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Nickel Determination via EDTA Titration

This document describes the procedure for determining the concentration of nickel in a solution using complexometric titration with EDTA. Nickel forms a 1:1 complex with EDTA at high pH (pH 10). The solution is first buffered to pH 7 using NH4Cl-NH4OH buffer and the nickel is complexed with the indicator murexide. The solution pH is then raised to 10 and titrated with standardized EDTA solution. The titration endpoint is identified by a color change of the indicator. Calculations are shown to determine the concentration of nickel in the original solution based on the titration results. Maintaining an accurate pH is important for forming stable complexes and obtaining correct results.
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0% found this document useful (0 votes)
914 views3 pages

Nickel Determination via EDTA Titration

This document describes the procedure for determining the concentration of nickel in a solution using complexometric titration with EDTA. Nickel forms a 1:1 complex with EDTA at high pH (pH 10). The solution is first buffered to pH 7 using NH4Cl-NH4OH buffer and the nickel is complexed with the indicator murexide. The solution pH is then raised to 10 and titrated with standardized EDTA solution. The titration endpoint is identified by a color change of the indicator. Calculations are shown to determine the concentration of nickel in the original solution based on the titration results. Maintaining an accurate pH is important for forming stable complexes and obtaining correct results.
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Theory:

Determination of nickel from a given solution is usually done by complexometric titration with
standardized EDTA. Nickel is a d-block element and EDTA is a hexadentate ligand. At higher
temperature and high pH such as pH =10. EDTA forms complex with Ni at the ratio of1:1. First
Ni makes complex with indicator and then the complex reacts with EDTA solution. For
determining Ni the stock solution must be buffered to the desired pH stated before. It is done
adding NH4Cl-NH4OH buffer and titrated directly against EDTA.

Here, Ni cannot be titrated directly and hence an indicator Murexide is needed to form a
complex. pH of the solution is kept about 10. If it is not done, there may appear an error in result,
because, EDTA acts as a hexadentate ligand at higher pH only.

Chemistry involved:

1. Required reagents:
a. NH4OH(1M)
b. Nickel solution
c. Redistilled water
d. Murexide indicator
e. Buffer solution
f. EDTA solution
2. Chemical reactions:
Ni+In(Murexide)=Ni-In
Ni-In +EDTA=Ni-EDTA+In
3. Hints of calculation
1ml 0.02M EDTA≡0.5871mg of Ni

Procedure:

First, 1M NH4Cl solution is prepared by dissolving 26.75g of NH 4Cl in redistilled water and
making upto 500ml in a graduated flask. Then 10ml Ni solution is taken into a conical flask with
a pipette and dilute to about 100ml with redistilled water. After adding Murexide indicator, 1M
ammonium chloride solution is added to keep pH 7. Then it is titrated with standardized EDTA
solution keeping final pH about 10 by adding concentrated NH 3 solution. The colour of solution
being clear yellow indicates the end point.

Data Table:

Table-1: Standardization of EDTA with standard MgSO4 solution:

No. of Volume of Burette reading(ml) Volume of Average Volume of


Initial Final
Obs. EDTA MgSO4 ml MgSO4 ml
1 Solution 0.0 10.0 10.0
2 10 10.0 20.0 10.0 10.033
3 20.0 30.1 10.1

Table-2: Determination of nickel with EDTA solution

Burette reading(ml) Volume of Average Volume of


Volume of
No. of Nickel
EDTA EDTA
Obs. Solution Initial Final
ml
ml ml
1 11.6 21.3 9.7
2 10 21.3 31.1 9.8 9.85
3 31.1 41.0 9.9

Calculation:

V 1×N 1
Normality of EDTA, N2=
V2

10× 0.01
=
10.033

=0.00997M

1ml 0.011M EDTA ≡ 0.5871 g of Ni

9.85ml0.01 M EDTA ≡ 5.7829 mg of Ni

= 5.7829mg of Ni

10ml solution contains =5.7829 mg Ni

1000ml solution contains=578.29mg/L

=0.5783g/L

Error Analysis: Error:=0.6-0.5783

=3.61%
 Discussion:
 The most important thing we need to pay attention―
 pH plays a significant character such of pH value is not accurate then the correct result
will be missing. At first step, NH4Cl and NH4OH is added to make the pH value of this
solution up to 7, then Ni-indicator complex formed. After more NH 3 solution was added
for making pH=10, which is needed to form Ni-EDTA complex, otherwise unstable
complex would form, and result would be erroneous.
 Precautions must be taken in washing burette, pipette, conical flask etc with distilled
water and rinse solution.
 During titration, EDTA solution was added dropwise with care because to get the exact
colour change and accurate end point.

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