EXPERIMENT 5

SYNTHESIS OF THE LINKAGE ISOMERS- NITROPENTAAMMINECOBALT(III)

CHLORIDE, [Co(NH3)5NO2]Cl AND NITRITOPENTAAMMINECOBALT(III)
CHLORIDE, [Co(NH3)5ONO]Cl2

OBJECTIVES
- Synthesize linkage isomers of pentaamminenitritocobalt(III) chloride and
pentaamminenitrocobalt(III) chloride complexes

PROCEDURES

Part A Preparation of the nitropentaamminecobalt(III) chloride, [Co(NH3)5(NO2)]Cl2

1. An aqueous ammonia solution was prepared by adding 10 mL of concentrated

ammonia solution to 30 mL of distilled water.
2. 0. 9 g pentaamminechlorocobalt(III) chloride (from experiment 3) was dissolved into
12 mL aqueous ammonia solution.
3. The solution was heated in water bath until the compound dissolves completely.
4. The solution was neutralized by adding concentrated HCl (4M) slowly and it was
tested with litmus paper.
5. 0.9 g sodium nitrate was added and stirred until the all sodium nitrate dissolve.
6. The solution was cooled in an ice bath for 1-2 hours. The time needed to be prolonged
if red solids was not formed within the designated period.
7. The red product was filtered and washed with cool water (0-10℃).
8. The product was dried in the oven (30-40℃).

Part B Preparation of the nitritopentaamminecobalt(III) chloride, [Co(NH3)5ONO]Cl2

1. An aqueous ammonia solution was prepared by adding 10 mL of concentrated

ammonia solution to 30 mL of distilled water.
2. 0.6 g pentaamminechlorocobalt(III) chloride was added in 8 mL aqueous ammonia
solution.
3. The solution was heated in a water bath until the compound dissolves completely.
4. The resulting product was cooled and HCl solution (4M) was added slowly until a pH
4 was obtained.
5. 0.8 g sodium nitrite was added and the product was heated slowly until red precipitate
appeared again.
6. The heating process was continued until the red precipitate back to the solution. We
waited until all the red precipitate dissolves.
7. The resulting product was cooled to room temperature and put into an ice bath.
8. 8 mL of concentrated HCl were dropped wisely into the solution.
 9. The solution was cooled again in an ice bath and then the yellowish crystals were
filtered by using vacuum filtration.
10. The product was washed with ethanol (5 mL x 3 times).

RESULTS

Part A Part B

Mass 0.9000 0.6000

[Co(NH3)5Cl]Cl2(g)
Mass of 0.3622 0.3595
filter paper (g)
Mass of filter paper + 0.5287 0.8239
product (g)
Mass of 0.1665 0.4644
product

CALCULATIONS

Part A Preparation of the nitropentaamminecobalt(III) chloride, [Co(NH3)5(NO2)]Cl2

Equation involved in this experiment:

[Co(NH3)5Cl]Cl2 + NaNO2 + H+ → [Co(NH3)5(NO2)]Cl2 + NaCl

From the balanced equation,

The ratio is 1:1.
0.9000 𝑔
Moles of [Co(NH3)5Cl]Cl2 = 250.446 𝑔𝑚𝑜𝑙−1

= 3.593 x 10-3 mol

1 mol of [Co(NH3)5Cl]Cl2 ≡ 1 mol of [Co(NH3)5NO2]Cl2
3.593 x 10-3 mol of [Co(NH3)5Cl]Cl2 ≡ 3.593 x 10-3 mol of [Co(NH3)5NO2]Cl2

Theoretical mass of [Co(NH3)5NO2]Cl2 = 3.593 x 10-3 mol x RMM [Co(NH3)5NO2]Cl2

= 3.593 x 10-3 mol x 260.9975 g
= 0.9378 g
𝑎𝑐𝑡𝑢𝑎𝑙 𝑦𝑖𝑒𝑙𝑑
% yield = 𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑦𝑖𝑒𝑑 x 100%
0.1665 𝑔
= 0.9378 𝑔 x 100%

= 17.75%

Part B Preparation of the nitritopentaamminecobalt(III) chloride, [Co(NH3)5ONO]Cl2

[Co(NH3)5Cl]Cl2 + NaNO2 → [Co(NH3)5(ONO)]Cl2 + NaCl

From the balanced equation,

The ratio is 1:1.
0.6000 𝑔
Moles of [Co(NH3)5Cl]Cl2 = 250.446 𝑔𝑚𝑜𝑙−1

= 2.396 x 10-3 mol

1 mol of [Co(NH3)5Cl]Cl2 ≡ 1 mol of [Co(NH3)5ONO]Cl2

2.396 x 10-3 mol of [Co(NH3)5Cl]Cl2 ≡ 2.396 x 10-3 mol of [Co(NH3)5ONO]Cl2

Theoretical mass of [Co(NH3)5ONO]Cl2 = 2.396 x 10-3 mol x RMM [Co(NH3)5ONO]Cl2

= 2.396 x 10-3 mol x 260.9975 g
= 0.6254 g
𝑎𝑐𝑡𝑢𝑎𝑙 𝑦𝑖𝑒𝑙𝑑
% yield = 𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑦𝑖𝑒𝑑 x 100%
0.4644𝑔
= 0.6254𝑔 x 100%

= 74.26%
DISCUSSION

CONCLUSION
The linkage isomers of isomers of pentaamminenitrocobalt(III) chloride and
pentaamminenitritocobalt(III) chloride complexes are synthesized. Two equations can be
derived from the experiments which are, the first one for pentaamminenitrocobalt(III)
chloride is
[Co(NH3)5Cl]Cl2 + NaNO2 + H+ → [Co(NH3)5(NO2)]Cl2 + NaCl
while the second equation for synthesize of pentaamminenitritocobalt(III) chloride is
[Co(NH3)5Cl]Cl2 + NaNO2 → [Co(NH3)5(ONO)]Cl2 + NaCl
The percentage yield for both complexes are determined by calculating using formula
𝑎𝑐𝑡𝑢𝑎𝑙 𝑦𝑖𝑒𝑙𝑑
% yield = 𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑦𝑖𝑒𝑑 x 100%

The percentage yield obtained for pentaamminenitrocobalt(III) chloride is 17.75% while for
pentaamminenitritocobalt(III) chloride is 74.26%.

REFERENCES

Synthesis and Isomerization of Nitro and Nitritopentaamminecobalt(III) Chloride, Linkage

isomers. Retrived from http://www.markedbyteachers.com/university-degree/physical-
sciences/synthesis-and-isomerization-of-nitro-and-nitritopentaamminecobalt-iii-chloride-
linkage-isomers.html

Alom, R. Inorganic Chemistry Practical. Retrieved from

https://www.slideshare.net/RobeulAlom/inorganic-chemistry-practical-50865319