SAFETY AND BASIC LABORATORY TECHNIQUES
(SIC1011)
INORGANIC CHEMISTRY
NAME: DAYANA SYAZANA BINTI MOHD NOOR
MATRIC NUMBER: U2103536
EXPERIMENT: GRAVIMETRIC DETERMINATION AND
IR-CHARACTERIZATION OF NICKEL COMPLEX.
LECTURE NAME: DR. MUGGUNDHA RAOOV A/L
RAMECHANDRAN
OCCURANCE: 4
TITLE: GRAVIMETRIC DETERMINATION AND IR-CHARACTERIZATION OF NICKEL
COMPLEX.
OBJECTIVES:
1. To understand the concept of gravimetric analysis.
2. To derive the mass of nickel calculated from the mass of precipitate.
RESULTS:
Part A
Weight of weighed No.4 sintered glass A with bis(dimethylglyoximato)nickel (ii)
Weight (g) 1 2 3
Mass of empty 29.0260 29.0260 29.0260
crucible (g)
Average mass of 29.0260
crucible (g)
Mass of crucible + 29.2720 29.2720 29.2720
precipitate (g)
Mass of precipitate (g) 0.2460 0.2460 0.2460
Average mass of 0.2460
precipitate (g)
Weight of weighed No.4 sintered glass B with bis(dimethylglyoximato)nickel (ii)
Weight (g) 1 2 3
Mass of empty 28.2020 28.2020 28.2020
crucible (g)
Average mass of 28.2020
crucible (g)
Mass of crucible + 28.4480 28.4480 28.4480
precipitate (g)
Mass of precipitate (g) 0.2460 0.2460 0.2460
Average mass of 0.2460
precipitate (g)
+¿¿
Equation given : ¿2 +¿¿ + 2𝐶4𝐻8𝑂2𝑁2 → 𝑁𝑖(𝐶4𝐻7𝑂2𝑁2 )2 + 2 H
Relative molecular mass of Ni(C4H7O2N2)2
=58.693+2((4×12.011)+(7×1.008)+(2×15.999)+(2×14.007))
= 288.917 g/mol
sintered glass A:
0.2460 g
n Ni(C4H7O2N2)2 = = 8.5146 ×10−4 mol.
288.917 g /mol
1 mol Ni(C4H7O2N2)2 : 1 mol of ¿2 +¿¿
n ¿2 +¿¿ : 8.5146 ×10−4 mol.
Mass of Ni = moles of Ni molar mass of Ni
58.6930 g
= 8.5146 ×10−4 mol
1mol of ∋¿ ¿
= 0.0500g.
Mass
[¿2 +¿¿] =
Volume
0.0500 g
= = 2 g/L.
25× 10−3 L
sintered glass B:
0.2460 g
n Ni(C4H7O2N2)2 = = 8.5146 ×10−4 mol.
288.917 g /mol
1 mol Ni(C4H7O2N2)2 : 1 mol of ¿2 +¿¿
n ¿2 +¿¿ : 8.5146 ×10−4 mol.
Mass of Ni = moles of Ni molar mass of Ni
58.6930 g
= 8.5146 ×10−4 mol
1mol of ∋¿ ¿
= 0.0500g.
Mass
[¿2 +¿¿] =
Volume
0.0500 g
= = 2 g/L.
25× 10−3 L
0.0500 g
Percentage of Ni in Ni(C4H7O2N2)2: % of Ni = 100%
0.2460 g
= 20.33 %
Part B
B
ANALYSIS AND DISCUSSION:
Part A
Based on the experiment, the amount of nickel ions is determined by the precipitation
of dimethylglyoxime in ammonia solution. After 25mL nickel (II) solution is pipetted, 5mL
of dilute HCl and 200mL of distilled water is added. Dilute hydrochloric acid is used to
acidify the solution to ensure the solution is not highly ammonia.
Then, the solution is heated to 70°C. Precipitation is occurs effectively at high
temperatures. Ammonium hydroxide was added drop by drop in the solution to prevent any
abrupt changes in the solution. Then, a red precipitate is formed. More dimethylglyoxime
solution (1%) is added is to ensure no further precipitation occurred.
After 30 minutes heated, the precipitate is filtered through a weighted No. 4 sintered
glass crucible to separate the precipitate from any ions in the solution. Then, the
bis(dimethylglyoximato) nickel (II) precipitate is washed with cool distilled water until there
is no chloride. To test the presence of chloride, a silver nitrate solution is added to the
solution and if cloudy formation formed, washed it again and test again until the solution is
colourless to ensure there is no chloride anymore.
Next, the precipitate is dried overnight before weighing to ensure that all water is
removed. After it has completely dry, the concentration of nickel (II) ions in solution is
determined which is 2.0000 g/L. The analysis is repeated two times.
There are some errors in this experiment, first, the precipitate is not being completely
dried, which causes the weight to be inaccurate. After that, instead of adding ammonium
hydroxide drop by drop, a significant amount of it is applied all at once. Last but not least, the
precipitate has not been thoroughly washed in cool distilled water. In this experiment, the
precipitate is dried overnight to ensure that there is no water remains. The mass of the nickel
is determined which is 0.0500g by multiplying the average of mass of precipitate with the
division of molar mass of nickel and molar mass of Nickel bis(dimethylglyoximato). The
percentage of nickel in nickel complex is 20.33 %.
Part B
For part B, the IR spectra is gained. Based on the absorption frequency, the group of the
compounds is well classified. The main group in the precipitate of Nickel bis(dimethylglyoximato) is
C-H stretching, which has a frequency absorption of 2924.00 cm-1 and 2922.65 cm-1, based on the IR
spectra results. This corresponds to the frequency absorption range of C-H stretching in the IR
spectrum table which is between 3000 and 2840. The compound class is alkane.
In this experiment, some precautions must be taken, such as thoroughly cleaning the KBr plates to
avoid contamination of future samples. In addition, to prevent fogging, handle the experiment with
gloves. Make sure there is not any direct interaction with the soluble solvents.
QUESTION AND ANSWER:
1. Draw the structural formula of bis(dimethylglyoximato)nickel(II) and describe the
type of hybridization involved.
=The type of hybridization is dsp2 (d from 3d, s from 4s and 2p from 4p). Ni forms
octahedral, square planar and tetrahedral complexes in +2 oxidation state. All
electrons of nickel are paired.
2. Explain why the temperature of the solution must be maintained at 60 – 80°C during
the precipitation process.
=The temperature of the solution must be maintained at 60-80⁰C during the
precipitation process due to precipitate that react and formed under high temperature.
Since the solubility of dimethylglyoxime is low in water, increasing the temperature
will increase the solubility of the ionic compounds thus improve the formation of
precipitate. It is a volatile solution.
SUMMARY:
As a conclusion, the concept of gravimetric analysis can be understood well especially in
precipitation gravimetry. The mass of nickel from the mass of precipitate can be derived
which is 0.0500 g. Next, the concentration of nickel (II) ion in the solution was achieved
which is 2.000 g/L. The percentage of nickel in nickel complex is 20.33 %.
REFERENCES:
Lancester S. (2017, April 24). How To Test the Completeness of Precipitation of An Ion.
Retrieved from https://sciencing.com/test-completeness-precipitation-ion8419920.html
StuDocu. (n.d). Retrieved from https://www.studocu.com/my/document/universiti-
malaya/inorganic-chemistry-1/inorganic-1-labreport-u2004-818-exp1/13452514
Edrey, L. (1965). Gravimetric Analysis Part 2. Retrieved from
https://www.sciencedirect.com/book/9781483197647/gravimetric-analysis
Mathias J. (2015, February 1). How Does FTIR Work. Retrieved from
https://www.innovatechlabs.com/newsroom/672/stuff-works-ftir-analysis/
