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B. PURPOSE
C. BASIC THEORY
:
Precipitation Titration
Thus far we have examined titrimetric methods based on acidbase,
complexation, and redox reactions. A reaction in which the analyte and titrant form an
insoluble precipitate also can serve as the basis for a titration. We call this type of
titration a precipitation titration.
One of the earliest precipitation titrationsdeveloped at the end of the
eighteenth centurywas the analysis of K2CO3 and K2SO4 in potash. Calcium nitrate,
Ca(NO3)2, was used as the titrant, forming a precipitate of CaCO 3 and CaSO4. The
titrations end point was signaled by noting when the addition of titrant ceased to
generate additional precipitate. The importance of precipitation titrimetry as an
analytical method reached its zenith in the nineteenth century when several methods
were developed for determining Ag+ and halide ions.
Basic reaction of precipitation titration is the happen of precipitate in the
reaction between analyte substance, example:
Ag+ + X- AgX(s)
where x: halogen
(sorrel)
Precipitation Titration
(red)
Indicator of K2CRO4 used in the titration between halide ion and silver ion,
where excess of Ag+ ion will be react with CrO42- forms silver chromate and the color
is brick red (Mohr way).
At equivalent point:
Equivalent Ag+ = equivalent ClIndicator of Fe3+ can be used in the titration between silver ion and SCN - ion
where the excess of SCN- ion will be react with Fe3+ ion that give a red color. Or can
be used in the titration between halide ion and excess of silver ion, and the excess of
silver ion will be titrated with thiosianat ion (Volhard way).
At equivalent point:
Sum of equivalent Ag+ recidu = sum of equivalent SCNOr
Sum of equivalent Ag+ total = sum of equivalent (Cl- + SCN-)
Selecting and Evaluating the End point
At the beginning of this section we noted that the first precipitation titration
used the cessation of precipitation to signal the end point. At best, this is a
cumbersome method for detecting a titrations end point. Before precipitation
titrimetry became practical, better methods for identifying the end point were
necessary.
In any titration, it is necessary to have some method of detecting when just
enough of the titrant has been added -- a procedure known as detecting the endpoint
of the titration. The endpoint of this titration can be detected if the rapid change in
either the concentration of silver ion or the concentration of chloride ion which
occurs at the endpoint can be made apparent to an observer. Either instrumental
Precipitation Titration
methods or equilibrium methods can be used. The equilibrium methods are fairly
straightforward. In this case we can use Ag2CrO4, because a solution of CrO42- is
yellow while Ag2CrO4 is blood-red.
Finding the End point With an Indicator
There are three general types of indicators for precipitation titrations, each of
which changes color at or near the titrations equivalence point. The first type of
indicator is a species that forms a precipitate with the titrant. In the Mohr method for
Cl using Ag+ as a titrant, for example, a small amount of K 2CrO4 is added to the
titrands solution. The titrations end point is the formation of a reddish-brown
precipitate of Ag2CrO4.
The Mohr method was first published in 1855 by Karl Friedrich Mohr.
Because CrO42 imparts a yellow color to the solution, which might obscure
the end point, only a small amount of K2CrO4 is added. As a result, the end point is
always later than the equivalence point. To compensate for this positive determinate
error, an analyte-free reagent blank is analyzed to determine the volume of titrant
needed to affect a change in the indicators color. Subtracting the end point for the
reagent blank from the titrands end point gives the titrations end point. Because
CrO42 is a weak base, the titrands solution is made slightly alkaline. If the pH is too
acidic, chromate is present as HCrO4 instead of CrO42, and the Ag2CrO4 end point is
delayed. The pH also must be less than 10 to avoid the precipitation of silver
hydroxide.
A second type of indicator uses a species that forms a colored complex with
the titrant or the titrand. In the Volhard method for Ag+ using KSCN as the titrant,
for example, a small amount of Fe 3+ is added to the titrands solution. The titrations
end point is the formation of the reddish-colored Fe(SCN) 2+ complex. The titration
Precipitation Titration
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E. PROCEDURE
:
a. Determination (Standardization) AgNO3 Solution 0,1 N with NaCl as
primary standard solution.
-
0,5 grams
- Weighing in weights bottle
NaCl - Moved into volumetric flask 100 mL
Burette
- Washed with AgNO3 solution
Sorrel
precipitate
- Read and note the number on the buret at the beginning and
titration
Calculated the concentration of AgNO3 solution
Repeated 3 times
Calculated the average of AgNO3 solution
Average of AgNO3
Application of Precipitate
a. Determination of the content of Cl- in the tap water
Tap Water
- Measured the density of tap water with picnometer
Precipitation Titration
Solution
Took 10 mL
Added 5 drops of K2CrO4 5%
Titrated with AgNO3
Brick Red
Precipitate
- Repeated 3 times
Precipitation Titration
F. EXPERIMENT RESULT
No
Procedure of Experiment
.
1.
Result
Determination AgNO3 Solution Before:
- NaCl: white
0,1 N with NaCl as primary
powder
standard solution
- K2CrO4: yellow
- AgNO3:
1,5 grams
NaCl
Weighing in weights
bottle
Moved into volum-
Experiment
colorless
- Aquades:
colorless
After:
- NaCl + aquades:
colorless
- NaCl + aquades
+ K2CrO4: yellow
- NaCl + aquades
+ K2CrO4 +
solution
Pipette with
Burette
volumetric pipette
10 mL of NaCl
-
solution
Entered into
Erlenmeyer 250 mL
Added 10 mL
aquades
Added 1 mL K2CrO4
indicator
Titrated with AgNO3
V1
AgNO3=5.6mL
V2
AgNO3=5.7mL
V3
AgNO3=6.0mL
and mix it
Precipitation Titration
Hypothesis
Conclusion
At the
Concentration
beginning of
of AgNO3
titration:
=0.147 N
AgNO3 + NaCl
AgCl(s) +
NaNO3(aq)
white
precipitate
Approach
equivalent
point:
2AgCl +
K2CrO4
Ag2CrO4 + 2
KCl sorrel
precipitate
Stop
Sorrel
precipitate
volume
of
titration
Calculated the concentration of AgNO3
solution
Repeated 3 times
Calculated
the
average of AgNO3
solution
2.
Application of Precipitate
Determination of the content of
Cl- in the tap water
Tap Water
Precipitation Titration
Before:
- NaCl: white
crystal
- Aquades:
colorless
- K2CrO4: Yellow
10
picnometer
After:
- Noted the place of
- NaCl + aquades:
sample
colorless
- Pipette 10 mL
- NaCl + aquades
- Diluted in the volum+ K2CrO4 =
etric flask 250 mL
yellow
- NaCl + aquades
Solution
+ K2CrO4 +
-
Took 10 mL
AgNO3 = sorrel
Added 5 drops of
precipitate
K2CrO4 5%
V1
- Titrated with AgNO3
AgNO3=0.5mL
V2
Sorrel
Precipitate
AgNO3=0.8mL
V3
Repeated 3 times
Calculated the content AgNO =0.5mL
3
of Cl in the tap water
Precipitation Titration
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Precipitation Titration
12
H. CONCLUSION
Based on experiment that we have done, we can conclude that :
1. AgNO3 concentration is 0.147N
2. The precentage of Cl- in tap water is 0.0051%
Precipitation Titration
13
AgNO3
5 mmol
2,5 mmol
2,5
2,5
2,5
2,5
2,5
AgCl + NaNO3
NaCl +
AgNO3
5 mmol
4.99 mmol
4.99
4.99
4.99
0.01
4.99
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NaNO3
NaCl +
AgNO3
5 mmol
5 mmol
+s
AgNO3
5 mmol
5,01 mmol
0.01
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AgCl +NaNO3
NaNO3
NaCl +
AgNO3
5 mmol
6 mmol
Titration Curves
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NaNO3
the analyte.
Potentiometric end point
o Potential between a silver electrode and a reference electrode
whose potential is constant is measured
o Independent of the added reagent
Amperometric end point
o Current generated between a pair of silver microelectrodes in the
Precipitation Titration
17
yellow-green.
The fluoresceinate ions forms an intensely red silver
salt.However, Its concentration is never large enough to
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Precipitation Titration
19
http://chemwiki.ucdavis.edu/Analytical_Chemistry/Analytical_Chemistry_2.
0/09_Titrimetric
_Methods/9E_Precipitation_Titrations Accessed on Sunday, December
Accessed on Sunday,
December 21st 2013 at 16.30
Jeffery, GH, Bassett J, Mendhan J,Denny RC, 1989.VOGELs Textbook of
Quantitative Chemical Analysis. Ed 5. London : Logman Group
Tim.2013.Panduan Praktikum Kimia Analitik I Dasar-Dasar Kimia Analitik.
Surabaya:Jurusan Kimia FMIPA UNESA
Precipitation Titration
20
K. ATTACHMENT
PICTURE
EXPLANATION
Precipitation Titration
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Precipitation Titration
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L. CALCULATION
1. Known: V AgNO3
= V1= 5,6 mL; V2= 5,7 mL; V3= 6,0 mL
Mr of NaCl = 100 mL = 0,1 L
Mass of NaCl= 0,5 grams
Asked : N AgNO3?
Answer
=Mxn
= 0,085 M x 1 = 0,085 N
1) At V AgNO3= 5,6 mL
Molek AgNO3 = Molek NaCl
N1 . V1
= N2 . V2
N1 . 5,6 mL = 0,085 N . 10 mL
N1
= 0,151 N
2) At V AgNO3= 5,7 mL
Molek AgNO3 = Molek NaCl
N1 . V1
= N2 . V2
N1 . 5,7 mL = 0,085 N . 10 mL
N1
= 0,149 N
3) At V AgNO3= 6,0 mL
Molek AgNO3 = Molek NaCl
N1 . V1
= N2 . V2
N1 . 6,0 mL = 0,085 N . 10 mL
N1
= 0,141 N
N Average
= 0,147 N
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2. Known: V AgNO3 = V1= 0,5 mL; V2= 0,8 mL; V3= 0,5 mL
Asked : Percentage of Cl- on tap water?
Answer
:
m tap water
tap water = picknometer V
=
m
49,23
49,33
= 0,9 grams/mL
=.V
= 0,9 . 10
= 9 grams
Vaverage =
= 0,00882 N
M Cl- = 0,00882 N / 1 eq
= 0,00882 M
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% Cl
0,0464 grams
x 100
9 grams
= 0,0051%
Precipitation Titration
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