SPECTROSCOPY
PART A: Operating Parameters and Calibration Solution Concentrations:
1.
TABLE # 1: Instumental Settings Information:
Instrument
Data format
Absorbance
700.00 nm
400.00 nm
Software
Insight:1.4
Application
Scan- Scan
Band width
1 nm
Integration time
0.100 sec
Data interval
1.00 nm
Baseline correction
100 %T
Scan speed
600.00 nm/min
Derivative order
None
Smooth level
None
Result Type
Peak Pick
Sample ID
PATEL TVISHA
Absorbance
991313983
1.080
2. In order to calculate the actual concentration of Fe2+ in ppm ,first of all we need to find
out the mole of iron(ii)ammonium sulphate hexahydrate (Fe(NH4)2SO4 *6H2O) .
1.7583 grams of iron (ii) ammonium sulphate hexahydrate (Fe(NH4)2SO4 *6H2O) was
weighed and the size of the volumetric flask used for making the stock solution was
2000 ml.
The unknown sample containing iron in well water : FE #60
Hydroxyl amine = 100.1478 g/L
1,10-Phenonthraline = 400.07 g/4L
Molecular weight of Fe 2+ = 55.85 g/mole
Molecular weight of (Fe(NH4)2SO4 *6H2O) = 392.05 g
Actual Concentration in ppm of Fe2+ in the stock solution =
1.7538 g of salt
1 mole of salt
1 mole of Fe 55.85 g of Fe 1000 mg 1000 ml
2000 ml
392.05 g of salt 1 mole of salt 1mole of Fe
1g
1L
= 125.24 ppm of Fe 2+
Therefore,the concentration of Fe2+ stock solution was found to be 125.24 ppm
2+
C1V1 = C2 V2
PATEL TVISHA
991313983
C 1V 1
V2
125.2 ppm10.00 ml
100.00 ml
= 12.52 ppm
Therefore, the concentration of Fe2+ sub stock solution was found to be 12.52 ppm
4. The actual concentration in ppm of Fe2+ in external standard calibration solution based on
the volume of Fe2+ sub stock solution is:
c1 v 1
v2
12.52 ppm1.00 ml
25.00 ml
= 0.5008 ppm
PATEL TVISHA
991313983
125.2ppm
2000ml volumetric
fflask ffflask flask
5.
10
.0
0m
12.52ppm
7.
5.00ml
m
00
111111111
PATEL TVISHA
991313983
1
2
3
4
5
2+
Substock Fe volumes
2+
Calculated Fe
Absorbance at
511.6nm (Max)
pipette(ml)
1.00
3.00
5.00
7.00
10.0
concentration (ppm)
0.500
1.502
2.504
3.506
5.008
0.129
0.340
0.542
0.748
1.081
4.701
4.834
4.947
0.993
1.037
1.052
Unknown#
FE 60
FE 601
FE 602
FE 603
1
2
3
4
5
Substock
pipette(ml)
1.00
3.00
5.00
7.00
10.0
Unknown#
FE 60
FE 601
FE 602
FE 603
PATEL TVISHA
2+
fe
volumes
Calculated
2+
Fe
Absorbance at
570nm (Min)
concentration (ppm)
0.500
1.502
2.504
3.506
5.008
0.014
0.043
0.051
0.073
0.103
4.701
4.834
4.947
0.098
0.099
0.102
991313983
Regression equation
(511.6 nm)
0.021 + (0.210)C
Regression equation
(570 nm)
0.007 + (0.019)C
1.000
0.982
8.
Calculating the unknown concentration of Fe2+ (ppm) for 511 nm wavelength :
Absorbance = 0.021 + (0.210)C
0.993 = 0.021 + (0.210)C
0.993 0.021 = (0.210)C
So, C =
0.972
0.210
= 4.628 ppm
TABLE # 6: Concentration of Fe2+ in unknown sample: (511.6 nm)
Serial #
Calculated
concentration in ppm
Absorbance at
511.6nm
1
2
3
4.628
4.838
4.909
0.993
1.037
1.052
PATEL TVISHA
Final
concentration in
ppm
57.85
60.47
61.36
991313983
Calculated
concentration in ppm
Absorbance at 570
nm
1
2
3
4.789
4.842
5.000
0.098
0.099
0.102
Final
concentration in
ppm
59.86
60.52
62.50
9.
In order to calculate the final concentration of Fe2+ in original sample of well water, we
have to do the back calculation.(for 511.6 nm)
Final concentration of Fe2+ =
25 ml
4.628 ppm
2ml
= 57.85 ppm
10.
(i)
Qexp
gap
= range
60.4757.85
61.3657.85
= 0.746
Qexp <Qtable
PATEL TVISHA
991313983
= 59.89 ppm
(iii)
standard deviation=
( x x )
n1
Where,
N=number of values
x=an individual value
x = mean or average of the value
(x- x )2 =sum of the square of the difference from the mean for all values.
{6.657 }
2
1.824
PATEL TVISHA
991313983
= x m
95
= 59.89
t XS
N
4.303 X 1.824
2
= 59.89 5.550
95
95
Standard deviation
1.824 %
True value at
95%confidence
interval
65.44 (by addition)
54.34 (by
subtraction)
Qexp
0.746
Standard deviation
1.373 %
True value at
95%confidence
interval
65.13 (by addition)
56.78 (by
subtraction)
Qexp
0.250
11.
PATEL TVISHA
991313983
Relative error =
value
100
|absolute
true value |
|59.8964.60
|100
64.60
= 7.29 %
A
bc
Where,
A =absorption of a complex at 511.6 nm( maximum wavelength )
a =absorption coefficient
b =cuvette width(1cm)
c =concentration of the external used in mg/L
PATEL TVISHA
10
991313983
1.081
1 5.008
0.215 L/cm*mg
Concentration in
ppm
0.500
1.502
2.504
3.505
5.008
Absorbance
(511.6 nm)
0.129
0.340
0.542
0.748
1.081
Absorptivity
coefficient L/cm*mg
0.025
0.067
0.108
0.149
0.215
14.
TABLE # 11: For Absorptivity Coefficient and the corresponding Slope:
Absorptivity coefficient
0.215
Absorptivity coefficient
0.020
PART D: Discussion:
15.
I think the reason behind this is, as the wavelength increase, the absorbance of the
compound is being affected because it is known that the wavelength depends on the
presence of the light absorbing groups in the compound. Hence some compounds have
maximum absorption while some of them have minimum absorption depending upon the
capacity of the passage of the light through it. Even the solutions have different spectral
sensitivity at different wavelengths. Thus, affects the absorbance value.
PATEL TVISHA
11
991313983
18.
In order to minimize the relative error one should recommend doing more accurate
dilution, in this experiment dilution is crucial because even a point difference can affect
the concentration of the solution.
Second recommendation to minimize the error is by accurate pipetting of each solution
and by proper calibration of instrument used in experiment.
19.
TABLE #12 : Absoptivity coefficient and Slope value
Wavelength(nm)
PATEL TVISHA
Absorptivity coefficient
12
Slope value
991313983
0.210 L/cm* mg
0.020 L/cm* mg
0.210
0.019
20.
At 511.6 nm, Green colour is absorbed by Fe2+ 1,10- phenanthroline complex and
Yellowish green at 570 nm .Green colour is transmitted at 511.6 nm and Yellowish green
at 570nm by human eye.
REFERNCE:
Tyrer N., Rankin K., Chem 25415 Instrumental Analysis Laboratory Manual, Sheridan
College, Brampton, ON, fall 2013. Page no. 4.1-4.12
PATEL TVISHA
13
991313983