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INTRODUCTION
I.1. Objective
a. Mohr Methods.
The indicatore used in this method is K2CrO4 and the titrant is AgNO3. Mohr
methods is mainly used for determination of chloride or bromide. A solution
of chloride titrated with AgNO3 solution, there will be:
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The end point of the titration can be expressed by the indicator K2CrO4
solution with ion Ag+ (excess) produce red brick precipitate of AgCrO4.
When the pH used too low (acid) can make ion CrO4 change into Cr2O7
which causes the precipitation doesn’t appear. (Harjadi,1986)
b. Volhard method.
In Volhard method, NH4SCN or KSCN are used as titrant and Fe3+ solution
is used as indicator. To determine the equivalent point, the reaction must
occur between a titrant and Ag, forming white precipitate.
c. Vajans method
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surface of colloidal AgCl. After all chloride is used, the first drop of Ag+ will
react with fluorescein (FI-) forming a reddish color. (Underwood, 2002).
Fluorescein itself in the solution has green-yellowish color. The end point of
the titration is known when the white precipitate changes its color to pinkish
and becomes more brittle. The other change that indicates that the end point
has been reached is when the solution becomes more clear and colorless.
(Harjadi, 1986)
To minimize the use of titrant, the necessary corrections can be done by blank
titration. Blank titration, performed to reduce errors caused by reagents, solvents or
experimental conditions. The procedure is the same as the titration of the test
substance, but without the use of the test substance. (Garcia,2008)
I.2.4 Buffer
Buffer is made from weak acid (HA) and its conjugate base (A-) or vice versa, and
this cause both the acid and base components to be present in the solution. If a strong
base is added to a buffer, the weak acid will give up its H+ in order to transform the
base (OH-) into water (H2O) and the conjugate base:
HA + OH-→ A- + H2O
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Since the added OH- is consumed by this reaction, the pH will change only slightly.If
a strong acid is added to a buffer, the weak base will react with the H+ from the
strong acid to form the weak acid HA:
H+ + A- → HA
The H+ will be absorbed by the A- instead of reacting with water to form H3O+ (H+),
so the pH changes only slightly. (Wikipedia, 2017)
I.2.5 Materials
a. Sodium Chloride
b. Silver Nitrate
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Density = 4.35 g/cm3 (240C)
c. Potassium Oxalate
d. Sodium Bicarbonate
e. Table Salt
Table salt is one of the most common household chemicals. Table salt is 97% to
99% sodium chloride, NaCl. Pure sodium chloride is an ionic crystal solid.
However, other compounds are present in table salt, depending on its source or
additives that may be included before packaging. In its pure form, sodium
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chloride is white. Table salt may be white or may have a faint purple or blue
tinge from impurities. (ToughtCo, 2017)
f. Calcium Carbonate
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CHAPTER II
EXPERIMENTAL METHOD
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II.2. Solution Preparation
Tolerance ±10%
0.2922 − 0.02922 = 0.26298 ≈ 0.2630 gram
0.2922 + 0.02922 = 0.32142 ≈ 0.3214 gram
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Preparing AgNO3 solution:
1. 1.3 gram of AgNO3 powder was weighed by using hard balance.
2. AgNO3 powder was dissolved by using distilled water in beaker glass until 0.05
L.
=2.5 grams
1. K 2 CrO4 solid was weighted 2.5 grams with watch glass using hard balance.
2. K 2 CrO4 solid was dissolved in beaker glass using distilled water until 50 ml.
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1. 10 ml of NaCl solution was taken with pipette volume and moving it into
Erlenmeyer.
2. 2 drops of K 2 CrO4 5% was expelled and 0.5 grams of NaHCO3 was given into
Erlenmeyer.
3. AgNO3 was poured into burette until 50 ml.
4. The solution in the Erlenmeyer was titrated with AgNO3 solution.
5. The volume of AgNO3 solution needed for the titration was recorded and the
changes that happened.
6. The experiment was repeated once.
II.2.6 Blank Titration
1. 20 ml of distilled water was added into Erlenmeyer with measuring cylinder.
2. 2 drops of K 2 CrO4 5% was expelled, 0.5 grams of NaHCO3 , and 0.5 grams of
CaCO3 was given into Erlenmeyer.
3. AgNO3 was poured into burette until 50 ml.
4. The solution in the Erlenmeyer was titrated with AgNO3 solution.
5. The experiment was repeated once.
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II.4.1 Standardization of AgNO3 solution with a standard solution of NaCl
CHAPTER III
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RESULT AND DISCUSSION
III.1. Results
2. Titration result
Indicator: K2CrO4 5%
V of sodium chloride V of AgNO3 solution
Color change
solution (mL) (mL)
10 11.1 White precipitate
10 11 red brownish
Average: 10 11.05 precipitate
Table 3.1.1: This table shows the volume of AgNO3 (V1) solution to titrate 10 mL of sodium
chloride and the change in precipitated color when end point was reached.
1. Standard solution was prepared by weighing 0.5168 g sample, then dissolved and
diluted with distilled water until 100 ml.
2. Titration result
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Indicator: K2CrO4 5%
V of sample solution V of AgNO3 solution
Color change
(mL) (mL)
10 18.1 White precipitate →
10 18.1 red brownish
Average: 10 18.1 precipitate
Table 3.1.3: This table shows the volume of AgNO3 (V3) solution to titrate 10 mL of sample
solution and the change in precipitated color when end point was reached.
III.2. Calculation
= 0.0497 N
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True volume of AgNO3 solution = V3 – V2
= 18.1 − 0.4
= 17.7 mL
= 0.2932 gram
𝑀𝑎𝑠𝑠 𝑜𝑓 𝐶𝑙−
Percentage = 𝑀𝑎𝑠𝑠 𝑜𝑓 𝑠𝑎𝑚𝑝𝑙𝑒 × 100%
0.2932 g
= 0.5168 𝑔 × 100%
= 56.7%
III.2.4 Precentage of NaCl in table salt
= 0.4827 gram
𝑀𝑎𝑠𝑠 𝑜𝑓 𝑁𝑎𝐶𝑙
Percentage = 𝑀𝑎𝑠𝑠 𝑜𝑓 𝑠𝑎𝑚𝑝𝑙𝑒 × 100%
0.4827 g
= 0.5168 𝑔 × 100%
= 93.4%
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In this experiment, argentometry titration are aimed to determine the concentration of
Cl- from a sample of table salt. Table salt used was from “cap Kapal” brand, a local
table salt that often use for cooking essential. In the argentometry titration, it involves
a precipitate reaction to determine the concentration of the titrate. A silver nitrate
(AgNO3) used as a titrant to titrating the sample solution and the precipitating agent.
In this titration, the end point was detected by the formation of second colored
precipitate or usually known as the Mohr method.
In this titration of standardizaztion of AgNO3, the primary standard solution used was
NaCl (Sodium Chloride). Since the NaCl was the primary standard, the preparation
was done precisely; thus, the weight of NaCl was obtained using analytical balance.
The NaCl was weighed about 0.2902 gram and then dissolved and diluted with
distilled water until 100 mL.
The indicator used to detect the end point of the titration of standardizaztion of AgNO3
was K2CrO4 5% solution. The chromate ions in K2CrO4 will react with the silver ions
from AgNO3 and produced Ag2CrO4, which is a red-brownish colored precipitate.
When the red-brownish colored precipitate shows up, it means that all the NaCl
solution has been used up.
Figure III.3.1 The white precipitate was formed Figure III.3.2 The precipitate changed color
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The color changed from a white precipitate into sheer red-brownish precipitate. White
precipitate was formed as reaction between Cl- ion and Ag+ ion went by. The titration
end point was formed due to the reaction between Ag+ ion and CrO42- ion. The color
of the precipitate had been changing although the color of the solution was stillthe
same. However, the titration end point was shown by the precipitate color alteration
not in the solution.
Beside the indicator, NaHCO3 is added to the analyte. NaHCO3 is a buffer that is made
from weak acid (HCO3-) and salt of weak acid (Na2CO3). It is added in order to keep
the pH constant. NaHCO3 buffer works according to this equation:
(H+) + HCO3- ↔ H2CO3
This equation happens when acid is added to the buffer where the excess H+ will
react with HCO3- to form H2CO3.
NaHCO3 ↔ (H+) + CO3-
The change in precipitate’s color was due to the reaction of Ag+ ion and CrO42- ion,
it means that the volume of AgNO3 used for titrating NaCl and sample was already
excessive. This little excessive amount of AgNO3 solution was not used for titrating
both NaCl solution and sample solution, but for reacting with K2CrO4 to give the
titration end point. Therefore, blank titration was done in order to get the volume of
AgNO3 solution needed to form red-brownish precipitate.
Blank titration could minimize the error in determining the concentration of both
NaCl solution and sample solution. Thus, with the help of the blank titration, the
concentration at the titrant solutions could be known precisely. CaCO3 (Calcium
Carbonate) was added in blank titration to give the same salt environment as both
NaCl solution and the sample of table salt solution. CaCO3 was insoluble in distilled
water. Thus, it would remain as solid and could be seen at the bottom of the
erlenmeyer as white precipitate if it is under normal circumstances.
From blank titration, it was determined that 0.4 mL of AgNO3 needed to titrate 11
mL of aquadest with 5% K2CrO4 indicator, 0.5 gram of CaCO3, and 0,5 gram of
NaHCO3. The volume of distilled water in erlenmeyer used was the same volume as
AgNO3 in the standardization, which was 11 mL.
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From standardization of AgNO3 with sodium chloride and blank titration, it was
determined that 10.65 mL of AgNO3 (11.05-0.40 mL) needed to titrate 10 mL of
NaCl with normality 0.0530 N. From the calculation above, it has been determined
that the normality of AgNO3 is 0.0497 N.
To determine the percentage of Cl- in the sample, 0.5168 g of the sample of table salt
“cap Kapal” was obtained using analytical balance. It was then diluted with distilled
water below to 100 mL in beaker glass. This solution was poured into volumetric
flask and aquadest was added until 100 mL was reached. Then this solution was
shaken in order to make sure that it was diluted completely. After that the solution
was transferred to beaker glass so it would be pipetted easily.
The sample solution was moved using pipette volume 10 mL to the erlenmeyer. 2
drops of 5% K2CrO4 and 0,5 gram of NaHCO3 were also added to erlenmeyer. From
this titration, it was recorded that 18.1 mL of AgNO3 was needed to titrate 10 mL of
sample solution. And from blank titration, the real volume of AgNO3 that titrated
table salt solution was known, which was 17.1 – 0.4 mL = 17.7 mL. By using the
normality of AgNO3 from standardization of AgNO3, the normality of Cl- can be
calculated. The normality of Cl- obtained is 0.0826 N. From the normality of Cl-
calculated, 56.73% was obtained as the percentage of Cl- and 93.4017% as the
percentage of NaCl. Therefore, it was proved that this table salt mostly consists of
NaCl.
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Figure III.3.4 The determination of Cl- result
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CHAPTER 4
IV.1 Conclusion
IV.2. Suggestion
The precipitate of Ag2CrO4 only can be seen clearly enough to human eye
after the amount is quite a lot. As a result, the observation needs to be done very
carefully to not exceed the limit of end point too much. The exceed can be reduced
with blank titration. The red-brownish precipitate formed in the Blank titration just
needs few drops of the AgNO3. Mostly nearly all of the groups were repeating
another experiment due to miscalculated the end point while the titrated is really
expensive. So the titrated was limited at that time and time-wasting for everyone.
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REFERENCES
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