SKT3033: Basic Inorganic Chemistry

LABORATORY MANUAL

SKT3033 BASIC INORGANIC CHEMISTRY

SEMESTER 2 SESSION 2022/2023

Department of Chemistry Faculty of Science and

Mathematics UNIVERSITI PENDIDIKAN SULTAN IDRIS

No Experiment Pages

1 Determination of water hardness by edta 7

2 Inorganic qualitative analysis 11

1
SKT3033: Basic Inorganic Chemistry

3 Relative reactivity of metals using salt solutions 16

4 Properties of halogen 21

GUIDELINE TO WRITE LAB REPORT

OBJECTIVE
State the objective clearly in a complete sentence. A few explanatory sentences may be
included, if needed.
The objective should answer the question: What is the lab objective designed to determine?

EXPERIMENTAL PROCEDURE
The experimental methods should give a detailed description in your own words of how YOU
accomplished the experimentation (Passive voice sentences).
*Tips: This should include equipment used in the experiment as well as how it was used. The
description should have sufficient detail so that another experimenter could duplicate your
efforts. Use sketches and diagrams to describe the experimental set-up. Label the main
components.
Tips: Any information copied directly from Lab manuals or other references should be stated
within quotes and referred, otherwise, it is considered plagiarism.

RESULTS AND DISCUSSION

This is the most important part of the report. Summarize your results in the introductory
sentence. Relate your results to your objective. Present the results in the easiest way for your
reader to understand: graphs, tables, figures, etc.
Spreadsheets are often an ideal tool for organizing the data, analyzing the data, and generating
graphs and tables. All tables and figures should be accompanied by comments or discussions in
the text of report; use a numbering system for identification of each one.
All figures and tables must have numbers and captions. While the table captions should be
placed over the table, figure captions should be placed below the figure.
Explain the results of the experiment, comment on the results you obtained, compare obtained
results with expected results, give probable reasons for discrepancies from the correct results,
answer any questions outlined in the instructions and solve any problems that may have been
presented. Tell why things happened, not only that they did happen. Implementation errors
should be discussed here.

2
SKT3033: Basic Inorganic Chemistry

CONCLUSIONS
State your discoveries, judgments and opinions from the results of this experiment and relate it
with your experiment objectives. Suggest ways to improve the results of this experiment.

3
 SKT3033: Basic Inorganic Chemistry

REFERENCES

How to write references:

1. When citing a website, the basic structure is as follows:

Author surname, initial(s). (Year, month day). Title. Retrieved from URL

1. Mitchell, J.A. (2012, Dec 21). Rate of Reaction of Sodium Thiosulfate and Hydrochloric acid.
Retrieved from http://m.youtube.com/watch?v= r4IZDPpN-bk
2. Kennedy, J. F. (2013, Nov 03). Bromination of Acetone. Retrieved from
http://chemlab.truman.edu/physical-chemistry/physical-chemistry-laboratory/bromination-
ofacetone/

2. How to Cite a Book (Title, not chapter) in APA Format

1. Weller, M. T., Overton, T., Rourke, J., & Armstrong, F. (2018). Inorganic chemistry. Oxford:
Oxford University Press.
2. Housecroft, C. E., & Sharpe, A. G. (2018). Inorganic chemistry. Harlow, England: Pearson.

SAFETY RULES AND REGULATIONS IN CHEMISTRY LABORATORY

1. DO NOT ENTER the laboratory without the permission of the laboratory instructor.
2. All bags should be placed on the rack provided. All gadgets (handphone, tablet, etc) are
NOT ALLOWED during experiments.

4
SKT3033: Basic Inorganic Chemistry

3. Please wear a proper attire to work in the lab (Short pants, short skirt, “purdah”,
sleeveless shirt are not permitted).
4. Wearing jewellery is not permitted in the laboratory.
5. Long hair and scarf must be properly manageable.
6. DO NOT wear contact lenses.
7. Wearing personal protection equipment (PPE) is compulsory in laboratory such as lab
coat, cover shoes and safety glasses, gloves and etc.
8. Student are NOT ALLOWED to smoke, drink, eat, play around and run in laboratory
9. Know the location of all safety equipment.
10. No experiment can be performed without the permission of the laboratory instructor.
11. Read the label on the container of a chemical twice to make sure you are using the right
chemicals. Follow the instructions properly. DO NOT waste chemicals. Use required
amount only.
12. DO NOT contaminate chemicals. Once chemical has been removed from their containers,
DO NOT put it back into the stock container.
13. DO NOT use cracked or chipped glassware.
14. NEVER use mouth suction when using a pipette. Use a pipette filler/bulb.
15. DO NOT leave any heating, vigorous or rapid reaction unattended.
16. Always use fume hood when working with flammable organic compounds, strong acid and
base, volatile solvent, corrosive and toxic materials.
17. DO NOT heat flammable materials directly.
18. Make sure your surrounding is safe before using Bunsen burner.
19. While heating chemicals in test tubes, NEVER point the tubes to yourself or others.
20. Waste chemicals must be disposed properly by placing them in waste container provided.
Ask your instructor how to discard used reagents.
21. Broken apparatus, water and gas leakage must be reported to laboratory assistant on
duty immediately.
22. In case on fire or hearing emergency siren, evacuate the laboratory quickly in orderly
manner. In case of small accident or small fire occurs, try to overcome them wisely.

23. Report any accidents (minor or major) to your laboratory instructor. This accident must be
recorded in log book “CATATAN KEMALANGAN”.
24. Clean all glassware and place them appropriately before leaving laboratory. Make sure to
switch off instruments, water and gas supplies.
25. Final year project students should require permission from supervisor and head of
department if they want to work after normal working hours.

5
SKT3033: Basic Inorganic Chemistry

AN EXPERIMENT DONE WELL IS......

AN EXPERIMENT DONE SAFELY

6
 SKT3033: Basic Inorganic Chemistry

EXPERIMENT 1

DETERMINATION OF WATER HARDNESS BY EDTA

1.1 OBJECTIVES

Students should be able to:

Determine calcium and magnesium content is water sample by complexometric titrations using
EDTA

1.2 INTRODUCTION

Water quality is evaluated using a number of parameters, including total ionic content, pH, total
dissolved solids, organic compounds, and water hardness. Water hardness is always defined as
the sum of the concentrations of Ca2+ and Mg2+ in water. “Hard” water typically contains high
concentrations of Ca2+ and Mg2+, which react with fatty acids in soap, causing them to precipitate.
Both Ca2+ and Mg2+ can be determined by titration with a chelating agent,
ethylenediaminetetraacetic acid (EDTA), usually in the form of disodium salt (H2Y2-). The
complexation reaction of EDTA with either Ca 2+ and Mg2+ can be represented in the following ways,
where M2+ represents the metal ion:

M2+(aq) + H2Y2-(aq) → MY2-(aq) + 2H+ (aq)

Erichrome Black T is commonly used as indicator for the above titration. At pH 10, M 2+(aq) ion first
complexes with the indicator as MIn+(aq) which is wine red. As the stronger ligand EDTA is added,
the MIn+(aq) complex is replaced by the MY 2-(aq) complex which is blue. The end point of titration
is indicated by a sharp colour change from wine red to blue.

Titration using Erichrome Black T as indicator determined total hardness due to Ca 2+ and Mg2+
ions. The hardness of water is structured by a numerical range. Determination of Ca 2+ and Mg2+
concentration in ppm is helpful in classifying the water hardness level in the water sample.

Apparatus
Pipette
Burette
Dropper
400 mL beaker
1 L volumetric flask
100 mL volumetric flask
500 mL volumetric flask
250 mL Erlenmeyer flask

7
 SKT3033: Basic Inorganic Chemistry

Chemicals
Ethanol
Distilled water
Concentrated Hydrochloric Acid, HCl (37%)
Calcium Carbonate, CaCO3
Ammonium Chloride, NH4Cl Concentrated
Ammonia, NH3
Erichrome Black T indicator
Disodium dihydrogen EDTA dehydrate

1.3 PROCEDURE

PART A: PREPARATION OF A STANDARD EDTA SOLUTION

1. Weigh approximate 4.0 g of disodium dihydrogen EDTA dehydrate into a 400 mL beaker.
2. Dissolve the solids in distilled water and transfer this solution into 1 L volumetric flask. (This
process might take about 15 minutes. You may warm the solution gently to help the process
along)
3. Dilute to the mark with distilled water and mix thoroughly.
4. Keep solution capped when not in use.

PART B: PREPARATION OF STANDARD CALCIUM CHLORIDE SOLUTION

1. Weigh accurately 0.4 g calcium carbonate.

2. Transfer the solid to a 500 mL volumetric flask and dissolve with 100 mL distilled water.
3. Add concentrated HCl until there is no effervescence and the solution is clear.
4. Dilute to the mark with distilled water and mix thoroughly.

PART C: PREPARATION OF AMMONIA-AMMONIUM CHLORIDE BUFFER

1. Dissolve 6.75 g of NH4Cl in 57 mL concentrated NH3.

(Make sure to handle concentrated ammonia in fume hood)
2. Transfer into a 100 mL volumetric flask and dilute with distilled water to the mark.

PART D: STANDARDIZATION OF EDTA SOLUTION

1. Pipet 50 mL of the CaCl (Part B) solution into three (3) 250 mL Erlenmeyer flasks.
2. Add 5 mL of ammonia-ammonium buffer solution (Part C) and 15-20 drops of Erichrome
Black T indicators into each flask, respectively.
(The indicator solution was prepared by dissolving 0.50 g of the Erichrome Black T indicator in
100 mL of alcohol)
3. Titrate this solution with EDTA, until the colour of the solution change from wine-red to pure
blue. (Do not stop titrating at a violet or purple colour).
4. Repeat this titration with all three trials and record the volume.
5. Calculate the average molarity of the EDTA solution from the concentration of CaCl solution
and the volume of EDTA used to titrate.
8
 SKT3033: Basic Inorganic Chemistry

PART E: DETERMINATION OF Ca2+ and Mg2+ CONCENTRATION IN WATER SAMPLE

1. Pipet 50 mL of water sample containing unknown amount of Ca2+ into three (3) 250 mL
Erlenmeyer flasks, respectively.
2. Add 5 mL of ammonia-ammonium buffer and 15-20 drops of Erichrome Black T indicator.
3. Titrate with EDTA until a blue colour appears.
4. Use the volume and molarity of EDTA to calculate the water hardness in ppm.
5. Repeat step (1-4) using water sample containing unknown amount of Mg2+.
1.4 REFERENCES

1. Beran, J. A. (2014). Laboratory Manual for Principals of General Chemistry (7 th). Hoboken,
NJ: Wiley.
2. Heasley, V. L., Christensen, V. J. & Heasley, G. E. (2013) Chemistry and life in the
laboratory: Experiments. USA: Pearson.

1.5 WORKSHEET

PART B: FINDING MOLARITY OF CALCIUM CARBONATE

Weigh of sodium-EDTA used :

Weigh of CaCO3 :

Molarity of CaCO3 :

(Grams of CaCO3 / MW of CaCO3)

litres of solution
Moles of Ca2+ in 50.00 mL aliquot :

PART D: FINDING MOLARITY OF EDTA FROM STANDARD SOLUTION

Trials Final Volume EDTA Initial Volume EDTA Volume of EDTA used
1
2
3
Average volume of EDTA used:
M2+(aq) + H2Y2-(aq) → MY2-(aq) + 2H+ (aq)

Moles of EDTA were used:

9
 SKT3033: Basic Inorganic Chemistry

Molarity of EDTA:

PART E: FINDING CONCENTRATION OF Ca2+ IN WATER SAMPLE

Trials Final Volume EDTA Initial Volume EDTA Volume of EDTA used
1
2
3
Average volume of EDTA used:
Moles of EDTA were used:

10
 SKT3033: Basic Inorganic Chemistry

Moles of Ca2+ in 50.00 mL water sample:

Molarity of Ca2+ in water sample:

Concentration of Ca2+ in water sample (ppm): [Ca2+] x MW Mg2+ x 1000 mg

1 ppm = 1 mg/L 1g

PART E: FINDING CONCENTRATION OF Mg2+ IN WATER SAMPLE

Trials Final Volume EDTA Initial Volume EDTA Volume of EDTA used
1
2
3
Average volume of EDTA used:
Moles of EDTA were used:

Moles of Mg2+ in 50.00 mL water sample:

Molarity of Mg2+ in water sample:

Concentration of Mg2+ in water sample (ppm): [Mg2+] x MW Mg2+ x 1000 mg

1 ppm = 1 mg/L 1g

__________________________ _____________________________
DATE LECTURER’SSIGNATURE/STAMP

EXPERIMENT 2
11
 SKT3033: Basic Inorganic Chemistry

INORGANIC QUALITATIVE ANALYSIS

2.1 OBJECTIVES

Students should be able to:

1. understand and describe the procedures of qualitative analysis

2. know the difference between qualitative and quantitative analysis

2.2 INTRODUCTION

Unlike covalent compounds which can be identified using physical properties like boiling point and
refractive index, ionic compounds are more appropriately identified with their chemical properties.
In the qualitative analysis procedure, the chemical properties of an unknown substance are
determined by systematically reacting the unknown with a number of different reagents. By
predetermining what the particular reaction will produce if a specific ion is present, the ions that
actually are in the solution can be identified. For example, if a reaction is known to produce a
precipitate if ion A is present and a precipitate is formed when the reaction is run, then ion A may
be present in solution (there may be and usually are other ions that will also precipitate with a
particular reagent). If no precipitate is formed when the reaction is run, the ion A is clearly not
present in the unknown solution and a different reaction will have to be run to determine what ions
are present.

Apparatus
Boiling and test tube Graduated
cylinder
Graduated cylinder Dropper

Chemicals
Lead(II) nitrate
Iron(II) chloride
Calcium carbonate
Calcium hydroxide solution (lime water)
Nitric acid (1 M, 3 M and 6 M)
Sodium hydroxide solution (1 M)
Ammonia solution (3 M and 6 M)
Acetic acid (6 M)
Sodium acetate (0.2 M)
Dimethylgloxime
Silver nitrate (0.1 M) Sulfuric
acid (2 M)
Concentrated sulphuric acid
FeSO4.7H2O solid Distilled
water

12
 SKT3033: Basic Inorganic Chemistry

2.3 PROCEDURE

PART A a. Appearance of compound

1. Identify the colour and shape of the solid iron (III) chloride (A), lead (II) nitrate (B) and
calcium carbonate (C).

b. Heating test
1. Put half spatula of solid compound in boiling tube. Heat the compound using Bunsen
burner (about 10 to 15 minutes). If a gas is given off, note the colour and odour of
the gas.
(Note: Hold the boiling tube at an angle, as shown below and point it away from
yourself and other people.)

c. Solubility with water

1. Place half spatula of compound in 2 ml of distilled water in boiling tube and shake.
2. If the compound does not dissolve, add another 3 ml of distilled water. Shake and
stir the mixture.
3. If the compound is soluble this amount will dissolve after considerable stirring. If the
compound is moderately soluble, some of this amount will dissolve. If the compound
is insoluble, even a very small amount will not dissolve

d. Reaction with nitric acid

1. Put half spatula of solid compound in boiling tube. Add 15 ml of nitric acid (1M) to
the compound and observe any reaction that occurs (Set up the apparatus as
shown below).
2. Don’t throw the mixture. Keep the solution for the reaction with sodium hydroxide
and ammonia.

13
 SKT3033: Basic Inorganic Chemistry

e. Reaction with sodium hydroxide

1. Add 1 M of solution NaOH drop wise to the solution (used solution from test tube in
reaction with nitric acid), stir or shake the solution until precipitate form. Observe
any reactions happen.

14
 SKT3033: Basic Inorganic Chemistry

f. Reaction with ammonia

1. Add 3 M of solution NH3 drop wise to the solution (used solution from test tube in
reaction with sodium hydroxide), stir or shake the solution and observe any
reaction. Observe any reactions happen.

PART B:
Predict the ions that present in the UNKNOWN compounds.

i. Cation Identification Test

Compound D

1. Acidify half spatula of compound D with 2 mL of acetic acid (6 M).

2. Add 1 mL of 0.2 M of sodium acetate solution.
3. Add 1 mL of dimethylglyoxime solution and add another 1 mL drop wise. Observe any
changes colour.

Compound E
1. Acidify half spatula of compound E with 5 mL HNO 3 (3 M). Test the solution with litmus
paper.
2. Add 0.1 M NH4SCN solution drop wise. Observe any changes colour.

ii. Anion Identification Test

Compound F
1. Acidify half spatula of compound F with 5 mL HNO 3 (3 M) in the test tube. Test the solution
with litmus paper.
2. Pour half of the above solution in the centrifuge tube. Add several drops of 0.1 M AgNO 3
until white precipitate forms. Centrifuge and remove the supernatant.
3. Add drop wise 6 M NH3 to the precipitate with stirring until dissolved.
4. Add 6 M HNO3 to the solution until white precipitate forms.

Compound G

1. Acidify half spatula of compound G with 10 mL H2SO4 (2 M) in the boiling tube.

2. Dissolve one-half spatula full of solid FeSO4.7H2O.
3. Cool the solution with some ice for 20 minutes.
4. Add carefully 0.5 mL of concentrated H2SO4 by allowing it to flow down the side of the tilted
test tube.
5. Allow the solution to sit undisturbed for 2 hours so that the sulphuric acid forms a definite
layer.

2.4 REFERENCES

1. Beran, J. A. (2014). Laboratory Manual for Principals of General Chemistry (7th).

Hoboken, NJ: Wiley.
2. Heasley, V. L., Christensen, V. J. & Heasley, G. E. (2013) Chemistry and life in the
laboratory: Experiments. USA: Pearson.
15
 SKT3033: Basic Inorganic Chemistry

2.5 WORKSHEET

PART A a. Appearance of compound

Colour of solid Shape of solid
Iron (III) chloride (A)

Lead (II) nitrate (B)

Calcium carbonate (C)

b. Heating test
Colour of the gas emitted Odour of the gas emitted
Iron (III) chloride (A)

Lead (II) nitrate (B)

Calcium carbonate (C)

c. Solubility with water

Soluble / moderately soluble / insoluble
Iron (III) chloride (A)

Lead (II) nitrate (B)

Calcium carbonate (C)

d. Reaction with nitric acid

Observe any reaction occurs
16
 SKT3033: Basic Inorganic Chemistry

Iron (III) chloride (A)

Lead (II) nitrate (B)

Calcium carbonate (C)

e. Reaction with sodium hydroxide

Observe any reaction occurs
Iron (III) chloride (A)

Lead (II) nitrate (B)

Calcium carbonate (C)

f. Reaction with ammonia

Observe any reaction occurs
Iron (III) chloride (A)

Lead (II) nitrate (B)

Calcium carbonate (C)

PART B Cation Identification Test

Predict the ion that present in the UNKNOWN compound
Compound D

Compound E

17
 SKT3033: Basic Inorganic Chemistry

Anion Identification Test

Predict the ion that present in the UNKNOWN compound
Compound F

Compound G

____________________________ _____________________________
DATE LECTURER’SSIGNATURE/STAMP

18
 SKT3033: Basic Inorganic Chemistry

EXPERIMENT 3

RELATIVE REACTIVITY OF METALS USING SALT SOLUTIONS

3.1 OBJECTIVES

Students should be able to:

● observe the reaction of Zn, Al, Cu and Mg metals on the following salt solutions: ZnSO 4,
AgNO3, CuSO4 and Al2(SO4)3.

● arrange Zn, Al, Cu and Mg metals in the decreasing order of reactivity based on the
above results.

3.2 INTRODUCTION

Metals are elements and are good conductors of heat and electricity. Most metals are
electropositive in nature and the metal atoms lose electrons in chemical reactions to form cations.
The more reactive a metal, the greater tendency it has to form a positive ion in a chemical reaction.
For example:

Na → Na+ + ē

Displacement reactions are very common in metals. They can be used to find out the relative
reactivities of metals. In a displacement reaction, a more reactive metal can displace a less
reactive metal from its salt solution. The reaction is often known as metal displacement reaction.
Some of the commonly used metals have been arranged in the decreasing order of reactivity. This
is known as the reactivity series or activity series. The activity series of metals is an important
concept in chemistry. The activity series of metals is an important tool for predicting the products of
displacement reactions and the reactivity of metals in other reactions. Potassium is the most
reactive metal, while platinum is the least reactive.

The higher the metal in the series, the more reactive it is and the more vigorously it reacts with
water, oxygen and acid. A metal in the activity series can displace any metal below it in the series
from its compound. The elements potassium, sodium, lithium and calcium are very reactive and
they react with cold water to produce hydroxides and hydrogen gas. The elements magnesium,
aluminium and iron are also considered as active metals and they react with steam to produce
oxides and hydrogen gas. The metals above hydrogen are more reactive than hydrogen. These
metals can displace hydrogen from acids or water and liberate hydrogen gas. The metals copper,
silver gold and platinum are less reactive than hydrogen and they do not replace hydrogen from
water or acid.

Apparatus

Spotting tile
Forcep
Zinc metal strip

19
 SKT3033: Basic Inorganic Chemistry

Iron metal strip

Copper metal strip
Magnesium metal strip

Chemicals

Zinc(II) sulfate (ZnSO4, 1.0 M)

Silver(I) nitrate (AgNO3, 1.0 M) Copper(II)
sulfate (CuSO4, 1.0 M)
Aluminium sulfate (Al2(SO4)3, 1.0 M)

3.3 PROCEDURE

PART A: REACTION WITH IRON METAL

1. Using a pipette, transfer 1.0 M solution of ZnSO 4, CuSO4 and Al2(SO4)3 into each dimple
of a spotting tile labelled with ZnSO4, CuSO4 and Al2(SO4)3.
2. Take a strip of cleaned iron metal and cut it into small pieces of suitable size. Always
clean the metallic strips before use with a sand paper.
3. Add ONE (1) piece of iron metal into each dimple of a spotting tile labelled with ZnSO 4,
CuSO4 and Al2(SO4)3.
4. Keep the spotting tile undisturbed in a safe place until the reaction continues. After
some time, note the changes in colour of solutions, appearance of metal surfaces, or
any other changes.

Solutions Metals

Fe

Cu

20
 SKT3033: Basic Inorganic Chemistry

Zn

Mg

PART B: REACTION WITH COPPER METAL

1. Using a pipette, transfer 1.0 M solution of ZnSO 4, AgNO3 and Al2(SO4)3 into each dimple
of a spotting tile labelled with ZnSO4, AgNO3 and Al2(SO4)3.
2. Take a strip of cleaned iron metal and cut it into small pieces of suitable size. Always
clean the metallic strips before use with a sand paper.
3. Add ONE (1) piece of copper metal into each dimple of a spotting tile labelled with
ZnSO4, AgNO3 and Al2(SO4)3.
4. Keep the spotting tile undisturbed in a safe place until the reaction continues. After
some time, note the changes in colour of solutions, appearance of metal surfaces, or
any other changes.

PART C: REACTION WITH ZINC METAL

1. Using a pipette, transfer 1.0 M solution of CuSO 4, AgNO3 and Al2(SO4)3 into each dimple
of a spotting tile labelled with CuSO4, AgNO3 and Al2(SO4)3.
2. Take a strip of cleaned iron metal and cut it into small pieces of suitable size. Always
clean the metallic strips before use with a sand paper.
3. Add ONE (1) piece of zinc metal into each dimple of a spotting tile labelled with CuSO 4,
AgNO3 and Al2(SO4)3.
4. Keep the spotting tile undisturbed in a safe place until the reaction continues. After
some time, note the changes in colour of solutions, appearance of metal surfaces, or
any other changes.

PART D: REACTION WITH MAGNESIUM METAL

1. Using a pipette, transfer 1.0 M solution of ZnSO4, CuSO4 and AgNO3 into each dimple of
a spotting tile labelled with ZnSO4, CuSO4 and AgNO3.
2. Take a strip of cleaned iron metal and cut it into small pieces of suitable size. Always
clean the metallic strips before use with a sand paper.
3. Add ONE (1) piece of magnesium metal into each dimple of a spotting tile labelled with
ZnSO4, CuSO4 and AgNO3.
4. Keep the spotting tile undisturbed in a safe place until the reaction continues. After
some time, note the changes in colour of solutions, appearance of metal surfaces, or
any other changes.

3.4 REFERENCES

3. Beran, J. A. (2014). Laboratory Manual for Principals of General Chemistry (7th).

Hoboken, NJ: Wiley.
21
 SKT3033: Basic Inorganic Chemistry

4. Heasley, V. L., Christensen, V. J. & Heasley, G. E. (2013) Chemistry and life in the
laboratory: Experiments. USA: Pearson.

3.5 WORKSHEET
Metal Salt Note any changes in the colour of solutions, Inference
solution the look of metal surfaces, or any other
changes after reaction.
Iron ZnSO4

CuSO4

Al2(SO4)3

Copper ZnSO4

AgNO3

Al2(SO4)3

Zinc CuSO4
22
 SKT3033: Basic Inorganic Chemistry

AgNO3

Al2(SO4)3

Magnesium ZnSO4

CuSO4

AgNO3

____________________ _____________________________
DATE LECTURER’S SIGNATURE/STAMP
EXPERIMENT 4

PROPERTIES OF HALOGEN

23
 SKT3033: Basic Inorganic Chemistry

4.1 OBJECTIVES

Students should be able to:

● compare the solubility and colours of the halogens in water and non-aqueous solvents
● explain the displacement reactions

4.2 INTRODUCTION

Halogens are the elements of Group VII that exist as covalently bonded diatomic molecules. As the
group is descended, physical state of the elements moving from gas to liquid to solid due to
strengthening of Van der Waals’ forces effect of increasing relative molecular mass.

Halogen Colour Physical state Melting point / OC Boiling point / OC

Fluorine Yellow Gas -220 -188
Chlorine Yellow-green Gas -101 -35
Bromine Red-brown Liquid -7 59
Iodine Grey-black Solid 114 183

Halogens are the most reactive non-metals elements and exhibit good solubility in non-polar
solvents compare in water. Still, chlorine will form a mixture of two acids named hydrochloric acid,
HCl and chloric(I) acid, HClO which contains chlorate(I) ions when reacts with water. This is an
example of disproportionation as the chlorine is both oxidised to chloric(I) acid and reduced to
hydrochloric acid.

Cl2(g) + H2O(l) → HCl(aq) + HClO(aq)

Apparatus

Eye protection
Test-tube rack
Test tubes
Cork / rubber septa Pipettes
Graduated cylinder Spotting
tiles
pH paper

Chemicals
Cyclohexane or hexane (any non-polar solvent)
Liquid Chlorine, 0.1% (w/v) Harmful
Liquid Bromine, 0.1 % (w/v) Harmful Liquid
Iodine, 0.1 M
Potassium chloride
Potassium bromide
Potassium iodide

24
 SKT3033: Basic Inorganic Chemistry

4.3 PROCEDURE PART A: Solubility of Halogens

1. Prepare six clean test tubes.

2. Fill two test tube with 2 mL of chlorine water. Test the solution with pH paper.
3. Fill two test tube with 2 mL of bromine water. Test the solution with pH paper.
4. Fill two test tube with 2 mL of iodine water. Test the solution with pH paper.
5. Add 4 mL of hydrocarbon solvent to each test tube. Close the test tube with a stopper.
Shake the mixture by inverting the test tube a few times.
6. Allow the two layers to settle. Observe and record the colour of each layer.

PART B: Displacement Reactions

1. Using a pipette put five drops of potassium chloride solution to each of the three dimples in
column 1 (C1) of the spotting tile.
2. Using a pipette put five drops of potassium bromide solution to each of the three dimples in
column 1 (C2) of the spotting tile.
3. Using a pipette put five drops of potassium iodide solution to each of the three dimples in
column 1 (C3) of the spotting tile.
C1 C2 C3

R1

R2

R3

4. Using a pipette, add five drops of chlorine water to each of the three dimples in row 1 (R1)
of the spotting tile. Observe and record any colour changes that take place.
5. Using a pipette, add five drops of bromine water to each of the three dimples in row 1 (R2)
of the spotting tile. Observe and record any colour changes that take place.
6. Using a pipette, add five drops of iodine water to each of the three dimples in row 1 (R3) of
the spotting tile. Observe and record any colour changes that take place.
4.4 REFERENCES

3. Beran, J. A. (2014). Laboratory Manual for Principals of General Chemistry (7 th). Hoboken,
NJ: Wiley.
4. Heasley, V. L., Christensen, V. J. & Heasley, G. E. (2013) Chemistry and life in the
laboratory: Experiments. USA: Pearson.

25
 SKT3033: Basic Inorganic Chemistry

4.5 WORKSHEET

PART A: Solubility of Halogens

Colour BEFORE shaking Colour AFTER shaking with Effect on indicator paper
with hydrocarbon solvent hydrocarbon solvent
Cl2 (aq)

Br2 (aq)

I2 (aq)

PART B: Displacement Reactions

KCl KBr KI

Cl2 (aq)

Br2 (aq)

I2 (aq)

___________________ _____________________________

26
SKT3033: Basic Inorganic Chemistry

DATE LECTURER’S SIGNATURE/STAMP

27
 SKT3033: Basic Inorganic Chemistry

RUBRIC: PRACTICAL

Item 3 5 8 10 Marks
Spelling, many grammar and many errors (>20) in spelling, sporadic errors in spelling, <5 errors in spelling, punctuation,
Punctuation spelling errors made the punctuation, capitalization & punctuation, capitalization & grammar capitalization & grammar
Grammar paper difficult to read. grammar
Format and Any three of list (i – iv) Any two of list (i – iv) Any one of list (i – iv) requirements not i). Report contains appropriate Title.
Style requirements not met. requirements not met met ii). Report contains appropriate sections
(with appropriate headings).
iii). Report contains properly formatted
figures/tables with appropriate numbers
and legends. iv). Methods and results
are written in the past tense. Scientific
names are italicized or underlined.

Introduction Introduction contains Introduction contains very Background information is not Gives sufficient background such that an
very little background little background completely sufficient, or is too educated reader can understand the
information. Introduction information. Hypothesis or verbose (does not focus on justifying reason for performing the experiment.
does not state the purpose of the experiment the experiment), and/or background Connects the experimental goals or
hypothesis or purpose of is in the introduction, but information seems disconnected from methods to previous research (from lab
the experiment. may or may not be clear. the experiment, but the hypothesis or handouts, text, journal articles, etc.).
purpose of the experiment is clearly
Clearly states the hypothesis or purpose
stated. Alternatively, background
of the experiment.
information in sufficient but the
purpose or hypothesis is not clearly
stated

Materials No materials described. Doesn’t provide enough Materials are mentioned but without Materials and amounts are identified.
information of materials to amounts.
represent an experimental.

Methods Written in a way such Lacks appropriate detail for Lacks appropriate detail for one Written with level of detail necessary for
that a classmate could one or two procedures, and procedure or one of the other three a classmate to replicate the experiment.
not replicate the one of the other three requirements is not met. Appropriate subheadings used to divide
experiment. requirements may not be the section. Appropriate rationales given
met. Or the section is written for the methods when necessary.
with sufficient detail but two Written in paragraphs and full sentences,
of the other requirements are
not as numbered lists.
not met.
 SKT3033: Basic Inorganic Chemistry

Results Does not report pertinent Reports sufficient data. Reports all appropriate data. Draws Reports all appropriate data. Tables or
data collected during the Tables and graphs present attention to trends or major findings. Graphs contain sufficient information to
experiment. Tables but might not be stand- be understood outside of the report.

and/or graphs may be alone. Speculations One of the other two requirements is Draws attention to trends or major
omitted. or conclusions may be not met. findings. Does not draw conclusions
included. about the data or speculate about
anything based on the data.

Discussion Interpretation of results Provides some interpretation Provides meaningful interpretation of Provides meaningful interpretation of
is not clearly explained. of results. results. Provides some reasoning for results. Provides scientific reasoning for
negative or unexpected results if unexpected or negative results if
appropriate. One of the other two appropriate
requirements not met.
Conclusion No conclusions are Includes some sort of Includes a conclusion paragraph. Includes a conclusion paragraph.
made based on the conclusions. Draws insufficient/inappropriate Draws appropriate conclusions based on
results conclusions based on the data that the data that are not overly broad.
are not overly broad.
References References are listed in Some references are cited Sufficient and appropriate sources Sufficient and appropriate sources cited.
some format. in the text and listed in a cited. Sources are cited in the text. Sources are cited appropriately in the
References are not cited reference cited section, Most references are formatted text. All references are formatted
in the text. however, formatting is appropriately according to APA appropriately according to APA
incorrect for all references, guidelines. guidelines
or insufficient or
inappropriate references are
used.
Conceptual Several of the major The author has inaccurately Some scientific terms are misused All scientific terms are used accurately
understanding concepts are described one of the major and/or some key background and appropriately. Scientific concepts are
inaccurately described or scientific concepts, and may information necessary to support the well explained. The purpose of the
missing, and/or the have left out some key purpose or conclusions has been left experiment is well justified and the
results are background information. out, but the author still demonstrates conclusions are well supported by the
misinterpreted. However, the conclusions that he/she understands the major experimental evidence
are still well supported by scientific concepts pertinent to the
the experimental evidence. report. The conclusions are well
supported by the experimental
evidence.

Deductions -10 -20 -30 -40 Marks

 SKT3033: Basic Inorganic Chemistry
Lateness <24hr late 24-48h late 48-72h late >72h late

TOTAL = 100 Marks