Experiment 2 Uv-Visible Determination of An Unknown Concentration of Kmno Solution

EXPERIMENT 2
UV-VISIBLE DETERMINATION OF AN UNKNOWN CONCENTRATION OF KMnO 4 SOLUTION
Objectives
 To determine the maximum wavelength of potassium permanganate.

 To plot the calibration curve of potassium permanganate.
 To determine the concentration of an unknown solution of potassium permanganate.
Apparatus
 Beaker
 Burette
 Glass rod
 Volumetric flask 100 mL
 Dropper
Chemicals
 Potassium permanganate (KMnO4)

 Distilled water
Procedure
A. Preparation of the KMnO4 Standard Solutions
1. 0.01 g of KMnO4 was weighed to the nearest mg, on a weighing paper. The readings had
recorded. The solid was transferred to a 100 mL volumetric flask by using a funnel.
2. The solid was dissolved with a few mL of distilled water. Stopper and shaken. Distilled
water was added to the mark, using a medicine dropper to add the last few drops. The
flask stopper and had shaken several times to homogenize the solution.
3. The ‘stock’ solution had poured into a beaker labelled as ‘100 ppm’
4. The ‘stock’ solution had pipetted and diluted with distilled water in a 100 mL volumetric
flask.
5. The ‘stock’ solution had transferred into a beaker and labelled as ‘5 ppm’
6. Step 4 had repeated with 10 mL,15 mL and 20 mL stock solution and transfer into small
beakers.
7. The beaker had labelled as ‘10 ppm’, ’15 ppm’ and ’20 ppm’ respectively.
B. Preparation of the Unknown
1. The ‘stock’ KMnO4 solution had pipetted between 5.00 mL to 20.0 mL and diluted with
distilled water in a 100 mL volumetric flask.
2. The solution then had transferred into a beaker and labelled as ‘Unknown’
C. Operation of the UV-Vis Spectrophotometer
Instrument : Varian/Cary 50 Uv-Vis Spectrophotometer
Operating Instructions
1. Cary Win UV icon had selected.
2. ‘Scan’ had clicked.
3. Setup is chosen, the ‘CARY’ had clicked and then the required start and stop scan
wavelength (nm) is keyed in.
i. Y-mode (min = 0 and max = 1).
ii. X-mode = 800-200 nm
iii. Beam mode = Dual Beam
4. Cycle mode had selected if more than 1 cycle required.
5. “Scan Control Speed” is selected to fast.
6. ‘Baseline’ icon and check ‘Baseline Correction Function’ had clicked.
7. ‘Accessories 1’ is clicked and check on the Use Cell Charger cells had selected.
8. At the peak table option, maximum peak is selected.
9. In the Auto Store icon, ‘storage on (Prompt At Start)’ had set.
10. To save the method, go to the file and the scan method had saved.
11. The ‘BLANK’ cuvette solution had filled with distilled water.
12. The ‘BLANK’ cuvette solution is put and ‘Baseline’ had clicked.
13. The ‘BLANK’ cuvette had removed and the ‘SAMPLE’ cuvette is put.
14. ‘Start’ icon had clicked to start the measurement
D. Determination of the Unknown Concentration
1. The concentration icon had clicked.
2. Setup had chosen, Cary icon clicked, then maximum wavelength, max keyed in.
3. Replicate = 3 had selected.
4. ‘Standard’ icon had clicked, the ‘Calibrate During Run’ function checked.
5. The calibration standard unit (mg/L) and the number of the standard samples had set.
6. The Fit Type (Linear Direct) had selected.
7. Sample icon had chosen, the number of the samples had selected and the unknown key in.
8. Report icon had clicked, operator name and the comment key in.
9. In the Auto Store icon, ‘Storage on (Prompt at start)’ had set.
10. To save the method, ‘File Save Method As Ok’ had clicked.
11. The ‘BLANK’ cuvette had put and ‘Zero’ clicked.
12. The ‘BLANK’ cuvette had removed and the ‘SAMPLE’ cuvette put in.
13. ‘Start’ icon is clicked to start the concentration measurements.
Result
Table 2.1 : Table of Concentration and Absorbance
Solution Concentration(ppm) Absorbance

Standard 1 5 0.0785
Standard 2 10 0.1558
Unknown ? 0.1443
Mass of KMnO4 = 0.0102 g
λmax =525.40 nm
Show the sample calculation for the preparation of standard 3.
M1V1= M2V2
(100 ppm)(V1)= (15 ppm)(100 mL)
V1= (15 ppm)(100 mL) / (100 ppm)
V1 = 15 mL
Concentration of unknown: 9.6053 ppm
Questions
1.Why is glass not a suitable cell material for use in UV spectroscopy ?
Glass is not a suitable cell material for use in UV spectroscopy because the glass will absorb
some of the UV light and will cause result to be not accurate for the experiment as the reading
will be higher than the exact one.
2.State one advantage of using the UV-Vis Spectrophotometer compared to a Spectronic 20 for
this analysis.
Advantage of UV-Vis Spectrophotometer’ is over the Spectronic 20 is that the scanning
spectrophotometer can rapidly scan a range of wavelengths and record absorbances at each
wavelength while Spectronic 20 is only well suited for quantitative absorption measurements at
a single wavelength.
Discussion
For this experiment, the stock solution was prepared by using 5 mL (5 ppm),10 mL (10
ppm),15 mL (15 ppm) and 20 mL (20 ppm) respectively. Then,10.0 mL of ‘stock’ KMnO 4 solution
had pipetted and diluted with distilled water in a 100 mL volumetric flask and labelled as
‘Unknown’. Then, the absorption maximum (λ max) had determined to be 525.40 nm by using
UV-Vis spectrophotometer. Next,the concentration of the unknown had determined by putting
the solution into a cuvette until ¾ full and must be wiped with kimwipe properly so that no
fingerprint will attached to the cuvette and disrupting the concentration determination right
before going into UV-Vis spectrophotometer.
A spectrometers are a devices that are used to measure the spectra of samples.A
spectrophotometer is a type of spectrometers which used to measures ultraviolet,visible and
near infrared light either reflected from or transmitted through a sample. System focuses
electromagnetic energy from the light onto material sample. Light will be either reflected off
the sample or transmitted through it. The sample will interact with light, it is focused onto the
entrance slit of the monochromator that will separate the light by wavelength using a
dispersing element. Commonly, optical grating was used. Next, it will be focus onto CCD
detector which is made up of thousands of individual light detectors to measure the intensity of
light at each wavelength. The CCD read-off to a computer resulting to spectrum which show the
intensity of each wavelength of light.
UV spectrophotometer principle follows the Beer-Lambert Law. Obeying this law, if a beam of
monochromatic light passes through a solution with absorbing substance, the decreasing rate
of the radiation intensity along with the thickness of the absorbing solution is proportional to
the concentration of the solution and the incident radiation.
A = log (I0/I) = ECI
A= Absorbance
I0=Intensity of light upon a sample cell
l = Intensity of light departing the sample cell
C = Concentration of the solute
L= Length of the sample cell
E = Molar absorptivity
According Beer-Lambert Law state that greater the number of the molecules that are capable of
absorbing light at a certain wavelength means the greater the extent of the absorption of light.
Conclusion
In conclusion, the maximum wavelength of potassium permanganate is determined to be
525.40 nm. Besides, the calibration curve of potassium permanganate was plot. Moreover,the
concentration of an unknown solution of potassium permanganate to be 9.6053 ppm.
References
 Martin, P. (n.d.). UV-visible-NIR Spectrophotometry. Retrieved from
http://www.microspectra.com/technical-support/248-spectrophotometer-design.
 Libretexts. (2019, September 30). Spectrophotometry. Retrieved from

https://chem.libretexts.org/Bookshelves/Physical_and_Theoretical_Chemistry_Textboo
k_Maps/Supplemental_Modules_(Physical_and_Theoretical_Chemistry)/Kinetics/Reacti
on_Rates/Experimental_Determination_of_Kinetcs/Spectrophotometry.
 Choudhary, A. (2018, September 7). The principle of Ultra Violet (UV)

Spectrophotometer. Retrieved from https://medium.com/@ankur1857/principle-of-
ultra-violet-uv-spectrophotometer-e6a1c435d258.

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EXPERIMENT 2

UV-VISIBLE DETERMINATION OF AN UNKNOWN CONCENTRATION OF KMnO 4 SOLUTION

 To determine the maximum wavelength of potassium permanganate.

 Potassium permanganate (KMnO4)

Solution Concentration(ppm) Absorbance

 Libretexts. (2019, September 30). Spectrophotometry. Retrieved from

 Choudhary, A. (2018, September 7). The principle of Ultra Violet (UV)

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