Praktikum Anorganik Nitrogen Dan Ammonia

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I.

Title of Experiment : Nitrogen and Ammonia


II. Date of Experiment : Wednesday, 2nd of October at 09.30-12.00
III. Purposes of Experiment
1. To know the procedures of nitrogen and ammonia production in Lab
2. To know the properties of Nitrogen and its compound
3. To identify nitrogen gas, ammonium, and its compound
IV. Basic Theory
Nitrogen is colourless and odourless gas. The name is derived from the greek ‘nitron’
and ‘genes’ meaning nitre forming (Emsley, 2011). In laboratory, N2 gas could be
obtained by heating ammonia nitrous. N2 also could be produce by oxidizing
ammonia. Below are the reaction.
NH4Cl + NaNO2 → NaCl + NH4NO2 → N2 + H2O
4NH3 + 3Ca(OCl)2 → 2N2 + 3CaCl2 + 6H2O
8NH3 + 3Br2 → N2 + 6NH4Br
2NaN3 → 3N2 + 2Na (Lutfi, 2016)
A. Some Nitrogen Compound
1. Ammonia
Ammonia is produced thorugh Haber process that is dihydrogen and dinitrogen
are reacted at ~1000 atm pressure and temperature ~500oC using iron as
catalysator, based on reaction below.
N2 (g) + 3H2 (g) → 2NH3 (g)
Liquid ammonia is used in solvent either inorganic compound or organic
compound. Ammonia has been sel-ionization based on the equation reaction
below.
2NH3 (l) ⇌ NH4+ (l) + NH2− (l)
Ammonia is also prepared by following methods.
a. Ammonia gas is usually prepared in laboratory by gently heating
ammonium chloride (NH4Cl) and slaked lime [Ca(OH)2].
2NH4Cl + Ca(OH)2 → CaCl2 + 2 NH4OH
Ammonia gas is lighter than air, necessitating its collection by the
downward displacement of air. Because it highly soluble in water it cannot
be collected over it. Passing ammoniagas over quicklime (CaO) dries it.
Being a basic gas, ammonia cannot be dried passing it through
concentrated sulphuric acid or phosphorous pentoxide (P2O5), as it reacts

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with them to form ammonium sulphate or ammonium phosphate
respectively
2NH3 + H2SO4 → (NH4)2SO4
P2O5 + 4NH3 + 3H2O →2(NH4)4PO4 (Cotton & Wilkinson, 1930)
Ammonia gas may be identified by its odour (cautiously smell) the vapour
after removing the test tube, by the formataionof white fumes of
ammonium chloride when a glass rod moistened with concentrated
hydrochloric acidis held in the vapour, by its turning moistened red litmus
paper blue or turments paper brown, by its ability to turn filter paper
moistened with mercuru (I) nitrate solution black, and by filter paper
moistened with a solution of manganese (II) chloride and hydrogen
peroxide gives a brown colour (Shevla, 1979).
Ammonia reacts with both oxygen and water. Normal combustion in air
following reaction below.
4NH3 (g) + 3O2 (g) = 2N2 (g) + 6H2O (g)
However ammonia can be made to react with oxygen as shown in equataion
below, eventhough the process is thermodynamically much more favorable,
4NH3 + 5O2 = 4NO + 6H2O
By carrying out the reaction at 750 to 900 in the presence of platinum or
platinum-rhodium catalyst.
In aqueous solution ammonia is probably hydrated in a similar manner.
Although aqueous solution are commonly referral to as solutions of the weak
base NH4OH, called ammonia hydroxide. This is to be discourage, since there
is no evidence that undissosiated NH4OH exist and there is reason to believe
that if probably do not (Cotton & Wilkinson, 1930).
Ammonia is colourless pungent gas. The liquid has a large heat of evaporation
(1.37 kJ g-1 at the boiling point ) and is therefore fairly easily handled in
ordinary laboratory equipment. Liquid ammonia resembles water in physical
behaviour being highly associated beacuse of the polarity of the molecules and
strong hydrogen bonding (Cotton & Wilkinson, 1930).
Liquid ammonia has lower reactivity than H2O toward electropostive metals,
such metals reacting immediately with water evolve hydrogen. Liquid
ammonia, on other hand, dissolves many electropositive metals to give blue
solution containing metal ions solvated electrons.

2
Ammonium salts. There are many rather stable crystallinesalts of the
tetrahedral NH4+ ion; most of them are water soluble, like alkali metal salts.
Salts of strong acids are fully ionized, and the solutions are slightly acidic:
NH4Cl = NH4+ + Cl−
NH4+ + H2O = NH3 + H3O+ K25 = 5.5 x 10−10
Thus a 1 M solution will have a pH of ~4.7. The constant for the second
reaction is sometimes called the hydrolysis contant; howeverit may equally
well be considered to be the acidity constant of the cationic acid NH4+, and the
system regarded as an acid-base system.
2. Nitrates
All nitrates are soluble in water. Nitrates is couldn’t tasted, smelled, or seen in
water. there are several test to test nitrate. One of which is brown ring test. The
brown ring test is performed by adding iron (II) sulfate to the sample and then
a concentrated acid, typically slfuric acid. In acidic environment, the iron (II)
sulfate and the nitrates react with each othe to form an iron nitrate compound
that forms a brown ring. The reaction are
2NO− 2+ 3+ 2−
3 (aq) + 4H2SO4 (aq) + 6Fe (aq) → 6Fe (aq) + 2NO (g) + 2SO4 (aq) +

H2O (l)
Fe2+ (aq) + NO (g) → [Fe(NO)]2+ (aq)
3. Ammonium sulfide
Ammonia react with hydrogen sulfide to produce ammonium sulfide.
Ammonium sulfide is yellow-orange crystals. It is found as colorless to yellow
crystal below~18oC or as yellow orange crystals. It also has strong odor of
rotten gas ammonia.
Ammonia sulfide aquades solution is colourless to yellow liquid, with an odor
of rotten eggs. Materials in aqueous from the hydrosulfide which with acid
from H2S.
4. Oxides of Nitrogen
The known oxides of nitrogen are listed in Table 1. (Cotton & Wilkinson,
1930)
Formula Name Color Remarks
N2O Nitrous oxide Colourless Rather unreactive
NO Nitric oxide Colourless Moderately reactive
N2O3 Dinitrogen Dark Blue Extensively dissociated

3
trioxide as gas
NO2 Nitrogen dioxide Brown Rather reactive
Extensively dissociated
Dinitrogen
N2O4 Colourless to NO2 as gas and partly
tetroxide
as liquid
Dinitrogen Unstable as gas; ionic
N2O5 Colourless
pentoxide solid
Not well characterized
NO3; N2O6 - -
and quite unstable

V. Tools and Materials


A. Tools
1. Erlenmeyer flask 100 ml 1 pc
2. Distilled Flask 1 pc
3. Graduated Cylinder 100 ml 1 pc
4. Separated funnel 1 pc
5. Tripod 1 pc
6. Clamps and stative 1 pc
7. Bunsen burner 1 pc
8. Test tubes 7 pc
9. Pipettes 1 pc
10. Graduated cylinder 250 ml 1 pc
11. Box 1 pc
12. Stirer 1 pc
13. Balance 1 pc
14. Rubber cover 1 pc
15. Wood
B. Materials
1. NaNO2 crystal 7. Concentrated Ammonia
2. NH4Cl Crystal 8. H2S gas (from FeS and
3. Concentrated HCl HCl)
4. Ca(OH)2 9. Concentrated H2SO4
5. Amylum 10. H2SO4 1M; 0,1M
6. KI solution 11. FeSO4 solution
4
12. Concentrated HNO3 15. NH4OH 2M; 0,1M
13. HCl Solution 16. Sulphur
14. Phenolphtalein

VI. Lanes Work and Reaction


1. Producing nitrogen gas and identification with flame test

0,3 g NaNO2 + 10 ml 0,3 g NH4Cl + 10 ml


aquadest aquadest
- Entered into - Entered into
distilation flask separated funnel
- The tools is set as the
picture
- Heated
- Opened the separated-
funnel
- Collected the gas in the
upside down graduated
cylinder

Gas

- Tested the gas if the


graduated cylinder was
full of gas with flame
(burning wood)

The flame
distinguish

Rx : NaNO2(s) + H2O(l)  NaNO2(aq)


NH4Cl(s) + H2O(l)  NH4Cl(aq)
2NH4Cl(aq) + 2NaNO2(aq)  2N2(g) + 4H2O(l) + 2NaCl(aq)
2. Producing nitrogen gas and knowing its properties
0,25 g NaNO2

- Entered into test tube


- Added 2,5 ml aquades

Solution

- Divided into two part

5
Part A Part B

- Added some drops of - Diluted in 2 ml


H2SO4 aquadest
- Observed the fume - Added KI and
and the solution amylum
- Added diluted H2SO4
Colorless
- Observed the process
and slighlty
brown gas, Brown-purple color
also bubble and bubble
Rx : NaNO2(s) + H2O(l)  NaNO2(aq)
2NaNO2(aq) + H2SO4(aq)  Na2SO4(aq) + 2HNO2(aq)
4HNO2(aq)  2NO2(aq) + 2NO(g) + 2H2O(l)
2NO(g) + O2(g)  2NO2(g)
2NaNO2(aq) + 2H2SO4(aq) + 2KI(aq)  Na2SO4(aq) + K2SO4(aq)
+ NO(g) + I2(aq) + H2O(l)

(aq) + nI2 (aq) →

n (aq)

3. Reaction of Tengguli ring


1 ml HNO3

- Added H2SO4 concentrate 1 ml


- Colded
- Added FeSO4 0,2 M carefully through the wall of the tube
- Observed the process

6
Ring formation
Rx : 6FeSO4(aq) + 2HNO3(aq) + 3H2SO4(aq)  3Fe2(SO4)3(aq) + 2NO(s) +
4H2O(l)
HNO3(aq) + 2H2SO4(aq)  4NO(g) + H2O(l) + 2H2SO4(aq)
2NO3- + 4H2SO4(aq) + 6Fe2+(aq)  2NO(g) + 4SO42-(aq) + 4H2O(l)
Fe2+(aq) + NO(g)  [Fe(NO)]2+(aq)
4. Forming of ammonium precipitate

1 ml NH4OH 2M

- Flowed by H2S gas while 2 minutes


- Added 1 ml ammonium 0,1M
- Added sulfur
- Shaken
- Filtered

Residue Filter

- Observed the colour


- Added diluted HCl until
form precipitate

Turbid solution
Rx : FeS(s) + HCl(aq)  H2S(g) + FeCl3(aq)
NH4OH(aq) + H2S(g)  H2O(l) + (NH4)2S(aq)
(NH4)2S(aq) + S(s)  (NH4)2S2(s)
(NH4)2S2(aq) + HCl(aq)  NH4Cl(aq) + H2S(g) + S(s)
5. Ammonium gas production and identification with litmus paper

NH4Cl 4M

- Entered into test tube


- Added a bit of small spoon Ca(OH)2
- Heated carefully
- Tested by wet-litmus on the top of test tube
- Observed the change of litmus

Red litmus become blue

- Added HCl concentrate by spoon that has been dipped


- observed

White smoke

7
Rx : 2NH4Cl(aq) + Ca(OH)2(aq)  2NH3(g) + 2H2O(l) + CaCl2(s)
NH3(g) + H2O(aq)  NH4OH(aq)
NH4OH(aq) + HCl(aq)  NH4Cl(g) + H2O(l)
6. Ammonium gas production and identification the exist

5 ml NH4OH concentrate

- Entered into flask erlenmeyer 100 ml


- Heated carefully
- Collected the gas to the dry test tube which
has already closed by rubber cover

Gas
- Tested by two ways

- Dipped HCl - Phenolphtalein indicator


concentrate dropped into beaker
spoon glass which is contain
water and the gas
White
smoke Turbid solution

Rx : NH4OH(aq)  NH3(g) + H2O(l)


NH3(g) + HCl(l)  NH4Cl(g)
NH3(g) + H2O(l)  NH4OH(aq)
NH4OH(aq) + pp  pink solution

8
VII. Observation Result
No Lanes work Observation Result Hypotheses/ reaction Conclusion
1. − Prepared tools and materials Before  NaNO2(s) + H2O(l)  Based on the experiment,

− Entered 0,3 g NaNO2 with 10 ml  NaNO2 : white crystal NaNO2(aq) it can be conclude that N2
aquades into erlenmeyer flask  NH4Cl : white powder  NH4Cl(s) + H2O(l)  gas can be produced by
− Entered 0,3 g NH4Cl with 10 ml  Aquadest : colorless NH4Cl(aq) the reaction NaNO2 and
aquades into separated funnel liquid  2NH4Cl(aq) + 2NaNO2(aq)  NH4Cl proven by bubble
− Then the tools is set as the picture After 2N2(g) + 4H2O(l) + 2NaCl(aq) gas formed and the flame
− Heated  NaNO2 + aquadest : The flame distinguish this due to N2 distinguish
− Opened separated-funnel dissolve and colorless gas is inert gas
− Collected the gas in the upside solution
V theory = 44.828 L at STP
down graduated cylinder  NH4Cl + aquadest :
− Tested the gas if the graduated dissolve and colorless
cylinder was full of gas with flame solution
(burning wood)  NaNO2 + NH4Cl =
− Then the color change on flame formed bubble gas
2. − First, entered 0,25g NaNO2 into Before  NaNO2(s) + H2O(l)  Based on the experiment,
test tube  NaNO2 : white crystal NaNO2(aq) it can be concluded that
− Added 2,5 ml aquades  Aquadest : colorless  2NaNO2(aq) + H2SO4(aq)  NO and NO2 gas can be
− After that, divided the solution into liquid Na2SO4(aq) + 2HNO2(aq) produced by the reaction
two part  H2SO4 : colorless  4HNO2(aq)  2NO2(aq) + of NaNO2 and H2SO4
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No Lanes work Observation Result Hypotheses/ reaction Conclusion
− For part A, added some frops of solution 2NO(g) + 2H2O(l)
H2SO4  KI : colorless solution  2NO(g) + O2(g)  2NO2(g)
− Observed the fume and the solution  Amylum : turbid  2NaNO2(aq) + 2H2SO4(aq) +
− Result brown gas and bubble solution 2KI(aq)  Na2SO4(aq) +
− Whereas, for part B, diluted in 2 ml After K2SO4(aq) + NO(g) + I2(aq) +
aquades  NaNO2 + aquadest : H2O(l)
− Added KI and amylum dissolve and colorless
− Added diluted H2SO4 solution
− Observed the process  NaNO2 + aquadest +
− The solution become blue and H2SO4 : colorless,
bubbles formed bubble, brown
fumes (aq) + nI2 (aq) →
 NaNO2 + aquadest +
KI : colorless
+ amylum : turbid
solution
+ H2SO4 : blue-purple 
solution, formed n (aq)

bubbles
3. − 1 ml of HNO3 entered into H2SO4 Before  6FeSO4(aq) + 2HNO3(aq) + Based on the experiment,
10
No Lanes work Observation Result Hypotheses/ reaction Conclusion
concentrate 1 ml  HNO3 : colorless 3H2SO4(aq)  3Fe2(SO4)3(aq) + it can be concluded that
− Then, colded solution 2NO(s) + 4H2O(l) NO gas can be formed by
− Added FeSO4 0,2 M carefully through
 H2SO4 : colorless  HNO3(aq) + 2H2SO4(aq)  the reaction of HNO3 and
the wall of the tube
solution 4NO(g) + H2O(l) + 2H2SO4(aq) H2SO4.
− Observed the process
 FeSO4 : orange  2NO3- + 4H2SO4(aq) + 6Fe2+(aq)
− Ring formation
solution  2NO(g) + 4SO42-(aq) + 4H2O(l)
After  Fe2+(aq) + NO(g) 
 HNO3 + H2SO4 [Fe(NO)]2+(aq)
concentrate :
colorless solution,
the tube is warm
+ FeSO4 : formed
two layers
 HNO3 + H2SO4 +
FeSO4 : formed
brown ring in
between thosw two
layers
 Upper layer :
colorless

11
No Lanes work Observation Result Hypotheses/ reaction Conclusion
 Lower layer :
colorless
4. − 1 ml NH4OH 2M entered into test Before  FeS(s) + HCl(aq)  H2S(g) + Based on the experiment,

tube  NH4OH : colorless FeCl3(aq) it can be concluded that


− Flowed by H2S gas 2 minute solution  NH4OH(aq) + H2S(g)  H2O(l) H2S(g) can be formed by
− Added 1 ml ammonium 0,1M  FeS : black stone + (NH4)2S(aq) the reaction FeS and HCl
− Added sulfur  HCl : colorless  (NH4)2S(aq) + S(s) 
− Shaken solution (NH4)2S2(s)
− Then filtered  Sulphur : yellow  (NH4)2S2(aq) + HCl(aq) 
− Observed the colour of filtrate powder NH4Cl(aq) + H2S(g) + S(s)
− Added diluted HCl until form After
precipitate  FeS + HCl : black
− Turbid solution solution and white gas
formed
 NH4OH + H2S :
colorless and fumes
+ sulphur : doesn’t
dissolve, colorless
solution
 After filtered : yellow

12
No Lanes work Observation Result Hypotheses/ reaction Conclusion
solution, yellow
residue
 Filtrate + 2 ml HCl :
turbid solution
5. − NH4Cl 4M 2ml entered into test Before  2NH4Cl(aq) + Ca(OH)2(aq)  Based on the experiment,
tube  NH4Cl : colorless 2NH3(g) + 2H2O(l) + CaCl2(s) it can be concluded that
− Added a bit of small spoon liquid  NH3(g) + H2O(aq)  ammonia could be
Ca(OH)2  Ca(OH)2 : white NH4OH(aq) produced from reaction
− Heated carefully powder  NH4OH(aq) + HCl(aq)  between NH4Cl and

− Tested by wet litmus on the top of  HCl : colorless liquid NH4Cl(g) + H2O(l) Ca(OH)2 which is shown
test tube After Properties of NH4OH is alkaline by changing the colour of
− Observed the change of litmus  NH4Cl + Ca(OH)2 : compound wet red litmus paper
paper turbid solution, little become blue and white
− The color changeing from red into bit Ca(OH)2 smoke with concentrate
blue  Heated : formed HCl
− Added HCl concentrate by spoon bubble and turbid
that has been dipped solution
− Observed  Litmus + aquadest
− Gas formation and result white Red  red
smoke Blue  blue
13
No Lanes work Observation Result Hypotheses/ reaction Conclusion
 Gas formed + litmus :
Red  blue
Blue  blue
 Gas formed + HCl :
white smoke
6. − 5 ml of NH4OH concentrate Before  NH4OH(aq)  NH3(g) + H2O(l) Based on the experiment,
entered into erlenmeyer flask 100  NH4OH : colorless  NH3(g) + HCl(l)  NH4Cl(g) it can be concluded that
ml liquid  NH3(g) + H2O(l)  NH4OH(aq) ammonia gas can be
− heated carefully  HCl : colorless  NH4OH(aq) + Inpp  NH4In(aq) produced by the reaction
− collected the gas to the dry test tube solution + H2O(l) heated of NH4OH and
which has already closed by rubber  Pp : colorless solution HCl, and when tested
cover After with pp indicator yields
− gas resulted  Heated : colorless pink solution
− tested by two ways solution and formed

− first, dipped HCl concentrate spoon bubbles

− result white smoke  Dipped by HCl


− second, phenolphtalein indicator to concentrate spoon :
the beaker glass which is contain formed white smoke
water and the gas  Test with pp and
aquadest in the beaker
14
No Lanes work Observation Result Hypotheses/ reaction Conclusion
− the solution become pink solution glass : pink solution

15
VIII. Analysis and Explanation
The experiment that already started and done at Wednesday, October 2nd 2019
at 9.30 – 12.00 have a title “Nitrogen and Ammonia” and generally have some purpose
that are:
1. To know the procedures of nitrogen and ammonia production in Lab
2. To know the properties of Nitrogen and its compound
3. To identify nitrogen gas, ammonium, and its compound
A. First experiment (Preparation of N2 gas in laboratory scale)
The first experiment was to know the procedure how to make nitrogen gas.
Nitrogen gas (N2) could be produced from sodium nitrite through the procedure
will be explained. Sodium nitritewas white crystal was weighed as much as 0.3
gram. These sodium nitritewas dissolved in aquades 10 ml. The molarity of
sodium nitritewas 0,43 M. Sodium nitritewas colourless solution afterwards
sodium nitritesolution was placed into distilled flask. In other side, we prepare 0.3
g ammonium chloride (NH4Cl) dissolved in 10 ml aquades then it was entered into
separated funnel. Ammonium chloride was white crystal. When it was dissolved it
became colourless solution. The tools in this experiment was set look like picture
1. The separated funnel was closed before sodium nitritewas heated. After all the
tools were ready to be used, the sodium nitritewhich was in distilled flask was
heated by spirtus. After the solution is boiled, the ammonium chloride was entered
drop by drop by adjusting the faucet of the separated funnel. Ammonium chloride
wasn’t being mixtured directly with sodium nitritebecause ammonium chloride
was volatile. Because of its volatility, if ammonium chloride was entered directly it
would cause ammonium chloride would been reacted partly while the others will
evaporate. Whereas, if it was entered drop by drop, a few of ammonium chloride
will react with sodium nitrite perfectly.

16
The heating process was required for speeding up the rate reaction. The heating
process made the kinetic energy of the particle raises so the collision which was
occured would be more greater. The reaction between ammonium chloride
solution and sodium nitritewould yielded gas. The gas was collected in the
graduated cylinder which was placed upside down in the water. The distilled flask
was connected with these graduated cylinder through the pipe. The graduated
cylinder was full of water before the gas was obtained. The gas push the water and
fill the graduated cylinder. The gas which was produced was Nitrogen as the
reaction below.
NaNO2 (aq) + NH4Cl (aq) → NaCl (aq) + N2 (g) + 2 H2O (l)
After collecting the gas, it was tested by flame (burning wood). The burning wood
was entered into the graduated cylinder contain the gas results the flame is off.
Nitrogen gas was inert gas that’s why causing the flame off. The volume of the gas
theoretically is 9.32 ml at standar temperature and pressure (STP).
B. The second experiment (Preparation of NO gas and NO2 gas)
The second experiment was to know the procedure how to make nitrogen
monoxide and nitrogen dioxide gas. Those two gas could be produced from
sodium nitrite solution. As much as 0.25 grams was weighed and diluted by
aquades 2,5 ml. The molarity of sodium nitritewas 1.44 M. The sodium nitritewas
white crystal and its solution was colourless. The solution made was divided into
two parts equally.
1. The first part was added by a few drops of H2SO4 1M. The solution remain
colourless and there was bubbles. The bubble was brown. The bubble showed
that was being yielded nitrogen dioxide gas.
Sodium nitrite can also be used in the production of nitrous acid via sulfuric
acid. This reaction first yields nitrous acid and sodium sulfate:
2NaNO2 (aq) + H2SO4 (aq) → Na2SO4 + 2HNO2
The nitrous acid then, under normal conditions, decomposes:
2HNO2 → NO (g) + NO2 (aq) +H2O (l)
So the total reaction occurs were
2NaNO2 (aq) + H2SO4 (aq) → Na2SO4 (aq) + NO (g) + NO2 (aq) +H2O (l)
2. The second part was diluted by adding aquades 2 ml. The purpose of dilution
was to reduce the concentration of sodium nitrite solution. Next potassium
iodide (KI) solution was added into the solution also amylum solution.
Potassium iodide was colourless solution and was amylum too. The sodium
17
nitrite once added sodium iodide and amylum solution remain colourless. Yet,
the solution became purple solution and formed bubble. The bubble was
nitrogen monoxide gas as the reaction below.
2NaNO2 (aq) + 2KI(aq) + 2H2SO4 (aq) → Na2SO4 (aq) + K2SO4 (aq) + I2 (aq)
+ 2NO (g) +2H2O(l)
The principle of the reaction was redox reaction. The sulphuric acid was the
catalyst of the reaction. Sulphuric acid could lowering the activation energy of
the reaction by looking for the shorter way. The reductor in this reaction was
I − (iodide ion) in potassium iodide solution. Iodide ions was oxidized became
iodine (I2). The oxidation number of I (iod) changes from −1 became 0. Iodide
ions reduced nitrogen in sodium nitrite became nitrogen monoxide gas. The
oxidation number nitrogen changes from +3 became +2. Amylum solution
addition had function to indicate the presence of iodine which was formed. The
iodine which was formed from the redox reaction would react with amylum
and form complex (iod-amylum complex) which is purple.

n + nI2 →

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

H OH OH I n
I I (purple solution)
The sulphuric acid was added as the key of the reaction. Because of dilution of
sdium nitrite earlier, the reaction didn’t occur directly yet requiring sulphuric
acid as catalyst in order to ease the observation of gas formation. The reaction
are redox reaction. The reductor and the oxidator as each potential reduction.
The potential reduction of I2 is +0.53 as the reaction below
I2 (s) + 2e− → 2I − (aq) Eo = +0.53 V
While NO2 gas has the potential reduction +0.8 V
NO3- (aq) + 2H+ (aq) + e-→ NO2 (g) + H2O(l) Eo = +0.80 V
C. The third experiment (Tengguli rings reaction)
The third experiment was to identify thr presence of nitrate ions by ring brown
formation. As much as 1 ml of nitrate acid (HNO3) was entered into test tube.

18
Nitrate acid was colourless solution. Afterward, concentrated sulphuric acid
(H2SO4) was added into the test tube. The solution remain colourless and the test
tube became warm. It showed that the reaction was exothermic. Exothermic
reaction releases heat. Let the mixture until cold. Iron (II) sulphate (FeSO4) was
yellow solution. FeSO4 was dropped in a circle in test tube carefully. Wait till
brown ring was formed. Brown ring was located in the middle of the solution. The
solution was consisting of 2 phases which were Fe2SO4 and HNO3.
4HNO3 (aq) + H2SO4 (aq) → 4NO2 (g) + O2 (g) + 2H2SO4 (aq)
2NO− 2+ 3+ 2−
3 (aq) + 4H2SO4 (aq) + 6Fe (aq) → 6Fe (aq) + 2NO (g) + 2SO4 (aq) +

H2O (l)
Iron (II) ions forms complex with nitrogen monoxide, below are the reaction.
Fe2+ (aq) + NO (g) → [Fe(NO)]2+ (aq)
D. The fourth experiment (identifying the properties of nitrogen and its compound)
This experiment has purpose to recognize by identifying the properties of nitrogen
and the compound. First step was entering 1 ml ammonium hydroxide (NH4OH)
2M into test tube. Those compound was flowed by H2S gas. H2S gas was obtained
from reaction between FeS and concentrated HCl. FeS was black stone while HCl
was colourless solution. When FeS and HCl wes mixtured, the gas was formes and
yield bad odour.
FeS (s) + 2HCl (l) → H2S (g) + FeCl2 (aq)
H2S gas flowed thorugh the pipe for 2 minutes. When hydrogen sulfide (H2S) was
flowed into test tube, H2S would react with ammonium hydroxide in the test tube.
The main product which was produced was ammonium sulfide [(NH4)2S].
Ammonium sulfide solution was colourless solution.
2NH4OH (aq) + H2S (g) → (NH4)2S (aq) + 2H2O(l)
Then, the mixture was added 1 ml ammonium 0.1 M. Ammonium addition to
complete the reaction between ammonium hydrogen sulfide may there were
hydrogen sulfide left. Afterthat, sulfur was added into test tube. Sulfur was yellow
powder. Sulfure couldn’t be dissolve in the solution. Therefore, the mixture was
being shaken in order to homogen. Yet, the sulfur still couldn’t be dissolve in.
After shaking the solution, the solution was filtered. There is filtrate and residue.
The filtrate was yellow solution and the residue was yellow precipitate. The yellow
solution formed was ammonium disulfide [(NH4)2S2].
(NH4)2S (aq) + S(s) → (NH4)2S2 (s)

19
Finally, ammonium disulfide was added hydrochloric acid (HCl) till form the
precipitate. The reaction between ammonium disulfide and hydrochloric acid yield
the earlier product.
(NH4)2S2 (s) + 2 HCl (aq) → 2NH4Cl (aq) + H2S(g) + S(s)
E. The fifth experiment (producing and identifying ammonia)
The fifth experiment has purpose to prepare and identifying ammonia. As much as
2 ml of ammonium chloride (NH4Cl) 4M was entered into test tube. Afterthat, a
few spoon of calsium hydroxide was added. Ammonium chloride was colourless
solution and calsium hydroxide was white powder. Ammonium chloride when it
was addes by calsium hydroxide, became white solution and didn’t all calsium
hydroxide dissolved. Then, the mixture was heated. When the mixture was heated,
the solution formed bubbles. To determine the properties of the gas, we use two
ways to recognize it.
1. Using red litmus paper.
The reaction which was occured was
NH4Cl (aq) + Ca(OH)2 (s) → CaCl2 (aq) + 2NH3 (g) + 2H2O(l)
Ammonia which was formed was gas. To identify it, we used red litmus paper.
Red litmus paper was given aquades then it was put on the top of test tube.
Aquades (H2O) in litmus paper will bind the ammonia which was produced in
the reaction. Ammonia when react with aquades became ammonium (NH4OH).
NH3 (g) + H2O (aq) → NH4OH (aq)
Ammonium solution was base which turnes red litmus paper to be blue.
2. Reaction with hydrochloric acid (HCl)
Glass spatula was dipped in concentrated hydrochloric acid. Then, thus
moistened spatula was placed in the top of the tes tube. Directly white smoke
was formed. White smoke formed was NH4Cl. The reaction below.
NH3 (g) + HCl (aq) → NH4Cl (g)
F. Sixth Experiment (producing and identifying ammonia)
The sixth experiment also has purpose to prepare and identifying ammonia. As
much as 5 ml of ammonium chloride (NH4Cl) was entered into test tube.
Ammonium chloride was colourless. Then, it was heated and formed bubbles. To
determine the properties of the gas, we use two ways to recognize it.
1. Using phenoplhtalein indicator
The reaction which was occured was
NH4Cl (aq) + Ca(OH)2 (s) → CaCl2 (aq) + 2NH3 (g) + 2H2O(l)
20
Ammonia which was formed was gas. The gas was flowed to the the
aquades in beaker glass through the pipe. Ammonia when react with aquades
became ammonium (NH4OH).
NH3 (g) + H2O (aq) → NH4OH (aq)
Ammonium solution was base which the solution turns to be pink after
phenolphtalein addition in few drops. Phenolphtalein has pH range about 8.3 –
10.0 from colourless until pink. It means when the soultion becomes pink that
the pH of the solution is as same as 10.0 or bigger or we could indetify as bas
solution.
2. Reaction with hydrochloric acid (HCl)
Glass spatula was dipped in concentrated hydrochloric acid. Then, thus
moistened spatula was placed in the top of the tes tube. Directly white smoke
was formed. White smoke formed was NH4Cl. The reaction below.
NH3 (g) + HCl (aq) → NH4Cl (g)

IX. Conclusion
Based on the experiment we have conudcuted and the explanation above, we could
conclude that:
1. Nitrogen gas can be made in a laboratory by reacting the NaNO2 solution with
NH4Cl by heating. Nitrogen gas is very unreactive if it reacts with other elements
or compounds. And if tested with a flame, the flame will die which proves the
inactivity of nitrogen gas.
2. NO gas that reacts with air (O2) will form a yellow NO2 gas compound and NO
that reacts with halogen (I2) will form concentrated purple nitrosil iodide.
3. Nitrogen can form complex compounds with Fe, namely [Fe(NO)2] 2+, which is
proven by the formation of brown moth rings.
4. NH4OH If it is drained with H2S gas and reacted with sulfur flowers (S) a yellow
precipitate is formed (NH4)2S
5. NH4Cl if witnessed with calcium hydroxide (C (OH)2) NH3 gas will be formed
which is alkaline because it changes red litmus to blue, and litmus
X. References
Cotton, F. A., & Wilkinson, G. (1930). Advanced Inorganic Chemistry. New York:
John Wiley & Sons Inc.

Emsley, J. (2011). Nature's Building Blocks : An A-Z Guide to The Elements. New
York: Oxford University Press.
21
Lutfi. (2016). Kimia Anorganik : Unsur-Unsur Golongan Utama . Yogyakarta:
Absolute Media.

Shevla. (1979). Vogel's Textboo of Macro and Semimicro Qualitative Inorganic


Analysis. United States of America: Longman, Inc.

XI. Answering Question


1. Explain the laboratory preparation of nitrogen gas and ammonia!
Answer :
Laboratory preparation of nitrogen gas
a. By heating NH4NO2
NH4NO2 → N2 + 2H2O
b. By oxidation of NH3
2NH3 + 3CuO → N2 + 3Cu + 3H2O
c. By thermal decomposition through heating ammonium compound CNH4NO2
CNH4 NO2(s ) → N2 + 2H2 O
d. Gradual distillation of liquid air
Air that contains nitrogen undergo the process of liquefaction of air, so the air
liquid only contains argon, nitrogen, and oxygen. The gases are separated by
gradual distillation and obtained in the form of gas most on the distillation.
In industry, the way of gradual distillation and thawing (distillation of air
liquid) for N2 has a point of boiling lower than O2 then it is first evaporated as
a fraction of the first. In spectroscope N2 pure in created by the decomposition
of thermal Sodium Barium azide, the undergo reaction as follows:
2NaN3 → 2Na + 3N2
Laboratory preparation of ammonia gas
a. Reaction of nitride and water
Mg3N2 (s) + 6 H2O (l) → 3 Mg(OH)2 (aq) + 2 NH3 (g)
b. Reaction of ammonium chloride and strong base
NH4Cl (aq) + NaOH(aq) → NaCl (aq) + H2O (l) + NH3 (g)
2. Explain the chemical properties of nitrogen!
Answer :
a. N2 molecule binds covalently double-three, having relatively large bind energy,
946 kJ/mol so very unstable or difficult to react at a high temperature
(endothermic reaction) with the help of a catalyst .

22
b. At the room temperature N2 reacts very slowly with a Li metal produce Li3N.
While the with other metals, can be done by way of doing the fire of electricity
through gas pressure low of nitrogen, the process is catalysed by the presence
of oxygen homo formed nitrogen active (N2 to 2N) which can form nitride
compounds with certain metals.
c. Nitrogen reacts with hydrogen or oxygen at a high temperature such as in fire
electricity, forming gas NH3 and NO3
3. Write the reaction equations of all the experiments above!
Answer :
a. Preparation and identification of N2 gas
NaNO2 (aq) + NH4Cl (aq) → NaCl (aq) + NH4NO2 (aq)
NH4NO2 (aq) → N2 (g) + 2H2O (l)
b. Preparation of NO and NO2 gas
NaNO2 (aq) + H2SO4 (aq) → Na2SO4 (aq) + 2HNO2 (aq)
2HNO2 (aq) → H2 (g) + 2NO2 (g)
NaNO2 (aq) + H2SO4 (aq) + 2KI (aq) → Na2SO4 (aq) + I2 (aq) + NO (g)
c. Brown ring formation
2NO33- (aq) + 4 H2SO4 (aq) + 6 Fe2+ → 6 Fe3+ + 2 NO (g)
4 Fe2+ + NO (s) → [Fe(NO)]2+
d. Formation of H2S gas
NH4OH (aq) + H2S (g) → NH4HS (aq) + H2O (l)
e. Preparation and identification of ammonia
NH4Cl (aq) + Ca(OH)2 (s) → CaCl2 (aq) + NH3 (g) + H2O (l)
NH3 (g) + HCl (aq) → NH4Cl (g)
f. Preparation and identification of ammonia
NH4OH (aq) → NH3 (g) + H2O (l)
NH3 (g) + HCl (aq) → NH4Cl (g)

4. Mention the uses ammonium!


Answer :
The function of ammonium in this experiment is as forming alkaline ambience so
the reaction can undergo

23
XII. Attachment
XIII. DOCUMENTATION

Apparatus and Materials

The apparatus that used for Nitrogen and The materials that used for Nitrogen and
Ammonia Experiment Ammonia Experiment

1. Preparation and Identification of Nitrogen gas

Weighed 0.3 g of NaNO2 using analytical Taken 10 ml distilled water using graduated
balance cylinder

Diluted crystal NaNO2 with 10 ml distlled


water
Entered NaNO2 solution into pipe-sided
erlenmeyer flask

24
Weighed 0.3 g white crystal NH4Cl using Diluted NH4Cl with 10 ml distilled water
analytical balance

Entered diluted NH4Cl into separatory funnel Set the apparatus and materials as shown the
figure above

2. Preparation of NO and NO2 gas

Entered 0.25 g NaNO2 into test tube

Added 2.5 ml distilled water into test tube

25
Divided the solution into tow different test For tube A added some drops of H2SO4
tubes with the same amount, labelled with solution
tube A and tube B

In the tube A formed bubbles and brown For tube B added 3-5 drops of KI and amylum
fumes solution then bubbles formed in the colorless
solution

In tube B added diluted H2SO4 solution and


the color changed purple-blue also formed
bubbles

3. Brown Ring Formation

26
Measured 1 ml diluted HNO3 with graduated Added 1 ml concentrated H2SO4
cylinder, then entered into test tube

After cooled it down, prepared FeSO4 0.2 M Added 1ml FeSO4 0.2 M carefully through the
solution in the fume hood wall of the tube

Wait a minute, then the brown ring formed

4. Formation of H2S gas

27
Prepared 1 ml NH4OH 2 M in the fume hood Flowed by H2S gas for 2 minutes

Added colorless 1 ml NH4OH 0.1 M solution Added yellow powdered sulfur into test tube,
shaken the test tube then filtered it. Added
diluted HCl solution until it formed
precipitate
XIV.

5. Preparation and Identification of Ammonia

Prepared colorless 2 ml NH4Cl 4 M in the Added a bit of small spoon white powdered
fume hood, then transferred it into test tube Ca(OH)2, the solution appearance became
turbid

Heated carefully Tested by litmus that already moistened with


distilled water

28
The litmus paper changed color from red to Tested the gas with the spoon that already
blue, while blue still blue dipped in concentrated HCl solution, then the
white fumes formed
XV.

6. Preparation and Identification of Ammonia

Prepared 5 ml colorless concentrated NH4OH Transferred it into pipe-sided Erlenmeyer


in the fume hood flask 100 ml

Connected the pipe using plastic hose then Tested the gas with the spoon that already
Closed the Erlenmeyer using rubber cover and dipped in concentrated HCl solution, then the
heated carefully white fumes formed

29
Flowed the gas into beaker glass filled with The final look of test tube still formed white
distilled water and phenolphthalein indicator, fumes
then the solution changed into pink solution

30

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