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UNIVERSITI TEKNOLOGI MARA

FAKULTI KEJURUTERAAN KIMIA


ENGINEERING CHEMISTRY LABORATORY
(CHE485)

NAME : NURLINA SYAHIIRAH BINTI MD TAHIR


STUDENT NO. : 2017632214
GROUP : EH2203J
EXPERIMENT : DETERMINATION OF CHROMIUM (VI)
CONCENTRATIONS VIA ABSORPTION
SPECTROSCOPY
DATE PERFORMED : 27TH OCTOBER 2017
SEMESTER :3
PROGRAMME / CODE : FACULTY OF CHEMICAL ENGINEERING
SUBMIT TO : SIR HANAFIAH ZAINAL ABIDIN

No. Title Allocated Marks (%) Marks


1 Abstract/Summary 5
2 Introduction 5
3 Aims 5
4 Theory 10
5 Apparatus 5
6 Methodology/Procedure 10
7 Results 10
8 Calculations 10
9 Discussion 20
10 Conclusion 5
11 Recommendations 5
12 Reference 5
13 Appendix 5
TOTAL MARKS 100

Remarks:

Checked by :

---------------------------

Date :
TABLE OF CONTENT

1.0 ABSTRACT ........................................................................................................................ 2


2.0 INTRODUCTION.............................................................................................................. 3
3.0 OBJECTIVES .................................................................................................................... 4
4.0 THEORY ............................................................................................................................ 5
5.0 MATERIALS & APPARATUS ........................................................................................ 7
6.0 METHODOLOGY ............................................................................................................ 8
7.0 RESULTS ........................................................................................................................... 9
8.0 SAMPLE OF CALCULATIONS ................................................................................... 10
9.0 DISCUSSION ................................................................................................................... 12
10.0 CONCLUSION .............................................................................................................. 14
11.0 RECOMMENDATIONS ............................................................................................... 15
12.0 REFERENCES ............................................................................................................... 16
13.0 APPENDIX ..................................................................................................................... 17

Lab Report on Determination of The Chromium (VI) Concentrations Via Absorption Spectroscopy 1
1.0 ABSTRACT

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. Natural
waters whose Cr (VI) concentrations exceed 0.100 ppm may not be used for drinking water
or for agricultural purposes. The objective of the experiment is to determine whether the lake
water sample suitable for drinking and agricultural purposes by comparing the quantity of
Chromium (VI) present in a polluted water sample using a spectrophotometer and a set of
standard Chromium (VI) solutions. The standards Chromium (VI) solutions is prepared at
concentration 15ppm, 30pmm, 60ppm, 75ppm, 100ppm and 300ppm by diluting 300ppm
Chromium (IV) solutions with distilled water and the absorbance value for the standard
solutions is 0.030, 0.048, 0.056, 0.066, 0.073 and 0.159 respectively. The lake water sample
is taken at lake located in Seksyen 7, Shah Alam, Selangor with average absorbance value of
0.148. The concentration of chromium (VI) in the lake water sample is estimate of about
274.4186ppm using Data Interpolation method and 294.25ppm using the Linear Graph
Equation. The percentage difference between the two method approximately 7%. The lake
water sample is not suitable for drinking and agricultural purposes due to high concentration
of Chromium (VI) which passes the 0.1ppm standard by EPA and 0.05ppm standard by the
Ministry of Health Malaysia. The objectives are successfully obtained, therefore the
experiment is successfully done.

Lab Report on Determination of The Chromium (VI) Concentrations Via Absorption Spectroscopy 2
2.0 INTRODUCTION

Many heavy metals, such as chromium, are undeniably toxic at low aqueous solution
concentrations. Chromium ions are commonly found in either trivalent, Cr (III), or
hexavalent, Cr (VI) states. 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. 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. State and federal regulatory agencies consider Cr (VI) to be toxic at
concentration level more than 0.100 ppm. Natural waters whose Cr (VI) concentrations
exceed 0.100 ppm may not be used for drinking water or for agricultural purposes. Therefore,
it is important to take note about the level of Cr (VI) concentrations in water sources. If it
does not exceed 0.100 ppm then it is eligible to be consumed as for drinking water and
agricultural purposes.

In this experiment, we had determined the concentration of chromium (VI) via


absorption spectroscopy to conclude whether the water sample is suitable for drinking or
agricultural process. Spectroscopy pertains to the interactions of radiation and matter. It
basically aims to measure the amount of radiation emitted or absorbed by a molecular or
anatomic species. It is particularly useful in the determination of concentration of elements in
alloy steel so as to predict its mechanical properties and resistance to corrosion. Spectroscopy
can be comprise any interaction of radiated energy as function of its wavelength.

In terms of environmental effects, chromium enters air, water and soil in the form of
Cr (III) and Cr (VI). Various activities that human had been done that increase the
concentration of chromium such as, chemical, textile and leather manufacturing, electro
painting. Quantity of Cr (VI) present in polluted water sample will be detect using a
spectrophotometer and a standard solutions. From this we can conclude whether the sample
is suitable for drinking and agricultural purposes.

Lab Report on Determination of The Chromium (VI) Concentrations Via Absorption Spectroscopy 3
3.0 OBJECTIVES

1) To determine whether the lake water sample suitable for drinking and agricultural
purposes.
2) To determine the absorbance value for the prepared standard Chromium (VI) solutions
and the lake water sample via absorption spectroscopy.
3) To compare the absorbance value between the lake water sample and the standard
Chromium (VI) solutions.
4) To determine the concentration of Chromium (VI) present in the lake water sample.
5) To plot graph of the absorbance value against the concentration of the standard solution.

Lab Report on Determination of The Chromium (VI) Concentrations Via Absorption Spectroscopy 4
4.0 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).

The main human activities that increase Chromium (VI) concentrations are chemical,
leather and textile manufacturing, electro painting and other Chromium (VI) applications in
the industry. Automobiles industries is also one of the common source of chromium
contamination in natural waters as it is contain a component in various automobile brakes as
well as parts of engine. Chromium that is deposited on highroads originated from brake dusts
and exhaust of automobile engine can unfavorably permeate into any water streams nearby
via flowing rainwater. Therefore, lakes and water streams which are 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, 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 low level
concentrations of Chromium (VI) in a lake water sample. Theoretically, colored aqueous
solutions have chemical species contents which absorb significant wavelengths of light.
Similarly, heavy metals can be identified via absorption of wavelengths of light. Furthermore,
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 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

Lab Report on Determination of The Chromium (VI) Concentrations Via Absorption Spectroscopy 5
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 parts per million
(ppm) of Chromium (VI) standard solution. Five standard solutions need to be prepared from
the concentrated Chromium (VI) standard solution. To calculate the dilute solutions volume,
the solution dilution formula can be used, as what is written below:

Where;
M1: concentration of given Chromium (IV) stock solution = 300ppm
V1: Volume of Chromium (IV) solution required to perform dilution
M2: Concentration of Chromium (IV) solution after dilution
V2: Volume of Chromium (IV) solution after dilution

Quantitative analysis using spectrophotometer is based on Beer-Lambert Law:

Where;
A: absorbance value (dimensionless, thus no units is represented)
ɛ: molar absorbance (L / mol.cm)
L: path length of the cuvette in which the sample is contained (cm)
C: 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, ɛ, 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 with the
appropriate wavelength, hence the low concentrations of a compound with a high molar
absorbance can be easily detected.

Lab Report on Determination of The Chromium (VI) Concentrations Via Absorption Spectroscopy 6
5.0 MATERIALS & APPARATUS

5.1) Material
1) 300ppm Chromium (VI) Solutions
2) Distilled Water
3) Lake Water Sample from a lake located at Seksyen 7, Shah Alam, Selangor.

5.2) Apparatus
1) Spectrophotometer
2) 10mL Square Cuvette Bottles
3) 5mL Volumetric pipette
4) 20mL Volumetric flask with Lid

Lab Report on Determination of The Chromium (VI) Concentrations Via Absorption Spectroscopy 7
6.0 METHODOLOGY

6.1) Preparation Of Standard Chromium Solutions

1) The volume of 300ppm Chromium (VI) solution needed to dilute the concentration to
15ppm is calculated.
2) The result is then tabulated in Table 1.
3) The 1mL of 300ppm Chromium (VI) solution is then measured using volumetric pipette
and put into 20mL volumetric flask.
4) About 19mL of distilled water is then poured into the 20mL conical flask to get the
volume of 20mL as the size of the volumetric flask and to prepared the 15ppm Chromium
(VI) solutions. Then, the volumetric flask is closed with a lid to prevent interaction with
the air.
5) Step 1 until 3 is repeated for 2mL, 4mL, 5mL, 6.67mL and 20mL of Chromium (VI)
solutions to prepare 30ppm, 60ppm, 75ppm, 100ppm and 300ppm of Chromium (VI)
solutions with addition of 18mL, 16mL, 15mL, 13.33mL and 0mL of distilled water
respectively.

6.2) Determination Of Absorbance Value Using Spectrophotometer

1) The 10mL cuvette bottle is filled with 10mL of distilled water as blank sample and placed
in the spectrophotometer slot. A zeroing step was done to ensure that all data obtained is
accurate.
2) The six standard Chromium (VI) solutions is then measured for their respective
absorbance value tabulated in Table 1.
3) The graph of the standard Absorbance value versus concentration of Chromium (VI)
Solutions is then plotted.
4) The 10mL cuvette bottle is filled with 10mL of lake water sample and placed in the
spectrophotometer slot. The absorbance value is then measured.
5) Step 4 is repeated for another two times to get the average absorbance value to ensure
accurateness and consistency of data.

Lab Report on Determination of The Chromium (VI) Concentrations Via Absorption Spectroscopy 8
7.0 RESULTS

Table 1 – Determination Absorbance Value For Standard Solutions Using Spectrometer


Concentration Volume of Chromium (VI) Volume of Distilled Absorbance
(ppm) (mL) Water (mL)
15 1.00 19.00 0.030
30 2.00 18.00 0.048
60 4.00 16.00 0.056
75 5.00 15.00 0.066
100 6.67 13.33 0.073
300 20.00 0.00 0.159

Table 2 – Average Absorbance Value For Lake Water Sample


Lake Water Sample Absorbance
Trial 1 0.151
Trial 2 0.149
Trial 3 0.145
Average Values of Trials 0.148

Lab Report on Determination of The Chromium (VI) Concentrations Via Absorption Spectroscopy 9
8.0 SAMPLE OF CALCULATIONS

Sample Calculation For Preparing Standard Chromium (Cr) Solutions :-

( ) ( )
( )

Sample Calculation For Concentration Of Chromium (VI) by Data Interpolation :-

( )( )

( )( )
(Experimental Value)

Where, xi = Absorbance Value at the wanted value


xo = Absorbance value before the wanted value
xi+1 = Absorbance value after the wanted value
Ci = Concentration of Chromium (VI) at the wanted value
Co = Concentration of Chromium (VI) before the wanted value
Ci+1 = Concentration of Chromium (VI) after the wanted value

Sample Calculation For Concentration Of Chromium (VI) by Linear Graph Equation :-

(Theory Value)

Where, x = Concentration of Chromium (VI) at the wanted value


y = Absorbance value at the wanted value

Lab Report on Determination of The Chromium (VI) Concentrations Via Absorption Spectroscopy 10
Sample Calculation For Percentage Error :-

( ) | |

( ) | |

( )

Where, x1 = Concentration of Chromium (VI) in Lake Water Sample (Interpolation)


x2 = Concentration of Chromium (VI) in Lake Water Sample (Graph Equation)

Lab Report on Determination of The Chromium (VI) Concentrations Via Absorption Spectroscopy 11
9.0 DISCUSSION

The objective of the experiment is to determine whether the lake water sample suitable for
drinking and agricultural purposes by comparing the quantity of Chromium (VI) present in a
polluted water sample using a spectrophotometer and a set of standard Chromium (VI)
solutions. Distilled water is used to dilute the Chromium (VI) in order to get a set of standard
solutions. The lake water sample is obtained from a Lake located at Seksyen 7, Shah Alam,
Selangor.

Concentration Of Chromium (IV) versus Absorbance


0.18
0.16
0.14
Absorbance Value

0.12
0.1 y = 0.0004x + 0.0303
0.08 Absorbance
0.06 Linear (Absorbance)
0.04
0.02
0
0 100 200 300 400
Concentration Of Chromium (IV), ppm

Figure 1 - Graph Of Concentration Of Chromium (IV) versus Absorbance Rate

The graph shows as the concentration of Chromium (VI) increases, the absorbance
value also increases. Based on the results obtained, the average value for absorbance for Lake
Water Sample is 0.148. In order to compare the amount of Chromium (VI) exist in the Lake
Water Sample, the data obtained for the absorbance value at particular concentration of
Chromium (VI) is interpolated using data from Table 1 to get the exact concentration of
Chromium present in the Lake Water Sample. Assuming that the only heavy metal present in
the Lake Water Sample is Chromium (VI), the concentration of the heavy metal is about
274.4186ppm by using Data Interpolation method. Linear Graph Equation method yields the
theoretical value for the concentration of Chromium (VI) in the Lake water sample which is
294.25ppm. Thus, comparing both value the percentage error is about 7% and acceptable
since the error is small.

Lab Report on Determination of The Chromium (VI) Concentrations Via Absorption Spectroscopy 12
For the calculation to determine the experimental value of the concentration of the
Chromium (VI) in the Lake Water sample, the student used Data Interpolation method due to
the fact that lacking of data concerning the Beer Lambert Law such that the path length of the
cuvette in which the sample is contained and the molar absorbance.

Agricultural water is water that is used to grow fresh produce and sustain livestock.
The use of agricultural water makes it possible to grow fruits and vegetables and raise
livestock, which is a main part of our diet. (Agricultural Water, 2016) The presences of heavy
metals in drinking water could lead to many health risks such that reduced growth and
development, cancer, organ damage, nervous system damage and in extreme cases, death.
(Water)

EPA has put a standard for drinking water of 0.10 mg/L or 0.10 ppm for total
chromium present in the water. (EPA) The maximum allowed concentration for total
chromium is about 0.05mg/L or 0.05ppm for drinking water according to Engineering
Services Division, Ministry Of Health Malaysia. Therefore, EPA only allows for about
0.1ppm of total chromium to be present in drinking water while Ministry of Health Malaysia
lower which is 0.05ppm. (Engineering Services Division) However, if compared to the result,
the concentration of chromium (VI) is about 2744 and 5480 times the allowed standards
respectively based on Data Interpolation method. Thus, the Lake Water sample is really not
suitable for drinking and need further process to remove the heavy metals before humans or
animal can consume the water.

Lab Report on Determination of The Chromium (VI) Concentrations Via Absorption Spectroscopy 13
10.0 CONCLUSION

The standard Chromium (VI) solutions is successfully prepared at concentration 15ppm,


30ppm, 60ppm, 75ppm, 100ppm and 300ppm with absorbance value of is 0.030, 0.048,
0.056, 0.066, 0.073 and 0.159 respectively. The graph of the absorbance value against the
concentration of the standard solution is successfully plotted. The absorbance value of the
lake water sample is successfully obtained of 0.151, 0.149 and 0.145 with average value of
0.148. The absorbance value between standard Chromium (VI) solutions and Lake Water
Sample is compared and yield the experimental value for the Chromium (VI) concentration.
The theoretical and experimental value of the Chromium (VI) concentration in the Lake
Water Sample are 294.25ppm and 274.4186ppm respectively which yields the percentage
error of about 7%. Based on EPA’s and Engineering Division, Ministry of Health Malaysia’s
standard, the lake water sample is not suitable to use for drinking and agricultural purposes
due to the very high concentration of Chromium (VI) in the water sample. The objectives are
successfully obtained, therefore the experiment is successfully done.

Lab Report on Determination of The Chromium (VI) Concentrations Via Absorption Spectroscopy 14
11.0 RECOMMENDATIONS

Students should read and research more about the experiment before conducting the
experiment. This is to ensure the students able to conduct the experiment smoothly and
within the allocated time limit without facing confusion about the next step during the
experiment. Preparation for the data table should be done before the experiment to avoid
confusion and all the data for the experiment get to be recorded for the report.

The students should properly learn how to handle instrument and apparatus. As for the
experiment, the students having a difficulties in using the 5mL volumetric flask due to the big
size of the instrument. Besides, the square cuvette bottle must be cleaned and dried properly
using the specified tissue provided in the lab.

The eye of the students should be parallel to the 10mL line mark at cuvette bottle in
order to avoid parallax error from occurring. Since this could lead to inaccurate absorbance
value obtained from the spectrophotometer.

The students should wear complete PPE such as gloves, goggles, face mask, covered
shoes and lab coat throughout the experiment to ensure the safety of the students. The
students should consistent in calculating the data. For example, the readings or the calculated
data should be in four decimal places.

Lab Report on Determination of The Chromium (VI) Concentrations Via Absorption Spectroscopy 15
12.0 REFERENCES

Agricultural Water. (2016, October 11). Retrieved November 8, 2017, from Centers For
Disease Control & Prevention:
https://www.cdc.gov/healthywater/other/agricultural/index.html

Determination Of Concentration Of Chromium. (n.d.). Retrieved November 9, 2017, from


Scribd: http://www.scribd.com/doc/110293635

Engineering Services Division, M. O. (n.d.). Drinking Water Quality Standard. Retrieved


November 6, 2017, from Drinking Water Quality Surveillance Programme,
Engineering Services Division, Ministry Of Health Malaysia:
http://kmam.moh.gov.my/public-user/drinking-water-quality-standard.html

EPA. (n.d.). Chromium in Drinking Water. Retrieved November 6, 2017, from United States
Environmental Protection Agency:
http://www.epa.gov/dwstandardsregulations/chromium-drinking-water

Lab Manual. (n.d.). Retrieved October 6, 2017, from http://i-learn.uitm.edu.my/

Water, A. (n.d.). Health Risks Of Heavy Metals. Retrieved November 6, 2017, from APEC
WATER: http://www.freedrinkingwater.com/water-education/quality-water-
heavymeatal.html

Lab Report on Determination of The Chromium (VI) Concentrations Via Absorption Spectroscopy 16
13.0 APPENDIX

Figure 2 - Spectrophotometer used in The Experiment

Figure 3 - Fume Cupboard used To reduce the interaction of the Chromium (VI) solutions
interaction with air

Lab Report on Determination of The Chromium (VI) Concentrations Via Absorption Spectroscopy 17
Figure 5 - The prepared standard Chromium (VI) solutions inside 10mL volumetric flasks

Figure 4 - The standard Chromium (VI) solutions inside 10mL cuvette bottle before
entering the spectrophotometer

Lab Report on Determination of The Chromium (VI) Concentrations Via Absorption Spectroscopy 18
Figure 6 - The Lake Water Sample in 10mL Cuvette Botle before entering the
spectrophotometer

Lab Report on Determination of The Chromium (VI) Concentrations Via Absorption Spectroscopy 19
Table 2 – Engineering Division, Ministry of Health Malaysia Drinking Water Quality
Standard

DRINKING
RECOMMENDED
WATER
RAW WATER
QUALITY
QUALITY
STANDARDS
Parameter Group
Maximum
Acceptable Value
Acceptable Value
(mg/litre (unless
(mg/litre (unless
otherwise stated))
otherwise stated))
Total Coliform 1 5000 MPN / 100 ml 0 in 100 ml
E.coli 1 5000 MPN / 100 m 0 in 100 m
Turbidity 1 1000 NTU 5 NTU
Color 1 300 TCU 15 TCU
pH 1 5.5 - 9.0 6.5 - 9.0
Free Residual Chlorine 1 - 0.2 - 5.0
Combined Chlorine 1 - Not Less Than 1.0
Temperature 1 - -
Clostridium perfringens (including
1 - Absent
spores)
Coliform bacteria 1 - -
Colony count 22° 1 - -
Conductivity 1 - -
Enterococci 1 - -
Odour 1 - -
Taste 1 - -
Oxidisability 1 - -
Total Dissolved Solids 2 1500 1000
Chloride 2 250 250
Ammonia 2 1.5 1.5
Nitrat 2 10 10
Ferum/Iron 2 1.0 0.3
Fluoride 2 1.5 0.4 - 0.6
Hardness 2 500 500
Aluminium 2 - 0.2
Manganese 2 0.2 0.1
Chemical Oxygen Demand 2 10 -
Anionic Detergent MBAS 2 1.0 1.0
Biological Oxygen Demand 2 6 -
Nitrite 2 - -
Total organic carbon (TOC) 2 - -

Lab Report on Determination of The Chromium (VI) Concentrations Via Absorption Spectroscopy 20
Mercury 3 0.001 0.001
Cadmium 3 0.003 0.003
Arsenic 3 0.01 0.01
Cyanide 3 0.07 0.07
Plumbum/Lead 3 0.05 0.01
Chromium 3 0.05 0.05
Cuprum/Copper 3 1.0 1.0
Zinc 3 3 3
Natrium/Sodium 3 200 200
Sulphate 3 250 250
Selenium 3 0.01 0.01
Argentum 3 0.05 0.05
Magnesium 3 150 150
Mineral Oil 3 0.3 0.3
Chloroform 3 - 0.2
Bromoform 3 - 0.1
Dibromoklorometana 3 - 0.1
Bromodiklorometana 3 - 0.06
Fenol/Phenol 3 0.002 0.002
Antimony 3 - 0.005
Nickel 3 - 0.02
Dibromoacetonitrile 3 - 0.1
Dichloroacetic acid 3 - 0.05
Dichloroacetonitrile 3 - 0.09
Trichloroacetic acid 3 - 0.1
Trichloroacetonitrile 3 - 0.001
Trihalomethanes - Total 3 - 1.00
Aldrin / Dealdrin 4 0.00003 0.00003
DDT 4 0.002 0.002
Heptachlor & Heptachlor Epoxide 4 0.00003 0.00003
Methoxychlor 4 0.02 0.02
Lindane 4 0.002 0.002
Chlordane 4 0.0002 0.0002
Endosulfan 4 0.03 0.03
Hexachlorobenzena 4 0.001 0.001
1,2-dichloroethane 4 - 0.03
2,4,5-T 4 - 0.009
2,4,6-trichlorophenol 4 - 0.2
2,4-D 4 0.03 0.03
2,4-DB 4 - 0.09

Lab Report on Determination of The Chromium (VI) Concentrations Via Absorption Spectroscopy 21

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