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Titrimetric Analysis

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18 views

Titrimetric Analysis

Uploaded by

aylin
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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TITRIMETRIC ANALYSIS

In titrimetric analysis
a solution of exactly known concentration,the
titrant,
is slowly added in small increments to
a solution of unknown concentration, the
analyte.
This process is called titration.

Types of titrations used in titrimetric analysis are :


1.Neutralization titrations
2.Oxidation-Reduction titrations
3.Complexation titrations
4.Precipitation titrations
Neutralization titrations:

Neutralization titration reaction can be expressed as


t T + aA  products
t :the number moles of titrant
a :is the number moles of analyte

equivalent number moles of the titrant =


equivalent number moles of the analyte
standard solutions:

• accuracy of the result  accuracy of the


concentration of the titrant

• Standard solutions: solutions of exactly known


concentrations

If the concentration of a solution is expressed in four


significant figures after the decimal point ( i.e
0.09805 M HCl solution) its concentration is
exactly known It is an std.HCl solution.
• Standard solutions can be prepared in two ways:
1- Direct method
2- Indirect Method
direct method:

A primary standard is an ultrapure compound


(99.9% pure) that serves as the reference material
for a titrimetric method of analysis.

Primary standards must

• be avaliable in a state of high purity.

• be stable in air and nonhygroscopic.

• have a known composition and must

• not undergo any change on heating.

• have a reasonably high molecular weight or


equivalent weight
Indirect method

Example: The commercially available NaOH (s) contains


some amount of Na2CO3 and Na2O, also it is hygroscopic,
and picks up moisture from the atmosphere very easily.

M NaOH=??????

• the concentration of such a solution is determined only by


titrating it aganist a primary standard solution and this
titration process is called standardization.

• the titrant solution which is standardized against a primary


standard is now called a secondary standard solution.
Equivalence point:
The point at which the amount of titrant is chemically equivalent
to the amount of analyte is called equivalence point.

Indicators:
In order to visualize a physical change at or near
equivalence point indicators are added to the analyte
solution.

End-point:
indicators usually give an observable physical
change ( usually a color change or formation of turbidity)
when a few drops excess of the titrant is added to
the reaction vessel beyond the equivalence point.

This point is called the end point of the titration


Titration error:

The difference in volumes of titrant consumed between the


equivalence point and the end point is known as
titration error,

E t = V ep – V eq

Vep = the actual volume of reagent required to reach the


end point
Veq = the theoretical volume to reach the equivalence
point.
Preparation of a Secondary Standard Solution and
Standardization of NaOH
Purpose:
0.1 M NaOH solution is prepared and then standardized
aganist primary standard potassium hydrogen phtalate,
KHP (KHC8H4O4 : 204.22g/mol. ) using phenolphtalein as
an indicator.

After all KHP is consumed one excess drop of NaOH reacts


with pht. And leads to a color change.
• Open structure of pht and its structure with NaOH

H2In In -2
• pH transition range for phenolphtalein is 8.0
(colorless) to 9.6 (pink).
Carbonate error:

• (1) CO2 (g) + 2OH- ⇌CO32- (aq) + H2O

• (2) CO32 - + H3O + ⇌ HCO3- + H2O

• in the overall titration, one mole of KHP reacts with two


moles of base instead of one. This leads to a systematic
error which is called carbonate error.
Phenolphtalein changes its color from pink to colorless in
reaction (2)

Things that can be done for preventing carbonate


error:

• The water used to prepare NaOH and KHP solution should


be boiled to expel the dissolved carbon dioxide gas.
• The NaOH solution should be stored in airtight containers to
prevent reabsorption of carbon dioxide.
• Deionized water can be used instead of distilled water since
deionized water does not contain significant amounts of
carbon dioxide.
WARNING: Concentrated
solutions of NaOH(and
KOH) are extremely
corrosive to skin. Safety
goggles, rubber gloves
and protective clothing
must be warn at all times.
Procedure:
I. Preparation of ~0.10 M HCl
1- Take a 1L of a storage bottle. Wash it well with soap or
detergent first. Rinse it out with tap and then with distilled
water couple of times.
2- Measure 1000 -mL of distilled water into a beaker. Heat the
water to boiling to expel CO2 and then cool it to room
temperature (cover it up with a watch glass during this
step)
3- Add about 12 mL of concentrated HCl (12M), mix it well and
store it in a stoppered bottle. Label the bottle with your
own name on it.
II. Standardization of HCL solution
1- Weigh duplicate ~0.20 to 0.25 g (± 0.1 mg) samples of
previously dried primary standard Na2CO3. Dissolve the
samples in ~100- mL distilled water; if it does not dissolve
quickly, you may warm the solution.

2 - Cool the solution to room temperature and add ~3 drops of


bromocresol green indicator, solution turns into blue.
Titrate it with HCl until green color is reached.
Na2(CO)3 + HCl  NaHCO3 + NaCl

3 - Heat and boil out CO2 gently. You should obtain a blue
color again at the end of this step.
H2CO3 (aq)  CO2(g)+ H2O(l)

Cool to room temperature, and continue the titration until


yellow color is reached.
NaHCO3 + HCl  H2CO3 +NaCl

4 -Calculate the molarity of HCl. Results should agree to about


two parts per thousand. If they do not agree, repeat the
procedure for the third time and take the averageof the two
closest results.
Procedure:

I. Preparation of ~0.10 M NaOH


1- Take a 1 L of a storage bottle. Wash it well with soap or
detergent first. Rinse it out with tap and then with distilled
water couple of times.
2- Measure 1000 -mL of distilled water into a beaker. Heat the
water to boiling, then cool. Add about 4 g of NaOH pellets
weighed on an watch glass, mix it well and store it in a
rubber stoppered bottle. (Caution : NaOH is very corrosive,
do not spill and if you do, wash it off immediately with an
excess of water.)

II. Standardization of ~0.10M NaOH


1- Weigh duplicate samples of 0.50-0.60 g of previously dried
standard KHP into 250- mL flasks. Dissolve each sample
in ~100- mL boiled distilled water.
2 - Cool to room temperature, add 2-4 drops of
phenolphthalein indicator. Titrate it with NaOH until the first
appearance of a permanent, pink color.
3 - Back titrate with your standard HCl if you miss the end
point. Calculate the molarity of NaOH solution.
4 - If runs do not agree to about two parts per thousand,
repeat for the third time and take the average of the two
closest results.
Preparation and

Standardization of a Secondary Standartd Solution, HCl


• Purpose: 0.1 M HCl solution is prepared. It is standardized
aganist a primary standard Na2(CO)3 using bromocresol green
as an indicator.

• 1st end-point
Na2(CO)3 + HCl  NaHCO3 + NaCl
blue greenish-blue

• 2nd end-point
NaHCO3 + HCl  H2CO3 +NaCl
greenish blue yellow

• in between these two end points, NaHCO3 (unreacted)


and H2CO3 buffer is formed which is almost in
greenish-blue color.
boiling

• H2CO3 (aq)  CO2(g)+H2O(l)


greenish blue blue
WARNING: Hydrochloric acid
is extremely corrosive.
Inhalation of vapour can cause
serious injury. Ingestion may be
fatal. Liquid can cause severe
damage to skin and eyes.
Safety goggles, rubber gloves
and protective clothing must
be warn at all times. Work
under the hood.

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