A.

TITLE OF EXPERIMENT : Nitrogen and Ammonia

B. DATE AND TIME OF EXPERIMENT : Wednesday, 2nd October 2019 at
09.00 until 12.00
C. AIMS OF EXPERIMENT :
1. To know how to make nitrogen and ammonia gas in laboratory
2. To know the properties of nitrogen and ammonia and its compounds
3. To identify nitrogen and ammonia gas and its compounds

D. BASIC THEORIES
1. Nitrogen

2. Ammonia
E. TOOLS AND MATERIALS
1. Tools
a. Sided pipe erlenmeyer 100 ml 1 piece
b. Distilled jar 1 piece
c. Graduated cylinder 100 ml; 10 ml 1 & 1 piece
d. Tripod 1 piece
e. Statif and clamp 1 & 1 piece
f. Bunsen burner 1 piece
g. Wood stick 1 piece
h. Test tube sufficiently
i. Test tube shelf 1 piece
j. Dropped pipettes sufficiently
k. Container 1 piece
l. Spatula glass 1 piece
m. Analytical balance 1 piece
n. Rubber stop 1 piece
o. Beaker glass 3 pieces
2. Materials
a. NaNO2 crystal Sufficiently
b. NH4Cl crystal Sufficiently
c. Concentrated HCl Sufficiently
d. Concentrated H2SO4 Sufficiently
e. Ca(OH)2 Sufficiently
f. Starch solution Sufficiently
g. KI solution Sufficiently
h. Concentrated ammonia Sufficiently
i. H2SO4 1M; 0,1 M Sufficiently
j. FeSO4 0,2 M Sufficiently
k. Concentrated HNO3 Sufficiently
l. PP indicator Sufficiently
m. NH4OH 2M;0,1M Sufficiently
F. PROCEDURE
1. N2 gas forming

0,3 g of NaNO2 0,3 g of NH4Cl

- Diluted in 10 ml distilled - Diluted in 10 ml distilled water

water - Poured into separated funnel
- Poured into Erlenmeyer - Open the cap slowly and
flask carefully when the NaNO2
- Heated until shimmering already shimmering

Gas Form
- Place the gas that formed into graduated cylinder
with full water by standing upside down
- Measured the volume

Volume of gas

- Test with burning wood

The flame will off

Reaction :
NaNO2(s) + H2O(l) → NaNO2(aq)
NH4Cl(s) + H2O(l) → NH4Cl(aq)
NaNO2(aq) + NH4Cl(aq) → NaCl(aq) + N2(g) + 2H2O(l)
2. Identification and formation of NO gas

0,25 g of NaNO2

- Diluted into 2,5 ml distilled water

- Divided into 2 test tube

Test tube 1 Test tube 2

- Added 3-5 ml of H2SO4 1 - Added 2 ml of
M distilled water
- Observed the vapour and - Added 3-5 drops of
the colour of solution KI and starch solution
Brown yellowish - Added diluted H2SO4
solution and form gas Blackish purple
solution

Reaction :
NaNO2(s) + H2O(l) → NaNO2(aq)
Test tube I :
2NaNO2(aq) + H2SO4(aq) → Na2SO4(aq) + 2HNO2(aq)
3HNO2(aq) → HNO3(aq) + 2NO(g) + H2O(l)
Test tube II:
2NaNO2(aq) + H2SO4(aq) + 2KI(aq) → Na2SO4(aq) + K2SO4(aq) + NO(g)
+ I2(aq) + H2O(l)
 3. Brown ring test from NO

1 ml diluted HNO3 solution

- Entered into test tube

- Added 1 ml of H2SO4 concentrated
- Colled down
- Added 0,5 ml of FeSO4 0,2 M
- Poured carefully on test tube wall
- observed

Blackish purple solution

Reaction :
 4HNO3(aq) + 2H2SO4(aq) → 4NO(g) + O2(g) + 2H2SO4(aq)
 2NO3-(aq) + 4H2SO4(aq) + 6Fe2+ → 2NO(g) + 4SO42-(aq) + 6Fe3+(aq) +
4H2O(l)
 Fe2+(aq) + NO(g) → [Fe(NO)]2+(aq)

4. Ammonia properties test

1 ml of NH4OH 2M solution

- Entered into test tube

- Flowed H2S gas (from HCl+FeS)
- Added 1 ml NH4OH 0,1 M
- Shaked it with sulfur
- Filter it

Residue as yellow precipitate Filtrate

- Observed it

Yellow solution

- Added 1 ml HCl diluted

until form precipitate
- Observed

Yellow solution
 Reactions :
 2HCl(aq) + FeS(s) → H2S(g) + FeCl2(aq)
 2NH4OH(aq) + H2S(g) → (NH4)2S(aq) + H2O(l)
 (NH4)2S(aq) + S(s) → (NH4)2S2(s)
 (NH4)2S2(s) + HCl(aq) → NH4Cl(aq) + H2S(g) + S(s)+NH4SH(aq)

5. NH4Cl gas forming

2 ml of NH4Cl 4 M

- Entered into test tube

- Added a small amount of Ca(OH)2
- Heated slowly

Gas Form

- Test and observed

Litmus paper test HCl concentrated test

- Tested with litmus paper - Entered the stirrer that

above the test tube dipped in HCl concentrated
- Observed the gas

Red litmus become blue White vapour

Reactions :
 2NH4Cl(aq) + Ca(OH)2(s) → 2NH3(g) + CaCl2(aq) + 2H2O(l)
 NH3(g) + HCl(aq) → NH4Cl(g)
 NH4Cl gas is exist as white vapour
6. Ammonia properties test

5 ml of NH4OH concentrated

- Entered into erlenmeyer

- Heated slowly
- Placed the gas come put with dry test
tube that closed with rubber stop
- Wait in minutes
Gas form

- Tested with entered stirrer that dipped in

HCl concentrated

NH4Cl vapour

- Tested with PP indicator into beaker glas

with water in which a gas test tube has
been inserted
Pink solution

Reactions :
 NH4OH(aq) → NH3(g) + H2O(l)
 NH3(g) + HCl(aq) → NH4Cl(g)
 NH3(g) + H2O(l) → NH4OH
 NH4OH(aq)+HIn(aq) → NH4In(aq) + H2O(l)
 G. OBSERVATION RESULT
Result Observation
NO. Procedure Hypothesis or Reaction Conclusion
Before After
N2 gas formation and test  NaNO2 :  NaNO2 + H2O =  NaNO2(s) + H2O(l) → NaNO2(aq) According to the
a. 0,3 grams of NaNO2; diluted in 10 ml white colourless  NH4Cl(s) + H2O(l) → NH4Cl(aq) observation, the
distilled water crystal solution  NaNO2(aq) + NH4Cl(aq) → NaCl(aq) + gas which
b. 0,3 grams of NH4Cl; diluted in 10 ml  NH4Cl :  NH4Cl + H2O = N2(g) + 2H2O(l) produced is N2
distilled water white colourless  Theoretical volume which gotten = 86 mL gas, it proven by
c. Poured NaNO2 in the Erlenmeyer crystal solution  Theoretical flame test = the flame will turned off the
which placed over the Bunsen burner  Distilled  NaNO2 + turn off flame.
and the hose which connected to the water : NH4Cl =
1.
upside down graduated cyllinder colourless colourless
d. Poured NH4Cl in the separated funnel liquid solution
which already setting up over the  Heated = form
Erlenmeyer. bubbles
e. Heated the NaNO2, and observed the  Flame test =
changes turned off the
f. If the NaNO2 already in shimmering flame woof
phase (form little bubble and water
 Result Observation
NO. Procedure Hypothesis or Reaction Conclusion
Before After
vapour in Erlenmeyer wall), dropped  Volume gas
drop by drop of NH4Cl solution which gotten =
g. Observed the gas which form and 100mL
measured the volume
h. Do the flame test to gas which
formed
i. The gas will turned off
NO gas formation and properties testing  NaNO2 :  NaNO2(aq) + NaNO2(s) + H2O(l) → NaNO2(aq)  Gas can
a. 0,25 grams of NaNO2; diluted non white H2O(l) : Test tube I : produce by
2,5 ml distilled water crystal colourless 2NaNO2(aq) + H2SO4(aq) → Na2SO4(aq) + reaction of
b. Divided into 2 different test tube  H2SO4 : solution 2HNO2(aq) NaNO2 and
c. For test tube 1, added 3-5 drops of colourless Test tube 1 : 3HNO2(aq) → HNO3(aq) + 2NO(g) + H2SO4
2.
H2SO4 1M solution - NaNO2(aq) + H2O(l) (brown
d. Observed the colour and vapour that  Diluted H2O(l) = Test tube II: yellowish)
changes H2SO4 : colourless 2NaNO2(aq) + H2SO4(aq) + 2KI(aq) → which
e. For test tube 2, added 2 mL of colourless solution and Na2SO4(aq) + K2SO4(aq) + NO(g) + identify as
distilled water form bubble and I2(aq) + H2O(l) NO gas.
 Result Observation
NO. Procedure Hypothesis or Reaction Conclusion
Before After
f. Added 3-5 dropped of KI and starch solution brown gas.  The 2 test
solution  Distilled Test tube 2 : tube change
g. Added diluted H2SO4 water : - NaNO2(aq) + into dark
colourless H2O(l) = purple which
solution colourless identify as
 KI : solution NO gas.
colourless - + KI and starch
solution solution =
 Starch colourless
solution: solution.
colourless - + H2SO4 diluted
solution = form dark
purple solution.
Making complexes from NO  Diluted  HNO3 + H2SO4  4HNO3(aq) + 2H2SO4(aq) → 4NO(g) +  NO2 gas can
a. 1 ml dilutes HNO3 solution; entered HNO3 : concentrated : O2(g) + 2H2SO4(aq) be formed
3.
into test tube colourless colourless  2NO3-(aq) + 4H2SO4(aq) + 6Fe2+ → by reacted
b. Added 1 ml of H2SO4 concentrated solution solution HNO3
 Result Observation
NO. Procedure Hypothesis or Reaction Conclusion
Before After
and cooled down  H2SO4 :  After added 2NO(g) + 4SO42-(aq) + 6Fe3+(aq) + solution and
c. Added 0,5 M of FeSO4 0,2 M colourless FeSO4 : pale 4H2O(l) H2SO4 that
d. Poured carefully on test tube wall solution yellow solution  Fe2+(aq) + NO(g) → [Fe(NO)]2+(aq) proven by
e. Waited 2-3 minutes and observed it  FeSO4 0,2 and colourless brown ring.
f. The brown precipitate float between M : yellow solution (2
HNO3 and FeSO4 solution likely ring solution phase)
 after waited 3
minutes form
brown floated
precipitate
likely ring
between HNO3
and FeSO4.
Ammonia properties test  NH4OH 0,2  HCl+FeS : form  2HCl(aq) + FeS(s) → H2S(g) + FeCl2(aq) - H2S can
4. a. 1 ml of NH4OH 2M solution; entered M : H2S gas which  2NH4OH(aq) + H2S(g) → (NH4)2S(aq) + form by mix
into test tube colourless identify as H2O(l) HCl and FeS
 Result Observation
NO. Procedure Hypothesis or Reaction Conclusion
Before After
b. Flowed H2S, which form from HCl solution unpleasant  (NH4)2S(aq) + S(s) → (NH4)2S2(s) - (NH4)2S2
and FeS  HCl : odour and grey  (NH4)2S2(s) + HCl(aq) → NH4Cl(aq) + can react
c. Added 1 ml NH4OH 0,1 M, then colourless solution H2S(g) + S(s)+NH4SH(aq) with
shaked it carefully solution  +NH4OH 0,2 M  NH4Cl is white vapour NH4OH and
d. Filtered it, the residue is yellow and  FeS : black + H2S : H2S gas
the filtrate is clear yellow solution solid colourless with sulphur
e. Added 1 ml HCl diluted until form  NH4OH : solution - After added
precipitate colourless  + sulphur : with HCl
f. In final result, there is white solution yellow solution will turn to
precipitate and turbid solution  Sulphur: and yellow white turbid

yellow precipitate solution and

powder  After filtration; white

 HCl : the residue is precipitate

colourless pale yellow and which

solution the filtrate is identified as

clear yellow NH4Cl
 Result Observation
NO. Procedure Hypothesis or Reaction Conclusion
Before After
solution
 Filtrate + HCl;
become white
turbid and form
white
precipitate
NH4Cl gas forming  NH4CL 4M  NH4Cl +  2NH4Cl(aq) + Ca(OH)2(s) → 2NH3(g) + NH3 gas produce
a. 2 ml of NH4CL 4 M; entered in to : colourless Ca(OH)2 : white CaCl2(aq) + 2H2O(l) by reacted
test tube solution solution and  NH3(g) + HCl(aq) → NH4Cl(g) NH4Cl and
b. Added some small amount of  Ca(OH)2 : white  NH4Cl gas is exist as white vapour Ca(OH)2 it
Ca(OH)2 white precipitate proven by litmus
5. c. Heated it slowly powder  After heated : paper test which
d. Observed the gas forming in the  HCl : turbid solution change into red,
beaker glass concentrate  Litmus paper and kept the blue
e. After few minutes, test with HCl d colourless tested : change one.
concentrated which already dipped solution the red into blue NH4Cl gas also
by spatula proven with HCl
 Result Observation
NO. Procedure Hypothesis or Reaction Conclusion
Before After
f. Also test the gas forming using and kept the concentrated
litmus paper blue colour which form
 Forming white vapour.
unpleasant
odour and white
vapour
6. Ammonia properties test  NH4OH =  NH4OH+heated  NH4OH(aq) → NH3(g) + H2O(l)  NH4Cl gas
a. 5ml of NH4OH concentrated, entered colourless = forming gas  NH3(g) + HCl(aq) → NH4Cl(g) can form
into Erlenmeyer solution and bubble  NH3(g) + H2O(l) → NH4OH reacted
b. Heated it slowly  HCl =  Gas + HCl =  NH4OH(aq)+HIn(aq) → NH4In(aq) + NH4OH gas
c. Observed and placed the gas that colourless form white H2O(l) with HCl
form into dry test tube which is solution vapour concentrated,
already covered with rubber stop  PP indicator  PP indicator + proven with
d. Wait in minutes until the gas form : colourless distilled water + white vapour
e. Collect the gas to the distilled water solution gas = pink forming with
until enough and do PP indicator test solution unpleasant
f. Open the rubber stop, and do HCl
 Result Observation
NO. Procedure Hypothesis or Reaction Conclusion
Before After
concentrated test using spatula glass odour and
change the
PP indicator
into pink.
H. ANALYSIS AND EXPLANATION
I. REFERENCES

Lee, J. (1991). Concise Inorganic Chemistry. New York: Chapman and Hall.
Lutfi, A. e. (2018). Kimia Anorganik Unsur-Unsur Golongan Utama. Surabaya:
UNIPRESS.
Miessler, G., Fischer, P., & Tarr, D. (2014). Inorganic Chemistry. New York:
Pearson.
Svehla, G. (1979). Vogel's Textbook of Macro and Semimicro Qualitative
Inorganic Analysis. London: Longman.
Tim Penyusun, P. (2019). Panduan Praktikum Kimia Anorganik. Surabaya:
Jurusan Kimia.

J. QUESTION ANSWER
1. Explain how to make Cl2 gas in laboratory scale!
Answer :
In lab scale, Cl2 gas can produce by electrolysis process of its salt such as
NaCl either its solution or liquid by reaction below :
2NaCl(aq) + 2H2O(l) → 2NaOH(aq) + Cl2(g) + 2H2(g)
2NaCl(l) → 2Na(s) + Cl2(g)
Cl2 gas also can produce by reaction between NaCl and strong acid such as
H2SO4 with MnO2 as catalyst, this reaction named as oxidation reaction.
The reaction is written below :
MnO2(s) + NaCl(s) + H2SO4(aq) → Cl2(g) + Na2SO4(aq) + MnSO4(aq) +
2H2O(l)
Another method to produce Cl2 gas in lab scale is by oxidized HCl using
MnO2 by reaction below :
4HCl(aq) + MnO2(s)→Cl2(g) + MnCl2(aq) + 2H2O(l)
2. Mention the usage of Cl2 gas and its compound!
Answer:
a. Large amounts of chlorine are used for bleaching textiles, wood, pulp,
and paper.
b. Chlorine is widely used throughout developed world to purify drinking
water, because its ability to kills bacteria.
 c. Chlorine salt (NaCl) is important micronutrient for human body, it also
used as flavour for cooking.
d. Chlorine commonly used as an antiseptic and it used to treat
swimming pools and water container (calcium hypo chloric (CaClO)).
e. Another larger amounts of chlorine used for plastics, dyes, medicine,
antiseptics, insecticides, solvents, and paints
f. HCl when mixed with H2O forms hydrochloric acid, a strong
commercially important acid.
g. Chloroform (CHCl3) used as solvent and anaesthetic.
3. Write all the reactions in this experiment!
Answer :
a. Chlorine and Bromine Production by Oxidation its salts using MnO2
MnO2(s) + 2NaCl(s) + 2H2SO4(aq) → Cl2(g) + 2H2SO4(aq) +
MnSO4(aq) + 2H2O(l)
MnO2(s) + 2KBr(s) + 2H2SO4(aq) → Br2(g) + 2H2SO4(aq) +
MnSO4(aq) + 2H2O(l)
b. Chlorine and Bromine Ion Identification by Precipitate
AgNO3(aq) + NaCl(aq) → AgCl(s) + NaNO3(aq)
HgNO3(aq) + NaCl(aq) → Hg2Cl2(s) + NaNO3(aq)
Pb(CH3COO)2(aq) + NaCl(aq) → PbCl2(s) + CH3COONa(aq)
AgNO3(aq) + KBr(aq) → AgBr(s) + NaNO3(aq)
HgNO3(aq) + KBr (aq) → HgBr(s) + KNO3(aq)
Pb(CH3COO)2(aq) + KBr (aq) → PbBr2(s) + CH3COOK(aq)
c. Chlorine Ion Identification (Bleaching Property)
Ca(ClO)2(s) + H2O(l) → Ca(OH)2(aq) + HOCl-(aq)
HOCl-(aq) + H+(aq) + Cl-(aq) → Cl2(g) + H2O(l)
d. Cl, Br, and I Compounds Identification
2NaCl(s) + H2SO4(aq) → 2HCl(aq) + Na2SO4(aq)
2KBr(s) + H2SO4(aq) → 2HBr(aq) + K2SO4(aq)
2KI(s) + H2SO4(aq) → 2HI(aq) + K2SO4(aq)
e. Halogen Gas Forming and Its Identification
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)
f. Iodine Solubility
I2(s) + H2O(l) → no reaction
I2(s) + HCl(aq) → 2HI(aq) + Cl2(g)
I2(s) + KI(aq) → KI3(aq)

4. Why Iodine did not solve in water but in KI ?

Answer :
Iodine has a very solubility in water because iodine is non polar. I2 is
polar because it contain two identical atoms and have equal
electronegativity. As a result, an I2 molecule cannot form strong
interactions with water molecules (no hydrogen bonds or permanent
dipole-dipole interactions). Whereas water molecules do form strong
interactions with each other. It’s therefore energetically disadvantageous
to have iodine molecules mixing with water molecules, since they will
get in the way of the water molecules forming maximum interactions
with each other. Hence, low solubility. In contrast, iodine is quite soluble
in non-polar solvents, like hydrocarbons, because their intermolecular
attractions are also weak, and they don’t suffer an energy disadvantage
by interacting with iodine molecules. This is a more detailed explanation
of the rule of thumb that “like dissolves like”: polar solutes dissolve in
polar solvents, and non-polar solutes dissolve in non-polar solvents.
The I2 molecules in iodine are not very soluble in water because they are
not alike. I2 is non-polar whereas H2O is polar. But KI solution contains
I- ions which combine with the I2 molecules to form I3- ions because
these are charged they dissolve in the water which is a polar solvent.
5. How’s the precipitate which form in second experiment ?
Answer :
AgNO3 + NaCl → NaNO3 + AgCl (white precipitate ++)
HgNO3 + NaCl → NaNO3 + HgCl (turbid)
Pb(CH3COO)2 + NaCl → 2 CH3COONa + PbCl2 (white precipitate +++)
 AgNO3 + KBr → KNO3 + AgBr (white precipitate +++)
HgNO3 + KBr → KNO3 + HgBr (turbid +)
Pb(CH3COO)2 + KBr → 2 CH3COOK + PbBr2 (white precipitate +++)
6. Why in 4th experiment the result are not HBr and HI ?
Answer :
HI and HBr can not produce using H2SO4. It because H2SO4 is strong
oxidation agent which will oxidize HBr into Br2 and HI into I2.
K. ATTACHMENT