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EXPERIMENT 5
Chemical Interferences in Atomic Absorption
Spectrophotometric Measurements
Vanessa Olga J. Dagondon and Ken M. Menez
Department of Chemistry, College of Arts and Sciences,
University of the Philippines Visayas, Miag-ao Iloilo
ABSTRACT
Calcium content in prepared samples containing other
species such as K, P, La, EDTA and Al was determined using
AAS or Atomic Absorption Spectroscopy. Four schemes were
adapted in the experiment: (1) absorbance of Ca standards
determined using air/acetylene flame; (2) absorbance of Ca +
K standards determined using air/acetylene flame; (3)
absorbance of Ca standards determined using N2O/acetylene
flame; and (4) absorbance of Ca + K standards determined
using N2O/acetylene flame. Addition of K and P contributes to
the chemical interference due to the incomplete dissociation
of compounds. This can be minimized by using a high
temperature
flame
N2O/acetylene
flame
instead
of
air/acetylene and by adding a releasing agent, La. Addition of
Al can cause another type of chemical interference using
interference due to effects of ionization. This can be
minimized by using a low temperature flame, air/ acetylene
and by adding a protective agent such as EDTA.
INTRODUCTION
Atomic spectroscopy is a series of different qualitative analyses
regarding the concentration of a specific substance in an analyte, with
each analysis applied based on the characteristics of the substance. 1 As
with any atomic spectroscopic method, the identity and concentration of a
substance in a sample solution could be determined by exciting the
molecules of the solution using a source, such as heat or strong light. This
excitation produces neutral atoms in the gas phase, which emit a specific
wavelength and intensity of light that gets captured and analyzed by
detectors.1 These processes are considered very successful in a wide array
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machines.10
This experiment uses the flame atomic
Figure 2. A schematic diagram for the process of
atomic absorption spectroscopy.1
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AND
DISCUSSION
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0.0030
0.0068
0.0779
0.0824
0.1818
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0.0029
0.0070
0.0897
0.0908
0.1367
0.1000
0.0500
0.0000
0 1 2 3 4 5 6
Concentration of Ca + K Standards (mg/L)
0.1500
Absorbance 0.1000
0.0500
0.0000
0 1 2 3 4 5 6
Concentration of Ca Standards (mg/L)
(a)
(b)
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0.1000
Absorbance
0.0500
0.0000
0 1 2 3 4 5 6
6.0000
4.0000
2.0000
0.0000
0 f(x)
1 =2 3 4 5 6
R = 0
Concentration of Ca Standards (mg/L)
(c)
(d)
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CONCLUSION
Atomic Absorption Spectroscopy (AAS) is a technique for measuring
quantities of chemical elements present in a sample by measuring the
absorbed radiation by the chemical element of interest. The sample is
excited by radiation making its atoms absorb ultraviolet or visible light
and make transitions to higher energy levels. In this experiment, flame
atomic spectroscopy is used to excite the analyte using different mixtures
of acetylene flame. The analyte in this experiment is calcium. Calcium
content of 6 samples containing interferences and other components were
determined. To determine the calcium content in the samples, two sets of
calcium standards (Ca standards and Ca+K standards) were prepared to
create calibration curves. The absorbances of the standards were
determined using air/acetylene and N2O/acetylene flames as indicated in
the four schemes followed in the experiment. Four calibration curves were
obtained in the experiment. Effects of interference in the determination of
calcium in the sample were examined. Potassium and phosphorus caused
a chemical interference due to incomplete dissociation of compounds. This
interference can be aided by using a higher temperature flame
(N2O/acetylene flame instead of air/acetylene) and also by adding
Lanthanum which is a releasing agent. Aluminum can cause another type
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1.
2.
3.
4.
5.
6.
7.
8.
LITERATURE CITED
Introduction. Determination of Calcium by Atomic Spectroscopy.
Chem 334: Quantitative Analysis Laboratory, Colorado State
University. March 24, 2016. p. 1 2.
Standard Conditions: Al (Aluminum). Flame Atomic Absorption
Spectrometry: Analytical Methods. Agilent Technologies, Australia.
13th ed. November 2015. p. 16.
Standard Conditions: Ca (Calcium). Flame Atomic Absorption
Spectrometry: Analytical Methods. Agilent Technologies, Australia.
13th ed. November 2015. p. 24.
Standard Conditions: K (Potassium). Flame Atomic Absorption
Spectrometry: Analytical Methods. Agilent Technologies, Australia.
13th ed. November 2015. p. 42.
Standard Conditions: La (Lanthanum). Flame Atomic Absorption
Spectrometry: Analytical Methods. Agilent Technologies, Australia.
13th ed. November 2015. p. 43.
Standard Conditions: P (Phosphorus). Flame Atomic Absorption
Spectrometry: Analytical Methods. Agilent Technologies, Australia.
13th ed. November 2015. p. 54.
Amos, M. D. & Willis, J. B. Choice of Flame. Spectrochimica Acta:
Use of high temperature pre mixed flames in atomic absorption
spectroscopy. Pergamon Press Ltd., Northern Ireland. vol. 22. 1966.
p. 1327.
Martizano, J. Materials & Procedures. Chemical Interferences in
Atomic Absorption Spectrophotometric Measurements. University of
the Philippines Visayas Miagao Campus, Philippines. March 2016.
p. 1.
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APPENDICES
I. Tables
Table 4. Statistical Data for the Schemes 1, 2,3 and 4
Statistical
Parameter
M
B
sr
sm
sb
sc
r
Scheme 1
Scheme 2
Scheme 3
Scheme 4
0.040304054
-0.016868919
2.28x10-2
5.93x10-3
1.66x10-2
6.22x10-1
0.939
0.036798649
-0.01057703
1.96 x10-02
5.10 x10-03
1.43 x10-02
6.42 x10-01
0.036439189
-0.01916622
2.28 x10-02
5.92 x10-03
1.65 x10-02
6.91 x10-01
0.0286
0.0019
2.15 x10-02
5.60 x10-03
1.56 x10-02
8.34 x10-01
0.9454
0.9267
0.8969
x2
y2
xy
0.0005
0.0000002
5
0.0020
0.000004
0.002
0.0778
0.0824
0.1963
25
sum
11
0.3590
39
ave
2.2
0.0718
7.8
0.0060528
4
0.0067897
6
0.0385336
9
0.051380
54
0.010276
10
( x )2
( 11 )2
S xx = x
=39
=14.8
n
5
2
( y )2
( 0.3590 )2
S yy = y
=0.05138054
=0.02560434
n
5
2
( xy )
[ ( 11 ) ( 0.3590 ) ] =0.5965
S xy =xy
=1.3863
n
5
m=
b=
S xy 0.5965
=
=0.040304054
S xx
14.8
y
x 0.3590
11
m
=
( 0.02560434 )
=0.01686892
n
n
5
5
( )
( )
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0.1556
0.2472
0.9815
1.3863
0.27726
(y1mx1+b)2
0.0003016
79
0.0004594
65
0.0001977
06
0.0004684
3
0.0001356
91
0.001562
97
0.000312
59
0.0824+0.01686892
=2.4630 mg/ L
0.040304054
Uncertainty of Measurement
0.040304054
( 2)(14.8)
0.02560434
=2.28 102
52
S yy m2 S xx
=
N2
s r=
sr
(2.28 102 )2
=
=5.93 103
S xx
14.8
s m=
xi
N
1
s b=s r
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y
n
0.040304054
0.3590
0.0824
5
1 1
+ +
1 5
( 2)(14.8)
2.28 102
0.02560434
2
( m S xx |=
1 1
+ +
M N
sr
m
sc =
uncertainty=(2.28 102 )2+(5.93 103 )2+(1.66 102 )2+(6.22 101 )2 =6.22 101
*All calculations for the remaining schemes are done is the same way
shown.
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