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Analysis of Elements in An Alloy by Colorimetry

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Experiment Analysis of elements in an alloy by colorimetry

Problem definition Mechanical properties of steel depend on its composition. Hence its
analysis is important for its use in industry.

Methodology Colorimetric method using dimethylglyoxime as complexing agent to


form brown-red colored solution for measurement of absorbance at
λmax of 440 nm.

Solution Estimation of percentage of nickel in different steel samples

Student learning Students will learn to perform


outcomes a) Complexometric reaction and estimation by colorimetric
technique
b) Composition of nickel in different grades of steel

Experimental procedure

Principle: Dimethylglyoxime reacts with nickel ions and forms a pink coloured Ni(dmg)2
complex in alkaline medium. Nickel forms a brown-red, water soluble oxidized nickel-
dimethylglyoxime complex with potassium ferricyanide in alkaline medium as shown in the
scheme below. The absorption spectrum of the oxidized complex shows absorption maximum
at a wavelength of 440 nm (Figure 1). After drawing calibration graph the determination of
nickel concentration in a given unknown sample can be done by colorimetry applying Beer-
Lambert law.
OBSERVATION AND CALCULATIONS

A
b
s
o
r
b
a
n
c
e

Wavelength λ (nm)

Figure 1: Absorption spectrum of oxidized Figure 2: Model calibration


Ni(II)-DMG complex showing λmax at 440 nm carve for Ni(II) determination

Table-1: Experimental Data

S. No Concentration (mg/L) Absorbance (Y axis)

(X axis)

1.

2.

3.

4.

5.

6. Unknown
Requirements:

Solutions required
1. Steel sample containing Nickel (II) solution – Prepare a standard nickel(II) solution by
weighing 450 mg of NiSO4.6H2O. Quantitatively transfer the weighed sample to a 100 mL
volumetric flask and dissolve the salt in distilled water. Finally make the volume to 100l mL
with distilled water. This solution contains 1000 mg of Ni per liter (1000 mg/L). For
calibration graph make a working stock solution (100 mg/L) by diluting 1 ml of 1000 mg/L
solution to 100 ml.
2. Potassium Ferricyanide solution – Dissolve 1.5 g of K3Fe(CN)6 in a 100 mL volumetric
flask with distilled water.
3. Dimethylglyoxime in NaOH solution – Take 2.0 g of dimethylglyoxime and 8 g of NaOH
in a 100 mL volumetric flask and dissolve the salts with 25 mL distilled water and make the
volume to 100 mL with distilled water.
4. Sodium Hydroxide solution – Dissolve 40 g of NaOH in 1000 mL of distilled water.
Procedure:
Take 6 standard 100 mL volumetric flasks (including the unknown). To every flask add 1.00
mL of dimethylglyoxime solution by a pipette followed by 1,00 mL of potassium ferricyanide
solution by a burette. Then add 1.00, 2.00, 3.00, 4.00, and 5.00 mL of the steel containing
nickel(II) solution from a burette to the flask. All flasks are shaken well and made up to 100
mL mark with 1N NaOH solution. Allow the flasks at least for 15 minutes after the addition
of all the reagents for the complete complex formation. Then the absorbance of the formed
brown-red solution is measured at 440 nm against the distilled water blank. Record these
absorbance readings in Table-1. Draw a calibration graph taking concentration of nickel (II)
as X-axis and absorbance readings as Y-axis and a straight line that passes through the origin
is obtained as shown in Figure 2. From the molar concentration of nickel solution and cell
path length, calculate the molar absorptivity of the oxidized nickel-dimethylglyoxime
complex at 440 nm. From the calibration plot, measure the concentration of nickel in the
unknown sample.
Result
Concentration of Nickel in the steel sample = ppm (mg/L)
Evaluation of result

Sample Experimental value Actual Percentage of Marks awarded


number Value error

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