Supervisor: Saleh Suleiman

Chem426
Name: Lina abukwik
ID number:1171067

Spectrophotometric Determination of Manganese in Steel

Abstract:
The overall objective of this experiment is to determine the percentage of
manganese in a steel sample, using colorimetric methods of analysis.

The mass percentage of the Mn2 + in the steel sample = 0.37%

The molar absorptivity ε of the KMnO4 solution =134,241. 𝑐𝑚−1𝑚𝑜𝑙−1
The concentration of Mn2 + in the unknown sample code A =2.0058*10-4 M
The maximum wave length of the absorbance = 525 nm

Introduction:
The aim of this experiment was to determine the percentage of Mn²⁺
presented in an unknown steel sample by spectrophotometric analysis.
It is crucial to know this because within an known steel sample, it is usually
composed of a variety elements which include cooper, manganese, and
silicon. These elements provide different physical and chemical properties
for steel which makes it an alloy.
Furthermore, due to steel not containing enough manganese, it would have
to be oxidized in this experiment in order for it to form as a permanganate
ion. This permanganate ion would then cause a physical reaction with the
steel mixture that induces a purple color change. Due to this, the
permanganate solution creates an absorption of light that allows it to be
visible on a spectrum. This visible spectrum can be measured through the
use of spectroscopy as it would create an absorbance value based off of the
visible range of the electromagnetic spectrum.
permanganate solution of the standard steel sample was then placed
under four series of dilutions and placed into a spectrophotometer to get
the absorbance and concentration of manganese. Once placed into the
spectrophotometer, amonochromatic light source would pass through the
solution as it would measure the amount of absorbance present in the
solution and would be read by a light detector. This light detector is
important to creating a Beer’s law plot as it takes into account the
concentration of the solution and absorbance value.
In addition to the permanganate ion undergoing spectroscopy, the
following reaction is used to successfully oxidize manganese and to remove
any chemical properties that would have prevented the formation of the
permanganate ion.
2Mn²⁺₍aq₎+ 5IO⁴⁻₍aq₎+ 3H₂O₍i₎→ 2MnO⁴⁻₍aq₎+ SIO³⁻₍aq₎+ 6H⁺₍aq₎
The wavelength of any sample is then determined by an analysis based on
the highest peak in the spectrophotometer. Once that wavelength is
established, the absorbance versus concentration plot can be created and
the molar absorptivity can then be determined. This molar absorption is
found based off of Beer’s law and is used to determine the concentration of
manganese in an unknown sample.
Methodology:
Prepare a standard solution of KMnO4:
0.079 g of KMnO4 was dissolved in 250 mL volumetric flask, the solution
was heated until KMnO4 crystals was dissolved then it was cooled and 2ml
of concentrated sulfuric acid was added, the solution one was pipetted 25
ml from above solution then was diluted to 100 ml.
Preparation of calibration curve:

A) 25 mL of aliquots from the stock KMnO4 was transferred to 100

mL volumetric flasks then was diluted to the mark. This step was
repeated three times; each step was pipetted from the previous
step.
B) The wavelength range was scanned between 400 and 700 nm and
ƛmax was determined by the solution prepared in step a, the blank
cell was filled with deionized water.

 Prepare unknown solution:

1) 1.47 g of unknown steel was placed in 400mL beaker, 50mL of

dilute nitric acid was added then was heated in a hood
2) 1 g of ammonium persulfate was added to beaker then was
boiled for 15 minutes

each solution was Diluted to about 100 ml, 15 ml of 85% phosphoric acid
and 0.5g of potassium periodate was added. then was boiled for 3 minutes
to oxidize the manganese (II) to permanganate. then it was cooled, then 0.2
g portion of potassium periodate was added. then was boiled for 2 minutes
the solution was Transferred to 500-ml volumetric flask and diluted to
volume.
Result and dissection:

By using beer’s law and spectrophotometric determination, the

unknown manganese percent of A was determined to be 0.37%
and the concentration of Mn²⁺ to be 2.0058*10⁻⁴ M.
As expected of beer’s law plot, the relationship between the
absorbance and concentration was proven to be linearly related
and strong. The R² was determined to be 0.9999 which was close
to 1, this indicated that the standard error of regression was
minimum and the values reflected the data. The maximum
wavelength obtained from the samples was at a absorbance
reading of 525 nm. Although the R² value reflected a precise and
accurate result, there could have potentially been present
standard errors within the data that may have skewed the results.
For example, there could have been experimental errors where
there could have been smudged fingerprints on the cuvette which
could of potentially altered the absorbance readings of the
samples. Or there could have been bubbles left in the cuvette that
potentially could have altered the absorbance readings.
Furthermore, potential human errors could have resulted in
incorrect data, such as incorrectly calculating the concentrations
within the dilution part of the experiment. Overall, this
experiment required time and careful meticulous observation in
order to get an accurate result.
Results:

Column
Solution Number Concentration of Mn2+ ions (M) Absorbance
1 0.0005 1.22160
2 0.000125 0.29691
3 0.00003125 6.9898E-02
4 0.00000781 1.7372E-02
Unknown (A) 2.0061E-04 0.48910
Table 1: Absorbance values vs Concentration of manganese:

Absorbance vs Concentration
1.4
1.2
f(x) = 2438.41 x
1 R² = 1
Absorbance

0.8 Abs.
0.6 Linear (Abs.)
0.4
0.2
0
0 0 0 0 0 0 0
Concentration (M)

Figure 1: Calibration plot of absorption vs. Concentration of manganese(PPm):

Mass of KMnO4 = 0.0791 g

Volume of KMnO4 solution = 250 ml = 0.25L
Mass of unknown sample = 1.47g
from Beer’s law A= εbc
c = 0.5 mg/L b=1
= 0.5𝑋 10−3𝑔/𝐿\ 54.938 𝑔/ 𝑚𝑜𝑙 = 9.1*10-6 mol\L
so ε = 1.22160 /((9.1*10-6)(1)) = 134,241. 𝑐𝑚−1𝑚𝑜𝑙−1
From figure 1 : Y = 2438.4x
X mean concentration and y the absorbance of unknown
So 0.48910=2438.4x
then X = 2.0058*10-4 M
Mass of manganese = mole* molar mass of manganese
Mole= concentration * volume.
= 2.0058*10-4 * 0.5 = 1.0029*10-4 mole
So mass of manganese = 1.0029*10-4 *54.9380
=5.5097*10-3 g

For the dilution series:

(M1 V1 =M2V2)

% mass = mass of Mn+2/ total mass *100%

Molecular weight of MnO4 = 118.936 g\mol

Mass of unknown = moles * m.mass

= 5.39*10-3 * 0.5* 118.936 = 0.32 g

% mass = mass of Mn / total mass *100%

(5.5097*10-3\ 1.47)*100% = 0.37%

Conclusion:
we determined The percentage of manganese in a steel sample by
spectrophotometric method where found as 0.37% which is the aim of this
experiment, and the molar absorptivity ε of the KMnO4 solution of the
result was 134,241. 𝑐𝑚−1𝑚𝑜𝑙−1
and the concentration of Mn2+ in the unknown sample has been calculated
as 2.0058*10-4 M and the maximum wave length of the absorbance was
found to be 525 nm

References:

Harris, D.C,; Lucy C. A., Quantitative Chemical Analysis, 8th ed.; New
York, 2016; pp. 393-422

Harris, D.C,; Lucy C. A., Quantitative Chemical Analysis, 9th ed.; New
York, 2016; pp. 432-440
 Appendix:
Beer’s law A= εbc
Mass of manganese = mole* molar mass of manganese
Mole= concentration * volume.
For the dilution series:
(M1 V1 =M2V2)
% mass = mass of Mn+2/ total mass *100%

Figure 1- the absorption value of visible light

Chemical Symbol Mass (g/mol)

Nitric acid (5N) HNO3 63.01 g/mol

Manganese Mn 54.93 g/mol

Sodium Sulfite Na2SO3 126.04 g/mol

Sulfurous acid H2SO3 82.07 g/mol

Potassium Periodate KIO4 230.00 g/mol

Phosphoric Acid H3PO4 97.99 g/mol