SYSTEMATIC SEPARATION AND IDENTIFICATION OF CATIONS OF GROUP 3

RAMÓN, Laura Juliana. VALBUENA, Jonathan David. Universidad Distrital Francisco José de
Caldas. Facultad de Ciencias y Educación. Licenciatura en Química. Análisis químico inorgánico.

ABSTRACT.

The process of identification of group 3 cations was carried out using the techniques of
precipitation, solubility and colorimetry according to the classification by groups of the ions and
based on the already known rules of solubility. It was possible to appreciate the formation of
precipitates, and solutions with different characteristics (color, solubility, pH etc.) Knowing in a
detailed way in the analytical processes that allow us to separate and determine the different cations.
On the other hand, a description of the experience held in the laboratory will be carried out, a
procedure that was followed for the identification and the results obtained which will be presented
with their respective analysis and conclusions.

KEYWORDS

Precipitation, pH, cations, solubility, Dissolution, precipitating agent, analytical marches,

qualitative analysis, colorimetry.

THEORIC FRAME.

Cation

They are the positive ions, that is to say, they
are atoms with a deficiency of electrons in the
orbitals more external. The elements that
normally have the greatest facility to
positively ionize, that is, the elements that
normally tend to lose electrons, are metals,
although this quality also occurs in non-
metals and elements. The size of the cations
is smaller than that of the neutral atoms and
the anions due to their loss of electrons from
their outermost layer.
A sequence of reagents is more or less
selective if it occurs with more or less
problems. A reagent is specific (more
selective) when it reacts with very few
cations and anions. They will be called
general reagents (less specific) when they
react with many cations and anions. The
selectivity of a reagent can be changed by
three different methods

The analytical march. Group 3

In Analytical Chemistry the analytical march
is a technical and systematic process (a series
of unitary operations), of identification of
inorganic ions in a solution by means of
chemical reactions in which the formation of
complexes or salts of unique and
characteristic color takes place.
To the solution containing the cations of
Group III and following we add NH3 and
NH4Cl, precipitating the cations of Group
IIIA: Fe (OH) 3 (red), Al (OH) 3 (white), Cr
(OH) 3 (green ), but not those of Group III
and following. To identify the cations of
Group IIA, NaOH and H2O2 are added, so
that Fe (OH) 3 does not dissolve, but the rest
give AlO2-, CrO2- (although with H2O2 it
gives CrO42-). To recognize iron, this
precipitate is dissolved in HCl and divided
into two positions: one of them is added with
KSCN (if there is iron, an intense scarlet red
precipitate is produced), and the other portion
is added with K4Fe ( CN) 6 (if iron exists, a
dark blue precipitate of prussia forms). To the
solution containing aluminum and chromium
we add HCl to neutral pH; then NH3 is added
and Al (OH) 3 precipitates; to be able to see
this disulfment, Congo red is added, we add
HCl, Congo red turns blue, we add NH3, red
Congo red becomes red again and Al (OH) 3
turns red.
On the solution, we added H2S and NH3,
leaving the cations of group IIIB: MnS
(pink), CoS (black), NiS (black) and ZnS
(white), leaving aside those of Groups IV and
V. On the precipitates we added HCl, leaving
on the one hand Mn2 + and Zn2 +, and on the
other NiS and CoS. In the first tube with
NaOH and H2O2 gives ZnO22- and a brown
precipitate of MnO2. To recognize the zinc it
is treated with H2S giving a white precipitate
of ZnS; The Montequi A and Montequi B
reagents can also be used to give a violet-
colored precipitate. In the second tube we
dissolve with regia water, giving Ni2 + and
Co2 +. One of the portions is neutralized with
NH3 and continues adding to basic pH and
then add dimethylglyoxime; if Ni2 + exists, a
pink precipitate forms. For Co2 + it is first
neutralized with NH3, buffered with acetic
acid and sodium acetate together with KSCN;
if we add acetone the acetonic phase takes a
blue color.
DATA CHART.
CATION
GROUP 3
Known Unknown
𝐵𝑎2+ + +
𝐶𝑎2+ + -
𝑀𝑔2+ + +
Table 1. information cations
DATA.
In practice for the identification of the ions
corresponding to group 3 the reactions were
carried out by means of precipitating agents
by means of which we have the reactions.
1. (NH4)2SO4(aq) + Ba2+(aq) + Ca2+(aq)
+ Mg2+(aq) → BaSO4(aq) +
CaSO4(aq) + MgSO4(aq)
2. K2CrO4(aq) + BaSO4(aq) → BaCrO4↓
3. 3Ca2+(aq) y 3Mg2+(aq) +
(NH4)2C2O4(aq) → CaC2O4↓ +
MgC2O4↓
4. Mg2+(aq) + 2NaOH(aq) + Magnesòn
→ Mg(OH)2(aq)↓ (color azul)
When adding the acid, we showed that there
is a white precipitate in which are found the
phosphates of the alkali metals which are
insoluble, therefore the existence of these
ions is evident in the precipitate. Then we
will perform two procedures on the one hand
we will seek to separate each ion from the
phosphates in the form of precipitate that we
obtained and on the other we will try to find
the ion Zn ^ (2+) that we need to check its
presence in the solution.
To the solution obtained from the ions that
are soluble we will add acetic acid giving as a
result the following:
S3 + 𝐶𝐻3 𝐶𝑂𝑂𝐻 → 𝑍𝑛𝑁𝐻4 𝑃𝑂4 + S4
By adding the acetic acid and this is not
soluble with the complex that forms the zinc
we see the formation of a white precipitate
and a solution that contains the ions of group
4 which we will talk about later. What we
will proceed to do is that the precipitate we
obtained previously we added some reagents
in order to more clearly and accurately
demonstrate the ion Zn ^ (2+). We will add to
the HCl solution in order to obtain a diluted
solution, solubilized and colorless to be able
to perform the respective tests
2+
𝑍𝑛𝑁𝐻4 𝑃𝑂4 + HCl → 𝑍𝑛 + HCl + 𝐻𝑃𝑂42−
Now we will divide the solution in two to the
first we will add [𝐹𝑒(𝐶𝑁)6 ]3− and to the
second we add Cu ions (2+) and a few drops
of the Hg complex 𝐻𝑔{𝑆𝐶𝑁4 }2−
Z𝑛2+ + [𝐹𝑒(𝐶𝑁)6 ]3− → 𝑍𝑛3 [𝐹𝑒(𝐶𝑁)6 ]
This complex when coming into contact with
the solution will give us a hazel color
precipitation.
Z𝑛2+ + 𝐶𝑢2+ + 𝐻𝑔{𝑆𝐶𝑁4 }2−
When adding to the solution containing the
zinc ions, the solutions of 𝐻𝑔{𝑆𝐶𝑁4 }2− y
𝐶𝑢2+ must have formed a lilac precipitate; but
at the time of performing the practice some
inconveniences arose which resulted in a
negative test for the Zn(2+) ion. We do not
know exactly what factor was due although it
is believed that it was due to the
concentration of some of the reagents As
previously mentioned, we will now take the
precipitate where the phosphates are
contained and proceed to perform the
recognition of each of the ions. First we will
take the precipitate and add HCl in order to
solubilize the precipitate and create a
colorless solution. In which the ions are
found as chlorides.
𝐵𝑎3 (𝑃𝑂4 )2 + 6𝐻𝐶𝑙 → 3𝐵𝑎𝐶𝑙2 + 2𝐻3 𝑃𝑂4
𝐶𝑎3 (𝑃𝑂4 )2 + 6𝐻𝐶𝑙 → 3𝐶𝑎𝐶𝑙2 + 2𝐻3 𝑃𝑂4
𝑀𝑔3 (𝑃𝑂4 )2 + 6𝐻𝐶𝑙 → 3𝑀𝑔𝐶𝑙2 + 2𝐻3 𝑃𝑂4
After having achieved a complete solubility
we proceed to incorporate the
(𝑁𝐻4 )2 𝑆𝑂4 Resulting in sulfates of the
different ions, in the case of Barium this is an
insoluble sulfate therefore during the reaction
it will form a white precipitate where the
barium ion will be and apart you will have a
solution where all the other ions are 𝐶𝑎2+ /
𝑀𝑔2+
(𝑁𝐻4 )2 𝑆𝑂4 + 𝐵𝑎 𝐶𝑙2 → 𝐵𝑎𝑆𝑂4 + 2𝑁𝐻4 𝐶𝑙
(𝑁𝐻4 )2 𝑆𝑂4 + 𝐶𝑎 𝐶𝑙2 → 𝐶𝑎𝑆𝑂4 + 2𝑁𝐻4 𝐶𝑙
(𝑁𝐻4 )2 𝑆𝑂4 + 𝑀𝑔𝐶𝑙2 → 𝑀𝑔𝑆𝑂4 + 2𝑁𝐻4 𝐶𝑙
With the barium sulfate that we obtained we
can affirm, that we obtained ions of Ba(2+),
which is a white precipitate; but if we want to
specify the existence of ions Ba(2+) we can
add a solution of 𝐾2 𝐶𝑟𝑂4 to the precipitate
and we proceed to carry out a brief heating,
which will give us a yellow coloration in the
solution and a stronger yellow color in the
precipitate.
𝐵𝑎𝑆𝑂4 + 𝐾2 𝐶𝑟𝑂4 → 𝐵𝑎𝐶𝑟𝑂4 + 𝐾2 𝑆𝑂4
The solution has an orange color due to the
conversion 𝐶𝑟𝑂42− en 𝐶𝑟 2 𝑂72− but Ba (2+)
is also present, which is colorless. With this
solution a flame test is carried out. A greenish
yellow color confirms the presence of Ba
(2+). In these two ways or through these two
substances we can demonstrate the presence
of Ba(2+) ions in the solution.
As we obtained a solution of the procedure
performed previously by adding (𝑁𝐻4 )2 𝑆𝑂4 in
which the ions of Ca (2+) and Mg (2+) are
contained, we will try to identify each ion
separately, so we will continue to perform
different procedures to obtain the different
solutions.
To this solution we are going to add
ammonium oxalate ((NH4) 2C2O4) and
sodium acetate (C2H3NaO2) and centrifuge
it; The presence of a white precipitate and a
colorless solution will be evident. In the
precipitate we will find the calcium ions and
in the solution the magnesium ions. The
precipitate formed on centrifugation
corresponds to Calcium oxalate (CaC2O4).
For the solution in which the Magnesium ions
are, two tests will be carried out to observe a
change of color by means of some identifying
reagents that are responsible for coloring the
solution showing us the ions that are present.
2 NaOH + Mg → Mg (OH) 2 + 2 Na
CONCLUSIONS
 The systematic analysis of cations
brings as a result the knowledge
of solubility in each situation.
When we talked about
compounds such as phosphates in
an ammonia solution in group 3.
We use the techniques of the
solubility rules for the knowledge
of the precipitating action of this
anion in the barium. Therefore we
find the qualitative presence of
this ion in conjunction with
another for the recognition of it.
 The formation of complexes in the
production of substances is evident
in this formation of complex ions,
which are formed by the union of
compounds by a coordination bond.
In this ion we will find the union of a
central atom, called metallic cation
linked by other molecular entities
called ligands.
 The rules of solubility and
precipitation are very important
which allow us to identify the ions
by groups by reactions with
precipitating agents generating
changes from a reaction either as a
precipitate, or change of color in the
solution, by means of centrifugation
techniques or heating which allow
the identification of ions of the same
group.
BIBLIOGRAPHY
 Martí, F. B. (2002). Química
analítica cualitativa. Editorial
Paraninfo.
 DE CATIONES, M. A., & Y III, G. I.
PRÁCTICA 3.
 Luna, M. C., Moyano, P. L., De La
Rosa, P. G., & Espinoza, V. P.
Química Analítica.