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ABSTRACT

Spectroscopy is a technique that uses the interaction of energy with a


sample to perform an analysis. The data that is obtained from spectroscopy
is called a spectrum. A spectrum is a plot of the intensity of energy detected
versus the wavelength of the energy. In this experiment, the
spectrophotometer was used to determine the concentration of Chromium
(VI) via the absorption.

Cr is a symbol for chemical element called Chromium with atomic


number of 24. It is the first element in Group 6. It is a steely-gray, lustrous,
hard metal that takes a high polish and has a high melting point. It is also
odorless, tasteless, and malleable. Chromium does not occur freely in nature.
Chromite are the main mineral in the Chromium. As was mentioned earlier,
chromium compounds can be found in waters only in trace amounts. The
element and its compounds can be discharged in surface water through
various industries. It is applied for example for metal surface refinery and in
alloys. Stainless steel consists of 12-15% chromium. Chromium metal is
applied worldwide in amounts of approximately 20,000 tons per year. It may
be polished and it does not oxidize when it comes in contact with air.
Chromium may be present in domestic waste from various synthetic
materials. Through waste incineration it may spread to the environment
when protection is insufficient.

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INTRODUCTION

In this experiment, the spectroscopy was used to determine the


concentration of Chromium (VI) via the absorption. Spectroscopy is the study
of the interaction between matter and radiated energy. Usually, spectroscopy
originated through the study of visible light dispersed according to its
wavelength. Later the concept was expanded greatly to comprise any
interaction with radiated energy as a function of its wavelength or frequency.
Spectroscopic data is often represented by a spectrum, a plot of the
response of interest as a function of wavelength or frequency.

Chromium metal is used in for a large variety of applications ranging


from an additive in the manufacture of stainless steel to chromium plating. It
is used for motorcycle exhausts and some older types of car bumpers to the
colorizations of Rubies and Emeralds. Chromium metal has a more important
use, it is a very hard transition metal and is normally amalgamated with
titanium to make replacement hips in the USA and UK.

Chromium compounds (such as Chromic acid) are used in the


electroplating industry as both an additive and (in the case of Chromic acid)
as a highly powerful oxidizing agent. Chromic acid is roughly 3 times as
powerful an oxidizing agent as sulphuric acid due to the oxidizing power of
the Chromium (VI) itself.

With all industrial processes, a waste product is inevitably formed. In


the Chromium industries (plating and manufacturing), it is normally the
Chromium (VI) compound (such as chromic acid and other high oxidizing
Chromium (VI) cleaners). As was mentioned earlier, chromium compounds
can be found in waters only in trace amounts. The element and its
compounds can be discharged in surface water through various industries. It
is applied for example for metal surface refinery and in alloys.

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Hexavalent chromium has been detected in groundwater across the
United States due to industrial and military operations, including plating,
painting, cooling-tower water and chromate production. Because inhalation
of Chromium (VI) can cause lung cancer in some persons exposed to a
sufficient airborne concentration, questions have been raised about the
possible hazards associated with exposure to Chromium (VI) in tap water via
ingestion, inhalation, and dermal contact. Although ingested Chromium (VI)
is generally known to be converted to Chromium (III) in the stomach
following ingestion, prior to the mid-1980s a quantitative analysis of the
reduction capacity of the human stomach had not been conducted.

The water sample will be analyzed by the spectroscopy in order to get


the absorbance value. From the result we can calculate the concentration of
Chromium (VI) and know whether the water sample is suitable for drinking or
other uses.

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OBJECTIVES

The objectives of conducting this experiment are to determine the Chromium


(VI) content which present in simulated lake water sample using a
spectrophotometer, to demonstrate the proper method of diluting solution to
prepare a series of standard solution in the range of 5-200 part per million
(p . p . m) to be used in the calibration of the spectrophotometer , and thus,
to analyze whether the simulated lake water sample test is suitable for
drinking water and agriculture purposes .

THEORY

Chromium occurs naturally as a trace component of most crude oils,


and the concentrations of chromium found in residual and distillate oils have
been measured. Available information suggests that the chromium is emitted
in the trivalent state from oil combustion, sewer sludge incineration, cement
production, municipal waste incinerators and refractories. Chromium is used
for corrosion resistance, steel production, and as protective coating for
automotive and equipment accessories. It is a permanent and stable
inorganic pigment used for paints, rubber, and plastic products. Chromium
has also been detected but not quantified in motor vehicle exhaust by the Air
Resources Board (ARB) .

Chrome plating is a source of Chromium (VI) emissions in the state.


Chrome electroplating operations are conducted in baths containing chromic
acid and during the plating process, bubbles of gas are emitted through the
surface of the bath. These bubbles carry entrained Chromium (VI) into the
air. Chromium emissions can occur from Chromium (VI) firebrick lining of
glass furnaces. Although it is a minor source of emissions, the most
commonly seen hexavalent chromium is lead chromate. Lead chromate is
the pigment in the yellow paint used to mark traffic lanes. In addition,
hexavalent chromium in water solution is converted through electroplating
(decorative chrome plating) to the bright metallic chromium coating seen on

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plastic or metal products such as shower heads or car bumpers. Although not
commonly seen by the general public, one of the most important uses of
chrome plating is to apply a hard, smooth surface to machine parts such as
crankshafts and printing rollers. This process is known as "hard" chrome
plating. Chromic acid anodizing is another industrial metal finishing process
which uses hexavalent chromium.

Chromium that is deposited on highroads originated from brake and


dusts and exhaust of automobile engine can unfavorably permeate into any
water streams nearby via flowing rainwater. Lakes and water streams which
is nearer a typical congested with automobiles areas are the most
susceptible areas to be contaminated by such chromium. Due to its cancer-
risk character and toxicity even at mere concentrations, a lot of federal
environmental agencies are doing researches to determine its presence in
many environmental samples. Thus, in this experiment absorption
spectroscopy will be used to detect the concentrations of Chromium (VI) in a
water sample.

As a matter of fact, colored aqueous solutions have chemical species


contents which absorb significant wavelengths of light. Similarly, heavy
metals can be identified via absorptions of wavelengths of light. The amount
of light absorbed is linearly proportional to the concentration of metal ions.
Absorption spectroscopy operates on the measuring principle of light.

Absorption spectroscopy refers to spectroscopic techniques that


measure the absorption of radiation, as a function of frequency or
wavelength, due to its interaction with a sample. The sample absorbs
energy, i.e., photons, from the radiating field. The intensity of the absorption
varies as a function of frequency, and this variation is the absorption
spectrum. Absorption spectroscopy is performed across the electromagnetic
spectrum. Absorption spectroscopy measuring principle of light before and
after it passes through an aqueous metal solution. The amount of light

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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 sample. 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 the in solution are detected.

In this experiment, standard stock solutions are prepared by diluting


300 parts per million (p.p.m) of Chromium (VI) standard solution Five
standard stock solutions being prepared from the concentrated Chromium
(VI) standard solution with range from 15 p.p.m to 300 p.p.m. To calculate
the dilute solutions volume needed, the solution dilution formula can be
used:

M1V1 = M2V2

M1 : is a concentration of standard Chromium (VI) solutions, which is 300


p.p.m.

V1 : is volume of distilled water needed to dilute Chromium (VI) solutions

M2 : is a concentration of stock solution of Chromium (VI) solutions, which are


5, 20,
40, 60, 80, 100 and 200 p.p.m.

V2: is a volume of volumetric flask which is 50mL

Quantitative analysis using spectroscopy is based on Beer-Lambert


Law. Beer-lambert Law states that absorbance value depends on total
quantity of the absorbing compound in the light path through the cuvette.

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Thus, if we plot a graph of absorbance versus concentration of the compound
solution, we get a straight line passing through the origin .A compound with
high molar absorbance is very effective at absorbing light. Hence, low
concentrations of a compound and high molar absorbance can be easily
detected by the spectroscopy. The Beer-Lamberts Law

A = LC

A : is absorbance value from the spectroscopy

: molar absorbance (L/mol.cm)

L : path length of the cuvette in which the sample is contained C :


Concentration of the compound in solution (mol/L)

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APPARATUS

1. Spectrometer.
2. 10 mL of cuvette.
3. Pipette.
4. Dropper.
5. Measuring cylinder.
6. 50 mL volumetric flask.
7. Stopper.
8. Beaker

MATERIALS

1. Distilled water.
2. Stock solution of chromium (VI) solution (200ppm)
3. 7 set of diluted chromium (VI) solutions which are 200 ppm, 100 ppm, 80
ppm, 60 ppm, 40 ppm, 20 ppm and 5 ppm.
4. Lake Sample

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PROCEDURE

1) All the materials and apparatus are setup.


2) The standard solutions of chromium are prepared with the different
concentrations which are 200 ppm, 100 ppm, 80 ppm, 60 ppm, 40 ppm,
20 ppm and 5 ppm.
3) By using the pipette, 0.33 mL, 1.33 mL, 2.67 mL, 4.00 mL, 5.33 mL, 6.67
mL and 13.33 mL of chromium (VI) solution is taken and placed in the
different volumetric flask and it labeled. All the preparations are
conducted in the fume hood.
4) The volumetric flask is filled with the distilled water until it reaches the
mark on the volumetric flask.
5) The volumetric flask is closed with the stopper and then shake 2 times or
more to make the solution mix well.
6) The spectrometer is switched on.
7) 10 mL of distilled water is filled into the square cuvette and the placed in
the spectrometer slot. Before that, make sure there are no bubbles in the
cuvette because it can affect the reading of the absorbance.
8) To ensure the all data obtained are accurate, the zeroing step is done first.
9) The diluted solution which known as standard solution, is transferred into
the square cuvette.
10) After that, the cuvette is placed in the spectrometer slot. Before that,
make sure the cuvette is cleaned from dirt and also fingerprint to avoid
from error reading of absorbance of the solution.
11) The reading of absorbance is recorded and tabulated into a data.
12) After that, the water sample is filled into the cuvette and placed in the
spectrometer slot to get the reading of absorbance.
13) All the data is recorded and analyzed.

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RESULT

Volume Of Concentration Of Absorbance Value


Chromium(VI) mL Chromium(VI)
Part/Million (p.p.m)
M1V1 = M2V2 5 0.001
300(V1) = (5)(20)
V1 = 0.33 mL
M1V1 = M2V2 20 0.011
300(V1) = (2)(20)
V1 = 1.33 mL
M1V1 = M2V2 40 0.014
300(V1) = (40)(20)
V1 = 2.67 mL
M1V1 = M2V2 60 0.026
300(V1) = (60)(20)
V1 = 4.00 mL
M1V1 = M2V2 80 0.034
300(V1) = (80)(20)
V1 = 5.33 mL
M1V1 = M2V2 100 0.043
300(V1) = (100)(20)
V1 = 6.67 mL
M1V1 = M2V2 200 0.052
300(V1) = (200)(20)
V1 = 13.33 mL

Table : Absorbance value of Chromium (VI)

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Lake Water Sample Absorbance Value

Tasik Cheras (outlet) 0.014

Tasik Seksyen 7 (100m from 0.031


inlet)

Tasik Cheras (50m from inlet) 0.058

Tasik Cheras (inlet) 0.080

Tasik Seksyen 7 (50m from 0.097


intlet)

Tasik Seksyen 7 (100m from 0.118


inlet)

Table 2 : Absorbance value of different water sample

0.06
f(x) = 0x

0.05

0.04

0.03
Absorbance Value

0.02

0.01

0
10 30 50 70 90 110 130 150 170 190 210
0 20 40 60 80 100 120 140 160 180 200

Concentration of Chromium (VI) solution (p.p.m)

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Figure 1 : Graph of absorbance value versus concentration of Chromium (VI)
solution (p.p.m)

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CALCULATIONS

For 15 p.p.m

mg. mol 1g g . mol



5 ppm = 5 L 1000 mg. mol = 0.005 L

1L
20 mL Chromium solution = 0.02 L Chromium solution
1000 mL

n= MV

g . mol
0.005 0.02 L = 0.0001 g.mol Chromium
L

Mass = no of moles molar mass

52 g chromium
0.0001 g.mol Chromium = 0.0052 g of chromium
1 mol chromium

For 20 p.p.m

mg. mol 1g g . mol



20 ppm = 20 L 1000 mg. mol = 0.02 L

1L
20 mL Chromium solution = 0.02 L Chromium solution
1000 mL

n= MV

g . mol
0.02 0.02 L = 0.0004 g.mol Chromium
L

Mass = no of moles molar mass

52 g chromium
0.0004 g.mol Chromium = 0.0208 g of chromium
1 mol chromium

For 40 p.p.m

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mg. mol 1g g . mol

40 ppm = 40 L 1000 mg. mol = 0.04 L

1L
20 mL Chromium solution = 0.02 L Chromium solution
1000 mL

n= MV

g . mol
0.04 0.02 L = 0.0008 g.mol Chromium
L

Mass = no of moles molar mass

52 g chromium
0.0008 g.mol Chromium = 0.0416 g of chromium
1 mol chromium

For 60 p.p.m

mg. mol 1g g . mol



60 ppm = 60 L 1000 mg. mol = 0.06 L

1L
20 mL Chromium solution = 0.02 L Chromium solution
1000 mL

n= MV

g . mol
0.06 0.02 L = 0.0012 g.mol Chromium
L

Mass = no of moles molar mass

52 g chromium
0.0012 g.mol Chromium = 0.0624 g of chromium
1 mol chromium

For 80 p.p.m

mg. mol 1g g . mol



80 ppm = 80 L 1000 mg. mol = 0.08 L

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1L
20 mL Chromium solution = 0.02 L Chromium solution
1000 mL

n= MV

g . mol
0.08 0.02 L = 0.0016 g.mol Chromium
L

Mass = no of moles molar mass

52 g chromium
0.0016 g.mol Chromium = 0.0832 g of chromium
1 mol chromium

For 100 p.p.m

mg. mol 1g g . mol



100 ppm = 100 L 1000 mg. mol = 0.1 L

1L
20 mL Chromium solution = 0.02 L Chromium solution
1000 mL

n= MV

g . mol
0.1 0.02 L = 0.002 g.mol Chromium
L

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Mass = no of moles molar mass

52 g chromium
0.002 g.mol Chromium = 0.104 g of chromium
1 mol chromium

For 200 p.p.m

mg. mol 1g g . mol



200 ppm = 200 L 1000 mg. mol = 0.2 L

1L
20 mL Chromium solution = 0.02 L Chromium solution
1000 mL

n= MV

g . mol
0.2 0.02 L = 0.004 g.mol Chromium
L

Mass = no of moles molar mass

52 g chromium
0.004 g.mol Chromium = 0.208 g of chromium
1 mol chromium

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DISCUSSION

The aims of this experiment was to to determine the Chromium (VI) content
which present in simulated lake water sample using a spectrophotometer, to
demonstrate the proper method of diluting solution to prepare a series of
standard solution in the range of 5-200 part per million (p.p.m) to be used in
the calibration of the spectrophotometer, and thus, to analyze whether the
simulated lake water sample test is suitable for drinking water and
agriculture purposes .

This experiment involved spectroscopy method, which is a technique


that uses the interaction of energy with a sample to perform an analysis.
Chromium (VI) content that present in Tasik Seksyen 7 (100m from inlet)
sample is 98 p.p.m.

The proper method of diluting solution to prepare a series of standard


solution in the range of 5 - 200 part per million (p . p . m) is by using
formula :

M1V1 = M2V2

From this formula, the volume of chromium to be diluted can be calculated.


Then part per million can be prepared.

The water sample will be analyzed by the spectroscopy in order to get


the absorbance value. From the result we can calculate the concentration of
Chromium (VI) and know whether the water sample is suitable for drinking or
other uses. The concentration of Chromium (VI) is 98 p.p.m that is optimum
and suitable for convenient purpose.

The objective of this experiment is achieved. Chromium (VI) content


that present in Tasik Seksyen 7 (100m from inlet) sample is 98 p.p.m. M 1V1 =
M2V2 formula is used to prepared the volume of chromium, and the water
sample is suitable for drinking or other uses.

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CONCLUSION

The proper method of diluting solution to prepare a series of standard solution in the
range of 5 200 part per million (Ppm) is demonstrated in this experiment and it is used
in the calibration of the spectrophotometer. The Chromium (VI) content which present in
simulated lake water sample is . It is obtained using a spectrophotometer. Drinking
water should be less than 500 ppm, and water for agriculture should be less than 1200
ppm. The lake water sample is 98 p.p.m.

RECOMMENDATIONS

These are the recommendations and precautions that can be considered in the
experiment to get a better and accurate result. Firstly, all the apparatus that are used
like cuvette, beaker, dropper and equipment like spectrophotometer are in good
condition. Secondly, make sure the volume of the standard solution used must be taken
correctly by avoiding parallax error. Thirdly, obtain the lake water sample from more
places. In this experiment, all groups only obtain the sample from two lakes. Fourthly,
the standard solution that is used should be a hundred percent pure and stable at room
temperature. Lastly, the spectrophotometer. This spectrophotometer is a precision
instrument and deserves careful handling. Always wipe fingerprints and spilt sample off
the outside of the cuvette before measuring. Dont forget to close the door to the cuvette
compartment before reading the result.

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REFERENCE / APPENDIX

1. (2014, November 02). Determination of Chromium (VI) Concentration via


Absorption

Spectroscopy Experiment. Retrieved from

https://www.scribd.com/doc/39166236/Determination-of-Chromium-VI-

Concentration-via-Absorption-Spectroscopy-Experiment

2. (2014, November 02). Determination of concentration of chromium.


Retrieved from

https://www.scribd.com/doc/110293635/determination-of-concentration-
of-chromium

3. (2014, November 02). Spectroscopy Introduction. Retrieved from

http://chemistry.about.com/od/analyticalchemistry/a/spectroscopy.htm

4. Refer to the attachment provided in the next page.

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