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APPLIED CHEMISTRY LABORATORY (BEP 1021)

NO. OF EXPERIMENT: 3
TITLE OF EXPERIMENT: Determination of Concentration of Potassium
Dichromate Solution by UV-VIS Absorption Spectroscopy
NAME: Arrianna Paulina Peter
ID: 1002162633
GROUP: 2
DATE OF EXPERIMENT: 17 Jan 2023
TUTOR: Ms. RAFIZAH BINTI ZAITON

SCHOOL OF ENGINEERING
FACULTY OF ENGINEERING, TECHNOLOGY & BUILT
ENVIRONMENT

2023
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Table of Contents

No. Topic Page(s)


1. Objective 3

2. Problem statement 3

3. Introduction 3-4

4. Hypothesis 4

5. Apparatus and materials 4

6. Procedure 4-7

7. Results and calculations 7-9

8. Discussion 9 - 10

9. Limitations/ Safety precautions 10 - 11

10. Conclusion 11

11. Reference 11– 12

12. Appendix 13 - 14

13. Rubric 15 - 18

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Experiment 3: Determination of Concentration of Potassium Dichromate Solution by UV-VIS
Absorption Spectroscopy

Objectives:

1. To determine the wavelength of maximum absorbance, λ max a potassium dichromate


solution.
2. To determine the wavelength of absorbance for each of the potassium dichromate solutions.
3. To examine the relationship between the absorbance and concentration of potassium
dichromate solutions
4. To prepare and run a standard calibration curve and determine the concentration of an
unknown potassium dichromate solution.

Problem Statement:

1. What is the relationship between the absorbance and the concentration of potassium
dichromate solutions?
2. How do you determine the concentration of an unknown solution using UV-VIS
spectroscopy?

Introduction:

For the following experiment, we will determine the concentration of potassium dichromate
solution by using UV-VIS absorption spectroscopy. UV-VIS absorption spectroscopy is an
instrument which uses light in visible and adjacent ranges. The function of this instrument is
relatively straightforward. The absorption in the visible range directly affects the perceived colour
of the chemicals involved which is dichromate ion, Cr 2O7 2-
which is orange in colour. The apsorp
spectrum of potassium dichromate is determined within the wavelengths with range of 200nm.
Molecules can absorb ultraviolet or visible light. This causes the absorption of a potassium
dichromate solution to increase as the attenuation of the beam to increase. Thus, it is said that the

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absorbance of a potassium dichromate solution is directly proportional to the cell path length, b and
the concentration, c of the absorbing species. This can be related to Beer’s law, in which it states
that: -

Log10 I0/ I = A = ε bc

Where I0 is the incident light intensity, A is the absorbance, b is the cell path length in cm, c is the
solution concentration in moles/liter, and ε is the molar absorptivity, which has units of
liter/mole/cm.
Different molecules absorb radiation of different wavelengths. An absorption spectrum will show
several absorption bands corresponding to the structural groups within the molecule. However, if
the sample compound does not absorb light of a given wavelength, thus, it will be said as I= I 0.
Nonetheless, if the sample compound absorbs light, I < I 0. This difference will be plotted on the
graph versus wavelength. Absorption may be presented as transmittance, where T= I/ I 0 or
absorbance, A=log I0/ I.

Hypothesis:

The higher the dichromate concentration, the higher the absorbance for each potassium dichromate
solution.

Apparatus and Materials:

Measuring cylinder, pipette, volumetric flask, beakers, distilled water, potassium dichromate
solution, unknown dichromate solution, UV-VIS curette, UV-VIS spectrophotometer.

Procedure:

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1. Stock solution of Potassium Dichromate (1000ppm) done by the laboratory tutor.
2. By using the equation of M1V1= M2V2, five standard solutions of Potassium Dichromate are
prepared as shown in the Table 1:
*Let M1= 1000ppm, M2= no. of concentration (ppm) [in the table]
V1= volume needs to be pipette, V2= 30mL

Table 1: Standard Solutions of Potassium Dichromate


Concentration (ppm) Volume needed to be pipettes Volume of water added (mL)
(mL)
100 3 10
200 6 13.33
300 9 15
400 12 16
500 15 15
Unknown

Using the formula, M1V1= M2V2, we can find the volume needed to be pipette (mL) for

500ppm 400ppm 300ppm 200ppm 100ppm

V1=
[ (500 )( 30 ) ] V1=
[ ( 400 ) ( 30 ) ] V = [ ( 300 )( 30 ) ] V = [ ( 200 )( 30 ) ] V = [ (100 )( 30 ) ]
1 1 1
1000 1000 1000 1000 1000
V1= 15mL V1= 12mL V1= 9mL V1= 6mL V1= 3mL

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Measurement by UV- VIS

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1. The absorbance of the standard solutions are be assured by using distilled water as blank. A
blank is first prepared by filling a cuvette ¾ full with distilled water.

2. The absorbance for each of the solutions in Table 1 are measured by placing them into the
colorimeter, aligning the reference marks, closing the lid and determine the wavelength of
the maximum absorbance (λmax) as well as their absorbances.
3. The results are then recorded in your spreadsheet. We need to make sure to include the
values of the wavelength at which you are making your measurements.
4. A graph is prepared by using Excel which then is needed to plot absorbance vs.
concentration. The equation of the best-fit line is obtained by setting the y-intercept to zero.
The correlation coefficient (r2) is needed to be determined in this linear regression equation.
(Think: why should y-intercept be set to zero? What does the slope represent in Beer’s
law?)

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5. A cuvette is filled about ¾ full of your unknown sample of potassium dichromate. The
unknown number is then recorded. The absorbance of the unknown is measured as before.
If the absorbance is greater than any of the measurements used to prepare your trendline,
dilute the solution and measure the absorbance again. The volume used in your dilution
needs to be taken note of.

Results and Calculations:

Wavelength of maximum absorbance (Apex, nm): 430nm

Dichromate concentration (ppm) Height (Absorbance, Abs)


100 0.173
200 0.313
300 0.482
400 0.633
500 0.780
Unknown 0.263

1. Draw the graph height (Absorbance, Abs) against dichromate concentration (ppm).
2. Find the concentration of unknown dichromate solution from the graph.

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Graph of Height (Abs) against Dichromate Concentration (ppm)
0.9

0.8
0.78
f(x) = 0.00155685714285714 x + 0.00761904761904764
R² = 0.99932829732088

0.7

0.633

0.6

0.5
0.482
Height (abs)

Height (abs)
Linear (Height (abs))

0.4

0.313
0.3

0.2
0.173

0.1

0 0
0 100 200 300 400 500 600

Dichromate Concentration (ppm)

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Concentration of unknown dichromate solution:

Y= 0.0016x + 0.0076

When Y= 0.263,
0.263= 0.0016x + 0.0076
0.263 – 0.0076
x=
0.0016
x= 159.625ppm

Discussion:

The aim of the experiment is to prepare and run a standard calibration curve and determine the
concentration of an unknown potassium dichromate solution. Five different concentration of
potassium dichromate solution is prepared and transferred to UV-VIS spectrophotometer to
determine the absorbance of the five different concentrations of potassium dichromate solution
including the unknown potassium dichromate solution concentration.

After obtaining the value of absorbance of all the given concentrations of potassium dichromate
solution, the graph of absorbance against concentration of potassium dichromate solution is then
plotted and the function of the graph is determined. The relationship between the absorbance and
the concentration of potassium dichromate solution is found out that absorbance is directly
proportional to the dichromate concentration.

The value of absorbance of unknown concentration of potassium dichromate solution is 0.263 Abs.
By using the function of the graph, y= 0.0016x + 0.0076, by substituting y= 0.263 Abs into the
function and the concentration of potassium dichromate solution is found out to be 159.625ppm.
Thus, we can say that our result is accurate. However, there may be some errors occurred
throughout the experiment.
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1. What is the Beer- Lamnert law?
The Beer- Lambert law, also known as Beer’s law, relates the attenuation of light to the properties
of the material through which the light travels. The law is commonly applied to the chemical
analysis measurements and is used in understanding attenuation in physical optics for photons,
neutrons or rarefied gases.

2. What is a blank? When is it recorded? Why is it recorded?


A blank solution is a solution that contains little to no analyse of interest which are usually used to
calibrate instruments like colorimeter. According to EPA, the ‘primary purpose of blanks is to trace
sources of artificially introduced contamination’. Different blanks are used to identify sources of
contamination in the sample. The type of blanks included equipment blank, field blank, trip blank,
method blank, and instrument blank. To measure the absorbance of a particular substance in a
reaction mixture, it is necessary to ‘zero out’ the spectrophotometer first so that the absorbance of
the substance of interest is measured. This is done with a blank, also known as a cuvette which
contains all carrier solvents except substance of interest. A separate blank is needed for every
unique reaction mixture. Formulation of the blank depends on the experiment and may involve the
use of dyes or other colorimetric indicators.

3. What is the typical energy range of light for UV-VIS spectroscopy?


The typical energy range of light for UV-VIS spectroscopy, ultraviolet region falls between the
range of 190 -380nm, the visible region falls between 380 -750nm.

Safety Precautions/ Limitations:

To minimise possible errors, we should always consider the following aspects of good sample
handling, which are: —

1. A pipette is needed to fill and empty the cuvettes.

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2. The optical surface of the cuvettes should be taken care of by not being dirty with
fingerprints or any other substances.
3. To verify the quality and cleanliness of the cuvettes used, a reference sample of air should
be measured, and a sample of the cuvette should be filled with distilled water before sample
measurement.
4. When using a conventional scanning spectrophotometer, the reference should be measured
in the same wavelength range as the sample measurements.
5. When carrying out the experiment, we are required to work
in the dark places or use foil to cover thecontainers or amber bottles to store the samplesolut
ions to avoid light exposure as it mayabsorbance or reflect the light and decompose
that sample.

Conclusion:

Spectroscopy is said to be an easy method to use to determine the concentration of an unknown


species due to their only needs which are molar absorptivity of the sample, the absorbance and the
cell path length to calculate the concentration of the analyse. The law used is called — Beer’s law
which governs the overall process of spectroscopy since it gives the relationship of the quantities
obtained for, spectophotometric data to identify the quantity of the unknown in the sample. The
absorbance can be directly measured from the spectrometer or can be derived from Beer’s law to
derive the transmittance of substance at certain wavelengths. Beer’s Law’s plot of Absorbance
(Abs) against the Concentration (ppm) shows that it is directly proportional. Thus, the hypothesis of
the experiment is said to be true.

Reference:

1. R. W. Burke and R. Mavrodineanu, (May 18, 1976), Journal of Research of the National
Bereau of Standards — A. Physics and Chemiss Vol, 80A, No.4 (online) Available at:

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<https://nvlpubs.nist.gov/nistpubs/jres/80a/jresv80an4p631_a1b.pdf > [Accessed 21 Jan
2023]

2. Starnia Scientific Limited, (2023), Potassium Dichromate (235-430nm) (online), Available


at: < https://www.starna.com/uv-absorbance/potassium-dichromate#description-and-
discussion> [Accessed 21 Jan 2023]

3. Agilent Technologies, (2000), Fundamentals of UV- visible spectroscopy (workbook)


(online), Available at: <https://www.agilent.com/cs/library/primers/Public/5980-
1398E.pdf#page71> [Accessed 21 Jan 2023]

4. A. M. Balaoing, J. B. Erlano, (2011), Experiment No. 6 Spectros (online) Available at:


<https://www.scribd.com/doc/75582500/Experiment-No-6-Spectroscopy> [Accessed 21 Jan
2023]

5. Jim Clark, (2007), UV-VIS Absorption Spectra (online), Available at: <
http://www.chemguide.co.uk/analysis/uvvisible/theory.html> [Accessed 22 Jan 2023]

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(Appendix) Raw Data:-

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UV-VIS readings: (height, Abs)

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