SKT1013: Introduction To Inorganic Chemistry

LABORATORY MANUAL

SKT 1013
INTRODUCTION TO INORGANIC CHEMISTRY

Department of Chemistry
Faculty of Science and Mathematics
UNIVERSITI PENDIDIKAN SULTAN IDRIS

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SKT1013: Introduction To Inorganic Chemistry

No Experiment Pages

0 Safety Rules and Regulations in Chemistry Laboratory 3

1 Complex Ion of Nickel(II) Chloride 7

2 A Study of Copper (II) complexes with different ligands 10

3 Oxidation States of Manganese 12

4 Preparation of Potassium Tri(oxalate)aluminate(III) trihydrate 15

5 Determination Of Aluminium Metal In Potassium Tris(Oxalato)Aluminate(III) 18

Trihydrate Complex Using Inductively Coupled Plasma Optical Emission
Spectrometry (ICP-OES) Analyser

6 Ligand Replacement Reaction For Synthesis of [Ni(NH3)6]Cl2 21

7 Characterisation of [Ni(NH3)6]Cl2 Using UV-VIS Spectrophotometer 24

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SKT1013: Introduction To Inorganic Chemistry

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.
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.

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SKT1013: Introduction To Inorganic Chemistry

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.

AN EXPERIMENT DONE WELL IS......

AN EXPERIMENT DONE SAFELY

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SKT1013: Introduction To Inorganic Chemistry

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.

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.

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SKT1013: Introduction To Inorganic Chemistry

REFERENCES
List the book, publication or website that you referenced in writing your report. Provide authors,
publisher, date of publication, page number, etc.
*Tips: Follow the standard format for typing a reference:
[1] Little, P., and Cardenas, M., “Use of Studio Methods in the Introductory Engineering Design
Curriculum,” Journal of Engineering Education, Vol. 90, No. 3, 2001, pp. 309-318.
[2] Nunally, J., Psychometric Theory, 2nd ed., New York, N.Y.: McGraw-Hill, 1978.
[3] Lister, B., “Next Generation Studio: A New Model for Interactive Learning,”
www.ciue.rpi.edu/pdfs/nextGenStudio.pdf.

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SKT1013: Introduction To Inorganic Chemistry

EXPERIMENT 1
COMPLEX ION OF NICKEL (II) CHLORIDE

1.1 OBJECTIVE
Upon completion of this experiment, students should be able to:
1. describe a colour change in a complex ion due to ligand substitution

1.2 INTRODUCTION
A metal complex has a central metal surrounded by a set of ligands. Ligand is a molecule, atom
or ion that is bonded directly to a central metal by donating a pair of electron (Figure 1.1). The
atom in the ligand (Lewis bases) that forms the coordinate covalent bond to the central atom is
called the donor atoms, because it donates the electron used in bond formation. So, the ligand
must contain at least one lone pair electron. The metal ion or atom (Lewis acid) is the acceptor
atoms because they accept pairs of electrons from ligand. Complex ions containing transition
metals are usually coloured, whereas the complex ions are not if the metal ions from non-transition
metals. The colour of complex ion can be influenced by some factors such as type of central
metal, oxidation state of metal and type of ligands. In this experiment student will learn the effect
of different ligand on the colour of complex ion formed through ligand substitution. A ligand
substitution (exchange) reaction is a reaction in which one ligand in a complex ion is replaced by
another ligand. Therefore, this experiment describes some common ligand substitution
(exchange) reactions involving nickel(II) chloride (NiCl2) as complex metal ion. Different ligands
such as NH3, en, CN- and EDTA generally used in ligand substitution reaction.

Figure 1.1 Ligand is bonded directly to a central metal by donating a pair of electron

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SKT1013: Introduction To Inorganic Chemistry

Chemicals

Nickel(II) chloride hydrate, NiCl2.6H2O (0.1 M)

Concentrated ammonia solution, NH3
Ethylenediamine (en), C2H4(NH2)2
Potassium cyanide, KCN (1.0 M)
Ethyldiaminetetraacetate (EDTA), C10H16N2O8

Apparatus
Test tube
Graduated cylinder
Dropper
Test tube rack

1.3 PROCEDURE
1. Put 3 mL of NiCl2.6H2O in five (5) test tubes.
2. Add 3 mL of concentrated NH3 to test tube-2.
3. Add 3 mL of en to test tube-3.
4. Add 3 mL of EDTA to test tube-4.
5. Add 3 mL of KCN to test tube-5. (CAUTION: KCN is poisonous. Wash the skin thoroughly
and immediately after contact)
6. Add an excess of the ligand-containing solution if any precipitate forms, especially for CN-
ligand.
7. Compare the appearance of the test solutions with controlled test tube.

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SKT1013: Introduction To Inorganic Chemistry

WORKSHEET EXPERIMENT 1
Test Tube Observation
1 0.1 M NiCl2.6H2O (controlled)
2 0.1 M NiCl2.6H2O + concentrated NH3
3 0.1 M NiCl2.6H2O + C2H4(NH2)2
4 NiCl2.6H2O + C10H16N2O8
5 NiCl2.6H2O + KCN

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DATE LECTURER’S SIGNATURE/STAMP

REFERENCES
1. Gispert, J. R. (2008). Coordination Chemistry. John Wiley & Sons.
2. Weller, M., Overton, T., Rourke, J., & Armstrong, F. A. (2014). Inorganic chemistry.
Oxford: Oxford University Press.
3. https://www.chemguide.co.uk/inorganic/complexions/ligandexch.html

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SKT1013: Introduction To Inorganic Chemistry

EXPERIMENT 2
A STUDY OF COPPER (II) COMPLEXES WITH DIFFERENT LIGANDS

2.1 OBJECTIVE
Upon completion of this experiment, students should be able to:
1. Observe a various colour change in a complex ion due to ligand substitution.

2.2 INTRODUCTION
Anhydrous copper sulphate is a white powder, while its pentahydrate compound (CuSO4·5H2O),
formed in bright blue solid. When dissolved in water it dissociates to positively charges of copper
ion and negatively charges of sulphate ion. Copper ions being attracted to the oxygen atom of
water molecule due to the polarity of water to give hexaaquocopper(II) ion, [Cu(H2O)6]2+ which
has octahedral molecular geometry. The water molecules act as ligand to provide lone pair
electrons to copper ion. The complex ion produced blue colour due to the existence of partially
filled d sublevel electrons (Cu2+: 3d9) which absorb visible wavelengths and move to slightly higher
energy d orbitals. In this experiment student will investigate whether there is a change of colour if
using a different ligand to replace the existing ligand in the coordination sphere of CuSO 4·5H2O
through ligand substitution reactions.

Chemicals
Copper sulphate, CuSO4.5H2O (0.025 M)
Concentrated ammonia solution, NH3
Concentrated hydrochloric acid, HCl
Ethylenediamine (en), C2H4 (NH2)2
Potassium cyanide, KCN (1.0 M)
Ethyldiaminetetraacetate (EDTA), C10H16N2O8

Apparatus
Test tube
Graduated cylinder
Dropper
Test tube rack

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SKT1013: Introduction To Inorganic Chemistry

2.3 PROCEDURE
1. Put 3 mL of 0.025 M CuSO4.5H2O in six (6) test tubes.
2. Add 3 mL of HCl to test tube-2. (CAUTION: Handle carefully, does not allow concentrated
HCl to contact skin or clothing. Flush immediately with water if contact with skin)
3. Add 3 mL of NH3 to test tube-3.
4. Add 3 ml of en to test tube-4.
5. Add 3 mL of EDTA to test tube-5.
6. Add 3 mL of 1.0 M KCN to test tube-6.
7. Compare the appearance of the test solutions with controlled test tube.

WORKSHEET EXPERIMENT 2
Test Tube Observation
1 0.025 M CuSO4.5H2O
2 0.025 M CuSO4.5H2O + HCl
3 0.025 M CuSO4.5H2O + NH3
4 0.025 M CuSO4.5H2O + C2H4(NH2)2
5 0.025 M CuSO4.5H2O + C10H16N2O8
6 0.025 M CuSO4.5H2O + KCN

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DATE LECTURER’S SIGNATURE/STAMP

REFERENCES

1. Jespersen, N. D., Hyslop, A., & Brady, J. E. (2015). Chemistry: The molecular nature of
matter and change. Hoboken, NJ: Wiley.
2. Miessler, G. L., Fischer, P. J. & Tarr, D. A. (2014). Inorganic Chemistry (5th). Essex,
England: Pearson International Ed.

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SKT1013: Introduction To Inorganic Chemistry

EXPERIMENT 3
OXIDATION STATES OF MANGANESE

3.1 OBJECTIVE
Upon completion of this experiment, students should be able to:
1. Observe the colour of manganese complexes with different oxidation state.

3.2 INTRODUCTION
Oxidation states is the physical state of the element and equivalent to its oxidation number. One
of the main characteristics of transition metals is they have variable oxidation states. This variable
of oxidation number will give different of partially filled d sublevel electrons for its central metal
ion. Thus the colour of complex compounds can be also influenced by its oxidation state of metal
ion. For instances, manganese has several possible oxidation states from +2 to +7. Thus, the
common oxidation states are +2, +4, and +7, while the less common are +3, +5, and +6. Each
oxidation state has different colour. Mn2+ has a pale pink colour while Mn+7 is purple in colour.

Element Oxidation States

Sc +3

Ti +2 +3 +4

V +2 +3 +4 +5

Cr +2 +3 +4 +5 +6

Mn +2 +3 +4 +5 +6 +7

Fe +2 +3 +4 +5 +6

Co +2 +3 +4

Ni +2 +3

Cu +1 +2 +3

Zn +2

Table 3.1 The most common oxidation states for first row transition metals

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SKT1013: Introduction To Inorganic Chemistry

Chemicals
Sulphuric acid, H2SO4 (3.0 M)
Sodium hydroxide, NaOH (2.0 M)
Potassium permanganate, KMnO4 (0.01 M)
Sodium bisulfite, NaHSO3 (0.02 M)
Sodium bisulfate, NaHSO4 (0.02 M)

Apparatus
Test tube
Graduated cylinder
Test tube rack

3.3 PROCEDURE
1. Put 1 mL of KMnO4 to four (4) test tubes.
2. Add 1 mL of NaOH to test tube-2. Then, add NaHSO3 (7 x 1 mL). Observe the colour
changes.
3. Add 1 mL of H2SO4 to test tube-3. Then, add NaHSO3 (7 x 1 mL). Observe the colour
changes.
4. Add NaHSO3 (7 x 1 mL) to test tube-4. Observe the colour changes.
5. Add 1 mL of NaOH to test tube-5. Then, add NaHSO4 (7 x 1 mL). Observe the colour
changes.
6. Add 1 mL of H2SO4 to test tube-6. Then, add NaHSO4 (7 x 1 mL). Observe the colour
changes.
7. Add NaHSO4 (7 x 1 mL) to test tube-7. Observe the colour changes.

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SKT1013: Introduction To Inorganic Chemistry

WORKSHEET EXPERIMENT 3
Test Tube Observation
1 KMnO4
2 KMnO4 + NaOH + NaHSO3
3 KMnO4 + H2SO4 + NaHSO3
4 KMnO4 + NaHSO3
5 KMnO4 + NaOH + NaHSO4
6 KMnO4 + H2SO4 + NaHSO4
7 KMnO4 + NaHSO4

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DATE LECTURER’S SIGNATURE/STAMP

REFERENCES
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.
3. Mishra, A. K. (2012). Transition metals: Characteristics, properties and uses.
Hauppauge, NY: Nova Science.

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SKT1013: Introduction To Inorganic Chemistry

EXPERIMENT 4
PREPARATION OF POTASSIUM TRIS (OXALATO) ALUMINATE (III) TRIHYDRATE

4.1 OBJECTIVE
Upon completion of this experiment, students should be able to:
1. synthesise potassium tris(oxalato)aluminate(III) trihydrate

4.2 INTRODUCTION
Aluminium (Al) is located in p-block with principal oxidation state of 3+.The Al surface is protected
from being oxidise by a layer called aluminium oxide (Al2O3). When Al2O3 dissolves in excess
hydroxide, the aluminium hydroxide, [Al(OH)4]- ion is formed (eq. 1). The addition of oxalic acid,
(H2C2O4) will produce the dioxalatoaluminate ion, [Al(C2O4)]3- and subsequently neutralise the
excess hydroxide ion, OH-. The [Al(C2O4)]3- will be precipitated as potassium salt by addition of
ethanol.
Al2O3 + 2OH- + 3H2O → 2[Al(OH)4]- (eq. 1)
Al + 3KOH + 3H2C2O4.2H2O → K3[Al(C2O4)3].3H2O + 6H2O + 3/2H2 (eq. 2)

Chemicals
Potassium hydroxide, KOH
Oxalic acid dihydrate, H2C2O4.2H2O
Ethanol
Acetone
Distilled Water
Ice

Apparatus
Aluminium foil
Beaker (250 mL)
Graduated cylinder
Filter paper
Watch glass
Hot plate

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SKT1013: Introduction To Inorganic Chemistry

Glass rod
Buchner funnel

4.3 PROCEDURE
1. Weigh 0.50 g aluminium foil that been cut to 1 cm2 and put into a 250 mL beaker.
2. Add 30 mL water and 15 mL 4.0 M KOH into the beaker and stir vigorously.
3. Stir until most of the aluminium foil are dissolved, then heat the solution to dissolve any
unreacted aluminium.
4. Add gradually 8.0 g H2C2O4.2H2O to the hot solution.
5. Filter the hot solution using gravity filtration (Figure 4.1) with fluted filter paper and transfer
the filtrate to a 250 mL Erlenmeyer flask.
6. Put the Erlenmeyer flask containing the filtrate in an ice bath and cool it to 10C.
5. Add 20 mL ethanol and leave the Erlenmeyer flask in ice bath until crystallisation process
complete around 15-20 minutes.
6. Recover the product by suction filtration (Figure 4.2).
7. Wash with 10 mL acetone, and allow the product to air dry.
8. Weigh the product and record.

Figure 4.1 Gravity filtration Figure 4.2 Vacuum filtration

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SKT1013: Introduction To Inorganic Chemistry

WORKSHEET EXPERIMENT 4
Mass of Aluminium (g)
Volume of water (mL)
Volume of KOH (mL)
Mass of oxalic acid dehydrate (g)
Mass of filter paper (g)
Mass of filter paper + K3[Al(C2O4)3].3H2O (g)
Mass of K3[Al(C2O4)3].3H2O (g)

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DATE LECTURER’S SIGNATURE/STAMP

REFERENCES
1. McCormick, A. L. (2019). Aluminum. New York, NY: Enslow Publishing.
2. Dingle, A. (2018). Periodic table. London: Dorling Kindersley.
3. Jolivet, J., Henry, M., Livage, J., & Bescher, E. P. (2003). Metal oxide chemistry and
synthesis: From solution to solid state. Chichester: John Wiley.

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SKT1013: Introduction To Inorganic Chemistry

EXPERIMENT 5
DETERMINATION OF ALUMINIUM METAL IN POTASSIUM TRIS(OXALATO)ALUMINATE(III)
TRIHYDRATE COMPLEX USING INDUCTIVELY COUPLED PLASMA OPTICAL EMISSION
SPECTROMETRY (ICP-OES) ANALYSER

5.1 OBJECTIVE
Upon completion of this experiment, students should be able to:
1. Identify and quantify the aluminium metal in potassium tris(oxalato)aluminate(III)
trihydrate, K[Al(C2O4)3].3H2O complex

5.2 INTRODUCTION
Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES), is one method of optical
emission spectrometry with a dynamic linear range and moderate detection limits. The ICP source
is made by ionising argon gas. The sample is dissociated into its constituent atoms or ions and
subsequently being excites to high energy level. Emission rays that correspond to the photon
wavelength are released when the excited atoms return to low energy level. The position of the
photon rays will identify the type of element while the rays' intensity determines the content of
each element.
Chemicals
Potassium tris(oxalato)aluminate(III) trihydrate complex (synthesised in Experiment 4)
Concentrated nitric acid, HNO3
Concentrated sulphuric acid, H2SO4
Distilled water

Apparatus
Volumetric flask
Beaker
Dropper
Hot plate

5.3 PROCEDURE
1. Weigh 0.125 g K3[Al(C2O4)3].3H2O (from Experiment 4) and put into a 25 mL beaker.
2. Digest the complex with 10 mL concentrated HNO3 and heat the solution.
3. Add 10 mL of concentrated sulphuric acid when brown gas has ceased.

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SKT1013: Introduction To Inorganic Chemistry

4. Continue heating until brown gas is completely ceased and become clear solution.
5. Cool the solution and transfer to 100 mL volumetric flask.
6. Prepare the stock solution by adding distilled water until calibration mark.
7. Pipette 0.4 mL stock solution and transfer into 10 mL volumetric flask to prepare a diluted
solution. Add distilled water until calibration mark.
8. Calculate experimental mass of aluminium metal according to the formula:
𝑐𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛 𝑜𝑓 𝐴𝑙(𝑚𝑔𝑑𝑚−3 ) x Volume of diluted sample, (𝑑𝑚−3 ) x 𝑑 (𝑑𝑖𝑙𝑢𝑡𝑖𝑜𝑛 𝑓𝑎𝑐𝑡𝑜𝑟)
𝑚𝑎𝑠𝑠 𝑜𝑓 𝑡ℎ𝑒 𝑚𝑒𝑡𝑎𝑙 𝑖𝑛 𝑠𝑎𝑚𝑝𝑙𝑒 =
𝑀𝑎𝑠𝑠 𝑜𝑓 𝑠𝑎𝑚𝑝𝑙𝑒 (𝑚𝑔)

WORKSHEET EXPERIMENT 5
A. PREPARATION OF STOCK SOLUTION TRIS(OXALATO)ALUMINATE(III) TRIHYDRATE
Weight of K2[Al(C2O4)3].3H2O (g)
Volume of solution (HNO3 + H2SO4 + H2O), (mL)
Molarity of K2[Al(C2O4)3].3H2O (M)

B. PREPARATION OF DILUTED TRIS(OXALATO)ALUMINATE(III) TRIHYDRATE

M1: Molarity of K2[Al(C2O4)3].3H2O before dilution
V1: Volume of pipetted stock solution
V2: Volume of volumetric flask (mL)
M2: Molarity of diluted K2[Al(C2O4)3].3H2O

d: Dilution factor

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SKT1013: Introduction To Inorganic Chemistry

C. DETERMINATION MASS (g) OF ALUMINIUM IN TRIS (OXALATO) ALUMINATE (III)

TRIHYDRATE
𝑚𝑎𝑠𝑠 𝑜𝑓 𝑡ℎ𝑒 𝑚𝑒𝑡𝑎𝑙 𝑖𝑛 𝑠𝑎𝑚𝑝𝑙𝑒
𝑐𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛 𝑜𝑓 𝐴𝑙(𝑚𝑔𝑑𝑚 −3 ) x Volume of diluted sample, (𝑑𝑚−3 )x 𝑑 (𝑑𝑖𝑙𝑢𝑡𝑖𝑜𝑛 𝑓𝑎𝑐𝑡𝑜𝑟)
=
𝑀𝑎𝑠𝑠 𝑜𝑓 𝑠𝑎𝑚𝑝𝑙𝑒 (𝑚𝑔)

Concentration of aluminium ion (ppm)

from ICP-OES
*ppm = mgdm-3
Mass (g) of Aluminium ion in
K[Al(C2O4)3].3H2O

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DATE LECTURER’S SIGNATURE/STAMP

REFERENCES
1. Scott, R. A., & Lukehart, C. M. (2007). Applications of physical methods to inorganic and
bioinorganic chemistry. Hoboken, NJ: Wiley.
2. Nölte, J. (2003). ICP emission spectrometry: A practical guide. Weinheim: Wiley-VCH.

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EXPERIMENT 6
LIGAND REPLACEMENT REACTION FOR SYNTHESIS OF [Ni(NH3)6]Cl2

6.1 OBJECTIVE
Upon completion of this experiment, students should be able to:
1. synthesise hexaamminenickel(II) chloride

6.2 INTRODUCTION
In metal salt aqueous solution, the water molecules act as ligand to form bond to the metal ions
with octahedral molecular geometry bearing six ligands which are symmetrically arranged around
the central atom. The complexes will produces different colours depends on the central metal,
oxidation state of central metal and types of ligand used. For instances, when water molecules
bind to different central metal, the colour of complexes varies from pink [Co(H2O)6]2+, green
[Ni(H2O)6]2+ and pale-blue [Cu(H2O)6]2+. By addition of ammonia into the complex solutions, a
series of substitution reactions occur in which water molecules are replaced by ammonia
molecules.
Below is an example equation of common substitution reaction when the addition of NH3 into
octahedral complex ion solution. The H2O molecule will be replaced by NH3 ligand (eq.1) until all
the H2O molecules are replaced by NH3 ligands (eq. 2):
[M(H2O)6]2+ + NH3 → [M(H2O)5(NH3)]2+ + H2O (1)
[M(H2O)(NH3)5]2+ + NH3 → [M(NH3)6]2+ + H2O (2)

Chemicals
Nickel (II) chloride hydrate, NiCl2.6H2O
Concentrated aqueous ammonia, NH3
Ethanol (95%)
Distilled water
Ice
Apparatus
Graduated cylinder
Erlenmeyer flask
Filter paper
Buchner funnel

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SKT1013: Introduction To Inorganic Chemistry

6.3 PROCEDURE
1. Dissolve 6 g NiCl2.6H2O in 10 mL warm water.
2. Add 12.5 mL concentrated aqueous NH3 to NiCl2.6H2O solution. Leave the solution in ice
bath until the crystal formed.
3. Filter the product by suction filtration and wash the filtrate with 5 mL ethanol twice (2 x 5
mL). Air dry the product.
4. Weigh the product and record.
5. Find the % yield of product.
6. Put a small amount of product into a test tube and test the solubility in water.
7. Keep the product in a vial for UV-vis characterisation (Experiment 7).

WORKSHEET EXPERIMENT 6

Mass of NiCl2.6H2O (g)

Volume of H2O (mL)
Volume of NH3(conc.) (mL)
Mass of filter paper (g)
Mass of filter paper +
[Ni(NH3)6]Cl2 (g)
% yield of [Ni(NH3)6]Cl2 𝐴𝑐𝑡𝑢𝑎𝑙 𝑦𝑖𝑒𝑙𝑑 (𝑔)
%𝑦𝑖𝑒𝑙𝑑 = 𝑥 100%
Actual yield: Amount of product 𝑇ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑦𝑖𝑒𝑙𝑑 (𝑔)
obtained from a chemical reaction
Theoretical yield: Amount of
product obtained from the
stoichiometric equation, using the
limiting reactant to determine
product

Solubility in water

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REFERENCES
1. Weller, M., Overton, T., Rourke, J., & Armstrong, F.A. (2014). Inorganic chemistry.
Oxford: Oxford University Press.
2. Bajia, S. C. (2013). Synthesis and characterization of some group 9 and 10 metal
complexes: with ligands containing group 16 elements. Riga Latvia: Scholar’s Press.

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SKT1013: Introduction To Inorganic Chemistry

EXPERIMENT 7
CHARACTERISATION OF [Ni(NH3)6]Cl2 USING UV-VIS SPECTROPHOTOMETER

7.1 OBJECTIVE
Upon completion of this experiment, students should be able to:
1. analyse the hexaamminenickel(II) chloride using UV-Visible spectroscopy

7.2 INTRODUCTION
Ultraviolet-visible spectroscopy (UV/Vis) can be define as absorption spectroscopy in the
ultraviolet-visible spectral region. This technique uses light in the visible (380 – 700 nm) and near-
UV (100 – 400 nm) and near-infrared (NIR) (750 – 950 nm) ranges. UV/Vis spectrophotometer is
used in the quantitative determination of concentration of the analyte in solution. According to
Beer’s Law, the absorbance changes with concentration. The absorbance is directly proportional
to the concentration of analyte and the cuvette path length. Thus, for a fixed cuvette path length,
UV/Vis spectroscopy can be used to determine the concentration of the analyte by plotting a
calibration curve.
A=cLԑ
A = absorbance
c = concentration of analyte in mol dm-3
L = length in of cuvette (1 cm)
ԑ = extinction coefficient in L mol-1 cm-1
A plot of ԑ (or A with L and c specified) versus wavelength () is known as absorption spectrum.
The spectrum shows wavelengths of light that are absorbed by analyte.

Figure 7.1 Absorption spectra of 5,15-di(4-aminophenyl)-10,20-diphenylporphyrinatozinc(II)

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SKT1013: Introduction To Inorganic Chemistry

Chemicals
Hexaamminenickel(II) chloride, [Ni(NH3)6]Cl2 (from experiment 6)
Distilled water
Apparatus
Volumetric flask
Beaker
Dropper

7.3 PROCEDURE
1. Prepare a solution of 0.01 M hexaamminenickel(II) chloride.
2. Record the data.

WORKSHEET EXPERIMENT 7
A. PREPARATION OF 0.01 M HEXAAMMINENICKEL (II) CHLORIDE
Molarity of [Ni(NH3)6]Cl2 (M)
Volume of Volumetric flask (mL)
Mole of [Ni(NH3)6]Cl2 (mol)
Molar mass of [Ni(NH3)6]Cl2 (gmol-1)
Mass of [Ni(NH3)6]Cl2 (g)

B. Electronic Spectrum of NH3 and [Ni(NH3)6]Cl2

[Ni(NH3)6]Cl2
Wavelength (nm) Absorbance

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SKT1013: Introduction To Inorganic Chemistry

REFERENCES

1. Jackson, T., & Best, A. (2017). The periodic table: A visual guide to the elements.
London: Aurum Press.
2. Granger, R. A., & Yochum, H. (2016). Instrumental Analysis. Kettering: Oxford University
Press USA.
3. Mustafar, S., Wu, K., Toyoda, R., Takada, K., Maeda, H., Miyachi, M., Sakamoto, R. &
Nishihara, H. (2016). Electrochemical fabrication of one-dimensional porphyrinic wires
on electrodes. Inorganic Chemistry Frontiers,3(3), 370-375.
4. Lampman, G. M. (2010). Spectroscopy. Australia: Brooks/Cole Cengage Learning.

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