Module 5 : Titrimetric

Methods of Analysis
Rachel Anne E. Lagunay March 12, 2021
Department of Chemistry
College of Science and Mathematics
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 What’s Ahead
v Aspects of Volumetric Titrimetry (Standard Solution, Equivalence
Point, End Point, Primary Standard)

v Gravimetric Titrimetry

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 Learning Goals..
v Ability to compute concentration, % purity of analytes from
titrimetric data

v Perform experiment to prepare dilute solutions of acid and base to be

used in volume ratio determination, standardization and unknown
titrations

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 Titrimetric Methods of Analysis
Ø based upon measuring the amount of reagent of known concentration that is
consumed by the analyte.

q Volumetric Titrimetry – involves measuring the volume of a solution of

known concentration that is needed to react essentially and completely with the
analyte.

q Gravimetric Titrimetry – differs only in that the mass of the reagent is

measured instead of its volume.
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 Titrimetric Methods of Analysis
Ø based upon measuring the amount of reagent of known concentration that is
consumed by the analyte.

q Coulometric Titrimetry – the reagent is a constant direct electric current of

known magnitude that is directly or indirectly reacts with the analyte, here, the
time required to complete the electrochemical reaction is measured.

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 General Aspects of Volumetric Titrimetry
q Titrimetric methods of analysis are capable of rapid and convenient analyte
determinations with high accuracy and precision.

q Titrimetric analysis is based on the complete reaction between the analyte and
a reagent, the titrant:
aA + tT  products

where A and T represent the analyte and titrant, respectively, and a and t
are the stoichiometric coefficients.

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 Quantitative Determination of the Analyte
Concentration Requires the Following:
q There is a stoichiometric reaction between analyte and titrant. This reaction
should be fast and complete, and the values of a and t must be known.

q The concentration of the titrant solution, CT, must be known accurately.

q The titrant solution must be standardized either by preparing it using a primary

standard or, more commonly, titrating it against a solution prepared with a
primary standard.

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 General Aspects of Volumetric Titrimetry

q Titrations are often classified by the nature of this titration reaction: acid-base,
redox, precipitation and complexation reactions are the most common reaction
types.

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 Quantitative Determination of the Analyte
Concentration Requires the Following:

q The endpoint volume must be measured accurately using an appropriate

chemical indicator or instrumental method. If an instrumental method is used
to follow the progress of the titration reaction, a titration curve may be
generated, which allows for the analysis of mixtures and/or the detection of
interferences.

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 Titration Solution
q Standard solution is a reagent of exactly known concentration that is used in a
titrimetric analysis
q Primary standard is an ultrapure compound that serves as the reference
material for a titrimetric method of analysis.
Ø Requirements:

v high purity; established methods for confirming purity should be available.

v stability towards air

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 Titration Solution
Ø Requirements:

v absence of water of hydration so the composition of the solid does not

change with variation in humidity
v ready availability at modest cost
v reasonable solubility in the titration medium
v reasonably large molar mass so that the relative error associated with
weighing the standard is minimized

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 Titration Solution
q Secondary standard is a compound whose purity has been established by
chemical analysis and that serves as the reference material for a titrimetric
method of analysis.
q Titration is a process in which a standard reagent is added to a solution of an
analyte until the reaction between the analyte and the reagent is judged to be
complete.
q Back-titration is a process in which the excess of a standard solution used to
consume an analyte is determined by titration with a second standard solution.
q

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 Titration Solution
q Standardization is a process in which the concentration of a volumetric solution
(secondary standard) is determined by using it to titrate a known mass of a primary
standard or an exactly known volume of another secondary standard solution.
q The equivalence point is the point in a titration when the amount of added standard
reagent is exactly equivalent to the amount of analyte.
q The end point is the point in a titration when a physical change occurs that is
associated with the condition of chemical equivalence.
q The difference in volume or mass between the equivalence point and the end point is
the titration error

titration error: Et = Vep-Veq

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 Titration Solution

q Indicators are added to the analyte

solution to produce an observable
physical change (the end point) at or
near the equivalence point: change in
color or appearance or disappearance
of turbidity

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 Desirable Properties of Standard Solutions
q The ideal standard solution for titrimetric method will:
v be sufficiently stable so that it is only necessary to determine its
concentration once.
v react rapidly with the analyte so that the time required between
the additions of reagent is minimized.
v react more or less completely with the analyte so that satisfactory
endpoints are realized.
v undergo a selective reaction with the analyte that can be
described by simple balanced equation.

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 Methods of Establishing the Concentration
of Solutions
q Direct Method – here, a carefully weighed quantity of a primary
standard is dissolved in a suitable solvent and diluted to an exactly
known volume in a volumetric flask.

q Standardization – here, the titrant to be standardized is used to

titrate:
a.) a weighed quantity of primary standard,
b.) a weighed quantity of secondary standard,
c.) a measured volume of another standard solution

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 Titrations can be classififed by the type of reaction
diffirent types of titration reaction include:
q Acid-base titration is based on the neutralization reaction between
the analyte and an acidic or basic titrant. These most commonly use
a pH indicator, a pH meter, or a conductance meter to determine the
endpoint.

q Redox titration is based on an oxidation-reduction reaction between

the analyte and titrant. These most commonly use a potentiometer or
a redox indicator to determine the endpoint. Frequently either the
reactants or the titrant have a color intense enough that an additional
indicator is not needed.

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 Titration Methods
q Complexometric titration is based on the formation of a complex
between the analyte and the titrant.

q The chelating agent EDTA is very commonly used to titrate metal

ions in solution. These titrations generally require specialized
indicators that form weaker complexes with the analyte.

q A common example is Eriochrome Black T for the titration of

calcium and magnesium ions.

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 Titration Methods
• Precipitation titration. The titrant forms an insoluble product with
the analyte. Example is the titration of chloride ion with silver nitrate
solution to form silver chloride precipitate. Indicators can be used to
detect the end point or potential of the solution can be monitored
electrically.

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 1. Mass percentage
2. Volume percentage
3. Parts per million; parts per billion; pptrillion
4. mole fraction
5. Molality, m
6. Molarity, M
7. Normality, N

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 Calculate the molar concentrations of 1.00 ppm solution Pb2+ (207.2 g/mol).

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 What weight of Pb(NO3)2 (331.2 g/mol) will have to be dissolved in 1.00 liter of
water to prepare a 100 ppm Pb2+ (207.2 g/mol) solution?

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Calculate the molar concentration of ethanol in aqueous solution that contains
2.30 g of ethanol (46.07 g/mol) in 3.50 L of solution.

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Calculate the analytical and equilibrium conc. of the solute species in aq. solution that
contains 285 mg of trichloroacetic acid Cl3CCOOH (163.4 g/mol) in 10.0 mL (the acid is
73% ionized in water).
Note:
Analytical Molarity – is the total number of moles of a solute, regardless of its chemical
state, in 1 L of solution; specifies a recipe by which the solution can be prepared

Equilibrium Molarity – is the molar concentration of a particular species in a solution at

equilibrium

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Calculate the analytical and equilibrium conc. of the solute species in aq. solution that contains 285 mg
of trichloroacetic acid Cl3CCOOH (163.4 g/mol) in 10.0 mL (the acid is 73% ionized in water).

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Calculate the analytical and equilibrium conc. of the solute species in aq. solution that contains 285 mg
of trichloroacetic acid Cl3CCOOH (163.4 g/mol) in 10.0 mL (the acid is 73% ionized in water).

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Describe the preparation of the following:
a. 2.00 L of 0.108 M BaCl2 from BaCl22H2O (244.3 g/mol)
Describe the preparation of the following:
b. 500 mL of 0.0740 M Cl– solution from solid BaCl22H2O

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 A solution is prepared by dissolving 1.26 g AgNO3 (169.9 g/mol) in a 250. mL volumetric flask
and diluting to volume.
a.) Calculate the molarity of the silver nitrate solution.
b.) How many millimoles AgNO3 were dissolved?

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A solution is prepared by dissolving 1.26 g AgNO3 (169.9 g/mol) in a 250. mL volumetric flask
and diluting to volume.
a.) Calculate the molarity of the silver nitrate solution.

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A solution is prepared by dissolving 1.26 g AgNO3 (169.9 g/mol) in a 250. mL volumetric flask
and diluting to volume.
b.) How many millimoles AgNO3 were dissolved?

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Calculate the concentration of potassium ions in grams per liter after mixing 100. mL of 0.250 M KCl
and 200. mL of 0.100 M K2SO4. (Assume volumes are additive)
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Given the reaction below:
a. H2SO4 + 2NaOH → 2H2O + Na2SO4
b. 5 C2O42- + 2 MnO4- + 16 H+ → 10 CO2 + 2 Mn2+ + 8 H2O
Balance each reaction and calculate the equivalent weights of the following substances in terms of its
formula weights when used in the above reaction.
a. H2SO4 (98.08 g/mol) NaOH (40.00 g/mol)
b. KMnO4 (158.03 g/mol) Na2C2O4 (134.02 g/mol)

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Given the reaction below:
a. H2SO4 + 2NaOH → 2H2O + Na2SO4
b. 5 C2O42- + 2 MnO4- + 16 H+ → 10 CO2 + 2 Mn2+ + 8 H2O
Balance each reaction and calculate the equivalent weights of the following substances in terms of its
formula weights when used in the above reaction.
a. H2SO4 (98.08 g/mol) NaOH (40.00 g/mol)

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Given the reaction below:
a. H2SO4 + 2NaOH → 2H2O + Na2SO4
b. 5 C2O42- + 2 MnO4- + 16 H+ → 10 CO2 + 2 Mn2+ + 8 H2O
Balance each reaction and calculate the equivalent weights of the
following substances in terms of its formula weights when used in the
above reaction.
a. H2SO4 (98.08 g/mol) NaOH (40.00 g/mol)

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Given the reaction below:
a. H2SO4 + 2NaOH → 2H2O + Na2SO4
b. 5 C2O42- + 2 MnO4- + 16 H+ → 10 CO2 + 2 Mn2+ + 8 H2O
Balance each reaction and calculate the equivalent weights of the
following substances in terms of its formula weights when used in the
above reaction.
b. KMnO4 (158.03 g/mol) Na2C2O4 (134.02 g/mol)

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Given the reaction below:
a. H2SO4 + 2NaOH → 2H2O + Na2SO4
b. 5 C2O42- + 2 MnO4- + 16 H+ → 10 CO2 + 2 Mn2+ + 8 H2O
Balance each reaction and calculate the equivalent weights of the
following substances in terms of its formula weights when used in the
above reaction.
b. KMnO4 (158.03 g/mol) Na2C2O4 (134.02 g/mol)

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Given the reaction below:
a. H2SO4 + 2NaOH → 2H2O + Na2SO4
b. 5 C2O42- + 2 MnO4- + 16 H+ → 10 CO2 + 2 Mn2+ + 8 H2O
Balance each reaction and calculate the equivalent weights of the
following substances in terms of its formula weights when used in the
above reaction.
b. KMnO4 (158.03 g/mol) Na2C2O4 (134.02 g/mol)

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Given the reaction below:
a. H2SO4 + 2NaOH → 2H2O + Na2SO4
b. 5 C2O42- + 2 MnO4- + 16 H+ → 10 CO2 + 2 Mn2+ + 8 H2O
Balance each reaction and calculate the equivalent weights of the
following substances in terms of its formula weights when used in the
above reaction.
b. KMnO4 (158.03 g/mol) Na2C2O4 (134.02 g/mol)

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 mass solute = M x V x MWsolute

mass solute = N x V x MWsolute

a
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Calculate the (a) molarity and (b) normality of a 13.0% (by weight) H2SO4 solution with a
density of 1.090. (c) To what volume should 100. mL of this solution be diluted to prepare
1.50 N solution?

(a)
 Calculate the (a) molarity and (b) normality of a 13.0% (by weight) H2SO4 solution with a
specific gravity of 1.090. (c) To what volume should 100 mL of this solution be diluted to
prepare 1.50 N solution?

(b)

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 Calculate the (a) molarity and (b) normality of a 13.0% (by weight) H2SO4 solution with a
specific gravity of 1.090. (c) To what volume should 100 mL of this solution be diluted to
prepare 1.50 N solution?

(c)

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A water sample is 0.00026 M in CaCO3 (100.09 g/mol). Calculate the concentration in
ppm.

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 Gravimetry Titrimetry
q mass of titrant is measured rather than the volume
q Weight titration – a balance and a solution dispenser are substituted
for a buret and its markings
q Calculations associated with Weight Titrations
q Weight molarity. Mw
v no. of moles of reagent in 1 kg of solution
v no. of mmoles solute in 1 g of solution
Cw = nA/msoln
Thus, aqueous 0.1 Mw NaCl contains 0.1 mol of the salt in 1 kg of
soln or 0.1 mmol in 1 g of soln
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 Titration of 0.824 g of potassium hydrogen phthalate (KHP) (FW 204.23) required 38.314
g of NaOH solution to reach the end point detected by phenolphthalein indicator. Find
the weight molarity of the NaOH solution.

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 Treatment of Titration Data

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Titration of 1.0000 g of potassium hydrogen phthalate (KHP) (204.23 g/mol) required
38.35 mL of NaOH solution to reach the end point detected by phenolphthalein indicator.
Find the molarity and normality of the NaOH solution.

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Titration of 1.0000 g of potassium hydrogen phthalate (KHP) (204.23 g/mol) required
38.35 mL of NaOH solution to reach the end point detected by phenolphthalein indicator.
Find the (a) molarity and (b) normality of the NaOH solution. N

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An approximately 0.10 M HCl is prepared by 120 fold dilution of concentrated HCl. It is
standardized by titrating 0.1876 g of dried primary standard sodium carbonate:
CO32– + 2H+  H2O + CO2
The titration required 35.86 mL acid. Calculate the molarity and normality of the HCl
solution.

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 Calculate the normality of NaOH and HCl given the following data:
1.000 m L of HCl  0.7005 mL NaOH
mass of KHP used = 0.4998 g
total volume of NaOH used = 21.00 mL
total volume of HCl used = 1.25 mL

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A solution of HClO4 was standardized by dissolving 0.3745 g of primary standard HgO (FW 216.59) in
a solution of KBr:
HgO + 4Br– + H2O  HgBr42– + 2OH-–
The liberated OH– required 37.79 mL of the acid to be neutralized. Calculate the molarity of the
HClO4 solution.

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A solution of KMnO4 is standardized using pure Na2C2O4 as the primary standard
5C2O42– + 2MnO4– + 16H+  10CO­2 + 2Mn2+ + 8H2O
A sample of Na 2 C 2 O 4 (134.00 g/mol) weighing 0.3248 g requires 44.22 mL of KMnO 4 for
titration. Calculate the (a) molarity and (b) normality of the KMnO4 solution.

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A solution of KMnO4 is standardized using pure Na2C2O4 as the primary standard
5C2O42– + 2MnO4– + 16H+  10CO­2 + 2Mn2+ + 8H2O
A sample of Na 2 C 2 O 4 (134.00 g/mol) weighing 0.3248 g requires 44.22 mL of KMnO 4 for
titration. Calculate the molarity and normality of the KMnO4 solution.

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A solution of KMnO4 is standardized using pure Na2C2O4 as the primary standard
5C2O42– + 2MnO4– + 16H+  10CO­2 + 2Mn2+ + 8H2O
A sample of Na 2 C 2 O 4 (134.00 g/mol) weighing 0.3248 g requires 44.22 mL of KMnO 4 for
titration. Calculate the molarity and normality of the KMnO4 solution.

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 Aliquot:
A sample of pure CaCO3 (FW 100.09) weighing 0.4148 g is dissolved in 1:1 hydrochloric acid, and the
solution is diluted to 500.0 mL in a volumetric flask. A 50.00 m L aliquot is withdrawn with a pipet and
placed in an Erlenmeyer flask. The solution is titrated with 40.35 mL of an EDTA solution using
Eriochrome Black T (EBT) indicator. Calculate the molarity of the EDTA solution. The reaction in the
titration is:
Ca2+ + EDTA  Ca[EDTA]

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 Aliquot:
A sample of pure CaCO3 (FW 100.09) weighing 0.4148 g is dissolved in 1:1 hydrochloric acid, and the
solution is diluted to 500.0 mL in a volumetric flask. A 50.00 m L aliquot is withdrawn with a pipet and
placed in an Erlenmeyer flask. The solution is titrated with 40.35 mL of an EDTA solution using
Eriochrome Black T (EBT) indicator. Calculate the molarity of the EDTA solution. The reaction in the
titration is:
Ca2+ + EDTA  Ca[EDTA]

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 Aliquot:
A sample of pure CaCO3 (FW 100.09) weighing 0.4148 g is dissolved in 1:1 hydrochloric acid, and the
solution is diluted to 500.0 mL in a volumetric flask. A 50.00 m L aliquot is withdrawn with a pipet and
placed in an Erlenmeyer flask. The solution is titrated with 40.35 mL of an EDTA solution using
Eriochrome Black T (EBT) indicator. Calculate the molarity of the EDTA solution. The reaction in the
titration is:
Ca2+ + EDTA  Ca[EDTA]

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 of a solution is the mass (in mg) of a substance that is chemically
equivalent to 1 mL of the solution.
Calculate the Na2CO3 titer in mg/mL of a 0.1200 M solution of HCl.

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 of a solution is the mass (in mg) of a substance that is chemically
equivalent to 1 mL of the solution.

Calculate the normality of a solution of NaOH which has a KHP (FW 204.23) titer of 20.05
mg/mL.

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 Percent Purity
q To analyze a sample of unknown purity the analyst weighs accurately a
portion of the sample, dissolves it appropriately, and titrates it with a
standard solution. If the titration reaction is
a A + t T  products
v where a molecules of the analyte, A, react with t molecules of the
titrant, T, then at the equivalence point

t x mmol A  a x mmol T
OR meq A  meq T
a
mmol A  x mmol T
t
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 Percent Purity
 If V and M represents the volume (mL) and molarity (mmol/mL),
respectively, of the titrant, and FW A is the formula weight of the
analyte, then

a
mmol A  x V x M
t
a
mg A  x V x M x MW A
t

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 Percent Purity
 The percent by weight of A is

mg analyte
% A x 100
mg sample
a
x V (mL) x M (mmol / mL) x MWA (mg / mmol )
% A t x 100
weight of sample (mg )

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 Percent Purity
• In terms of normality, N of the titrant and equivalent weight, EWA,
of the analyte:

meq A  meq T
mg A  V x N x EWA
mg analyte
% A x 100
mg sample
V (mL) x N (meq / mL) x EWA (mg / meq)
% A x 100
weight of sample ( mg )

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 Percent Purity
• The organic matter in a 3.776 g sample of a mercuric ointment is
decomposed with HNO3. After dilution, the Hg2+ is titrated with 21.30 mL of a
0.1144 M solution of NH4SCN. Calculate the percent Hg (FW 200.59) in the
ointment. The titration involves the formation of a stable neutral complex,
Hg(SCN)2:
Hg2+ + 2SCN–  Hg(SCN)2

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 Kjeldahl Method for Notrigen Determination

In the Kjeldahl method for nitrogen, the element is converted into

NH3, which is then distilled into a known volume of standard acid.
There is more than enough acid to neutralize the NH3, and the excess is
titrated with standard base.

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A 1.047 g sample of canned tuna was analyzed by the Kjeldahl method. The
liberated NH 3 required 24.65 mL of 0.1180 M HCl. Calculate the percentage
nitrogen and protein in the sample. Assume that the protein factor is 6.25, i.e. %
protein = % N x 6.25

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A 1.047 g sample of canned tuna was analyzed by the Kjeldahl method. The
liberated NH 3 required 24.65 mL of 0.1180 M HCl. Calculate the percentage
nitrogen and protein in the sample. Assume that the protein factor is 6.25, i.e. %
protein = % N x 6.25

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 The ammonia from a 1.325 g sample of fertilizer is distilled into 50.00 mL of 0.1015 M
H2 SO4 , and 25.32 mL of 0.1980 M NaOH is required for back-titration. Calculate the
percentage of nitrogen in the sample.

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 The ammonia from a 1.325 g sample of fertilizer is distilled into 50.00 mL of 0.1015 M
H2 SO4 , and 25.32 mL of 0.1980 M NaOH is required for back-titration. Calculate the
percentage of nitrogen in the sample.

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Thank you
for
listening!!!
RAE LAGUNAY, 07/22/20|