SURNAME AND INITIALS: KABEKWA BM

STUDENT NUMBER: 201933674

DATE: 24 AUGUST

TITLE: GRAVIMETRIC ANALYSIS: DETERMINATION OF NICKEL AS

DIMETHYLGLYOXIMATE
ABSTRACT

The method gravimetric analysis of an almost century old method for analysing nickel as
dimethylglyoxime was rigorously examined for nickel analysis, and several of the method
gravimetric analysis were found to have a substantial effect on Ni recovery. To get reliable
and exact Ni results, the residual Ni concentration in the filtrates should also be quantified.

The solubility of the precipitate should be considered; to produce an accurate result, the
solubility of a precipitate must be as low as possible. A complete analytical technique's
accuracy must be greater than or equal to 0.1 percent, which indicates that the precipitate
must include at least 99.9% of the analyte. The precipitate has a mass of 1g after subtracting
the crucible, the mass of nickel is 0.594g, the volume of dimethylglyoxime is 29.7 ml then the
percentage of nickel in the precipitate is 5.94% with stoichiometry calculations.
INTRODUCTION

The constituent sought is transformed into a material that can be isolated from the sample
and weighed in gravimetric analysis, which is one of the most exact and precise methods of
quantitative measurement. Physical gravimetric, thermal gravimetric, precipitation gravimetric,
and electrodeposition are all examples of gravimetric analysis [1]. When high accuracy is
required, only the electrogravimetry approach can be considered a competitor. Ni
manufacturers, raw material providers, and independent umpire laboratories have all created
Ni determination procedures in their own labs around the world, but there hasn't been enough
reporting [2]. Methods also do not necessitate the use of frequently pricey equipment.

The substance to be weighed must be easily removed by filtration to perform precipitative

gravimetric analysis. A non-filterable precipitate must be supersaturated with respect to its
solubility product constant to form. Crystal nucleation may occur at a rate quicker than crystal
growth if it is too far above the saturation limit (the addition of molecules to a crystal nucleus,
eventually forming a non-filterable crystal). Rather than a few giant crystals, a vast number of
microscopic microcrystals emerge when this happens. Micro-crystals may behave like colloids
and pass through a fibrous filter in the most severe situation [3].

The weight percent of nickel in the sample is determined using the precipitation gravimetric
method in this experiment. When a precipitating reagent is introduced to a solution containing
the desired analyte in precipitation gravimetric analysis, an insoluble compound is produced.
There are two key aspects of any precipitation gravimetric analysis [4]. The Ni (DMG)2
precipitate is exceptionally stable, according to thermo gravimetric tests, and does not lose
any weight until temperatures reach 200°C. To ensure that all excess DMG is sublimated
during drying, a temperature of 150°C is recommended as the drying temperature [5].

Although one proton is lost from one oxime group (NOH) on each of the two molecules of
dimethylglyoxime, the chelation reaction is mediated by electron pairs on the four nitrogen
atoms rather than electrons on the oxygen atoms. To keep the pH of the solution from falling
below 5, the reaction is carried out in a solution buffered with either ammonia or citrate [6].

APPARATUS

 Beaker 500ml
  Watch glass
 Stirring rod
 Dropper
 Ice bath
 Filter paper
 Volumetric flask
 Conical flask
 Mantle heater

REAGENTS AND SOLUTIONS

 Ammonium nickel sulfate - 0.4g

 HCl – 5ml
 H₂O – 10ml
 Nickel – 0.0594g
 Nickel dimethylglyoxime – 1g
 Dimethylglyoxime – 1g in 90% ethanol

METHOD

The method was followed as outlined in SCHA022 practical manual from page 25-26

RESULTS

1 mol
Moles of H₂ON₂NiO14S₂ =0.400 g
395.0 g/mol

= 0.00101 mol

N= m/M m= M x n =58.6934 x 0.00101 = 0.0594g Ni

Volume of dimethylglyoxime = 5ml x 0.0594/0.01 =1mg x 0.001g

= 29.7ml = 0.01g

Mass of precipitate in sample = crucible + precipitate mass – crucible

= 30.57g - 29.57g = 1g
 0.0594
Percentage of nickel = x 100
1

= 5.94%

DISCUSSION

Gravimetric analysis is a technique for determining the amount of a substance by first

determining its mass and then utilizing that mass to calculate the quantity. Obtaining a
precipitate from a solution and eliminating any impurities to determine its net mass is one of
the most popular gravimetric analysis techniques. Stoichiometry is the study of the
correlations between the amounts of reactants and products in chemical reactions, and it's
employed in a lot of molar and mass ratio calculations.

Using ammonium nickel sulfate as a reagent, the goal of this experiment is to achieve a
percentage yield of nickel ions in a nickel dimethylglyoxime solution. The experiment began
with the dissolution of 0.4g ammonium nickel sulfate dried salt in distilled water and a solution
5ml HCl. In this solvation procedure, the acid solution is mixed with distilled water first, then
the salt is added, resulting in a homogeneous dilute acid solution.

The colour of the salt is blue but when adding the water, it changed to colourless. When
adding ammonia to the solution dropwise, the solution changed to red as dropping and
became red fully as 10ml of internal was added. Then precipitation started after the solution
was steamed for 20-30 minutes. crystallization occurred when the solution was allowed to sit
in ice bath for one hour.

The percentage yield of nickel precipitate was 5.94% percent after the calculations. The low
number of errors in the nickel sample was primarily caused by one missing step, which was
an incomplete precipitation reaction due to insufficient precipitating agent. The precipitating
agent should be used in a minimum of 29.7ml. However, the minimum amount was not met in
this experiment, resulting in a poor percentage yield of products. As a result, the experiment
can be enhanced by minimizing gravimetric mistakes, which result in a reduced precipitate
mass.
CONCLUSION

The procedure gravimetric analysis of the original Ni as dimethylglyoxime determination

method were optimized. We discussed the final improved procedure in detail and
demonstrated that it can produce accurate and reliable results. The percentage of nickel was
found to be 5.94% and the properties of precipitate was found to be red chelate as its colour.

References

[1] A. Rahman, "Course Hero," [Online]. Available: http://www.coursehero.com. [Accessed 28 August 2021].

[2] p. junnila, "Academia," 14 April 1999. [Online]. Available: http://www.academia.edu. [Accessed 28 August
2021].

[3] S.J.Lyle and R. Maghzian, "PRECIPITATION OF NICKEL DIMETHYLGLYOXIME," ScienceDirect, vol. 14, no. 9,
pp. 1021-1028, 1967.

[4] Harshilganag, "scribd," 21 June 2015. [Online]. Available: http://www.scribd.com. [Accessed 28 August
2021].

[5] A.Claassen and L. Blastings, "SpringerLink," 02 October 1958. [Online]. Available: http://link.springer.com.
[Accessed 28 August 2021].

[6] "gravimetric estimination of nickel," AMRITU VISHWA VIDYAPEETHAM, 2011.