C.

O Maleka
14066361
CMY 383

Experiment 4: The extraction of nickel from a

simulated steel sample

Abstract
In this experiment we separated and then extracted Nickel from a simulated steel
sample. We prepared a standard solution of Nickel sulphate and we determined the
absorbance value of the solution at 430nm after separation using a UV-Vis
spectrometer. A straight line graph of absorption versus concentration of the Nickel in
the sample was drawn. The solution sample from number 5, 6 and 7 were measured in
the UV-Vis spectrometer. The absorbance value to the three samples was almost
identical. We also calculated the concentration of the standard prepared

Concentration of the Nickel standard solution:

NiSO4.7H20 in 250mL solution

n= 1.120g/280.08630g.mol-1 = 3.98878x10-3 mol.
c= 3.98878x10-3 mol/0.250L = 0.0159 M

NiSO4.7H20 in 100mL solution is:

C1V1 = C2V2
(0.0159) (0.250) = C2 (0.100)
C2 = 0.03988 M
Method
A standard solution was prepared by using 1.1203g NiSO4.7H2O, dissolved in 10mL
of distilled water. 1mL of HNO3 was added and neutralized by NaOH and acetic acid
is used to dissolve the precipitate, Ni(OH)2.

NiSO4.7H2O(s) + H2O (l) Ni2+ (aq) + SO42+ (aq)

Ni2+ (aq) + 4HNO3 Ni(NO3)2 (aq) + 2NO2 (g) + 2H2O (l)

Ni(NO3)2(aq) + 2NaOH Ni(OH)2 (s) + Na(NO3) + NO2(g) + H2O(l)

The solution is diluted to 250mL and 10-fold diluted again by taking out 10mL of the
above solution and diluting to 100mL. From the diluted solution, 1mL with 9mL
dH2O, 2ml with 8mL dH2O, and 3mL with 7mL dH2O was prepared in three
separating funnels, number 2, 3 and 4 respectively.

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 Results
1mL of the above solution in 9mL H2O, to make up standard solution 2, and the
concentration on standard 2 is:
C2V2 = C3V3; (0.03988) (0.001) = C3 (0.01); C3 = 3.988x10-3 M

2mL of the above solution in 8mL H2O, to make up standard solution 3, and the
concentration on standard 3 is:
C2V2 = C3V3; (0.03988) (0.002) = C3 (0.01); C3 = 7.976x10-3 M

3mL of the above solution in 7mL H2O, to make up standard solution 4, and the
concentration on standard 2 is:
C2V2 = C3V3; (0.03988) (0.003) = C3 (0.01); C3 = 1.196x10-2 M

The Absorbance measured at 430nm of the Nickel Standard Solution at different

concentrations.

Standard Solution
Concentration of
number and Absorbance at 430 nm.
Solution (M):
composition:
2 (1mL of Standard
3.988x10-3 0.0381
Solution with 9mL H2O)
3 (2mL of Standard
7.976x10-3 0.0923
Solution with 8mL H2O
4 (3mL of Standard
1.196x10-2 0.1522
Solution with 7mL H2O)

The absorbance measured at 430 nm from 3 solutions sample no. 3

Individual Sample
Absorbance at 430 nm.
Solution Number:
5 0.0797
6 0.0771
7 0.0733
Average Absorbance: 0.1778

Discussion
The extraction of Nickel from a simulated steel sample involves isolation of Nickel by
binding it to neutral dimethyl glyoxime to form Bis (2,3-butane dione-
diosimato)Nickel(II), known as Ni-dmg complex. This Isolation is used as there are
various metals in steel, such as Fe, Cu and Ni. The Ni-dmg complex is non-polar and
soluble in chloroform, making the chloroform the extraction agent. This solution,
containing Ni-dmg complex in chloroform is analyzed in a UV-spectrometer.

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To get the simulated steel sample in solution, the sample needed to be oxidized, to
form Fe2+, Fe3+, Cu2+ and Ni2+ ions in the steel. HNO3 was used as oxidizing agent and
NO2 (g) formed. This sample was diluted to 100mL and was green in colour. 2mL of
this prepared sample was each added to 8mL of distilled water in 3 separating funnels,
numbered 5, 6 and 7. At this point, each of the separating funnels should have the
same concentration of the oxidized steel sample. Note that in each of the samples,
Ni2+, Fe2+/3+ and Cu2+ is present. We had to use a powder Sodium thiosulphate for 5,6
and 7 since the cubes fixed.

After all analytes were added to the six separating samples, chloroform was added,
mixed and allowed to separate. The chloroform layer extracted from solutions 2, 3 and
4 was measured at 430 nm to make up our standard curve. The solutions containing
the individual samples, was measured at 430nm with UV/Vis-spectrometry. The data
collected was used on the standard curve, to calculate our concentration of Nickel in
the steel sample, as well as too observe how well the isolation of Nickel was
practiced.

1. Ni2+ + 2C4H8N2O2 (C4H7O2N2)2Ni + 2H+

2. 5mL of buffer solution, pH of 6.5.
This buffer solution is to keep the pH of the solution at 6.5. When we look at;

Ni2+ (aq) + 4HNO3 Ni(NO3)2(aq) + 2NO2 (g) + 2H2O(l),

The equilibrium will shift to the left if the pH drops. With a low pH, the
amount of H-ions are abundant in the solution and will bind to the NO2(g) to
form HNO3. The pH is held slightly acidic, to keep the amount of free Ni2+-
ions in the solution. When the pH rises, the Ni2+ and Cu2+ will bind more
efficiently to HNO3 to compensate for the loss of H-ions in the solution.
3.

4. The Copper ions in the solution, needs to be removed. Sodium thiosulfate

forms a complex with copper ions and thus removing the interference of
Copper.

Cu2+ (aq) + 2S2O31- (aq) Cu(S2O3)22-(aq)

This complex is anionic and will dissolve in the aqueous phase. The Copper
will not be extracted with the Nickel in the Chloroform phase. The Copper is
blocked. However, Nickel can also react with thiosulfate and form Ni(S 2O3)22-
complex. This complex is not as stable as the Cu(S 2O3)22- complex, as the
stability constant of Ni(S2O3)22- complex is log1=2.06, where the log1=12.2

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for the Cu(S2O3)22- complex much higher is. Thus, the Cu(S 2O3)22- complex
will form.