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 9

3 Oxidation States of Manganese 11

4 Preparation of Potassium Tri(oxalate)aluminate(III) trihydrate 13

5 Determination Of Aluminium Metal In Potassium Tris(Oxalato)Aluminate(III) 15

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

6 Ligand Replacement Reaction For Synthesis of [Ni(NH3)6]Cl2 17

7 Characterisation of [Ni(NH3)6]Cl2 Using UV-VIS Spectrophotometer 19

8 Synthesis of Copper Oxalate Complex KaCub(C2O4)c.2H2O 21

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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 transition metal complex has a central metal ion or atom that bound to other atoms or
molecules. The bound molecules are called 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).

These entities can function as ligands

since they possess lone (nonbonding)
pairs of electrons.

Lewis bases can approach and

subsequently ‘coordinate’ to transition
metal cations via the participation of
nonbonding electron pairs. Electron
deficient transition metal cations are
strong Lewis acids.

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

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.
The anhydrous salt of nickel(II) chloride is yellow, but the more familiar hydrate NiCl2·6H2O is
green. Nickel(II) chlorides are deliquescent, absorbing moisture from the air to form a solution.
In addition, nickel(II) chloride solutions are acidic, with a pH of around 4 due to the hydrolysis of
the Ni2+ ion.

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SKT1013: Introduction To Inorganic Chemistry

Chemicals
Nickel(II) chloride hydrate, NiCl2.6H2O (0.1M)
Concentrated ammonia solution, NH3
Ethylenediamine (en)
Potassium cyanide, KCN (1.0M)
Ethyldiaminetetraacetate (EDTA)

Apparatus
Test tube
Graduated cylinder
Dropper
Test tube rack

1.3 PROCEDURE
1. Place 5 mL of NiCl2.6H2O in each of five (5) test tubes.
2. Add 5 mL of concentrated NH3 in the first test tube.
3. Add 5 mL of ethylenediamine in the second test tube.
4. Add 5 mL of EDTA in the third test tube.
5. Add 5 mL of KCN in the fourth test tube. (CAUTION: KCN is poisonous. Wash the skin
thoroughly and immediately after contact)
6. If any precipitate forms in any of the solutions, add an excess of the ligand-containing
solution; this is especially true for CN - ligand. Compare the appearance of the test
solution with that in the fifth test tube which contains only NiCl2.6H2O.

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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
Copper(II) sulphate, also known as cupric sulphate is the inorganic compound with the chemical
formula CuSO4(H2O)x, where x can range from 0 to 5. The pentahydrate (x = 5) is the most
common form. The pentahydrate (CuSO4·5H2O), the most commonly encountered salt, is bright
blue. It exothermically dissolves in water to give the aqua complex [Cu(H2O)6]2+, which
has octahedral molecular geometry. The structure of the solid pentahydrate reveals a polymeric
structure wherein copper is again octahedral but bound to four water ligands. The Cu(II)(H 2O)4
centres are interconnected by sulphate anions to form chains. Anhydrous copper sulphate is a
white powder. The pentahydrate is used as a fungicide, algaecide and herbicide. It is sometimes
a precursor in the manufacture of other copper compounds and is useful as a mordant in textile
dyeing and as a wood preservative. The compound is employed in a wide variety of ways, from
tanning leather to toning photographs. It is available commercially in relatively high purity as a
root killer for use in sewer pipes.

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

Apparatus
Test tube
Graduated cylinder
Dropper

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SKT1013: Introduction To Inorganic Chemistry

Test tube rack

2.3 PROCEDURE
1. Place 5 mL of 0.025 M CuSO4.5H2O in each of six (6) test tubes.
2. Add 5 mL of hydrochloric acid, HCl in the first test tube. (CAUTION: Handle carefully,
does not allow concentrated HCl to contact skin or clothing. Flush immediately with
water if contact with skin)
3. Add 5 mL of ammonia in the second test tube.
4. Add 5 ml of ethylenediamine in the third test tube.
5. Add 5 mL of EDTA in the fourth test tube.
6. Add 5 mL of 1.0M KCN in the fifth test tube.
7. Compare the colour changes in each test tube with the colour of solution in the sixth test
tube which contains only CuSO4.5H2O.

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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. illustrate the colours of several oxidation state of manganese

3.2 INTRODUCTION
Atoms of some elements, like manganese, have many possible oxidation states. Oxidation-
reduction reactions lead to changes in the oxidation state. In its compounds, manganese
exhibits oxidation states from +2 to +7. The common oxidation states are +2, +4, and +7, but
the less common +3, +5, and +6 states are easily prepared. In addition, manganese which is in
the middle of the period, has the highest number of oxidation states, and indeed the highest
oxidation state in the whole period since it has five unpaired electrons (Table 3.1).

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

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SKT1013: Introduction To Inorganic Chemistry

Chemicals
H2SO4 sulphuric acid (3.0 M)
NaOH sodium hydroxide (2.0 M)
KMnO4 potassium permanganate (0.01 M)
NaHSO3 sodium bisulfite (0.02 M)
NaHSO4 sodium bisulfate (0.02 M)

Apparatus
Test tube
Graduated cylinder
Test tube rack

3.3 PROCEDURE
1. Place 1 mL of KMnO4 in each of 4 test tubes.
2. Add 1 mL of NaOH to test tube 2. Then, add NaHSO 3 (5 x 1 mL) while stirring with glass
rod until there is evidence of a reaction. Note and record the evidence for reaction.
3. Add 1 mL of H2SO4 to test tube 3. Then, add NaHSO3 (5 x 1 mL) while stirring with glass
rod until there is evidence of a reaction. Note and record the evidence for reaction.
4. Add NaHSO3 (5 x 1 mL) to test tube 4, while stirring with glass rod until there is evidence
of a reaction. Note and record the evidence for reaction.
5. Predict the effect of replacing NaHSO3 with NaHSO4. Test the prediction.

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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 metal develops a layer of aluminium oxide that will protect the metal surface from
oxidising. Therefore, in this experiment the oxide coating is dissolved in excess hydroxide,
forming the [Al(OH)4]- ion and the reaction is as follows: Al2O3 + 2OH- + 3H2O → 2[Al(OH)4]-
Next, oxalic acid (H2C2O4) is added, which neutralises the excess hydroxide and
provides a source of the oxalate ion. Lastly, the [Al(C2O4)]3- ion that is produced will be
precipitated as the potassium salt by the addition of ethanol. The overall reaction is represented
by the equation shown: Al + 3KOH + 3H2C2O4.2H2O → K3[Al(C2O4)3].3H2O + 6H2O + 3/2H2

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
Glass rod
Buchner funnel

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SKT1013: Introduction To Inorganic Chemistry

4.3 PROCEDURE
1. Cut aluminium foil into roughly one centimetre squares (1 cm2) and measure
approximately 0.50 grams (this should require 12-14 squares of foil). Record the exact
mass used and transfer them to a beaker (250 mL).
1. Using a graduated cylinder, add 30 mL of water and 15 mL of 4.0 M KOH. If necessary
use a stirring rod to be sure the aluminium foil is immersed.
2. When the reaction has decreased, heat the solution to boiling on a hotplate to dissolve
any unreacted aluminium. Next, add 8.0 grams of oxalic acid dihydrate, in small portions,
to the hot solution.
3. Filter the hot solution through a gravity funnel and transfer the filtrate to a 250 mL beaker
(Figure 4.1).

Figure 4.1 Gravity filtration

4. Place the beaker in an ice bath and cool it to 10C.
5. Add approximately 20 mL of ethanol and leave the beaker in the ice bath until
crystallisation process complete. (this could take up to 15-20 minutes)
6. Recover the product by suction filtration, rinse with 10 mL of acetone, and allow it to air
dry (Figure 4.2).

Figure 4.2 Vacuum filtration

7. Weigh the product and record.

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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 complex

5.2 INTRODUCTION
Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES) is an analytical
technique used for the detection of chemical elements. Principally, the solution to analyse is
conducted by a peristaltic pump though a nebulizer into a spray chamber (Figure 5.1). The
produced aerosol is lead into an argon plasma. Plasma is the fourth state of matter, next to the
solid, liquid and gaseous state. In the ICP-OES the plasma is generated at the end of a quarts
torch by a cooled induction coil through which a high frequency alternate current flows. As a
consequence, an alternate magnetic field is induced which accelerated electrons into a circular
trajectory. Due to collision between the argon atom and the electrons ionization occurs, giving
rise to a stable plasma. The plasma is extremely hot, 6000-7000 K. In the induction zone it can
even reach 10000 K. In the torch desolvation, atomization and ionizations of the sample takes
place. Due to the thermic energy taken up by the electrons, they reach a higher "excited" state.
When the electrons drop back to ground level energy is liberated as light (photons). Each
element has an own characteristic emission spectrum that is measured with a spectrometer.
The light intensity on the wavelength is measured and with the calibration calculated into a
concentration.

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SKT1013: Introduction To Inorganic Chemistry

Figure 5.1 ICP-OES Schematic Diagram

Chemicals
Potassium tris(oxalato)aluminate(III) trihydrate complex (Experiment 4)
Concentrated nitric acid, HNO3
Concentrated sulphuric acid, H2SO4
Distilled water

Apparatus
Volumetric flask (10, 100 mL)
Beaker
Dropper
Hot plate

5.3 PROCEDURE
Part A. Sample Preparation
1. Weigh out 0.125 g of potassium tris(oxalato)aluminate(III) trihydrate complex (from
Experiment 4)
2. Digest the complex with 10 mL of concentrated HNO 3 in a hot plate heater. After the
evolution of the brown nitrogen dioxide gas has ceased, add 10 mL of concentrated
sulphuric acid.
3. Continue heating until all the brown vapours of nitrogen dioxide was completely stopped
and the solution become clear.
4. Cool the solution and dilute with distilled water to 100 mL volumetric flask.
5. From this solution, take 0.4 mL and dilute again to 10 mL volumetric flask.
6. Calculate experimental percentage of aluminium metal according to the formula:

Concentration ( ppm) x 0 . 25
% aluminium = Weight of sample taken( g)

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SKT1013: Introduction To Inorganic Chemistry

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
Many transition metals form octahedral complexes with H2O when in aqueous solution.
Examples include pink [Co(H2O)6]2+, green [Ni(H2O)6]2+ and pale-blue [Cu(H2O)6]2+. Addition
of ammonia to such solutions results in a series substitution reactions in which the water
molecules are replaced by ammonia molecules. For example, when concentrated aqueous
ammonia is added, the green colour changes to the violet colour of the ion.
NH3 ligand displaces H2O in a stepwise method, and each replacement is accompanied
by the evolution of heat. For example, the reaction:
[Ni(H2O)6]2+ + NH3  [Ni(H2O)5(NH3)]2+ + H2O H = -17kJ/mol
is followed by
[Ni(H2O)5(NH3)]2+ + NH3  [Ni(H2O)4(NH3)2]2+ + H2O H = -17kJ/mol
and so on, until all the water molecules are replaced by ammonia molecules.

Chemicals
Nickel (II) chloride hydrate, NiCl2.6H2O
Concentrated aqueous ammonia
Ethanol (95%)
Distilled water
Ice

Apparatus
Graduated cylinder
Beaker
Filter paper

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SKT1013: Introduction To Inorganic Chemistry

Buchner funnel
6.3 PROCEDURE
1. Dissolve 6 grams of NiCl2.6H2O in 10 mL of warm water.
2. Add 12.5 mL of concentrated aqueous ammonia to NiCl 2.6H2O solution. Cool the
resulting dark violet solution in ice bath.
3. Filter the product by suction filtration and wash it twice with 5 mL of ethanol (2 x 5 mL).
Air dries the product.
4. Find the % yield of product.
5. Determine the solubility of product in water.

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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. learn how to analyse the hexaamminenickel(II) chloride using UV-Visible spectroscopy

7.2 INTRODUCTION
Beer's Law is useful in the analysis of solutions containing coloured compounds. The
absorbance of light by a sample depends on the concentration of absorbers, the path length of
the light through the sample, and the extinction coefficient:
A=cLԑ
A = absorbance
c = concentration of absorbing species in mol L-1
L = length in of cuvette (1 cm)
ԑ = extinction coefficient in L mol-1 cm-1
ԑ, is proportionality constant between absorbance and concentration, for a given path length. A
high ԑ value means that a substance absorbs light strongly at the particular wavelength. A plot
of ԑ (or A with L and c specified) versus wavelength () is known as the absorption spectrum of
a substance. This spectrum shows which wavelengths of light are absorbed and which are not.
At a particular wavelength, Beer's Law can be used to relate absorbance and concentration.
Since A = cLԑ, a plot of absorbance vs. concentration, for fixed ԑ and L, will be a straight line
and can determine the concentration of metal complex in a solution you have been prepared.

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SKT1013: Introduction To Inorganic Chemistry

Figure 4.1: Schematic for a UV-Vis spectrophotometer

Chemicals
Hexaamminenickel(II) chloride (from experiment 6)
Distilled water (solvent)

Apparatus
Volumetric flask
Beaker
Dropper

7.3 PROCEDURE
1. Accurately prepare 10.00 ml of 0.01 M solution of product in water.
2. Determine the electronic spectra of the compounds by measuring the absorbance from
350 to 700 nm and molar absorptivity.

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SKT1013: Introduction To Inorganic Chemistry

EXPERIMENT 8
SYNTHESIS OF COPPER OXALATE COMPLEX KaCub(C2O4)c.2H2O

8.1 OBJECTIVES
Upon completion of this experiment, students should be able to:
1. synthesise copper(II) oxalate complex
2. study how to characterise the complex using the redox titrimetric analysis

8.2 INTRODUCTION
Copper, a transition metal, has an electronic configuration of [Ar]3d 10 4s1. Copper exhibits two
common oxidation states, Cu(II) and Cu(I) with electronic configuration of [Ar]3d 9 and [Ar]3d10,
respectively. The Cu(II) uses its one 4s, three 4p and two vacant 4d atomic orbital’s to create a
total of six vacant metal orbital’s (hybridised sp3d2), which can receive as many as 12 electrons
(6 electron pairs) from ligands.
In this experiment, a sample of the hydrate potassium salt of oxalate-copper(II) complex
will be prepared. When a solution of potassium oxalate (K2C2O4) is added to Cu(II) in aqueous
solution, copper oxalate complex will be formed. Each oxalate ligand bonds to the copper
through its two oxygen atoms (each oxygen atom donates a pair of electrons to the copper).
Therefore, oxalate is known as bidentate ligand.
Cu(II) is nearly always determined by reduction to the monovalent state by iodide ion
and followed by titration the liberate iodine with sodium thiosulphate. Oxalate, however, would
interfere and must be determined first. The half reactions involved in this experiment are:
MnO4- + 8H+ + 5e- Mn2+ + 4H2O E0 = 1.51 V
2Cu2+ + 2I- + 2e- 2CuI E0 = 0.86 V
I2 + 2e- 2I- E0 = 0.54 V
S4O62- + 2e- 2S2O32- E0 = 0.08 V
2CO2 + 2e- C2O42- E0 =-0.49 V
and therefore the reaction with permanganate is favourable, i.e., 
2MnO4- + 5C2O42- + 16 H+ → 2Mn2+ + 10CO2 + 8H2O, E ° = 1.02 V 

The copper(II) ion is mildly oxidising and can be used as the starting material for the
synthesis of complexes of copper(I) as well as copper(II). Since the chemistry of the copper ion
is modified by the presence of the surrounding ligands, in this experiment we will prepare and
characterise the complex and investigate the oxalate ligands on the chemistry of the copper ion.

Chemicals

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SKT1013: Introduction To Inorganic Chemistry

Copper(II) sulphate pentahydrate, CuSO4.5H2O

Potassium oxalate monohydrate, K2C2O4H2O
Dilute sulphuric acid, H2SO4
Standard potassium permanganate solution, KMnO4 (0.02M)
Potassium iodide
Sodium thiosulphate, Na2S2O3 (0.05M)
Potassium thiocyanate
Starch
Ethanol

Apparatus
Erlenmeyer flask (250 mL)
Hot plate
Burette
Dropper
Buchner funnel
Filter paper
Filter funnel
Petri dish
Retort stand
Beaker
Measuring cylinder

8.3 PROCEDURE
Part A. Preparation of Copper Oxalate Complex
1. Dissolve 1.2 g of copper(II) sulphate pentahydrate in 3 mL of hot water and add to this a
solution of 3.5 g of potassium oxalate hydrate in 20 mL hot water. (CAUTION: Oxalic
acid and oxalates are toxic and must not be ingest)
2. Allow to cool to room temperature and finally to about 10C in ice bath.
3. Filter the product by suction and dry thoroughly in air.
4. Record the weight obtained.
Part B. Determination of the Oxalate Content

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SKT1013: Introduction To Inorganic Chemistry

1. Weight accurately about 0.125 g of the air-dried complex (The complex was prepared in
Part A) into a conical flask.
2. Add 25 ml of dilute sulphuric acid to dissolve.
3. Heat the solution to about 70 C and titrate slowly with approximately 0.02 M potassium
permanganate solution provided. (CAUTION: Potassium permanganate solution is a
powerful oxidant and the dilute solution is a disinfectant. Avoid skin contact, but if you do
spill it on yourself, simply wash with cold water. Any remaining brown stain will soon
disappear).
4. During the initial stages of the titration the solution is cloudy due to undissolved complex.
This clears during the titration. If the solution remains pink after adding the first drop or
two, keep swirling the flask and wait until it clears before continuing the titration.
5. Continue the titration slowly until permanent pale pink solution is obtained. (NOTE: The
temperature should not be less than 60° C at the end point. If it falls below this during
the titration, the solution must be reheated).
6. Take care NOT OVERSHOOT the endpoint as the presence of a large excess of
permanganate makes the copper determination difficult.
7. Record the volume of potassium permanganate taken. Preserve the resulting liquid for
the determination of copper in Part C.
8. Calculate the percentage oxalate in the complex.

Part C. Determination of the Copper Content

1. Ensure that the solution obtained above in Part B contains no excess permanganate by
boiling until the purple colour is discharged.
2. To the cooled solution, add 1 g of potassium iodide and titrate the liberated iodine with
0.05 M sodium thiosulphate (Na2S2O3).
3. When the colour of the resulting suspension is pale yellow, add 6-7 drops of starch and
continue titrating until the blue colour begins to fade.
4. Continue the titration until a white suspension is obtained.
5. Record the total volume of sodium thiosulphate.
6. Calculate the copper to oxalate ratio in the complex. From these results deduce the likely
values of a, b, and c.

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