosulphate titration and
asked to determine the equation for the reaction between the Iodide and Iodate ions in acid
solution

Apparatus and Materials


Burette (50 cm3), beaker (250 cm3), measuring cylinder (100 cm3), pipette (20 cm3), conical
flasks (250 cm3)
Potassium iodate solution (3.00 g/dm3), potassium iodide solution (15g/dm3), dilute sulphuric
acid, sodium thiosulphate solution (0.10 M), starch solution

Procedure
1. Pipette 25.0cm3 of potassium iodate solution into a 250 cm3 conical flask.
2. To the same flask, use a measuring cylinder to add approximately 25 cm3 of potassium iodide
solution and approximately 10 cm3 of molar sulphuric acid. The solution should become brown
as iodine is liberated.

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Chemistry @ MBCC Pre-University Science Year 1

3. Titrate the liberated iodine with the 0.10 M sodium thiosulphate solution until the solution in
the titration flask becomes pale yellow. Add about 1 cm3 of starch solution to the pale yellow
solution. A blue colour should be observed due to the complex formed between starch and
iodine.
4. Continue titrating until the blue colour disappears. The endpoint is indicated by the sudden
removal of the bluish-black colour, leaving a colourless solution.
5. Repeat until two concordant results are obtained.

Results and Calculations


1. Write the half-equation for the reduction of iodine
2. How many moles of thiosulphate ions, S2O32-, react with one mole of iodine, I2?
3. Write the overall equation for the reaction that occurs between the thiosulphate ion and iodine.
4. How many moles of thiosulphate ions were used in the reaction?
5. How many moles of iodine were liberated by the pipetted volume of potassium iodate
solution?
6. What is the molarity of the given potassium iodate solution?
7. How many moles of iodate ions are present in the potassium iodate solution you used?
8. How many moles of iodine are formed when one mole of iodate reacts with excess iodide
ions?
9. Write a balanced equation for the reaction between iodate and iodide ions in acid solution

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Chemistry @ MBCC Pre-University Science Year 1

Experiment 11: Determination of the Heat of Neutralisation of HCl and NaOH

Aim
In this experiment you will determine the molar enthalpy change of neutralization for
hydrochloric acid with sodium hydroxide.

Apparatus and Materials


Thermometer, polystyrene cup, lid, stop-watch, beaker, pipette (25 cm3)
Hydrochloric acid (1 M), sodium hydroxide (1 M)

Procedure
1. Place a clean, dry polystyrene cup inside a glass beaker.
2. Pipette 50.0 cm3 of 1.0 M hydrochloric acid into the polystyrene cup.
3. Pipette 50.0 cm3 of the 1.0 M sodium hydroxide solution into a beaker.
4. Allow both solutions to equilibrate for 5 minutes. Record the temperature of each solution.
The average of both solutions will be T1.
5. Add the sodium hydroxide solution quickly to the polystyrene cup containing the acid, without
splashing. Record the temperature in 30 second intervals for 5 minutes.

Results
Table 1: Temperature change for enthalpy change of neutralisation of HCl with NaOH
Time (seconds) 0.0 30 60 90 120 150 180 210 240 270 300
Temperature
(oC) T1

Calculations
1. Plot the temperature (vertical axis) against time (horizontal axis).
2. Extrapolate the curve back to 30 seconds to determine the maximum temperature reached (T2)
as shown below (Figure 1).

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Chemistry @ MBCC Pre-University Science Year 1

Figure 1: Temperature vs. time graph for neutralisation reaction between HCl and NaOH

3. Calculate the temperature rise (ΔT) using your initial (T1) and final temperatures (T2).
4. Taking the density of the solution to be 1.0 g cm-3and assuming the total volume of liquid has
not changed, calculate the heat change during the reaction.
ΔH = m c ΔT
where m = mass of solution (g)
c = specific heat capacity of water = 4.18 J g–1 K–1
ΔT = rise in temperature (K)
5. Calculate the molar enthalpy change, ΔH, for the neutralization of HCl by NaOH, taking into
account the number of moles used in the reaction.

Discussion
1. The literature value for the molar enthalpy of neutralization is –57.6 kJ mol-1. What is the
difference between your answer and the correct answer? What is your percentage error?
2. Calculate the percentage apparatus error using the following information:
Thermometer ±0.1 oC
Pipette (2 readings were taken) ±0.05 cm3
3. Comment on your answer to parts 1 and 2.
4. Identify the main source error in the experiment and suggest how accuracy could be improved.

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Chemistry @ MBCC Pre-University Science Year 1

Experiment 12: Molar Enthalpy Change for the Displacement of Cu2+ by Zn

Introduction
Zinc reacts with aqueous copper (II) sulphate as shown by the following displacement reaction:
Zn(s) + Cu2+(aq) Zn2+ (aq) + Cu(s)

Aim
You are asked to determine the molar enthalpy change for the displacement of copper sulphate
solution by zinc

Apparatus and Materials


Pipette (25cm3), polystyrene cup with lid, top loading balance, beaker (250 cm3), thermometer,
stop-watch, weighing bottle
Copper (II) sulphate solution (1.0 M), zinc powder

Procedure
1. Place a clean, dry polystyrene cup inside the 250 cm 3 glass beaker.
2. Pipette 25.0 cm3 of 1.0 mol dm-3 copper sulphate solution into the polystyrene cup.
3. Weigh 6g of zinc powder in the weighing bottle on the top loading balance.
4. Put the thermometer through the hole in the lid, stir, and record the temperature, to 1 decimal
place, every half minute for 2½ minutes in the table below.
5. At precisely 3 minutes, add the zinc powder to the polystyrene cup.
6. Continue stirring the mixture carefully and record the temperature (in a similar table below)
for an additional 6 minutes until the temperature stops rising.

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Chemistry @ MBCC Pre-University Science Year 1

Results and Calculations


Table 1: Temperature change during displacement reaction between copper sulphate and
zinc

4.5
Time /minutes 0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0
not
Temperature /oC done

9.5
Time /minutes 5.0 5.5 6.0 6.5 7.0 7.5 8.0 8.5 9.0

Temperature /oC

6. Plot the temperature (vertical axis) against time (horizontal axis).


7. Extrapolate the curve back to 3.0 minutes to establish the maximum temperature rise as shown
in the example below:

Figure 1: Plot of temperature vs time

8. Calculate the enthalpy change, ΔH, for the quantities used during the reaction. (Taking the
density of the solution to be 1.0 gdm-3, the specific heat capacity to be 4.18 JK-1g-1 and assuming
the total volume of liquid has not changed.)

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Chemistry @ MBCC Pre-University Science Year 1

ΔH = m c ΔT
where m = mass of solution (g)
c = specific heat capacity of water = 4.18 J g–1 K–1
ΔT = rise in temperature (K)

9. Calculate the number of moles of copper sulphate and zinc used and deduce which one is in
excess.
10. Hence, calculate the enthalpy change for the reaction of one mole of Zn and CuSO4(aq).
(Include a sign and units in your answer.)
11. Calculate the maximum percentage error for each piece of apparatus, and then the total
overall apparatus error.
12. The accepted value for this reaction is –217 kJ mol–1. Compare your result with this value by
calculating the percentage error in your answer:
experiment al value − accepted value
% error =  100%
accepted value

Discussion
1. Compare your total apparatus error with your answer to part 8 above – is the apparatus error
enough to account for any difference between the accepted value and your experimental value?
2. List some possible reasons for any difference between your value and the accepted value
(these should not be the apparatus errors mentioned above)
3. Why do you think the temperature increases for a few readings after adding the zinc? (Hint:
the temperature does not go even higher if more zinc is used, or if the powder is finely divided).

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Chemistry @ MBCC Pre-University Science Year 1

Experiment 13: Heat of Hydration of Copper (II) Sulphate (Approximate Method)

Prelab Exercise
This experiment enables an approximate determination of the heat of hydration of copper (II)
sulphate to be made by the application of Hess’ Law of constant heat summation. The heat
change when one mole of anhydrous copper (II) sulphate is dissolved in water is first
determined. Secondly, the heat of solution of copper (II) solution pentahydrate in water is
determined.
1. State Hess’ Law of Constant Heat Summation
2. Write the equation for the reaction taking place, in such a way that they may be linked
together in an energy cycle.
3. Label the energy cycle as follows:
ΔH1 = Heat of solution of anhydrous copper (II) sulphate
ΔH2 = Heat of solution of copper (II) sulphate pentahydrate
ΔH3 = Heat of hydration of copper (II) sulphate
Write an expression for the heat of hydration of copper (II) sulphate in terms of the other two
quantities.

Aim
In this experiment, you will determine the heat of hydration for copper (II) sulphate using the
approximate method.

Apparatus and Materials


Measuring cylinder (100 cm3), thermometer, watch glass, Polystyrene cup
Distilled water, anhydrous copper (II) sulphate (10g), copper (II) sulphate pentahydrate

Procedure
1. Using a measuring cylinder, place 100 ml of distilled water in a polystyrene cup and record
the initial temperature of the water. Weigh a dry watch glass, and add to it 8.0g of anhydrous
copper (II) sulphate. Add the anhydrous copper (II) sulphate to the water in the polystyrene
cup and stir to dissolve it as quickly as possible. Record the highest temperature of the
solution. Set out the results as shown in the table below.

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Chemistry @ MBCC Pre-University Science Year 1

2. Proceed as in Part I, but use 12.5g of copper (II) sulphate pentahydrate instead of the
anhydrous salt. Set out the results as shown in the table below.

Table 1: Experimental Results


Anhydrous salt Hydrated salt
Weight of watch glass (g)
Weight of watch glass + copper sulphate (g)
Weight of copper sulphate added (g)
Initial temperature of water (0C)
Highest temperature of solution (0C)
Change in temperature (0C)

Discussion Questions
1. What is the molar heat of the solution of anhydrous copper (II) sulphate, ΔH 1?
2. What is the molar heat of the solution of copper (II) sulphate pentahydrate, ΔH2?
3. What value does this give for the heat of hydration of copper (II) sulphate, ΔH 3?
4. What assumptions have you made in calculating ΔH 1 and ΔH2?
5. What errors are there in this experiment?
6. How could these errors be minimized?

Experiment 14: Planning and Designing I

Problem Statement
A Mechanical Engineer observed that steel manufactured in India rusts easier than steel
manufactured in the USA. Based on observations, the Engineer suggests that steel made in India
has a higher iron content than that made in the USA. Plan and design an experiment to validate
or discredit this claim.

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Chemistry @ MBCC Pre-University Science Year 1

MODULE 2: KINETICS AND EQUILIBRIA

Experiment 15: Factors affecting the rate of a chemical reaction

Introduction
The rate of reaction is defined as the change in concentration of reactants or products per
unit time. It is affected by several factors such as concentration of reactants, temperature, surface
area and catalysts. According to the collision theory, effective collisions between reactant
particles result in chemical reactions. The collision theory model provides a qualitative
explanation of chemical reactions and the rates at which they occur.
In this experiment, the effect of concentration of reactants and temperature on the
reaction rate will be investigated. In the reaction being investigated, molecular iodine (I2) reacts
with starch solution to produce a characteristic dark blue colour. The rate of the reaction is
measured by the time it takes for the blue colour to appear when two solutions are mixed.
The reaction takes place in two stages and can be represented by the following ionic
equations:
1. IO3- (aq) + 3HSO3- (aq) → I- (aq) + 3SO42- (aq) + 3H+ (aq)

2. 5I- (aq) + 6H+ (aq) + IO3- (aq) → 3I2 (aq) + 3H2O (l)

In the first stage, iodate ions (IO3-) are reduced to iodide ions (I-). The iodide ions
produced react with more iodate ions to produce molecular iodine in the second stage.
To determine the effect of temperature and concentration on the rate of formation of
molecular iodine, the experiment will be conducted in two parts. In Part 1, the effect of
concentration will be investigated by varying the concentration of one of the reactants (at
constant temperature). In Part 2, the temperature is varied while keeping reactant concentrations
constant.

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Chemistry @ MBCC Pre-University Science Year 1

Aim
To investigate the effect of i) concentration and ii) temperature on the rate of reaction

Apparatus and Materials


2 Beakers (100 cm3), 2 Beakers (50 cm3), measuring cylinder (25 cm3), test tubes (4),
thermometer, stopwatch, glass rod, ice, hot plate
Solution A (containing 0.02M IO3-), Solution B (containing 0.02M HSO3- ion), starch solution
(4g/L), distilled water

Procedure
Part 1 – Effect of concentration
1. Using a measuring cylinder, transfer 10 cm3 of Solution A to a 50 cm3 beaker
2. Transfer 10 cm3 of Solution B into a second 50 cm3 beaker.
3. Pour solution A into solution B and allow the mixture to stand. Start the stopwatch
immediately as Solution A comes in contact with Solution B. Stop timing as soon as the
characteristic blue colour appears and record the elapsed time.
4. Repeat the steps above with decreasing concentrations of Solution A (Use Table 1 as a
guide). Record data as shown in Table 1 below.

Part 2 – Effect of temperature


***This part of the experiment must be conducted in pairs.
1. Prepare an ice bath in a 250 cm3 by adding ice cubes to about 20 cm3 of water. Use a
thermometer to measure and record the temperature of the ice bath.
2. Add 10 cm3 of Solution A to a test tube and 10 cm3 of Solution B into a test tube. Submerge
the test tubes into the ice bath for 5 minutes to allow them to equilibrate.
3. Pour both solutions into an empty beaker simultaneously. Start the stopwatch immediately.

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Chemistry @ MBCC Pre-University Science Year 1

4.

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Chemistry @ MBCC Pre-University Science Year 1

Experiment 16: Investigation of the Order of the Reaction of Iodine with Acetone

Prelab Exercise
1. Sketch a diagram to show how concentration varies with time for:
a) Zero order reactions
b) First order reactions
c) Second order reactions
2. Sketch a diagram to show how rate of reaction varies with concentration for:
a) Zero order reactions
b) First order reactions
c) Second order reactions

Introduction
Chemical kinetics involves the investigation of the rates at which chemical reactions occur. This
topic is of great importance in chemistry as it enables the exploration of reaction mechanisms.
Even the simplest chemical reactions may consist of a complex sequence of events. As a result,
it is customary to simplify matters by devising experiments in which the concentration of one
species only is changing. Using this method the chemist is able to obtain information about the
reaction such as the rate of the reaction and the order of the reaction.
The order of a reaction with respect to each reagent must be determined experimentally.
In order to do this, the initial concentrations of reactants are systematically varied. The iodination
of acetone is a convenient reaction to do a rate study. The aqueous iodine has a characteristic
brown colour and is readily observable, therefore change in in the concentration of aqueous
iodine can be easily monitored visually. In addition, the rate of the reaction is fast enough to
allow multiple runs, but not so fast to be difficult to measure. The chemical equation for the
reaction between iodine and acetone is shown below:

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Chemistry @ MBCC Pre-University Science Year 1

Aim
You will be required to determine the order of the reaction between iodine and acetone.

Apparatus and Materials


Burette (50 cm3), pipette (10cm3 and 25 cm3), conical flasks (250 cm3)
1.0 M Acetone dissolved in water, 0.02 M I2 in aqueous KI solution, 1.0M sulphuric acid, 0.5 M
sodium bicarbonate solution, very dilute sodium thiosulphate solution, starch indicator

Procedure
1. Each pair of students should prepare one of the combinations of solutions indicated below:
Table 1
Student Pair 1 2 3 4 5
FLASK A
Volume of I2 solution (cm3) 50.0 50.0 50.0 50.0 50.0
FLASK B
Volume of H2SO4 solution (cm3) 25.0 25.0 25.0 25.0 25.0
Volume of acetone solution (cm3) 25.0 20.0 15.0 12.5 6.25
Volume of distilled water (cm3) 0 5.0 10.0 12.5 18.75

2. Stopper the flasks and allow contents to equilibrate to room temperature.


3. Fill a burette with the dilute sodium thiosulphate solution.
4. Pipette 10cm3 of NaHCO3 into each of five, clean conical flasks. Have ready a clean 10 cm3
pipette and a stop-watch.
5. When you are ready, mix the contents of flasks A and B thoroughly. Have your partner start
the stop-watch as soon as the contents are mixed.
6. Record the temperature of your mixture.
7. After 5 minutes, quickly pipette 10.0 cm3 of the reaction mixture into one of the flasks
containing the NaHCO3 solution. Record the exact time at which the reaction mixture was added
to NaHCO3.
8. Mix the contents of the flask thoroughly and titrate its contents against the dilute sodium
thiosulphate solution. When the mixture is nearly colourless, add two or three drops of fresh
starch solution.
9. Continue to titrate until the one drop of sodium thiosulphate solution discharges the blue
starch-iodine complex colour.

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Chemistry @ MBCC Pre-University Science Year 1

10. Repeat steps 7-10 at 10, 15, 20 and 30 minutes. Record all times (exact) and titration data as
follows:
Table 2
Time (min)
Final burette reading (cm3)
Initial burette reading (cm3)
Total volume Na2S2O3 required (cm3)
Temp of mixture (0C)

Results
1. Graph 1: Plot the volumes of sodium thiosulphate needed to react with the remaining iodine
against the times at which 10 cm3 samples of the reaction mixture were added to NaHCO 3
solution.
2. Record the gradients of graph 1 obtained by the whole class as shown below:
Table 3

Student Pair # 1 2 3 4 5

Gradient (cm3 min-1)

3. Graph 2: Plot the gradients of graphs 1 against the initial volume of acetone solution added.

Analysis and Discussion


1. Write an equation for the reaction between sodium thiosulphate and iodine.
2. The reaction between the acetone and iodine is catalyzed by acid. What is the function of the
sodium bicarbonate (NaHCO3)?
3. How can the rate of the reaction be determined from Graph 1?
4. Did the iodine concentration change at a uniform rate throughout the experiment? Is the rate of
the reaction dependent on the iodine concentration?
5. What is the order with respect to iodine?
6. What is the significance of the intercept of Graph 1?
7. What must the concentration of the sodium thiosulphate have been?
8. How did the rate depend on the acetone concentration?
9. What is the order of the reaction with respect to acetone?

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Chemistry @ MBCC Pre-University Science Year 1

Experiment 17: Principles of Chemical Equilibria

Prelab Exercise
1. State Le Chatelier’s principle.
2. Using a named industrial process you have studied in class, explain how Le Chatelier’s
principle may be applied to optimize production.

Aim
In this experiment you will investigate the effect of concentration changes on equilibria

Introduction
Iron (III) ions and thiocyanate ions react in solution to produce the complex ion
thiocyanotoiron(III) according to the equation shown below:

Fe3+(aq) + SCN- Fe(SCN)2+

pale yellow colourless blood-red

The colour produced by the complex ion can indicate the position of the equilibrium.
Ammonium chloride removes Fe3+ ions from the equilibrium by forming complex ions such as
FeCl4-. A possible reaction is:

Fe3+(aq) + 4Cl-(aq) FeCl4-(aq)

Apparatus and Materials


Test-tubes, test-tube rack, teat pipettes
Distilled water, potassium thiocyanate, ammonium chloride, potassium thiocyanate (0.5 M), iron
(III) chloride (0.5 M)

Procedure
1. Mix together two drops of 0.5 M iron (III) chloride and two drops of 0.5 M potassium
thiocyanate in a test-tube. Add about 10 cm3 of water to form a pale, orange-brown solution.
2. Divide this solution into seven equal parts in separate test tubes. Keep one test tube as a
control, to be used to compare the colour changes occurring in the other test tubes.

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Chemistry @ MBCC Pre-University Science Year 1

3. To one test tube, add two drops of 0.5M iron (III) chloride. Compare the solution to control
sample and record the colour change.
4. To another test tube, add two drops of 0.5M potassium thiocyanate. Compare the solution to
control sample and record the colour change.
5. To a third test tube, add a spatula-full of solid ammonium chloride and shake well. Compare
the colour of this solution with the control and note your observation.
6. To the fourth test tube, add a few drops of AgNO3. Silver ions react with thiocyanate ions to
form insoluble AgSCN in the aqueous solution. Note and record colour change in the
solution.
7. Place the fifth test tube in a hot water bath and record the colour change that occurred.
8. Place the sixth test tube in an ice bath and record the colour change that occurred.

Results and Calculations


Table 1

CHANGE OBSERVATION CAUSE INFERENCE


In what direction
e.g. [Fe3+]
1. Addition of [Fe3+] ions does the equilibrium
increased
position shift?

2. Addition of [SCN-) ions

3. Addition of NH4Cl

4. Addition of AgNO3

5. Heating

6. Cooling

Discussion
1. Complete the table as shown above (Table 1)
2. Suggest a cause for each colour change observed, and then suggest what can be inferred about
a shift in the position of equilibrium
3. Based on the results for test tubes 5 and 6, determine whether the equilibrium reaction for iron
(III) thiocyanate is exothermic or endothermic? Explain your answer

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Chemistry @ MBCC Pre-University Science Year 1

Experiment 18: Chemical Equilibria – Determination of Equilibrium Constant, Kc

Aim
In this experiment you will determine the value of the equilibrium constant, Kc, for an
esterification reaction. This experiment will be conducted over a two week period.

Introduction
Ethyl ethanoate is an ester which is manufactured from ethanoic acid and ethanol. The
overall reaction can be represented as follows;
CH3COOH + CH3CH2OH CH3COOCH2CH3 + H2O
The reaction requires a strong acid catalyst. The purpose of this experiment is to find the value of
the equilibrium constant, Kc , for this reaction at a constant temperature. The procedure
involves setting up a known mixture of ethanoic acid, ethanol, dilute hydrochloric acid (the
strong acid catalyst) and water and leaving it for a period of time to allow the mixture to reach
equilibrium. At the same time, a control is prepared containing only dilute hydrochloric acid.
Titration of the reaction mixture against NaOH gives a measure of the total concentration of acid
(ethanoic acid and dilute HCl) that is present in the equilibrium mixture. Titration of the control
allows the concentration of dilute hydrochloric acid to be determined and from the two titration
results, the equilibrium concentration of ethanoic acid can be determined. Provided the initial
concentrations of ethanoic acid, ethanol, water and dilute hydrochloric acid are known, the
equilibrium concentrations of each of these compounds can be calculated and hence a value of
Kc can be found for the reaction under the conditions of the experiment.
The first part of the experiment involves the setting up of a mixture of ethanoic acid,
ethanol, water along with dilute hydrochloric acid and allowing it to come to equilibrium. A
control containing only the acid catalyst is also set up. The second part of the experiment
involves titrating both the equilibrium mixture and the control with standard 0.100 mol dm-3
sodium hydroxide solution using phenolphthalein as indicator and using the results from these
titrations to calculate Kc for the equilibrium.

Apparatus and Materials


Part 1 (Week 1)
Mass balance (2 d.p), measuring cylinder (50 cm3), conical flask (250 cm3), burette (50 cm3)

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Chemistry @ MBCC Pre-University Science Year 1

Ethyl ethanoate, ethanoic acid (glacial acetic acid), ethanol, hydrochloric acid, distilled water
Part 2 (Week 2)
Pipette (10 cm3), conical flask (250 cm3), burette (50 cm3)
1M NaOH, phenolphthalein indicator

Procedure
Part 1 – Preparing the equilibrium mixture
1. Using the communal burettes provided, each pair of students should prepare ONE of the
following combinations (1-8) in a conical flask (see table below). In another conical flask, each
pair should also prepare a control.
Table 1
Pair # Volume (cm3)
HCl Water Ethyl ethanoate Ethanoic acid Ethanol
Control 5 5 0 0 0
1 5 0 5 0 0
2 5 1 4 0 0
3 5 2 3 0 0
4 5 3 2 0 0
5 5 0 4 0 1
6 5 0 4 1 0
7 5 0 0 1 4
8 5 0 0 2 3

2. Swirl thoroughly the mixtures in the conical flasks. Stopper the flasks and leave to stand for 1
week.
3. Determine the weight of a clean, dry measuring cylinder. Record this weight as W1. Add 5ml
of ethanoic acid to the measuring cylinder and weigh (W2). The difference between the two
weights will be due to the liquid only (W3). Use this information to calculate the density of the
ethanoic acid.
4. Repeat step 3 for dilute HCl, ethyl ethanoate and ethanol.

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Chemistry @ MBCC Pre-University Science Year 1

Part 2
1. Rinse, and then fill a burette with the sodium hydroxide (1M) solution.
2. Add 25 cm3 of distilled water to the conical flask containing your reaction mixture followed
two drops of phenolphthalein indicator. Rapidly titrate the contents of the flasks against sodium
hydroxide. Record the volume of sodium hydroxide required to reach the endpoint. You will
only have ONE opportunity to carry out this titration, so you must do it with care.
3. Repeat step 2 above for the conical flask containing the control.

Results
Table 2
Ethyl ethanoate Ethanoic Ethanol
Weight (g) HCl (cm3) 3
Water (cm ) (cm3) acid (cm3) (cm3)
W2
W1
W3
Density (g/ml)

Table 3

Total Volume of NaOH (cm3) 1 2 3 Control


Final Volume
Initial Volume

Total Volume used

Average Titre Volume

Table 2
# of moles Ethanoic acid Ethanol Ethyl ethanoate Water
Initial
Change (or difference)
Equilibrium

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Chemistry @ MBCC Pre-University Science Year 1

Calculations and Analysis


1. Write an equation for the reaction of ethanoic acid with sodium hydroxide.
2. Calculate the number of moles of sodium hydroxide required to neutralise the reaction
mixture.
3. Write an equation for the reaction of hydrochloric acid with sodium hydroxide.
4. Calculate the moles of sodium hydroxide required to neutralise the control.
5. Calculate the number of moles of hydrochloric acid present in the mixture, hence, calculate
the number of moles of ethanoic acid which must be present in the mixture.
6. Deduce the moles of ethanol, ethyl ethanoate and water in the equilibrium mixture.
7. Calculate the Kc for your reaction mixture.
8. Collect the Kc results from the other student pairs. What do you notice about the values of the
Kc calculated from the other reaction mixtures? Does this support the theory you learned in
class?
9. Suggest one way in which the ester (ethyl ethanoate) yield can be increased. Explain your
answer.

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Chemistry @ MBCC Pre-University Science Year 1

Experiment 20: Determining the Solubility Product Constant, Ksp, for Calcium Hydroxide

Introduction
Calcium hydroxide is only sparingly soluble in water. A saturated solution of calcium
hydroxide has the solid in equilibrium with its ions as shown below:
Ca(OH)2(s) ⇌ Ca2+(aq) + 2OH-(aq)
Recall that a saturated solution is a solution that contains the maximum amount of
dissolved solute possible at a given temperature. A saturated solution contains undissolved solute
in equilibrium with the solution. In this type of equilibrium, the equilibrium constant is called the
solubility product constant, and is represented by the symbol Ksp. The Ksp expression for
calcium hydroxide is written as:
Ksp = [Ca2+] [OH-]2
The solubility product constant, Ksp, is a useful quantity that allows us to predict and calculate
the solubilities of substances in solution. Calcium hydroxide is a base and releases hydroxide
ions in solution. Determination of the hydroxide ion concentration may be used to determine the
Ksp for calcium hydroxide.

Aim
The purpose of this experiment is to determine the Ksp of aqueous calcium hydroxide by
titration.

Apparatus & Materials


Calcium hydroxide solution, 0.01 M hydrochloric acid, phenolphthalein indicator
burette (50 cm3), pipette (25 mL), beakers (250 cm3), conical flasks (x3), measuring cylinder,
retort stand, burette clamp, funnel, filter paper

Procedure
1. Prepare 50 cm3 of saturated calcium hydroxide in a beaker. Measure and record the
temperature of the calcium hydroxide solution.
2. Filter the saturated Ca(OH)2 solution into a clean 250 cm3 beaker. (Filter your solution as
close as possible to the time it will be used, and do not let it stand around in the air for long
periods of time, to avoid any CO2 reacting with the Ca(OH)2 and forming chalk, CaCO3).

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Chemistry @ MBCC Pre-University Science Year 1

3. Fill the burette with filtered Ca(OH)2 solution and record the initial volume of Ca(OH)2 in
the burette to two decimal places.
4. Pipette 10 cm3 of HCl solution into a conical flask and add one or two drops of
phenolphthalein solution.
5. Titrate the contents of the conical flask until a permanent pale pink endpoint is reached.
Record the final burette reading to two decimal places.
6. Repeat titration until two titre readings agree within +/- 0.1cm3.

Results and Calculations


1. What is the average volume of Ca(OH)2 required to reach the endpoint of the titration.
2. Write a balanced chemical equation for the reaction of HCl with Ca(OH)2.
3. Determine the number of moles of HCl required to reach the endpoint.
4. Calculate the number of moles of calcium hydroxide in the pipetted volume.
5. Determine the number of moles of (a) hydroxide ion and (b) calcium ions in the pipetted
volume
6. Calculate the Ksp for calcium hydroxide at the temperature measured.
7. Why was the temperature of the calcium hydroxide solution measured and recorded.

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Chemistry @ MBCC Pre-University Science Year 1

Experiment 21: Planning and Designing II

Problem Statement
A research laboratory fabricated a new metal, X24, which reacts with hydrogen peroxide to
liberate oxygen. The scientist at this research lab claims that the rate of the reaction between X 24
and hydrogen peroxide decreases with increasing temperature. Plan and design an experiment to
test the scientist’s claims.

Experiment 22: Planning and Designing III

Problem Statement
In a discussion about indicators (methyl orange, phenolphthalein and methyl red) and their
effectiveness, one of the students, Maria, stated that of the three indicators mentioned above,
methyl orange is the most suitable indicator to be used in the titration between ammonia and
hydrochloric acid. Plan and design an experiment to test Marie’s claim.

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Chemistry @ MBCC Pre-University Science Year 1

MODULE 3: CHEMISTRY OF THE ELEMENTS

Experiment 24: Flame Tests

Introduction
Many cations of s and d-block elements may be identified by a flame test. The energy from the
burning gas causes promotion of electrons in the ions to higher energy levels. The excited ions
then lose energy and undergo electronic transition to a lower energy level, giving off the extra
energy in the form of electromagnetic radiation. The frequency of this radiation usually falls in
the visible region of the spectrum, so a coloured flame is observed.

Procedure
1. Clean a nichrome or platinum wire by dipping it in concentrated hydrochloric acid and
placing it in a non-luminous Bunsen flame.
2. Continue this cleaning process until no colour at all is produced when the wire is in the
flame.
3. Moisten the wire with concentrated hydrochloric acid, dip it in the sample, and hold it in the
flame again.
4. Record the colour observed.
5. Carry out a flame test on each of the other samples supplied.
6. Record your results in the table below.

Results

Metal ion
Colour

Discussion and Analysis


1. Why are different colours observed?
2. Identify any ion or ions for which there was no colour imparted to the flame
3. Suggest an explanation for this.
4. Why is the cleaning of the nichrome wire necessary before performing a flame test?

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Chemistry @ MBCC Pre-University Science Year 1

Experiment 25: Qualitative Analysis I – Test for Cations

Aim
You will carry out qualitative tests to identify various cations in solution

Introduction
In this experiment you will identify cations dissolved in an aqueous system. You will not need to
quantify the amount of each cation present, but instead merely determine its presence. This is
referred to as qualitative analysis.

Apparatus and Materials


Test tubes, beakers, spatula, Bunsen burner
Sodium hydroxide, ammonium hydroxide, ammonium thiocyanate, potassium hexacyanoferrate
(II), potassium hexacyanoferrate (III), dilute hydrochloric acid, dilute nitric acid, dilute sulphuric
acid, potassium iodide, potassium dichromate, litmus paper, nitrate solutions containing Fe2+,
Fe3+, Cu2+, Cr3+, Mn2+, Pb2+, Ca2+, Ba2+, Al3+, Mg2+, Zn2+ and NH4+ cations

Procedure Observation Inference


Appearance and colour
1. Note the colour of the
solution
Preliminary Tests:
2. Aqueous NaOH
a) To a small portion of
the test solution, add
NaOH dropwise and
record observations
b) Continue adding
NaOH until in excess.

3. Aqueous Ammonia
a) To a small portion of
the cation solution, add
aqueous ammonia
dropwise. Record
observations.
b) Continue adding
aqueous ammonia until
in excess.
Confirmatory Tests:

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Chemistry @ MBCC Pre-University Science Year 1

Procedure Observation Inference


4. Perform the appropriate
confirmatory test on the
given cation.

Confirmatory Tests:
Fe2+
1. Add potassium hexacyanoferrate (II) dropwise to the test solution and record
observations.
2. Add potassium hexacyanoferrate (III) dropwise to the test solution and record all
observations.
Fe3+
1. Add potassium hexacyanoferrate (II) dropwise to the test solution and record
observations.
2. Add potassium hexacyanoferrate (III) dropwise to the test solution and record all
observations.
3. Add a few drops of ammonium thiocyanate to the test solution.
Cu2+
1. Add potassium hexacyanoferrate (II) dropwise to the test solution and record
observations.
2. Add potassium hexacyanoferrate (III) dropwise to the test solution and record all
observations.
3. Add a few drops of potassium iodide to the test solution.
4. Add a few drops of potassium chromate (VI) followed by a few drops of dilute nitric acid
and then aqueous ammonia.
Cr3+
1. Add potassium hexacyanoferrate (II) dropwise to the test solution and record
observations followed by aqueous ammonia

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Chemistry @ MBCC Pre-University Science Year 1

Mn2+
1. Add potassium hexacyanoferrate (II) dropwise to the test solution followed by aqueous
ammonia and record observations.
2. Add potassium hexacyanoferrate (III) dropwise to the test solution and observe. Next add
a few drops of nitric acid followed by aqueous ammonia
Pb2+
1. Add dilute HCl to the test solution and observe. Next add aqueous ammonia
2. Add dilute HCl to the test solution and observe. Next add dilute sulphuric acid
3. Add dilute HCl to the test solution and heat. Record all observations.
4. Add KI to the test solution dropwise, then in excess. Next add dilute nitric acid.
Ca2+
1. Add potassium chromate (VI) dropwise to the test solution and observe. Next add dilute
nitric acid.
2. Add potassium chromate (VI) dropwise to the test solution and observe. Next add
ethanoic acid.
Ba2+
1. Add potassium chromate (VI) dropwise to the test solution and observe. Next add dilute
nitric acid.
2. Add potassium chromate (VI) dropwise to the test solution and observe. Next add
ethanoic acid.

NH4+
1. Add sodium hydroxide and heat. Use litmus paper to test any vapour evolved.

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Chemistry @ MBCC Pre-University Science Year 1

Experiment 26: Qualitative Analysis II – Tests for Anions

Aim
You will carry out qualitative tests for various anions

Apparatus and Materials


Test tubes, beakers, spatula, Bunsen burner
Dilute hydrochloric acid, dilute nitric acid, dilute sulphuric acid, lime water (Ca(OH)2), silver
nitrate, aqueous ammonia, lead ethanoate, hydrogen peroxide, concentrated H2SO4, ferrous
sulphate, litmus paper, solutions containing CO32-, NO3- SO32-, SO42-, CrO42-, Cl-, Br-, I-

Procedure Observation Inference


Test for carbonates (CO32-)
1. To the test solution add dilute HCl
and record observations.
Carefully introduce fresh lime
water (using a glass rod) into the
test tube in which the reaction is
occurring. Note observations.
2. To the test solution, add AgNO3
and record observations. Add
aqueous ammonia to the test tube
and record observations.

Test for sulphites (SO32-)


1. Add dilute HCl to the test
solution.
2. Add AgNO3 dropwise and note
observations. Add AgNO3 until in
excess. Add aqueous ammonia
and record observations.
3. Add potassium dichromate to the
test tube followed by two drops of
dilute H2SO4 and warm.
4. Add lead ethanoate to the test
solution and heat the test tube in
boiling water.

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Chemistry @ MBCC Pre-University Science Year 1

Procedure Observation Inference


Test for sulphates (SO42-)
1. Add barium chloride to the test
solution and acidify with dilute
HCl or dilute HNO3.

Test for nitrates (NO3-)


1. Brown Ring Test:
Add ferrous sulphate to the test
solution. Pour conc. H2SO4
gently down the side of the test
tube. Record observations.

2. Add conc. H2SO4 carefully to


the test solution followed by
copper turnings. Test the gas
evolved with moistened litmus
paper.

Test for chromates (CrO42-)


1. Add barium chloride and
observe. Next add dilute
HNO3. Record observations.

2. Add AgNO3 to the test


solution and observe. Add
dilute HNO3.

3. Add a few drops of dilute


hydrochloric acid followed
by hydrogen peroxide to the
test solution and observe.

Test for chlorides (Cl-)


1. Add conc. H2SO4 and heat.
Test any gas evolved with
moistened litmus paper.

2. Add AgNO3 dropwise and


observe. Add aqueous
ammonia and observe.

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Chemistry @ MBCC Pre-University Science Year 1

Procedure Observation Inference


3. Add AgNO3 dropwise and
observe. Add dilute HNO3
and observe.

Test for bromides (Br -)


1. Add AgNO3 dropwise and
observe. Add aqueous
ammonia and observe.

2. Add AgNO3 dropwise and


observe. Add dilute HNO3
and observe.

Test for iodides (I-)


1. Add AgNO3 dropwise and
observe. Add aqueous
ammonia and observe.

2. Add AgNO3 dropwise and


observe. Add dilute HNO3
and observe.

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Chemistry @ MBCC Pre-University Science Year 1

Experiment 27: Qualitative Analysis III – Identification of Unknown Compounds

Aim
You are required to ascertain the identity of two unknown compounds by identifying the cations
and anions present.

Background
In the qualitative analysis procedure, the chemical properties of an unknown substance are

determined by systematically reacting the unknown with different reagents to determine the

specific ions present in solution. Cations will be identified by their reactions with aqueous

ammonia and sodium hydroxide to form precipitates. The solubility of the precipitates are tested

by reacting with excess reagent. Anions are often tested by reacting with acids to liberate a gas

and testing the gas evolved. Anions may also be tested by reacting with particular reagents to

form precipitates.

Apparatus and Materials


Test tubes, beakers, spatula, Bunsen burner
Sodium hydroxide, aqueous ammonia, potassium iodide, copper metal, concentrated sulphuric
acid, litmus paper, ferrous sulphate, potassium hexacyanoferrate (II) solution, potassium
thiocyanate, silver nitrate

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Chemistry @ MBCC Pre-University Science Year 1

Procedure Observation Inference


Compound A
Note the colour and appearance of
compound A

Prepare a solution from compound A


and divide into five parts
To the first part:
i). Add NaOH dropwise and record
observations.
ii). Continue adding NaOH until in
excess.

To the second part:


i). Add aq. NH3 dropwise and record
observations.
ii). Continue to add aq. NH3 in excess

To the third part:


i). Add KI dropwise and record
observations.
ii). Add aqueous NH3 to the same test
tube until in excess

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Chemistry @ MBCC Pre-University Science Year 1

Procedure Observation Inference


To the fourth part:
Add a few pieces of copper metal. Next,
carefully add a few drops of
concentrated H2SO4 and warm the
solution. Record your observations. Test
any gas evolved with moistened litmus
paper.

To the fifth part:


Add a few crystals of ferrous sulphate.
Next, carefully pour conc. H2SO4 down
the sides of the test tube. Record
observations.
Compound B
Note the colour and appearance of
compound B

Prepare a solution from compound B


and divide into six parts
To the first part:
Add NaOH dropwise and record
observations.
Continue adding NaOH until in excess.

To the second part:


Add aq. NH3 dropwise and record
observations.
Continue to add aq. NH3 in excess

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Chemistry @ MBCC Pre-University Science Year 1

Procedure Observation Inference

To the third part:


Add potassium hexacyanoferrate (II)
solution and record observations.

To the fourth part:


Add potassium thiocyanate to the test
tube. Record observations

To the fifth part:


i). Add silver nitrate dropwise to test
tube. Decant the coloured liquid and
and record observations
ii). Next add aqueous ammonia to the
precipitate in the test tube and record
observations

To the sixth part:


Add a few drops of concentrated H2SO4
to the test tube, then heat. Test the gas
evolved using moistened litmus paper.
Record observations

Conclusion
Compound A
Cation present: ________________ Anion present: ____________________

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Chemistry @ MBCC Pre-University Science Year 1

Identity of Compound A __________________________________________________

Compound B
Cation present: ________________ Anion present: ____________________
Identity of Compound B __________________________________________________

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Chemistry @ MBCC Pre-University Science Year 1

Experiment 28: Planning and Designing IV

Problem Statement
The solubility of sulphates of group II elements demonstrates a particular trend. Derive a
hypothesis and plan and design an experiment to determine the trend in solubility of group II
sulphates.

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Chemistry @ MBCC Worksheets

WORKSHEETS
WORKSHEET 1: MOLARITY
1. Calculate the molarity of a solution that contains 0.0345 mol of NH4Cl in exactly 400 ml of
solution. How many moles of HNO3 are present in 35.0 ml of a 2.20M solution of nitric acid?
How many millilitres of a 1.50M KOH solution are needed to provide 0.125 mol KOH?

2. A person suffering from hyponatremia has a sodium ion concentration in the blood of 0.118M
and a total blood volume of 4.6L. What mass of the sodium chloride would be needed in the
blood to bring the sodium ion concentration up to 0.138M, assuming no change in the blood
volume?

3. Some sulphuric acid is filled on a lab bench. It can be neutralized by sprinkling sodium
bicarbonate on it and the mopping up the resultant solution. The sodium bicarbonate reacts
with sulphuric acid as follows:

2NaHCO3(s) + H2SO4 → Na2SO4 + 2H2O(l) + 2CO2(g)

Sodium bicarbonate is added until the fizzing due to the formation of CO2 (g) stops. If 27 ml of
6.0M H2SO4 was spilled, what is the minimum mass of NaHCO3 that must be added to
neutralize the acid.

4. If you have a stock solution of 14.8M NH3. How many millilitres of this solution should you
dilute to make 100.0 ml of 0.250M NH3? If you take a 10.0 ml portion of the stock solution
and dilute it to a total volume of 0.250L, what will be the concentration of the diluted
solution?

5. Recently many lakes in highly industrialized areas have developed low pH values due to acid
rain containing sulphuric (VI) acid. In order to analyse the acid concentration of Lake Tahia,
three 10cm3 samples of lake water were pipetted in separate conical flasks and titrated with a
0.025 mol dm-3solution of sodium hydroxide. The following results were obtained:

Titration 1 2 3

Volume of alkali (cm3) 14.70 14.50 14.55


i). Determine the volume of acid to be used in your calculations.

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Chemistry @ MBCC Worksheets

ii). Determine the volume of sodium hydroxide to be used in your calculations.


iii). Calculate the number of moles of NaOH used in the titration.
iv). Deduce the number of moles of sulphuric (VI) acid present in the solution.
v). Calculate the concentration of acid in the lake in mol dm-3.
vi). Name one suitable indicator for this analysis.

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Chemistry @ MBCC Worksheets

WORKSHEET 2: TITRATION CALCULATIONS


1. Succinic acid has the formula (CH2)n(COOH)2 and reacts with dilute sodium hydroxide as
follows:
(CH2)n(COOH)2 + 2NaOH → (CH2)n(COONa)2 + 2H2O
2.0g of succinic acid were dissolved in water and the solution made up to 250 cm3. This
solution was placed in a burette and 18.4 cm3 was required to neutralise 25 cm3 of 0.1M
NaOH. Deduce the molecular formula of the acid and hence the value of n.

2. Sodium carbonate exists in hydrated form, Na2CO3.xH2O, in the solid state. 3.5 g of a sodium
carbonate sample was dissolved in water and the volume made up to 250 cm3. 25.0 cm3 of this
solution was titrated against 0.1 mol dm-3 HCl and 24.5 cm3 of the acid were required.
Calculate the value of x given the equation:
Na2CO3 + 2HCl → 2NaCl + CO2 + H2O

3. 25 cm3 of a sample of vinegar (CH3COOH) was pipetted into a volumetric flask and the
volume was made up to 250 cm3. This solution was placed in a burette and 13.9 cm3 were
required to neutralise 25 cm3 of 0.1 moldm-3 NaOH. Calculate the molarity of the original
vinegar solution and its concentration in gdm-3, given that it reacts with NaOH in a 1:1 ratio.

4. 2.5g of a sample of ethanedioic acid, H2C2O4.nH2O, was dissolved in water and the solution
made up to 250 cm3. This solution was placed in a burette and 15.8 cm3 were required to
neutralise 25 cm3 of 0.1 moldm-3 NaOH. Given that ethanedioic acid reacts with NaOH in a
1:2 ratio, calculate the value of n.

5. A toilet cleaner containing sodium hydrogensulphate, NaHSO4 is believed to have been


contaminated. 5.678 g of the sample were dissolved in water and the solution was made up to
250 cm3. This solution was placed in a burette and 23.1 cm3 of it were required to neutralise
25 cm3 of 0.1 moldm-3 sodium hydroxide. Calculate the percentage purity of the sample given
that the species react in a 1:1 ratio.

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6. When silicon tetrachloride is added to water, the following reaction occurs:


SiCl4(l) + 2H2O(l) → SiO2(s) + 4HCl(aq)
1.2 g of impure silicon tetrachloride was dissolved in excess water, and the resulting solution
was made up to 250 cm3. A 25 cm3 portion of the solution was then titrated against 0.10
moldm-3 sodium hydroxide, and 18.7 cm3 of the alkali were required. What was the
percentage purity of the silicon tetrachloride?

7. 13.2 g of a sample of zinc sulphate, ZnSO4.xH2O, was strongly heated until no further change
in mass was recorded. On heating, all the water of crystallisation evaporated as follows:
ZnSO4.xH2O → ZnSO4 + xH2O
Calculate the number of moles of water of crystallisation in the zinc sulphate sample given
that 7.4 g of solid remained after strong heating

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WORKSHEET 3: REDOX REACTIONS


5. A chemist carried out an experiment to test the oxidizing properties of halogens by their
displacement reactions.
a) Complete the table below with the expected observations and inferences. Use equations
where appropriate to illustrate your inferences.

Table 3: Displacement Reactions of Halogens


TEST OBSERVATION INFERENCE
Chlorine gas was bubbled
through a solution of
potassium bromide. Hexane
was then added and the
contents mixed.
Chlorine gas was bubbled
through a solution of
potassium iodide. Hexane
was then added and the
contents mixed.
Bromine liquid is added to a
solution of sodium chloride.
Hexane was then added and
the contents mixed.
Bromine liquid is added to a
solution of potassium iodide.
Hexane was then added and
the contents mixed.
Iodine is added to a solution
of sodium chloride. Hexane
was then added and the
contents mixed.

Iodine is added to a solution


of sodium chloride. Hexane
was then added and the
contents mixed.

b) Use the data in the table above to rank the halogens in order of increasing oxidizing ability.

c) Justify your answer.

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______________________________________________________________________________
______________________________________________________________________________
______________________________________________________________________________
_____________________

WORKSHEET 4: REDOX REACTIONS II


1. A chemist carried out some experiments to determine whether a compound M is an
oxidizing agent or reducing agent. The table below shows the information that was recorded
by the chemist. Complete the table by filling in the inference column. Use equations where
appropriate to illustrate your inferences.

TEST OBSERVATION INFERENCE


1 ml of a solution of Fe2+
ions was added to a test Solution changed from pale
tube. A few drops of green to reddish brown.
solution M was then added
and the mixture shaken.
A strip of iodide paper
was moistened in starch The iodide paper becomes
and then dipped into blue- black.
solution M.
1 ml of solution M was
added to a test tube
containing about 1 ml of
No visible reaction
acidified potassium
dichromate. The test tube
warmed.

b) Based on the information in the table above, state whether compound M is an oxidizing or
reducing agent. Justify your answer.
__________________________________________________________________________

__________________________________________________________________________

__________________________________________________________________________

_____________________

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c) What would you expect to observe in the test tube if solution M is reacted with hydrogen

sulphide (H2S)?

__________________________________________________________________________

_______

2. You are provided with three metals X, Y and Z and the nitrates of these metals. Outline an
experiment that would determine the order of reactivity of these metals.

3. Outline an experiment you would use to rank the halogens in terms of their oxidising ability.
Your answer should include appropriate apparatus and materials to carry out the experiment.

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WORKSHEET 5: QUALITATIVE IDENTIFICATION OF COMPOUNDS


Substance S is a simple salt containing one cation and one anion. Complete the inference column
of the table using the data in the Tests and Observations columns

Table 4 : Qualitative Identification of Compounds

TEST OBSERVATION INFERENCE

Describe the appearance of the salt


S white solid

Carry out a flame test on the salt S apple-green flame

Dissolve a spatula measure of S in about 10 cm3 of water

To about 1 cm3 of the solution of S


add an equal volume of ammonium
sulphate followed by dil. HCl. white precipitate

To about 1 cm3 of the solution of S


add an equal volume of sodium
carbonate solution. white precipitate

To about 1 cm3 of the solution of S


add about 2 cm3 of NaOH and boil
carefully. pungent smelling gas
Then add a small piece of
aluminium foil (or granules). damp red litmus turns blue

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WORKSHEET 6: TRANSITION METALS


Consider the following equation and answer the question below:
[Co(H2O)6]2+ + 4Cl- ⇄ [CoCl4]2- + 6 H2O

1. What is the colour of the following complexes?


a) [Co(H2O)6]2+
----------------------------------------------------------------------------------------------------------
b) [CoCl4]2-
----------------------------------------------------------------------------------------------------------

2. What would you expect to observe after the following changes?


a) Addition of concentrated HCl to the equilibrium mixture
----------------------------------------------------------------------------------------------------------
b) Addition of water to the equilibrium mixture
----------------------------------------------------------------------------------------------------------

3. Name and State the principle which was used to explain the observations in question 2 above.

----------------------------------------------------------------------------------------------------------------

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APPENDICES
APPENDIX A: CONSTANTS AND MEASUREMENTS
Constants
Molar gas constant, R= 8.314JK-1 mol-1
Specific heat capacity of water, c = 4.18 Jg-1K-1
Speed of light in a vacuum, c = 3.00 x 108 ms-1
Planck’s constant, h = 6.63 x 10-34Js

Measurements
It is expected that students will become familiar with the SI fundamental units, those derived
from combing SI unit system.
Fundamental units
• Mass kilograms, kg
• Length meter, m
• Time second, s
• Temperature Kelvin, k
• Amount of chemical substances mole, mol
Derived units
• Force newton, N= kgms-2
• Pressure Pascal, Pa= Nm-2 = kgm-1s-2
• Energy joules, J= Nm =kgm2s-2
• Density kgm-3
Units outside the strict SI system
• Mass tonne (metric ton), t 1 t =106 g=1000kg
• Volume litre, L 1 L= 1 dm 3 = 10-3 m3
• Celsius temperature 0
C 00C =-273.15 K
• Pressure atm 1 atm= 101.325 Pa
Commonly used prefixes for small quantities
Deci, d 10-1 Centi, c 10-2 Milli, m 10-3
Nano, n 10-9 Pico, p 10-12 Micro, µ 10-6

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Chemistry @ MBCC Appendix

APPENDIX B: PREPARATION OF STANDARD SOLUTIONS


A standard solution is a solution whose concentration is accurately known. The concentration is
usually given in mol dm-3. When making up a solution it is important that the correct mass of
substance is accurately measured. It is also important that ALL the mass is successfully
transferred to the volumetric flask used to make up the solution.

Background calculations
1. Work out the number of moles needed to make up a solution with the required volume and
concentration.
2. Work out the relative formula mass of the chosen substance.
3. Work out the mass of the substance needed using your answers from steps 1 to 2.

Making up the solution


1. Take a watch glass and place it on the balance. Tare the balance (set to zero). Carefully weigh
out the required mass of substance.
2. Transfer this amount to a beaker. Add distilled water from a wash bottle to dissolve. Make
sure that all the substance is washed off the glass. It may be necessary to rinse twice.
3. Stir with a glass rod until the solid is dissolved, and then transfer the solution to the volumetric
flask. Use more distilled water to rinse out the beaker and the glass rod at least twice.
4. Add water to just below the line on the volumetric flask. And then add the final drops with a
teat pipette to ensure that the bottom of the meniscus is on the line.
5. Place the lid on the flask and turn the flask over a couple of times to mix the solution.
6. Label the solution with your name, date the contents.
7. Wash up all the apparatus.

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APPENDIX C: QUALITATIVE ANAALYSIS OF INORGANIC COMPOUNDS


Identification of Cations and Anions
Qualitative analysis of inorganic compounds involves the identification of the ions in the
sample. Unlike quantitative analysis, we are not concerned with the exact amount of a substance
present in a sample but only with its identity. Ideally when performing chemical tests to identify
individual ions, there should be no interference from any other ions. Unfortunately, when
multiple ions are present, there may often be complications which can end up masking some of
the tests.
In determining the cations and anions that make up ionic compounds the following tests
may be performed:
• Observing the appearance of the compound (both solid and in solution)
• Flame Tests
• Testing for colour and solubility of hydroxides (using sodium hydroxide and aqueous
ammonia
• Evolution of gases
• Formation of precipitates

1. Flame Tests
Table 5: Flame tests for selected metal ions in solution
Metal Colour
Lithium Magenta
Sodium Yellow
Potassium Lilac
Calcium Brick red
Strontium Blood red
Barium Apple green

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Chemistry @ MBCC Appendix

2. Test for Gases


Table 6: Distinguishing Tests and results for common gases evolved
DISTINGUISHING
TEST CHARACTERISTICS TEST OBSERVATIONS
• Colourless gas A lit splint is held near the
• Odourless gas Burns with a yellow flame - pops in
opening of the tube
Hydrogen (H2) air
• Neutral gas containing the gas
• Colourless gas A lit splint is held near the
Oxygen (O2) • Odourless gas opening of the tube Rekindles a glowing splint
• Neutral containing the gas
• Greenish-yellow gas Test gas with moistened Cl2 turns blue litmus red and
• Pungent odour litmus paper bleaches it
Chlorine (Cl2)
• Acidic gas Bubble gas through KBr Solution changes from colourless to
solution reddish - brown
• Colourless gas
Bubble gas through White precipitate; limewater
Carbon dioxide (CO2) • Odourless gas
limewater becomes cloudy
• Neutral gas
Test gas with moistened Turns damp blue litmus red (gas is
litmus paper acidic)
• Colourless gas bubble gas through
Sulphur dioxide (SO2) • Pungent smell acidified potassium Solution changes from orange to
• Acidic Gas dichromate (VI) solution; green; dichromate paper turns from
pass gas over orange orange to green
dichromate paper
• Colourless gas Test gas with moistened Turns damp blue litmus red; Fumes
Hydrogen Chloride • Odourless gas litmus paper in moist air to give a mist
(HCl) • Acidic gas Forms white fumes due to presence
• Forms fumes in moist air Test with ammonia gas
of ammonium chloride (NH4Cl)
Test gas with moistened
Ammonia (NH3) • Colourless gas Turns red litmus blue
litmus paper
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Chemistry @ MBCC Appendix

• pungent smell Forms white fumes due to presence


Test with HCl gas
• Alkaline gas of ammonium chloride (NH4Cl)

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3. Tests for Anions


Halides – (Cl-, Br-, and I-)
Test the solution of halide ions (Cl-, Br- and I-) with Ag+ followed by NH3 (aq)

Table 7
HALIDE Ag+ (aq)
White precipitate insoluble in dilute HNO3.
Chloride Soluble in dilute NH3 (aq)
Soluble in conc. NH3
Cream precipitate insoluble in dilute HNO3.
Bromide Insoluble in dilute NH3 (aq)
Soluble in conc. NH3
Yellow precipitate insoluble in dilute HNO3.
Iodide Insoluble in dilute NH3 (aq)
Insoluble in conc. NH3 (aq)

Carbonate, CO32- and hydrogen carbonate, HCO3-


Test aqueous solutions of CO32- and HCO3- with dilute acid and Mg2+(aq)

Table 8

TEST CO32- (aq) HCO3- (aq)


Dilute acid CO2 gas is evolved
CO2 gas is evolved
2H+(aq) + CO32-(g) → CO2(g) + H2O(l)
No precipitate [Mg(HCO3)2, is soluble]
Mg2+(aq) White precipitate of MgCO3 On heating it decomposes forming a
precipitate of MgCO3

Sulphate (V1) ion, SO42- and sulphate (IV) ion, SO32-


Test aqueous solutions of SO42- and SO32 with dilute acid and Ba2+(aq)

Table 9

TEST SO42- (aq) SO32- (aq)


no reaction
acrid, choking SO2 gas evolved; gas turns
Dilute acid H+(aq) + HCO3-(g) → CO2(g) +
dichromate paper from orange to green
H2O(l)
white precipitate; soluble in HCl
dense white precipitate of BaSO4;
Ba2+(aq) + SO42–(aq) → BaSO4(s)
BaCl2 + HCl insoluble in HCl
BaSO3(aq) + 2HCl(aq) → BaCl2(s) + H2O(l) +
Ba2+(aq) + SO42–(aq) → BaSO4(s)
SO2(s)

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Chemistry @ MBCC Appendix

Dilute HCl +
dense white precipitate of BaSO4
no precipitate
BaCl2 Ba2+(aq) + SO42–(aq) → BaSO4(s)

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Chemistry @ MBCC Appendix

Nitrate (V) ion, NO3-


a) Dissolve 2 or 3 small crystals in one quarter of a test tube of sodium hydroxide
solution. Add a small quantity of aluminium. Warm the mixture.
Ammonia gas is evolved which turns moistened red litmus blue
5OH- + 18H2O + 3NO3- + 8A1→3NH3 + 8Al(OH)4-

b) Brown-ring Test: Dissolve ferrous sulphate crystals in test solution. Pour concentrated
H2SO4 gently down the side of the test tube.
Where the liquids meet a brown ring forms

c) Add copper turnings to the test solution followed by careful addition of concentrated
H2SO4. Brown gas (NO2) is evolved which turns blue moistened litmus paper red.
General thermal decomposition occurs:
2M(NO3)2(s) → 2MO(s) + 4NO2(g) + O2(g)

Chromate (V) ion, Cr2O42-


a) Add dilute acid to the test solution
The yellow solution turns orange as the dichromate (VI) ion is formed
2CrO42–(aq) + 2H+(aq) → Cr2O72–(aq) + H2O(l)

b) Add barium chloride or barium nitrate solution


A yellow precipitate of barium chromate (VI) is formed which is soluble in dilute nitric
acid
Ba2+(aq) + CrO42–(aq) → BaCrO4(s)
c) AgNO3 is added to the test solution followed by dilute HNO3
A brick red precipitate forms which is soluble in nitric acid
CrO42+(aq) + 2Ag+(aq) ⇌ Ag2CrO4(s)

d) Hydrogen peroxide is added to the acidified test solution.


Deep blue solution results. After a while bubbles are seen and the colour gradually fades
to a pale blue-green due to formation of chromium (III) ions.
2CrO42–(aq) + 2H+(aq) → Cr2O72–(aq) + H2O(l)
Cr2O72– (aq) + H2 O2 (aq) + 8H+ (aq) → 2Cr3+(aq) + 5H2 O(I) + 2O2 (g)

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4. Tests for Cations


Colour of solution
Colourless – indicates the absence of transition metal ions

Coloured solution – indicates the presence of a transition metal ions

Table 10
Colour of
solution Possible metal ions present
Colourless NH4+, Ca2+, Ba2+, Mg2+, Zn2+, Pb2+, Al3+
Pale pink Mn2+
Pale green Fe2+
Yellow-brown Fe3+
Green Ni2+
Blue Cu2+
Dark green/purple Cr3+
Rose Co2+
Violet Co3+

Preliminary Tests with NaOH and aqueous NH3


NaOH:
Formation of insoluble metal hydroxides using aqueous NaOH
M2+(aq) + 2OH-(aq) →M(OH)2 (s)

NH4+ ions when treated with aqueous NaOH release a pungent gas which turns red litmus blue
NH4+ (aq) + OH- (aq) → NH3 (g) + H2O (l)

Al(OH)3, Pb(OH)3, Zn(OH)2 and Cr(OH)3 are soluble in excess NaOH due to their amphoteric
nature.
Al(OH)3 (s) + 3OH-(aq) → [Al(OH)6]3–(aq)
Pb(OH)2 (s) + 2OH-(aq) → [Pb(OH)4]2–(aq)
Cr(OH)3 (s) + 3OH-(aq) → [Cr(OH)6]3–(aq)
Zn(OH)2 (s) + 2OH-(aq) →[Zn(OH)4]2–(aq)

Aqueous NH3:
Formation of insoluble metal hydroxides using aqueous NH3
NH3 (aq) + H2O →NH4+ (aq) + OH-(aq)
M2+(aq) + 2OH-(aq) →M(OH)2 (s)

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Chemistry @ MBCC Appendix

Cu(OH)2, Zn(OH)2, Ni(OH )2 are soluble in excess ammonia due to the formation of complex
ions
M(OH)2 (s) + 4NH3 (aq) → [M(NH3 )4]2+(aq) + 2OH-(aq)

** Ba2+ ions do not give a hydroxide precipitate because barium hydroxide, Ba(OH)2 is too
soluble
Table 11: Test for colourless ions using NaOH and aqueous NH3
Ca2+ Mg2+ Al3+ Zn2+ Pb2+
NaOH(aq)
white ppt. white ppt. white ppt. white ppt. white ppt.
dropwise
NaOH(aq) in excess insoluble insoluble soluble soluble soluble
NH3(aq) dropwise white ppt. white ppt. white ppt. white ppt.
Aq. NH3 (aq) in No ppt.
insoluble insoluble soluble insoluble
excess

Table 12: Test for coloured ions using NaOH and aqueous NH3
Cu2+ Fe2+ Fe3+ Ni2+ Cr3+ Mn2+
NaOH(aq) reddish- grey-green off-white
blue ppt. green ppt. green ppt.
dropwise brown ppt. ppt. ppt.
NaOH(aq) in
insoluble insoluble insoluble insoluble soluble insoluble
excess
NH3(aq) reddish- grey-green off-white
blue ppt. green ppt. green ppt.
Dropwise brown ppt. ppt. ppt.
Aq. NH3 (aq) in deep blue dark blue
insoluble insoluble insoluble insoluble
excess solution soln

Confirmatory Tests
Manganese (II) - Mn2+
When treated with excess 2M sodium hydroxide, a white precipitate is formed
Mn2+ (aq) + 2OH- (aq) → Mn(OH)2 (s)
Addition of 20 vol hydrogen peroxide gives a black precipitate of manganese (IV) oxide (MnO2)
with evolution of oxygen.

Iron (II) - Fe2+


To a solution of Fe2+ add a solution of potassium hexacyanoferrate (III) : dark blue precipitate.
Fe2+ (aq) + [Fe(CN)6] 3- (aq) → Fe3+ (aq) + [Fe(CN)6] 4- (aq)
K+ (aq) + Fe3+ (aq) + [Fe(CN)6] 4- (aq) →KFeIII[FeII(CN)6] (s)

Iron (III) - Fe3+

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To a solution of Fe3+ add a solution of potassium thiocyanate. A deep red/blood-red complex is


formed.
[Fe(H2O)6] 3+ (aq) + SCN (aq) → [Fe(H2O)5SCN] 2+ (aq) + H2O (l)

Cobalt(II) - Co2+
A few drops of concentrated hydrochloric acid added to a pink solution of cobalt (II) results in a
colour change from pink to blue.
[Co(H2O)6] 2+ (aq) + 4Cl- (aq) → 6 [CoCl4] 2- (aq) + 6H2O (l)
pink blue

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Lead (Pb2+)
Addition of halide ions forms a precipitate with lead (II) ions
Pb2+(aq) + 2X-(aq) → PbX2 (s)

Table 13
Pb2+ (aq)
White precipitate
Chloride Soluble in hot water which forms needle-shaped crystals on
cooling
Cream precipitate
Bromide
Soluble in hot water
Bright yellow precipitate
Iodide
Soluble in hot water; forms thin, dense golden flakes on cooling

References:
1. Maraj, S., Sami, A., Chemistry for CAPE, (2nd/2011 Edition), Caribbean Educational
Publishers
2. Lambert, E.N., Mohammed M.J., Comprehensive Qualitative Analysis for Advanced Level
Chemistry, Heinemann, 1978
3. UWI Mona (Chemistry Department), C06J/K Chemistry Lab Manual, 2012
4. http://www.chemguide.co.uk
5. http://www.ausetute.com.au/

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