EXPERIMENTAL INORGANIC CHEMISTRY: A GUIDE TO LABORATORY PRACTICE

Chemistry Study Program

By
Inorganic Chemistry Teaching Team

Chemistry Laboratory
Faculty of Mathematics and Natural Sciences
UNIVERSITAS NEGERI GORONTALO
2021
 PRACTICUM GUIDELINES

A. Laboratory Equipment
Each group of students will get a set of equipment for each experiment that will be used
alternately with other groups in the next practicum.
1. Workbench and group work tools must always be clean. It is not permissible to leave the
equipment in a dirty state on the work desk. At the end of the work, you must clean the work
table with a clean wet cloth.
2. Don't borrow tools from other tables. If you need additional equipment, please borrow from
the assigned laboratory, and record it in the loan book.
3. If there is equipment damaged or broken, it must be reported immediately to find out and get
it replaced. Failure to report sanctions.
4. Large equipment for shared use is located outside the workbench, inside the laboratory
room. Please use responsibly.

B. Chemicals used
Chemicals are used together and stored on shelves on the workbench. Special reagents
needed and not available will be explained by the assistant.
1. Liquid, solids and residual solutions must be disposed of / collected into a waste container
that has been provided, according to the label.
2. Take just enough for the experiment, reagents or chemicals that have been taken from the
place should not be returned to the original container.
3. Bottles of materials that have been used must be returned to the shelf. Not allowed to be
taken to your own place, because it will interfere with usage by other groups.

C. Safety
Chemical laboratories are dangerous to work areas. It is not justified to work alone in the
laboratory.
1. Protective goggles must be worn while in the laboratory.
2. Every activity and while in the laboratory, must dress properly, wear laboratory coats as
they should, shoes, and if necessary use gloves and masks.
3. Long hair or veil must be neatly clamped so that it does not interfere with your work,
snare equipment or catch fire.
4. Knowing the location of the PPPK box, exit/emergency and fire department in the area
around the laboratory. Don't force yourself to work if your physical condition is not
healthy.
5. If the chemical falls on the skin, immediately rinse the skin with running water and report
to the assistant. If chemicals fall on clothing, remove and wash the skin underneath with
water.
6. Do not smell the reaction mixture directly. Reduce your exposure by chemical fumes
directly. If you want to smell something, steam it by hand to your face.
7. Work in a fume hood when using concentrated concentrations and hazardous
ingredients. Trap toxic vapors that come out of the reaction into water or suitable
ingredients or experiment in a fume hood.
 8. To dilute the acid, pour concentrated acid into the water, not vice versa.
9. Don't rub your eyes or other limbs with hands that might have been contaminated with
chemicals.
10. It is prohibited to use mobile phones/laptops, eat, drink and smoke in the laboratory.

D. Work Instructions at the Laboratory

1. Students are required to be able to work independently and in groups.
2. Students are allowed to enter the laboratory 10 minutes before starting, by
showing a preliminary report. Delays of more than 15 minutes are not permitted
to take part in the practicum. The practicum schedule can be seen on the
Chemistry Laboratory announcement board.
3. The bag is left in the place provided, do not forget to secure your items.
4. Students must follow the practical assistant's instructions, work in groups calmly,
and work on reports individually.
5. Record all results on the data sheet as soon as the trial is complete. The report
writing format will be explained by the assistant.
6. Only students who are absent due to illness (permission from a doctor) and
assignments from majors/ faculties/universities, who are permitted to take part in
a follow-up practicum, in another class.
7. Sanctions will be given if students violate instructions or carry out activities
outside the practicum activities, for example, working on other coursework
during practicum activities, doing activities that endanger themselves or other
students, etc.

E. Assessment
The assessment system is set to maintain the objectivity of student work without reducing the
purpose and objectives of this practicum.
1. The final value of the practicum is obtained from the preliminary examination and pretest
scores (15%), the experimental value (25%), the reported value (35%) and the final
examination score (35%).
2. Students are allowed to take part in the practicum if they have a preliminary examination
score of at least 65. The preliminary examination and final practicum examination will be
conducted orally and in writing.
3. Students who have equipment dependents must immediately pay it off. The final value of
the practicum is only issued to students who have been free of dependents.
 COURSE OUTLINE

Module I:
Chemical reactions of the main group compounds

Module II:
Synthesis of Calcium Sulphate from Limestone

Module III:
Alumina Extraction from Mud

Module IV:
Modification of Sulfur

Module V:
Synthesis of Urea-Hydrogen Peroxide

Module VI:
Zeolite Synthesis from Rice Husk Ash (RHA)

Module VII:
Synthesis of Manganese (VI) and Manganese (III) Compounds

Module VIII:
Observing Redox Reactions in Nitrogen Compounds
 MODULE I
Chemical reactions of the main group compounds

1. Introduction
A chemical reaction is said to take place if a reaction product is observed, which can be: (i)
sediment, (ii) gas, (iii) changes in the pH of the solution, and (iv) changes in the color of the
solution. In general, nitrate, halide, acetate and chlorate compounds from the main group dissolve
well in water. While the hydroxide compounds, carbonate, sulfate, phosphate from group 2
elements have a small solubility in water compared to class 1 element compounds.
Based on the differences in solubility, the solubility properties were used in a qualitative
analysis of main class salts. Acid-base or redox reactions of the main group compounds are also
used in gas formation, such as the formation of hydrogen, oxygen, nitrogen dioxide, sulfur dioxide,
and chlorine gas. In this module, several reactions will be carried out using the main group
compounds.

2. Objectives
Know the chemical and physical properties of several main group compounds and can write
down the equation of the reaction well.

3. Tools and Materials

3.1 Tools:
3.1.1 Category 1
- Mica paper - Reagent tube - Measuring flask
- Black cardboard - Glassware - Measuring cup (100 mL)
- Drop pipette - Spatula - Beaker Glasses (250 mL)
3.1.2 Category 2
- Analytical balance - Distillation Apparatus
- Fume hood

3.2 Materials
3.2.1 General Materials :
- Distilled water - Washing soap
- Tap water - Tissue

3.2.2 Specific Materials (1 M each)

Cation solution: NH4Cl, NaNO3, KNO3, Mg(NO3)2, Ca(NO3)2, Ba(NO3)2, Al(NO3)2,
Pb(NO3)2, and HCl; Anion solution: NaOH, Na2CO3, Na2SO3, Na3PO4, Na2HPO4,
Na2CrO4, dan Na2S.

4. Procedure
4.1 Reactions of cations and anions
• Prepare transparent mica plastic, the bottom of which is mixed with black cardboard so
that it can observe the reaction product (gas bubbles, sediment, or color change)
• Test 1: Each cation solution (8 sequences) is dripped on the mica plastic as much as 1-2
drops, given the distance between the solutions with each other. Each solution of the
cation is reacted with HCl solution. After observation, mica plastic paper is cleaned with
tissue.
• Test 2: do the same as in test 1, HCl solution is replaced with a NaOH solution.
• Test 3: do the same thing as in test 1, HCl solution is replaced with a Na2CO3 solution.
• Test 4: do the same thing as in test 1, HCl solution is replaced with a Na2SO3 solution.
• Test 5 do the same thing as in test 1, HCl solution is replaced with a Na2SO4 solution.
• Test 6 do the same as in test 1, HCl solution is replaced with a Na3PO4 solution.
• Test 7 do the same thing as in test 1, HCl solution is replaced with a Na2HPO4 solution.
• Test 8 do the same thing as in test 1, HCl solution is replaced with a Na2CrO4 solution.
 • Test 9 does the same thing as in Test 1, HCl solution is replaced with a Na2S solution.

4.2 Identification of cation and anion solutions

• The group is given a sample solution containing the salt solution mixture used in the
reaction above.
• Identification of 2 cations and 2 anions contained in the sample solution.
Task (summarized in the practicum report)
• Write down the equation of reaction (equivalent reaction) of each
experiment.
• Any solution that forms sediment and color. Explain why it happened!

Observation data
Reaction of cations and anions
Observation result
Sediment
Reagent Gas formed Solution Sediment
formed
Color color
Yes No Yes No

Gas identification
Solution Cation Anion
1
2
3
4
 MODULE II
Synthesis of Calcium Sulphate from Limestone
1. Introduction
Limestone is abundant in Indonesia. Limestone has the chemical formula CaCO 3 with general
impurities in the form of silica, iron, and magnesium. Limestone can be dissolved by rainwater
more easily than other rocks. Under the influence of high pressure, limestone is morphed into
marble metamorphic rock. Under certain conditions, calcite contained in limestone is altered into
dolomite rock. One of the uses of limestone is for the manufacture of chemicals, including
calcium sulfate.Calcium sulfate is generally white, depending on the impurity minerals with a
degree of hardness of 1.5-2 and density of 2.31-2.35. Calcium sulfate includes calcium salts which
are easy to settle with a Ksp value of 2.4x10-5. Calcium sulfate can be used as one of the ingredients
for cement Portland, chalk raw materials, hardening additives for building materials, etc.

2. Objectives
Study the synthesis of calcium sulfate from limestone.

3. Tools and Materials

3.1 Tools
3.1.1 Category 1
- Evaporation cup - Test tube - Glass stirrer
- Measuring flask - Spatula - Reagent bottle
- Drop pipette - Mortar
- Sieve (100 mesh) - Analytical balance
- Beaker glasses (250 mL) - Watch glasses
- Erlenmeyer (250 mL) - Spray bottle
3.1.2 Category 2
- Oven - Analytical balance
- Fume hood - Furnace
- Distillation Apparatus - Vacuum Filter

3.2 Materials
3.2.1 General Materials
- Limestone - Distilled water - Washing soap
- Tissue - Tap water
3.2.2 Specific Materials
- Sulfuric acid - Potassium thiocyanate
- Hydrochloric acid - Sodium carbonate
- Nitric acid - Sodium oxalate

4. Procedure
• Weigh 2.0 g of finely ground limestone (approximately 100 mesh), then heat in a kiln at 900
ºC for 1 hour.
• Soaking the powder produced by pouring with 50mL of distilled water and 25 mL
of 1M HCl (2: 1 v/v) for 15 minutes while stirring, then strain and take the filtrate.
• Concentrate the solution by evaporating the solution but not to form a precipitate (if
formed, stop heating and add drop by drop of distilled water until it dissolves again).
• Add drop by drop of 1M H2SO4 while stirring until a white solid is formed. Help
with cooling if necessary.
• Filter the precipitate formed then dry it. Weigh solids formed.
 Qualitative Test
a. Dissolve a little solid from syntheses in sulfuric acid and drops with 1M KSCN. Observe
the changes that occur?
b. Take a small amount of the synthesized solid and dissolve it with 10 mL 1M nitric acid and
add a few drops of sodium oxalate or 1M sodium carbonate. Observe the changes that
occur?

Task (summarized in the practicum report)

1. What is the heating function in the furnace? Write the equation for the reaction!
2. When added with distilled water and HCl, what impurities do not dissolve? Write a reaction
equation for impurities and limestone!
3. Explain the analysis based on the results of qualitative tests!

Results (data) collected to assistant:

a. Calcium sulfate mass is obtained
b. Qualitative test results
 MODULE III
Alumina Extraction from Mud

1. Introduction
Aluminum oxide or alumina is the main component in bauxite, which is the main aluminum
ore. Alumina has a hardness of 9 on the Mohs scale. This causes alumina to be widely used as an
abrasive to replace much more expensive diamonds. Some types of sandpaper and CD / DVD
cleaners also use aluminum oxide.
Apart from minerals, alumina can be extracted from sludge. Soil or clay is an accumulation of
mineral particles whose bonds between particles are weak, which are formed by weathering from
rocks. The weak bond is caused by the influence of carbonate/oxide compounded between particles,
or because of the presence of organic matter. Generally in soil contains alumina (Al 2O3) and silica
(SiO2) in the dominant amount other than other metal oxides from alkali groups (Na2O, K2O),
alkaline earth (MgO, CaO) and little metal oxides from transitions (Fe2O3, TiO2, etc.).
Extraction of alumina from sludge must pay attention to the presence and nature of alumina
and other compounds so that the extraction process can be effective and produce alumina with high
purity.

1. Objectives
Study the extraction of metal oxides from mud and characterize compounds produced by FTIR.

2. Tools and Materials

3.1 Tools
3.1.1 Category 1
- Beaker glass(50 mL) - Spray bottle - Glass stirrer
- Measuring cup (10mL) - Glass funnel - Erlenmeyer
- Watch glass - Measuring flask - Reagen bottle
- Desiccator - Spatula
3.1.2 Category 2
- Magnetic stirrer - Hot plate - Oven
- Analytical balance - Fume hood - Distillation Apparatus

3.2 Materials
3.2.1 General materials
- Dry mud - Tap water - Filter paper
- Distilled watern - Tissue - Washing soap
- Universal pH indicator paper
3.2.2 Specific materials
- KOH - HCl - KBr

3. Procedure
3.1. Method 1
1. Take 2.5 g of dried mud that has been calcined and places it in a beaker 50ml, then add
15ml of 2M NaOH solution, stirring with a magnetic stirrer for 30 minutes.
2. Separate the sediment with filter paper, then transfer the filtrate to a 50mL beaker.
3. Add 2M HCl to pH 8, use universal pH indicator paper.
4. Heat the solution (70 ° C) to form a precipitate, then cool the solution to room temperature
and separate the precipitate formed.
 5. Wash the sediment with distilled water until the pH of the water is neutral washing, then
the precipitate is heated in an oven at 110 °C to a constant weight.
6. Record the final sediment mass obtained then analyze with FTIR, compare it to the
standard spectra of Al2O3 and SiO2.

3.2. Method 1
1. Take 2.5 g of calcined dried mud and place it on a 50mL beaker, then add 15mL of 2M
HCl solution.
2. Cover the beaker with a watch glass, stir and heat the solution with a magnetic stirrer for
30 minutes in the fume hood.
3. Separate the sediment with filter paper, then transfer the filtrate to a 50mL beaker.
4. Add 2M NaOH to pH 3, use a universal pH indicator paper.
5. Separate the precipitate formed when the filtrate added 2M NaOH to pH 8.

Task (summarized in the practicum report)

1. Explain the stages of separation that occur in the two methods above, along with the
reaction!
2. Explain which work results are better than the two methods above!

Results (data) collected to assistant:

a. mass and Al2O3 levels in mud samples
b. IR spectra of isolated compounds from the two methods
 MODULE IV
Modificatio of Sulfur

1. Introduction
Sulfur is a chemical element in the periodic table that has the symbol S and atomic number 16.
The shape is non-metal that has no taste, no smell and is multivalent. Sulfur, in its original form,
is a yellow crystalline solid. In nature, sulfur can be found as a pure element or as sulfide and
sulfate minerals. It is an essential element for life and is found in two amino acids. Its commercial
use is mainly in fertilizer but also in gunpowder, matches, insecticides and fungicides.
Sulfur is pale yellow, a fragile solid, which is not soluble in water but dissolves easily in CS2
(carbon disulfide). In various forms, whether gas, liquid or solid, sulfur occurs in more than one
allotropic form or mixture. With different forms, the result is different in nature and the
relationship between the nature and form of allotropy is still not understood.

2. Objectives
a. To study several modification of sulfur.
b. To study characteristics of hydrogen sulfide and H2SO4.

3. Tools and Materials

Category 1 - Glass stirrer
- Beaker glass (500 mL) - Tube clamp
- Measuring cup (10mL) - Measuring flask
- Test tube
- Test tube shelf Category 2
- Evaporation cup - Hot plate
- Bunsen burner - Analytical balance
- Drop Pipette - Distillation Apparatus
- Statif + burette - Fume hood
- Watch glass

General Materials
- Tap water - Tissue - Sucrose
- Distilled water - Washing soap - Ethanol
- Copper chip - Filter paper
Specific Materials
-CH3COOH(aq) - HNO3 (l) - Sulfur
-Na2SO3 (s) - HNO3 (aq) 2M
-K2CrO4 (aq) - H2SO4 (l)

4. Procedure
➢ Modification of Sulfur
1. Blend 0,5 gr of sulfur in evaporation cup by heating the sulfur until it melts and let it freeze.
Observe crystal stripes
2. Heat 0.5 gr of sulfur powder in the test tube while shaking the tube. Observe the sulfur color change

➢ Characteristics of Sulfuric Acid

1. Heat a piece of copper in a test tube containing 1 mL H2SO4 (not boiling). Observe the activity in
the test tube. Write the reaction equation
2. Place the filter paper moistened with K2CrO4 solution in the mouth of test tube (test tube in step 1).
Observe the color change on the filter paper. Write the reaction equation!
 3. Put sucrose into the test tube and a few drops of concentrated H2SO4. Observe and take a note the
activity in the test tube!
4. Put 2 mL of acetic acid into the tube, add 2 mL of ethanol and 2 mL of concentrated H2SO4. Heat
the test tube using a Bunsen burner. Observe and take a note the activity in the test tube! Write the
reaction equation!

Task (summarized in the practicum report)

1. How is the state of sulfur I nature?
2. Sort types of allotrope from sulfur! Explain the difference!
3. Explain
4. What the mean by plastic sulfur?
5. What Happens if H2S dioxide? Explain!
6. Sort important reactions in the manufacture of sulfuric acid according to the Kontak procces!
7. Sort the important chemical properties of sulfuric acid and give an example!
 MODULE V
Synthesis of Urea-Hydrogen Peroxide

1. Introduction
Hydrogen peroxide, H2O2, can oxidize or reduce various kinds of inorganic compounds and organic
compounds in certain reaction conditions. For example, H 2O2 can oxidize Fe2+ to Fe3+, SO32- ions
into SO 42- under acidic conditions.In addition, KMnO is4 reduced to Mn2+ by H O under
22
acidic
conditions. Hydrogen peroxide is widely used in various chemical industries. Hydrogen peroxide is
an environmentally friendly chemical because H 2O2easily decomposes into H2O and O2gas
spontaneously in solution
2H2O2⟶ 2H2O + O2 (ΔHo = -98,2 kJ/mol)

One way to stabilize H2O2 is to react H2O2with urea, which will produce solid urea-hydrogen
peroxide (UHP) which is relatively more stable than the H2O2 solution.The solid UHP is formed by
the presence of hydrogen bonds between urea and H2O2.The reaction of making UHP solids is
relatively easy and inexpensive, and the ability as an oxidizing agent is similar to H 2O2.In this
experiment, UHP solid synthesis will be carried out.
The amount of H2O2 in the synthesized UHP sample can be determined using the
permanganometric titration method. Hydrogen peroxide reduces KMnO 4 to Mn2+ in an acidic
conditions, with the following equation:
2MnO4- + 5H2O2 + 6H+→ 2Mn2+ + 8H2O + 5O2 (Eo = 0,81 sel V)

Based on the mole ratio between KMnO 4 and H2O2 in the above equation, the amount of H 2O2 in
UHP solid samples can be determined. In this titration, a KMnO4 solution is used as a titrant. The
change in the color of the solution observed at the equivalent point is from colorless to pink, which
indicates that MnO4-is reduced to Mn2+.
2. Objectives
Synthesis of urea-hydrogen peroxide (UHP) crystals, qualitative analysis, and quantitative
analysis of the amount of H2O2 in UHP synthesized using permanganometric titration method.

3. Tools and Materials

3.1 Tools:
3.1.1 Category 1
- Beaker glass (100 mL) - Drop pipette - Glass stirrer
- Burette (25 mL) - Test tube shelf - Spatula
- Volumetric flask (100 mL) - Thermometer - Measuring cup
- Watch glasses - Test tube
3.1.2 Category 2
- Hot plate - Analytical balance - Oven
- Destilator - Fume hood
3.2 Materials:
3.2.1 General Materials
- Tap water - Tissue - Filter paper
- Distilled water - Washing soap
3.2.2 Specific Material
- Hydrogen peroxide (H2O2)30% - Manganese dioxide (MnO2)
- Potassium Permanganate 0.02M (0.1N) - Urea(CON2H4)
4. Procedure
4.1 Synthesis of urea-hydrogen peroxide (UHP)
• Take 3.4% H2O2solution as much as 3.4 mL using a pipette then the solution is transferred
to a 10 mL Erlenmeyer flask.
• Weigh 1.2 grams of urea then put it in H2O2 solution and stir until the urea solids dissolve
completely.
• Fill a beaker with 250 mL of tap water as much as 150-200 mL and heated to a temperature
of 60o C. The water will be used as a water bath.
• Erlenmeyer flask containing a mixture of H2O2 and urea dipped in a water bath. Erlenmeyer
pumpkin neck pin using a clamp.
• Heat the solution a few minutes until the solution becomes clear. Note: do not let the bath
water enter the Erlenmeyer flask.
• After the solution has become clear, remove the solution on the watch glass so that the
solvent can evaporate slowly until there is a needle-shaped crystal.
• After the crystallization process is complete, place the crystal on filter paper and dry it.
After drying, the resulting crystal is weighed.
• Observe the form of UHP crystals synthesized using a microscope, then describe the crystal
shape.
4.2 Qualitative analysis
Weigh 0.1 g of the synthesized crystal and put it in a test tube and dissolve it with 2-3 mL of
water. Add the MnO2 solid to the test tube and observe the O2 gas bubbles that are formed.
4.3 Quantitative analysis
• Prepare a titration set (burette, valve, standard) and attach it properly. A burette is filled
with a standard 0.02 M KMnO4solution.
• Weighing 0.62 grams of synthesized UHP solids then put it in a 100 mL beaker glass and
dissolve it with 50 mL of aquadest. Then add 5 mL of H2SO4 2 M to the solution.
• Transfer the solution into a 100 mL volumetric flask and dilute it with water.Pipette the
solution as much as 10 mL and transfer it to a 50 mL Erlenmeyer flask, then titrate with
0.02 M KMnO4standard solution until the color of the solution becomes pink.
• The same thing as step (ii) - (iii), for blank solutions. Blank solution: 10 mL of aquadest
was pipetted and transferred to a 50 mL Erlenmeyer flask, then titrated with
0.02 KMnO4standard solution. Record the KMnO4 volume used for the titration.
• Titration of UHP solution and blank solution is carried out at least 2 times.
Tasks (summarized in the practicum report):
a. What can cause H2O2 to decompose?
b. What is the excess of peroxide in the form of UHP solids compared in liquid form?
c. Calculate theoretically the KMnO4 volume needed to determine the amount of H2O2 in the
UHP sample, according to the work procedure above.
d. Write down the chemical reaction equation for the UHP qualitative test.
 MODULE VI
Zeolite Synthesis from Rice Husk Ash
(RHA)

1. Introduction
Zeolite is a group of minerals produced from hydrothermal processes in alkaline igneous
rocks. This mineral is usually found filling fissures or cracks from these rocks. In addition, a zeolite
is also a precipitate of volcanic activity which contains a lot of silica (Saputra, 2006).The term
zeolite refers to a three-dimensional inorganic polymer network of an aluminosilicate crystal
family. Zeolite minerals are formed from tetrahedral (Si, Al) O4 which are interconnected with
shared use of hydrogen atoms (Subaer, 2012). Synthesis of zeolite is a chemical compound that has
the same physical and chemical properties as natural zeolite. This zeolite is made from other
materials with the synthesis process. Because zeolite is generally able to absorb, exchange ions and
become a catalyst (Saputra, 2006).

2. Objectives
Synthesize Zeolite from RHA
3. Tools and Materials
3.1 Tools
3.1.1 Category 1
- Watch glass - Drop pipette - Mortar
- Beaker glass - Stirring rod - Measuring flask
- Measuring cup - Spatula - Sieve (100 Mesh)
3.1.2 Category 2
- Analytical balance - Hot plate - Oven
- Distiller - Fume hood

3.2 Materials
3.2.1 General Materials
- Samples (Rice Husk Ash) - Filter paper - Distilled water
- Tap water - Tissue - Washing soap
3.2.2 Specific Materials
- KOH
- Al2(SO4)3

4. Procedure
a. Weigh the sample (Rice Husk Ash) as much as 15 gr for 3 comparisons
b. Weigh KOH with different gram compositions. Each as much as 10 gr: 8.75 gr: 7.5 gr. And add
10 mL of water each
c. Weigh Al2(SO4)33.75 gr for 3 comparisons and add 10 mL of water each
d. Mixing KOH solution with Al2(SO4)3 and rice husk ash for each comparison. Then heated with a
water bath while stirring until the solution is thick.
e. The thick solution is transferred into the watch glass and then dried in the oven.
f. Observe the changes that occur
 MODULE VII
Synthesis of Manganese (VI) and Manganese (III) Compounds

1. Introduction
Manganese is a transitional group which is a gray-white metal that looks similar to cast iron.
Has a high melting point of approximately 1250 °C. It reacts with warm water to form manganese
(II) hydroxide and hydrogen. Light photogeneration at Mn(CO)4L radical 1,2-diax-Mn2(CO)5L2
presence of organic halides or physical mixtures of Mn2(CO)3L2. (L = PR3) and the organic halide
solution produced by Mn(CO)5-yLyX as the only result.
The highest oxidation level for manganese corresponds to the total number of 3d electrons and
4s, but only occurs in oxo compounds MnO4-, Mn2O7 and MnO3F. These compounds show some
similarities to the corresponding halogen compounds. Manganese is relatively abundant, and is
present in many deposits, especially oxides, hydrated oxides, or carbonates. Metals can be obtained
from it or from Mn3O4 obtained by roasting it, by reducing it with Al. Manganese is quite
electropositive and easily dissolves in non-oxidizing acids.
In addition to its high melting point, electrical conductivity is another characteristic of
manganese. In addition, manganese has moderate hardness due to the rapid availability of electrons
and orbitals to form metal bonds.
The most important use of manganese is in steel production, and for this purpose, a mixture of
manganese iron, ferromanganese, is usually used. Ferromanganese is produced by reducing the
mixture of iron and manganese oxide with carbon. The most important manganese ore is pyrolusite,
MnO2.
MnO2 + Fe2O3 + 5C ⟶ Mn + 2Fe + 5CO
In steel production, Mn participates in iron purification by reacting with sulfur and oxygen and
transferring it through crust formation. Another function is to increase steel hardness. Large
proportions of Mn-containing steel, very hard and durable, are used as trains and bulldozer
machines.
The Mn electron configuration is (Ar) 3d5 4s2using 2 4s electrons and then the five unpaired 3d
electrons. Mn has an oxidation number between +2 and +7. The important chemical reactions of
manganese compounds are oxidation and reduction reactions. Six manganese oxides are known as
MnO, MnO, Mn2O, MnO2, MnO3, Mn2O7, and Mn3O4. Five of these oxides have an oxidation state
of +2, +3, +4, +5 and +7, while the latter Mn3O4, is manganese (II) oxide, (MnO, Mn2O3).
The main source of manganese compounds is MnO 2. If MnO2 is heated with the addition of
alkali and oxidizing agents, salt permanganate will form.
3MnO2 + 6KOH + KClO3→ 3K2MnO4 + KCl + 3H2O
K2Mn4 is extracted from the mixture in water and can be oxidized to KMnO4 (for example with Cl2
as an oxidizing agent). Alternatively, if acidified MnO4 is produced MnO4. KMnO4 is an important
oxidizing agent. For chemical analysis, it is usually used in acidic solutions, where the compound is
reduced to Mn2+.
Manganese (II) cation is derived from manganese (II) oxide. It forms colorless salts, although if
the compound contains crystalline water and is in solution, the color is rather pink, this is caused by
the presence of hexaakuomanganese (II) ions (MnO(H 2O)6)2+ manganese (III) ions are unstable ,
but there are complexes containing manganese in the +3 oxidation state known to people. Easily
reduced to manganese (II) ions. Manganese (II) compounds with the exception of manganese (IV)
oxide are unstable, because this manganese (IV) ions are easily reduced to manganese (II).
Manganese (VI) compounds are stable in alkaline solutions and are green.
 In neutralization the disproportionation reaction occurs, forming manganese dioxide deposits and
manganate (VII) ions or permanganate. If manganese (VI) oxide is treated with acid, manganese ions
(II) are formed. Manganese (VII) compounds contain manganate (VII) ions or MnO4- permanganate.
Alkaline permanganate is a stable compound that produces a violet solution. All of them are strong
oxidizing agents.

2. Objectives
Synthesizing manganese (VI) and manganese (III) compounds

3. Tools and Materials

3.1 Tools:
3.1.1 Category 1
- Beaker glass - Test tube - Measuring Flask
- Drop pipette - Test tube rack - Spatula
- funnel - Measuring cup - Glass stirrer
3.1.2 Category 2
- Analytical balance - Fume hood
- Distiller

3.2 Materials
3.2.1 General Materials
- Filter paper - Distilled water - Tissue
- Tap water - Washing soap
3.2.2 Specific Materials
- KMnO4 (aq) 0.01M - Concentrated H2SO4 - MnSO4 (s)
- KMnO4 (aq) 0.1M - H2SO4 (aq) 1 M - MnO2 (s)

4. Procedure
Manganese (VI) Compound
Test tube 1
• Mix 10 mL 0.01M KMnO4with 5 mL 1 M H2SO4
• Add a little MnO2 then shake it
• Filter the solution
Test tube 2
• Mix 10 mL 0.01M KMnO4with 5 mL 2 M NaOH
• Add a little MnO2 then shake it
• Filter the solution
b. Manganese (III) Compounds
• Weigh 0.5 grams of MnSO4 then react with 2 mL of 1M H2SO4
• Add 10 drops of concentrated H2SO4
• Cool with cold water
• Add 5 drops of 0.1 M KMnO4
• Mix in 50 mL of distilled water
• Observe the changes that occur!

Tasks (summarized in the practicum report):

a. Does the color difference from each experiment occur? Explain!
b. Write down all the similarities of the reactions that occur!
 MODULE VIII
Observing Redox Reactions in Nitrogen Compounds

1. Introduction
Nitrogen is a non-metallic element in the periodic table located in group VA or group 15 and
has the symbol N with atomic number 7. At room temperature, it is a colorless, odorless,
odorless, and diatomic (N2) gas. The liquefied nitrogen is also colorless and odorless.
Redox (reduction / oxidation) is a term that explains the change in the oxidation number
(oxidation state) of atoms in a chemical reaction. This can be a simple redox process such as
carbon oxidation that produces carbon dioxide, or carbon reduction by hydrogen to produce
methane (CH4), or it can be a complex process such as oxidation of sugar in the human body
through a complex series of electron transfers. The term redox comes from two concepts,
namely reduction and oxidation. It can be explained easily as follows:
- Oxidation describes the release of electrons by a molecule, atom, or ion.
- Reduction describes the addition of electrons by a molecule, atom, or ion

2. Objective
To study the redox reaction of nitric acid and nitric salt, the redox reaction of nitrite and the
redox reaction of ammonia and ammonia ions.

3. Tools and Materials

3.1 Tools
3.1.1 Category 1
- Beaker glass (250 mL) - Watch glass - Spatula
- Measuring flask - Test Tube - Bunsen burner
- Erlenmeyer flask (100 mL) - Stirring bar - Reagent bottle
- Test Tube Shelf - Drop pipette - Glass stirrer
3.1.2 Category 2
- Analytical balance - Fume hood
- Distiller - Hot plate

3.2 Materials
3.2.1 General Materials
- Distilled water - Indicator paper - Copper Chip (Cu)
- Washing soap - Tap water - Tissue
3.2.2 Specific Materials
- Potassium Iodide (KI) - Concentrated Nitric Acid (HNO3)
- Dilute Sulfuric Acid (H2SO4 1M) - Copper Nitrate (Cu (NO3)2
- Dilute sodium hydroxide (NaOH) - Sodium Nitrate (NaNO3)
- Potassium Permanganate (KMnO4) - Potassium Nitrate (KNO3)
- Ammonium Chromate ((NH4)2CrO7
4. Procedure
4.1 Redox reaction of Nitric Acid and Nitrate Salts
4.1.1 Reaction between Nitric Acid with Copper
1. Put a piece of copper in the test tube
2. Add a few drops of concentrated HNO3 and observe the activity in the test tube
Further treatment
1. Dilute 2 mL of concentrated HNO3 to obtain a 7 M solution. Put in the test tube
2. Add 3 pieces of copper and observe the gas bubbles formed!

4.1.2 Heating Nitric Acid

1. Put solid KNO3 and solid Cu(NO3)2 into each test tube before heating them
2. Observe the activity in each test tube

4.1.3 Reduction of Nitric in base solution

1. Put 2 mL HNO3 2 M in the test tube
2. Add dilute NaOH solution
3. Add a piece of copper
4. Put them into the beaker containing water
5. Heat the beaker and observe the activity in the test tube

3.1 Redox reaction of Nitric Acid

1. Put 1 mL dilute H2SO4 into the test tube
2. Let it cool for 5 minutes in excitatory or use cubes ice
3. Put the cold sulfuric acid into a test tube containing 1 gr of NaNO3. Observe the gas
formed!
4. Divide the solution into 3 parts and put them into each test tube
5. Heat a test tube containing a solution of nitric acid without adding another solution. The
heating is stopped when the color of the solution turns brown.
6. for second test tube containing nitric acid solution, add a little KI then heat it. Use litmus
paper to check the gas formed. The heating is stopped when litmus paper changes color
from red to blue
7. for the third test tube containing a solution of nitric acid, add enough KMnO4 solution then
heat it. Observe the activity in the test tube.