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I.

Title of Experiment : Chlorine, Bromine, and Iodine


II. Date of Experiment : Wednesday, 25th of September at 09.30-12.00
III. Purposes of Experiment
1. To know the properties of chlorine, bromine, iodine, and its compound
2. To identify chlorine, bromine, iodine, and its compound
3. To recognize how to make chlorine, bromine, and iodine gas
IV. Basic Theory
A. Halogens (Chlorine, Bromine, and Iodine)
None of the halogens occur in the elemental state in Nature; this is because of their
high reactivity. The increase in color of the elements and of theircovalent
compounds with increasing size is due in general to a progressive shift of
electronic absorption bands to longer wavelegths in the absorption spectrum
(Cotton & Wilkinson, 1930).
Halogens forms diatomic molecules (of the form X2, whre X denotes a halogen
atom) in their elementa states. As a general rule, fluorine is the most reactive
halogen and astatine is the last reactive. All halogens form group 1 salts with
similar properties. In addition, halogens act as oxidizing agents. Therefore, most of
the chemical reactions that involve halogens are oxidation-reduction reactions in
aqueous solution (Hill & Holman, 2000).
Chlorine has the atomic number 17. It was discovered in 1974 by extracting it rom
hydrochloric acid. At room temperature it appears as a light green gas. Most
abundant compound of chlorine is sodium chloride (NaCl). The reaction are
below:
H2SO4(aq) + NaCl → HCl + NaHSO4
4 HCl + MnO2 → MnCl2 + 2H2O + Cl2 (Lutfi, 2016)
Chlorine has such similar and chemical properties with bromine and iodine that it
is convenient to consider the together (McQuarrie, 2011).
All three halogens could be prepared by the oxidation of halide salt by manganese
dioxide in concentrated sulfuric acid, for example;
2NaCl (s) + 4H+ (aq) + MnO2 (s) → Mn2+ (aq) + 2Na+ (aq) + 2H2O (l) + Cl2 (g)
(McQuarrie, 2011).
Chlorine is evolved which is identified by its suffocating odour, yellowish-green
colour, and turning of potassium iodide-starch paper blue (Shevla, 1979).
The formation of free chlorine, bromine, and iodine may be effected by one of two
chemical methods: (i) oxidation of halide derivatives, and (ii) reduction of

1
compounds of the halogens in positive oxidation states, e.g. ClO− or IO3− (Downs &
Adams, 1973).
Iodine occurs as iodide in brines and in the form of sodium and calcium
iodates.production of iodine involves either oxidizing I − or reducing iodates to I−
followed by oxidation to the elemental state. A commonly used oxidation reaction,
and one suited to laboratory use when necessary, is oxidation of I − in acid solution
with MnO2 (also used for preaparation of Cl2 and Br2 from X − ) (Cotton &
Wilkinson, 1930).
Iodine is a black solid with a sllight metallic luster. At atmosperic pressure it
sublimes (violet vapor) without melting. Its solubility in water is slight. It is
readily soluble in nonpolar solvents such as CS2 and CCl4 to give violet solutions;
spectroscopic studies indicate that ”dimerization” occurs in solutions to some
extent:
2I2 ⇌ I4 (Cotton & Wilkinson, 1930).
Iodine solution are brown in solvents such as unsaturated hydrocarbons, liquid
SO2, alcohols, and ketones, and pinkish brown in benzene.
Iodine forms the well-known blue complex with the amylose form of starch
(Cotton & Wilkinson, 1930).
The halogens are all to some extent soluble in water. Depending on the precise
conditions of pH, all three halogens should threfore be capable of oxidizing water.
In contrast with the behaviour of fluorine, the reaction tends to be slow, however,
and disproportiionation is the initial result:
X2 + H2O ⇌ HOX + H+ + X −
The weak hypohalous acid so produced then undergoes slow decomposition, e.g
HOCl → HCl + ½ O2
2HOBr → Br2 + H2O + ½ O2 (Downs & Adams, 1973)
Below are the appearencae and the colour of some halogens.
Halogen In Pure Forms In non-polar Solvents In Water
Chlorine Pale green gas Pale green gas Pale green solution
Bromine Dark red liquid Orange solution Orange solution
Iodine Grey Solid Purple solution − (Insoluble) but forms
a brown solution it
excess Ki is present

2
The halogens are usually used in aqueous solution. Although iodine is insoluble in
water, it is soluble if iodidie ions are present. The iodine reacts with iodide ions to
for triiodide ions as follows.
I2(aq) + I− (aq) → I3− (aq)
The triiodide ions give the solution its brown colour (Ramsden, 2000).
B. Reaction with silver ions
The silver (I) ion, Ag+, forms insoluble precipitates with the chloride, bromide, and
iodide ions. The following reactions take place
Ag+ (aq) + Cl− (aq) → AgCl (s) white precipitation
Ag+ (aq) + Br − (aq) → AgBr (s) cream precipitation
Ag+ (aq) + I− (aq) → AgI (s) yellow precipitation (Ramsden, 2000)
C. Displacement reactions between halogens and halides ion
The displacement reactions of halogens with halide ions provides a clear
illustration of the trends in oxidazing properties of halogens and the trends in
reducing properties of the halide ions in aqueous solution.
The more reactive halogens (i.e the strongest oxidizing agents) will displace the
more reactive halides from solution of thei ions:
− Chlorine will displace bromide snd iodides ion from solution
− Bromine will displace iodide from solution, butrot chloride ions. Reaction as
follows:
1. Cl2 (g) + 2Br − (aq) → 2Cl− (aq) + Br2 (aq)
Orange colour will appear in solution
2. Cl2 (g) + 2I− (aq) → 2Cl− (aq) + I2 (aq)
Brown colour will appear in solution on chlorine addition
3. Br2 (g) + 2I − (aq) → 2Br − (aq) + I2 (aq)
Brown colour will appear in solution (Ramsden, 2000).
D. Reaction of halide ions with concentrated sulphuric acid
The variation in reducing strength of the halides can be clearly seen in the reaction
of the sodium halideswith concentrated sulphuric acid.
1. Concentrated sulphuric acid is a strong acid can convert the sodium salts of the
halides into the hydrogens halides:
2. Concentrated sulphuric acid, as an oxidizing agent, it can be reduced either to
SO2, to S, or to H2S
H2SO4 + 2H+ + 2e− → SO2 + 2H2O
H2SO4 + 6H+ + 6e− → S + 2H2O
3
H2SO4 + 8H+ + 8e− → H2S + 4H2O
3. Chloride ions (Cl− ) is not strog reducing agent so it is not oxidised by H2SO4.
Only the acid-base reaction takes place and HCl gas is formed
H2SO4 + Cl− → HSO−
4 + HCl

White fumes of HCl will be seen. The fumes will turn blue litmus paper red
(Ramsden, 2000).
V. Tools and Materials
A. Tools
1. Pippettes ± 10pcs
2. Funnel glass 1 pc
3. Beaker glass 100 ml ± 3pcs
4. Statif and clam 1 set
5. Porcelain spoon 1 pc
6. Spatula 1 pc
7. Pipe-side test tube 1 pc
8. Asbes glass 1 pc
9. Rubber cover 1 pc
10. Hose ± 3pcs
11. Beaker glass 250 ml ± 2 pcs
12. Asbes gauze 1 pc
B. Materials
1. MnO2 crystal 1 spoon spatula
2. HCl 0,1 M ± 3 ml
3. Ca(OCl)2 1 spoon spatula
4. H2SO4 concentrated ± 3 ml
5. NaCl 0,1 M ± 1 ml
6. AgNO3 0,1 M ± 2 ml
7. HgNO3 0,1 M ± 2 ml
8. KI solution 0,1 M ± 1 ml
9. Pb(CH3COO)2 0,2 M ± 2 ml
10. Amylum solution ± 2 ml
11. KBr solution ± 1 ml
12. Salt 1 spoon spatula
13. KI, KBr crystal 1 spoon spatula
14. Colour paper 1 – 2 sheets
15. CS2 solution ± 3 ml

4
VI. Lanes Work and Reaction
1.
A tip teaspoon of powdered MnO2
− Entered into test tube
− Added some pieces of NaCl
− Added a bit of H2SO4 solution
− Observed the changes
− heated
Gas
− Put the filter paper that already given KI solution and amylum
on the top of gas
− Observed the color changes of gas formed
− Repeated the same steps for KBr
Gas color is changed

Reaction:
− MnO2 (s) +NaCl (s) + H2SO4 (aq) → Na2SO4 (aq) + MnSO4 (aq) + 2 H2O
(l) + Cl2 (g)
− 2KI (aq) + Cl2 (g) → I2 (g) + 2KCl (aq)
− MnO2 (s) + KBr (aq) + H2SO4 (aq) → K2SO4 (aq) + MnSO4 (aq) + 2H2O (l)
+Br2 (g)
− 2KI (aq) + Br2 (g) → I2 (g) + 2KBr (aq)

− n + nI2 →

CH2OH CH2OH
O O
I I I
OH H OH
O O O

H OH OH I n
I I

2. 1 mL NaCl 1 mL NaCl 1 mL NaCl

− Added into test tube − Added into test tube − Added into test tube
− Added AgNO3 0.1 M − Added HgNO3 0.1 M − Added Pb(CH3COO)2 0.1 M
− Compared all of the precipitation color
− Repeated all the steps for KBr solution

Color precipitation

5
Reaction:
− NaCl (aq) + AgNO3 (aq) → AgCL (s) + NaNO3 (aq)
− NaCl (aq) + Hg(NO)3 (aq)  HgCl (s) + NaNO3 (aq)
− 2NaCl (aq) + Pb(CH3COO)2 (aq)  PbCl2 (s) + 2CH3COO Na(aq)
− KBr (aq) + AgNO3 (aq)  AgBr (s) + KNO3 (aq)
− KBr (aq) + HgNO3 (aq)  HgBr (s) + KNO3 (aq)
− KBr (aq) + Pb(CH3COO)2 (aq)  PbBr2 (s) + KCH3COO (aq)

3. A small spoon of calcium hypochlorite

− Entered into beaker glass


− Added one test tube distilled water
− Stirred the filtered

Residue Filtrat
e − Divided into two parts

Filtrate Filtrat
1 − Added 1 ply colored-tissue − Added some
− Let it in open-room drops of HCl 0.1
− Observed the changes M solution
− Added 1 ply
Result colored-tissue
− Observed the
changes

Result

Reaction
− 2Ca(COCl)2 (aq) + H2O (l)  2HOCl (aq) + Ca(OH)2 (aq)
− HOCl (aq) + HCl (aq)  Cl2 (g) + H2O (l)

4. One little spoon NaCl

− Entered into test tube


− Added concentrated H2SO4 solution
− Close the test tube with rubber cover and connected hole to water
in beaker glass
− Heated slowly and wait for a few minutes

6
Gas
− Tested the water in beaker glass with litmus paper
− Repeated the experiment for KBr and KI
− Tested the gas with litmus paper − Tested by filter paper that
already given KI-starch
Litmus paper changed color Blue color
into red

Reaction:
− 2NaCl (aq) + 2H2SO4 (aq)  Cl2↑ (g)+ Na2SO4 (aq) + SO2 + 2H2O (l)
− 2KBr (aq) + 2H2SO4 (aq)  Br2↑ (g) + K2SO4 (aq) + SO2 + 2H2O (l)
− 2I- (aq) + 2H2SO4 (aq)  I2↑ (g) + SO2 +SO24- (aq) + 2H2O (l)
− KBr (s) + H2SO4 (aq)  Br2 (g) + SO2 (aq) + 2K2 SO4 (aq) + 2H2O (aq)
− Br2 + I −  Br- + I2
− 2KI (s) + H2SO4 (aq)  HI (g) + KHSO4 (aq)

− n + nI2 →

CH2OH CH2OH
O O
I I I
OH H OH
O O O

H OH OH I n
I I

5.
1 mL NaCl 1 mL NaCl 1 mL NaCl

− Connected by chlorine gas slowly


− Added CS2 solution
− Compared the color

Formed 2 layers Formed two layers Formed two layers

7
Reaction:
− NaCl (aq) + Cl2 (g) + CS2 (aq)  NaCl (aq) + Cl2 (g) + CS2 (aq)
− 2KBr (aq) + Cl2 (g) + CS2 (aq)  2 KCl (aq) + Br2 (g) + CS2 (aq)
− 2KI (aq) + Cl2 (g) + CS2 (aq)  2 KCl (aq) + I2 (g) + CS2 (aq)

6.
Iodine stone

− Entered into two different test tubes

test tube test tube test tube


1 2 3
− Added H2O − Added KI − Added HCl
− Compared − Compared − Compared

Little bit The most soluble Soluble and


soluble and and red-brick orange solution
yellow solution solution

Reaction:
 I2 (s) + H2O (l) → HI (aq) + HIO (aq)
 I2 (s) + KI (aq)  KI3 (aq)
 I2 (s) + 2HCl (aq) 2HI (g) + Cl2 (g)

8
VII. Observation Result
No Lanes work Observation Result Hypotheses/ reaction Conclusion
1. − Prepared the apparatus and materials Before  MnO2 (s) +NaCl (s) + H2SO4 (aq) → Based on the
− Entered a tip teaspoon of powdered  MnO2 : black powder Na2SO4 (aq) + MnSO4 (aq) + 2 H2O (l) experiment, it can

MnO2 into test rube  NaCl : white crystal + Cl2 (g) be concluded that
− Then, added some pieces of NaCl  H2SO4 : colorless  2KI (aq) + Cl2 (g) → I2 (g) + 2KCl (aq) Bromine and
− Continue with added a bit of H2SO4 solution  MnO2 (s) + KBr (aq) + H2SO4 (aq) → chlorine gas
solution  KI : colorless solution K2SO4 (aq) + MnSO4 (aq) + 2H2O (l) formed shown by
− Then observed the changes  Amylum : turbid +Br2 (g) the color changing
− After that, heated solution  2KI (aq) + Br2 (g) → I2 (g) + 2KBr (aq) of filter paper that
− The undergo reaction will formed gas  KBr : colorless The color of chlorine gas is greenish- has been dropped
− Then, put the filter paper that already solution yellow (MSDS, no year) with KI and
given KI and amylum solution After amylum into blue
The color of filter paper that already
− Observed the changes of gas color  MnO2 + NaCl : grey spot
given KI+amylum changed into blue
that formed in the filter paper crystal
− Then, repeated the same ways for  MnO2 + NaCl + H2SO4
KBr solution replacing NaCl (s) : grey solution, grey n+
precipitate (crystal) nI2 →
 Heated : melted CH2OH CH2OH
O O
I I
formed blackish-grey I
OH H OH
O O O
n
melt (liquid) I H OH
I
OH I

9
No Lanes work Observation Result Hypotheses/ reaction Conclusion
 Out the filter paper (KI
+ amylum) : blue spot
 MnO2 + KBr + H2SO4
: grey solution, grey
crystal (can not
dissolved)
 Heated : blackish-grey
melt (liquid)
 Tested with filter paper
(KI + amylum) : blue
spot
2. − First, added 1 ml NaCl solution into Before  NaCl (aq) + Hg(NO)3 (aq)  HgCl (s) Based on the
three different test tubes  NaCl : colorless + NaNO3 (aq) experiment, it can
− For the tube 1, added AgNO3 0.1 M; for solution  2NaCl (aq) + Pb(CH3COO)2 (aq)  be concluded that
the tube 2 added HgNO3 0.1 M; and for
 AgNO3 : colorless PbCl2 (s) + 2CH3COO Na(aq) the comparison of
the tube 3 added Pb(CH3COO)2 0.1 M
solution  KBr (aq) + AgNO3 (aq)  AgBr (s) + the amount of
− Then, compared all the precipitate color
 HgNO3 : colorless KNO3 (aq) precipitate is
− After that, continued with repeating the
same ways experiment for KBr solution
solution  KBr (aq) + HgNO3 (aq)  HgBr (s) + AgCl > PbCl2 >

replacing NaCl solution  Pb(CH3COO)2 : KNO3 (aq) HgCl2

colorless solution  KBr (aq) + Pb(CH3COO)2 (aq)  AgBr > PbBr >

10
No Lanes work Observation Result Hypotheses/ reaction Conclusion
 KBr : colorless PbBr2 (s) + KCH3COO (aq) HgBr
solution
After Ksp AgCl 1.77 x 10-10
 NaCl + AgNO3 : turbid Ksp Hg2Cl2 1.43 x 10-18
solution, formed Ksp PbCl2 1.70 x 10-5
precipitate (after 5 Ksp AgBr 5.35 x 10-13
drops) Ksp Hg2Br2 6.40 x 10-23
 NaCl + HgNO3 : Ksp PbBr2 6.60 x 10-6
colorless solution (after The comparison of the amount of
25 drops) precipitate is

 NaCl + Pb(CH3COO)2 PbCl2 < AgCl < HgCl2

: turbid solution, PbBr < AgBr < HgBr

formed precipate (after


5 drops, and let it for a
while turned into
colorless solution)
 KBr + AgNO3 : turbid
formed precipitate
(after 5 drops)
 KBr + HgNO3 :

11
No Lanes work Observation Result Hypotheses/ reaction Conclusion
colorless solution (after
25 drops)
 KBr + Pb(CH3COO)2 :
turbid solution, formed
precipate (after 5
drops, and let it for a
while turned into
colorless solution)
3. − A small spoon of calcium hypochlorite Before  2Ca(COCl)2 (aq) + H2O (l)  2HOCl Based on the
entered into beaker glass  Ca(OCl)2 : white (aq) + Ca(OH)2 (aq) experiment, it can
− Then, added one test tube-sized of powder  HOCl (aq) + HCl (aq)  Cl2 (g) + H2O be concluded that
distilled water  HCl : colorless (l) in tube 2 the time
− Stirred then filtered, and it will gives solution that needed for
residue and filtrate
 Ca(OCl)2 + H2O : tissue to change
− After that, divided the filtrate into two
turbid solution, white color for is faster
different test tubes
precipitate than tube 1.
− For the tube 1 added 1 ply colored-
tissue, let it in open room and observed
 Filtered : filtrate is

the changes colorless


− For the tube 2, added the filtrate with  Tube 1 (filtrate) :
some drops of HCl solution, then added colorless solution

12
No Lanes work Observation Result Hypotheses/ reaction Conclusion
1 ply of colored-tissue and observed the  Tube 2 (filtrate + HCl)
changes : colorless solution
− Finally, the colored-tissue will lost its
 Added 1 ply colored
color (paler)
tissue
-Tube 1 : pale (+)
-Tube 2 : pale (++)
4. − One little spoon of NaCl entered into Before  2NaCl (aq) + 2H2SO4 (aq)  Cl2↑ (g)+ Based on the
test tube  NaCl : white crystal Na2SO4 (aq) + SO2 + 2H2O (l) experiment, it can
− Then, added concentrated H2SO4  Concentrated H2SO4 :  2KBr (aq) + 2H2SO4 (aq)  Br2↑ (g) + be concluded that
solution in the fume hood colorless solution K2SO4 (aq) + SO2 + 2H2O (l) the reaction yields
− Closed the test tube with rubber  KBr : white crystal  2I- (aq) + 2H2SO4 (aq)  I2↑ (g) + SO2 chlorine, bromine,
cover and connected the plastic hole  KI : white powder +SO24- (aq) + 2H2O (l) iodine gas or halide
to the water in the beaker glass After salts based on the
Tested with litmus paper will change the
− The undergo reaction will formed gas  NaCl + H2SO4 : NaCl test of litmus paper
color from blue into red
− Then, tested with litmus paper in the slightly dissolve and filter paper
beaker glass filled with water  Heated: NaCl − KBr (s) + H2SO4 (aq)  Br2 (g) + SO2
− The changes that occur is the litmus dissolved, formed gas (aq) + 2K2 SO4 (aq) + 2H2O (aq)
(little greenish-yellow − Br2 + I  Br + I2
− -
paper will changed its color
− After that, tested the gas with filter solution) − 2KI (s) + H2SO4 (aq)  HI (g) +
paper that already given KI and  Tested with litmus KHSO4 (aq)

13
No Lanes work Observation Result Hypotheses/ reaction Conclusion
amylum solution paper CH2OH CH2OH
O O

− The changes that occur is the filter - Blue → red O


OH H
O
OH
O

H OH OH
n + nI2
paper will appeared a colored-spot - Red → red
CH2OH CH2OH
− Repeated the same ways of  Tested with filter I
O
I O I
OH H OH
O O O
experiment for KBr and KI solution paper: nothing changed OH n
→ I H OH
I
I

replacing NaCl (s)


 KBr + H2SO4 : slightly
dissolve
 Heated: NaCl
dissolved, formed gas,
yellow solution
 Tested with litmus
paper : nothing
changed
 Tested with filter
paper: blue spot

 KI + H2SO4 : yellow
solution
 Heated: orange

14
No Lanes work Observation Result Hypotheses/ reaction Conclusion
solution
 Tested with litmus
paper :
- Blue → red
- Red → red
 Tested with filter
paper: nothing changed
5. − First, entered 1 mL NaCl solution, 1 mL Before  NaCl (aq) + Cl2 (g) + CS2 (aq)  NaCl Based on the
KBr solution, and 1 mL KI solution into  NaCl : colorless (aq) + Cl2 (g) + CS2 (aq) experiment, it can
three different test tubes solution  2KBr (aq) + Cl2 (g) + CS2 (aq)  2 be concluded that
− Connected each test tube with chlorine  KBr : colorless KCl (aq) + Br2 (g) + CS2 (aq) the reaction formed
gas from Experiment 1 solution  2KI (aq) + Cl2 (g) + CS2 (aq)  2 KCl two layers
− Then, added CS2 solution into each test
 KI : colorless solution (aq) + I2 (g) + CS2 (aq)
tube after given chlorine gas
 CS2 : colorless solution
− It will formed two layers
After
− After that, compared the color of each
solution  NaCl + Cl2 (g) :
colorless solution
 NaCl + Cl2 (g) + CS2 :
formed two layers (+)
 KBr + Cl2 (g) :
15
No Lanes work Observation Result Hypotheses/ reaction Conclusion
colorless solution
 KBr + Cl2 (g) + CS2 :
formed two layers (++)
 KI + Cl2 (g) : colorless
solution
 KI + Cl2 (g) + CS2 :
formed two layers
(+++)

6. − First, prepared an iodine stone and Before  I2 (s) + H2O (l) → HI (aq) + HIO (aq) Based on the
washed it using filter paper and dropped  Iodine stone : black  I2 (s) + KI (aq)  KI3 (aq) experiment, it can
with some water crystal  I2 (s) + 2HCl (aq) 2HI (g) + Cl2 (g) be concluded that
− Entered the same size and amount of  Distilled water : iodine cant
iodine stone into three different test tube colorless solution dissolved in water,
labelled with tube 1, tube 2, and tube 3
 KI : colorless solution dissolved in KO
− For the tube 1 added H2O, for the tube 2
 Concentrated HCl : solution, and
added KI solution, and for the tube 3
colorless solution slightly dissolved
added HCl solution
After in HCl solution
− Then, compared all the color solution
and its solubility  Iodine stone + distilled
water : orange solution,

16
No Lanes work Observation Result Hypotheses/ reaction Conclusion
black crystal (after 5
minutes : yellow pale
solution, black crystal)
 Iodine stone + KI : red
brick solution, black
crystal (after 5 minutes
: orange solution (+)
getting pale
 Tube 1 : I2 + H2O cant
dissolve
 Tube 2 : I2 + KI
dissolved
 Tube 3 : I2 + HCl
slightly dissolved

17
IX. Analysis and Explanation
The experiment that already started and done at Wednesday, September 25th
2019 at 9.30 – 12.00 have a title “Chlorine, Bromine, and Iodine” and have some
purpose that are:
1. To know the properties of chlorine, bromine, iodine, and its compound
2. To identify chlorine, bromine, iodine, and its compound
3. To recognize how to make chlorine, bromine, and iodine gas
A. First experiment
The first experiment is to find out how to make chlorine and bromine gas and
identify the gas by testing it with filter paper dropped by potaasium iodide (KI)
and amylum. In this experiment the produce of chlorine gas is called the Weldon
process.
1. Preparing the side-pipe test tube, its pipe also the rubber cover. The pipe is set
into the side-pipe test tube. The tube is filled with a tip of teaspoon of kawi
stone or manganese (MnO2). Kawi stone has grey grain appearance. Afterthat,
it is added by sodium chloride (NaCl) and sulfuric acid (H2SO4) solution. NaCl
is white crystal while H2SO4 is colourless solution. After NaCl addition the
mixture is grey grain. Then after H2SO4 addition, the solution is a murky black.
Afterthat, the side-pipe test tube is closed by rubber cover and it is heated. The
heating process produces white smoke coming out of the solution which is turn
becomes green when its cooled.
White smoke is chlorine which is yielded in that reaction. While the mixture is
melted formed blackish grey melt-liquid. The reaction which is happen are
below.
MnO2 (s) + NaCl (aq) + H2SO4 (aq)  Na2SO4 (aq) + MnSO4 (aq) + H2O (aq)
+ Cl2 (g)↑
Filter paper that has been dropped by KI and amylum is placed on the tip of
pipe. Earlier, the filter paper is white, KI and amylum are colourless. After the
filter paper is dropped by KI and amylum, the filter paper remaining white.
Then, after it is placed in the tip of pipe, the color turns purple due to the
release of iodine by chlorine gas. KI and amylum in this reaction is as an
indicator that the reaction yielded chlorine gas. While chlorine and KI has react
alike
2I − (aq) + Cl2 (g) → I2 (g) + 2 Cl- (aq)

18
Iodine which is product from the reaction between potassium iodide and
chlorine reacts with amylum form complex called iod-amylum complex. That’s
why the filter paper change into purple. The reaction between iodine and
amylum is shown below.

n + nI2 →

CH2OH CH2OH
O O
I I I
OH H OH
O O O

H OH OH I n
I I

Above are commonly used oxidation reaction which is oxidation of Cl− in acid
solution with MnO2. Acid solution here is sulphuric acid. Heating process is to
fasten the reaction occurs, while MnO2 as the oxidizer
2. Preparing the side-pipe test tube, its pipe also the rubber cover. The pipe is set
into the side-pipe test tube. The tube is filled with a tip of teaspoon of kawi
stone or manganese (MnO2). Kawi stone has grey grain appearance. Afterthat,
it is added by potassium bromide (KBr) and sulfuric acid (H2SO4) solution.
KBr is white powder while H2SO4 is colourless solution. After KBr addition
the mixture is grey grain. Then after H2SO4 addition, the solution is grey and
some crystal doesn’t dissolve. Afterthat, the side-pipe test tube is closed by
rubber cover and it is heated. The heating process produces smoke coming out
of the solution. The smoke is bromine which is yielded in that reaction. While
the mixture is melted formed blackish grey melt-liquid. The reaction which is
happen are below.
MnO2 (s) + KBr (aq) + H2SO4 (aq)  K2SO4 (aq) + MnSO4 (aq) + H2O (aq) +
Br2 (g)↑
Filter paper that has been dropped by KI and amylum is placed on the tip of
pipe. Earlier, the filter paper is white, KI and amylum are colourless. After the
filter paper is dropped by KI and amylum, the filter paper remaining white.
Then, after it is placed in the tip of pipe, the color turns purple due to the
release of iodine by chlorine gas. KI and amylum in this reaction is as an
indicator that the reaction yielded chlorine gas. While chlorine and KI has react
alike
19
2I − (aq) + Br2 (g) → I2 (g) + 2 Br − (aq)
Iodine which is product from the reaction between potassium iodide and
bromine reacts with amylum form complex called iod-amylum complex.
That’s why the filter paper change into purple. The reaction between iodine
and amylum is shown below.

n + nI2 →

CH2OH CH2OH
O O
I I I
OH H OH
O O O

H OH OH I n
I I

Above are commonly used oxidation reaction which is oxidation of Br − in acid


solution with MnO2. Acid solution here is sulphuric acid. Heating process is to
fasten the reaction occurs, while MnO2 as the oxidizer.
B. The second experiment is to find out the reaction of chlorine and bromine ions
with silver ions, mercury ions, and lead ions. The first experiment use 1 ml sodium
chloride (NaCl) solution which was filled in 3 differenttubes. Then the first tube is
added by some drops silver (I) nitrate (AgNO3) which is here we add AgNO3 as
muchb as 5 drops. NaCl is colourless solution while AgNO3 is also colourless. It is
yielding a clear, colorless solution and a white precipitate (+++). The second tube
is added by some drops mercury (I) nitrate as much as 25 drops and it produce a
clear and colorless solution. The third tube is added 5 drops lead (I) acetate
produces a clear, colorless solution, there is a white precipitate (++). According to
the following reaction equation:
1. Tube I: AgNO3 (aq) + NaCl (aq)  NaNO3 (aq) + AgCl (s)
2. Tube II: HgNO3 (aq) + NaCl (aq)  NaNO3 (aq) + HgCl (s)
3. Tube III: (CH3COO)2Pb (aq) + 2NaCl (aq)  2CH3COONa (aq) + PbCl2 (s)
The second experiment was to repeat the first experiment by replacing sodium
chloride solution with potassium bromide (KBr). So get the following results:
1. Tube I: AgNO3 (aq) + KBr (aq)  KNO3 (aq) + AgBr (s) Clear colorless
solution, white precipitate (+++)

20
2. Tube II: HgNO3 (aq) + KBr (aq)  KNO3 (aq) + HgBr (s) Clear colorless
solution
3. Tube III: (CH3COO)2Pb (aq) + 2KBr (aq)  2CH3COOK (aq) + PbBr2 (s)
Clear colorless solution, white precipitate (++).
Based on the theory, the precipitate has Ksp (solubility product constant) value.
Each product has different Ksp value. The value of the constant identifies the
degree of which the compound could dissolve in water. Based on the theory, the
higher the Ksp the more soluble the compound is. Here are the Ksp value of some
substances which is being a product in the reaction.
Compound Ksp
AgCl 1.77 x 10-10
Hg2Cl2 1.43 x 10-18
PbCl2 1.70 x 10-5
AgBr 5.35 x 10-13
Hg2Br2 6.40 x 10-23
PbBr2 6.60 x 10-6
So based on the theory, both Hg2Cl2 and Hg2Br2 should produce the most
precipitate in the same drops because they have the smallest Ksp in each part.
Among the chloride ions, Hg2Cl2 has the smallest Ksp and among the bromide
ions, Hg2Br2 also has the smallest Ksp. But in fact, both are hard to form
precipitate even becoming turbid eventhough it has been added 25 drops. In other
side, the biggest Ksp value is owned by PbCl2 and PbBr2 in each ions. So, actually
the solution should be harder to form precipitate. Yet the reality is not. PbCl2 and
PbBr2 could form white precipitate. While AgCl and AgBr is the easiest to form
precipitate.
The experiment which doesn’t fit with the theory could be caused by the tools or
another factors that could be affected the result.
C. The third experiment was to find out the manufacture of chlorine gas by reacting
chlorine with an aqueous solution containing chlorine, which was marked by the
fading of colored paper when dipped in this solution. The first process is
dissolving chlorine solids (CaOCl2) into water then the solution is filtered to
produce a clear, colorless filtrate. The filtrate was divided into 2 test tubes, the first
tube was added with colored paper and left in the open air so that the color paper
faded and produced chlorine gas.

21
CaOCl2 (s) + H2O(l) + CO2 (g)  CaCO3 (aq) + HOCl (aq) + CaCl2 (aq)
The second tube plus a solution of hydrochloric acid and color paper so that color
paper fades faster and produces chlorine gas, p this is due to the addition of acidic
solution that contains chlorine will increase the composition of chlorine in the
solution so that it accelerates the formation of chlorine gas and color paper fades
faster.
HOCl (aq) + H+ + Cl-  Cl2 (g) ↑ + H2O (aq)
D. The fourth experiment was to determine the produce of HCl, HBr, and HI gases
which were identified with blue litmus and filter paper moistened with KI and
starch solution.
1. The first tube was filled with solid sodium chloride (NaCl) and concentrated
sulfuric acid solution. The test tube then covered with a rubber cover which is
connected with pipe. Afterthat, the test tube is heated. The gas formed is
connected into a beaker containing water. After the solution is heated HCl gas
will be formed.
NaCl (s) + H2SO4 (aq)  HCl (g) + NaHSO4 (aq)
HCl gas will turn blue litmus paper to red because it is acidic, and filter paper
moistened with KI + amylum does not change color because iodine formation
cannot occur.
2. The second tube is given the same treatment as tube I but the sodium chloride
solid is replaced by the potassium bromide solid. 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 which is
dipped into aquades flowed the gas does not change color, but the filter paper
moistened with KI + amylum flowed the gas changes to purple due to the
release of iodine by bromine gas as shown below:
KBr (s) + H2SO4 (aq)  Br2 (g) + SO2 (aq) + 2K2 SO4 (aq) + 2H2O (aq)
Then, Br2 + I−  Br- + I2
After that the reaction between iodine and amylum is happen make the filter
paper turn to blue/purple

22
n + nI2 →

CH2OH CH2OH
O O
I I I
OH H OH
O O O

H OH OH I n
I I

3. The third tube is given the same treatment as the first and the second tube but
the solid is replaced by the potassium iodide solid. After the solution is heated,
HI gas is formed which has acid characteristics. It is shown that the blue litmus
which is dipped into aquades flowed the gas change into red and the red litmus
remains red, but the filter paper moistened with KI + amylum flowed the gas
doesn’t changes. The reaction shown below:
2KI (s) + H2SO4 (aq)  HI (g) + KHSO4 (aq)
After that the reaction between iodine and amylum is happen make the filter
paper turn to blue/purple
E. The fifth experiment is to test the pressing reaction of chlorine gas to halogen salts.
The experiment was carried out by filling test tube I with sodium chloride solution
flowed by chlorine gas which is produce in the first experiment. There’s no change
couldn’t be obsrved. Afterthat we add CS2 solution into the test tube. Produces
clear colorless solution, there are bubbles, the solution is separated into 2 layer
which means form two phases.
NaCl (aq) + Cl2 (g) + CS2 (aq)  NaCl (aq) + Cl2 (g) + CS2 (aq)
Chlorine gas forces the Cl− ion to form sodium chloride salt.
Tube II was filled with a solution of potassium bromide flowed with chlorine gas
the its is added by CS2 solution. It produces clear colorless solution, there are
bubbles, the solution is separated into 2 phases.
2KBr (aq) + Cl2 (g) + CS2 (aq)  2KCl (aq) + Br2 (g) + CS2 (aq)
Chlorine gas forces the Cl− ion to form potassium bromide salt and Br2 gas
Tube III is filled with a solution of potassium iodide flowed with chlorine gas and
CS2 solution is added. Produces clear colorless solution, there are bubbles, the
solution is separated into 2 phases.
2KI (aq) + Cl2 (g) + CS2 (aq)  2KCl (aq) + I2 (g) + CS2 (aq)

23
Chlorine gas forces I − ions to form potassium iodide salts and I2 gas.
F. The last experiment is to find out the solubility of I2 in solution. By inserting solid
grayish black I2 in 3 different tubes with the same amount.
1. Tube I is added aquades so the solution is clear yellow pale solution and there
is some I2 which is left after 5 minutes, this is because I2 is not soluble in
water.
I2 (s) + H2O (l)  I2 (s) + H2O (l)
2. Tube II is added potassium iodide (KI) solution so the solution is red brick
solution and a little I2 which is left. The I2 which is dissolve in KI is greater
than dissolve in water shown by the I2 which is left there. I2 which is added
with KI solution will form polyhide ion I3− so it dissolves more quickly. The
reaction whic
I2 (s) + KI (aq)  KI3 (aq)
3. Tube III is added with HCl so the solution is clear orange and there is I2 which
is still left. Deposits will dissolve but require a longer time, because HCl
solubility is smaller than KI. I2 will oxidize Cl-ions to form chlorine gas
according to the following equation:
I2 (s) + HCl (aq)  HI (g) ↓ + Cl2 (g)
X. Conclusion
Based on the experiment we have conudcuted and the explanation above, we culd
conclude that:
1. In the laboratory, chlorine gas can be made from NaCl and sulfuric acid with kawi
stone as an oxidizer which will produce white colored chlorine gas. It can also be
done to make bromine gas by replacing NaCl with KBr. The formed gas is tested
with filter paper moistened with KI and starch solution, so that if the gas is formed
iodine liberation will occur.
2. Halogens that react with Pb2 +, Ag +, and Hg + will form salts that do not dissolve
in water and produce precipitate
3. The ability of chlorine to fade color on color paper depends on the amount of
chlorine gas composition. The more the composition of chlorine gas, the faster the
solution to fade the color.
4. 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
5. Chlorine gas can undergo an urgent reaction. By urging Br and I from potassium
bromide and potassium iodide and expelling Cl from sodium chloride. Because the
halogen which is located higher in group VII A in a diatomic state is able to force
the halogen ion from the salt located below it, thus forming a chlorine salt.
24
6. Iodine is insoluble in water but dissolves in KI solution and slightly soluble /
imperfectly soluble in concentrated HCl solution. Because in KI solution, iodine
will form polyhide ion.
XI. References
Cotton, F. A., & Wilkinson, G. (1930). Advanced Inorganic Chemistry. New York:
John Wiley & Sons Inc.
Hill, G., & Holman, J. (2000). Chemistry in Context 5thEdition . United Kingdom:
Nelson Thornes.
Lutfi. (2016). Kimia Anorganik : Unsur-Unsur Golongan Utama . Yogyakarta:
Absolute Media.
Malcolm, D. (1965). The Natural Historty of Oxygen. The Journal of General
Psychology.
McQuarrie, D. A. (2011). General Chemistry Fourht Edition. United Kingdom:
University Science Book.
Ramsden, E. N. (2000). A-Level Chemistry . United Kingdom: Nelson Thornes.
Shevla. (1979). Vogel's Textboo of Macro and Semimicro Qualitative Inorganic
Analysis. United States of America: Longman, Inc.
XII. Answering Question
1. Explain how to make chlor gas in laboratory
Answer :
Chlor gas can be made by industrial or laboratory method. Based on experiment
that been done, chlor gas that producing in laboratory can be made by :
a. React MnO2 crystal with NaCl and H2SO4 with heated slowly, chlor gas will be
released. The function of heated as catalyst to speed up this reaction. For
identified the gas is resulted or not, can tested by filter paper that have dropped
KI and amylum solution. The paper will changed result blue color.
b. Filtrate of calcium hyphochlorite which added by HCl, the reaction willbe
released chlor gas and result bubble. For identified the gas is resulted or not,
can tested use ply colored paper, the part of paper entered into the solution, and
other part leave it in dry condition. The part which enteren into solution when
little dry will showing if the color paper changing become faded.
2. Mention use of chlor gas and its compound?
Answer :
Use of chlor gas and its compound consist of : PVC producing; solvent producing
of paint, to clean metal from fats, dry cleaning; to produce metals (Mg, Ti, Br2);
organic compound producing, insecticide; HCl used in metal industry. To extract
the metal; NaCl used as salt; KCl used as plant fertilizer; NH4Cl as fuels materials
of battery; NaClO used to breaching agent for fabric and paper; ClO- + coloring
25
agent  Cl- + colorless subtence; ZnCl2 as soldering iron; CaOCl2 as chlor
powder; [Ca(OCl2)2] as disinfectant agent in tap water; KCl as materials of
fireworks and matches.
3. Written reaction equation of all experiment?
Answer :
a. MnO2(s) + 2NaCl(s) + H2SO4(aq)  Na2SO4(aq) + MnSO4(aq) + 2H2O(l) +
Cl2(g)
2KI(aq) + Cl2(g)  I2(g) + 2KCl(aq)
MnO2(s) + 2KBr(s) + H2SO4(aq)  K2SO4(aq) + MnSO4(aq) + 2H2O(l) +
Br2(g)
2KI(aq) + Br2(g)  I2(g) + 2KBr(aq)

n + nI2 →

CH2OH CH2OH
O O
I I I
OH H OH
O O O

H OH OH I n
I I

b. NaCl(aq) + AgNO3(aq)  AgCl(s) + NaNO3(aq)


NaCl(aq) + HgNO3(aq)  HgCl(s) + NaNO3(aq)
NaCl(aq) + Pb(CH3COOH)2(aq)  PbCl2(s) + 2CH3COONa(aq)
KBr(aq) + AgNO3(aq)  AgBr(s) + KNO3(aq)
KBr(aq) + HgNO3(aq)  HgBr(s) + KNO3(aq)
KBr(aq) + Pb(CH3COOH)2(aq)  PbBr2(s) + 2CH3COOK(aq)
c. 2Ca(OCl)2(aq) + H2O(l)  2HOCl(aq) + Ca(OH)2(aq)
HOCl(aq) + HCl(aq)  Cl2(g) + H2O(l)
d. Tested by litmus paper
NaCl(s) + H2SO4(aq)  HCl(aq) + NaHSO4(aq)
KBr(s) + H2SO4(aq)  HBr(aq) + KHSO4(aq)
KI(s) + H2SO4(aq)  HI(aq) + KHSO4(aq)
Tested by KI-starch filter paper
2NaCl(s) + 2H2SO4(aq)  Cl2(aq) + Na2SO4(aq) + SO2(g) + 2H2O(l)
2KBr(s) + 2H2SO4(aq)  Br2(aq) + K2SO4(aq) + SO2(g) + 2H2O(l)
2KI(s) + 2H2SO4(aq)  I2(aq) + K2SO4(aq) + SO2(g) + 2H2O(l)
26
n + nI2 →

CH2OH CH2OH
O O
I I I
OH H OH
O O O

H OH OH I n
I I

e. NaCl(aq) + Cl2(g)  NaCl(aq) + Cl2(g)


2NaCl(aq) + CS2(aq)  Na2CS2(aq) + Cl2(g)

2KBr(aq) + Cl2(g)  2KCl(aq) + Br2(g)


2KBr(aq) + CS2(aq)  K2CS2(aq) + Br2(g)
2KI(aq) + Cl2(g)  2KCl(aq) + I2(g)
2KI(aq) + CS2(aq)  K2CS2(aq) + I2(g)
f. I2(s) + H2O(l)↛
I2(s) + KI(aq)  KI3(aq)
I2(s) + HCl(aq)  HI(aq) + ClI(aq)
4. Why iod can’t dissolve in water but can dissolve in potassium iodide solution?
Answer :
Because ion that dissolve in KI solution will be form polyhalide I3-, so that is
soluble in KI solution, whereas iod im water not dissolve because water can’t
oxidizing iod and not occur reaction between of both.
5. How the precipitate which resulted on experiment number 2?
Answer :
a. NaCl(aq) + AgNO3(aq)  AgCl(s) + NaNO3(aq)  result white precipitate
and the solution become turbid. Precipitate that result is so much and look so
clear.
NaCl(aq) + HgNO3(aq)  HgCl(s) + NaNO3(aq)  nothing precipitate result
until 25 dropped by NaCl, the solution still colorless.
NaCl(aq) + Pb(CH3COOH)2(aq)  PbCl2(s) + 2CH3COONa(aq)  result
white precipitate, but isn’t clear like AgCl precipitate. The solution become
turbid, but if the solution leave in open room the precipitate will lost and the
solution become colorless again.

27
b. KBr(aq) + AgNO3(aq)  AgBr(s) + KNO3(aq)  result white precipitate and
the solution become turbid. Precipitate that result is so much and look so clear.
KBr(aq) + HgNO3(aq)  HgBr(s) + KNO3(aq) nothing precipitate result until
25 dropped by NaCl, the solution still colorless.
KBr(aq) + Pb(CH3COOH)2(aq)  PbBr2(s) + 2CH3COOK(aq)  result white
precipitate, but isn’t clear like AgCl precipitate. The solution become turbid,
but if the solution leave in open room the precipitate will lost and the solution
become colorless again.
6. Why on experiment number 4 not result HBr and HI?
Answer :
Because HI and HBr can’t to obtained with using H2SO4 reactant, that is causing
H2SO4 is strong oxidator compound which will oxidizing HBr become Br2 and
oxidizing HI become I2

28
XIII. Attachment
Documetation

Figure 1. Preparation of Tools Figure 2. Preparation of Materials

First Experiment

Figure 3. Entering manganese into the Figure 4. NaCl crystal addition into test
test tube tube after manganese

Figure 5. Adding some Sulphuric acid Figure 6. Heating the test tube containing
0.1 M into test tube manganese, NaCl, and some drops H2SO4

Figure 8. Dropping amylum solution after


Figure 7. Dropping KI solution into KI solution dropping into filter paper for
filter paper for identifying gas identifying gas

Figure 9. Collecting the gas to be tested Figure 10. The filter paper change into
with filter paper which has already purple

29
given by KI and amylum

Second Experiment

Figure 12. Adding some drops (25 drops)


Figure 11. Entering 1 ml of NaCl to of HgNO3, some drops of AgNO3, and
three test tube some drops of (CH3COO)2Pb into each
test tube which has been contained 1 ml
of NaCl

Figure 13. The result of the


Precipitation

Third Experiment

Figure 14. A small spoon of Figure 15. Adding aquades into


hypochlorite is taken and put in beaker hypchlorite and stir it homogeneously
glass

Figure 17. The filtrate is divided into two


Figure 16. Filtering the solution parts

30
Figure 18. The filtrate after being
divided two parts and added 1 ply Figure 19. Comparison the result
colores (left), added HCl and 1 ply
colored tissue (right)

Fourth Experiment

Figure 20. One little spoon of NaCl Figure 21. One little spoon of KBr
entered into test tube

Figure 23. Initial appearance of red and


Figure 22. Added by concentrated blue litmus paper
sulphuric acid (H2SO4)

Figure 24. The gas is entered into Figure 25. Red litmus is remain red
aquades in beaker glass

31
Figure 27. Blue litmus change into red
Figure 26. Red litmus remain red (left), (left), red litmus remain red (right),) in KI
blue litmus change into red (Right) in test tube, while filter paper remain white
NaCl test tube

Fifth Experiment

Figure 28. Entering 1 ml of NaCl, 1 ml Figure 29. The final result after Chlorine
of KBr, 1 ml of KI into three different gas and CS2 addition
test tube

Sixth Experiment

Figure 30. After being washed, iodine


stone is entered into three different test Figure 31. The result after each test tube
tube with the same amount is added by H2O (Left), by KI (middle),
and by HCl (right)

32

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