Name: Jericho P.

Encarnacion CYS: BSES 2A-M Date Submitted: June 20, 2022

Experiment No. 11
Determination of Manganese in Water through Persulfate Method

Introduction
Spectroscopy is another analytical technique used in determining
unknown concentration in a sample through visible absorption spectroscopy. In a
manganese solution, the intensity of the color after titration states the
concentration of the solution. Once the wavelength is determined, the
absorbance can now be obtained, and it is directly proportional to the
concentration in the solution as per Beer’s Law.
Objectives
At the end of this experiment, the students should be able to:
1. Use the acquired absorbance to determine the slope and intercept of the
curve;
2. Demonstrate skills on measuring manganese concentration through
spectroscopy; and
3. Calculate for the concentrations of cuvettes.
Materials and Apparatus
Mercuric sulfate, 85% phosphoric acid, silver nitrate, 0.1 N Standard Manganese
solution, sodium oxalate of primary standard, ammonium persulfate, sodium
bisulfite solution, (1+1) sulfuric acid, hydrogen peroxide, concentrated nitric acid,
distilled water, test tubes, beaker, fume hood, pipette, weighing scale, analytical
balance, watch glass, funnel, measuring cylinder, volumetric flask, reagent bottle
Procedure
A. Preparation of Necessary Reagents
As for preparation of special reagent, a 50.0 mL distilled water was added
in the 500 mL beaker. Then, a 100.0 mL concentrated nitric acid was added and
pipetted in the beaker. Afterwards, an 18.75 g mercuric sulfate was weighed and
added to the beaker and stirred. After that, a 50 mL phosphoric acid was added
through a measuring cylinder to the beaker and stirred. Then, a 0.0090 g silver
nitrate was weighed out in an analytical balance and added in a volumetric flask
then properly rinsed the watch glass and funnel and stirred. Meanwhile, the
solution was transferred into a 250 mL volumetric flask and diluted to the mark
then shook well.
 As for preparation of standard manganese solution of 0.1 N, a 1.6 grams
potassium permanganate was weight out. After that, it was transferred into a 500
mL A grade volumetric flask then rinsed the watch glass and funnel with distilled
water. Then, added with distilled water up to half of the volumetric flask and
shook well. Next, diluted the solution to the 500 mL mark of volumetric flask then
shook well and transferred into the reagent bottle.
As for preparation of sodium bisulfite solution, a 10.0 g sodium bisulfite
was weighed out. Then, it was transferred into a 100 mL A grade volumetric flask
and properly rinsed the watch glass and funnel with distilled water. After that,
diluted up to the half of the flask and shook well. Then, a final volume was made
by diluted it to 100 mL mark and shook well then transferred into a reagent bottle.
As for preparation of (1+1) sulfuric acid, an equal amount of distilled water
and concentrated sulfuric acid were mixed then pipetted with 50 mL distilled
water and added to a reagent bottle. Then, the solution was placed in a fume
hood for several minutes and let it cool and shook well.
B. Standardization of Potassium Permanganate Solution
A sodium oxalate was weighed out about near 200 mg, 150 mg, 100 mg,
50 mg, and 1 mg in clean and dry watch glass. Then, a five clean and dry 50 mL
beaker were labelled with the corresponding amount of sodium oxalate taken yet
diluted to 100 mL mark with distilled water and stirred. Afterwards, a (1+1)
sulfuric acid was taken and shaken well and pipetted a 10 mL then added to
each beaker. Next, the beakers were heated upto 95 oC and titrated with
potassium permanganate immediately.
For blank titration, three 500 mL beakers were added with 100 mL distilled
water each and a (1+1) sulfuric acid was taken and shaken well and pipetted a
10 mL then added to each beaker. Next, the beakers were heated upto 95 oC and
titrated with 0.1 mL potassium permanganate.
C. Preparation of Calibration Standards, Sample and Blank Titration
A 50-ppm manganese standard solution was diluted into 10 ppm then
placed in a 250 mL A grade volumetric flask and added with distilled water up to
half of the flask. Next, a final volume was made up to 250 mL mark. Afterwards, a
calibration standard of 0.5 ppm, 1.0 ppm, 1.5 ppm, 2.0 ppm, 2.25 ppm, and blank
were prepared in six 400 mL beakers. For blank, an 85 mL distilled water was
added. Then, a 5.0 mL special reagent was pipetted and added to each beaker.
After that, one drop 30% hydrogen peroxide was added to each beaker. Then,
diluted each beaker to 90 mL mark with distilled water. Afterwards, a 1 g
ammonium persulfate was added to each beaker. Finally, the beakers were
boiled for 1 minute then cooled with tap water. The process was repeated for
sample preparation.
Data Analysis
Table 1
Absorbance of the Solution at 580 nm with Varying Concentration

Figure 1
Calculations for Table 1
 Figure 2
Calibration Curve

Concentration Vs. Absorbance Graph

0.8
0.738
0.7

0.6 0.577

0.5
ABSORBANCE

0.442
0.4
0.301
0.3
0.217
0.2 0.147
0.1 0.072
0.03
0

CONCENTRATION

Results Discussion
The above table shows the absorbance of the solution at 580 nm
wavelength. The concentration varies ranging from 1.00 ppm to 25.00 ppm. It
also shows the square of concentrations and square of absorbance altogether
 with the product of both concentration and absorbance which are needed to
calculate the unknown concentration of the sample.
On Figure 2, the calibration curve for this experiment was shown. It shows
that there is a direct relationship between the concentration and absorbance at
constant wavelength. According to the curve, as the concentration increases, the
absorbance increases. With respect to the trend, the value of unknown
concentration with an absorbance of 0.356 at 580 nm is 12.13080885 which is
close enough to the manually computed concentration of 12.14 ppm.
Conclusion
Based on the data and results, the following conclusions were drawn:
1. Beer's Law is commonly written as A=abc, where A denotes absorbance, c
represents concentration, b represents cuvette path length, and a denotes a
constant parameter of the substance under study conducted. The y-intercept
is equivalent to 0 in the ideal Beer's Law, A=abc.
2. The linear regression approach yields A = mc + (y-intercept) on the y-axis, a
straight line with a y-intercept arising from tiny deviations induced by your
procedure and the instrument you use. The slope is represented by "m,"
which is equivalent to "ab" in the Beer's Law equation. The concentration is
displayed on the x-axis as "c." The "c" in the Beer's Law equation is the same.
3. The solutions you will be given are basically colorless and contain
manganese ions, Mn2+aq. In an acidic solution, manganese ions are easily
oxidized to form permanganate ions, MnO 4-aq, a bright purple complex.
Because of the strong color, even with small amounts of manganese in the
sample, the analysis can be quite sensitive because the light absorption will
be rather large.
Application
Spectrophotometers have found their way into a wide range of scientific
and manufacturing fields. They're everywhere, from the field to the warehouse to
the assembly line and beyond. Spectrophotometric technology offers a wide
range of applications both inside and outside the laboratory, including the
following: agriculture, food additives, pharmaceuticals, chemical analysis,
plastics, processed foods, water analysis, coffee roasting, tea fingerprinting,
forensics, biomedical optics, paints & coatings, and cosmetics.
Reference
Methods, W. Q. A. L. (2019, January 2). 01) Manganese in Water - Persulfate Method
(Preparation of Necessary Reagents) [Video]. YouTube.
https://www.youtube.com/watch?v=d5trPkhHvww&feature=youtu.be
Methods, W. Q. A. L. (2020, July 26). 05) Manganese in water (Persulfate method) -
Preparation of Calibration standards, Sample & Blank [Video]. YouTube.
https://www.youtube.com/watch?v=Y9bmM6ahH-U&feature=youtu.be
Methods, W. Q. A. L. (2021, September 4). 02) Manganese in Water (Persulfate
Method) Standardization of Potassium permanganate solution [Video]. YouTube.
https://www.youtube.com/watch?v=HDtmZB6gDTM&feature=youtu.be