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Jan 9, 2024
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Fe: Spectrophotometric Determination of Iron
Date submitted: 2022
By:
Lab section:
TA:
Procedure:
1.
25.00 ml of a concentrated standard solution that contained 0.2500 g/L of iron were pipetted
into a 500.00 ml volumetric flask. The solution was diluted up to the mark with distilled water
and was mixed well as it was filled.
2.
Six calibration standards of the diluted standard iron solution were prepared, containing 0.05
mg, 0.10 mg, 0.15 mg, 0.20 mg, 0.25 mg of iron.
3.
10.00 ml of an unknown iron sample was pipetted into a 250.00 ml volumetric flask and was
diluted to the mark with distilled water while being mixed.
4.
Two 25.00 ml aliquots of this were pipetted into two different 50.00 ml volumetric flasks.
5.
4.0 ml 10% hydrixykamine hydrochloride and 4.0 ml 0.3% ortho-phenanthroline were pipetted
into each of the eight 50 ml volumetric flasks.
6.
Each flask was diluted to the mark with distilled water after 10 minutes had passed.
7.
The wavelength on the spectrophotometer was set to the value chosen.
8.
2/3 of a cuvette was filled with the blank solution and was zeroed in the spectrophotometer.
9.
The cuvette was rinsed with the most dilute solution after emptying the blank solution from it.
The absorbance was measured after the cuvette was filled to 2/3 with this solution.
10.
After the solution was emptied, the same process was repeated and the absorbance of each
solution was measured, in order of increasing levels of concentration.
11.
The cuvette was rinsed with distilled water and subsequently rinsed with a small amount of the
first unknown solution. The absorption of the first unknown was measured before the cuvette
was rinsed with a small amount of the second unknown solution. The cuvette was then filled and
the absorption of the second unknown was measured.
Data and Observations:
Concentration (mg/50mL)
Absorbance
0
0.000
0.05
0.201
0.10
0.389
0.15
0.587
0.20
0.787
0.25
1.023
Unknown trial 1
0.674
Unknown trial 2
0.677
0
0.05
0.1
0.15
0.2
0.25
0.3
0
0.2
0.4
0.6
0.8
1
1.2
f(x) = 4.04 x − 0.01
R² = 1
Iron: Spectrophotometric
Concentration (Fe/50ml)
Absorption
Figure 1:
Plot of Absorbance vs. Concentration of the standard iron solutions
Calculations and Discussion:
Calculating the concentration of the first unknown sample (in mg/50mL)
y
=
4.0406
x
−
0.0072
0.674
=
4.40406
x
−
0.0072
x
=
0.15468
mg
50
mL
Converting the concentration to mg/mL
C
1
=
x
50
C
1
=
0.15468
50
C
1
=
0.0030281
mg
mL
Calculating the average concentration of the two unknown samples
C
av
=
C
1
+
C
2
2
C
av
=
0.0030281
+
0.0030417
2
C
av
=
0.0030349
mg
mL
Calculating the dilution factor
d
=
(
v
f
1
v
i
1
)(
v
f
2
v
i
2
)
d
=
(
250
10
)(
50
25
)
d
=
50
x
Calculating the concentration of iron in the undiluted unknown sample
C
ud
=
d
∗
C
1
∗
g
1000
mg
∗
1000
mL
L
C
ud
=
50
∗
0.0030281
mg
mL
∗
g
1000
mg
∗
1000
mL
L
C
ud
=
0.15141
g
L
Calculating the error of our value
Error
=
experimental
−
actual
actual
×
100%
Error
=
|
0.15141
−
0.1735
|
0.1735
×
100%
Error
=
12.732%
Calculating the precision
p
=
(
high
−
low
average
)
∗
1000
ppt
p
=
(
0.15468
−
0.15141
0.15304
)
∗
1000
ppt
p
=
21.367
ppt
Extinction Coefficient
ϵ
=
11282
Conclusion:
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In this laboratory experiment, the concentration of iron from the unknown sample was calculated to be
0.15141 mg/mL, the actual value being 0.1735 producing an error of 12.732%. The relative spread was
21.367ppt. The extinction coefficient was calculated to be 11282 mol*cm.
References:
Archer, D.W., Burk, R.C., White, C.A., Wolff, P.A., Levac, S., Mesnic, N., Hunt, V., CHEM 1101 Chemistry
for Engineers Lab Manual, Carleton University, 2021-2022
.
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