Applications of Acid-Base/Neutralization Titration

https://www.youtube.com/watch?v=lHcBLp
Kjeldahl Method for McS4M

Organic Nitrogen
Determination
Step 1. Digestion
The sample is oxidized in
hot, concentrated H2SO4
and turns black
To convert Carbon and
Hydrogen to CO2 and H2O
To convert Amides and
Amines to NH4+
To convert . . . Azo, Azoxy
and Nitro Group to N or its
oxide

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Catalysts
Potassium Sulfate (K2SO4) increases the
boiling point of sulfuric acid
Mercuric Oxide (HgO) increases the rate of
reaction
Selenious Acid (H2SeO3) best catalyst

Applications of Acid-Base/Neutralization Titration

Kjeldahl Method for
Organic Nitrogen
Determination
Step 2. Distillation
The oxidized solution is
cooled and then treated withh
NaOH to liberate ammonia
gas:NH4+ + HO- NH3(g)
+ H 2O
Glass or Porcelain beads are added to avoid bumping
In some modifications, hydrogen peroxide is added to decompose
organic matrix formed
If mercuric oxide, HgO is used as a catalyst, it is necessary to add
sodium thiosulfate, Na2S2O3 to precipitate mercuric sulfide, HgS.
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Applications of Acid-Base/Neutralization Titration

Kjeldahl Method for
Organic Nitrogen
Determination
Step 3. Titration
1.Using an excess amount
of HCl: NH3 + HCl
NH4Cl
The excess HCl is
determined using a standard
NaOH solution: HCl +
NaOH NaCl +
H 2O

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2. Ammonia distilled is collected in a

boric acid solution
NH3 + H3BO3 NH4+ + H2BO3-2
Titrate the H3BO3NH3 solution with
standard acid
H2BO3-2 + H3O+ H3BO3 +
H 2O

Applications of Acid-Base/Neutralization Titration

Kjeldahl Method for
Organic Nitrogen
Determination
Percentage Protein in the
Sample
% protein = % N * f
f= 5.70 (cereals)
6.25 (meat products)
6.38 (dairy products)
1. A 5.8734 g sample of beef was analyzed for
its N content and the liberated NH3 was
collected in a 50 ml of 0.4691 M HCl and a
12.55 ml back titration with 0.0256 M NaOH
was required. Calc. the % protein in the
beef sample.
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Kjeldahl Method
1. A 0.5843 g sample of a plant food preparation was
analyzed for its content by the Kjeldahl method, the
liberated NH3 being collected in 50.00 mL of 0.1062 M
HCl. The xcss acid required an 11.89 mL back titration
with 0.0975 M NaOH. Express the result of this analysis
in terms of %N and % (NH4)2(SO4)

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Two Titration/Double Indicator Method for Carbonate

and Carbonate Mixtures
Volume Relations in Carbonate Titrations
Constituents in the
sample

For equal volume of

sample

For single sample

NaOH

Vo-ph = Vo-mr

Vph-mr = 0

Na2CO3

Vo-ph = 1/2Vo-mr

Vo-ph = Vph-mr

NaHCO3

Vo-ph = 0; Vo-mr >0

Vo-ph =0

NaOH, Na2CO3

Vo-ph > 1/2Vo-mr

Vo-ph > Vph-mr

Na2CO3, NaHCO3

Vo-mr < 1/2Vo-mr

Vo-ph < Vph-mr

General Relationship:
Amt. NaOH + Amt. Na2CO3 = (Vo-ph) (CHCl)
Amt. Na2CO3 + Amt. NaHCO3 = (Vph-mr) (CHCl)
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[Applications of Neutralization
Titrations]
Two Titration/Double Indicator Method for Carbonate and
Carbonate Mixtures
First case: (equal volume of sample)
Sample
1
Carbonate
sample

w/ ph
Titrate with
stdzd. HCl
Record: Vo-mr

Sample
2
w/ mr
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Titrate with
stdzd. HCl
Record: Vo-ph

[Applications of Neutralization
Titrations]
Example: (First case)
1. A sample consisting of Na2CO3, NaHCO3 and inert matter
weighs 1.179 g. It is titrated with 0.1N HCl with phenolphthalein
as the indicator and the soln became colorless after the addition
of 24 ml. Another duplicate sample was titrated with HCl using
methyl orange as indicator. It required 50.25 ml of the acid for
the color change. What is the % of NaHCO3 and Na2CO3 in the
sample?

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[Applications of Neutralization
Titrations]
Solution:
From the general relationship (1)
=0
Amt. NaOH + Amt. Na2CO3 = (Vo-ph) (CHCl)
= 24 ml(0.1mmol/ml)= 2.4 mmol
Since Vo-mo Vo-ph = Vph-mo
From the general relationship (2)
Amt. Na2CO3 + Amt. NaHCO3 = (Vph-mo) (CHCl)
2.4 mmol + Amt. NaHCO3= (50.25-24)ml (0.1mmol/ml)
Amt. NaHCO3= 0.225 mmol
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[Applications of Neutralization
Titrations]

2011 Pearson Education, Inc.

[Applications of Neutralization
Titrations]
Two Titration/Double Indicator Method for Carbonate and
Carbonate Mixtures
Second case: (single sample)

1. Titrate with
stdzd. HCl
Record: Vo-ph

Carbonate
sample

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2. Titrate with
stdzd. HCl
Record: Vph-mr

[Applications of Neutralization
Titrations]
Example: (Second case)
1. A sample consisting of Na2CO3, NaOH and inert matter
weighs 1.179 g. It is titrated with 0.2239 M HCl with
phenolphthalein as the indicator and the soln became colorless
after the addition of 45.62 ml. Methyl orange is then added and
12.85 ml more of the acid are needed for the color change.
What is the composition of the sample?

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[Applications of Neutralization
Titrations]
Solution:
From the general relationship (2)
=0
Amt. Na2CO3 + Amt. NaHCO3 = (Vph-mo) (CHCl)
= 12.85 ml(0.2239 mmol/ml)= 2.8771 mmol
From the general relationship (1)
Amt. NaOH + Amt. Na2CO3 = (Vo-ph) (CHCl)
Amt. NaOH + 2.8871 mmol = 45.62 ml (0.2239mmol/ml)
Amt. NaOH = 7.3272 mmol
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[Applications of Neutralization
Titrations]

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[Problems]
1. A 4.017 g sample that may contain NaOH, NaHCO3 or
Na2CO3 or a permissible mixture of the bases was
dissolved in enough water to make 500 ml soln.
Titration of a 50 ml aliquot using the two-indicator
method requires 14.42 ml of 0.1052 M HCl to reach the
phenolphthalein endpt. and an additional 26.58 ml to
reach the methyl orange endpt. Calc. the percentage of
each.

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