UNIVERSITY OF BOTSWANA DEPARTMENT OF CHEMISTRY

CHE 314: ANALTICAL CHEMISTRY LAB

NAMES MONGALE T.
STUDENT ID. 201401514
EXPERIMENT 1 GRAVIMETRIC ESTIMATION OF NICKEL (II)
LAB GROP MONDAY
DATE 27/02/2023
ABSTRACT
Nickel was precipitated as nickel dimethylglyoxime by adding a solution of dimethylglyoxime
C4H6 (NOH) 2 in alcohol, as well as aqueous ammonia solution. A mass of 0.206775 g of Ni
(C4H7O2N2)2 precipitate was obtained, and it was quantitatively found that 0.042 g of nickel ions
were contained in the precipitate.

AIM

The aim of this experiment was

to use the analytical tool, TLC,
to find the composition of
solutions of amino acids and
combination analgesics, then
use the results to determine the
composition of unknown
compounds.
The aim of this experiment was
to use the analytical tool, TLC,
to find the composition of
solutions of amino acids and
combination analgesics, then
use the results to determine the
composition of unknown
compounds.
The aim of this experiment was
to use the analytical tool, TLC,
to find the composition of
solutions of amino acids and
combination analgesics, then
use the results to determine the
composition of unknown
compounds.
The aim of this experiment was
to use the analytical tool, TLC,
to find the composition of
solutions of amino acids and
combination analgesics, then
use the results to determine the
composition of unknown
compounds.
The aim of this experiment was
to use the analytical tool, TLC,
to find the composition of
solutions of amino acids and
combination analgesics, then
use the results to determine the
composition of unknown
compounds.
The aim of this experiment was
to use the analytical tool, TLC,
to find the composition of
solutions of amino acids and
combination analgesics, then
use the results to determine the
composition of unknown
compounds.
The aim of this experiment was
to use the analytical tool, TLC,
to find the composition of
solutions of amino acids and
combination analgesics, then
use the results to determine the
composition of unknown
compounds.
The investigation was carried out in order to determine nickel gravimetrically using the ligand
dimethylglyoxime.

INTRODUCTION

A process known as precipitative gravimetric analysis is applied, which according to Hefferren

(2013) is an analytical technique that employs precipitation reactions to separate ions from
solutions. A precipitating agent is added to a solution so as to form a solid precipitate which will
be separated from the liquid component through filtration and drying, and the mass taken in
order to detect the change in mass of a substance. This kind of gravimetric analysis is used in
compounds of high ionic strengths in order to reduce the salting out effect of the slowly forming
crystals by reducing the electrostatic repulsion between precipitating molecules and crystals,
hence increasing the rate of crystal formation. In the estimation of nickel, the ligand
dimethylglyoxime in alcoholic solution is used as the precipitant species, which coordinates to
the metal through the nitrogen atoms, such that:

NiSO4 + 2 C4H8O2N2 Ni (C4H7O2N2)2 + H2SO4

Dimethylglyoxime is chelating, since it can coordinate with two of its nitrogen atoms, therefore,
when the pH is buffered (using ammonia) in the range of 5 to 9, a chelation reaction occurs,
where red chelate forms in the solution due to electron donation by nitrogen atoms.

A structure of the dimethylglyoxime complex with nickel ions:

Source: Claudel, 2020.
MATERIALS REQUIRED

Reagents Apparatus
1. precipitating reagent: 100 mL measuring cylinder
1% dimethylglyoxime in alcohol 2 x 100 mL beaker
2. ammonia solution: 1:1 ammonia solution Stirring rod
3. washing solution: distilled water heated in Dropper
70-80℃ Hot plate
4. unknown sample solution of Nickel (II) Crucible
5. Sulphuric acid Sintered glass crucible
Buchner funnel
Oven
Desiccator
Analytical balance

PROCEDURE

100 mL of distilled water and 1 mL of methyl red were added to 25.0 mL of the unknown
sample. Thereafter, dilute ammonia was added dropwise to the mixture, to neutralize the mineral
acid, whilst stirring until color change occurred from red to yellow. Dilute acetic acid was then
added to change the color form yellow to orange again (making solution acidic again).
Subsequently, the solution was heated to about 70-80℃ , with 30 mL of 1% dimethylglyoxime
added with continuous stirring, followed by a dropwise addition of 1:1 ammonia solution until
the solution was alkaline. The precipitate was then digested on a water bath for an hour, and
then tested for complete precipitation by adding a few drops of dimethylglyoxime solution to the
clear supernatant liquid, followed by cooling for an hour. The cooled supernatant liquid was
transferred to a weighed sintered crucible and the precipitate was washed three times with hot
distilled water, and then transferred to the crucible. The precipitate on the sintered glass crucible
was washed with hot distilled water until it was free from Cl - and SO2−¿¿4 ions, then dried in an
oven at temperature of about 110 ℃ for an hour. The crucible with precipitate was cooled for a
further 30 minutes before weighing, then the process of further drying of precipitate in oven,
cooling and weighing was repeated to obtain a total of four masses.
RESULTS AND ANALYSIS

Mass of empty crucible: 74.8193 g

A table showing the obtained masses of crucible + Ni (C4H7O2N2)2

1 2 3 4
Initial mass of 74.8193 74.8193 74.8193 74.8193
crucible (g)
Final mass of 75.0263 75.0260 75.0260 75.0260
crucible (g)
Net weight of 0.207 0.2067 0.2067 0.2067
precipitate (g)

NiX + 2 C4H8O2N2 Ni (C4H7O2N2)2

Average mass of Ni (C4H7O2N2)2;

0.207+( 3∗0.2067)
= 0.206775 g
4
Molar mass of Ni (C4H7O2N2)2= 288.9146 g/mol

Number of moles of Ni (C4H7O2N2)2

mass 0.206775 g
n= = = 0.00072 moles
molar mass 288.9146 g /mol

Mass of Nickel;
1 mole of Ni (C4H7O2N2)2 contains 1 mole of Ni2+ ions. Thus,

288.9146 g of Ni (C4H7O2N2)2 contain 58.7 g of Nickel.

288.9146g: 58.7g
0.206775g: x

(58.7∗0.206775) g
x= = 0.042 g 42 mg
288.9146 g
DISCUSSION
A sample containing nickel (II) was reacted with dimethylglyoxime to obtain a precipitate of
(dimethylglyoximate) nickel (II). The results obtained indicate that there was approximately 42
mg of Ni2+ in the obtained precipitate, which is a similar yield to an experiment carried out by
CONCLUSION

REFERENCES

1. Hefferren J. J., Li N., & Li K., Quantitative Chemical Analysis, World Scientific
Publishing Company, 2013, page 191.
2. Claudel M., Schwarte J., & Fromm, K. New Antimicrobial Strategies Based on Metal
Complexes Chemistry, 2020. 2. 851.
. For beaker 1, the loss of
precipitate might have occurred during cooling of the
heated mixtures, whereby excessive water in the basin has
caused the beakers to nearly capsize. In the process,
beaker 1 might have been the worst affected since a small
amount of cooling water entered the beaker causing traces
of precipitate washed out. Throughout the experiment,
beaker 2 was kept intact and t herefore the high
concentration value.
Smaller amounts of precipitate in beakers 1 and 3 might
have also been caused during addition of DMG after the
heating of the solution replicates. All replicates were heated simultaneously
but as the glassware used to

contain the DMG was limited, the reagent was added to the
replicates one after another. This causes the DMG to
react with the solution at different temperatures and
thereby affecting the amount of precipitate produced.
Replicate 2 was added DMG first at the ideal temperature
and thereby the higher concentration value. During the
filtration of precipitate, a small amount of the mixture
of replicate 3 had spilled out of the crucible due to
hasty pouring of the mixture into the crucible, thereby
decreasing the amount of precipitate filtered.
However, in the calculations, the calculated average
concentration value is far smaller than the ideal value
(0.250 mg/mL) and the standard deviation is deemed too
large (The smaller the standard deviation, the more
closely the data are clustered about the average value).
Therefore, in this case, the average value is discarded
and the concentration value of replicate 2 (0.109 mg/mL)
is taken as the concentration of Ni
2+
of the sample
solution since it is not only nearest to the ideal value,
but it is also considered the best handled replicate
sample throughout this experiment. This means that every
millilitre of the sample solution contains 0.109 mg of
Ni
2+
.