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A.

TITLE OF EXPERIMENT
Chlor, Brom and Iod

B. DATE OF EXPERIMENT
Wednesday, 25th September 2019 / 09:30 – 12:00 WIB

C. PURPOSE OF EXPERIMENT
1. Knowing the properties of chlorine, bromine, iodine and its compounds
2. Identifying chlorine, bromine, iodine and its compounds
3. Knowing how to make chlorine, bromine and iodine gas

D. BASIC THEORIES
1. Chlorine
Chlorine is a chemical element with the symbol Cl and atomic number
17. Chlorine is a yellow-green gas at room temperature. It is an extremely
reactive element and a strong oxidising agent: among the elements, it has
the highest electron affinity and the third-highest electronegativity on the
Pauling scale, behind only oxygen and fluorine. Like all halogens, it is thus
one electron short of a full octet, and is hence a strong oxidising agent,
reacting with many elements in order to complete its outer shell (Greenwood
& Earnshaw, 1997). Chloride ion is a weaker reducing agent than bromide,
but a stronger one than fluoride.
Chlorine is intermediate in reactivity between fluorine and bromine,
and is one of the most reactive elements. simplest chlorine compound is
hydrogen chloride, HCl, a major chemical in industry as well as in the
laboratory, both as a gas and dissolved in water as hydrochloric acid. It is
often produced by burning hydrogen gas in chlorine gas, or as a byproduct
of chlorinating hydrocarbons. Another approach is to treat sodium chloride
with concentrated sulfuric acid to produce hydrochloric acid, also known as
the "salt-cake" process:
150℃
NaCl + H2SO4 → NaHSO4 + HCl
540−600℃
NaCl + NaHSO4 → Na2SO4 + HCl
(Greenwood & Earnshaw, 1997)

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In the laboratory, hydrogen chloride gas may be made by drying the
acid with concentrated sulfuric acid. Deuterium chloride, DCl, may be
produced by reacting benzoyl chloride with heavy water (D2O) (Greenwood
& Earnshaw, 1997).
At room temperature, hydrogen chloride is a colourless gas, like all
the hydrogen halides apart from hydrogen fluoride, since hydrogen cannot
form strong hydrogen bonds to the larger electronegative chlorine atom.
Hydrochloric acid is a strong acid (pKa = −7) because the hydrogen bonds
to chlorine are too weak to inhibit dissociation (Greenwood & Earnshaw,
1997).
Occurrence and production
Chlorine is too reactive to occur as the free element in nature but is
very abundant in the form of its chloride salts. Small batches of chlorine gas
are prepared in the laboratory by combining hydrochloric acid and
manganese dioxide, but the need rarely arises due to its ready availability.
In industry, elemental chlorine is usually produced by the electrolysis of
sodium chloride dissolved in water (Greenwood & Earnshaw, 1997).
2NaCl + 2H2O → Cl2 + H2 + 2NaOH
The electrolysis of chloride solutions all proceed according to the
following equations:
Cathode : 2H2O + 2e− → H2 + 2 OH−
Anode : 2Cl− → Cl2 + 2e−
In the Deacon process, hydrogen chloride recovered from the
production of organochlorine compounds is recovered as chlorine. The
process relies on oxidation using oxygen:
4HCl + O2 → 2Cl2 + 2H2O
The reaction requires a catalyst. As introduced by Deacon, early
catalysts were based on copper. Commercial processes, such as the Mitsui
MT-Chlorine Process, have switched to chromium and ruthenium-based
catalysts (Schmittinger et al., 2006).

2 | (C h l o r , B r o m a n d I o d )
2. Bromine
Bromine is the third halogen, being a nonmetal in group 17 of the
periodic table. Like all halogens, it is thus one electron short of a full octet,
and is hence a strong oxidising agent, reacting with many elements in order
to complete its outer shell (Greenwood & Earnshaw, 1997). Like solid
chlorine and iodine, solid bromine crystallises in the orthorhombic crystal
system, in a layered lattice of Br2 molecules.
Bromine is intermediate in reactivity between chlorine and iodine, and
is one of the most reactive elements. Bromine tends to react with compounds
including M–M, M–H, or M–C bonds to form M–Br bonds (Greenwood &
Earnshaw, 1997). The simplest compound of bromine is hydrogen
bromide, HBr. Reduction of bromine with red phosphorus is a more
practical way to produce hydrogen bromide in the laboratory:
2P + 6H2O + 3Br2 → 6HBr + 2H3PO3
H3PO3 + H2O + Br2 → 2HBr + H3PO4
(Greenwood & Earnshaw, 1997)
At room temperature, hydrogen bromide is a colourless gas, like all
the hydrogen halides apart from hydrogen fluoride, since hydrogen cannot
form strong hydrogen bonds to the large and only mildly electronegative
bromine atom.
Occurrence and production
Bromine is significantly less abundant in the crust than fluorine or
chlorine, comprising only 2.5 parts per million of the Earth's crustal rocks,
and then only as bromide salts. Salt lakes and brine wells may have higher
bromine concentrations: for example, the Dead Sea contains 0.4% bromide
ions. It is from these sources that bromine extraction is mostly economically
feasible (Tallmadge, Butt, & Solomon, 1964)(Al-Weshah, 2000).
The main sources of bromine are in the United States and Israel. The
element is liberated by halogen exchange, using chlorine gas to oxidise Br−
to Br2. This is then removed with a blast of steam or air, and is then
condensed and purified. The bromine industry is about one-hundredth the
size of the chlorine industry. Laboratory production is unnecessary because

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bromine is commercially available and has a long shelf life (Greenwood &
Earnshaw, 1997).

3. Iodine
Iodine is the fourth halogen, being a member of group 17 in the
periodic table, below fluorine, chlorine, and bromine; it is the heaviest stable
member of its group (the scarce and fugitive fifth halogen, the radioactive
astatine, is not well-studied due to its expense and inaccessibility in large
quantities, but appears to show various unusual properties due to relativistic
effects). The halogens darken in colour as the group is descended: fluorine
is a very pale yellow gas, chlorine is greenish-yellow, and bromine is a
reddish-brown volatile liquid. Specifically, the violet colour of iodine gas
results from the electron transition between the highest occupied
antibonding πg molecular orbital and the lowest vacant antibonding σu
molecular orbital (Greenwood & Earnshaw, 1997).
The melting and boiling points of iodine are the highest among the
halogens, conforming to the increasing trend down the group, since iodine
has the largest electron cloud among them that is the most easily polarised,
resulting in its molecules having the strongest van der Waals interactions
among the halogens. Similarly, iodine is the least volatile of the halogens
(Greenwood & Earnshaw, 1997).
Though it is the least reactive of the halogens, iodine is still one of the
more reactive elements. For example, while chlorine gas will halogenate
carbon monoxide, nitric oxide, and sulfur dioxide (to phosgene, nitrosyl
chloride, and sulfuryl chloride respectively), iodine will not do so. The
simplest compound of iodine is hydrogen iodide, HI. It is a colourless gas
that reacts with oxygen to give water and iodine. Commercially, it is usually
made by reacting iodine with hydrogen sulfide or hydrazine:
𝐻2 𝑂
2I2 + N2H4 → 4HI + N2
(Greenwood & Earnshaw, 1997)
At room temperature, it is a colourless gas, like all of the hydrogen
halides except hydrogen fluoride, since hydrogen cannot form strong
hydrogen bonds to the large and only mildly electronegative iodine atom.

4 | (C h l o r , B r o m a n d I o d )
Aqueous hydrogen iodide is known as hydroiodic acid, which is a strong
acid. Hydrogen iodide is exceptionally soluble in water: one litre of water
will dissolve 425 litres of hydrogen iodide, and the saturated solution has
only four water molecules per molecule of hydrogen iodide (Wiberg,
Wiberg, & Holleman, 2001).
Occurance and Production
An iodine solution is produced, but is dilute and must be concentrated.
Air is blown into the solution to evaporate the iodine, which is passed into
an absorbing tower, where sulfur dioxide reduces the iodine. The hydrogen
iodide (HI) is reacted with chlorine to precipitate the iodine. After filtering
and purification the iodine is packed.
2HI + Cl2 → I2↑ + 2HCl
I2 + 2H2O + SO2 → 2HI + H2SO4
2HI + Cl2 → I2↓ + 2HCl
(Kogel, Trivedi, Barker, & Krukowski, 2006)
Alternatively, the brine may be treated with silver nitrate to precipitate
out iodine as silver iodide, which is then decomposed by reaction with iron
to form metallic silver and a solution of iron(II) iodide. The iodine may then
be liberated by displacement with chlorine (Greenwood & Earnshaw, 1997).

E. TOOLS AND SUBSTANCES


Tools
1. Drop pipette Sufficiently
2. Sided-piped test tube 1 pcs
3. Glass funnel 1 pcs
4. Asbestes gauze 1 pcs
5. Beaker glass 100 mL 3 pcs
6. Rubber cover 1 pcs
7. Statips and clamps 1 set
8. Connecting pipes 1 pcs
9. Porcelain spoon 1 pcs
10. Glass stirer 1 pcs

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Substances
1. Kawi stone powder (MnO2) Sufficiently
2. Potassium iodide 0,1 M solution Sufficiently
3. Concentrated hydrochloric acid solution 0,1 M Sufficiently
4. Lead solution 0,2 M 5-25 drops
5. Chlorine starch solution Sufficiently
6. Potassium bromide solution Sufficiently
7. Concentrated sulfuric acid solution Sufficiently
8. Kitchen salt 6 mL
9. Sodium chloride 0,1 M solution Sufficiently
10. Crystal KI, KBr ± 1 tea spoon
11. Silver nitrate 0,1 M solution 5-25 drops
12. Colored paper Sufficiently
13. Mercury (I) nitrate 0,1 M solution 5-25 drops
14. CS2 solution Sufficiently

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F. LANES WORK
1. Manufacture and identification of Cl2 and Br2 gas

A teaspoon of Kawi stone (MnO2)

- Entered into test tube


- Added a few grains of sodium chloride
- Added a few sulfuric acid 0,1 M

Mixed solution

- Heated

Cl2 gas formed

- Filter paper moistened with KI and


amylum/starch solution placed on top
- of the gas

The color of filter


paper changed

- Repeated, NaCl changed with KBr

Compared the difference


between the two

Reactions:
MnO2(s) + NaCl(s) + H2SO4(aq) → Na2SO4(aq) + MnSO4(aq) + H2O(l) +
Cl2 (g)
2I-(aq) + Cl2(g) → I2(g) + 2Cl-(aq)
MnO2(s) + KBr(s) + H2SO4(aq) → K2SO4(aq) + MnSO4(aq) + H2O(l) +
Br2 (g)
2I-(aq) + Br2(g) → I2(g) + 2Br-(aq)

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2. The properties of chlorine, bromine, iodine and its compounds

1 mL NaCl 1 mL NaCl 1 mL NaCl

- Added into test - Added into test - Added into test


tube 1 tube 2 tube 3
- Added a few - Added a few - Added a few
drops of AgNO3 drops of HgNO3 drops of lead
0,1 M acetate

Greenish yellow
White precipitate White precipitate
precipitate

- Repeated, NaCl changed with KBr

Result

- Compared all precipitate colors

A comparison of all the


colors of the precipitate

Reactions:
AgNO3(aq) + NaCl(aq) → NaNO3(aq) + AgCl(s)
HgNO3(aq) + NaCl(aq) → NaNO3(aq) + HgCl(s)
(CH3COO)2Pb(aq) + 2NaCl(aq) → 2CH3COONa(aq) + PbCl2(s)
AgNO3(aq) + KBr(aq) → KNO3(aq) + AgBr(s)
HgNO3(aq) + KBr(aq) → KNO3(aq) + HgBr(s)
(CH3COO)2Pb(aq) + KBr(aq) → 2CH3COOK(aq) + PbBr2(s)

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3. The properties of chlorine, bromine, iodine and its compounds

Calcium hypochlorite (Ca(OCl)2)

- Added one test tube of water


- Put in a beaker on filtered

Filtrate Residue

- Divided into 2 test tube

Filtrate 1 Filtrate 2

- Entered with a piece of - Added a few drops of


colored paper HCl 0,1 M
- Left in the open air - Entered with a piece of
- Observed the color colored paper
changes - Left in the open air
- Observed the color
changes

Paper color fades Paper color fades


slowly quickly

Reactions:
CaOCl2(s) + H2O(l) + CO2(g) → CaCO3(aq) + HOCl(aq) + CaCl2(aq)
HOCl(aq) + H+ + Cl- → Cl2(g) + H2O(l)

10 | (C h l o r , B r o m a n d I o d )
4. Manufacture and identification of HCl, HBr and HI

One teaspoon of NaCl

- Put in a reaction flask


- Added a little concentrated H2SO4
- Covered (closed)
- Concentrated the hose to a test tube filled
with water
- heated

Colorless solution

- Tested with litmus paper

The color of litmus paper changed

- Repeat the experiment with KBr and KI hablur


- The first repetition was tested with litmus paper
- The second repetition was tested with filter
paper dripped with a solution of potassium
iodide and starch

Result comparison

Reactions:
NaCl(s) + H2SO4(aq) → HCl(aq) + NaHSO4(aq)
2KBr(s) + 4H2SO4(aq) → Br2(g) + 2SO2(aq) + 4H2O(l) + 2KSO4(aq)
2I-(aq) + 2H2SO4(aq) → I2(g) + SO42-(aq) + 2H2(g)

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5. Halogen crushing reaction

1 mL NaCl 1 mL KBr

- Charged with chlorine gas - Charged with chlorine gas


- Added CS2 solution - Added CS2 solution
- observed - observed

Cl2 gas Br2 gas

1 mL KI

- Charged with chlorine gas


- Added CS2 solution
- observed

I2 gas

Reactions:
NaCl(aq) + Cl2(g) + CS2(aq) → NaCl(aq) + Cl2(g) + CS2(aq)
2KBr(aq) + Cl2(g) + CS2(aq) → 2KCl(aq) + Br2(g) + CS2(aq)
2KI(aq) + Cl2(g) + CS2(aq) → 2KCl(aq) + I2(g) + CS2(aq)

6. Solubility of I2 in several solvents

I2(s) I2(s)

- Added H2O - Added KI


- Pay attention to its - Pay attention to its
solubility and observe the solubility and observe the
color color
-
Not dissolve Dissolved

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I2(s)

- Added HCl concentrated


- Pay attention to its
solubility and observe the
color

Partially dissolve

Reactions:
I2(s) + H2O(l) →
I2(s) + KI(aq) → KI3(aq)
I2(s) + 2HCl(aq) → 2HI(aq) + Cl2(g)

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G. OBSERVATION RESULT
Experiment Result Conclusion
No. Procedure Prediction/Reaction
Before After
1 Manufacture and identification of Cl2 and Br2 gas ▪ MnO2 = ▪ MnO2 + NaCl Reactions: Formed Cl2
black powder = no ▪ MnO2(s) + NaCl(s) + H2SO4(aq) gas indicated
▪ NaCl(s) = changing → Na2SO4(aq) + MnSO4(aq) + by the color
white crystal ▪ H2SO4(aq) = H2O(l) + Cl2 (g) of filtered
▪ H2SO4 0,1 M colorless + ▪ 2I-(aq) + Cl2(g) → I2(g) + 2Cl-(aq) paper
= colorless black powder ▪ MnO2(s) + KBr(s) + H2SO4(aq) → (amylum +
solution ▪ +heated = K2SO4(aq) + MnSO4(aq) + H2O(l) KI) changing
▪ Filter paper = grey solution + Br2 (g) into purple
white ▪+ black ▪ 2I-(aq) + Br2(g) → I2(g) + 2Br-(aq)
powder =
formed gas
Cl2
▪ Filter paper +
amylum + KI
= colorless

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filter paper +
gas = purple
▪ MnO2 + KBr
= no
changing
▪ +H2SO4 =
grey solution
+ black
powder
▪ +heated =
yellow
blackish
solution +
black powder
▪ Formed gas
Br2
▪ Gas + filter
paper (KI +
amylum) =

15 | (C h l o r , B r o m a n d I o d )
purple +
yellow color
2 The properties of chlorine, bromine, iodine and its ▪ NaCl = ▪ NaCl + Reactions: Formed
compounds colorless AgNO3 (5 ▪ AgNO3(aq) + NaCl(aq) → AgCl and
▪ AgNO3 = drops) = NaNO3(aq) + AgCl(s) PbCl2 on this
colorless white ▪ HgNO3(aq) + NaCl(aq) → experiment,
▪ HgNO3 = precipitate, NaNO3(aq) + HgCl(s) also AgBr
colorless white ▪ (CH3COO)2Pb(aq) + 2NaCl(aq) and PbBr2
▪ Pb(CH3COO) solution → 2CH3COONa(aq) + PbCl2(s) indicated by
= colorless V = 5 drops ▪ AgNO3(aq) + KBr(aq) → the
▪ KBr = ▪ NaCl + KNO3(aq) + AgBr(s) formation of
colorless HgNO3 = white
▪ HgNO3(aq) + KBr(aq) →
turbid precipitation
KNO3(aq) + HgBr(s)
V = 30 drops
▪ (CH3COO)2Pb(aq) + KBr(aq) →
▪ NaCl +
2CH3COOK(aq) + PbBr2(s)
Pb(CH3COO)
= turbid
V = 25 drops

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▪ KBr +
AgNO3 (5
drops) =
white
solution,
greenish
yellow
precipitate
▪ KBr +
HgNO3 =
turbid (30
drops)
▪ KBr +
Pb(CH3COO)
= turbid +
white
precipitate
(10 drops)

17 | (C h l o r , B r o m a n d I o d )
3 The properties of chlorine, bromine, iodine and its ▪ Ca(OCl)2 = ▪ Ca(OCl)2 + ▪ Reactions: Calcium
compounds white powder H2O = turbid ▪ CaOCl2(s) + H2O(l) + CO2(g) → hypochloride
▪ Aquades = ▪ Filtrate = CaCO3(aq) + HOCl(aq) + which added
colorless colorless CaCl2(aq) wih HCl can
▪ Residue = ▪ HOCl(aq) + H+ + Cl- → Cl2(g) + fade the
white H2O(l) color of
▪ Filtarte 1 paper
entered with quicker than
piece of paper calcium
= paper color hypochloride
fades slowly without HCl.
▪ Filtrate 2
entered with
piece of paper
= paper color
fades quickly
Paper color
change

18 | (C h l o r , B r o m a n d I o d )
Filtrate 1 <
Filtrate 2
4 Manufacture and identification of HCl, HBr and HI ▪ NaCl(s) = ▪ NaCl + Reactions: Formed Cl2,
white crystal H2SO4 = ▪ NaCl(s) + H2SO4(aq) → HCl(aq) Br2, and I2
▪ H2SO4 colorless + + NaHSO4(aq) indicated by
concentrated NaCl crystal ▪ 2KBr(s) + 4H2SO4(aq) → Br2(g) the color of
= colorless ▪ +heated = + 2SO2(aq) + 4H2O(l) + filtered
▪ KBr(s) = pale yellow 2KSO4(aq) paper (KI +
white crystal solution + ▪ 2I-(aq) + 2H2SO4(aq) → I2(g) + amylum)
▪ KI(s) = white NaCl crystal SO42-(aq) + 2H2(g) changes into
crystal partially purple. On
didn’t this
dissolve experiment
▪ Filter paper + formed HCl
KI + amylum indicated by
= colorless the color of
▪ Gas + filter blue litmus
paper = paper change
purple into pink

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▪ +red litmus
paper = no
changing
▪ +blue litmus
paper +
change to
pink
▪ KBr + H2SO4
= colorless +
KBr crystal
▪ +heated =
orange
solution +
KBr partially
didn’t
dissolve
▪ Gas + filtered
paper = puple

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▪ +red litmus
paper = no
changing
▪ +blue litmus
paper = no
changing
▪ KI + H2SO4 =
yellow
greenish
solution
▪ +heated =
dark
brownish
▪ +red litmus
paper = no
changing
▪ +blue litmus
paper = no
changiing

21 | (C h l o r , B r o m a n d I o d )
▪ Amylum+KI
= puple
▪ The color of
gas = purple
5 Halogen crushing reaction ▪ NaCl = ▪ NaCl + Cl2 = Reactions: All of the
colorless no changing ▪ NaCl(aq) + Cl2(g) + CS2(aq) → solution are
▪ Chlorine gas ▪ +CS2 (1 NaCl(aq) + Cl2(g) + CS2(aq) colorless and
= colorless minute) = ▪ 2KBr(aq) + Cl2(g) + CS2(aq) → forming 2
stingy odor formed 2 2KCl(aq) + Br2(g) + CS2(aq) layer.
▪ KBr = layers ▪ 2KI(aq) + Cl2(g) + CS2(aq) → Indicated by
colorless ▪ KBr + Cl2 = 2KCl(aq) + I2(g) + CS2(aq) the presence
▪ CS2 = no changing of Cl2, Br2,
colorless ▪ +CS2 (1 and I2
▪ KI = colorless minute) =
formed 2
layers
▪ KI + Cl2 = no
changing

22 | (C h l o r , B r o m a n d I o d )
▪ +CS2 (1
minute) =
formed 2
layers
6 Solubility of I2 in several solvents ▪ I2 = grey ▪ I2 + H2O = Reactions: The highest
blackish yellowish I2(s) + H2O(l) → solubility is
crystal (10 drops, 10 I2(s) + KI(aq) → KI3(aq) I2 + KI.
▪ H2O = mins) I2(s) + 2HCl(aq) → 2HI(aq) + Cl2(g) Then, the
colorless ▪ I2 + KI = reaction of I2
▪ KI = colorless brown with HCl,
▪ HCl solution and the
concentrated (10 drops, 10 lowest
= colorless mis) solubility is
▪ I2 + HCl = reaction of I2
orange with H2O
(10 drops, 10
mins)
Solubility level
ore

23 | (C h l o r , B r o m a n d I o d )
▪ I2 + H2O < I2
+ HCl < I2 +
KI

24 | (C h l o r , B r o m a n d I o d )
H. ANALYSIS
1. Manufacture and identification of Cl2 and Br2 gas
The first experiment was aimed at making and identifying Cl2 and Br2
gases. The experiment was started by inserting kawi stone (MnO2) in the
form of one teaspoon of black powder into a test tube, then adding a few
grams of NaCl (no change) and 5 drops of 0.1 M sulfuric acid, a mixed
solution in the form of a colorless solution with powder the remaining black.
MnO2 has function as catalyst, heated process function so the reaction goes
easily and faster, whitle H2SO4 has function to give acid condition. Then the
heating is done, the solution turns gray and black powder remains. With
reaction:
MnO2(s) + NaCl(s) + H2SO4(aq) → Na2SO4(aq) + MnSO4(aq) + H2O(l) +
Cl2 (g)
To prove the formation of Cl2 gas, the next step is to test the gas
formed. Tests carried out by dripping KI solution (colorless) and starch
solution (colorless) on filter paper. Put filter paper at the end of the hose
attached to the tube. Filter paper that was originally white has changed color
to purple. The following are chemical reactions that explain the above
event:
2I-(aq) + Cl2(g) → I2(g) + 2Cl-(aq)
Complex Reaction:

The reactivity of chlorine is greater than that of iodine. If chlorine gas


is reacted between with KI, then there will be a pressing reaction by chlorine
gas and a product is formed in the form of KCl and I2. Iodine (I2) that is

25 | (C h l o r , B r o m a n d I o d )
formed can react with amylose from starch (starch) and form a purple
complex.
Then the same steps are repeated by replacing NaCl with KBr. The
experiment was started by adding a spoonful of MnO2 (black powder) and
a few drops of KBr. Add H2SO4 0,1 M to the test tube. Then the mixture is
heated and the color of the gas is observed. Chemical reactions that occur
are:
MnO2(s) + KBr(s) + H2SO4(aq) → K2SO4(aq) + MnSO4(aq) + H2O(l) +
Br2(g)
Based on the above reaction, Br2 gas is formed. The color of Br2 gas
is theoretically reddish brown, but at the time of practicum, the gas formed
is colorless. The cause is the same, that is, gases that are prepared using
MnO2 must be purified first. Namely by passing the gas on water to remove
HBr, then passing it on concentrated H2SO4 to remove water. the possibility
that the gas still contains other components or impurities.
To prove the presence of Br2 gas, a test was carried out by dripping
KI (colorless) and starch (colorless) solutions on filter paper. Put filter paper
at the end of the hose attached to the tube. Filter paper that was originally
white has changed color to purple and slightly yellowish. The following
are chemical reactions that explain the above event:
2I-(aq) + Br2(g) → I2(g) + 2Br-(aq)
Complex reaction:

When reacted between bromine gas with KI, there will be a pressing
reaction by chlorine gas and a product is formed in the form of KCl and I2.

26 | (C h l o r , B r o m a n d I o d )
That is because bromine has a greater activeness than iodine. Iodine (I2) that
is formed can react with amylose from starch (starch) and form a purple
complex.

2. The properties of chlorine, bromine, iodine and its compounds


The experiment was started by inserting 1 mL of NaCl (colorless)
solution into 3 test tubes. Next is adding a few drops of 0.1 M AgNO3 to
tube 1, 0.1 M HgNO3 into tube 2, PbCH3COO 0.1 M into tube 3. Next is
observing the changes that occur in the mixture. In the first tube after
addition of 5 drops, the mixture turns to a cloudy white and a white
precipitate arises; the second tube after adding 30 drops, the mixture turns
turbid white without precipitate, and in the third tube after adding 25 drops
the mixture turns turbid white without precipitate. Appropriate reactions to
the above events are:
AgNO3(aq) + NaCl(aq) → NaNO3(aq) + AgCl(s)
HgNO3(aq) + NaCl(aq) → NaNO3(aq) + HgCl(s)
(CH3COO)2Pb(aq) + 2NaCl(aq) → 2CH3COONa(aq) + PbCl2(s)
Furthermore, it was repeated with the same steps but, NaCl was
replaced with KBr. The results obtained are: in the first tube a white solution
with yellowish green precipitate after the addition of 5 drops; the second
tube formed turbid solution without sediment after adding 30 drops; the
third tube formed a turbid solution with white precipitate after the addition
of 10 drops. Appropriate reactions to the above events are:
AgNO3(aq) + KBr(aq) → KNO3(aq) + AgBr(s)
HgNO3(aq) + KBr(aq) → KNO3(aq) + HgBr(s)
(CH3COO)2Pb(aq) + KBr(aq) → 2CH3COOK(aq) + PbBr2(s)
In theory Ag, Hg, and Pb are type I cations that can form precipitate
if they react to form halide salts. However, in practicum, only Ag is
observed to form sediment (with a maximum of 25-30 drops of drops). The
reason for this is the possibility that sediments have been formed that have
not been directly observed by the eye, impurities used, or the concentration
of the solution used is too small. From these experiments it can be related

27 | (C h l o r , B r o m a n d I o d )
to the concept that group I reacts strongly with the halide group, and the salt
formed has a very small Ksp so it easily settles.

3. The properties of chlorine, bromine, iodine and its compounds


The third experiment to find out one of the properties of halogen oxide
is the oxidation ability of halogen oxide which is often used as a whitening
agent. The experiment was started by inserting a spoonful of chlorine
(Ca(OCl)2) into a beaker, adding one test tube of water. Silent a few seconds
then filtering. Formed as filtrate and residur, the filtrate obtained is a
colorless solution which is then divided equally into 2 test tubes. Test tube
one is inserted into a piece of red color paper, left open and air color changes
occur. At the same time two test tubes were added a few drops of 0.1 M
HCl, inserted a piece of red colored paper, left in the open air and observed
changes.
After a while, in tube one the red paper fades to pink, whereas in tube
2, the paper also fades, but in tube 2 the color paper fades than the paper in
tube 1. It can be explained that the addition of HCl causes hypochlorous
acid formation which is an oxidizing agent. Chlorine water which contains
hypochlorous acid has the ability to whiten (as a bleaching agent) and
oxidizer. Actually calcium hypochlorite (chlorine) is also an oxidizer, but
chlorine cannot oxidize as strongly as hypochloric acid. Reaction shown
below:
CaOCl2(s) + H2O(l) + CO2(g) → CaCO3(aq) + HOCl(aq) +
CaCl2(aq)
HOCl(aq) + H+ + Cl- → Cl2(g) + H2O(l)

4. Manufacture and identification of HCl, HBr and HI


The fourth experiment aimed to determine the manufacture of HCl,
HBr, and HI gases identified by blue litmus and filter paper moistened with
KI and starch solution. The experiment was carried out in three test tubes.
Test tube one, The first tube is filled with one teaspoon of sodium
chloride solid and a solution of concentrated sulfuric acid is added and then
covered with a stopper that has been given a hose and heated. The gas

28 | (C h l o r , B r o m a n d I o d )
formed is channeled into a beaker containing water. After the solution is
heated a HCl gas will be formed. The results of the experiment show that
red litmus paper does not change color, while blue litmus paper turns red.
This is in accordance with the theory which states that HCl will change blue
litmus paper to red because it is acidic, and filter paper moistened with KI
+ starch does not change color because it cannot occur iodine formation. By
the reaction:
NaCl(s) + H2SO4(aq) → HCl(aq) + NaHSO4(aq)

Test tube two, test tube two was given the same treatment as test tube
one. The final results show that after the solution is heated HBr gas is not
formed but Br2 gas is formed, due to strong oxidative sulfuric acid which
will oxidize HBr to Br2. It is shown that the blue litmus does not change
color, but the filter paper moistened with KI + starch changes to purple due
to the release of iodine by bromine gas as in the following reaction:
2KBr(s) + 4H2SO4(aq) → Br2(g) + 2SO2(aq) + 4H2O(l) + 2KSO4(aq)

Test tube three, the third tube was given the same treatment as the one
I tube but the sodium chloride solid was replaced by the potassium iodide

29 | (C h l o r , B r o m a n d I o d )
solid. After the solution is heated not formed HI but I2, because sulfuric acid
is a strong oxidizing agent which will oxidize HI to I2. This is indicated by
the absence of blue litmus color change, and filter paper moistened with KI
+ starch does not change color either because I2 and I- will form polyhalides
I3-. According to the following reaction equation:
2I-(aq) + 2H2SO4(aq) → I2(g) + SO42-(aq) + 2H2(g)

5. Halogen crushing reaction


The fifth experiment aims to test the pressure reaction of chlorine gas
on halogen salts. The experiment was carried out by filling test tube I with
sodium chloride solution flowing with chlorine gas and adding CS2 solution.
Produces a clear colorless solution and the solution is separated into 2
phases. CS2 functions as a catalyst to speed up reactions. With the following
reaction.
NaCl(aq) + Cl2(g) + CS2(aq) → NaCl(aq) + Cl2(g) + CS2(aq)
Then in test tube II, Tube II was filled with a solution of potassium
bromide flowing with chlorine gas plus CS2 solution. Produces a clear
colorless solution and the solution is separated into 2 phases. with the
following reaction.
2KBr(aq) + Cl2(g) + CS2(aq) → 2KCl(aq) + Br2(g) + CS2(aq)
Last, in test tube III, Tube III was filled with a solution of potassium
iodide flowing with chlorine gas plus CS2 solution. Produces a clear
colorless solution and the solution is separated into 2 phases. with the
following reaction.
2KI(aq) + Cl2(g) + CS2(aq) → 2KCl(aq) + I2(g) + CS2(aq)
The results of the three test tubes, namely the formation of 2 layers,
indicate that the chlorine gas is pressing I ions to form potassium chloride
salts and I2 gas.

6. Solubility of I2 in several solvents


The sixth (final) experiment aims to find out the solubility of I2 (s) in
several solutions. I2 in the form of a gray solid crystal is put into 3 test tubes
with a mass of approximately the same, before I2 was washed with distilled

30 | (C h l o r , B r o m a n d I o d )
water by placing it on filter paper and then dripping with distilled water on
it. Test tube one is added with H2O as much as 10 drops, waited for about
10 minutes and its solubility is observed. Test tube two was added with KI
solution as much as 10 drops, waited for about 10 minutes and its solubility
is observed. Test tube three was added to the concentrated HCl solution
and as much as 10 drops, waited for about 10 minutes and its solubility is
observed.
The final result shows that the color of the solution in test tube one is
yellowish; the solution in the test tube two is brown; the solution in the test
tube three is orange. This indicates that the most soluble (with indicators the
more concentrated the color the higher the solubility) is I2 plus KI. With the
level of solubility sorted from the least / difficult to dissolve: I2 + H2O <I2
+ HCl < I2 + KI. By the reaction:
I2(s) + H2O(l) →
I2(s) + KI(aq) → KI3(aq)
I2(s) + 2HCl(aq) → 2HI(aq) + Cl2(g)
Since I2 is a non-polar covalent molecule, it does not ionize in water.
It cannot also be soluble in the polar water. KI, which is a polar, ionic
compound, will ionize and dissolve in water. When KI dissolves in water, it
ionizes to K+ and I−. The I− will react with I2 to form the complex ion I3−.
I3− being negatively charged will dissolve in water.

I. CONCLUSION
From the experiment that have been done, it can conclude that Cl2 and Br2
gas can be synthesized in the laboratory by reacting the salts with MnO2 and
H2SO4. Making HCl in the form of gas can use H2SO4 reagents. While the
manufacture of HBr gas and HI gas cannot use H2SO4 reagents because H2SO4
is a strong oxidizer that will oxidize HBr to Br2 and oxidize HI to I2, so for HBr
and HI gases H3PO4 reagents are used. Some properties possessed by chlorine
and its compound: The ability of chlorine to fade color on color paper, the more
the composition of chlorine gas, the faster the solution to fade the color; chlorine
gas is pressing I ions to form potassium chloride salts and I2 gas. Last is

31 | (C h l o r , B r o m a n d I o d )
regarding the solubility of I2, the level of solubility sorted from the least /
difficult to dissolve: I2 + H2O <I2 + HCl < I2 + KI.

32 | (C h l o r , B r o m a n d I o d )
REFERENCES

Al-Weshah, R. A. (2000). The water balance of the Dead Sea: An integrated


approach. Hydrological Processes, 14(1), 145–154.
https://doi.org/10.1002/(SICI)1099-1085(200001)14:1<145::AID-
HYP916>3.0.CO;2-N
Greenwood, N. N. (Norman N., & Earnshaw, A. (Alan). (1997). Chemistry of the
elements (2nd ed.). Oxford: Butterworth-Heinemann.
Kogel, J. E., Trivedi, N. C., Barker, J. M., & Krukowski, S. T. (2006). 101.3.2 Slip
Casting. In Industrial Minerals and Rocks - Commodities, Markets, and Uses.
Society for Mining, Metallurgy, and Exploration (SME). Retrieved from
https://app.knovel.com/hotlink/pdf/id:kt008MHCD2/industrial-minerals-
rocks/slip-casting BT - Industrial Minerals and Rocks - Commodities,
Markets, and Uses (7th Edition)
Schmittinger, P., Florkiewicz, T., Curlin, L. C., Lüke, B., Scannell, R., Navin, T.,
… Bartsch, R. (2006). Chlorine. In Ullmann’s Encyclopedia of Industrial
Chemistry. Weinheim, Germany: Wiley-VCH Verlag GmbH & Co. KGaA.
https://doi.org/10.1002/14356007.a06_399.pub2
Tallmadge, J. A., Butt, J. B., & Solomon, H. J. (1964). Minerals from sea salt.
Industrial and Engineering Chemistry, 56(7), 44–65.
https://doi.org/10.1021/ie50655a008
Wiberg, E., Wiberg, N., & Holleman, A. F. (Arnold F. (2001). Inorganic chemistry.
Academic Press.

33 | (C h l o r , B r o m a n d I o d )
ATTACHMENTS

A. Documentation

[1st Experiment] [1st Experiment] [1st Experiment]


MnO2(s) MnO2(s) + NaCl (s) Heating process

[1st Experiment] filter


paper charged with gas
st
[1st Experiment] tested [1 Experiment] tested (NaCl)
with litmus paper with litmus paper

(NaCl) (KBr)

[1st Experiment] filter [2nd Experiment] The [2nd Experiment] The


paper charged with gas final result of three test final result of three test
(KBr) tube (with NaCl) tube (with KBr)

34 | (C h l o r , B r o m a n d I o d )
[3rd Experiment] the [3rd Experiment] 3rd Experiment]
final result and Ca(OCl)2 + H2O + Ca(OCl)2 + H2O +
comparison of two test colored paper (Tube 1) colored paper (Tube 2)
tube

[4th Experiment] NaCl [4th Experiment] test [4th Experiment]


(s) + H2SO4 tube connected with heating process
concentrated hose to test tube filled
with water

[4th Experiment] the


final result of three test
tube

[5th Experiment] test [5th Experiment] the


tube charged with final comparison result
chlorine gas from three test tube

35 | (C h l o r , B r o m a n d I o d )
[6th Experiment] the
final result and
solubility comparison

[6th Experiment] I2 (s) [6th Experiment] I2 from three test tube

washed with H2O solid

B. Question Answers
1. Explain the manufacture of chlorine gas in the laboratory?
Answer:
The process to produce chlorine was to heat brine with acid and
manganese dioxide.
2NaCl + 2H2SO4 + MnO2 → Na2SO4 + MnSO4 + 2H2O + Cl2
Using this process, chemist Carl Wilhelm Scheele was the first to
isolate chlorine in a laboratory. The manganese can be recovered by the
Weldon process. Small amounts of chlorine gas can be made in the
laboratory by putting concentrated hydrochloric acid in a flask with a side
arm and rubber tubing attached. Manganese dioxide is then added and the
flask stoppered. The reaction is not greatly exothermic. As chlorine is denser
than air, it can be easily collected by placing the tube inside a flask where it
will displace the air. Once full, the collecting flask can be stoppered.
Another method for producing small amounts of chlorine gas in a lab
is by adding concentrated hydrochloric acid (typically about 5M) to sodium
hypochlorite or sodium chlorate solution. Potassium permanganate can be
used to generate chlorine gas when added to hydrochloric acid.

2. What is the use of chlorine gas and its compounds?


Answer:

36 | (C h l o r , B r o m a n d I o d )
Applications of chlorine
Sodium chloride is by a huge margin the most common chlorine
compound, and it is the main source of chlorine and hydrochloric acid for
the enormous chlorine-chemicals industry today. About 15000 chlorine-
containing compounds are commercially traded, including such diverse
compounds as chlorinated methanes and ethanes, vinyl chloride and its
polymer polyvinyl chloride (PVC), aluminium trichloride for catalysis, the
chlorides of magnesium, titanium, zirconium, and hafnium which are the
precursors for producing the pure elements, and so on.
Combating putrefaction
Labarraque's research resulted in the use of chlorides and
hypochlorites of lime (calcium hypochlorite) and of sodium (sodium
hypochlorite) in the boyauderies. The same chemicals were found to be
useful in the routine disinfection and deodorization of latrines, sewers,
markets, abattoirs, anatomical theatres, and morgues.
Disinfection
Labarraque's chlorinated lime and soda solutions have been advocated
since 1828 to prevent infection (called "contagious infection", presumed to
be transmitted by "miasmas"), and to treat putrefaction of existing wounds,
including septic wounds.
Public sanitation
The first continuous application of chlorination to drinking U.S. water
was installed in Jersey City, New Jersey in 1908. By 1918, the US
Department of Treasury called for all drinking water to be disinfected with
chlorine. Chlorine is presently an important chemical for water purification
(such as in water treatment plants), in disinfectants, and in bleach. Even
small water supplies are now routinely chlorinated.

3. Write reaction equations in all experiments?


Answer:
1) Manufacture and identification of Cl2 and Br2 gas
Reactions:

37 | (C h l o r , B r o m a n d I o d )
MnO2(s) + NaCl(s) + H2SO4(aq) → Na2SO4(aq) + MnSO4(aq) +
H2O(l) + Cl2 (g)
2I-(aq) + Cl2(g) → I2(g) + 2Cl-(aq)
MnO2(s) + KBr(s) + H2SO4(aq) → K2SO4(aq) + MnSO4(aq) + H2O(l) +
Br2 (g)
2I-(aq) + Br2(g) → I2(g) + 2Br-(aq)

2) The properties of chlorine, bromine, iodine and its compounds


Reactions:
AgNO3(aq) + NaCl(aq) → NaNO3(aq) + AgCl(s)
HgNO3(aq) + NaCl(aq) → NaNO3(aq) + HgCl(s)
(CH3COO)2Pb(aq) + 2NaCl(aq) → 2CH3COONa(aq) + PbCl2(s)
AgNO3(aq) + KBr(aq) → KNO3(aq) + AgBr(s)
HgNO3(aq) + KBr(aq) → KNO3(aq) + HgBr(s)
(CH3COO)2Pb(aq) + KBr(aq) → 2CH3COOK(aq) + PbBr2(s)

3) The properties of chlorine, bromine, iodine and its compounds


Reactions:
CaOCl2(s) + H2O(l) + CO2(g) → CaCO3(aq) + HOCl(aq) + CaCl2(aq)
HOCl(aq) + H+ + Cl- → Cl2(g) + H2O(l)

4) Manufacture and identification of HCl, HBr and HI


Reactions:
NaCl(s) + H2SO4(aq) → HCl(aq) + NaHSO4(aq)
2KBr(s) + 4H2SO4(aq) → Br2(g) + 2SO2(aq) + 4H2O(l) + 2KSO4(aq)
2I-(aq) + 2H2SO4(aq) → I2(g) + SO42-(aq) + 2H2(g)

5) Halogen crushing reaction


Reactions:
NaCl(aq) + Cl2(g) + CS2(aq) → NaCl(aq) + Cl2(g) + CS2(aq)
2KBr(aq) + Cl2(g) + CS2(aq) → 2KCl(aq) + Br2(g) + CS2(aq)
2KI(aq) + Cl2(g) + CS2(aq) → 2KCl(aq) + I2(g) + CS2(aq)

38 | (C h l o r , B r o m a n d I o d )
6) Solubility of I2 in several solvents
Reactions:
I2(s) + H2O(l) →
I2(s) + KI(aq) → KI3(aq)
I2(s) + 2HCl(aq) → 2HI(aq) + Cl2(g)

4. Why can't iod dissolve in water but dissolve in a solution of potassium


iodide?
Answer:
Since I2 is a non-polar covalent molecule, it does not ionize in water.
It cannot also be soluble in the polar water. KI, which is a polar, ionic
compound, will ionize and dissolve in water. When KI dissolves in water, it
ionizes to K+ and I−. The I− will react with I2 to form the complex ion I3−.
I3− being negatively charged will dissolve in water.

5. How the sediment produced in experiment no. 2?


Answer:
In theory Ag, Hg, and Pb are type I cations that can form precipitate
if they react to form halide salts. However, in practicum, only Ag is
observed to form sediment (with a maximum of 25-30 drops of drops). The
reason for this is the possibility that sediments have been formed that have
not been directly observed by the eye, impurities used, or the concentration
of the solution used is too small. From these experiments it can be related
to the concept that group I reacts strongly with the halide group, and the salt
formed has a very small Ksp so it easily settles.

6. Why did experiment 4 not produce HBr and HI?


Answer:
The final results show that after the solution is heated HBr gas is not
formed but Br2 gas is formed, due to strong oxidative sulfuric acid which
will oxidize HBr to Br2. While with Iodine, After the solution is heated not
formed HI but I2, because sulfuric acid is a strong oxidizing agent which
will oxidize HI to I2.

39 | (C h l o r , B r o m a n d I o d )