Lorenzo Carlos Baquiran, Charles Ashley Jimenez, Giana Leigh Mamaradlo, Clarisa May Oranda
Groups 9 & 10, Chem 18.1 MAB2, Sir Gabriel Luis Neri
November 26, 2015
I.
Abstract
A qualitative test is designed to identify the presence of a certain species in a sample. In this procedure,
the unknown is systematically subjected to a number of different reagents, taking advantage of the different
chemical properties of ions, such as solubility in a solution or complex formation, to ascertain the species in
the unknown. By predetermining the results of a specific reaction when a specific ion is present, we are able
to identify the ions present in a solution. In the test for cations, groups are selectively precipitated using
different reagents. For example, group I cations are separated from groups II to V by subjecting the solution
of unknown to HCl. This procedure takes advantage of the fact that group I cations are the only cation group
to form insoluble chlorides. Confirmatory tests then follow which will point to only a single species. In the test
for anions, characteristic precipitates and complexes are formed with specific reagents.
II.
III.
Keywords: Qualitative, unknown, precipitation, complex formation, confirmatory test, cation, anion.
Introduction
insoluble. For the samples that are sparingly
soluble or insoluble in water, the solubility is tested
Qualitative analysis is the determination of the
in the following solvents until a suitable solvent is
presence or absence of a certain species in a
found. These solvents were tried in order. The
sample. Even before the development of more
solvents were: a) 6M HCl b) concentrated HCl, c)
advanced techniques such as spectroscopy,
6M HNO3, d) concentrated HNO3, e) aqua regia
chemists are already doing different methods of
(concentrated HCl-concentrated HNO3 mixture).
qualitative analysis; that is, the sample is treated
with various reagents to test for reactions
characteristic of certain ions in solution, such as
PREPARATION OF THE CATION TEST
complex formation or precipitation. In analysis of
SOLUTION
cations, the ones that are tested for are essentially
the manipulation of solubility equilibria and
A pinch of the sample was dissolved in the
complex formation. We can group certain cations
appropriate solvent. The resulting solution was
by their tendencies to precipitate under given
then used as the cation test solution.
conditions, effectively separating a group of ions
from others and permitting confirmatory tests. On
GROUP I CATIONS
the other hand, analysis for anions also involves
formation of precipitates or reactions with strong
To 2 mL of the test solution, 8 drops of 6M HCl
acid. Confirmatory tests are also possible for
is added. The solution is then put in a centrifuge to
anions due to characteristic reactions and
separate group I cations. The decantate is saved
complexes that each anion may form with a given
for the separation and identification of group II
set of reagents.
cations. Group I cations are the only cations that
form insoluble chlorides (white precipitate). This
IV.
Methodology and Discussion
allows us to separate group I cations from group 24. If no precipitate is formed, it means there are no
SOLUBILITY TEST
group I cations in the unknown.
The solubility of the sample was determined by
Ag+ + Cl- -> AgCl
treating a very small portion of the finely powdered
substance (not exceeding the size of a grain of
Pb+2 + 2Cl- -> PbCl2
rice) with 2 drops of water and then stirred for 25
to 30 seconds. If the solid dissolved completely,
2 Hg2+ + 2Cl- -> Hg2Cl2
this meant that the sample is soluble in water. For
the samples that did not dissolve, 5 more drops of
To the white precipitate, 2 mL of hot water is
water were added and it was stirred for another 30
added. The solution is put in a centrifuge and
seconds. If the salt dissolved, it is somewhat
decanted while still hot. Another 2 mL of hot water
soluble in water. For the samples that still did not
is added and the solution is once again put in a
dissolve, 10 more drops of water were added and
centrifuge and decanted. The precipitate, to be
it was stirred once again. If the sample dissolved
called 1-A, is set aside. If a precipitate forms in the
during that time, it is considered to be sparingly
centrifugate, it is put in a hot water bath until the
soluble in water. For the samples that still did not
precipitate dissolves. 2 drops of 1M K2CrO4 is then
dissolve, it is said to be very slightly soluble or
added to the clear hot solution. The solubility of
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GROUP II CATIONS
The decantate from the separation of group I
cations is checked to have a pH of 0.5. If it is not,
the pH is adjusted using NaOH or HCl dropwise. 2
mL of 5% thioacetamide is then added to the
solution and stirred. It is then put in a boiling water
bath for 10 minutes. If any group II cations are
present in the test sample, a precipitate, black or
yellow, should form. Hydrogen Sulfide is generated
by hydrolyzing thioacetamide. This process is
hastened by the acidity of the solution.
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OF
THE
ANION
TEST
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C2O42-
Effervescence
2-
S
Cl-
Br-
I-
Purple fumes,
turns to a brown slurry
CrO42-
Orange solution
NO2-
(C2O42-),
Anion
CO32-
C2O42-
C2O42 2CO2
S2-
Cl-
Br-
I-
CrO42-
NO2-
Visible Result
NO3CH2COO
No visible reaction
(NO2-),
For nitrite
acidify 5 drops of the test
solution by adding 6M HOAc dropwise, then add
5 drops 0.1M K3Fe(CN)6. Let stand for one minute
and add 1 drop FeCl3. A deep red precipitate
indicates the presence of nitrite in the sample.
For permanganate (MnO4-), this confirmatory
test is unnecessary if the sample solution is
colorless. Using 2 drops of the test solution, add 2
drops H2O, 2 drops 0.02M Na2C2O4 and 2 drops
6M H2SO4. The disappearance of the color of the
solution within 30 seconds indicates the presence
of permanganate.
Discussion
Preliminary Tests for Anions
In the sulfuric acid test, the anion present in the
sample will dictate the reaction that will occur. The
table below explains the visible reaction for each
anion and the corresponding chemical equation for
each.
Anion
NO3-
CH2COO-
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colored
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VI.
Brown,
References
Theodore
E.,
Lemay,
Eugene
H.,Bursten,Bruce E.,Murphy, Catherine
(2008). Chemistry: The Central Science
(11th ed.), New York: Prentice Hall, ISBN
0136006175
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