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VIETNAM NATIONAL UNIVERSITY HO CHI MINH CITY

UNIVERSITY OF TECHNOLOGY
FACULTY OF CHEMICAL ENGINEERING



INORGANIC CHEMISTRY
LABORATORY REPORT

INSTRUCTOR: DR. LE MINH VIEN

GROUP 2 – HC14KSTN

LE PHUONG DUNG 1410535

LY ANH DUY 1410570

Ho Chi Minh City, 20th October, 2015

Page | 1
Unit 2: THE ALKALINE-EARTH METALS

Explanation – Equation - Calculation -


Experiment Process and Phenomena
Conclusion
Observing the color of the
alkaline-earth metals as fire:

 Dipping a part of filter-paper in  This phenomenon is explained that metal


saturated CaCl2 solution, then ion of salts absorb energy from flame, the
dry it over an alcohol lamp and outermost layer electrons are excited to
observe. The color is orange- higher energy levels. When the electrons
red. fall back to lower energy levels, they emit
light of various specific wavelengths in
 Do the same way with the the visible spectra.
saturated solutions of SrCl2 and
BaCl2.The color of SrCl2

1
solution is red and BaCl2
solution is yellow-green. Conclusion:
 Heating alkaline-earth metal cation (with
appropriate anion in compounds) will give
specific flame color. In the group IIA,
going from top to bottom, the
characteristic flame color will change
from red to yellow, increasing energy
because of increasing atomic radius,
electrons easily move to higher energy
levels. Certain bright lines in these spectra
cause the characteristic flame color, which
can be used to identify the metal or its
compounds.

Reaction between alkaline-earth

2 metals and water:

Drop 1-2 drops of water into 2  The reaction occurs very slowly because
tubes, then add a little amount of Mg(OH)2 covering the surface of Mg:
Mg powder and 1 drop of
phenolphthalein. Mg + H2O  Mg(OH)2↓ + H2↑ (1)

Page | 2
 Test-tube 1:  Since TMg(OH)2 = 10-9.22, Mg(OH)2 can
 At room temperature, reaction partly dissolve in water, producing OH- and
occurs very slowly. A part of turning phenolphthalein into pink at the
solution changes to pink and interface between Mg and water.
appearing air-bubble
(hydrogen). Mg(OH)2  Mg2+ + 2OH- (2)

 At high temperature: the  At high temperature, Mg(OH)2 dissolves


reaction occurs more strongly. more in water and creating more OH- so
The bubbles appear more that the pink gets darker. The cover of
obviously, the pink is darker Mg(OH)2 reduces at the same time and
and spread over the solution. reaction (1) occurs faster => the bubbles
escape more.

 Test-tube 2: add 5-6 drops of


NH4Cl solution. The Reaction  NH4Cl reacts with Mg(OH)2 to create
occurred vigorously. The color dissolved salt MgCl2. As a result, Mg is
becomes lighter and disappears free to react with water and release more
while more bubbles are gas.
produced. Finally, the pink re-
appeared. Mg(OH)2 + NH4Cl  MgCl2 + NH3↑ + H2O

 Because Mg(OH)2 is dissolved, the


balance (2) is gets into the direction of
reducing OH- so phenolphthalein is
colorless.
 The pink re-appears because of 2 reasons:
NH3 produces from the above reaction and
OH-produces from the reaction (2).

Conclusion:
The alkaline-earth metals react vigorously
with water when heating or having suitable
catalysts.

Prepare and properties of

3 Mg(OH)2
Prepare 3 test-tube: each one
contains Mg(OH)2 which formed MgCl2 + 2NaOH → Mg(OH)2↓ + 2NaCl
from the reaction between NaOH
and MgCl2. The resultant mixture
was centrifuged to remove the
liquid.

Page | 3
 Test-tube 1: Add HCl, the
precipitation dissolves and Mg(OH)2 + 2HCl → MgCl2 + 2H2O
solution is colorless.
 Test-tube 2: Add NH4Cl. The
precipitation dissolves, solution Mg(OH)2 + 2NH4Cl  MgCl2+ 2NH3↑ + 2H2O
is colorless,and have smell of
urine.
 Test-tube 3: Add NaOH. No NaOH and Mg(OH)2 are bases => no
phenomenon. reaction

Preparation and properties of the


alkaline-earth metals hydroxide:

 Add 1ml 0.5M salt solutions of Ca2+ + 2OH-  Ca(OH)2↓


Mg2+, Ca2+, Ba2+and
2+
Sr separately into 4 test-tubes; Ba2+ + 2OH-  Ba(OH)2
then add 0.5 mL of 1M NaOH Mg2+ + 2OH-  Mg(OH)2↓
solution. Centrifuge the Sr2+ + 2OH-  Sr(OH)2↓
produced precipitate.
 The amount of precipitate is in From Mg to Ba, the atomic radius increases,
the order of Ba2+<Sr2+<Ca2+< leading to the decrease in the electrical
Mg2+. Therefore, the solubility attraction between the nucleus and the
of their hydroxide is in the electron in the outermost layer. Since
reversed order. oxygen is highly negative, it strongly
attracted electrons which increases the
polarity of hydroxides. As a result, these
hydroxides can dissolve in water, a polar
solvent.
Conclusion:
The hydroxide of alkaline-earth metals can
be produced from the reaction between their
soluble salts and alkaline solutions. These
hydroxide are base.
Survey solubility of the alkaline-

4 earth metals sulfate salts:


 Add 1ml solutions of MgCl2,
CaCl2, BaCl2 and SrCl2
separately into 4 tubes, then
slowly add 2N H2SO4 solution.

Page | 4
 Test-tube 1: no phenomenon.
 Test-tube 2 is floral-white
because of creating less soluble Ca2++ SO4 2-  CaSO4↓ TCaSO4 = 10-5.04
compound.
+ Test-tube 3 is opalescent Sr2+ + SO4 2-  SrSO4↓ TSrSO4 = 10-6.49
solution.
+ Test-tube 4 is more opalescent. Ba2+ + SO4 2-  BaSO4↓ TBaSO4 = 10-9.97

 Add H2SO4 until excess [SO42-] increases, so the balance gets into the
direction which increasing precipitate.

Conclusion:
From Mg to Ba, the solubility of their
hydroxides and sulfate salts is opposite
because in sulfate salts the activation energy
of cations is higher than their lattice energy.
In addition, from Mg to Ba, the ionic radius
increases that leads to the decrease in their
polarity in water and hydration energy so
that the solubility is decreasing.
Determine hardness of water:
 Add 10 ml of hard water in V1 = 16.9 ml
erlen, add distilled water until V2 = 16.7 ml
the volume is 100ml. Then add VETDA = 16.8 ml

5 5 mL buffer solution at pH 10
and 5 drops of the indicator
Eriochrome Black T. Shake and
Vsample = 10 ml
CN ETDA = 0.02 N
Total content Mg2+ and Ca2+:
titrate it by ETDA 0.02N until X = V ETDA x CN ETDA x 1000/ Vsample
the color of solution turns from = 16.8 x 0.02 x 1000/ 10 = 33.6 (mN)
red to blue. Repeat this process.
V1 = 10.5ml, V2 = 10.3ml  VETDA = 10.4ml

6 Soften water:

 Add 50 mL hard water into a


Vsample = 10 ml
Total content Mg2+ and Ca2+ rest:
X = VETDA x CN ETDA x 1000/ Vsample
250 mL becher, add Na2CO3 = 10.4 x 0.02 x 1000/ 10 = 20.8 (mN)
solution 0.1M and 2ml slaked Reviews:
lime. Boil mixture in 3 minutes  X’ < X demonstrates that the amount of
and filter to remove the Mg2+ and Ca2+ in sample decreases =>
precipitate. Titrate the water water is softened because of the reaction
with the similar procedure as 5 between Na2CO3 and Ca(OH)2
experiment. Mg2+ + 2OH-  Mg(OH)2↓
Ca2+ + CO32-  CaCO3↓

Page | 5
 This reaction decreases the amount of
Mg2+ and Ca2+in the water after filtration.
Unit 6: Hydrogen – Oxygen – Sulphur
(Group VI-A)
Experiment Process and Phenomenon Explanation – Equation - Calculation
Number
- Conclusion

 Prepare H2
Fitting the air receiver as the
picture Zn + 2HCl  ZnCl2 + H2 ↑

 There are small explosions because


hydrogen reacts with oxygen mixed in the
test-tube. Initial oxygen is much, so the
explosion is big.

2H2 + O2 ⃗0
t H2 O
 Created steam impacts with the cold glass

1  Add 3 particles of zinc into the


test-tube and 5ml of
concentrated HCl acid. Collect
funnel and then condenses.

Conclusion:
the gas in a small test-tube by  Hydrogen can be made by reaction
displacement of water. of active metal like magnesium or zinc
 Burning the gas escape from the with a strong acid.
mouth of the tube until the  The mixture of hydrogen and oxygen is
explosion is light. The flame is an explosive mixtures. When the ratio of
blue-violet. H2 to O2 is approximate 2:1, the explosion
 Heating the glass funnel over is the biggest.
the flame, there are drops of
condensation on the funnel.

 Activation of hydrogen atom

2 and hydrogen molecule

 Add 8ml of 10% H2SO4


 Hydrogen molecules in test-tube 2 do not
have strong reduction so not react with

Page | 6
solution and 2 ml of 0.1M KMnO4.
KMnO4 solution into a test-
 Newly born hydrogen is atomic
tube. Shake it carefully and
hydrogen. Atomic hydrogen is extremely
then divide into 3 tube.
reactive, being more reactive than
 Test-tube 1: Use as standard ordinary, so it reacts with KMnO4 and
sample. then the solution color disappears.
 Test-tube 2: Let the hydrogen  Gas produced is atomic hydrogen which
gas flow go through. The color doesn’t combine with another atom to
is unchanged in compassion produce hydrogen molecule yet.
with test-tube 1. Zn + H2SO4  ZnSO4 + 2[H]
 Test-tube 3: Add in some zinc. 5[H] + MnO4- + 3H+  Mn2+ + 4H2O
The solution is transpicuous
and effervescent at the same Conclusion:
time. Atomic hydrogen is more reductive than
hydrogen molecule.

 Prepare O2
Blend 4g KClO3 and 1g MnO2
then put them in the dry test-tube.
Fitting the air receiver as the
picture
2KClO3

MnO 2 , t 0
2KCl + 3O2 ↑

3 (MnO2 is catalyst)

Conclusion:
Heat the test-tube and collect the
KClO3 is pyrolysed easily when using
escaping gas into a big test-tube
suitable catalysts and the reaction release
oxygen.

 Properties of oxygen

4  Take a little of burning Sulphur Sulphur have strong affinity with oxygen,
in the first test-tube of oxygen. so it can burn in air with the violet-blue
Sulphur bursts into violet-blue flame.

Page | 7
flame. ⃗
t0
S + O2 SO2
 Insert a glowing splint into the
second test-tube of oxygen, the The test-tube which has a large amount of
splint bursts into flame. The oxygen will increase the rate of reaction.
reaction is strongly exothermic. At the high temperature, carbon has strong
reduction, so it reacts strongly with oxygen.

C + O2 ⃗
t0 CO2↑
 Heat the copper wire and insert
it into the third test-tube of The black layer is due to copper is oxidized
oxygen. by oxygen and reduce copper (II) oxide

2Cu + O2 ⃗0
t 2CuO
Conclusion:
 Oxygen is strong oxidizer (especially at
high temperature), can easily oxidize
metal and nonmetal to produce oxide.
 Oxygen is needed for fires to burn.

 Chemical property of H2O2

5 a. Oxidizing property of H2O2:


2I- + H2O2 + 2H+ g I2 + 2H2O
 Put into the test tube 4 drops of Iodine solution — iodine dissolved in an
KI 0.5N + 3 drops of H2O2 3% + aqueous solution reacts with the starch,
a few drops of H2SO4 2N. The producing a purple-black color.
solution is brown. When starch
The brown of solution because I2 reacts
is present, the solution changes
with KI creating complex.
from brown to blue-black.
I2 + KI  KI3 (brown)

b. Decomposition of H2O2:
H2O2 + 2H++ 2e =2H2O E0= +1.77(V)
 Add 10 drops of H2O2 and a
small amount of MnO2 to the H2O2 + 2e = 2OH- E0= +0.87(V)
test-tube. We see bubbing liquid MnO2 is catalyst for the decomposition of
and gas escapes. H2O2.
2H2O2 ⃗
MnO 2
2H2O + O2↑

Page | 8
 Oxygen supports combustion so H2O2 is both reductant and oxidant 2I- +
a good method of testing for H2O2 + 2H+ g I2 + 2H2O
oxygen is to take a glowing Iodine solution — iodine dissolved in an
splint and place it in a sample of aqueous solution reacts with the starch,
gas, if it re-ignites the gas is producing a purple-black colour.
oxygen.
The brown of solution because I2 reacts
with KI creating complex.
I2 + KI  KI3 (brown)

H2O2 + 2H++ 2e =2H2O E0= +1.77(V)


H2O2 + 2e = 2OH- E0= +0.87(V)
MnO2 is catalyst for the decomposition of
H2O2.
2H2O2 ⃗
MnO 2
2H2O + O2↑

Conclusion:
H2O2 is unstable
H2O2 is both reductant and oxidant

 Reaction between S and Cu:  Copper wire reacts readily with hot sulfur
gas to form copper sulfide: 
- Place 1g of sulfur into the Cu(s) +S(g) → CuS(s) (black)
ceramic cup, heating. Put the
copper wire into the cup mouth

6 then it turns black.


- Put the black copper wire into
concentrated HCl. A part of it
 Which dissolving in HCl is CuO.
2Cu + O2 → 2CuO
CuO + 2HCl → CuCl2 + H2O
melts creating blue solution.
(blue)
Conclusion: Sulfur is a strong oxidant at
high temperature.

 Thiosulfate is a reductant

7 Prepare 2 test tube, add 2 drops


of Na2S2O3 0.5N to each.

Page | 9
 Test tube 1: slowly add mixture
solution of KMnO4 0.5N and 8MnO4 + 5S2O32-+ 14H+→ 10SO42- + 8Mn2+ + 7H2O
H2SO4 2N (ratio 1:2). We have
colorless solution, then it turns S2O32- + 2H+ → SO2 + S ↓ + H2O
turbid. Sulfur makes the solution cloudy.

 Test tube 2: add drop by drop


iodine. The charcoal solution
2S2O32- + I2 → 2I- + S4O62-
becomes colorless.
Replacing iodine with bromine
or chloride we also have the 5H2O+S2O32- + 4Br2 → HSO4-+ 8Br-+ 8H+
same result. 5H2O+S2O32- + 4Cl2 → HSO4- + 8Cl-+ 8H+

Conclusion:
Thiosunfate is a strong reductant and easy
to decompose in acidic environment.

ANSWER THE QUESTION


Question 1:
- According experiment 2, atomic hydrogen is more active than hydrogen molecule.
- Explaining: in chemical reactions, molecule hydrogen have to decompose to atomic
hydrogen, and this process requires a lot of energy. In another way, this is not
necessary with atomic hydrogen. So atomic hydrogen is more active than molecule
hydrogen.
- Equation:
10[H] + 2KMnO4 + 3H2SO4 → K2SO4 +2MnSO4 + 8H2O
Question 2:
The important reactions of oxygen is redox reaction. Especially is combustion:
C + O2 → CO2
C6H12O6 + 6O2 → 6CO2 + 6H2O

Page | 10
Oxygen has many applications in life: medical, life support and recreational use
(low-pressure breathing gas…), industrial (smelting of iron ore into steel, metal
cutting and welding…)
Question 3:
To preservation H2O2, we have to:
 Contain in dark-colored glass bottle, avoid sunshine.
 Add inhibitors like phosphoric acid or sunfuric acid.
Question 4:
- Sulfur is an oxidant:
S0 +2e → S2-
Example: H2 + S → H2S
- Sulfur is a reductant:
S0 – 4e → S4+
S0 – 64e → S6+

Example: S + O2 ⃗
t0 SO2

S + 6HNO3 → H2SO4 + 6NO2 ↑ + 2H2O.

Question 5:
Thiosunfate (S2O32- ) is a reduction because the oxidation numbers of sulfur are
+6 and -2 (reducing agent). Structure of Na2S2O3 :

Na –O O Na –O O
S or S
Na –O S Na –S O

2 S2O32- + I2 → 2I- + S4O62-


5H2O + S2O32- + 4Br2 → HSO4- + 8Br- + 8H+
5H2O + S2O32- + 4Cl2 → HSO4- + 8Cl- + 8H+

Page | 11
8MnO4- +5S2O32- +14H+ → 10SO42- + 8Mn2+ +7H2O

Unit 8: THE METALS OF GROUP IB

Chemcial reactions, interpretation and


Experiment Experimetal Description
calculation

 Prepare CuSO4.2H2O  The black is from CuO

 Add 2g CuO and then 15ml 4N CuO (black) + H2SO4  CuSO4 + H2O
H2SO4 (20% excess), heat and Cu2+forms the complexion [Cu(H2O)6]2+ to
stir carefully until it becomes produce a blue solution.
the pale blue solution
Cu2+ + 6 H2O  [Cu(H2O)6]2+ (blue)
 Filter and dry the filtrate until
the crystal scum appear. Keep  The crystal is CuSO4.5H2O.
it at room temperature, the blue CuSO4 + 5H2O  CuSO4.5H2O

1 crystal grows
 Filter the crystal under
vacuum. The mass of the
Efficiency:
m
mlt  CuO * M CuSO .5 H O  6.25 g
M CuO 4 2

crystal m = 4,72g
m
H *100%
mlt =64.48%
Conclusion:
 Cu2+can form complexion easily
 Cu2+ salts sometimes exist in the hydrate
form
 Cu2+ solutions are blue

 Properties of Cu(OH)2

2  Add 0.5ml of 5M CuSO4


solution separately into 3 test-
tubes, then add some drops of
CuSO4 + 2NaOH  Cu(OH)2 + Na2SO4

Page | 12
2M NaOH. The pale blue
precipitate appears.

 Tube 1: Heat → The Cu(OH)2 CuO + H2O


precipitate turns black (CuO)
 Tube 2: Add concentrated
solution of HCl, The Cu(OH)2 + 2HCl  CuCl2 + 2H2O.
precipitate dissolves to produce CuCl2 + 2Cl- [CuCl4]2-
the green solution
(green)

 Tube 3: Add NaOH (40% Cu(OH)2 + 2NaOHNa2[Cu(OH)4].


excess) and then burn. The
precipitate dissolved to (purple)
produce the blue-purple
solution.
Conclusion:
Cu(OH)2 cannot dissolve in aqueous solution,
dehydrate if heated.
Cu(OH)2 is weakly amphoteric

 Properties of Cu (II)
 Prepare a mixture of 0.1g Cu + Cu + CuCl2 2CuCl (white)
1ml of 2M CuCl2 + 1ml of 2M
HCl, the white precipitate
appears.
 Heat in 3 minutes, the CuCl + Cl- [CuCl2]-.

3 precipitate dissolved to -
produce the dark green solution [CuCl2] is black in blue  dark green
 Let it cool down, add water → [CuCl2]-is unstable and decomposed
The solution became blue and
[CuCl2]- Cl- + CuCl (white)
the white precipitate appeared

Conclusion:
Cu2+ is a weak oxidizer in the acidic medium

 Add 5 drops of 40% HCHO

4 solution separately into 5 test-


tubes. Heat it.
Cu2+ + HCHO + H2O  Cu+ + HCOOH + H+

Page | 13
 Add concentrated NaOH 2Cu+ + 2OH-Cu2(OH)2 (yellow)
solution then heat it → the Cu2(OH)2 Cu2O + H2O.
yellow precipitate appears then
turns brick-red
Conclusion: Cu2+ is a weak oxidizer

Prepare 2 test-tube:
 Tube 1: 5 drops of 0.5M CuSO4 Cu2+ + I- CuI2
then add 1M KI → the yellow CuI2 is unstable
precipitate appears and the
solution turn light brown. CuI2CuI (yellow) + I2
Heat → the purple vapor The purple vapor appears is due to I2
appears which turned the starch
Coordinate complex I3- makes the solution
glue blue. The solution become

5
turning brown.
brown and the white precipitate
appears I- + I2 I3-

 Tube 2: 5 drops of 0.1M AgNO3


Ag++ I-AgI (yellow)
+ KI → the yellow precipitate
appears
Heat → no phenomenon Conclusion:
Ag + is stable oxidation state of Ag.

Prepare 4 test-tube:

6  Tube 1 & 2: Add 5 drops of


0.5M CuSO4 and couple drops
of 2M NaOH → the blue
Cu2+ + 2OH-  Cu(OH)2 (blue)

precipitate appears.
 Tube 1: Add HNO3 → the Cu(OH)2 + 2HNO3 Cu(NO3)2 + 2H2O.
precipitate dissolved to produce (green)
a green solution
 Tube 2: Add 2M NH4OH → the
Cu(OH)2 + 4NH4OH  [Cu(NH3)4](OH)2 + 4H2O
precipitate dissolved slowly and
the solution become dark blue. (dark blue)

 Tube 3 & 4: Add 5 drops of

Page | 14
0.1M AgNO3 and couple drops AgNO3 + NaOH  AgOH + NaNO3.
of 2M NaOH. Centrifuge. The AgOH is not stable
fine black precipitate appears.
2AgOH  Ag2O + H2O

 Tube 3: Add HNO3 → the


precipitate dissolved to produce
a transparent solution. Ag2O + HNO3 AgNO3 + H2O
 Tube 4: Add NH4OH, The
precipitate dissolved to produce
a transparent solution Ag2O + 4NH4OH  2[Ag(NH3)2]OH + 3H2O

Conclusion:
The metals in group IB are weakly amphoteric
and can form the stable complexion with NH3

7 Add 5 drops of 0.1M AgNO3


separately into 3 test-tube.
 Tube 1: Add 10 drops of 0.1M Ag+ + Cl-AgCl (white)
NaCl → the white precipitate
appears
Then add NH4OH until excess
→ the precipitate dissolves into a AgCl + NH4OH  [Ag(NH3)2]Cl + H2O
colorless solution.
 Tube 2: Add 10 drops of 0.1M Ag+ + Br- AgBr (pale yellow)
NaBr → the light yellow
precipitate appears.
Then add NH4OH until excess AgBr + NH4OH  [Ag(NH3)2]Br + H2O.
→ the precipitate partly
dissolves
Ag+ + I-AgI (dark yellow)
 Tube 3: Add 0.1M NaI and
NH4OH until excess
Conclusion:
 The colors of the precipitate become

Page | 15
darker from Cl to I
 The solubility: AgCl>AgBr>AgI due to
the increase in their anion radius.

Add 5 drops of 0.1M AgNO3 AgNO3 + NH4OH AgOH + NH4NO3.

8
separately into a tube + 10% 2AgOH  Ag2O + H2O
NH4OH. Then add 5 drops of 40%
HCHO solution and heat up Ag2O + 4NH4OH  2[Ag(NH3)2](OH) + 3H2O
4[Ag(NH3)2](OH) + HCHO  4Ag +
(NH4)2CO3 + 6NH3 + 2H2O

ANSWER THE QUESTIONS


Question 1:
Although the metals in group IA and IB have the similar outer layer structure
with one electron, their properties are very different. This is because the barrier
effect of IB metals is weaker than that of IA metals, leading to their higher first
ionization energy. Consequently, the IB metals are less active than the IA metals.
Question 2:
Cu can be produced from a copper carbonate hydroxide mineral, malachite
CuCO3.Cu(OH)2
CuCO3.Cu(OH)2CuO + CO2 + H2O.
CuO + C  Cu + CO.

Page | 16
Unit 10: GROUP VIB (CHROME)

Experim Experimental Description Chemical reactions, interpretation and


ent calculation
Mix and grind carefully 2.5gMixgrin- - Grind the mixture to increase the conduct area
K2Cr2O7 and 1g sucroza. Add the and speed up the reaction.
mixture into a stainless bowl.
- Alcohol is solvent that dissolving
Add 3 ml alcohol and burn the sucroza and vaporizing water faster.
mixture until the alcohol run out.

After that, heat it at 600oC in 1 C12H22O11→ 12C + 11H2O.
hour, approximately.

1

Cool down at room temperature, K2Cr2O7 + 2C → Cr2O3 +K2CO3 + CO.
then wash it with water, filter The product is Cr2O3.
and dry the solid, weigh.
m( K 2Cr2O7 )
The mass of the solid m=1,13g m  * M (Cr2O3 )
Efficiency: M ( K 2 Cr2 O7 ) =
1,29g
mex
H *100% 1,13
m = 1,29 *100% = 87,6%

 Add 5g K2Cr2O7 and 25 ml of

2 distilled water into a beaker,


heat and stir carefully. The
solution is orange

 Slowly add 6 ml of K2Cr2O7 + H2SO4 2CrO3 + K2SO4 + H2O.


concentrated H2SO4 solution. H2SO4 and CrO3 take water out from the
The color of the solution solution so the color is getting darker.
becomes darker, the reaction
produces heat.
 2CrO3 + 3H2SO4 + 2C2H5OH  Cr2(SO4)3 +
CH3CHO + CH3COOH + 5H2O
Page | 17
 Cool down at room
temperature, put the beaker
into water and add 3 ml of 95o
alcohol. The solution changes The pungent odor is from CH3CHO
to blue, the pungent gas
The blue is from Cr3+
appear.
 Let it cool down, wait until In the solution, there are 2 salts which are
crystallization completed. Cr2(SO4)3 and K2SO4. The crystal is chrome
Filter the crystal and weigh it. alum [Cr2(SO4)3.K2SO4.24H2O]
The crystal was purple-blue, Efficiency:
with the mass m=8.40g
m( K 2 Cr 2 O7)
m= ×
M ( K 2 Cr 2 O7)
M([Cr2(SO4)3.K2SO4.24H2O]
=16,97g
mex
H x100% 8,40 ×100 %=¿
m = 16,97 49.50 %

Add 1ml Cr3+ solution separately


into 2 tubes, then slowly add the
dilute solution of NaOH. The Cr3+ + 3OH-Cr(OH)3 grey-blue.
grey-blue precipitate appears

 Tube 1: Add NaOH until Cr(OH)3 + 3NaOH  [Cr(OH)6]Na3

3 excess.The precipitate
dissolves to produce a pale
green solution.
(pale green)

 Tube 2: Add the dilute


Cr(OH)3 + 3H3O+ [Cr3(H2O)6]3+
solution of acid. The
precipitate dissolves to
produce a purple-blue
solution. Conclusion: Cr(OH)3 is amphoteric

4 Add 3 drops of 0.5N K2CrO7 and


 The blue is Cr3+.
Cr2O72- + 3NO2- + 8H+ 2Cr3+ + 3NO3- + 4H2O.
5 drops of 2N H2SO4 into a tube. Cr3+ + 6 H2O  [Cr(H2O)6]3+ brown-blue
Slowly add 0.5N NaNO2
The gas is NO
solution. The solution changes

Page | 18
from orange to brown-blue, the 3HNO2 HNO3 + 2NO + H2O.
bubble gas appears
Conclusion:
Cr2O72- is a strong oxidant in the acidic
medium
 Tube 1: add 3-4 drops of
K2CrO4 and then add drop by
2H+ + 2CrO42- Cr2O72- + H2O
drop of 2N H2SO4. The
solution changes from yellow
to orange.
 Tube 2: add 3-4 drops of
K2Cr2O7 and then add drop by Cr2O72- + 2OH- 2CrO42- + H2O

5
drop of 2N NaOH. The
solution changes from orange
to yellow.
Conclusion:
The balance between Cr2O72-(dichromate)
and CrO42- (chromate) changes with the
different pH values.
 Cr2O72-is stable in the acidic environment
 CrO42-is stable in the basic environment

6
Add 3 drops of 0.5N K2CrO4
separately into 5 tubes
- Tube 1: Add 2 drops of 0.5N Ba2+ + CrO42- BaCrO4
BaCl2. The precipitate is pale
yellow.
- Tube 2: Add 2 drops of 0.5N Sr2+ + CrO42- SrCrO4
SrCl2. The precipitate is
yellow. Pb2+ + CrO42- PbCrO4
- Tube 3: Add 2 drops of 0.5N
CaCl2 No phenomenon.
- Tube 4: Add 2 drops of 0.5N
Pb(NO3)2. The precipitate is
orange. Ag+ + CrO42- Ag2CrO4
- Tube 5: 2 drops of 0.5N
AgNO3 The precipitate is
brown-red Solubility:
Page | 19
T (CaCrO4 )  103,15  T ( SrCrO4 )  104.44 
T ( Ag 2CrO4 )  1011.95  T ( PbCrO4 )  1013.75
Therefore, CaCrO4 does not form any
Centrifuge, then add 1ml of 2N precipitate in the neutral medium
CH3COOH solution into each
tube. The precipitate in tube 1 The reaction between acid and insoluble salt:
dissolves partly. The precipitate
in tube 2 dissolves. The
SrCrO4 + 2H+ H2CrO4 + Sr2+
precipitate in tubes 4 and 5
almost doesn’t dissolve. 1
K 'Sr 2  1,2 * Tst  0,98 ( 6.5)
*104.44  103.04  100
10
Similarly,

K 'Ba2  102.45 K ' Ag   104.47 K 'Pb2  106.27

Therefore, SrCrO4candissolve more in


CH3COOH, BaCrO4 dissolve little and the
others almost don’t dissolve.
Conclusion:
The chromate salts are less soluble. However,
they can dissolve in the acidic medium easily
(except for the chromate salts of alkaline
metals, ammonia, magnesium, calcium)

Page | 20
Unit 12: TRANSITION METALS IN GROUP VIIIB

Explanation – Equation - Calculation


Experiment Process and Phenomenon
- Conclusion
Prepare Mohr salt
 Add 25ml of 4N H2SO4 and 2.5g Hydrogen gas is released
Fe, gas escapes, solution is Fe + H2SO4  FeSO4 + H2
black. Boil the mixture in a fume
hood until Fe dissolved The solution was black due to in fact that
completely. Keep the volume Fe was contaminated and the FeSO4
unchanged while heating → The solution was blue.
gas appeared and the solution Crystallized product is Mohr salt

1
was blue-black. (NH4)2Fe(SO4)2.6H2O.
Filter the solution to get the
filtrate
 Add 7g (NH4)2SO4 solid into
Efficiency:
filtered solution, boil until the
crystal scum appears 2,5
m = x M([(NH4)2Fe(SO4)2.6H2O] = 17,5g
56
 Let it cool to crystallize at room
temperature. Collect the crystal
after filtering under vacuum. The H= mex ×100 %=¿69.43%
mass of crystal is m =12.15g m

Properties of Fe2+ and

2 Fe3+compounds
1. Fe2+ :
Let Morh salt react with:
 K3[Fe(CN)6] → The blue Fe2+ + K3[Fe(CN)6]  KFe[Fe(CN)6]+2K+
precipitate appears (blue)

 H2O2/H2SO4. → The solution is 2Fe2+ + 3H2O2 + 2H+  2Fe3+ + 4H2O + O2


pale yellow and the gas appears

 K2Cr2O7/H2SO4.→ The solution


Page | 21
is dark green 6Fe2+ + Cr2O72- + 14H+  6Fe3+ + 2Cr3+7H2O
 KMnO4/H2SO4.→ The solution (yellow)
is pale yellow.
5Fe2+ + MnO4- + 8H+  5Fe3+ + Mn2+ + 4H2O

 (NH4)2S → The black precipitate (light yellow)


appears
Fe2+ + S2-  FeS (black)
 2N NaOH → the white-blue
precipitate appears and its color
turns to red-brown in the air. Fe2+ + OH-  Fe(OH)2 (blue)
4Fe(OH)2 + O2 + 2H2O  2Fe(OH)3
3+
2. Fe : (red brown)
 Slowly add 2 drops of 0.5N
FeCl3 + 2 drops of 2N H 2SO4 +
0.5N KI → the coal-purple
precipitate appears. When KI
excess, the precipitate dissolves
2Fe3+ + I-  Fe2+ + I2 (dark-orchid)
to produce a brown solution
which made starch glue blue. When KI excess:
 Prepare 2 test-tube: each tube I2 + KI  KI3 (brown-red)
contains 5 drops of FeCl3 0.5N
 Test-tube 1: Add 2 drops
NH4SCN → Solution has
blood-red.
 Test-tube 2: Add 1 drops Fe3+ + 3SCN-  Fe(SCN)3 (blood-red)
K4[Fe(CN)6] 0.5N → the
deep-blue precipitate appears.
Fe3+ + K4[Fe(CN)6]  KFe[Fe(CN)6]
(berlin-blue)

Conclusion:
 Fe2+ can be oxidized easily.
 Fe3+ salts are stable in the air and are
oxidants in the acidic medium.
 Fe3+ can form many complexions with
distinguishing colors.

Page | 22
Properties of hydroxide

3 a. Prepare 2 test-tube: each tube 5


drops CoCl2 dilute solution. CoCl2
solution is pink.
Pink is the color of [Co(H2O)6]2+ complex.

Add a few drops of 2N NaOH →


the solution turned to blue and the Initial: CoCl2 + NaOH  CoOHCl
red precipitate appears. (blue)
 Tube 1: Heat in the air. Then: CoOHCl + NaOH Co(OH)2 + NaCl
Precipitate is grey.
(red)
 Tube 2: Add a few drops of 3% 4Co(OH)2 + O2 + 2H2O  4Co(OH)3
H2O2 → the precipitate is grey
(grey)
and air bubbles appear.
2Co(OH)2 + H2O2  2Co(OH)3 

b. Prepare 2 test-tube: each tube (grey)


contains 5 drops NiCl2 and 2 drops 2H2O2  2H2O + O2 
NaOH 2N → the white-blue
precipitate appears.
 Tube 1: Put precipitate in the air
→ no phenomenon Ni2+ + 2OH-  Ni(OH)2  (white-blue)
 Tube 2: Add a few drops of 3%
H2O2 → the air bubble appears.

c. Prepare 4 test-tube: Oxygen gas is generated by the


 Tube 1: 5 drops Fe + a few
2+ composition of H2O2:
drops of NaOH → the white- 2H2O2  2H2O + O2
green precipitate appears.
Precipitate is divided into 2
parts:
 React to concentrated HCl
solution → the precipitate is Fe2+ + 2OH-  Fe(OH)2 (blue white).
dissolved, producing yellow
solution.
 React to concentrated NaOH
solution. No phenomenon.

Page | 23
 Tube 2: 5 drops Fe3+ and a few
drops of NaOH → the red- Fe(OH)2 + 2H+  Fe2+ + 2H2O.
brown precipitate appears.

Precipitate is divided into 2


parts:
 React to concentrated HCl
Fe3+ + 3OH-  Fe(OH)3  (red brown)
solution → the precipitate is
dissolved, the yellow
solution appears.
 React to concentrated NaOH Fe(OH)3 + 3H+  Fe3+ + 3H2O
solution. No phenomenon.
(yellow)
 Tube 3: 5 drops Co2+ and a few
drops of NaOH → the pink-red
precipitate appears.
Precipitate is divided into 2
parts:
 React to concentrated HCl Co2+ + 2OH-  Co(OH)2
solution → the precipitate (pink-red)
soluble a lot create pale pink
solution.
 React to concentrated NaOH
solution. No phenomena. Co(OH)2 + 2H+  Co2+ + 2H2O
(light pink)
 Tube 4: 5 drops Ni2+ + a few
drops of NaOH → the green
precipitate appears
Precipitate is divided into 2
parts:
 React to concentrated HCl Ni2+ + 2OH-  Ni(OH)2
solution. Precipitate soluble
(green)
create pale pink solution.
 React to concentrated NaOH
solution. No phenomena.

Ni(OH)2 + 2H+  Ni2+ + 2H2O

Page | 24
Conclusion:
 Stability of divalent compounds
ascending, stability of trivalent
compounds decreased from Fe to Ni.
 Their hydroxides have the base property
and are insoluble in the alkaline
solutions.
Color change of salt Co2+ and

4 Tsugaep Reaction of Ni2+


a. Use the saturated CoCl2
solution to write on filter- paper →
Co2+ + 6H2O [Co(H2O)6]2+ (pink)
the letters is pink. Dehydration in heated solution of the
complex [Co(H2O)6]2+ create smaller
Dry over alcohol flame. Pink color
complex [Co(H2O)4]2+ which is blue-violet.
disappear → the color changed
into blue-violet. [Co(H2O)6]2+  [Co(H2O)4]2++ 2 H2O
(blue purple)

b. Tsugaep reaction of Ni :
 Add 5 drops NiCl2 + 1 drop
NH4OH 2N in the test tube → Ni2+ + 2OH-  Ni(OH)2 (green)
the green precipitate appears, Ni(OH)2 + 6NH3  [Ni(NH3)6](OH)2
then the precipitate dissolved
and produce deep green (deep green)
solution.

 Add 1 drop demethyl glioxyme


→ the blood-red precipitate The complex is square, electrically
appears neutralize, strength of acid and base are
both weak. Therefore, create precipitate in
water or in dilute NH4OH solution, but
soluble well in strong acids and bases.
As a result, when instead NH4OH by
NaOH, using enough to create precipitate
Ni (OH) 2 with light red color or adding
NaOH to excess, the precipitate dissolved
immediately. This reaction is used for

Page | 25
quantitative and qualitative Ni2+ in solution.

The complexing of Co(II) and


Ni(II) with NH3 and Cl-
a. Prepare 2 test tubes, put into
each tube 0,5 ml CoCl2
 Tube 1: Slowly add the
2+ -
concentrated NH4OH solution Co + 2OH  Co(OH)2  (pink)
until excess → the pink Co(OH)2 + 6NH3  [Co(NH3)6](OH)2
precipitate appears then
dissolves to create the liquid (brown)
that

brown at top, pink at bottom,


green in the middle. When The concentrated NH4OH absorb the
shaking, the solution turns water of complex [Co(H2O)6]2+, create
brown. green color.
 Tube 2: Add the concentrated
[Co(H2O)6]2+ + 4Cl-  [CoCl4]- + 6H2O

5
HCl solution to excess → the
green solution appears (pink) (green)

b. Rather CoCl2 by NiCl2


Tube 1: Add slowly to excess
NH4OH → the blue precipitate Ni2+ + OH-  Ni(OH)2 (green)
dissolved immediately create deep Ni(OH)2 + 6NH3  [Ni(NH3)6](OH)2
green solution.
(deep green)
Tube 2: Add excess of the
concentrated HCl solution turns Ni(H2O)62+ + 4Cl- NiCl42- + 6H2O
yellow.
(green) (yellow)

Conclusion:
 Ni(OH)2 and Co(OH)2 dissolved in NH3
due to the capable of complex strength.
 Co2+, Ni2+ is capable of complexing with
Clo-, complex change color of solution.

Page | 26
ANSWER THE QUESTIONS
Question 1: From Fe
- Prepare Fe (II) salts: by the reaction between Fe and acid solution (not be a
oxidant)
Ex: Fe(s) + 2HCl(l)  FeCl2(l) + H2(g)
- Prepare Fe (III) salts: by the reaction between Fe and a hot concentrated
solution of H2SO4 or HNO3 (strong oxidant, excess):
Ex: 2Fe(s) + 6H2SO4(l) → Fe2(SO4)3(l) + 3SO2(g) + 6H2O(l)
Fe(s) + 6HNO3(l)Fe(NO3)3(l) + 3NO2(g) + 3H2O(l)

Question 2: The difference between double salts and complex salts

Double Salts Complex Salts

- A mixture of 2 salts which - A compound


crystalize at a same time. - Ionic bonding between the central
- Van der Waals bonding among the metal ion and ligands
salt molecules.

Question 3:
Morh’s Salt (NH4)2Fe(SO4)2.6H2O consist ions: NH4+ , Fe2+ , SO42-

Page | 27
Identify these ions:
 Add concentrated solution of NaOH, heat: appearing the moss-green precipitate
which is easily turns to brown in air → Fe2+, having smell of urine → NH4+.
Fe2+ + 2OH- → Fe(OH)2
2Fe(OH)2 + 1/2O2 + H2O → 2Fe(OH)3
NH4+ + OH- → NH3 + H2O
 Add BaCl2 solution: appearing the white precipitate which can’t dissolve in
strong acidic → SO42-
Ba2+ + SO42- → BaSO4

Question 4:
1. Dissolving Fe in a dilute acid to form Fe2+.
2. Heat the mixture to make the reaction occurring faster. But at high
temperature, it also concentrates H2SO4 solution, leading to oxidizes Fe2+ →
Fe3+. So we have to add H2O regularly to prevent the formation of Fe 3+ (keep
H2SO4 solution dilute).
3. Filter solution to remove impurities (such as Fe excess)
4. Add (NH4)2SO4 into the beaker when it still hot, collect and stir the solution
to form two saturated salts crystalize at the same time. (NH4)2SO4 is a reductant
to keep Fe2+ not to be oxidized to Fe3+.
5. Keep the beaker in the cold water so that the crystallization occurs better.

Question 5:
Distinguish Fe2+
- Fe2+ + K3[Fe(CN)6] → KFe[Fe(CN)6]+2K+.
(turbull)
- 6Fe2+ + Cr2O72- + 14H+→ 6Fe3+ + 2Cr3+7H2O
(moss-green)
- 5Fe2+ + MnO4- + 8H+ → 5Fe3+ + Mn2+ + 4H2O.
(yellow)

Page | 28
- Fe2+ + S2-→ FeS (black)

- Fe2+ + OH- → Fe(OH)2 (light blue).


4Fe(OH)2 + O2 + 2H2O → 2Fe(OH)3 (brown-red)
Distinguish Fe3+
Using I- (KI): 2Fe3+ + I- Fe2+ + I2 (purple)
I2 + KI  KI3
Using SCN- (KSCN): Fe3+ + 3SCN-Fe(SCN)3
Fe3+ + K4[Fe(CN)6] KFe[Fe(CN)6] + 3K+
(berlin)

Question 6:
Tsugaep reaction is a complex reaction, including 2 process:
Ni2+ + OH-  Ni(OH)2 (green)
Ni(OH)2 + 6NH3  [Ni(NH3)6](OH)2 ( deep green)
Tsugaep reaction is used to recognize Ni2+

Page | 29

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