Sofia Daphney B. Inventado Mr.

Noel Sabarillo
1CHEA June 25. 2019
Group 9 July 1, 2019
Experiment 1: Group Separation of Metallic Cations
ABSTRACT
It is important, especially for chemists and scientists, to understand the different techniques in finding out
different components (one of this is ions) of a solution or compound in able to accomplish a goal on an
experiment. One of the factors that matters is its solubility and its relationship among its reagents. In this
experiment, it is expected to perform the separation of cations into five different groups of a solution using
its reagents with respect to its solubility components. The experiment used diluted HCl, Thioacetamide
(C2H5NS), NH4OH, NH4Cl, (NH4)2CO3, and different lab equipments, for the separation of the precipitates
and its supernatant. As the result of the experiment, the solution contained only groups I, III and IV as these
are the only precipitates present in the performed experiment.
INTRODUCTION
Chemistry made it possible for everyone to determine various cations in just one solution. Cations
are positively charged ions which was formed through the loss of electrons in an atom. Most of the metals
become cations, for the reason that they always lose electrons. Metallic Cations can be found and
identified in a solution through its separation. Several processes of this kind, separation, as well as the
exchange of cation to anion of metal atoms have made possible by several great chemists. Tompkins,
Khym and Cohn, and Kimura, Minami and Honda have reported systematic procedures for the separation
of fission products by means of cation exchange. (Waki & Yoshimura, 1961) However, in this laboratory
experiment, the separation of cation to the solution is our focus. With this, the process of qualitative
analysis is the tool for this report. The composition of relatively complex mixtures of metal ions can be
determined using qualitative analysis, a procedure for discovering the identity of metal ions present in the
mixture (rather than quantitative information about their amounts). (Petrucci et al., 2019)
Table 1: Corresponding Reagents of Group Cations and Its Products

Group Precipitating Agent Precipitates Formed

I Cold and dilute HCl chlorides

II H2S in dilute HCl sulfides

III H2S in NH4Cl Buffer Sulfides or Al(OH)3

IV (NH4)2CO3 in NH4Cl carbonates

 V None (soluble salts)

However, the group cations do not precipitate just because of magic, or grouped into different
groups just because different chemists want us to do so, but cations are grouped depending on its
solubility as salts. The solubility of cations as salt and the solubility product constant are factors that
determine whether a cation would be precipitated only as salt; such that IP or the ion product must be
greater than the solubility product constant (IP > Ksp) in able to conclude that the cation will be
precipitated as salt. Solubility-product constants can be used to devise methods for separating ions in a
solution by selective precipitation. Selective precipitation is used to form a solid with one of the ions in
solution without disturbing the other ions. (“Solubility Product Principle and Qualitative Analysis”, 2017)
Figure 1: Cations per Group & Separation of Metallic Cations into Groups

This experiment aims to determine the separation of the cations into five different groups with
use of its corresponding precipitating agent. It is expected to identify the following group cations present
in the unknown solution. Understanding the process and relationship between the concepts of compounds
and solution, and its composition, such as its solubility and the solubility product constant, must be
established.
MATERIALS AND METHODOLOGY
In order to perform the experiment, the following are the materials needed:
Solution of Group I-V Cations Test tubes
0.5M HCl Centrifuge Tubes
Thioacetamide (C2H5NS) Centrifuge
NH4OH Water Bath
 NH4Cl Litmus Papers
(NH4)2CO3 Stirring rod
The experiment was started in determining whether the solution have Group I cations and
separating it through its precipitates. In a 1mL solution which contains Group I-V solution, a cold dilute
HCl was added dropwise while stirring until the solution turns acidic. Acidity was determined through a
litmus paper. One more drop of HCl was added to the solution. White precipitate was formed in the
mixture, giving the reason to confirm that the solution contains at least one Group I cations.
In preparation for the other cation groups, cold water was run into the outside of the test tube and
then centrifuged for 3 minutes. The supernatant that may contain Group II-V cations was transferred into
another clean test tube, while the white precipitates were combined with 1mL distilled water, centrifuged
and combined with the supernatant liquid.
From the supernatant liquid formed, dilute NH4Cl was added while stirring until the solution
turns basic. Dilute HCl will be added to the basic solution one drop at a time until it turns acidic, then
another one of HCl was dropped in the mixture. 10 drops of C2H5NS was added, mixed and placed in a
test tube in a water bath for 5 minutes. After the water bath, 1 mL distilled water was added and 10 more
drops of C2H5NS then mixed. The solution was boiled again for 5 minutes and expected to have dark
precipitate. But since dark precipitate did not exist, group II cations also do not exist, proceeding to
separating group III cations.

Figure 2: Centrifugation Process Figure 3: Addition of C2H5NS Figure 4: Water bath of

solution
A clean evaporating dish was prepared and used to evaporate and reduce the volume to
approximately 1mL of the supernatant from the group II procedure. The supernatant was transferred to a
clean test tube then consecutively added then mixed. The supernatant was boiled in a water bath for 5
minutes. A precipitate was formed in this process, confirming group III cations. Cold water was poured
into the outside of the test tube and centrifuged for 3 minutes. The supernatant, which could possibly
contain group IV and V cations, was transferred into a clean test tube. The precipitate was washed with
1mL distilled water, centrifuged and combined with the supernatant liquid.
The recent supernatant was acidified using HCl, then boiled for 10 minutes in a water bath. After
this, the outside of the test tube was wetted with running cold water, then centrifuged for 3 minutes. The
supernatant was decanted to a clean test tube, then 10 drops of NH4Cl and dropwise of NH4OH was added
while mixing until mixture turns basic. 10 drops of C2H5NS was also added, then boiled for 5 minutes.
White precipitate was formed which this time, confirms presence of group IV cation.
RESULTS AND DISCUSSION
Through performing the procedure, the substances present in the unknown solution was
identified. In mixing the unknown solution and cold, diluted HCl, white precipitate was formed. This
means at least one group I cation was present in the unknown solution. Otherwise, precipitate for
determination in group II cations did not appear in the process. The solution containing diluted HCl,
NH4OH and C2H5NS remained clear and the dark precipitate was non-existent in the test tube. This
concludes that there is not even one group II cations in the solution.
Proceeding to the group III cation test, precipitate was formed this time. Releasing the test tube
containing the mixture from the water bath, dark precipitate was visibly formed which tells the
experiment that group III cations does exist in the solution. Same as group III cations, precipitate for
group IV cations was formed during the experiment making it possible to have at least one group IV
cation present in the solution. The remaining supernatant was considered as group V cations thus, group
V cations are soluble, and does not react to four of the reagents added in the solution/

Figure 5: Group III precipitate Figure 6: Group IV Precipitate

A group of cations are separated from another group of cations because each group corresponds
to a specific precipitating agent. Through quantitative analysis, the group cations interact with their
respective reagents or precipitating agent which undergoes through its own specific chemical reaction and
yielding its own product. Example of this is the reaction: AgNO3(aq) + HCl(aq) --> AgCl(s) + HNO3(aq)
The silver cation which reacts with cold, diluted HCl, forms a solid silver chloride. This reaction can
explained shortly as: the silver cation reacts only to a certain reagent such as hydrochloric acid, making it
different to any other cation groups, causing it to precipitate. Table 1 contains the groups of cations and
their precipitating agents together with its precipitates.
If a student decided to test a hypothesis on an aqueous solution whether it contains group II
action, it is incorrect to just made a solution acid with dilute HCl and bubble H5S gas in it. Even though a
precipitate was obtained, it is not a hypothesis for group II ions. First, we prepare a solution of the given
mixture, then we add group reagent of Ist group which converts the cations of Ist group into insoluble
chlorides and separate them as precipitate and then we test for IInd group cations in the filtrate of Ist group.
(Shrivastava, 2015) Based on the schematic diagram provided in figure 1, in order to make a mixture in
determining group II cations, a precipitating agent of group II cation must be involved. Its supernatant
liquid is used together with hydrogen sulfide in order to produce its precipitate, and a supernatant for the
groups III-IV. Instead of finding group II cations, group I cations will be formed instead.
It is important to wash the supernatant after the process of centrifugation and decantation because
there may always be rooms for contaminants. Contamination must be avoided as possible as it can in
order to have smooth process and clear result. Cross-contamination is one of the most common causes for
false observations leading to incorrect conclusions. (“Qualitative Analysis of Group I Ions”, 2019)
Contaminants may remove ions that might interfere with the succeeding procedures. The solid should be
rinsed more than once. Successive washings help remove more impurities. (“Rinsing the Solid”, 2000)
Ksp or the solubility product constant defines the equilibrium between a solid and it ions. It
describes equilibrium concentration of ions in a solution. Solubility product constants are used to describe
saturated solutions of ionic compounds of relatively low solubility. A saturated solution is in a state of
dynamic equilibrium between the dissolved, dissociated, ionic compound and the undissolved solid.
(SolubilityofThings, 2019) The higher the solubility product constant, the more soluble the compound.
(LibreTexts, 2019) Different cations produce different precipitation and separation due to its solubility
and solubility product constant. As for this experiment, the relationship between the ion product (IP) and
solubility product constant describes the precipitation of salts, as cation is precipitated as salt only if
IP>Ksp.
CONCLUSION
Classifying different ions in a solution is not as complex as it sounds. Different useful concepts
and techniques are gathered and understood, especially the solubility of different salts into different
solutions, and how it is related to ions. In order to classify ions, qualitative analysis must be used. Thus,
qualitative process usually utilizes the reaction characteristic for the given chemical species and interprets
the obtained results using a reasonable logical thinking process. Different cation groups have its own
precipitating agent which makes them possible to be detected in a certain solution using a certain manner.
REFERENCES
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