Experiment 7

Volumetric Determination of an Unknown Chloride

Abstract

In addition to acid-base titrations, complexometric titrations, redox

titrations, and precipitation titrations are also available. This experiment

involves titration by precipitation using the Mohr Method.

Introduction

Volumetric analyses are usually faster and easier to perform than analyses by weight.

However, they are re- liable only if several conditions are met. First, there must be a single

known reaction occurring when the solutions are mixed, so that the reactants may be

quantitatively related to each other by the stoichiometry of the reaction. Second, the reaction

must be fast. Since the analysis involves mixing two solutions, the reac- tion must

essentially be over in the time of mixing. Finally, there must be some method of determining

when the reactants have just completely reacted with each other. This is called determining

the end point of the reaction.

Volumetric quantitative analyses are usually performed by a procedure called titration.

Titration is a tech- nique in which one reagent, called the titrant, is dispensed from a burette

into a flask containing a fixed amount of a second reagent. The addition is continued until

exactly enough titrant has been added to react completely with the second reagent.

End points are usually observed as distinct visible color changes in solution. The color

changes are often due to substances called indicators, which are added to the solution being
titrated. Indicators may be any of a variety of chemical substances that fulfill two

requirements. First, the color change observed must occur at the end point of the reaction.

Second, the color change must be sharp; one extra drop (0.03m1) of titrant should cause the

color change to be visible.

Once the end point of the titration has been detected, the concentration or composition

of the unknown sample can be calculated using the concentration and measured

volume of titrant used to reach the end point of the reaction, and the stoichiometry of

the reaction involved.

This experiment illustrates a typical analysis by titration. The percent of Cl - in a salt

will be determined by the Mohr method, which involves titration of the chloride

sample with a solution of silver nitrate, AgNO3. The reaction that occurs between the

sample and titrant is the formation of silver chloride, AgCl(s), which has a very low

solubility:

Ag+ (aq) + Cl-(aq) → AgCl(s)

Since the solubility of AgCl is so low, it is assumed reaction (l) goes to completion. As the

titration pro- ceeds, the added Ag+ is rapidly removed from solution. It reacts with Cl−

forming AgCl, a white solid, which gives the solution a cloudy appearance. At the end point
4 2 4
of the reaction, all of the Cl− in the sample has been precipitated as AgCl. Any further

addition of AgNO3 results in an excess of Ag+ in the solution. It is the first excess of Ag+

that must be "seen" to indicate the end point of the reaction. The indicator used to detect the

excess Ag+ is chromate ion, CrO 2-, which forms a red precipitate, Ag CrO (s), with any

excess Ag+.

2 Ag+ (aq)
4 + CrO
2-
(aq) → Ag2CrO4(s)

The chromate ion is added at the beginning of the titration as K2CrO4. The solubility of

AgCl and Ag2CrO4 at 25°C are 0.0018 grams/liter and 0.014 grams/liter respectively;
Ag2CrO4 is about ten times more soluble than AgCl. As AgNO3 is added to the solution

containing both Cl- and CrO42- the solubility of AgCl is ex- ceeded first and a precipitate of

AgCl forms. As long as Cl- remains in the solution, the Ag+ concentration never builds up to

the point where a precipitate of Ag2CrO4 can form. Once the chloride is completely re-

moved, as AgCl, the Ag+ concentration increases markedly with further addition of titrant.

At the end point of the titration the concentrations of Ag+ and CrO2-4 in the solution are such

that the solubility of Ag2CrO4 is exceeded and this precipitate forms.

As the titration proceeds, the reddish Ag2CrO4 sometimes forms where the titrant hits the

solution due to a local excess of Ag+. It re-dissolves when the solution is mixed thoroughly.

The end point of the titration oc- curs when the formation of Ag2CrO4 is permanent, as

seen by the first definite faint red coloration of the precipitate that does not fade.

At the end point of the titration the moles of AgNO3 required for the reaction is calculated

from the known molarity and volume of AgNO3 used. Equation (1) indicates that one mole of

Ag+ reacts with one mole of Cl-. From this, the number of moles, weight, and percentage of

Cl- in the sample is calculated using the atomic weight of chlorine and the original weight of

sample

Experimental

At first we need a 50mL burette and an unknown solid chloride sample. Weigh a piece of

paper itself and with 0.1g of sample on the weighing paper on the analytical balance.

Calculating these reading, will give us the actual mass of the sample and it should be about

0.1g. Then the next step will be transferring the sample to an Erlenmeyer flask. By

following the above steps we have to make total of 3 samples and they will be labeled as #1,

#2, and #3. Now we have to dissolve these samples in water by adding 50mL of distilled

water into each flask. Add 1 mL of 1M K2CrO4 solution. In a clean, dry, 250 mL beaker,

obtain about 100 mL of 0.05M AgNO3. Now we need a clean burette rinsed thoroughly once
by distilled water and twice by AgNO3 and then the burette will be filled with AgNO3. Then

we will keep adding AgNO3 in the samples and swirl until the sample turns reddish. The

difference between initial and final burette reading will give us the used amount of AgNO3.

Finally we have to calculate the moles of AgNO3 (and thus Ag+) used, the moles of Cl-

titrated, the grams of Cl-, and the percent chloride in the unknown to the correct number of

significant figures warranted by the data.

Results
Sample #1 Sample Sample
#2 #3
Weight of weighing paper + sample 0.516 g 0.507 g 0.511 g

Weight of weighing paper 0.909 g 0.405 g 0.404 g

Weight of sample to be titrated 0.107 g 0.108 g 0.107 g

Final burette reading 48 mL 40.20 mL 37.80 mL

Initial burette reading 0.50 mL 0.20 mL 0.80 mL

Volume of AgNO3 used 47.50 mL 90 mL 37 mL

Molarity of AgNO3 0.05 M

Moles of AgNO3 used 2.38 × 10-3 mol 1.00× 10-3 mol 1.50× 10-3 mol

Moles of Cl- titrated 2.380× 10-3 mol 2.00× 10-3 mol 1.85× 10-3 mol

Grams of Cl- titrated 0.084g 0.0704g 0.0656g

%Cl in unknown 66.2% 69.5% 66.5%

Average % Cl- 67.3%

Consequence’’

1, The weights of 3 samples of unknown chloride salt are 0.1030g, 0.1470g, 0.1130g.
2, The volumes of AgNO3 solution used to titrated into 3 samples of unknown chloride
salt solutions are 0.03730L, 0.05250L, 0.04040L.

The most significant thing in

the lab is the endpoint of the
titration. If the endpoint is
missed, then the all
calculations will be wrong. It
is important to get the
appropriate colour, in
this case the pink colour, in
order to get precise values.
The dichlorofluorescein which
was
used as an indicator helps to
determine the endpoint by
giving the colour.
During the lab, there were
some errors. As the first source
of error, the loss of some of
the samples when recording
its mass and taking it off of
the analytical balance can be
defined. Since the sample was
lost when removing the sample
from the balance this resulted
in a higher recorded mass of
the sample. Having an
inaccurate mass of sample
affects the
moles of Ag+ and moles of
Cl- in the sample. This error
can be avoided by measuring
the
mass of the sample 2 times,
before starting the lab.
Secondly, when adding to the
flask the
distilled water not all of the
solution came out of the
beaker. This means that some
of the
solutions were lost since it was
stuck inside the beaker and
would not go into the flask,
which
caused the loss in a mass of the
solution. This affects the mass
of the solution, the moles of
Ag+ and moles of Cl- in the
sample. This error can be
avoided by using a tool to help
remove
all the solution from the beaker
and getting out as much as
possible. By fixing all of these
errors a much more accurate
calculation of the
concentration of Cl- in the
unknown could
have been calculated.
The most significant thing in
the lab is the endpoint of the
titration. If the endpoint is
missed, then the all
calculations will be wrong. It
is important to get the
appropriate colour, in
this case the pink colour, in
order to get precise values.
The dichlorofluorescein which
was
used as an indicator helps to
determine the endpoint by
giving the colour.
During the lab, there were
some errors. As the first source
of error, the loss of some of
the samples when recording
its mass and taking it off of
the analytical balance can be
defined. Since the sample was
lost when removing the sample
from the balance this resulted
in a higher recorded mass of
the sample. Having an
inaccurate mass of sample
affects the
moles of Ag+ and moles of
Cl- in the sample. This error
can be avoided by measuring
the
mass of the sample 2 times,
before starting the lab.
Secondly, when adding to the
flask the
distilled water not all of the
solution came out of the
beaker. This means that some
of the
solutions were lost since it was
stuck inside the beaker and
would not go into the flask,
which
caused the loss in a mass of the
solution. This affects the mass
of the solution, the moles of
Ag+ and moles of Cl- in the
sample. This error can be
avoided by using a tool to help
remove
all the solution from the beaker
and getting out as much as
possible. By fixing all of these
errors a much more accurate
calculation of the
concentration of Cl- in the
unknown could
have been calculated.
The most significant thing in
the lab is the endpoint of the
titration. If the endpoint is
missed, then the all
calculations will be wrong. It
is important to get the
appropriate colour, in
this case the pink colour, in
order to get precise values.
The dichlorofluorescein which
was
used as an indicator helps to
determine the endpoint by
giving the colour.
During the lab, there were
some errors. As the first source
of error, the loss of some of
the samples when recording
its mass and taking it off of
the analytical balance can be
defined. Since the sample was
lost when removing the sample
from the balance this resulted
in a higher recorded mass of
the sample. Having an
inaccurate mass of sample
affects the
moles of Ag+ and moles of
Cl- in the sample. This error
can be avoided by measuring
the
mass of the sample 2 times,
before starting the lab.
Secondly, when adding to the
flask the
distilled water not all of the
solution came out of the
beaker. This means that some
of the
solutions were lost since it was
stuck inside the beaker and
would not go into the flask,
which
caused the loss in a mass of the
solution. This affects the mass
of the solution, the moles of
Ag+ and moles of Cl- in the
sample. This error can be
avoided by using a tool to help
remove
all the solution from the beaker
and getting out as much as
possible. By fixing all of these
errors a much more accurate
calculation of the
concentration of Cl- in the
unknown could
have been calculated.
The most significant thing in
the lab is the endpoint of the
titration. If the endpoint is
missed, then the all
calculations will be wrong. It
is important to get the
appropriate colour, in
this case the pink colour, in
order to get precise values.
The dichlorofluorescein which
was
used as an indicator helps to
determine the endpoint by
giving the colour.
During the lab, there were
some errors. As the first source
of error, the loss of some of
the samples when recording
its mass and taking it off of
the analytical balance can be
defined. Since the sample was
lost when removing the sample
from the balance this resulted
in a higher recorded mass of
the sample. Having an
inaccurate mass of sample
affects the
moles of Ag+ and moles of
Cl- in the sample. This error
can be avoided by measuring
the
mass of the sample 2 times,
before starting the lab.
Secondly, when adding to the
flask the
distilled water not all of the
solution came out of the
beaker. This means that some
of the
solutions were lost since it was
stuck inside the beaker and
would not go into the flask,
which
caused the loss in a mass of the
solution. This affects the mass
of the solution, the moles of
Ag+ and moles of Cl- in the
sample. This error can be
avoided by using a tool to help
remove
all the solution from the beaker
and getting out as much as
possible. By fixing all of these
errors a much more accurate
calculation of the
concentration of Cl- in the
unknown could
have been calculated.
The most significant thing in
the lab is the endpoint of the
titration. If the endpoint is
missed, then the all
calculations will be wrong. It
is important to get the
appropriate colour, in
this case the pink colour, in
order to get precise values.
The dichlorofluorescein which
was
used as an indicator helps to
determine the endpoint by
giving the colour.
During the lab, there were
some errors. As the first source
of error, the loss of some of
the samples when recording
its mass and taking it off of
the analytical balance can be
defined. Since the sample was
lost when removing the sample
from the balance this resulted
in a higher recorded mass of
the sample. Having an
inaccurate mass of sample
affects the
moles of Ag+ and moles of
Cl- in the sample. This error
can be avoided by measuring
the
mass of the sample 2 times,
before starting the lab.
Secondly, when adding to the
flask the
distilled water not all of the
solution came out of the
beaker. This means that some
of the
solutions were lost since it was
stuck inside the beaker and
would not go into the flask,
which
caused the loss in a mass of the
solution. This affects the mass
of the solution, the moles of
Ag+ and moles of Cl- in the
sample. This error can be
avoided by using a tool to help
remove
all the solution from the beaker
and getting out as much as
possible. By fixing all of these
errors a much more accurate
calculation of the
concentration of Cl- in the
unknown could
have been calculated.
3, The molarity of AgNO3 solution is 0.05M. So the moles of AgNO3 used to titrated
into 3 samples of unknown chloride salt solutions are
0.03730L*0.05mol/L=0.001865mol
0.05250L*0.05mol/L=0.002625mol
0.04040L*0.05mol/L=0.002020mol

3, The moles of Cl- in 3 samples of unknown chloride salt solutions are 0.001865mol,
0.002625mol, 0.002020mol.

4, The grams of Cl- in 3 samples of unknown chloride salt solutions are

0.001865mol*35.45g/mol=0.06611g
0.002625mol*35.45g/mol=0.09306g
0.002020mol*35.45g/mol=0.07161g

5, The percentage of Cl- in 3 samples of unknown chloride salt solutions are

0.06611g/0.1030g*100%=64.18%
0.09306g/0.1470g*100%=63.31%
0.07161g/0.1130g*100%=63.37%

6, The average percentage of Cl- in 3 samples of unknown chloride salt solutions is

(64.18%
+63.31%+63.37%)/3=63.62%
Discussion

The most significant thing in

the lab is the endpoint of the
titration. If the endpoint is
missed, then the all
calculations will be wrong. It
is important to get the
appropriate colour, in
this case the pink colour, in
order to get precise values.
The dichlorofluorescein which
was
used as an indicator helps to
determine the endpoint by
giving the colour.
During the lab, there were
some errors. As the first source
of error, the loss of some of
the samples when recording
its mass and taking it off of
the analytical balance can be
defined. Since the sample was
lost when removing the sample
from the balance this resulted
in a higher recorded mass of
the sample. Having an
inaccurate mass of sample
affects the
moles of Ag+ and moles of
Cl- in the sample. This error
can be avoided by measuring
the
mass of the sample 2 times,
before starting the lab.
Secondly, when adding to the
flask the
distilled water not all of the
solution came out of the
beaker. This means that some
of the
solutions were lost since it was
stuck inside the beaker and
would not go into the flask,
which
caused the loss in a mass of the
solution. This affects the mass
of the solution, the moles of
Ag+ and moles of Cl- in the
sample. This error can be
avoided by using a tool to help
remove
all the solution from the beaker
and getting out as much as
possible. By fixing all of these
errors a much more accurate
calculation of the
concentration of Cl- in the
unknown could
have been calculated.
The most significant thing in
the lab is the endpoint of the
titration. If the endpoint is
missed, then the all
calculations will be wrong. It
is important to get the
appropriate colour, in
this case the pink colour, in
order to get precise values.
The dichlorofluorescein which
was
used as an indicator helps to
determine the endpoint by
giving the colour.
During the lab, there were
some errors. As the first source
of error, the loss of some of
the samples when recording
its mass and taking it off of
the analytical balance can be
defined. Since the sample was
lost when removing the sample
from the balance this resulted
in a higher recorded mass of
the sample. Having an
inaccurate mass of sample
affects the
moles of Ag+ and moles of
Cl- in the sample. This error
can be avoided by measuring
the
mass of the sample 2 times,
before starting the lab.
Secondly, when adding to the
flask the
distilled water not all of the
solution came out of the
beaker. This means that some
of the
solutions were lost since it was
stuck inside the beaker and
would not go into the flask,
which
caused the loss in a mass of the
solution. This affects the mass
of the solution, the moles of
Ag+ and moles of Cl- in the
sample. This error can be
avoided by using a tool to help
remove
all the solution from the beaker
and getting out as much as
possible. By fixing all of these
errors a much more accurate
calculation of the
concentration of Cl- in the
unknown could
have been calculated.
The most significant thing in
the lab is the endpoint of the
titration. If the endpoint is
missed, then the all
calculations will be wrong. It
is important to get the
appropriate colour, in
this case the pink colour, in
order to get precise values.
The dichlorofluorescein which
was
used as an indicator helps to
determine the endpoint by
giving the colour.
During the lab, there were
some errors. As the first source
of error, the loss of some of
the samples when recording
its mass and taking it off of
the analytical balance can be
defined. Since the sample was
lost when removing the sample
from the balance this resulted
in a higher recorded mass of
the sample. Having an
inaccurate mass of sample
affects the
moles of Ag+ and moles of
Cl- in the sample. This error
can be avoided by measuring
the
mass of the sample 2 times,
before starting the lab.
Secondly, when adding to the
flask the
distilled water not all of the
solution came out of the
beaker. This means that some
of the
solutions were lost since it was
stuck inside the beaker and
would not go into the flask,
which
caused the loss in a mass of the
solution. This affects the mass
of the solution, the moles of
Ag+ and moles of Cl- in the
sample. This error can be
avoided by using a tool to help
remove
all the solution from the beaker
and getting out as much as
possible. By fixing all of these
errors a much more accurate
calculation of the
concentration of Cl- in the
unknown could
have been calculated.
The most significant thing in
the lab is the endpoint of the
titration. If the endpoint is
missed, then the all
calculations will be wrong. It
is important to get the
appropriate colour, in
this case the pink colour, in
order to get precise values.
The dichlorofluorescein which
was
used as an indicator helps to
determine the endpoint by
giving the colour.
During the lab, there were
some errors. As the first source
of error, the loss of some of
the samples when recording
its mass and taking it off of
the analytical balance can be
defined. Since the sample was
lost when removing the sample
from the balance this resulted
in a higher recorded mass of
the sample. Having an
inaccurate mass of sample
affects the
moles of Ag+ and moles of
Cl- in the sample. This error
can be avoided by measuring
the
mass of the sample 2 times,
before starting the lab.
Secondly, when adding to the
flask the
distilled water not all of the
solution came out of the
beaker. This means that some
of the
solutions were lost since it was
stuck inside the beaker and
would not go into the flask,
which
caused the loss in a mass of the
solution. This affects the mass
of the solution, the moles of
Ag+ and moles of Cl- in the
sample. This error can be
avoided by using a tool to help
remove
all the solution from the beaker
and getting out as much as
possible. By fixing all of these
errors a much more accurate
calculation of the
concentration of Cl- in the
unknown could
have been calculated.