Inorganic Chemistry (ICH602S)

Practical 3
Detection of Anions

Bachelor of Science (07BOSC)

Name of Lecturer: Dr E.H.Hess

214098540 Blandine B.D Naris

Date: 9 August 2016 Due Date: 16 August 2016

Title
Detection of Anions

Aim
To identify the anions in various salt solutions.

Introduction
Identifying positive and negative ions, that is, cations and anions, in solutions whose
composition is unknown is known as qualitative analysis. Qualitative analysis is the
identification a sample's components. Unlike a quantitative analysis, we are not concerned with
the amount of a substance present in a sample but only with its identity. Ideally there would be
chemical tests that could be used to identify individual ions without interference by any other
ions. Qualitative analysis work begins with methods of identifying four common anions in
solution: PO4 3 , phosphate Cl , chloride SO4 2 -, sulfate , NO3 nitrate. The separation of ions
in solution can be accomplished by the addition of a precipitating agent that will selectively
react with an ion in the solution and not with others that may be present. The solid that is
produced can then be removed from the liquid by centrifugation and decanting. Because many
ions may behave similarly, separation of individual ions from a complex mixture is not usually
possible. Instead, a group of ions with similar reactivity may be separated by precipitation from
a larger mixture. After they are isolated in a solid, they must be further separated and reacted
to confirm each one's identity. There are several types of reactions that can be used to confirm
the presence of ions in solution. The most common are precipitation and complexation. In a
precipitation reaction, an ion in solution reacts with an added reagent to form a solid. Whether
a solid will form from a given reaction can be predicted by the solubility product constant (Ksp)
of the solid under the given conditions. Solubility product constants are the equilibrium
constants for the dissolution of an "insoluble" ionic solid in water. A low Ksp implies that the
compound does not dissolve to an appreciable degree in water. If the two ions are mixed in
solution, a precipitate will tend to form. If steps have been taken to remove ions that form
competing precipitates, the presence of a properly coloured solid can be used to confirm the
presence of a given ion. If several different precipitates remain, the conditions of the solution
can be manipulated to selectively redissolve one or more of the solids. When the equilibria
involved are well understood, selective precipitation can be a powerful tool in the identification
of unknown ions.
Complexation can also be used to determine the presence of an ion in solution. In a
complexation reaction, a cation (typically a metal) forms covalent bonds with one or more
ligands .A ligand is a neutral or negatively charged species that donates electrons to the
positively charged metal to form a coordinate covalent, or dative, bond. These complexes may
either be neutral or charged, depending on the charge on the metal and on the ligand. When a
complex forms it may not precipitate (charged complexes are often quite soluble in water, for
example), and the formation of a complex is one way in which an insoluble metal ion can be
forced to dissolve. Similarly, complex formation can also be used to separate a mixture of ions
by keeping one or more in solution while others precipitate. If the complex formed between a
metal ion and a specific ligand has a distinct colour, complex formation can be used to
demonstrate the presence of a specific metal ion by simply adding the ligand to the solution.
They are useful in confirming the presence of a single ion after separation has been achieved.
The tendency to form a complex can be determined by the formation constant (Kf) of the
reaction. Formation constants are defined as the equilibrium constant for the reaction of the
metal ion with the ligand(s) to form a complex. A large Kf implies a strong tendency for
complex formation Qualitative analysis schemes have been performed by introductory
chemistry students for many years. There are several different approaches to these experiments.
In one case, a step-by-step procedure is given, often in the form of a flow chart, which they can
use to isolate and identify unknown ions in solution. In another, it must first analyse known
solutions to determine how different anions will behave when reacted with various reagents.
They then compile these results into their own flow chart that they apply to their unknowns.
The experiments can be carried out on solutions containing mixtures of cations (same anion),
mixtures of anions (same cation) or on salt mixtures. The creation of the flow chart from scratch
is very valuable but is also a very time consuming process. The reactivity of the different ions
with precipitating agents can be predicted based on the Ksp of the salt formed if the two were
to react. Ksp's will be used in several salts to determine the best way to cause their separation.
Then a flowchart can be prepared to separate and identify these components. The flowchart
will be tested in the lab. Ideally, creating a flowchart for the separation of the entire mixture.
Because of time constraints, the flowcharts for the remaining species you need to separate will
be given.

Materials
Test tubes labeled 1 2 2 3 and A B C D E
Chemicals
Sulfate solution
Barium chloride
Silver nitrate
2M ammonia solution
Iodide solution
Unknown solution A B C D E
Nitric acid
Hydrochloric acid

Method
Part A
A few drops of barium chloride was added to 1 ml of sulfate solution and observed.
A few drops of silver nitrate solution was added to a test tube containing 0.5 - 1.0 ml of
chloride solution and observed. A portion of the product was transferred to another test tube
and 2M NH3H2O solution added drop by drop, and observed.
A few drops of silver nitrate solution was added to 1 ml of iodide solution and observed.
Part B
1. A few drops of dilute nitric acid (Irritant) was added to the unknown solutions (A, B and
C) followed by a few drops of silver nitrate solution. After observation, ammonia solution
was added.
2. To unknown solution D, a few drops of barium chloride solution (Toxic) was added,
followed by a few drops of dilute hydrochloric acid.
3. To unknown solution D, dilute hydrochloric acid was added.

Data
(1) Ba2+(aq) + SO42(aq) ==> BaSO4(s)
Any soluble barium salt + any soluble sulphate forms a white dense barium sulphate
precipitate

(2) Ag+(aq) + Cl(aq) ==> AgCl(s)

Any soluble silver salt + any soluble chloride gives a white silver chloride precipitate that
darkens in light

(3) Ag+(aq) + I(aq) ==> AgI(s)

Any soluble silver salt + any soluble iodide ==> yellow silver iodide precipitate

Results
Sample Test Performed
A 1. Nitric acid
2. Silver Nitrate
3. Ammonia
B 1. Nitric acid
2. Silver Nitrate
3. Ammonia
C 1. Nitric acid
2. Silver Nitrate
3. Ammonia
D 1.Barium chloride
2. Hydrochloric acid
E 1. Hydrochloric acid
Result of Test (observations etc) &
Identify Anion
1. Clear blue
2. Light blue with white precipitate
3. light blue with white precipitate
1. Yellow precipitate
2.
3.
1. Clear
2. yellow with precipitate
3. milky (cloudy) Yellow
1. White precipitate
2.
Colourless not precipitate

A Chloride ion
B Iodide ion
C Iodide ion
D Sulfate ion
E no results/ incomplete test

Discussion and Conclusion

Qualitative analysis is very important for the identification of anions in an unknown solution.
The expected the results of this experiment was that upon the addition of solutions into the
unknown solution colouration and precipitation would appear, and from this changes in colour
and presence of precipitation and good judgment would be made about the possible present
anion. The expectations where met, in each experiment there was a change in appearance
expect for the last experiment sample unknown solution E, where there was no colour change
nor was there a formation of a precipitate. Possible errors for this experiment include, mixing
up the pipettes for the different solutions. When the pipette allocated for iodide solution is used
to pipette another solution, chemical reactions will already take place. This will contaminate
the solutions and the results which are obtained will not reliable. Another error would be adding
the wrong solution, to draw up the flow chart it is important that the correct solutions a mixed
to give the right colouration and precipitate on which the results for the unknown experiment
results can be based upon. When the wrong solutions are made the flow chart used for
determine the anions would also be wrong. Several ways on how to improve the experiment is
to include trails. Including trails always gives a better results for the experiment, as it eliminates
errors. The setup could have been made more effective if the solutions were available to every
station so students work individually and reduce human errors.
The results of the experiment were satisfactory, the obtained results coincide with research
done, and the experiment served its purpose.

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