Laboratory Report CHM 153 (Inorganic Chemistry)

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LABORATORY REPORT

CHM 153
(INORGANIC CHEMISTRY)
1. MUHAMMAD MIRZA HIZAMI BIN RAJIEI 2019289394
2. LUQMAN AL HAKIM BIN EMLIR 2019211818
3. NIGHTANGEL JANA ANAK FRANKIE 2019272822

PROGRAMME : AS115 2A
NO. AND TITLE OF EXPERIMENT : Elements Of The First Transition Series

DATE OF EXPERIMENT : 09 / 4 / 2020


DATE OF REPORT SUBMISSION : 30 / 4 / 2020
NAME OF LECTURER : Rabuyah Binti Ni

Laboratory Report Marking Scheme:


Criteria Full Marks (to be filled by
Mark(s) lecturer)
Objective of the Experiment
Introduction
Experimental Procedure
Results and Observations
Calculations
Discussion
Conclusion
Answers to Questions
References
Format
Total Marks
Objective:
To gain familiarity with some of the acid-base, oxidation-reduction and complexation
reactions of the elements of the first transition series

Introduction:
Transition metal is an element whose atom has a partially filledd sub-shell, or which can give
rise to cations with an incompleted sub-shell. This metal can be found in nature such as rocks
and minerals. The colour of many gemstones is due to the presence if transition metal ions.
As example, rubies are red due to the Cr and sapphires are blue due to presence of Fe and
Ti.Transition metals and their compounds have many useful applications such as Fe is used to
make steel and stainless steel, Ti is used to lightweight alloys and so on.To understand the
uses and applications of transition metals and their compounds, we need to understand their
chemistry.For this experiment, we will focusing on three elements of transition metal in the
first series.The elements is chromium, cobalt and nickel.

Procedure
:a) Reaction of Chromium :
1) An excess of 2 M NaOH was slowly added, to 2 ml of chrome alum solution. Then,2 ml of
6% hydrogen peroxide was added and warm it. The any colour changes or evolution of gases
was took careful note.
2) 2 M aqueous ammonia was slowly added to 2 ml of chrome alum solution. Any colour
changes was noted.
3) Excess 1 M sodium carbonate solution was added to 2 ml of chrome solution .The results
of this experiment was compared with those of experiment 1 and 2.
4) 2 ml of 6M HCl and granular zinc was added to 2 ml of the chromium (III) chloride
solution. The solution was warm until it was effervescing vigorously. Any change colour was
noted.The liquid was quickly decanted into 4 ml of a saturated solution of sodium
acetate.Any colour changed was noted carefully.
5) 2 ml of 6 M HCl (concentrated) and a granular of zinc was added to 2 ml of
the chromium(III) chloride solution and was warm until the solution effervesce
vigorously. The solution was cooled and the test tube was rotate while the
solution spreads in a thin layer over the wall.Thecolour changes occur was
noted.
6) 2 M sulphuric acid drop was added wisely to 2 ml of potassium dichromate
solution until ph was about 4 (test with pH paper). Then 2 M NaOH was
dropped wisely about ph was about 9. Then 2 M sulphuric acid was added to
bring the ph back to about 4. The colour changes was noted.
7) A few drops of 0.1 M BaCl2solution was added to 2 ml of potassium
dichromate solution and the observation was recorded.

b) Reaction of Cobalt:
1) 4 ml of water was added and 4 ml of 2 M NaOH solution was added slowly to
2 ml of the cobalt (II) solution.
2) 4 ml of 2 M NaOH was added slowly to 2 ml of the cobalt (II) solution. The
result was compared with the result from steps 1.
3) 4 ml of 1 M sodium carbonate solution was added to 2 ml of the cobalt (II)
solution. The result was compared with those in step 1 and 2.
4) 4 ml of 4 M aqueous ammonia was added slowly to 2 ml of the cobalt (II)
solution. The result was compared with the result of steps 1 to 3. Then, about 4
drops of 6% hydrogen peroxide and 2 ml of 2 M NaOH was added and was
boiled gently.
5) a) 1 ml of 2 M potassium thiocyanate solution and 1 ml of pyridine was
added to 1 ml of the cobalt (II) solution.
b) 1 ml of 2 M potassium thiocyanate and 1 ml of pyridine was added to 1 ml of
saturated zinc sulfate solution
c) 1 ml of 2 M potassium thiocyanate and 1 ml of pyridine was added to a
mixture of 1 ml of the cobalt (II) solution and 1 ml of saturated zinc sulfate
solution.
6) 1 ml of the cobalt (II) solution was acidify with acetic acid and a ¼ spatula of
solid potassium nitrite.Any changes was noted.
c) Reactions of Nickel:
1) 4 ml of 2 M NaOH was added to 2 ml of the nickel (II) solution and the
solution was boiled.
2) 4 ml of 4 M aqueous ammonia was slowly added to 2 ml of the nickel (II)
solution.The result was compared with the first part of experiment 1.About 4
drops of 6% hydrogen peroxide was added.Then,4 ml of 2 M NaOH was added
and boiled gently.The corresponding reaction of cobalt(II) was compared.
3) 4 ml of 1 M sodium carbonate solution was added to 2 ml of the nickel (II)
solution.The result was compared with those of the first parts of experiments 1
and 2.
4) 2 ml of 2 M potassium thiocyanate solution was added to 2 ml of the nickel(II)
solution.A few drops of pyridine was added.

Data and Result:


EXPERIMENT CHROMIUM COBALT NICKEL
1 -dark purple - 3layer -pink solutions -white precipitate
of colours formed 2 layers
-light green
-layer 1: clear brown -layer 1: dark blue
-layer 2: yellowish -layer 2: pale pink
green -after a few
minutes,solution
-layer 3: green-grey become clear and a
precipitate pale red precipitate
is formed
2 -colour changes to -becomes a pale pink -green precipitate
dusty green and solution
-colour changes
form green
-after a few from blue-green
precipitation
minutes,solution
-green precipitate become clear and a
turns into 3 layer of pink precipitate is
colours formed
-layer 1: clear purple
-layer 2: dusty grey
-layer 3: grey
precipitate
3 -colour changes to -pink to purple -no colour changes
cloudy blue-
-after a few -green precipitate
grey,formed 2 layer
minutes,pinkish
of colour
solution and a purple
-layer 1: dusty blue- precipitate are
grey formed
-layer 2: blue-grey
precipitate
4 -colour remains the -pink to dark maroon -colour changes
same after adding 4M of from green-light
aqueous ammonia blue
-granular of zinc
solution
completely dissolved -blue precipitate
-silver mirror
effect,clear
solution(slightly
brownish) and black
precipitate formed
after being boiled
5 -colour changes to a. cloudy pale pink
algae green
-after a few
-granular of zinc is minutes,clear
not completely solution and purple
dissolved precipitate formed
b. changes occur
after adding pyridine
and blue precipitate
formed
c. 2layer
-layer 1: cloudy pale
pink with a little
blue
-layer 2: red wine
solution
6 -after 10 drops of -before being
H2SO4, the pH of shaken, the solution
solution turns to 4 colour is orange and
and after 30 drops of dark green
NaOH the pH
-turns yellowish
becomes 9
brown after being
shaken, brown
-10 drops of H2SO4 precipitate formed
is needed to turn the with a strong scent
pH back to 4
-colour remain
unchanged
7 -colour changes to
neon orange after 5
drops of BaCl2
-yellow precipitate is
formed

Discussion:
a) Reaction of Chromium:
An excess of sodium hydroxide added to chrome alum solution to produce a
green hexahydroxocromate (III) ions.

[Cr(H2O)6]3+ → [Cr(H2O)3(OH)3] → [Cr(OH)6]3-

This is then being oxidized with hydrogen peroxide solution and turn into bright
yellow solution containing chromate (VI) ions.The ammonia acts as both a base and a ligand.
With a small amount ofammonia, hydrogen ions are pulled off the hexaaqua ion exactly as in
thehydroxide ion case to give the same neutral complex.

[Cr(H2O)6]3+ → 3NH3 → [Cr(H2O)3(OH)3] + 3NH3+

If you add sodium carbonate solution to hexaaquachromium (III) ions, you get
exactly the same precipitate as if you added sodium hydroxide solution or
ammonia solution. This time, it is the carbonate ions which which remove
hydrogen ions from the hexaaqua ion and produce the neutral complex.

2[Cr(H2O)6]3+ + 3CO32- → 2[Cr(H2O)3(OH)3] + 3CO2 + 3H2O

Dichromate ions can be reduced to chromium (III) ions and then to chromium
(II) ions using zinc and hydrochloric acid. Hydrogen is produced from a side
reaction between the zinc and acid. This must be allowed to escape, but need to
air out of the reaction. Oxygen in the air rapidly re-oxidises chromium (II) to
chromium (III).

b) Reaction of Cobalt:
We used 0.5 M cobalt (II) chloride as the solution. This solution gives pink
colour. The first reaction are with water and NaOH that form dark blue and pale pink
precipitate. When excess 4 M NaOH was added to the light pink cobalt solution,
a bright blue precipitate was formed, like in part 1. As the NaOH shifted
towards being in excess, the mixture became pink/grey cloudy mixture; less
dark than part 1.

2NaOH + CoCl2 2NaCl + Co(OH)2

When excess NaCO3 is added to the pink cobalt solution, a purple precipitate
was formed. Compared to reaction number one, the reaction of the cobalt did
not proceed as far due to the carbonate being a weaker base.

Na2CO3 + CoCl2 CoCO3 + 2NaCl

When excess aqueous NH3 was added to the pink cobalt solution, the color
change only formed a bright royal blue solution. Adding 4 drops of H2O2 (6%),
a green solution was obtained. Adding excess 4 M NaOH, a dark black/green
solution was obtained. The mixture was placed on the heat which yielded a
black precipitate formation.

CoCl2 +6NH3 [Co(NH3)6]Cl2


[Co(NH3)6]Cl2 + H2O2 [Co(NH3)6]Cl3 + 2OH-(aq)

When 1 mL of 2 M ammonium thiocyanate was added to 1 mL of cobalt


solution, the solution changed color to a purple/red grape juice color. Upon
addition of 1 mL of pyridine, a milky, pink solution was formed, with a white
precipitate.

Adding 1mL of 2 M ammonium thiocyanate (clear, colorless) to 1 mL of


saturated zinc sulfate (clear, colorless), then adding 1 mL of pyridine, a milky
solution with a white precipitate was obtained.

To a light pink mixture of 1 mL of cobalt(II) solution and 1 mL of saturated zinc


sulfate solution, 1 mL of 2 M ammonium thiocyanate solution was added, forming a darker
pink mixture, then 1 mL of pyridine was added, forming a pink/blue precipitate.

Acidifying 1 mL of the cobalt (II) solution with clear, colorless acetic acid, no
change was observed. Adding a little solid potassium nitrate resulted in a
yellow precipitate being formed.

c) Reaction of Nickel:
Nickel that used in this experiment is 0.5 M nickel (II) chloride solution that
gives green colour. When nickel (II) chloride solution (NiCl2) react with
sodium hydroxide (NaOH), a light green precipitate was formed. No particular
change of the solution when heated. The equation of reaction as shown below:

NiCl2(aq) + 2NaOH(aq) --> Ni(OH)2(s) + 2NaCl(aq)

That goes the same with the reaction of nickel(II) solution and aqueous
ammonia. The green precipitate was formed. With alkaline aqueous sodium
carbonate solutions, nickel(II) ions produces a precipitate of green precipitate of
nickel(II) carbonate.

Ni2+(aq) + CO32–(aq) ==> NiCO3(s)


The reaction of nickel (II) solution with potassium thiocyanate formed
white precipitate in the solution. Nickel is a transitional metal, but
which unlike most metals of this family, it does not form many coloured
precipitate or complex solutions.

Question :

1. The common oxidation states and electron configuration of chromium, cobalt and nickel:

a) Chromium:
[Ar]3d84s2
+6 = [Ar]3d4
+3 = [Ar]3d7
+2 = [Ar] 3d8

b) Cobalt :
[Ar]3d74s2
+3 = [Ar]3d6
+2 = [Ar]3d7

c) Nickel:
[Ar]3d54s1
+2 = [Ar]3d4

2. Interpret the result of the reactions carried out, write balance equations whenever possible.

[Cr(H2O)6]3+ → [Cr(H2O)3(OH)3] → [Cr(OH)6]3-

[Cr(H2O)6]3+ → 3NH3 → [Cr(H2O)3(OH)3] + 3NH3+

2[Cr(H2O)6]3+ + 3CO32- → 2[Cr(H2O)3(OH)3] + 3CO2 + 3H2O

2NaOH + CoCl2 2NaCl + Co(OH)2

Na2CO3 + CoCl2 CoCO3 + 2NaCl

CoCl2 +6NH3 [Co(NH3)6]Cl2

[Co(NH3)6]Cl2 + H2O2 [Co(NH3)6]Cl3 + 2OH-(aq)

NiCl2(aq) + 2NaOH(aq) --> Ni(OH)2(s) + 2NaCl(aq)

Ni2+(aq) + CO32–(aq) ==> NiCO3(s)


Conclusion:
As a conclusion, transition series is full of elements with colour. It has many
uses in our life. That’s why we need to know this series well to produce many
benefits in our life.

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