The Calorimetric Determination of Manganese in Paper Clips

Aim
The objectives of this experiment is to determine the mass percentage of Manganese in two
paper clips sample by visible spectroscopy, This is achieved by preparing standards solutions
which will be used to plot the calibration curve and later the calibration curve is used to
determine the manganese content in solutions of unknown Mn.

Method
The method outlined in the CEM2007F was followed closely with no alterations.
1. First you prepare the standards solutions of varying concentration such that the total
final solution of 5, 10, 15, 20 and 25 ppm of Mn will results. Note that the same
procedure performed with the standard solutions is followed with the blank and
unknown solutions of Mn we are going to test.
2. Add volumes of 100 ppm Mn as specified in (1) in 5 conical flasks.
3. Add 25 cm
3
of HNO
3
in each flask and include the sixth one with just 25 cm
3
HNO
3

for the blank solution in it.
4. Add two more flasks with paper clips in them, this will be the unknown solutions and
repeat (3).
5. Cover all the 8 flask with class lids and boil them until most of the paper clip has
dissolved
6. Allow cooling after all the paper clip has dissolved
7. Add 0.5 g of ammonium perodisulfate and repeat (5) and (6) except this time you
count time ( 5-15 min)
8. Add 5 cm
3
of concentrated phosphoric acid, 25 cm
3
of water and 0.4 g cm
3
KlO
4
to each flask
and repeat (5 and 6)
9. Now fill the volumetric flask to the mark with this solutions and measure absorbance using
spectrophotometer at the wavelength of 525.3 nm.

Results

Mass of paper clips
Mass1 = 0.3597 g
Mass2 = 0.3210 g

Table 1: Concentration of Mn and Absorbance Measured
Concentration of Mn in
100ml solution (ppm)
Absorbance at 525 nm
5 0.223
10 0.432
15 0.614
20 0.860
25 1.062

Table 2: Absorbance of Sample Measured
Sample 1 0.636 g
Sample 2 0.480 g

Calculations

Graph plot of absorbance vs concentration at the wavelength of 525.3 nm

y = 0.0421x + 0.0064
R = 0.9983
0.000
0.200
0.400
0.600
0.800
1.000
1.200
0 5 10 15 20 25 30
A
b
s
o
r
b
a
n
c
e

Concentration (ppm)
Graph of Absorbance Vs Concentration at the
wavelength of 525.3 nm
From the graph using excel we get the calibration curve equation of the straight line to be
y = 0.0421x + o.oo64
Where: y ~ absorbance
x ~ concentration (ppm)

Calculation of concentration of the samples
Sample1

x1 =

x1 =

= 11.2 ppm = 11.2 mg/l

Mass Mn in sample 1 = 11.2 x 0.1 = 1.12 mg

Sample2

x2 =

x2 =

= 14.96 ppm = 14.96 mg/l = 15 mg/l

Mass of Mn in sample 2 = 15 x 0.1 = 1.5 mg

Mass % of Mn in paper clips
Sample1

Mass1 % = Mass of Mn in sample1/Mass1 = (1.12mg)/(0.3597g) = 0.35%
Mass2% = Mass of Mn in sample1/Mass1 = (1.50mg)/(0.3210g) = 0.42%




Discussion and Conclusion
525.3 nm a Wavelength obtained from absorption spectrum of KMnO
4
was set . Standard
solution was used to zero the spectrophotometer each time a new samples was tested.
Hence a calibration curve was obtained to compare the absorbance of the unknown
solution of Mn. Paper clip we labelled 1 had 0.35% of Mn and paper clip 2 had 0.42% of
Mn.

References
1. Colorimetric Determination of Manganese in Steel." 123HelpMe.com. 30 Mar 2014
<http://www.123HelpMe.com/view.asp?id=148733>.

2. Skoog, D. A, West, D M and Holler, Fundamentals of Analytical Chemistry, 6
th
edition,
Saunders College Publishing, Fort Worth, 1992 chp 20C 2 to 7.