Synthesis and characterization of Ni(DMG)2

(Nickel (ii) dimethylglyoxime) complex

GROUP 2

Sibongisiwe Shongwe 202002403

Happy Mabuza 202002010

Temvelo Vilane 202004446

Temazwide Nxumalo 202003920

CHE402| 08 February 2024

Aim: To synthesize and characterize Nickel (ii) Dimethylglyoxime complex.

Introduction

Transition metal complexes play a crucial role in various fields including catalysis, material
science and coordination chemistry. Dimethylglyoxime acts as a bidentate ligand forming a
stable complex with Nickel ions and is used to detect presence of Nickel in solution. Nickel
reacts with Dimethylglyoxime to form a red precipitate of Nickel Dimethylglyoxime
complex. The Nickel Dimethylglyoxime complex (NiC8H14N4O4) is used in gravimetric
analysis of Nickel.

Fig 1. Nickel (ii) Dimethylglyoxime complex

Procedure
-20mL of NiSO4 solution was poured into a 400mL beaker along with 150mL of distilled
water and heated up to 71oC.
-30mL of 1% DMG was then added, under a fume hood, ammonia solution was them added
with produced a precipitate. The ammonia solution was added up until no more precipitate
could be formed.
-The solution was filtered after letting it settle for 30 minutes, the precipitate washed with
hot water (3 X 5mL).
-The precipitate was then dried in the oven at 100oC and the product weighed after drying.

Synthesis of Ni(DMG)2

M = n/V(l)

0.1 M = n / 0.25

n = 0.1 × 0.25 = 0.025

n = m/ Mw

m = n× Mw

m = 0.025× 280.86 = 7.0215 g

7.0215 g of Nickel sulphate (0.1M) was dissolved in 250 ml of distilled water and 20 mL of
the solution was taken for the synthesis

Equation for synthesis

NiSO4 •7H2O + 2C4H8O2N2 → Ni(C4H7O2N2)2 + H2SO4 + 7H2O

Results

Ni(DMG)2

Weight = 0.044g

Molar mass = 288.92 g/mol

Percentage yield = (actual yield/ theoretical yield) × 100%

Theoretical yield = number of moles × molecular mass

Number of moles

1. NiSO4 • 7H2O = m/ Mm
n = 7.0215 g / 280.86 g/mol

n = 7.0215 / 280.86 = 0.025 mol

1 mol (NiSO4•7H2O) = 1 mol Ni(C4H7O2N2)2

Meaning 0.025 mol NiSO4•7H2O = 0.025 mol Ni(C4H7O2N2)2

2. C4H8O2N2 = m / Mm. Mm= 116.12 g/ mol

m=p×V

m = 1.37 g/ cm3 × 30 ml

m = 41.1 g

Then; n = m/ Mm

n = 41.1 / 116.12 = 0.354 mol

2mol (C4N8O2N2) = 1 mol Ni (C4H7O2N2)2

Meaning; 0.354 mol = 0.177 mol

Number of moles of Ni(C4H7O2N2)2 = 0.025mol

Theoretical yield = 0.025 × 288.92 = 7.223 g

% yield = (0.044g / 7.223g) ×100%

= 0.61%

Determination of weight of nickel in the product

weight =molar mass of ∋ ¿ × weight of ∋(DMG )2 ¿
molar mass of ∋ ( DMG ) 2
58.69 g /mol
× 0.044 g=0.00894 g
= 288.91 g
mol

Characterization of Ni(DMG)2

Solubility testing of Nickel (ii) dimethylglyoxime complex show that:

(i) Water - insoluble

(ii) Methanol - partially soluble
(iii) Ethanol - soluble
(iv) Chloroform - partially soluble

Discussion
The synthesis of Ni(DMG)2 yielded a complex with a mass of 0.044g. Upon calculating the
percentage yield, it was found to be 0.61% which is a very low value. There could be a
number of reasons for this, including side reactions, incomplete reactions, or experimental
errors. A low percentage yield is frequently regarded as a not satisfactory outcome and may
be a sign of the reaction's inefficiency. The complex was red in colour indicating a sense of
accuracy as that is the colour of the complex according to literature.
Furthermore, the Ni(DMG)2 complex underwent solubility tests in varying solvents, namely
water, methanol, ethanol and chloroform. It was found to be insoluble in water, soluble in
methanol and partially soluble in both methanol and chloroform. The fact that it is insoluble
in water suggests that the complex is ionic as nonpolar molecular molecules often aren't
soluble in water, while ionic substances are. Moreover, both polar and nonpolar components
may be present in the complex based on its partial solubility in methanol. We may conclude
that because of nonpolar interactions between the complex and the methanol molecules that
the complex is partially soluble in methanol. The complex may interact with methanol in
particular way, for example by hydrogen bonding or dipole-dipole interactions.
The observation that the complex was soluble in ethanol indicates that it may have some
polarity. The complex's ability to dissolve in ethanol, a polar solvent, suggests that it may
have polar or ionic properties. The complex's solubility in ethanol suggests that it is capable
of participating in particular intermolecular interactions with the ethanol molecules, like
dipole-dipole or hydrogen bonding. Since chloroform is a nonpolar solvent, the complex's
partial solubility with it suggests that it may have both polar and nonpolar regions, which
could allow some degree of interaction with the chloroform molecules. Given its partial
solubility, the complex may interact with chloroform in particular ways, including van der
Waals forces.
The Ni(DMG)2 was then taken for IR spectroscopy for analysis and the result is attached.
Three peaks were observed at 3741.90, 2353.16, and 1620.21cm-1. The peak at 3741.90 cm-1
is indicative of an -OH group of an amide or a hydroxyl group (-OH) in the complex. This
corresponds to the structure of the Ni(DMG)2 complex as it has the oxime group which is
characterized by the presence of a hydroxyl group (-OH) bonded to the nitrogen atom of an
imine. The peak at 2353.16cm-1 is likely associated with the stretching vibration of the N-H
bond. Consequently, a peak at 2353.16 cm-1 in the context of IR spectroscopy indicates the
presence of an N-H bond in the complex. This doesn’t correspond to the formation of the
Ni(DMG)2 complex as it doesn’t have any N-H bond. Lastly, a peak is observed at
1620.21cm-1. The stretching vibration of the N=N bond is linked to this absorption frequency.
This isn’t consistent with the formation of the Ni(DMG)2 as it doesn’t have any N=N bond.
Conclusion

It was possible to successfully manufacture and analyze Ni(DMG)2 through a closely

watched experimental procedure. The chemical was produced following the correct synthesis
protocol, and the goals of the experiment were met. Nonetheless, to decrease the effects of
human error .We might increase our yields by double-checking all observations, records,
measurements, and computations in order to make sure that all measuring instruments are
correctly calibrated before conducting the experiment and to prevent erroneous results. Our
results demonstrate that Ni(DMG)2 was prepared effectively and that the experiment
proceeded as planned to get the desired outcome.

References

A. Dakhel, Y. Ahmed and F. Henari, Opt. Mater., 2006, 28, 925-929.

Q. Hu, G. Yang, Y. Zhao and J. Yin, Anal. Bioanal. Chem., 2003, 375, 831-835.

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