Hypothesis-testing Method Design Laboratory Activity Sheet

CEBU DOCTORS’ UNIVERSITY

COLLEGE OF ARTS AND SCIENCES

Physical Sciences Department

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Laboratory Activity Sheet No. 1
Title of the Experiment: Cations Analysis

I. Objectives:

1. To be able to follow an analytical scheme to separate and identify ions in a known mixture
and;

2. to be able to use this scheme in order to identify the unknown mixed with the 1st group cations.

II. Scenario

Each group was given a sample to be analyzed and this sample contains different cations. The
cations are Ag+, Hg2+2, Pb+2, Cu+2, Sn+2, Bi+3, Al+3, Cr+3, Co+2, Mn+4, Mg+2, Ba+2, Ca+2. They are categorized
according to their precipitants. Group 1 cation, Silver group are Ag +, Hg2+2, Pb+2 and they are precipitated
with 6M HCl. Group 2 cations, Copper-Arsenic group are Cu +2, Sn+2, Bi+3 and they are precipitated with
H2S in acidic medium, Group3 cations, Aluminum- iron group are Al +3, Cr+3, Co+2, Mn+4. These ions are
precipitated with H2S in basic medium like 6M NH 4OH and group 4 cations, Alkaline Earth metals are
Mg+2, Ba+2, Ca+2., Sr+2 and they are precipitated using (NH 4)2CO3. Design a method to separate Silver
group cation from the rest of the group of cations. What type of analysis is being used, qualitative or
quantitative? What method of analysis is employed to separate each group of ions? What are the
necessary reagents you need to do this task? After separating the Silver group from the rest of the
analytes, what group of cations are in the solution form or the spectator ions? Keep the precipitate for
confirmatory tests. What common laboratory operation is used to separate the precipitate from the
solution? To the spectator ions, a reagent was added to precipitate group 2 cations. What is the chemical
formula of this reagent and what is its condition, acidic or basic? What could be the possible precipitates
produced during precipitation reaction? How will you separate the precipitate from its solution? Keep the
precipitate for confirmatory tests. To the solution add another reagent to precipitate out the group 3
cations. Repeat the procedure until all the group of cations have been separated. Always save the
precipitate for further tests.

https://www.youtube.com/watch?v=LTBEvBO4cTA&t=106s

Watch this video to help you do this task.

II. Hypothesis-Testing Method Design

A. Problem:
1. How do you separate different groups of cations from one mixture?
 2. What are the reagents used in order to separate them?
3. Is the solubility rules applicable in this experiment?
4. Determine whether the analysis used is quantitative or qualitative.
5. How will you separate the precipitate from the solution?

B. Theory:
In qualitative analysis, the ions in a mixture are separated by selective precipitation.
Selective precipitation involves the addition of a carefully selected reagent to an aqueous mixture
of ions, resulting in the precipitation of one or more of the ions, while leaving the rest in solution.
Once each ion is isolated, its identity can be confirmed by using a chemical reaction specific to
that ion. The reaction that confirms the presence of a particular ion involves the creation of visible
products such as precipitate or colored species. A reaction that results in a precipitation can also
be used to separate ions from the solution.

C. Hypothesis:
If analysis always does not mean breaking of substance into its ultimate constituents, and
it is finding out the nature of substance and identity of its constituents then a qualitative analysis
should be used in determining different groups of cations in a mixture.
If qualitative analysis is an analytical procedure that answers the question “what is
present?” then this scheme can be used to separate substances in order to identify which
substances are present.

D. Procedure: You can have a schematic diagram

 ADD
6M
HCl
PREC
IPITA
TE

SEPAR ADD 0.1

ATE M H2S
SOLUTI solution
ON
CENTRI in 6M
FROM &
FUGE HCl PREC
PRECIP
DECANT IPITA
ITATE TE
ADD 0.1 SEPAR
M H2S ATE
solution SOLUTI
in 6M CENTRI
ON
PREC NH4OH FUGE
FROM &
IPITA DECANT
PRECIP
TE ITATE
ADD
SEPAR Ammoniu
ATE m
SOLUTI Carbonat
ON
CENTRI e PREC
FROM
FUGE & IPITA
PRECIP
DECANT TE
ITATE

E. Results and Discussion: Tabulate results and discussion

The overall scheme for the systematic analysis of mixtures of cations based on the IV major
groups is shown in the schematic diagram above. In summary, the ions with which we will be
concerned are the following:

GROUP CATIONS REAGENTS

1 Ag+, Hg2+2, Pb+2 6M HCl

2 Cu+2, Sn+2, Bi+3 0.1 M H2S solution in 6M

HCl

3 Al+3, Cr+3, Co+2, Mn+4 0.1 M H2S solution in 6M

NH4OH

4 Mg+2, Ba+2, Ca+2 Ammonium Carbonate

Group I (Ag+, Hg2+2, Pb+2) cations produce insoluble chlorides so they are precipitated with dilute
HCl, while other cations remain in solution. Group II ( Cu +2, Sn+2, Bi+3) cations produce very
insoluble sulfides (Ksp values less than 10-30) so they are precipitated by low amounts of sulfide
ion; acidic solution of H2S was added. Group III ( Al +3, Cr+3, Co+2, Mn+4) cations produce slightly
soluble sulfides (Ksp values more than 10-20) so they are precipitated by relatively high amounts
of sulfide ion; a basic solution of H2S was added. Group IV ( Mg +2, Ba+2, Ca+) cations, as well as
all of the above groups, produce insoluble carbonates so they are precipitated by the addition of
carbonate once the ions of the first three groups have been removed.

Group I Analysis: Ag+, Hg2+2, Pb+2

Net ionic equation Precipitate

Ag+ + Cl- ------> AgCl (s) White

Hg2+2 + 2Cl- -------> Hg2Cl2 (s) White

Pb2+ + 2Cl- -------> PbCl2 (s) White

When 6 M HCl is added to the solution, white precipitates of AgCl, Hg 2Cl2 and PbCl2 are formed.

Group II Analysis: Cu+2, Sn+2, Bi+3

Net ionic equation Precipitate

Cu+2 + H2S ------> CuS (s) + 2H+ Black

Sn+2 + H2S -------> SnS (s) + 6H+ Yellow

2Bi+3 + 3H2S -------> Bi2S3 (s) + 2H+ Black

 After the insoluble chlorides are isolated, the pH of the solution is adjusted to 0.1, and then
H2S(aq) is added. Since the concentration of Sulfide ion (S 2-) is very low at low pH, only those
metallic sulfides having very low Ksp values such as CuS, SnS and Bi 2S3 formed a precipitate.

Group III Analysis: Al+3, Cr+3, Co+2, Mn+4

Net ionic equation Precipitate

Al+3 + 3NH3+ 3H2O -----> Al(OH)3 (s) + 3NH4+ White, gelatinous

Cr+3 + 3NH3+ 3H2O -----> Cr(OH)3 (s) + 3NH4+ blue-green, gelatinous

Co+2 + H2S ------> CoS (s) + 2H+ Black

Mn+4 + H2S ------> MnS (s) + 2H+ Black

In an Alkaline solution, the concentration of S2- increases, and the metallic sulfides with larger Ksp
values such as CoS and and MnS, precipitate. Moreover, since the solution is basic, Al +3, Cr+3
Form insoluble hydroxides and are also separated from the solution.

Group IV Analysis: Mg+2, Ba+2, Ca+2

Net ionic equation Precipitate

Mg+2 + CO32-------> MgCO3 Do not ppt.

Ba+2 + CO32-------> BaCO3 White

Ca+2 + CO32-------> CaCO3 White

These three metallic cations all belong to Group IIA in the periodic table, and therefore their
chemical properties are very similar. They form soluble chlorides and sulfides, and hence are
separable from group I, II and III cations. However their carbonates precipitate in a mixture of
(NH4)2CO3.

Conclusion:

In this lab, qualitative analysis was used to determine the cations in a solution. Each step
that determined what cations were present , requires a test to separate a single substance from
the rest, and then a confirmatory test to further prove the presence of the isolated cation. In short,
each cation is determined by the observations seen when different reagents react with the
solution or only parts of the solution. We developed a separation scheme in order to fully identify
each of the cations present.

III. Laboratory Safety Supplementary Activity

Before you leave the laboratory room, you do housekeep. Dispose the waste chemicals and the unused
or excess chemicals to their proper receptacles. Solid wastes to the color-coded bins. Make a table to
address proper segregation of wastes.

Chemicals Receptacle

Hydrochloric acid HCl 1

Hydrogen sulfide H2S 1

Ammonium hydroxide NH4 OH 3

Ammonium carbonate - (NH4)2CO3 3

Yellow Bin Green Bin Black Bin

Face Mask /

Gloves /

Litmus paper /

IV. Real-Life Connection

How do you relate this activity into your daily life especially in waste segregation and safety to
human life, properties and environment?

In this laboratory activity, we learned about the different categories of cations according to their
precipitants. Cations are important because they have more protons than electrons which gives it a net
positive charge. In this activity, we were asked to separate the cations from different mixtures and to
determine the reagents used to separate the precipitants. However the chemicals and reagents used can
be very dangerous and can jeopardize the safety of the students. The reagents used are HCl (which is
corrosive to the eyes, skin, and mucous membrane), ammonium carbonate ( harmful when swallowed
and can irritate the eyes and skin), Ammonium hydroxide (causes skin irritation and can cause vomiting
and in severe cases, perforation). This not only teaches us on proper handling of these reagents which
can ensure safety within the laboratory, but it also teaches us the dangers of said reagents which can be
used in future experiments.

Cations are considered to be very important because they can be useful and can relate to our
daily lives. For example, cations are known to be highly essential when it comes to blood pressure
regulations and muscle contractions which can boost a healthy lifestyle among individuals. However,
some cations can be dangerous to the environment, that is why it is very important to be aware of the
different receptacles where each chemical should be disposed of. Improper handling with these chemicals
can lead to dangerous events and by avoiding these, we can guarantee safety not only to us and our
fellow colleagues, to the environment, but also safety inside the laboratory.