EXPERIMENT 5: DETERMINATION OF WEIGHT OF VARIATIONS AND

APPLICATION OF STATISTICAL TOOL

Lising, Audrey Nicole L., Logan, Frances Randolf J., Madariaga, Vic Lorence B.
College of Science
University of the Philippines Baguio
Chem 26.1 – FG

ABSTRACT
The objectives of this experiment are 1.) to learn the technique and calculations
involving blank titrations and 2.) to determine the iron content of a sample using
oxidation-reduction reaction and finally 3.) to illustrate the use of self- indicating
agent. The experiment involved the analysis of the iron content in a sample Iron
tablet by the use of titrimetric method with the standard KMnO4 solution. The
KMnO4 solution was standardized with the use of Na2C2O4 to determine its true
concentration . A blank was also obtained by titrating H2SO4 solution with the
KMnO4 solution. For the analysis of iron tablets, 2 sample iron tablets were
grinded and was added with H2SO4. The iron tablet solution was then titrated
with The KMnO4 solution. After deriving the data of the experiment, results show
that the data gathered for the standardization of KMnO4 solution were not
precise as supported by the large differences of the values of the three trials
and the computed RSD was 0.75% indicating erroneous data. For the analysis
of the iron tablet results shows that the computed iron content is not precise and
inaccurate with the iron content stated by the manufacturer. The calculated iron
content was 82.85 mg per tablet while the manufacturer’s indicated iron content
was 105 mg per tablet with a relative error of 21.35%. These inaccuracies are
attributed to observational errors of the experimenters during the experiment
such as incorrect reading of the measured value or improper weighing of the
materials needed. Environmental errors like atmospheric conditions such as
humidity, temperature, pressure and topographic region where the experiment
was conducted can also affect the elemental iron composition of the iron tablet.
After conducting and deriving results from the experiment it is concluded that all
objectives are met by the experimenters.
INTRO

Iron is an essential mineral used in many functions and it’s necessary for life as it play a role in
the making of red blood cells which carry oxygen. The human body gets its iron from the food
we eat or from supplements. It is very important that we have enough iron in our body as iron
deficiency can take a serious consequence such as anemia which causes low levels of red
blood cells. If a person is not getting enough iron through food he can also get enough iron by
taking iron supplements. Iron supplements contain soluble iron(II) salts to replenish them in the
human body in case of deficiency and it usually contain about 50mg per tablet of iron(II)
(Watson,2011)). In this experiment, the analysis of present iron in the sample iron supplement
tablet can be done by a redox titration reaction. In a redox reaction, transferring of electrons
occurs in the reacting ions present in the aqueous solutions during the chemical reaction. The
compound losing electrons is said to be oxidized and the compound gaining electrons is said to
be reduced. The total number of electrons lost in the oxidation half-reaction is equal to the
number of electrons gained in the reduction half-reaction (Bortoli,2015).There are three types of
redox titrations namely the Permanganate Titration, Dichromate Titrations and the Iodimetric and
Iodometric Titrations. The type of redox titration used in this experiment is the Permanganate
titration. In the Potassium permanganate redox titration the Potassium Permanganate is used as
the oxidant and it can act as the self-indicator in the titration. Because of this it doesn’t need an
indicator reagent as it can mark the endpoint of a titration by itself unlike acid-base titrations. The
dilute sulphuric acid is then used to maintain the potassium permanganate solution and it also
helps to increase the hydrogen ions present in the solution. In this technique, the reagent has
intense color due to the permanganate ion MnO4–. A blank titration was also conducted in this
experiment and is carried out by titrating a fixed and known concentration of titrant into a solvent
with zero analyte. The only difference from the regular titration is the absence of analyte. This
allows the amount of reactive substance within the plain solvent to be determined and hence
allows a determination of the error in future titration experiments using this solvent.
(Samuel,nd)The objective of the experiment is to learn the technique and calculation involving
blank titration, to determine the iron content of a sample using oxidation-reduction reaction and
finally to illustrate the use of self-indicating agent.
Samuel, M.(n.d). Blank Titration. Retrieved from https://education.seattlepi.com/blank-titration-
needed-4452.html

Watson, S. (2011). What you need to know about iron supplements. Retrieved from
https://www.webmd.com/vitamins-and-supplements/features/iron-supplements#1

Bortoli, A. (2015). Chemical Kinetics. Retrieved from

https://www.sciencedirect.com/topics/engineering/redox-reaction
EXP 6

Methods

For the preparation and standardization of 0.025N Sodium Thiosulfate the needed materials are
1.5 g sodium thiosulfate, 250 mL volumetric flask, 0.02 g sodium carbonate, potassium
dichromate, potassium iodide and starch solution. To start off, a 1.5 g of sodium thiosulfate
pentahydrate crystals and 0.02 g of sodium carbonate was dissolved and added in a 250 mL
volumetric flask using distilled water then the solution was placed in a bottle. Three 0.05 g of dry
potassium dichromate was weighed in a 250 mL flask. 50 mL of water was added with 1 mL of
concentrated sulfuric acid. For each sample 0.2 g of sodium carbonate was added with gentle
swirling. 0.5 g of potassium iodide with 3 mL of water was prepared and it was swirled, covered
and stand for 3 minutes. It was then diluted with 100 mL of water. It was then titrated with the
thiosulfate solution until the yellow color is gone and a 1 mL of starch solution was added then
continue the titration until the color blue solution was removed and turned into an emerald green
solution.

For the collection and analysis of water samples the winkler method was done by collecting water
in a calibrated wrinkler then a stopper was put for cover. 2 mL of 2.4 M MnSO4 and 2 mL of KI
was added by a pipet below the surface of the liquid. The stopper was replaced and the solution
was mixed and inverted. Upon the settling of the precipitate 2 mL of concentrated H₂SO₄ was
added and the stopper was replaced and the solution was mixed until precipitate was dissolved.50
mL of aliquot was drawn out using pipet and was put in an Erlenmeyer flask. It was titrated with
Na2S2O3 until pale straw color is achieved. 1 mL of 1% starch was also added until blue color
disappears. Four determinations were made in this experiment.
RESULTS

The following data below were gathered by performing and following the procedures in the
laboratory protocol provided.

Table 1. Data gathered from the standardization of Na2S2O3

TRIAL 1 TRIAL 2 TRIAL 3

Mass of K₂Cr₂O₇, 0.058 g 0.047 g 0.049 g
Initial burette reading 0 mL 0 mL 0 mL
Final burette reading 45 mL 39 mL 39.4 mL
Volume of Na2S2O3 45 mL 39 mL 39.4 mL

The data presented above shows the recorded values of the mass of K₂Cr₂O₇ and the volume of
Na2S2O3 used for the titration of the thiosulfate solution. From these data, it can already be
compared and deduced that the mass of K₂Cr₂O₇ is directly proportional to the volume of
Na2S2O3.That is the greater the mass of K₂Cr₂O₇ the more volume of Na2S2O3 will be needed to
complete the titration. It can also be deduced that the data for trials 1 and 2 are precise with each
other.

Table 2. Data gathered from the analysis of water sample

TRIAL 1 TRIAL 2 TRIAL 3 TRIAL 4

Vol. aliquot 50 mL 50 mL 50 mL 50 mL
initial burette 0 mL 2.3 mL 4.8 mL 8.3 mL
reading
Final burette 2.3 mL 4.8 mL 7.3 mL 10.6 mL
reading
Vol. Na2S2O3 2.3 mL 2.5 mL 2.3 mL 2.3 mL

The data presented above shows the recorded values for of the aliquot volume of the water
solution with the initial and final burette reading and the final volume of Na2S2O3 used to complete
the titration. From the data of the four trials it can already deduced that the values are almost
equal with each other and are precise with each other.

EXP 7

ABSTRACT

The objectives of this experiment are 1.) to get acquainted with chelating agents and 2.) to
strengthen technical skills involved in titrimetric analyses,3.) to learn and apply the concept of
titer and finally 4.) to study one physico-chemical characteristics of water. The experiment
involved the determination of water hardness or the dissolved calcium and magnesium in water
by the use of complexometric titrimetric method with the standard EDTA solution as the
chelating agent. The EDTA solution was standardized with the use of CaCO3 where the calcium
solution will turn from wine red to pure blue color. The standardization of the EDTA solution was
conducted to determine its true concentration to come up with the calculation of the CaCO3 titer
(mg/mL). From the results gathered from the three trials the values are very close with each other
and hence, these values are precise. The RSD is also low however slight random errors still
occurred in the experiment that will affect the accuracy of the calculated hardness of the water.
The analysis of the hardness of a water sample which in this experiment is the Viva purified
drinking water was determined using complexometric titration where the water solution will be
titrated with the standardized EDTA solution with the endpoint of the titration will be signaled
from the change of the water solution from wine red to pure blue. After deriving the results of the
experiment, results show that the data gathered from the performed three trials are very precise
with an RSD of 0% which indicated that only slight errors happened during the experiment. The
computed CaCO3 concentration was 130.72 ppm which is classified as slightly hard. This
calculated value was proven inaccurate with that of the indicated hardness of the water sample
of the manufacturer with a 3.16% relative error. This inaccuracy may be attributed to
observational errors made by the experimenters upon the formation of the complexed color
during the end-point of the titration. After conducting and deriving results from the experiment it
is concluded that all objectives are met by the experimenters
The following data were gathered by performing and following the procedures in the laboratory
protocol provided

Table 1. Preparation and Standardization of EDTA

TRIAL 1 TRIAL 2 TRIAL 3

Vol Ca2 solution mL mL mL
Initial burette reading 0 mL 0 mL 0 mL
Final burette reading 25.7 mL 25.9 mL 25.7 mL
Vol of EDTA used 25.7 mL 25.9 mL 25.7 mL
Mol. Of EDTA 17.5 M 17.4 M 17.5 M
Standard Deviation 0.078 Relative Standard 0.45%
Deviation
174.75 173.40 174.75
CaCO3 titer (mg/mL)
Mean CaCO3 titer 174.30
The data presented above shows the recorded values for the Ca solution used, Mean CaCO3
titer and the volume of EDTA used to complete the titration. From these values it can already be
compared and deduced that the volume of EDTA used to complete the titration for the three
trials are very precise with each other. This is supported by the closeness of their values and
the relative standard deviation have a small value.

Table 2. Analysis of Water Sample

TRIAL 1 TRIAL 2 TRIAL 3

Vol of sample mL mL mL
Initial burette reading 0 mL 7.6 mL 15.2 mL
Final burette reading 7.6 mL 15.2 mL 22.0 mL
Vol of EDTA reading 7.6 mL 7.6 mL 7.6 mL
Hardness (mg 53.0 53.0 53.0
CaCO3/L sample)
Mean hardness 53
Standard deviation 0 Relative standard 0%
deviation
The data presented above shows the recorded values for volume of the sample and the volume
of the EDTA used to complete the titration. The computed hardness or mg CaCO3/L sample was
computed for the three trials and the calculated results are all the same. From this results, it can
already be deduced that the values for the hardness are very precise as supported with the 0 %
relative standard deviation