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CM123L ANALYTICAL CHEMISTRY LABORATORY

4th Term SY 2018-2019

Determination of Metal from Various Samples Using Atomic Absorption Spectroscopy


(Experiment 14)
Santos, Nanette D.1, Jalmasco, Caleb D.2

1Teacher, School of Chemical, Biological, and Materials Engineering and Sciences, Mapúa University; 2Student, CM123L/B9, School of Chemical, Biological, and Materials
Engineering and Sciences, Mapúa University, cdjalmasco@mymail.mapua.edu.ph

ABSTRACT

Heavy metals may be present in water, wastewater, and even soil. Most metals present in these are in its dissolved state and
are conveniently determined through atomic absorption spectrophotometry. For this experiment, the experimenters
determined the concentration and percent amount of chromium in a water and soil sample through the application of atomic
absorption spectroscopy. To be specific, a flame atomic absorption spectroscopy was used for the experiment. The
experiment was divided into two parts, determination of Cr content from a water sample from Pampanga river, and
determination of Cr content from a soil sample from Mapua University. Each part was done in three methods, i.e. external
calibration method, standard addition method, and internal standards method. The chromium content of the water sample from
Pampanga river through external calibration technique is -5.4444 ppm. The chromium content of the sample through the
standard addition method is 4.3611 ppm. The chromium content of the sample through the internal standards method is 0.4
ppm. This suggests that Fe is more prevalent than Cr in the Pampanga river. The chromium content of the soil sample from
Mapua University through external calibration technique is 14.4433 ppm. The chromium content of the sample through the
standard addition method is 4.3611 ppm. The chromium content of the sample through the internal standards method is 2 ppm.
This also suggests that iron is more prevalent than chromium in the soils of Mapua. Overall the experiment was a success for
the set experiment objectives were met.

Keywords: external calibration, standard addition, internal standards, chromium, atomic absorption spectroscopy

INTRODUCTION
The presence of heavy metals in ecosystem, such as the metals are mercury (Hg), cadmium (Cd), arsenic (As),
aquaculture and land diversity, has far-reaching chromium (Cr), thallium (Tl), and lead (Pb).
implications directly to the biota and indirectly to man. Atomic Absorption Spectroscopy
They also cause irregularity in blood composition, badly Heavy metals may be present in water, wastewater, and
effect vital organs such as kidneys and liver. Heavy metals even soil. Most metals present in these are in its dissolved
including both essential and nonessential elements have a state and are conveniently determined through atomic
particular significance in ecotoxicology, since they are absorption spectrophotometry. Tsade (2016) defines it as
highly. (Tsade, 2016) With this, a need for the an analytical technique that measures the concentration of
determination of heavy metals in water and soil is a must. an element in a qualitative and quantitative manner. This
Determination of the concentrations of trace heavy approach is more beneficial in determining heavy metals as
elements in environmental samples is difficult and the it is low in cost but short in analysis time. In atomic
results obtained often vary according to the chosen absorption analysis, the element being determined must be
analytical technique. (Mohamed et al. 2012) reduced to its elemental state, vaporized, and imposed in
Heavy Metal the beam of radiation from the light source. Commonly,
A heavy metal is a member of a loosely defined subset of solutions from the sample are drawn out as fine mist into
elements that exhibit metallic properties. It mainly includes flame. This is then called a flame atomic absorption
the transition metals, some metalloids, lathanides and spectroscopy. It is simple, rapid, accurate, and highly
actinides. Heavy metals are metallic chemical element that specific form of atomic absorption analysis
are considered as toxins even at low concentration. Heavy In atomic absorption spectroscopy, there is a need to
metals are naturally a component in the Earth’s crust and it convert analytes into free gaseous atoms. This process is
can’t be degraded or destroyed. That is why there is an called atomization, and it may be achieved through flame
imminent need to develop ways to address the increasing atomization and electrothermal atomization. Flame
concentrations of heavy metals in the primary sources of atomization was used for the experiment. The more time an
livelihood. (Srikanth et al., 2013) Examples of heavy analyte spends in the flame, the greater the atomization
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CM123L ANALYTICAL CHEMISTRY LABORATORY
4th Term SY 2018-2019

efficiency is because the production of atoms increases in was used to cover the beaker. The mixture was reduced to at
height. For example, the comparison between chromium, least 50 mL, ensuring that the sample didn’t boiled in the
an easily oxidized heavy metal, and silver, a difficult one. process. Add 10 mL of conc. HNO3 until the sample became
For Cr, the concentration of free atoms is greatest just clear or light-colored. Once done, measure the pH of the
above the burner head; while for Ag, the concentration of water sample. And then transfer to a 250-mL volumetric flask.
free atoms increases steadily with height. Dilute to mark. Prepare duplicate.
For this experiment, the objectives set were as follows. II. Soil sample
The experimenters must gain a basic understanding to the Secure a soil sample. It was then dried inside an oven for at
principle and instrumentation of atomic absorption least 45 minutes or until the water has completely evaporated
spectroscopy or AAS. At the end, the amount of metal from the sample. Place inside a desiccator for cooling down.
present in the samples must be quantitatively determined After, weigh out 2.0 g of the sample and place it in a 250-mL
through AAS. The experimenters must also be introduced beaker. Add 18 mL of concentrated HNO3 and place in a hot
to different digestion procedures for solid and liquid plate. Cover the beaker with a watch glass. Heat the solution
samples. Lastly, for the experimenters to be able to to up to 30 minutes. After, cool it down and add 10 mL of
compare the resulted concentration of metal from various double-distilled water. Filter it using the filter paper and
methods of analysis. measure the pH once finished. Transfer the solution to a 250-
mL volumetric flask and dilute to mark. Prepare duplicate.
Three different methods of analysis were used for the
determination of chromium from soil and water sample. Preparation of the Standards
The three methods were external calibration method, I. External Calibration Method
standard addition method, and internal standards method. Find the assigned mother liquor. Weigh 0.0025 g or 25 mg of
the mother liquor in a beaker (10 ppm). Dissolve it with
MATERIALS AND METHODS double-distilled water. Transfer it to a 250-mL volumetric flask
and dilute to mark. Prepare five 50-mL volumetric flasks.
Reagents Transfer 1.25 mL (0.25 ppm), 2.5 mL (0.5 ppm), 6.35 mL
(1.25 ppm), 12.5 mL (2.5 ppm), and 25 mL (5 ppm) of the
Concentrated HNO3, concentrated HCl, Cr(NO3)3, Fe(NO3)3, stock solution. Adjust the pH of the solution to the pH of the
Pb(NO3)2, Cu(NO3)2, Zn(NO3)2, KCl, double-distilled water, sample through adding concentrated HCl. Once the pH levels
soil sample, water sample of the solution and the sample are the same, dilute it to mark.
Secure samples in a test tube and label properly.
Apparatus
II. Standard Addition Method
Hot plate, beakers, watch glass, stirring rod, Erlenmeyer From the prepared standard solutions, choose one
flasks, glass funnel, graduated pipettes (1 mL,10 mL & 25 concentration to be used in the standard addition method.
mL), volumetric pipettes (1 mL, 10 mL, & 25 mL), 100-mL Prepare six 50-mL volumetric flasks and transfer portions
volumetric flasks, 50-mL volumetric flasks, 25-mL according to table 1.
volumetric flasks, test tube, test tube rack, Whatman #40
filter paper, graduated cylinder, cathode lamps, acetylene Volume of Volume of Total
gas Analyte Sample, mL Volume,
Standard, mL mL
For the methodology of this experiment, it was divided into 0.00 5.0 50
three parts; digestion of sample, preparation of standards, 2.0 5.0 50
and the measurement of absorbance. The preparation of 4.0 5.0 50
the standards was done in three methods namely the 6.0 5.0 50
external calibration method, standard addition method, and 8.0 5.0 50
internal standards method. 10.0 5.0 50
Table 1. Standard Addition Method
Digestion of the Sample
I. Water sample Once added, dilute to mark. Transfer amounts to test tubes
Secure a water sample. Using a filter paper, 200 mL of the and label it. Construct then the standard addition curve and
water sample was filtered and as then transferred to a 400- use it for the determination of the metal.
mL beaker. 10 mL of a concentrated HNO3 was added
before the beaker was placed in a hot plate. A watch glass
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III. Internal Standards Method Conc. in Absorbance Average


Prepare 250 mL of 1.25 ppm of the internal standard Calib. Absorba
solution (Fe for Cr and Pb for Cu, vice versa). Prepare five Units, nce
25-mL volumetric flasks. Transfer the following (table 2) with mg/L
corresponding portions to each flask Trial 1 Trial 2 Trial 3
Conc. of Volume of Volume of Volume 0.25 -0.0004 0.0004 0.0000 0
External External Internal of 0.5 -0.0004 0.0009 0.0001 0.00020
Standard, Standard, Standard, Sample, 1.25 0.0025 0.0009 0.0005 0.00130
ppm mL mL mL 2.5 0.0002 0.0015 0.0006 0.00077
0.25 5.0 5.0 5.0 5.0 0.0021 0.0026 0.0006 0.00177
0.50 5.0 5.0 5.0 Table 4. External Calibration Method
1.25 5.0 5.0 5.0
2.5 5.0 5.0 5.0 Figure 1 then shows the graphical representation between
5.0 5.0 5.0 5.0 the concentration and absorbance. The slope is positively
Table 2. Internal Standards Method skewed implying a direct proportionality relationship between
the two.
Dilute to mark and transfer to separate test tubes.
Determine the absorbance of each solution and get the
ratio of absorbance of analyte vs. absorbance of internal
standard. Plot the internal calibration curve and use it for
the determination of the metal.

Measurement of Absorbance

Set up the instrument. Determine the absorbance per


solution and record it. Use it for the determination of the
concentration of metal in the sample.
Figure 1. Absorbance vs Concentration – External
Standards
RESULTS AND DISCUSSION
The equation of the line is:
The water sample was retrieved from the Pampanga river.
y = 0.0003x + 0.0002
The soil sample was retrieved from the gardens of Mapua
The coefficient R is:
University. The mother liquor assigned is Cr(NO3)3 and its
internal standard is Fe. The group was assigned for the R2 = 0.7044
determination of chromium from the soil and water sample.
The table below shows the absorbance reading of the To get the concentration of chromium using the external
samples in three methods through the use of flame atomic calibration method, the slope of the equation is used:
absorption spectroscopy.
𝑘𝐴 𝐶𝐴 𝑉𝑜 𝑘𝐴 𝐶𝑠𝑡𝑑
y = mx + b or 𝑆𝑠𝑝𝑖𝑘𝑒 (𝑦) = + × 𝑉𝑠𝑡𝑑
𝑉𝑓 𝑉𝑓
Water sample
Substituting the absorbance reading (y) to the regression line
Table 3 shows the absorbance of the digested water
gives out
sample. Table 4 shows the absorbance of the standards
−0.001433 − 0.0002
with various concentrations from 0.25 ppm to 5.0 ppm. 𝑥=
The pH of level of the solution for both tables is 1. 0.0003

x = -5.4433 mg/L or ppm


Water Absorbance Average
Sample Absorba
nce Using the external calibration method in finding the
concentration of chromium, the experimenters were able to get
Trial 1 Trial 2 Trial 3
A -0.0031 -0.0006 -0.0006 -0.001433
-5.4433 ppm of chromium.
B -0.0035 -0.0004 0.0004 -0.001433
Table 3. Absorbance of Digested Water Sample
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CM123L ANALYTICAL CHEMISTRY LABORATORY
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−5.4433 𝑝𝑝𝑚 Substituting the values of absorbance (y) into the equation, the
= −𝟎. 𝟎𝟎𝟎𝟓𝟒𝟒 % 𝑪𝒓 concentration of Cr is determined.
10,000
For 0 mL:
For the standard addition method, three trials were
conducted. Trial 1 used a concentration of 1.25 ppm. Trial 2 −0.0013 + 0.0013
𝑥=
used a concentration of 5 ppm. Trial 3 used a concentration of −6𝐸 − 05
0.25 ppm. Table 5 shows the absorbance per volume of
analyte for every trial, and the average absorbance. x = 0 mg/L or ppm

Volume Absorbance Average For 2 mL:


of Absorban
Analyte ce −0.00137 + 0.0013
Standard, 𝑥=
mL −6𝐸 − 05
Trial 1 Trial 2 Trial 3
x = 1.1667 mg/L or ppm
0 -0.0023 -0.0004 -0.0012 -0.0013
2.0 -0.0026 -0.0004 -0.0011 -0.00137
4.0 -0.0026 -0.0006
For 4 mL:
-0.0013 -0.0015
6.0 -0.0028 -0.0006 -0.0015 -0.00163
8.0 -0.0027 -0.0011 -0.0013 -0.0017
x = 3.3333 mg/L or ppm
10.0 -0.0032 -0.0010 -0.0014 -0.00187
Table 5. Standard Addition Method - Water For 6 mL:

Figure 2 then shows the graphical representation between x = 5.5 mg/L or ppm
the volume of the standard with fixed concentration and
absorbance. The slope is negatively skewed. It implies that For 8 mL:
with the increase of volume, absorbance decreases.
x = 6.6667 mg/L or ppm

For 10 mL:

x = 9.5 mg/L or ppm

Mean (x̅)

0+1.1667+3.3333+5.5+6.6667+9.5
x̅ =
6
̅ = 𝟒. 𝟑𝟔𝟏𝟏 𝒑𝒑𝒎
𝐱

Standard Deviation (s)


Figure 2. Absorbance vs Volume - Water

The equation of the line is: (x̅ − 𝑥1 )2 + (x̅ − 𝑥2 )2 + (x̅ − 𝑥3 )2


y = -6E-05 [Cr] – 0.0013 𝑠= √
𝑛−1
While the coefficient R is:
R2 = 0.988
To get the concentration of chromium using the standard s = 3.2481
addition method, the slope of the equation is used:
Using the standard addition method in finding the
𝑘𝐴 𝐶𝐴 𝑉𝑜 𝑘 𝐶 concentration of chromium, the experimenters were able to get
y = mx + b or 𝑆𝑠𝑝𝑖𝑘𝑒 (𝑦) = + 𝐴 𝑠𝑡𝑑 × 𝑉𝑠𝑡𝑑 4.3611 ppm of chromium.
𝑉𝑓 𝑉𝑓

4.3611 𝑝𝑝𝑚
= 𝟎. 𝟎𝟎𝟎𝟒𝟑𝟔 % 𝑪𝒓
10,000
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CM123L ANALYTICAL CHEMISTRY LABORATORY
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For the internal standards method, three trials were also For 0.5 ppm:
conducted. Table 6 shows the absorbance per concentration
of the sample and its average absorbance. −0.0016 + 0.0015
𝑥=
2𝐸 − 05
Conc. in Absorbance Average
Calib. Absorba x = -5 mg/L or ppm
Units, nce
mg/L For 1.25 ppm:
Trial 1 Trial 2 Trial 3
0.25 -0.0013 -0.0013 -0.0016 -0.0014 x = -1.5 mg/L or ppm
0.5 -0.0015 -0.0015 -0.0018 -0.0016
1.25 -0.0016 -0.0016 -0.0014 -0.00153 For 2.5 ppm:
2.5 -0.0016 -0.0016 -0.0014 -0.00153
5.0 -0.0014 -0.0014 -0.0014 -0.0014 x = -1.5 mg/L or ppm
Table 6. Internal Standards Method - Water
For 5 ppm:
Figure 3 then shows the graphical representation between
the concentration of the standard and absorbance. The
x = 5 mg/L or ppm
slope is positively skewed. It implies that with the increase
of concentration, absorbance also increases.
Mean (x̅)

5+−5+−1.5+−1.5+5
x̅ =
5
̅ = 𝟎. 𝟒 𝒑𝒑𝒎
𝐱

Standard Deviation (s)

(x̅ − 𝑥1 )2 + (x̅ − 𝑥2 )2 + (x̅ − 𝑥3 )2


𝑠= √
𝑛−1

s = 3.967
Figure 3. Absorbance vs Concentration - Water
Using the internal standards method in finding the
The equation of the line is: concentration of chromium, the experimenters were able to
y = 2E-05x – 0.0015 get 0.4 ppm of chromium.
The coefficient R is:
R2 = 0.173 0.4 𝑝𝑝𝑚
To get the concentration of chromium using the internal = 𝟎. 𝟎𝟎𝟎𝟎𝟒 % 𝑪𝒓
10,000
standard method, the slope of the equation is used:
The chromium content of the water sample from Pampanga
𝑘𝐴 𝐶𝐴 𝑉𝑜 𝑘𝐴 𝐶𝑠𝑡𝑑
y = mx + b or 𝑆𝑠𝑝𝑖𝑘𝑒 (𝑦) = + × 𝑉𝑠𝑡𝑑 river through external calibration technique is -5.4444 ppm.
𝑉𝑓 𝑉𝑓
The chromium content of the sample through the standard
addition method is 4.3611 ppm. The chromium content of the
Substituting the values of absorbance (y) into the equation, sample through the internal standards method is 0.4 ppm.
the concentration of Cr is determined.
For 0.25 ppm: Soil sample
−0.0014 + 0.0015 Table 7 shows the absorbance of the digested soil sample.
𝑥=
2𝐸 − 05 Table 4 shows the absorbance of the standards with
various concentrations from 0.25 ppm to 5.0 ppm. The pH
x = 5 mg/L or ppm of level of the solution for both tables is 1.
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Soil Absorbance Average


Sample Absorba x = 14.4433 mg/L or ppm
nce
Trial 1 Trial 2 Trial 3 Using the external calibration method in finding the
A 0.0123 0.0007 0.0006 0.004533 concentration of chromium, the experimenters were able to
B -0.0014 0.1028 0.1023 0.0679 get 14.4433 ppm of chromium.
Table 7. Absorbance of Digested Soil Sample
14. 4433 𝑝𝑝𝑚
Conc. in Absorbance Average = −𝟎. 𝟎𝟎𝟏𝟒𝟒𝟑 % 𝑪𝒓
10,000
Calib. Absorba
Units, nce
mg/L
For the standard addition method, three trials were conducted.
Trial 1 Trial 2 Trial 3 Trial 1 used a concentration of 0.5 ppm. Trial 2 used a
0.25 -0.0004 0.0004 0.0000 0
concentration of 5 ppm. Trial 3 used a concentration of 0.25
0.5 -0.0004 0.0009 0.0001 0.00020
ppm. Table 8 shows the absorbance per volume of analyte for
1.25 0.0025 0.0009 0.0005 0.00130
every trial, and the average absorbance.
2.5 0.0002 0.0015 0.0006 0.00077
5.0 0.0021 0.0026 0.0006 0.00177
Volume Absorbance Average
Table 4. External Calibration Method of Absorban
Analyte ce
Figure 1 then shows the graphical representation between Standard,
the concentration and absorbance. The slope is positively mL
skewed implying a direct proportionality relationship Trial 1 Trial 2 Trial 3
between the two. 0 -0.0001 -0.0006 -0.0007 -0.00047
2.0 -0.0009 -0.0004 -0.0002 -0.0005
4.0 -0.0012 -0.0006 -0.0006 -0.0008
6.0 -0.0013 -0.0006 -0.0008 -0.0009
8.0 -0.0015 -0.0003 -0.0008 -0.00087
10.0 -0.0017 -0.0008 -0.0008 -0.0011
Table 8. Standard Addition Method - Soil

Figure 4 then shows the graphical representation between


the volume of the standard with fixed concentration and
absorbance. The slope is negatively skewed. It implies that
with the increase of volume, absorbance decreases.
Figure 1. Absorbance vs Concentration – External
Standards

The equation of the line is:


y = 0.0003x + 0.0002
The coefficient R is:
R2 = 0.7044

To get the concentration of chromium using the external


calibration method, the slope of the equation is used:

𝑘𝐴 𝐶𝐴 𝑉𝑜 𝑘𝐴 𝐶𝑠𝑡𝑑
y = mx + b or 𝑆𝑠𝑝𝑖𝑘𝑒 (𝑦) = + × 𝑉𝑠𝑡𝑑
𝑉𝑓 𝑉𝑓
Figure 4. Absorbance vs Volume – Soil
Substituting the absorbance reading (y) to the regression
line gives out
0.004533 − 0.0002 The equation of the line is:
𝑥= y = -6E-05x – 0.0005
0.0003
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CM123L ANALYTICAL CHEMISTRY LABORATORY
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The coefficient R is: Using the standard addition method in finding the
R2 = 0.9066 concentration of chromium, the experimenters were able to get
4.3611 ppm of chromium.
To get the concentration of chromium using the standard
addition method, the slope of the equation is used: 4.3611 𝑝𝑝𝑚
= 𝟎. 𝟎𝟎𝟎𝟒𝟑𝟔 % 𝑪𝒓
10,000
𝑘𝐴 𝐶𝐴 𝑉𝑜 𝑘𝐴 𝐶𝑠𝑡𝑑
y = mx + b or 𝑆𝑠𝑝𝑖𝑘𝑒 (𝑦) = + × 𝑉𝑠𝑡𝑑
𝑉𝑓 𝑉𝑓
For the internal standards method, three trials were also
conducted. Table 9 shows the absorbance per concentration of
Substituting the values of absorbance (y) into the equation, the sample and its average absorbance.
the concentration of Cr is determined.
For 0 mL:
Conc. in Absorbance Average
Calib. Absorba
−0.00047 + 0.0005
𝑥= Units, nce
−6𝐸 − 05 mg/L
Trial 1 Trial 2 Trial 3
x = -0.5 mg/L or ppm 0.25 -0.0002 -0.0003 -0.0016 -0.0007
0.5 0.0000 -0.0004 -0.0018 -0.00073
For 2 mL: 1.25 -0.0005 -0.0005 -0.0014 -0.0008
2.5 -0.0008 -0.0004 -0.0014 -0.00087
−0.0005 + 0.0005 5.0 -0.0004 -0.0003 -0.0014 -0.0007
𝑥=
−6𝐸 − 05 Table 9. Internal Standards Method – Soil
x = 0 mg/L or ppm
Figure 5 then shows the graphical representation between
For 4 mL: the concentration of the standard and absorbance. The slope
is slightly positively skewed.
x = 5 mg/L or ppm

For 6 mL:

x = 6.6667 mg/L or ppm

For 8 mL:

x = 6.1667 mg/L or ppm

For 10 mL:

x = 10 mg/L or ppm Figure 5. Absorbance vs Concentration - Soil

The equation of the line is:


Mean (x̅)
y = 1E-05x – 0.0004
−0.5+0+5+6.6667++6.1667+10
The coefficient R is:
x̅ = R2 = 0.1045
6
̅ = 𝟒. 𝟑𝟔𝟏𝟏 𝒑𝒑𝒎
𝐱
Standard Deviation (s) To get the concentration of chromium using the internal
standard method, the slope of the equation is used:
(x̅ − 𝑥1 )2 + (x̅ − 𝑥2 )2 + (x̅ − 𝑥3 )2
𝑠= √ 𝑘𝐴 𝐶𝐴 𝑉𝑜 𝑘𝐴 𝐶𝑠𝑡𝑑
𝑛−1 y = mx + b or 𝑆𝑠𝑝𝑖𝑘𝑒 (𝑦) = + × 𝑉𝑠𝑡𝑑
𝑉𝑓 𝑉𝑓

s = 3.2481

Experiment 14│ Group No. 05│ July 20, 2019 7 of 9


CM123L ANALYTICAL CHEMISTRY LABORATORY
4th Term SY 2018-2019

Substituting the values of absorbance (y) into the equation, standard addition method is 4.3611 ppm. The chromium
the concentration of Cr is determined. content of the sample through the internal standards method is
For 0.25 ppm: 2 ppm.

−0.0003 + 0.0004 CONCLUSIONS AND RECOMMENDATIONS


𝑥=
1𝐸 − 07
Chromium, a heavy metal, is used in metal alloys and
x = 10 mg/L or ppm pigments for paints, cement, paper, rubber, and other
materials. Low-level exposure can irritate the skin and
For 0.5 ppm: cause ulceration. Long-term exposure can cause kidney
and liver damage, and damage too circulatory and nerve
−0.0004 + 0.0004 tissue. Chromium often accumulates in aquatic life, adding
𝑥= to the danger of eating fish that may have been exposed to
1𝐸 − 07
high levels of chromium.
x = 0 mg/L or ppm
Posing that threat, there is a need for maintaining low-level
For 1.25 ppm: of chromium concentrations in soil and water. With that,
atomic absorption spectroscopy provides an easy way for a
specific determination of metals. In atomic absorption
x = -10 mg/L or ppm
analysis, the element being determined must be reduced to
its elemental state, vaporized, and imposed in the beam of
For 2.5 ppm: radiation from the light source.

x = 0 mg/L or ppm The experiment was divided into two parts, determination of
Cr content from a water sample from Pampanga river, and
For 5 ppm: determination of Cr content from a soil sample from Mapua
University. Each part was done in three methods, i.e.
x =10 mg/L or ppm external calibration method, standard addition method, and
internal standards method. The chromium content of the
Mean (x̅) water sample from Pampanga river through external
calibration technique is -5.4444 ppm. The chromium
10+0−10+0+10 content of the sample through the standard addition method
x̅ = is 4.3611 ppm. The chromium content of the sample
5
̅ = 𝟐 𝒑𝒑𝒎
𝐱 through the internal standards method is 0.4 ppm. This
suggests that Fe is more prevalent than Cr in the
Standard Deviation (s) Pampanga river. The chromium content of the soil sample
from Mapua University through external calibration
technique is 14.4433 ppm. The chromium content of the
(x̅ − 𝑥1 )2 + (x̅ − 𝑥2 )2 + (x̅ − 𝑥3 )2 sample through the standard addition method is 4.3611
𝑠= √ ppm. The chromium content of the sample through the
𝑛−1
internal standards method is 2 ppm. This also suggests that
iron is more prevalent than chromium in the soils of Mapua.
s = 7.4833
However, it was observed that the chromium concentration
Using the internal standards method in finding the from both samples is present when in fact, the soil and the
concentration of chromium, the experimenters were able to water sample must be free of chromium. Measures that can
get 2 ppm of chromium. prevent an increase in chromium concentration is highly
recommended. More recommendations include the
2 𝑝𝑝𝑚 determination of other heavy metals present in the soil and
= 𝟎. 𝟎𝟎𝟎𝟐 % 𝑪𝒓
10,000 water sample.

The chromium content of the soil sample from Mapua It can be then concluded, based on the set objectives on
University through external calibration technique is 14.4433 the experiment, that the experiment was successfully done.
ppm. The chromium content of the sample through the
Experiment 14│ Group No. 05│ July 20, 2019 8 of 9
CM123L ANALYTICAL CHEMISTRY LABORATORY
4th Term SY 2018-2019

The experimenters gained a basic understanding to the REFERENCES


principle and instrumentation of atomic absorption
spectroscopy or AAS. At the end, the amount of metal Germer, T.A. & Tsai, B.K., (2014). Experimental Methods
(chromium) present in the samples was quantitatively in the Physical Sciences, Vol. 46. 11-66. DOI:
determined through AAS, in three methods. The org/10.1016/B978-0-12-386022-4.00002-9
experimenters were also introduced to different digestion
procedures for solid and liquid samples. Lastly, for the Lenntech (n.d). Heavy Metals. Retrieved from
experimenters was able to compare the resulted www.lenntech.com/processes/heavy/heavy-metals/heavy-
concentration of chromium from various methods of metals.htm
analysis and all methods agrees that iron is more
prevalent than chromium. R. A. Mohamed, A. M. Abdel-Lateef, H. H. Mahmoud & A.
I. Helal (2012) Determination of trace elements in water
and sediment samples from Ismaelia Canal using ion
chromatography and atomic absorption spectroscopy,
Chemical Speciation & Bioavailability, 24:1, 31-38, DOI:
10.3184/095422912X13257005726800

Smith, R. (1983). A Laboratory Manual for the


Determination of Metals in Water and Wastewater by
Atomic Absorption Spectrophotometry. Pretoria. South
Africa.

Srikanth, P & A Somasekhar, S & Kanthi, Krishna &


Korupolu, Raghu. (2013). ANALYSIS OF HEAVY
METALS BY USING ATOMIC ABSORPTION SPECTRO-
SCOPY FROM THE SAMPLES TAKEN AROUND
VISAKHAPATNAM.

Tsade HK (2016) Atomic Absorption Spectroscopic


Determination of Heavy Metal Concentrations in Kulufo
River, Arbaminch, Gamo Gofa, Ethiopia. J Environ Anal
Chem 3:177. doi:10.41722380-2391.1000177

Experiment 14│ Group No. 05│ July 20, 2019 9 of 9


CM123L ANALYTICAL CHEMISTRY LABORATORY
4th Term SY 2018-2019

Experiment 14│ Group No. 05│ July 20, 2019 10 of 9

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