UNIVERSITY TEKNOLOGI MARA PERLIS BRANCH

AUGUST 2022 – MARCH 2023

INORGANIC CHEMISTRY (CHM361)

LAB CASE STUDY REPORT

NAME OF GROUP NORSAL SABILA BINTI NOR RIZAN (2020824992)

MEMBERS
NUR ALYA ADRIANA BINTI MOHD EZHAN (2020495002)

NUR AIMAN NABILAH BINTI ISHAK (2020488804)

SITI NUR HANA BINTI MOHAMAD RAPANDI (2020617086)

MUS'AB BIN MALIKI (2020600746)

PROGRAMME AS120

GROUP RAS1205E

TITLE DETECTION OF COPPER ION (A STUDY ON TETRAAMMINECOPPER

(II) SULFATE)

NAME OF LECTURER DR.SHAFINAS BINTI ABDULLAH

TOPIC
Coordination compounds are essential in analytical chemistry because they may be used
to analyze chemical composition both qualitatively and quantitatively. The identification of the
coordination compounds in a sample is revealed by qualitative analysis, whereas quantitative
analysis indicates the amount of each coordination compound in a sample. We can use
quantitative analysis to detect ions in aqueous solution that can produce color changes, solid
formation, or other observable changes. Titrimetric and gravimetric analyses can be used for
quantitative analysis.
In our case study we have chosen a gravimetric analysis method. We will discuss one
experiment that is related to the gravimetric analysis of detection of copper ions. The experiment
comprised the production and characterization of tetraamminecopper (II) sulfate monohydrate
([Cu(NH3)4]SO4.H2O), a coordination compound.

OBJECTIVES
1) To observe the reagent used and chemical reaction involved in the experiment.
2) To identify the formula of a copper containing a coordination compound using
spectroscopy.
3) To study the properties of reagents involved.
4) To learn how determination of compounds are carried out.
INTRODUCTION

Tetraamminecopper (II) Sulfate

Coordination compound, any of a class of molecules with chemical structures in which a
central metal atom is surrounded by nonmetal atoms or groups of atoms, known as ligands, that
are chemically linked to it. The coordination compound may include such substances as vitamin
B12, hemoglobin, chlorophyll, dyes, pigments and catalysts where it can be used to prepare the
organic substances. Besides, coordination compound also is the product of a lewis acid-base
reaction, which the neutral molecules or anions (ligands) bond to the central metal atom by
coordinate or covalent bond. Many of the coordination compounds contain a metallic element as
the central atom and are therefore referred to as metal complexes. These types of coordination
compounds generally consist of a transition metal as the central atom. It can be noted that the
central atom in these complexes is called the coordination center. Some of the general properties
of coordination compounds are including the formation of the coordination compounds which is
by the transition elements will be coloured due to the presence of unpaired electrons that absorb
light in their electronic transitions. For example, the complexes containing Iron(II) can exhibit
green and pale green colors, but the coordination compounds containing Iron(III) have a brown
or yellowish-brown color. Beside that, when the coordination center is a metal, the corresponding
coordination complexes have a magnetic nature due to the presence of unpaired electrons. Next,
the coordination compounds exhibit a variety of chemical reactivity which can be a part of
inner-sphere electron transfer reactions as well as outer-sphere electron transfers. Lastly, the
complex compounds with certain ligands have the ability to aid in the transformation of
molecules in a catalytic or a stoichiometric manner.
 Gravimetric analysis is one of the frequently used quantitative methods in analytical
chemistry beside using the volumetric method. It should be cleared that the amount of an ion
present in the sample will be determined based on the parameter of mass. The principle of
gravimetric analysis is based on the estimation of the mass percent of an ion in an impure
compound of known quantity by determining the mass of the same ion in a pure compound. In
order to determine the mass, the ion of interest needs to be completely isolated. This isolation of
ions is done with the help of precipitation. Typical procedures used in gravimetric analysis
include making a solution with a known amount of the sample analyte, separation of the desired
ion/element/radical in pure forms by various separation methods, after the ion has been
separated, weigh the amount of the pure insoluble compound formed and lastly, the value of the
individual component of interest should be calculated, based on the weight of the compound
observed.
In order to detect and determine the copper ion from tetraamminecopper (II) sulfate
monohydrate, the gravimetric analysis was performed. The gravimetric analysis apparatus can be
shown as below:

Gravimetric Analysis Apparatus

FINDINGS
In this experiment, Copper sulfate (CuSO4) is utilized as the sample, water (H2O) is used
to dissolve the sample, ammonium hydroxide (NH4OH), and ethanol are used as the precipitating
agent and to wash the precipitate. The synthesis of coordination compound tetraamminecopper
(II) sulfate monohydrate can be prepared by combining a concentrated ammonia solution with a
saturated aqueous solution of copper sulphate pentahydrate, then precipitating the result with
ethanol and will form Cu(NH3)4(H2O)]2 that is salt of the metal complex with deep blue color. It
is also known as a Schweizer's reagent that is used in purifying cellulose. The reaction involved
in this experiment are :
Reaction 1:

Reaction 2:

Overall net equation of reaction:

COPPER SULFATE, CuSO4

Copper sulfate also is known as blue copperas, bluestone, blue vitriol, Roman vitriol, and
Salzburg vitriol. It occurs in nature as the mineral hydrocyanide. Physical and Chemical
Properties Copper sulfate occurs as the anhydride, a monohydrate, and the pentahydrate, which is
the form used as a fungicide or algicide. The molecular weight for the anhydride is 159.61, and
that for the pentahydrate is 267.6. The pentahydrate forms a blue, crystalline, odorless solid with
a metallic taste. It occurs in nature as the mineral chalcan- tithe. Its density at 15.6~ is 2.286.
Most formulations of copper sulfate contain 98-99% pure salt. The compound is soluble in water
(316 g/1 at 0~ but insoluble in ethanol and most organic solvents. Copper sulfate solutions are
strongly corrosive to iron and galvanized iron. The crystals are slightly efflores- cent in air.
AMMONIUM HYDROXIDE, NH4OH

Ammonium hydroxide(NH4OH), also known as ammonia water, aqua ammonia, or

aqueous ammonia.The physical and chemical properties of Ammonium hydroxide is a colorless
liquid that has a highly pungent odor. It has a density of 0.91 g/mL-1 and the melting point is
-57.5oC. Ammonium hydroxide has a boiling point of 37oC and it is highly miscible with the
water.Moreover,It is a strong alkaline reaction that dissolve copper and zinc.Fumes are formed
when ammonia water is brought near volatile acids.Ammonium hydroxide forms exothermic
reaction with sulfuric acid. Ammonium hydroxide is a weak base that is partially ionized in
water according to the equilibrium:
+ −
𝑁𝐻4𝑂𝐻 + 𝐻2𝑂 ⇌ 𝑁𝐻4 + 𝑂𝐻

The equilibrium comes in use for regulating the pH of the solutions due to the ion OH–
maximizes the pOH of the basicity level of any solution.

ETHANOL, C2H6O

Ethanol is a primary alcohol that is ethane in which one of the hydrogens is substituted by
a hydroxy group. It has a role as an antiseptic drug, a polar solvent, a neurotoxin, a central
nervous system depressant, and a teratogenic agent.It is a clear colorless,flammable solvent with
a boiling point of 78.5°C and it is also known as ethyl alcohol, grain spirits, or alcohol. Ethanol
is a polar solvent that is water-soluble and has a 55°F flash point. Ethanol has a vapor density of
1.59, which indicates that it is heavier than air.Ethanol’s specific gravity is 0.79, which indicates
it is lighter than water but since it is water-soluble it will thoroughly mix with water. Ethanol has
an auto-ignition temperature of 793°F and a boiling point of 173°F.

HYDROCHLORIC ACID, HCl

Hydrochloric acid also known as hydrogen chloride or muriatic acid is a strong corrosive
acid with a chemical formula HCl. Hydrochloric acid, HCl (aq) is a strong acid, meaning that
when it is dissolved in water, all the molecules ionize to form hydrogen ions, H+(aq), and
chloride ions, Cl - (aq). The reason that the hydrogen and chlorine ions dissociate when in an
aqueous solution is that HCl is polar covalent compound as the chlorine atom is more
electronegative when compared with the hydrogen atom. The hydrogen and chlorine atoms are
connected with a single covalent bond and it is highly reactive with metals as well as with
oxidizing agents, organic materials, alkalis, water.
Physical state and appearance of HCl are liquid, colorless- light yellow and it has a
pungent and strong irritating odor. The pH of concentrated HCl (aq) has a pH level of 0.
Furthermore,the boiling point of HCl is 108.58 °C @ 760 mm Hg (for 20.22% HCl in water) ,83
°C @ 760 mm Hg (for 31% HCl in water) and 50.5 °C (for 37% HCl in water).Moreover,its
melting point are -62.25°C (-80°F) (20.69% HCl in water), -46.2 °C (31.24% HCl in water) and
-25.4 C (39.17% HCl in water). The compound is soluble in cold water, hot water, diethyl
ether.In addition,hydrochloride acid is extremely corrosive in the presence of aluminum, copper,
or stainless steel. Non-corrosive in presence of glass and incompatible with copper and copper
alloys. It is one of the most corrosive of the non oxidizing acids in contact with copper alloys.
SODIUM HYDROXIDE, NaOH

Sodium hydroxide, also known as lye and caustic soda, is an inorganic compound with
formula NaOH. It is a white solid ionic compound consisting of sodium cations Na+ ion and
hydroxide anions OH−. Sodium hydroxide is a highly caustic base and alkali, that decomposes
proteins at the ordinary ambient temperatures and may cause severe chemical burns. It is highly
soluble in water and readily absorbs wet moisture and carbon dioxide from the air. It forms a
series of hydrates NaOH·nH2O. The monohydrate NaOH·xH2O (x=1) crystallizes from water
solutions between 12.3°C and 61.8 °C. The commercially available "sodium hydroxide" is often
this monohydrate, and published data may refer to it instead of the anhydrous compound. NaOH
is used in many industries in the manufacture of pulp and paper,textiles,drinking ,soaps and as a
drain cleaner.
The physical properties of pure sodium hydroxide is a colorless crystalline solid that
melts at 318 °C without decomposition while its boiling point is greater than 266 °F at 760
mmHg. It is highly soluble in water with a lower solubility in ethanol and methanol, but it is
insoluble in ether and other non-polar solvents.Similar to the hydration of sulfuric acid,
dissolution of solid sodium hydroxide in water is a highly exothermic reaction in which a large
amount of heat is liberated, posing a threat to safety through the possibility of splashing. The
resulting solution is usually colorless and odorless. As with other alkaline solutions, it feels
slippery when it comes in contact with the skin due to saponification.
ACETIC ACID, CH 3COOH

Acetic acid or ethanoic acid is a colorless liquid organic compound with the molecular
formula CH3COOH. When acetic acid is dissolved in water, it is termed glacial acetic acid. It is
a weak acid since the solution dissociates only slightly. But concentrated acetic acid is corrosive
and can damage the flesh. Properties of Acetic Acid is acetic acid is a smooth, colorless liquid
with a 1 ppm visible, poisonous and destructive, unpleasant vinegar odor. The melting point is
16.73 ° C and the usual 117.9 ° C boiling point. At 20°C, the density of pure acetic acid is
1.0491. It is highly hygroscopic acetic acid. It is possible to link the purity of the water solutions
to their freezing point. In carboxylic acids such as acetic acid, the hydrogen center in the
carboxyl group −COOH can differentiate from the molecule by ionization.

POTASSIUM IODIDE, KI

Potassium iodide is a metal-halide salt featuring an ionic bond between the potassium
cation (K+) and the iodide anion (I-). It is colorless to white, it appears as cubical crystals, or
powder or white granules. It has a highly bitter, saline taste. This compound is prepared by
iodine and mixing potassium hydroxide. It is one of the most effective and safe medicines
required in a health system and is in the list of the World Health Organization’s List of Essential
Medicines. The physical properties of potassium iodide is an inorganic chemical compound
which is denoted by the chemical formula KI. The molecular weight or molar mass of potassium
iodide, KI is 166.0028g/mol. The density of potassium iodide is 3.12g/cm3. The boiling point of
potassium iodide, KI is 1,330°C while the melting point is 681°C. The chemical properties of
Potassium iodide can be oxidized into an I2 molecule by introducing an oxidizing agent to it. An
example of such a reaction is provided below.
2𝐾𝐼 + 𝐶𝑙2 → 2 𝐾𝐶𝑙 + 𝐼2

This compound is used as an iodide source in several organic synthesis reactions. One such
example is the synthesis of aryl iodides from the diazonium salts of arenes.

SODIUM THIOSULFATE, NA2S2O3

It is typically found in its pentahydrate form which is either white in color, or colorless
altogether. In its solid form, it is a crystalline solid which has a tendency to readily lose water.
Sodium thiosulfate is readily soluble in water and is also referred to as sodium hyposulfite. The
physical properties of sodium thiosulfate, Na2S2O3 is In its anhydrous form, sodium thiosulfate
has a molar mass of 158.11 grams per mole. The more commonly available pentahydrate from,
Na2S2O3.5H2O has a molar mass of 248.18 g/mol. It has a white, crystalline appearance as a solid
and is odorless. The density of sodium thiosulfate corresponds to 1.667 grams per cubic
centimeters. The pentahydrate of this salt has a melting point of 321.4 K and a boiling point of
373 K. The solubility of sodium thiosulfate in water is 70.1g/100 mL at 20°C and 231g/100mL
at 100°C. The crystal structure of Na2S2O3 crystals is monoclinic. The chemical properties of
sodium thiosulfate, Na2S2O3. The sodium thiosulfate salt is neutral in charge. However, it
dissociates in water and some other polar solvents to yield Na+ and S2O32-. Despite being stable at
standard conditions, the sodium thiosulfate salt decomposes at high temperatures to yield sodium
sulfate along with sodium polysulfide. The chemical equation for the reaction described above is
given by
4𝑁𝑎2𝑆2𝑂3 ⟶ 3𝑁𝑎2𝑆𝑂4 + 𝑁𝑎2𝑆5

When exposed to dilute acids such as dilute hydrochloric acid, the sodium thiosulfate salt
undergoes a decomposition reaction to yield sulfur along with sulfur dioxide.
𝑁𝑎2𝑆2𝑂3 + 2𝐻𝐶𝑙 ⟶ 2𝑁𝑎𝐶𝑙 + 𝑆𝑂2 + 𝐻2𝑂 + 𝑆

The alkylation of Na2S2O3 yields S-alkyl thiosulfates. These compounds are commonly referred
to as Bunte salts.

METHYL RED, C 15H15N3O2

Methyl red (2-(N,N-dimethyl-4-aminophenyl) azobenzene carboxylic acid), also called

C.I. Acid Red 2, is an indicator dye that turns red in acidic solutions. It is an azo dye, and is a
dark red crystalline powder. Methyl red is a pH indicator; it is red in pH under 4.4, yellow in pH
over 6.2, and orange in between, with a pKa of 5.1. Murexide and methyl red are investigated as
promising enhancers of sonochemical destruction of chlorinated hydrocarbon pollutants. Methyl
Red has a special use in histopathology for showing acidic nature of tissue and presence of
organisms with acidic natured cell walls. Methyl Red is detectably fluorescent in 1:1
water:methanol (pH 7.0), with an emission maximum at 375 nm (UVA) upon excitation with 310
nm light (UVB).

STARCH

Starch is a tasteless, fluffy white powder that is insoluble in cold water, alcohol, and other
solvents. Starch is a polysaccharide made up of 1, 4 linkages between glucose monomers. The
chemical formula of the starch molecule is (C6H10O5)n. The properties of starch are numerous.
The structure of starch, especially amylose content, granule size distribution, granule form,
granule-granule interaction, granule volume fraction, and continuous phase viscosity, all
influence its rheological properties. Starch has a number of properties. Starch as carbohydrate
our main source of carbohydrates is starchy foods, which play an important role in a healthy diet.
Potatoes, bread, rice, pasta, and cereals are examples of starchy foods. Starch as polysaccharide
is a form of biological polymer that is widely used. In living organisms, their role is typically
related to the structure or storage. In plants, starch (a polymer of glucose) is present in the forms
of amylose and branched amylopectin and is used as a storage polysaccharide. Starch as a
non-reducing sugar it takes more than one hemiacetal “needle” in a haystack of “acetals” to give
a positive sugar-reduction test. As a result, polysaccharides are not classified as reducing sugars.
Starch, for example, results in a negative test. Starch and sucrose are both blue, indicating that
they are non-reducing sugars.

The molecular structure of tetraamminecopper (II) sulfate monohydrate ([Cu(NH3)4]SO4 . H2O)

This copper ion in the complex salt Cu(NH3)4 SO4.H2O could be determined by using an
iodometric method (indirect method) means we cannot use I2 directly, therefore we use KI as a
reducing agent. KI reduced the Cu2+ to Cu+ and KI itself oxidized to I2. The number of equivalents
of Cu+ equal to the number of equivalents I2. By using this method, we could determine the
number of equivalents of Cu2+ in the complex salt Cu(NH3)4 SO4.H2O. During titration we use
starch as an indicator. The color of solution changed to dark brown when titrated with Na2S2O3 at
the end point the color changed to colorless.

CONCLUSION
Tetraamminecopper(II) sulfate monohydrate [Cu(NH3)4]SO4.H2O is the coordination
chemical that we were able to produce and identify. The synthesis involves dissolving copper (II)
sulfate pentahydrate and adding extra ammonia (NH3) to it. By measuring the colors, we were
also able to ascertain the complex coordination chemical formula. The use of a spectrometer
could be used to confirm the substance further.

REFERENCES
1) Yasin, K. (2015, November 13). Preparations of tetraamminecopper (II) sulfate
monohydrate. Academia.edu. Retrieved January 15, 2023, from
https://www.academia.edu/18300222/Preparations_of_tetraamminecopper_II_sulfate_mo
nohydrate
2) Preparation and testing of a tetra-amine copper(ii) chitosan bead ... (n.d.). Retrieved
January 15, 2023, from
https://www.researchgate.net/publication/321290144_Preparation_and_testing_of_a_tetra
-amine_copperII_chitosan_bead_system_for_enhanced_phosphate_remediation
3) Synthesis and analysis of coordination compounds - lab manuals for ... (n.d.). Retrieved
January 15, 2023, from
http://www.chemistrylabmanual.com/uploads/2/5/6/1/25614215/synthesiscoordinationco
mpounds.pdf
4) manishajain1974. (2020, July 4). Preparation of tetraamminecopper(ii) sulfate
monohydrate. YouTube. Retrieved January 15, 2023, from
https://www.youtube.com/watch?v=TWYu4d6-xj8
5) Britannica, Coordination Compound, Retrieved December 28, 2022,
https://www.britannica.com/science/coordination-compound/Characteristics-of-coordinati
on-compounds
6) Byju’s, What is Coordination Compound, Retrieved December 28, 2022, from
https://byjus.com/jee/coordination-compounds/
7) Byju’s, Gravimetric Analysis: Definition, Types, Advantages and Disadvantages of
Gravimetric Analysis, Practice Problems and FAQs, Retrieved December 28, 2022, from
https://www.aakash.ac.in/important-concepts/chemistry/gravimetric-analysis#:~:text=The
%20principle%20of%20gravimetric%20analysis,needs%20to%20be%20completely%20i
solated.