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Volumetric Analysis
(aka Titrations)
Related Reading (Harris, 5th Ed.)
6.1 6.3
9.3 9.6
10.4
Volumetric Analysis
Review of Titrations
A titration is any procedure where increments of a known reagent solution (the titrant)
is added to a solution containing an unknown amount of the analyte until the reaction is
complete, called the equivalence point:
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Types of Titrations
There are two categories of titrations
direct titration:
back titration:
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Example
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=
5
Volumetric Analysis
If too much indicator is added in a titration, interactions with the indicator can become
significant and indicator error can be introduced.
The endpoint of a titration is generally found using an indicator. Indicators are either
They are added at such low concentration that they have no direct effect on any
equilibrium or redoximorphic state in solution but greatly affect the color of the
solution.
On a fundamental level, indicators act in a manner similar to buffers!
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Volumetric Analysis
Acid/Base Indicators
Thymol Blue
Most acid-base indicators are weak organic acids or bases whose various protonated
species have different colors.
pH
pH indicators act as buffers in response to pH changes, only showing a clear color
change over the effective range of the buffer (1 pH unit).
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Volumetric Analysis
pH Indicators
The closer the pKa of an indicator is to the pH at the equivalence point of the titration,
the smaller the titration error
Low pH
Color
Transition
pH range
High pH
Color
Low pH
Color
Transition
pH range
High pH
Color
Methyl violet
yellow
0.02.0
blue-violet
Bromocresol purple
yellow
5.26.8
purple
Leucomalachite green
yellow
0.0-2.0
green
Bromothymol blue
yellow
6.07.6
blue
Thymol blue
red
1.22.8
green
Neutral red
red
6.88.0
yellow
Methyl yellow
red
2.94.0
yellow
Phenol red
yellow
6.88.4
red
Bromophenol blue
yellow
3.04.6
purple
Cresol Red
yellow
7.28.8
redpurple
Congo red
blueviolet
3.05.0
red
colorless
7.38.7
greenblue
red
3.14.4
orange
yellow
8.09.6
blue
yellow
3.85.4
blue
Phenolphthalein
colorless
8.310.0
fuchsia
Methyl red
red
4.46.2
yellow
Thymolphthalein
colorless
9.310.5
blue
Litmus
red
4.5-8.3
green
Alizarine Yellow R
yellow
10.212.0
red
Azolitmin
red
4.58.3
blue
Leucomalachite green
green
11.614
colorless
Indicator
Methyl orange
Bromocresol green
Indicator
Naphtholphthalein
Thymol blue
Volumetric Analysis
Consider the use of thiocyanate (SCN-) as a complexation indicator for the presence of
free Fe3+ ions in solution:
3+ + +
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Dichlorofluorescein
+ charged
ionic atmosphere
Adsorbed DCF
+ +
+
+
+
+
AgCl
Free
DCF
+ + +
Often, both of these types of indicators are also pH sensitive with amphiprotic forms,
so pH must be carefully controlled when used.
10
Acid/Base Chemistry
Note: It is also possible to use a weak base and its conjugate acid (or a strong acid) to make a buffer.
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Acid/Base Chemistry
3. Using a pH meter, adjust the pH to the desired value with small volumes of 1 M
NaOH or 1 M HNO3.
4. Transfer the buffer to a volumetric flask (along with rinse from any containers) and
bring to the desired volume.
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