UNIT 2: ALKALINE EARTH METAL

I. Experiment purpose

-Verify some chemical properties of alkaline earth metal through their characteristic reactions.
- Know more about water hardness and how to soften hard water.

II. Experiment results

Experiment 1: Observation of the color of alkaline earth metal flames

1) Procedure and phenomenon:
-Dip a piece of clean filter paper into saturated CaCl 2 solution and then hold it over a flame, we
can see the flame’s color turn into orange.
-Conducting experiments similarly, we get the color of red for SrCl2 and yellow for BaCl2.
2) Explanation:
When metal ions absorb energy from the flame, their valence electrons are stimulated to higher
energy level.
⇒ When returning to the ground state, they will release energy with wavelengths in the visible
region and specific to each metal ion, thus having different colors to our eyes.
3) Conclusion:
Different alkaline earth metals' cation in salt will have different color of flame when burning.

Experiment 2: Reaction of alkaline earth metal with H2O

1) Procedure and phenomenon:
Prepare 2 test tubes with 2 ml of distilled water, a little Mg powder and 1 drop of
phenolphthalein.

Tube 1
The reaction happens slowly at room
temperature. The solution has a light pink
color and bubble (H2) appear.
When being heated, more bubble appears and
the pink color gets darker.
When being heated, more bubble appears and
the pink color gets darker.
Tube 2
Adding NH4Cl slowly into the tube, reaction
occurs intensively. The solution becomes
colorless at first, but then, a pink color re-
appear.

2) Reaction and explanation:

The reaction occurs slowly because the Mg(OH)2 produced covers the surface of Mg and prevent
it from reacting:
Mg + H2O → Mg(OH)2↓ + H2↑ (1)
−9.22
A small part of Mg(OH)2 dissolve in the solution (T Mg (OH ) =10
2
¿ and creates OH −¿¿,which
makes phenolphthalein turn into pink.
Mg(OH)2 ⇌ Mg2+ + 2OH −¿¿ (2)
At high temperature, Mg(OH)2 dissolve more into water and creates more OH −¿¿, making the
solution pinker. At the same time, the amount of Mg(OH) 2 covering the surface of Mg reduces;
hence reaction (1) happens faster and results in the appearance of more bubble.
When adding NH4Cl, Mg(OH)2 reacts with NH4Cl and Mg’s surface is exposed, causing reaction
(1) occurs intensively and releases lots of bubble (NH3):
Mg(OH)2 + NH4Cl → MgCl2 + NH3↑ + H2O (3)
Because Mg(OH)2 is dissolved, reaction (2) is shifted to the right based on Le Chatelier’s
principle, reducing OH −¿¿ in the solution causing phenolphthalein to lose its color. After that, the
pink color re-appears because the amount of NH 3 appearing in the reaction (3) can dissolve a
little in the solution and creates base environment:
NH3 + H2O ⇌ NH4+ + OH −¿¿
3) Conclusion:
The reaction of alkaline earth metals hardly occurs in water at room temperature, but they react
better at high temperature and intensively if using suitable catalysts.

Experiment 3: Alkaline earth metal hydroxide synthesis

Part a: Synthesis and properties of Mg(OH)2
1) Procedure, phenomenon and reaction:
-Adding hydroxide and magnesium salt to the test tube, a white precipitate appears (Mg(OH) 2)
and does not dissolve in water.
MgCl2 + 2NaOH → Mg(OH)2↓ + 2NaCl
-After centrifuging to remove the liquid and collect the precipitate, we divide it equally into 3
test tubes:

Tube 1: The precipitate dissolves and the solution becomes colorless

Adding HCl Mg(OH)2 + 2HCl → MgCl2 + 2H2O
Tube 2: The precipitate dissolves, the solution becomes colorless and a gas with
Adding NH4Cl distinct pungent smell is released (NH3)
 Mg(OH)2 + 2NH4Cl → MgCl2 + 2NH3↑ + 2H2O
Tube 3: No reaction and phenomenon because NaOH and Mg(OH)2 are both base.
Adding NaOH

2) Conclusion:
-Alkaline earth metal hydroxides can be synthesized by reaction between their soluble salt and
hydroxide.
-Alkaline earth metal hydroxides have base property.
Part b: Synthesis and properties of alkaline earth hydroxides
1) Procedure and phenomenon:
Preparing 4 test tube containing 1 mL of Mg2+, Ca2+, Ba2+ and Sr2+ 0.5M solutions, respectively.
After adding in each test tube 0.5 mL of NaOH 1M, precipitates appear. The precipitate quantity
increase in the order of Ba(OH)2, Sr(OH)2, Ca(OH)2, and Mg(OH)2.
⇒ The solubility in H2O of hydroxides:
Mg(OH)2 < Ca(OH)2 < Ba(OH)2 < Sr(OH)2

2) Reaction and explanation:

Mg2+ + 2OH −¿¿ → Mg(OH)2↓
Ca2+ + 2OH −¿¿ → Ca(OH)2↓
Sr2+ + 2OH −¿¿ → Sr(OH)2↓
Ba2+ + 2OH −¿¿ → Ba(OH)2
Because atomic radius increase from Mg to Ba, the attractive force between nucleus and valence
electrons decrease.
⇒ Oxygen which has high electron negativity can pull electrons in its direction more effectively
leading to higher polarity of hydroxides.
⇒ Increasing solubility in polar solvent (H2O).
3) Conclusion:
Alkaline earth metal hydroxides have increasing solubility in H2O from top to bottom.

Experiment 4: Evaluation of the solubility of solubility of alkaline earth metal

sulfate salts
1) Procedure and phenomenon:
Preparing 4 test tubes containing 1 ml of MgCl2, CaCl2, BaCl2, and SrCl2 solutions respectively.
Adding slowly 0.5 mL of H2SO4 2N to each test tube:
+ MgCl2: no phenomenon.
+ CaCl2: has a small amount of precipitates.
 + SrCl2: has a cloudy white color.
+ BaCl2: completely cloudy.
Centrifuging to collect precipitates and observing the amount of precipitates, we get the result
about solubility in H2O of alkaline earth metal sulfate salts:
SrSO4 < BaSO4 < CaSO4 < MgSO4
After that, adding H2SO4 to each test tube, we can see the amount of precipitates increases, which
means solubility decreases.
2) Reaction and explanation:
Ca2+ + SO42- → CaSO4↓
Sr2+ + SO42- → SrSO4↓
Ba2+ + SO42- → BaSO4↓
−5.04
Theoretically, MgSO4 is a soluble salt, T CaSO =10 4
>T SrSO =10−6.49 >T BaSO =10−9.97
4 4

⇒ Solubility in H2O of SrSO4 < BaSO4 < CaSO4 < MgSO4 and same with the experiment
results. The reason for this is that going from Mg to Ba, the radius of X2+ increases.
⇒ The distance from nucleus to the valence shell increase.
⇒ More difficult for the negative side of H2O to interact with the positive nucleus of cation.
⇒ Hydration energy becomes less negative and can not overcome the lattice energy.
⇒ Solubility gradually decreases from Mg to Ba.

When adding more H2SO4, the concentration of SO42- concentration increases

⇒ Based on Le Chatelier’s principle, the equilibrium shifts to the side that decreases SO42-, thus
increasing the amount of precipitate and decreasing the solubility.
3) Conclusion:
The solubility of hydroxide salts and sulfate salts of alkaline earth metals are opposite.

Experiment 5: Evaluation of water hardness

1) Procedure:
Using pipet to get 10 ml of hard water and add into a 250 ml erlenmeyer flask, following with a
sufficient amount of distilled water to get a total volume of 100 mL. After that, add 5 ml of pH
10 buffer solution and 7 drop of black Erio-T. Shake and titrate by ETDA 0,02N until the
solution’s color change from red-purple to complete blue. Conduct the procedure 2 times.
2) Experiment result and calculation:
First time: V EDTA0.02 N =9.0 mL
Second time: V EDTA0.02 N =8.5 mL
⟹ V EDTA 0.02 N =8.75 mL

Let X = total remaining content of Mg2+ and Ca2+

1000 1000
⟹ X=V EDTA 0.02 N × 0.02× =8.75 × 0.02× =17.5 mN
V hard water 10

Experiment 6: Water softening

1) Procedure:
Add 50 ml of hard water into a 250 mL beaker, following with 5 ml Na 2CO3 and 2mL of lime
milk. Boil the solution for 3 minutes and filter out the precipitates. Titrate the remaining liquid
with the procedure in experiment 5.
2) Experiment result and calculation:

First time: V EDTA0.02 N =6.3mL

Second time: V EDTA0.02 N =7.0 mL

⟹ V EDTA 0.02 N =6.65 mL

Let X’ = total remaining concentration of Mg2+ and Ca2+ after adding Na2CO3
1000 1000
⟹ X ' =V EDTA 0.2N × 0.02× =6.65 ×0.02 × =2.66 mN
V hard water 50

3) Explanation:
X’ > X because when adding Na2CO3, the following reactions happen:
Mg2+ + CO32- →MgCO3↓
Ca2+ + CO32- → CaCO3↓
⟹ The concentration of Mg2+ and Ca2+ in the solution decrease.

III. Answer the questions:

Q1. In reaction 2, explain the role of NH4Cl. Is it compulsory that NH4Cl be used or are
other NH4 salts also applicable?
+¿¿
The role of NH4Cl is to provide NH 4 for dissolving Mg(OH)2 ,causing Mg surface to be
exposed and increase the reaction rates between Mg and H2O.
⟹ We can use other NH4 salts like (NH4)2SO4 instead of NH4Cl.

Q2. Aside from using washing soda (Na 2CO3), are there any other methods for softening
hard water? Write down the equation for each method.
We can use Ca(OH)2 and Na3PO4 to soften hard water. Firstly, adding excess Ca(OH) 2 to the
hard water sample, making all Mg2+ precipitate as Mg(OH)2

Mg2+ + OH −¿→ ¿ Mg(OH)2↓

Next, adding excess Na3PO4 to make all Ca2+ precipitate as Ca3(PO4)2

3Ca2+ + 2(PO 4 )3−¿⟶ ¿ Ca3(PO4)2↓

 Unit 12: GROUP VIII TRANSITIONAL METALS

I. Experiment purpose

Verifying some properties of 𝐹𝑒 2+, 𝐹𝑒 3+, 𝑁𝑖 2+ , 𝐶𝑜 2+

II. Experiment results:

Experiment 1:
1)Procedure:
-Fill a 100mL beaker with 25mL of 4N H 2SO4 solution. Then add 2.5g of iron powder, place the
beaker under the fume hood for heating. Maintain the process until all the debris are completely
dissolved. Filter the solution then introduce to a 100 mL beaker, containing 7g of (NH 4)2SO4
solid. After finishing the filter process, let the mixture remain at an ambient temperature for
crystallization. Mixing is required.
-Dip the beaker in ice water for 30 mins.
-Vacuum filter to obtain crystals. Place the Morh’s salt (crystals) on filter paper, let air dry and
then weigh the product.
2) Reaction and phenomenon:
Fe + H2SO4 → FeSO4 + H2↑
⟹ A colorless gas appears (H2), the solution has both green color due to FeSO4 and black color
due to impurities in iron powder.
FeSO4 + (NH4)2SO4 + 6H2O → (NH4)2Fe(SO4)2.6H2O

⟹ The obtained crystallization product is (NH4)2Fe(SO4)2.6H2O (Morh’s salt)

3) Calculation:
CN 4
× V = × ( 25× 10 ) =0.05(mol)
−3
nH SO4 =C M × V =
2
n 2
2.5
n Fe = ≈ 0.045(mol)
56
7
n(NH ) SO = ≈ 0.053(mol)
4 2 4
132
⟹ H% is calculated based on Fe
mexperiment =5.25( g)
2.5
mtheory = × 393=17.5( g)
56
m experiment 5.25
H %= ×100 %= ×100 %=30 %
m theory 17.5
Experiment 2: Properties of Fe2+ amd Fe3+ compounds
Part a: Test of Fe2+
1) Procedure:
Use the Morh’s salt solution to react with the following solutions respectively:
- With the indicator K3[Fe(CN)6]
- With H2O2, a K2Cr2O7 solutiom, and a dilute KMnO4 solution which was previously acidized
using H2SO4
- With 0.2M (NH4)2S
- With dilute 2N NaOH. Place the resultant product under an ambient atmosphere.
2) Reaction and phenomenon:
- With the indicator K3[Fe(CN)6]: A blue precipitate appears (KFe[Fe(CN)6])
Fe2+ + K3[Fe(CN)6] ⟶ KFe[Fe(CN)6]↓ + 2K+
- With H2O2/H2SO4: Solution becomes yellow (Fe3+), a colorless gas emits (O2)
2Fe2+ + 3H2O2 + 2H+ ⟶ 2Fe3+ + 4H2O + O2↑
- With K2Cr2O7/H2SO4: Solution has a color of dark yellow
6Fe2+ + Cr2O7 2- + 14H+ ⟶ 6Fe3+ + 2Cr3+ + 7H2O
- With KMnO4/H2SO4: KMnO4 loses its color, solution has a color of light yellow
5Fe2+ + MnO4 - + 8H+ ⟶ 5Fe3+ + Mn2+ + 4H2O
- With 0,2M (NH4)2S: A black precipitate appears (FeS)
Fe2+ + S2- ⟶ FeS↓

- With dilute 2N NaOH: A green precipitate appears (Fe(OH) 2) and becomes brown-red when
contacting with air (Fe(OH)3)

Fe2+ + 2O H−¿⟶ ¿ Fe(OH)2↓

4Fe(OH)2 + O2 + 2H2O ⟶ 4Fe(OH)3↓
Part b: Test of Fe3+
1) Add 2 drops of either 0.5N Fe2(SO4)3 or 0.5N FeCl3 and 2 drops of 2N H2SO4 to a test tube.
Next, add 2-3 drops of 0.5N KI, we can see a purple precipitate appears (I2).
2Fe3+ + I-  Fe2+ + I2↓
−¿¿
When KI is excess, the precipitate is dissolved and form a brown solution ( I 3 ) that can turn
starch into blue.
I2 + KI  KI3
2) Use 2 test tubes, each containing 5 drops of either 0.5N FeCl3 or 0.5N Fe2(SO4)3
 Test tube 1: Add 2 drops of 0.01N NH4SCN
The solution has red-blood color (Fe(SCN)3)
Fe3+ + 3 SCN −¿¿ ⟶ Fe(SCN)3
Test tube 2: Add 1 drop of 0.5N K4[Fe(CN)6]
A Berlin-blue precipitate appears
(KFe[Fe(CN)6])
Fe3+ + K4[Fe(CN)6] ⟶ KFe[Fe(CN)6]↓

Conclusion:
-Fe2+ can be oxidized quite easily to Fe3+.
-Fe3+ is stable in air, has oxidization property in acidic solution, and can participate in
complexation reactions.

Experiment 3:
Part a:
1) Procedure:
Add 5 drops of CoCl2 to each of 2 test tubes prior to introducing a few drops of 2N NaOH.
Test tube 1 Test tube 2
Heat up. Record the color of precipitate. Use Add a few drops of 3% H2O2. Record the
a glass rod to stir the mixture steadily. Place phenomenon
the mixture in an ambient atmosphere for a
while. Observe the change in color

2) Reaction and phenomenon:

Co2+ solution has a pink color due to the formation of [Co(H2O)6]2+
Co2+ + 6H2O ⇌ [Co(H2O)6]2+
When adding NaOH, a blue precipitate appears (CoOHCl) and then turns into red (Co(OH)2)
CoCl2 + NaOH  CoOHCl
CoOHCl+ NaOH  Co(OH)2+NaCl

Tube 1 Tube 2
The precipitate turns into gray (Co(OH)3) The precipitate turns into gray (Co(OH)3) and
4Co(OH)2 + O2+2H2O  4Co(OH)3↓ gas emits (O2)
2Co(OH)2 + H2O2  2Co(OH)3
2H2O2  2H2O + O2↑
3) Conclusion: Co can be oxidized quite easily to Co3+
2+

Part b:
1) Procedure:
Add NiCl2 to 2 test tubes, 5 drops each. Then add 2 more drops of NaOH. Place the precipitate
from test tube 1 in an ambient atmosphere. Add 3% H2O2 solution to test tube 2.
2) Reaction and phenomenon:

When adding NaOH, a green precipitate appears (Ni(OH)2)

Ni2+ + 2OH- Ni(OH)2↓

Tube 1 Tube 2
No color change to the precipitate Gas bubbles appear (O2):
2H2O2  2H2O + O2↑
3) Conclusion: Ni is stable and hardly oxidized to Ni3+
2+

Part c:
1) Procedure:
Use 4 test tubes. Add 5 drops of different salt solutions, one kind to each: Fe2+ ,Fe3+ ,Co2+ ,Ni2+.
Introduce NaOH to these test tubes to create anhydroxide. Divide each of the previous
precipitates into 2 parts. Mix one part with concentrated HCl and the other part with concentrated
NaOH. Observe the phenomena.
2) Reaction and phenomenon:

Tube 1: Adding HCl ⇒ The precitipate dissolves

A white green precipitate
Tube 1,2:
appears (Fe(OH)2)
Fe2+
Fe2+ + 2OH-  Fe(OH)2↓
A brown red precipitate
Tube 3,4:
appears (Fe(OH)3)
Fe3+
Fe3+ + 2OH-  Fe(OH)3↓
A light red precipitate
Tube 5,6:
appears (Co(OH)2)
Co2+
Co2+ + 2OH-  Co(OH)2↓
Tube 7,8: A light green precipitate
appears (Ni(OH)2)
and solution changes to light green (Fe2+).
Fe(OH)2 + 2HCl  FeCl2 + 2H2O
Tube 2: Adding NaOH
⇒ No reaction and phenomenon
Tube 1: Adding HCl
⇒ The precitipate dissolves and solution changes
to yellow (Fe3+).
Fe(OH)3 + 2HCl  FeCl3 + 2H2O
Tube 2: Adding NaOH
⇒ No reaction and phenomenon
Tube 1: Adding HCl
⇒ The precitipate dissolves and solution changes
to light pink (Co2+).
Co(OH)2 + 2HCl  CoCl2 + 2H2O
Tube 2: Adding NaOH
⇒ No reaction and phenomenon
Tube 1: Adding HCl
⇒ The precitipate dissolves and solution changes
 to yellow (Ni2+).
Ni(OH)2 + 2HCl  NiCl2 + 2H2O
Ni2+ Ni2+ + 2OH-  Ni(OH)2↓
Tube 2: Adding NaOH
⇒ No reaction and phenomenon

3) Conclusion:
Hydroxides of Fe, Ni, Co have base property and do not dissolve in other bases.

Experiment 4:
1) Mark filter paper with a saturated CoCl2 solution, the mark has a color of pink due to the
complex [Co(H2O)6]2+ .
Co2+ + 6H2O ⇌ [Co(H2O)6]2+
Hovering the filter paper above the alcohol lamp, the mark change to blue because [Co(H 2O)6]2+
dehydrate to form [Co(H2O)4]2+
2) Add 5 drops of NiCl2, 1 drop of 2N NH4OH, and 1 drop of dimethylglyoxime respectively, to
a test tube, we can see a green precipitate forms (Ni(OH)2) and then dissolve to form a dark blue
solution ([Ni(NH3)6](OH)2).
Ni2+ + 2OH −¿¿  Ni(OH)2↓
Ni(OH)2 +6NH3  [Ni(NH3)6](OH)2

After adding dimethylglyoxime, a red-blood precipitate appears

Experiment 5:
1) Procedure:
Use 2 test tubes. Add 0.5mL of CoCl2 solution to each tube. Slowly add an excessive amount of
concentrated NH4OH solution to one test tube and HCl to other one. Repeat the procedure but
replace CoCl2 by NiCl2
2) Reaction, phenomenon and explanation:

Tube 1: Adding concentrated NH4OH

⇒ A pink precipitate appears (Co(OH)2↓) and then dissolve to form a brown
solution ([Co(NH3)6](OH)2 )
Tube 1,2: Co2+ + 2OH −¿¿  Co(OH)2↓
CoCl2 Co(OH)2+6NH3  [Co(NH3)6](OH)2
Tube 2: Adding HCl
⇒ The solution turn into blue ([CoCl4]2-)
[Co(H2O)6]2+ + 4Cl−¿¿ ⟶ [CoCl4]2- + 6H2O
Tube 3,4: Tube 1: Adding concentrated NH4OH
 ⇒ A light green precipitate appears (Ni(OH)2↓) and then dissolve to form a
blue solution ([Ni(NH3)6](OH)2 )
Ni2+ + 2OH −¿¿  Ni(OH)2↓
NiCl2 Ni(OH)2+6NH3  [Ni(NH3)6](OH)2
Tube 2: Adding HCl
⇒ The solution turn into light yellow ([NiCl4]2-)
[Ni(H2O)6]2+ + 4Cl−¿¿ ⟶ [NiCl4]2- + 6H2O

3) Conclusion:
Ni2+ and Co2+ can form stable complexes with NH3 and Cl−¿¿ leading to the change of solution’s
color.
Complexes of Ni2+ and Co2+ with NH3 are more stable than their precipitates with OH −¿¿, causing
Co(OH)2 and Ni(OH)2 to be able to dissolve in NH3.

III. Answer the question:

Q1. How are two-valent and three-valent salts synthesized form Fe metal? Write down the
reaction equations.

Double salt Complex salt

- Is the mixture of many salts crystalized - Is a compound

simultaneously - The bonding in complex is the bonding
- Van Der Waals bonding of central ion and ligands

Synthesize Fe Fe + 2HCl ⟶ FeCl2 + H2

2+

Synthesize Fe 2Fe + 3Cl2 ⟶2FeCl3

3+

Q2. How is double salt different from complex salt?

The main difference between double salt and complex salt is that a double salt is a combination
of two salt compounds whereas a complex salt is a molecular structure that is composed of
one or more complex ions.

Q3. What ions are present in the Morh’s salt solution?

NH4+, Fe2+ and SO42-
Q4. Explain the procedure for the synthesis of the Morh’s salt solution?
-Firstly, add Fe to H2SO4 solution to form Fe
-Heating helps the reaction occur quickly.
-Filter solution to eliminate the impurity.
-The filtered solution is introduced to a beaker containing (NH4)2SO4 to make both salt saturated
and crystalized simultaneously.
-Dip the beaker in ice water to make the crystalization process occur easily.
Q5. What reactions are used to detect the presence of Fe2+and Fe3+
Reaction used to detect presence Fe2+
Fe2+ +
+ K3[Fe(CN)6] ⟶ KFe[Fe(CN)6] + 2K
Reaction used to detect presence Fe3+
Fe3+
+ K4[Fe(CN)6] ⟶ KFe[Fe(CN)6] + 3K+
Fe3+ + 3SCN- ⟶ Fe(SCN)3
Q6. What kind of reaction as conducted in the Experiment 4b? What is it used for?
This reaction is used to qualify and quantify Ni2+ in solution.