You are on page 1of 14

_________________________________________________________

UNIVERSITI TEKNOLOGI MARA


FAKULTI KEJURUTERAAN KIMIA
ENGINEERING CHEMISTRY LABORATORY
(CHE485)
_________________________________________________________
EXPERIMENT

: DETERMINATION OF CHROMIUM (VI)


CONCENTRATION VIA ABSORPTION SPECTROSCOPY

DATE PERFORMED

: 15th APRIL 2015

SEMESTER

: 1(ONE)

PROGRAMME / CODE

: EH220

SUBMIT TO

: WAN HAMDAH BINTI WAN AMRAN

GROUP

: EH2201

GROUPS MEMBERS

: 1. MUHAMMAD SOLAHUDIN BIN MUSA (2014342085)


2. AZIANI BINTI AHMAD SHAARANI (2014728953)

3. NUR DINNIE SHAZLYN BINTI MOHD NOOR SALIZAN


(2014155031)
Remarks;
Checked by:

----------------------Date:
TABLE OF CONTENT:

No.
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.

Title
Abstract/summary
Introduction
Objective
Theory
Apparatus
Methodology/Procedure
Results
Calculations
Discussion
Conclusion
Recommendations
References
Appendix

INTRODUCTION
Many heavy metals, including chromium (Cr), are toxic even at low aqueous solution
concentrations. Chromium ions, Cr (III) or Cr (VI), are found naturally in rivers, lakes and
streams. Trivalent Cr (III) compounds are not usually considered as health hazard because it
favored as reducing environment, but hexavalent Cr (VI) compounds can be toxic if ingested or
inhaled because it favored as oxidizing environment and have been established as carcinogens.
Chromium (VI) is also classified as a strong oxidation agent and it poses a great deal of toxicity
to humans and animals as well due to its carcinogenetic. This health-risky situation has lead to

many studies and investigations on determining the presence and quality of chromium in
biological and environmental samples.

OBJECTIVE
1. To determine the chromium (VI) content that present in the polluted water samples using
spectrophotometer.
2. To demonstrate the proper method in preparing the standard solution.
3. To analyze whether the tested polluted water sample is suitable for drinking water and for
agricultural purpose.

THEORY
In this experiment, absorption spectroscopy will be used to detect low level concentration of
chromium (VI) in a polluted water samples. As a matter of fact, coloured aqueous solutions
have chemical species contents which absorb significant wavelengths of light. Similary, heavy
metals can be identified via absorption of wavelengths of light. Futhermore, the amount of light
absorbed is linearly proportional to the concentration of the solution metal ions.
Absorption spectroscopy operates on the measuring principle of light before and after it passes
through an aqueous metal solution. The amount of light absorbed by the chemical species in the
sample is equivalent to the difference in the amount of light before it enters the sample and after
it exits the samples. For the purpose of light to be absorbed by chemical species, the light must
be set to a specific wavelength. Every chemical species absorbs distinct wavelengths of light. In
absorption spectroscopy, the wavelengths of light absorbed by a metal in solution are detected.
In this experiment, standard solutions will be prepared by diluting 300 ppm of Chromium (VI)
standard solution. Five standard solutions need to be prepared from the concentrated
Chromium (VI) standard solution. To calculate the dilute solution volume, the formula below are
used:
M1V1 = M2V2 -----------(1)
Quantitave analysis using spectrophotometer is based on Beer-Lambert Law:
A = LC -------------(2)
Where;
A

= absorbance value (dimensionless)

= molar absorbance ( L / mol.cm )

= path length of the cuvette in which the sample is contained (cm)

= concentration of the compound in solution ( mol / L )

Beer-Lambert Law states that absorbance value depends on the total quantity of the absorbing
compound in the light path through the cuvette. Thus, if we plot a graph of absorbance versus
concentration of the compound solution, we get a straight line passing through the origin ( 0,0 ).
The molar absorbance, , is a constant for a particular substance, therefore if the concentration

of the solution is halved, so is the absorbance value. A compound with a high molar absorbance
is very effective at absorbing light (of the appropriate wavelength), and hence low
concentrations of a compound with a high molar absorbance can be easily detected.

APPARATUS
1. Distilled water
2. UV single beam spectrometer (HaCH)
3. 10 mL cuvette bottle
4. Pipette
5. Five sets of 10 mL of 1, 15, 45, 75, 100 ppm of diluted solution of chromium (VI)
6. Four sets of 300 ppm of standard chromium (VI) solution of 1.0 mL, 3.0 mL, 5.0 mL, 6.67 mL,
for 15 ppm, 45 ppm, 75 ppm and 100 ppm.
7. A set of 15 ppm of standard Chromium (VI) solution of 1.33 mL for 1 ppm.
8. polluted water samples.

PROCEDURE / METHODOLOGY

1) The apparatus and materials was prepared and set up.


2) Four series of diluted solution was prepared by using the dilution method with
distilled water from 300 ppm of Chromium (VI) standard solution for
concentration 15 ppm, 45 ppm, 75ppm, and 100 ppm.
3) One diluted solution is then prepared by using the same method in step 3 but
this time, the diluted solution was prepared from 15 ppm of Chromium (VI)
standard solution for concentration 1 ppm.
4) The 10 mL of cuvette bottle was filled up with distilled water and placed on the
spectrometer slot. A zeroing step was done to ensure that all the data obtained
was accurate.
5) Then, 10 mL of each series of diluted solution was poured into cuvette bottle
and placed on the spectrometer slot to check the absorbance value by using
spectrometer.
6) All the data obtained was recorded.
7) Then, 10 mL of each polluted water sample is poured into the cuvette bottle
and spectrometer was used to determine the Chromium (VI) concentration
contained in the water sample collected.
8) All the value obtained was analyzed and recorded.

RESULTS

TABLE 1: Determination of absorbance value using spectrometer


Volume of chromium

1.33

1.0

3.0

5.0

6.67

15

45

75

100

0.076

0.094

0.106

0.127

0.139

(VI), mL
Concentration of
chromium (VI), ppm
Absorbance

TABLE 2: Determination of absorbance value of water sample using spectrometer


polluted water sample

Absorbance

Tasik Taman Cahaya Alam

-0.045

Taman Cahaya Alam Drain

0.081

Delimas hostels drain

0.064

Dataran Cendiakawan pond

0.010

Tap water

-0.030

CALCULATIONS
A) Preparation of Cr (VI) standard solution
100 ppm 20 ml Cr (VI) standard solution
(M1) (V1) = (M2) (V2)
(300 ppm) (V1) = (100 ppm) (20 ml)
(V1) = 6.67 ml

75 ppm 20 ml Cr (VI) standard solution


(M1) (V1) = (M2) (V2)
(300 ppm) (V1) = (75 ppm) (20 ml)
(V1) = 5 ml

45 ppm 20 ml Cr (VI) standard solution


(M1) (V1) = (M2) (V2)
(300 ppm) (V1) = (45 ppm) (20 ml)
(V1) = 3 ml

15 ppm 20 ml Cr (VI) standard solution


(M1) (V1) = (M2) (V2)
(300 ppm) (V1) = (15 ppm) (20 ml)
(V1) = 1 ml

1 ppm 20 ml Cr (VI) standard solution


(M1) (V1) = (M2) (V2)
(15 ppm) (V1) = (1 ppm) (20 ml)
(V1) = 1.33 ml

B) Preparation of Cr (VI) standard solution


0.16
0.14

R ==0.98
f(x)
0x + 0.08

0.12
0.1
ABSORBANCE

0.08

Abs

0.06

Linear (Abs)

0.04

Linear (Abs)

0.02
0
0

20 40 60 80 100 120

CONCENTRATION of Cr (IV) (ppm)

Tasik Taman Cahaya Alam


Absorbance of water sample = -0.045
Y-axis = Absorbance of waste water
X-axis = Concentration of Cr (VI) in the waste water
Y = mX + C
y = 0.0006x + 0.0797
-0.045 = 0.0006x + 0.0797
X = -0.045 0.0797
0.0006
X = -208 ppm

Taman Cahaya Alam Drain


Absorbance of water sample = 0.081
Y = mX + C
y = 0.0006x + 0.0797
0.081 = 0.0006x + 0.0797
X = 0.081 0.0797
0.0006
X = 2 ppm

Delimas hostels drain


Absorbance of water sample = 0.064
Y = mX + C
y = 0.0006x + 0.0797
0.064 = 0.0006x + 0.0797
X = 0.064 0.0797
0.0006
X = -26 ppm

Dataran Cendiakawan pond


Absorbance of water sample = 0.010
Y = mX + C
y = 0.0006x + 0.0797
0.010 = 0.0006x + 0.0797
X = 0.010 0.0797
0.0006
X = -116 ppm

Tap water
Absorbance of water sample = -0.030
Y = mX + C
y = 0.0006x + 0.0797
-0.030 = 0.0006x + 0.0797
X = -0.030 0.0797
0.0006
X = -183 ppm

DISCUSSION
A solution of Cr3+ is deep violet for example, and a trace of Cr3+ in the Al2O3
crystal structure gives ruby its beautiful red hue. Chromium readily forms a thin,
adherent, transparent coating of Cr2O3 in air, making the metal extremely useful as
an attractive protective coating on easily corroded metals. Chromium metal and the
Cr2+ ion are potent reducing agents. The metal displaces hydrogen from dilute acids
to form blue Cr2+ (aq), which reduces O2 in air within minutes to form the violet Cr3+
ion:
4Cr2 + (aq) + O2 (g) + 4H+ (aq) 4Cr3+ (aq) + 2H2O (l)
Chromium (VI) compounds in acid solution are strong oxidizing agents
(concentrated solutions are extremely corrosive), the chromium (VI) being readily
reduced to chromium (III):
Cr2O72- (aq) + 14H+ (aq) + 6e- 2Cr3+ (aq) + 7H2O (l)
This reaction is often used to determine the iron content of a water or soil sample
by oxidizing Fe2+ to Fe3+ion. In basic solution, the CrO42-ion, which is a much weaker
oxidizing agent, predominates:
CrO42- (aq) + 4H2O (l) + 3e- Cr(OH)3 (s) + 5OH- (aq)
The experiment was conducted to achieve a few of main objective in this
experiment such as to determine the Chromium (IV) content which present in the
water sample by using the spectrometer, to demonstrate the proper method of
diluting solution to prepare of standard solution in the range 1 p.p.m to 100 p.p.m
and lastly to analyse wheter the water sample is suitable for drinking water and
agriculture purpose.
In chemistry, spectrophotometry is the quantitative measurement of the
reflection or transmission properties of a material as a function of wavelength and
the water sample. The water sample is used to examine the presence of chromium
is assumed that to be contaminant, the source of the water sample is the source of
water sample is located near a roadway where road users with automobiles use it
every day. This is due to rivers, lakes and any water streams which are near to
congested areas have the highest risk or most susceptible to contain heavy metals
such as chromium itself and is then classified as contaminated water source.
The first step in this experiment is to prepare 5 standard solution Cr(VI)
standard solutions using serial method as mentioned in the theory. The
concentrations for standard 1, standard 2,standard 3, standard 4 and standard 5 is
100 ppm, 75 ppm, 45 ppm, 15 ppm and 1 ppm respectively.
The absorbance for each five standard solutions and the lake water sample is
taken by using the spectrophotometer. The average absorbance is then calculated.
A graph of the absorbance is plotted against the concentration of standard
solutions.

Linear regression analysis is performed by using Microsoft Excel in order to


determine the linear best fit for the absorbance versus concentration data. The R 2
value indicates how well the regression analysis fits the absorbance-concentration
data. Since our R2 = 0.9797, that graph can be used to determine the concentration
of chromium with more accurately. In this graph, the points are all very close to the
best fit line, so the R-squared value is high. The closer the R 2 value is to 1.00, the
better the linear regression analysis has fit the data.

Results show a graph of absorbance versus concentration of five standard


solutions. The line determined from the regression analysis will be in the form of y =
mx + b, where y is the absorbance value and x is the concentration of the solution.
This equation also can be obtained by just select an option in Microsoft Excel.
Algebraic substitution of the absorbance value (y) for the unknown metal solution
into the linear regression equation for the line permits the determination of the
concentration (x) of the unknown solution. The linear relationship is found to be:

y = 0.0006x + 0.0797

The state and federal regulatory agencies consider that the chromium,
chromium (VI) to be toxic at concentration levels > 0.0300 ppm. Natural waters
whose chromium (VI) concentrations exceed 0.300 ppm may not be used for
drinking water or for agricultural purposes.
After doing some calculations based on the graph, the concentration of the
sample collected from Tasik Taman Cahaya Alam, Delimas hostels drain, Dataran
Cendiakawan pond, and tap water are determined to be at -208 ppm, -26 ppm, -116
ppm, and -183 ppm respectively which indicates that those four water sample are
free from chromium (Iv). The negative sign of value is the great sign to show that
those water sample are free from chromium (Iv). Therefore, Tasik Taman Cahaya
Alam, Delimas hostels drain, Dataran Cendiakawan pond, and tap water is suitable
for drinking water and for agricultural purposes. But, these water source are about
to use as drinking water, water must be clinically treat first. However, based on the
graph also, the concentration of the Taman Cahaya Alam Drain sample is
determined to be at 2 ppm which is not suitable for drinking water and for
agricultural purposes. By referring the state and federal regulatory agencies guide,
concentration level of chromium (Iv) in Taman Cahaya Alam Drain sample is 2ppm,
which it higher than 0.0300ppm which consider that chromium to be toxic.
Since the concentration of Chromium (VI) in the water sample of Taman
Cahaya Alam Drain is calculated to be 2 ppm. This high concentration of Cr (VI) in
waste water is mainly due to the activity at the surrounding of the Taman Cahaya
Alam Drain. There are several road and housing area that are situated nearby the
water source. When there is people, there is vehicle. I have stated before that
emission from engine exhaust is one of the main source of Cr (VI) contamination.

People tend to use their car to go to work every day and on Friday, lots of Muslim
use the road to go to the State Mosque for Friday Prayer. So, many vehicle come
back and forth at the surrounding of the water source. Beside Cr (VI), the emission
of the vehicle also contain a high concentration of greenhouse gases (water vapor,
carbon dioxide, methane, nitrous oxide, and ozone). Carbon oxide and other
contaminants somewhat contribute to the contamination of the water. The Taman
Cahaya Alam is also situated near Seksyen 7. Seksyen 7 are known to have many
restaurant that operate daily. Those restaurant does not have a proper sewage
system. The sewage is channel directly without any proper treatment into the water
system and it rain, the contaminated water will be washed off into the underground
water system and contaminate the water source of the Taman Cahaya Alam.

We also have discussed before that Cr (VI) is known to cause cancer in


humans when inhaled. Cr (VI) can also damage the lining of the nose and throat and
irritate the lungs. When swallowed, Cr (VI) can upset the gastrointestinal tract and
damage the liver and kidneys. Death may occur following cardiovascular shock. In
some occupational studies, increased incidences of genotoxic effects such as
chromosomal aberrations exchanges have been found in workers exposed to
chromium (VI) compounds. Drinking water can be treated by different pump and
treat remediation systems. Cr (VI) can be removed by an activated carbon filter,
reverse osmosis or ion exchange resin. Thus, the waste water is not suitable for
drinking and agricultural purposes.

CONCLUSION
From this experiment, it can be concluded that chromium (VI) are present in
the water sample from Taman Cahaya Alam Drain only. By using the
spectrophotometer, the concentration of chromium (VI) in the Taman Cahaya Alam
Drain water water is 2 ppm. Since it is above the level of standard allowed by the
Malaysian Environmental Quality (Sewage and Industrial Effluents) Regulations of
1979 which is 0.01ppm. Therefore, the water is concluded as contaminated and
does not suitable for drinking or agricultural purposes. But, water sample from Tasik
Taman Cahaya Alam, Delimas hostels drain, Dataran Cendiakawan pond, and tap
water are concluded as free from chromium (VI). The experiment was successfully
conducted.

RECOMMENDATION
1

Collect the test sample in clean bottles. Fill completely and cap tightly.

Use a damp towel followed by a dry one to remove finger prints or other
marks from the surface of the cuvette before taking the absorbance reading.

Use a clean beaker when diluting the 300.00 ppm Cr (VI) standard solution.

Take more absorbance reading.

Use a clean cuvette.

REFERENCES
1

http://en.wikipedia.org/wiki/Greenhouse_gas

http://www.lenntech.com/periodic/elements/cr.htm

http://www.cluin.org/contaminantfocus/default.focus/sec/chromium_VI/cat/Ov
erview

Janus JA, Krajnc EI. Integrated criteria document chromium: effects. Appendix. Bilthoven,
Netherlands, National Institute of Public Health and Environmental Protection,1990.

http://www.cluin.org/contaminantfocus/default.focus/sec/chromium_VI/cat/Treat
ment_
Technologies/