UV/VIS SPECTROSCOPY AND SPECTROPHOTOMETRY

LABORATORY REPORT

NUMBER OF EXPERIMENT: 1

TITLE OF EXPERIMENT: SPECTROPHOTOMETRIC ANALYSIS OF POTASSIUM

PERMANGANATE SOLUTIONS

NAME OF GROUP: VANESSA AIMEE C. ALECHA

MA. SHEENA C. HIZOLE

JULIE M. MORABE

JESTONI B. SALINAS

JEROME L. DEPOL

LESTE GRACE A. SINAHON

LECTURE’S NAME: BRIAN JOHN SANO

GROUP: 4
I. Introduction:

Spectrophotometric analysis is an essential and widely employed technique in both

academic and industrial laboratories for quantifying the concentration of analyses in solution.
This method hinges on the principle that molecules absorb light at specific wavelengths, with
amount of light absorbed correlating directly to the concentration of the absorbing species.
Among the myriad of substances analyzed through this technique, potassium permanganate
(KMnO4) stands out due to its distinct and intense violet coloration, which makes it particularly
suitable for spectrophotometric measurements.
Potassium permanganate is a strong oxidizing agent with widespread applications in
analytical chemistry, environmental testing, and medicine. Its strong absorbance spectrum,
specifically around 525 nm, allows for straightforward spectrophotometric analysis. This
characteristic wavelength is where KMnO4 exhibits maximum absorbance providing a reliable
means to determine in solution via Beer’s Law, which states that absorbance is directly
proportional to concentration and path length.
The process begins with the preparation of standard solutions of known concentration of
potassium permanganate. These standards are used to construct a calibration curve a crucial
step in quantitative spectrophotometric analysis. By plotting the absorbance values of these
standards against their respective concentrations, a linear relationship is typically established,
known as Beer’s Law plot. This calibration curve then serves as a reference for determining the
concentration of unknown potassium permanganate solutions.
To conduct analysis, the analysis, a spectrophotometer is employed. This instrument
measures the intensity of light before and after it passes through the sample solution. The
difference in light intensity is recorded as absorbance. Modern spectrophotometers, such as the
ability to scan across a range of wavelengths, which allows for the identification of the optimal
wavelength for analysis and the detection of `potential interfering substances.
Accurate spectrophotometric analysis of potassium permanganate solutions necessitates
careful consideration of several factors. First, the preparation of the sample and standards must
be meticulous to avoid contamination and ensure consistency. The use of high-purity reagents
and precise dilution techniques is paramount. Second, the instrument must be correctly
calibrated, and baseline measurements must be correctly calibrated, baseline measurements
must be taken to account for any instrumental noise or drift. Third, the path length of the
cuvette, typically 1 cm, should be consistent across all measurements to adhere Beer’s Law.
Interferences and deviations from ideal behavior can arise in spectrophotometric
analysis. Potassium permanganate’s strong oxidative properties can lead to reactions with other
substances in the solution, potentially affecting absorbance readings. Additionally, the presence
of colored species or particulate matter can lead to scattering and absorption at the same or
different wavelengths, complicating the analysis. Thus, sample preparation often includes
filtration or centrifugation steps to remove particulate properties, and in some cases, the use of
masking agents to mitigate interference from other reactive species.
In conclusion, spectrophotometric analysis of potassium permanganate solutions
exemplifies a robust and precise method for chemical quantification. By exploiting the distinct
absorbance properties of KMnO4, chemist can accurately determine its concentration in various
samples. This technique’s success hinges on meticulous sample preparation, careful calibration,
and an understanding of potential interferences. As a result, spectrophotometry remains a
cornerstone analytical technique in the scientific community, essential for research, quality
control, and numerous practical applications.

II. Materials and Equipment

 Potassium permanganate (KMnO4)
 Distilled water
 Analytical balance
 Volumetric flask (various sizes)
 Pipettes and pipette filter
 Spectrophotometer
 Cuvettes (1 cm path length)
 Blank solution (distilled water or appropriate solvent)

III. Procedure:

1. Prepare of Standard Solutions

1.) Stock Solution Preparation

An accurate amount of potassium permanganate, specifically 0.3162 g, was weighed using an

analytical balance. The weighed KMnO4 was then dissolved in a small volume of distilled water.
This solution was transferred to a 1-liter volumetric flask and diluted to the mark with distilled
water, resulting in a 0.002 M stock solution.

2.) Dilution to Prepare Standards

A series of standard solutions was prepared from the stock solution by serial dilution. For
example, a 0.0001 M solution was created by transferring 5 mL of the stock solution to a
volumetric flask and diluting it to the mark with distilled water. Similarly, a 0.00008 M solution
was made by transferring 10 mL of the stock solution to a 100 mL volumetric flask and diluting
it to the mark with distilled water. Standard solutions of 0.00016 M, 0.0004 M, and 0.0008 M
were prepared in a similar manner.Instrument Calibration and Blank Measurement

3.) Instrument Calibration:

The spectrophotometer was turned on and allowed to warm up according to the
manufacturer’s instructions. The wavelength was set to 400 nm, where KMnO4 has its
maximum absorbance. The spectrophotometer was then calibrated using a blank solution
of distilled water by filling a cuvette with the blank and placing it in the
spectrophotometer, adjusting the reading to zero absorbance.
2. Measurement of Standard Solutions
4.) Measure Absorbance of Standards:

A clean cuvette was rinsed with a small amount of the first standard solution. The cuvette was
then filled with the standard solution, wiped on the outside to remove any fingerprints or
droplets, and placed in the spectrophotometer. The absorbance was recorded. This process was
repeated for each standard solution, ensuring the cuvette was thoroughly rinsed between
different solutions to avoid contamination.
 3. Construction of Calibration Curve
5.) Plot the Calibration Curve:
4. Analysis of Unknown Sample
The recorded absorbance values were plotted against the concentrations of the standard
solutions. A best fit line was drawn through the points to create a calibration curve. The
equation of the line was determined to be y = mx + b, where y represents the absorbance,
x represents the concentration, m is the slope, and b is the y-intercept.
6.) Measurement Absorbance of Unknown Sample:
The unknown sample solution was prepared similarly to the standards. Its absorbance was
measured using the spectrophotometer set to 400 nm. All measurements were ensured to be
consistent with the conditions used for the standards.
7.) Determine the Concentration:

The calibration curve equation was used to calculate the concentration of the
unknown sample from its absorbance value.

1. Stock solution
(1) Mass of KMnO4 = 0.1274 g
(2) Molar mass of KMnO4 = 158.03 g/mol
(3) Moles KMnO4 = mass/molar mass = 8.061760425 x 10−4 mol KMnO4
(4) Molarity of stock solutions = mol KMnO4/0.100L = 0.00806 mol/L

2. Preparation of Standard Solutions

Standard solution 1 = 0.00008 M (.25 Ml stock to 25 mL water)
Standard solution 2 = 0.00016 M (.5 Ml stock to 25 mL water)
Standard solution 3 = 0. 0004 M (1.24 Ml stock to 25 mL water)
Standard solution 4 = 0.0008 M (2.5 Ml stock to 25 mL water)

3. The calibration curve at λmax = 400 nm

Standard Concentration Absorbance

1 0.00008 0.410
2 0.00016 0.584
3 0. 00040 1.482
4 0.0008 1.541
 KMnO4 Calibration Curve
1.8
1.6 f(x) = 1612.62755102041 x + 0.423704081632653
R² = 0.779606897695861
1.4
1.2
1
A 0.8
0.6
0.4
0.2
0
0 0.0001 0.0002 0.0003 0.0004 0.0005 0.0006 0.0007 0.0008 0.0009
C (mol/L)

Interpretation:
The provided calibration curve for potassium permanganate (KMnO4) illustrate the relationship
between the concentration of KMnO4 in mol/L (x-axis) and the absorbance (A) of a specific
wavelength (y-axis).

1. Linearity and Calibration Equation:

 The calibration curve is represented by a linear trend line with the equation: y = 1612x +
0.4237
 In this equation, y denotes the absorbance, and x dnotes the concentration of KMnO4 in
mol/L.
 The slope of the line is 1612/mol, and the y – intercept is 0.4237.
2. Coefficient of determination ( R2)
 The R2value is 0.7796, indication the degree of fit between the linear model and the
experimental data.
 An R2 value of 0.7796 suggest that approximately 77.96% of the variability in
absorbance can be explained by the KMnO4 concentration. While this indicates a
generally good fit, it also suggests there is some variability not explained by the linear
model, which might be due to experimental errors or other factors.

3. Data Points:
 The plot shows for data points corresponding to different concentrations of KMnO4.
 These points tie reasonably close to the trend line, supporting the linear relationship
between concentration and absorbance within this concentration range.
 4. Calibration Line Use:
 The calibration line can be used to determine the concentration of KMnO4 in unknown
y−0.4237
samples by measuring their absorbance and using the equation x =
1612.6
 Ensure that the absorbance readings of unknown samples fall within the range of the
calibration curve for accurate results.
5. Intercept Interpretation:
 The y – intercept (0.4237) suggest that there is some absorbance even when the
concentration of KMnO4 is zero. This could be due to instrument baseline absorbance,
impurities, or background absorbance in the solvent or cuvette.
6. Possible Improvements
 The R2 value indicates there is room improvement. Additional data points, especially at
lower and higher concentrations, could help to better define the calibration curve.
 Ensuring that all measurements are taken under consistent conditions and minimizing
potential sources of error (e.g., using high-purity reagents, precise sample preparation)
could improve the fit.

Conclusion:

The calibration curve provides a useful tool for determining the concentration of KMnO4 in
unknown samples. Define a reasonable good fit, the variability indicated by the R2 value suggests that
careful attention to experimental conditions and potential sources of error is important for achieving
precise and accurate measurements.

4. Calculations of the molar extinction coefficient ε at 400 nm.

Use the ∆- value of solution 1:

ε = ∆ / (C . 1), with 1 = 1 cm

A 0.410
ε = C .1 = 0.00008 = 5,125 or 5. 125 x 10
3

ε = 5125 m−1 cm−1