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TABLE OF CONTENT

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

Tittle
ABSTRACT
INTRODUCTION
OBJECTIVES
THEORY
PROCEDURE
APPARATUS & MATERIALS
RESULTS
SAMPLE OF CALCULATION
DISCUSSION
CONCLUSION
RECOMMENDATION
REFERENCE & ATTACHMENT

Page
3
4
4
5&6
6
7
7
8&9
10&11
12
12
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1.0

ABSTRACT

Chromium (VI) is classified as a strong oxidation agent and it poses a great deal of toxicity to
humans and animals due to its carcinogenetic. This health-risky situation lead to many studies
and investigations on determining the presence and quantity of chromium in biological and
environmental samples. In the present study, an absorption method for the determination of
chromium (VI) concentration is proposed and the method is operated spectrophotometrically
by tracing the presence of chromium (VI) at a wavelength of 435 nanometres. The
concentration of Chromium (VI) in the lake water sample tested is 49.8 parts per million. The
experiment is completed and successfully conducted. [1]
Spectroscopy is a technique that uses the interaction of energy with a sample to perform an
analysis. The data that gained from spectroscopy is called a spectrum. A spectrum is a plot of
the intensity of energy detected versus the wavelength (or mass or momentum or frequency,
etc.) of the energy. [2]
Naturally occurring Cr(VI) has recently been reported in ground and surface waters. Rock
strata rich in Cr(III)-bearing minerals, in particular chromite, are universally found in these
areas that occur near convergent plate margins. Chromium occurs in the environment
primarily in two valence states, trivalent chromium (Cr III) and hexavalent chromium (Cr
VI). Exposure may occur from natural or industrial sources of chromium. Chromium III is
much less toxic than chromium (VI).[4]
Apparatus used to identify the value of absorbance value was spectrophotometer.Firstly ,
Using The formula , the initial volume of 300 ppm Chromium (VI) was calculated.Five
Beaker was labelled with 60 ppm , 120 ppm , 150 ppm , 210 ppm , 270 ppm and 300 ppm
respectively .Chromium (VI) is pipette according to the volume calculated , using a
formula(M1V1=M2V2) .The Chromium (VI) is pipette into respective labeled beakers to obtain
the specific concentration of chromium (VI). Distilled water is added to the volumetric flask
until it reach calibration mark. Therefore , five standard solution is prepared .Distilled water
was put into cuvette of the spectrophotometer to calibrate 0.00 reading .Next ,
spectrophotometer was left to continue the experiment with standard solution prepared .This
procedures was proceed by placing the standard solutions with 60 ppm , 120 ppm , 150 ppm ,
210 ppm , 270 ppm and 300 ppm inside the cuvette one at the time .The reading of
absorbance of each solution that stated on spectrophotometer was recorded.
The result is obtained

2.0

INTRODUCTION
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Many heavy metals, such as chromium, are undeniably toxic at low aqueous solution
concentrations. Chromium ions are commonly found in either trivalent, Chromium (III), or
hexavalent, Chromium (VI), states. Chromium (VI) formation is favoured by an oxidizing
environment, while Chromium (III) is favoured by a reducing environment. It is found that
naturally alkaline rivers and lakes have much lower risk of such heavy metal contamination
of chromium ions in comparison with naturally acidic water streams.
Chromium (VI) is known to be a strong oxidizing agent, which apparently poses a
high risk yet negative impact to humans and animals due to its carcinogenetic properties. That
is why there are a lots of studies that have been done profusely in order to determine the
health-risky chromium in environmental as well as biological samples. [1]
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. Spectroscopy originated through the study of visible light
dispersed according to its wavelength. The concept was expanded greatly to comprise any
interaction with radiative 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. With all industrial processes, a waste product is formed.
In Chromium industries, it is normally the Chromium (VI) compound (such as
chromic acid and other high oxidizing Chromium (VI) cleaners). As was mentioned,
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.
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.

3.0 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 solutions in the range of 1
to 100 parts per million (p.p.m) to be used in the calibration of the spectrophotometer, and
thus, to analyze whether the simulated lake water sample tested is suitable for drinking water
and agriculture purposes.

4.0

THEORY
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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.
Chromium(VI) compounds are powerful oxidants at low or neutral pH. Most important are
chromate anion (CrO4) 2 and dichromate (Cr2O7) 2 anions, which exist in equilibrium:
2 [CrO4]2 + 2 H+

[Cr2O7]2 + H2O

Chromium(VI) halides are known also and include the hexafluoride CrF6 and chromyl
chloride (CrO2Cl2).[7]
Sodium chromate is produced industrially by the oxidative roasting of chromite ore with
calcium or sodium carbonate. The dominant species is therefore, by the law of mass action,
determined by the pH of the solution. The change in equilibrium is visible by a change from
yellow (chromate) to orange (dichromate), such as when an acid is added to a neutral solution
of potassium chromate. At yet lower pH values, further condensation to more complex
oxyanions of chromium is possible.
Both the chromate and dichromate anions are strong oxidizing reagents at low pH:[7]
Sodium chromate (Na2CrO4)Cr2O2-7 + 14 H3O++ 6 e 2 Cr3++ 21 H2O (0 = 1.33 V)
They are, however, only moderately oxidizing at high pH:[7]
CrO24 + 4 H2O + 3 e Cr(OH)3 + 5 OH(0 = 0.13 V)
Chromium(VI) compounds in solution can be detected by adding an acidic hydrogen
peroxide solution. The unstable dark blue chromium(VI) peroxide (CrO5) is formed, which
can be stabilized as an ether adduct CrO5OR2.
Chromic acid has the hypothetical formula H 2CrO4. It is a vaguely described chemical,
despite many well-defined chromates and dichromates being known. The dark red
chromium(VI) oxide CrO3, the acid anhydride of chromic acid, is sold industrially as
"chromic acid.It can be produced by mixing sulphuric acid with dichromate, and is a strong
oxidizing agent.
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.mto 300
p.p.m. To calculate the dilute solutions volume needed, the solution dilution formula can be
used:
M1V1=M2V2

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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 50,100, 150
,200,250 and 300 p.p.m.
V2: is a volume of volumetric flask

5.0

PROCEDURES
1. Using The formula , the initial volume of 300 ppm Chromium (VI) is calculated
2. Five Beaker is then labelled with 60 ppm , 120 ppm , 150 ppm , 210 ppm , 270 ppm
and 300 ppm respectively .
3. Chromium (VI) then pipette according to the volume calculated , using a formula
(M1V1=M2V2) .The Chromium (VI) was pipette into respective labelled beakers to
obtain the specific concentration of chromium (VI) .
4. Distilled water was added to the volumetric flask until it reach calibration mark
5. Therefore , five standard solution was prepared
6. Distilled water was put into cuvette of the spectrophotometer to calibrate 0.00
reading.
7. Next , spectrophotometer was left to continue the experiment with standard solution
Prepared .This procedures was proceed by placing the standard solutions with 60
ppm, 120 ppm , 150 ppm , 210 ppm , 270 ppm and 300 ppm inside the cuvette one at
the time .
8. The reading of absorbance of each solution that stated on spectrophotometer then
recorded.
9. Step 7 and 8 is repeated twice by using lake water sample
10. The average absorbance reading for water sample is calculated
11. The Beer-Lambert graph is then plotted .

6.0

APPARATUS AND MATERIALS

Material
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Standard solution of chromium (VI).


Distilled water
Diluted solution of chromium (VI).
Lake water sample
Apparatus
Spectrophotometer
10 ml of pipette
5 units 50 mL volumetric flask
10 mL square cuvette bottle

7.0

RESULTS

Table 1 :
ppm
0
60
120
150
210
270
300

Volume
0
4
8
10
14
18
20

Absorbance value
0
0.015
0.023
0.050
0.073
0.126
0.205

Lake water:0.144

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ABSORBANCE VALUE
0.25
0.2
ABSORBANCE VALUE
0.15

Linear (ABSORBANCE
VALUE)

0.1
0.05
0
0

50 100 150 200 250 300 350

Figure 1 shows Titration 1 curve of unknown acid neutralised by sodium hydroxide

8.0

SAMPLE OF CALCULATION

To dilute 10 millilitres standard solution of 1 p.p.m, the solution dilution formula is used in
order to calculate the volume of chromium (VI) solution.
(M1) (V1) = (M2) (V2).................... (1)
(300 ppm) (V1) = (60 ppm) (20 mL)
V1 = 4 mL
(300 ppm) (V1) = (120 ppm) (20 mL)
V1 = 8 mL
(300 ppm) (V1) = (150 ppm) (20 mL)
V1 = 10 mL
(300 ppm) (V1) = (210 ppm) (20 mL)
V1 = 14 mL
(300 ppm) (V1) = (270 ppm) (20 mL)
V1 = 18 mL
All the volumes of chromium (VI) solution needed to dilute each standard solution are stated
in Table 1.1.
By interpolating Graph 1.1, the equation of the linear line is given as;
y = 0.005 x + 0.004
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By substituting y with the average of absorbance value of water sample, which is 0.253,
hence we get that;
x

= y 0.004
0.005
= 0.253 0.004
0.005
= 49.8

Notice that x is equivalent to the concentration of Chromium (VI) contains in the water
sample, which is 49.8 parts per million.

9.0

DISCUSSION
This experiment is conducted to achieve a few objectives, which 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 solutions in the range of 1 to 100 parts per million (p.p.m) to be used in the
calibration of the spectrophotometer, and thus, to analyze whether the simulated lake water
sample tested is suitable for drinking water and agriculture purposes.
The lake water sample used to test for presence of chromium is believed to be
contaminated as the lake is situated near a roadway where road users with automobiles use it
every day. As mentioned before, 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.
According to the values of concentration of chromium (VI) which is apparently
calculated to contain 49.8 parts per million, this obviously means that there is a significant
content of chromium ions in the water. Based on the consideration of state and federal
regulatory agencies, natural waters are regarded to be toxic if the concentration of Chromium
(VI) is any higher than 0.100 parts per million. The lake water sample tested is then
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concluded to be unsafe and unhygienic for drinking water for public consumption or even
agricultural purposes.
However, a few steps might be done erroneously which results in such an outrageous
value of chromium (VI) content. First and foremost, the techniques applied to measure such a
small volume of diluting substance might not be suitable. This might lead to difficulties when
measuring the volume of chromium (VI) needed to dilute the standard solutions.
Besides that, wrong way of holding the square cuvette bottle used to contain the
diluted solutions might also lead to errors. Any fingerprints or smudge imprinted on the outer
surface of the cuvette can become an unfavourably interference for the solutions to absorb
wavelengths of light in the spectrophotometer. Thus, the reading of absorbance by the
instruments may not be accurate.
In addition, the experiment conducted to determine the absorbance value of diluted
solutions that contain chromium (VI) is done only once. Thus, no average value can be
obtained from the results, and so the accuracy of the value taken is not much convincing.
Others, the square cuvette bottle might not be cleansed properly with distilled water
each time before it is used for another attempt. This will lead to inaccurate contents of either
standard solutions or the chromium solution.
In determine the unknown acid there are two part of the experiment conducted .When
graph plotted the equivalence point can be obtained. Then, Ka value can be determined for
determination of unknown acid used. After giving a lot of thoughts, we determined the acid
using the table for Ka acid shows the unknown acid for part 1 is similar to propanoic acid and
for part 2 is oxalic acid
For part 1 ,The uknown acid Kas value is 110 -5 while the Ka value for propanoic
acid which merely different 1.34 10-5.Then the pKa value for the unknown acid is 5
whereas the pKa value for the propanoic acid is 4.87 . For part 2 , The Ka value for part
The main objective of the experiment is to determine the Ka value of the unknown acid so as
to identify the acid.However, an percentage error of Ka value and pKa value are 25.37 and
2.67 percents

after comparing the theoretical value with the experimental value is

obtained.As for half voume method the percentage error is 16.9%


Therefore, a few mistakes that must be considered when conducting the experiments
may be the reasons that lead to the error in calculations.
Firstly, the equivalence point is not necessarily being at pH of 7 as it occurs just when
the concentration of acid is equal to the concentration of base reacted in solution. Therefore,
the final pH depends on the major species of ions left in the solution after the reaction.
Then , the pH meter that might dindt give the definite readings, as the values that are
shown are always changing rapidly. Thus, one cannot tell the accurate readings of pH values.

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Therefore, these will also affect the titration curves as well as pKa values which correspond
to the pH values at half equivalence point.

10.0 CONCLUSION
The concentration of Chromium (VI) in the lake water sample tested is 49.8 parts per
million. Since it is more than 0.100 parts per million as what has been standardized by state
and federal regulatory agencies, the water sample is concluded to be contaminated and thus,
not suitable for drinking or agricultural purposes.
The experimental value for Ka value and pKa value are 110-5 and 5 respectively
.Furthermore , the theoretically Ka value and pKa value for the unknown acid which is
propanoic acid are 1.34 10-5 and 4.87 respectively .Therefore , the percentage of error for
Ka value is 26.37 % . while pKa is 2.67% . There is only a slight difference from the
theoretical value compared to experimental value.Therefore the unknown acid is identified as
propanoic acid.

11.0

RECCOMENDATION

1.In order to get more accurate values, a few recommendations and


precautions must be considered when performing the experiment.
2.Firstly, in this experiment, selection of wavelength value of light in the
spectrophotometer is quite essential. To get an ideal value, it is preferably to
use a wavelength where the component absorbs substantially.
3.Next, avoid leaving a fingerprints or any kind of smudge on the outer
surface which will corrupt the reading of absorbance value of
spectrophotometer.
4.Besides that, the determination of the absorbance value of each diluted
solutions must be done at least 3 trials. By doing so, more accurate values
can be obtained.

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5.Likewise, the square cuvette bottle must be cleansed thoroughly and


properly.

12.0 REFFERENCE AND APPENDIX


[1] https://www.scribd.com/doc/39166236/Determination-of-Chromium-VIConcentration-via-Absorption-Spectroscopy-Experiment

[2] http://chemistry.about.com/od/analyticalchemistry/a/spectroscopy.htm
[3] Laboratory manual CHE 485-Engineering Chemistry Lab, Universiti Teknologi Mara
[4] https://www3.epa.gov/airtoxics/hlthef/chromium.html

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