INORGANIC CHEMISTRY 1 FORMAL REPORT

Adamson University
900 San Marcelino, Ermita,
1000 Manila Philippines

Analysis of Group I Cations (Silver, Lead and Mercury)

*Cayabyab, Ma. Salma Kirsten A.
Dacanay, Marco Alberto
a
Department of Chemistry, College of Science, Adamson University, 900 San Marcelino, Ermita, Manila 1000, Philippines

FORMAL REPORT INFO ABSTRACT

Report history: April 9, 2019
Date Performed: March 26, 2019
Date Submitted: April 10, 2019
Keywords: qualitative analysis, analysis, cations,
group 1 cations, silver, lead, mercury
Group I Cations; silver, mercury and lead presence are confirmed with the
systematic analysis from the successful precipitation of the ions with their
respective insoluble chloride compounds. The precipitation of these ions is
based from the solubility in different mediums or reagents. The researchers
have conducted an analysis from a known solution which all tested positive of
the cations from Group I and the analysis of an unknown sample provided by
the instructor which contained and confirmed only the presence of the mercury
ion.

1.0 INTRODUCTION chloride compound of lead is slightly soluble in water at

The qualitative analysis of certain group of ions
can be performed to determine the presence of these ions
in a given sample and also their purity (Bradley, 1920).
The ions for this experiment performed belonged to the
Group I Cations.
The systematic analysis of common ions;
cations or anions are based from the successful
precipitation from the determination of the solubility of
each compound formed. This experiment involved the
precipitation of silver, lead and mercury ions. These ions
are then precipitated as insoluble chlorides.
These ions have specific solubilities in their
chloride compounds such as silver chloride having
1.56×10-10, mercury (II) chloride having 2×10-18 and
-4
lead (II) chloride having 1×10 . These values could
determine that the precipitation of silver and mercury
ions are almost to complete precipitation but with the
highly soluble lead (II) chloride, leads little to no
precipitate formed (Gilreath, 1954). Lead is highly
soluble in water such as lead nitrate or lead acetate. The
room temperature and highly soluble when heated to
100oC, which makes the separation of lead ions easier
than of the silver and mercury ions (Bradley, 1920).
Silver ions can be readily dissolved upon
reaction to ammonia forming the ammonia complex but
can also be reprecipitated. The mercurous ion
immediately confirms it presence with the auto-redox
reaction with ammonia upon the formation of the
insoluble mercury and mercuric aminochloride
(Gilreath, 1954).
The researcher prepared a known solution to
serve as a control or comparison for the succeeding tests
performed. The known solution was prepared using the
nitrates of silver, lead and mercury. After the analysis of
the known solution, the researchers were provided with
an unknown solution that may contain either one of the
three Group I cations.
2.0 METHODOLOGY
The experiment required thirteen reagents for
the analysis of the Group I Cations namely; 0.1 M
sodium chloride, 0.1 M lead chloride, 0.1 M mercury (II)
chloride, 0.05 M mercury (II) nitrate, 0.1 M potassium
bromide, 1 M potassium chromate, 0.1 M potassium
iodide, 0.1 M silver nitrate, 1 M sodium thiosulfate, 6 M
hydrochloric acid, 6 M ammonia, 6 M sodium hydroxide
and 6 M nitric acid. The mentioned reagents were
handled well and in accordance to the laboratory safety
rules, and the researchers using their personal protective
equipment. The researchers were given an unknown
sample which may contain ions of silver, lead or mercury
and this was analyzed below.
The researchers were instructed to analyze a
known sample by creating a solution with 2 mL of each;
0.1 M AgNO3, 0.1 M Hg(NO3)2 and 0.1 M Pb(NO3)2.
This known solution was made as a control for the
analysis of the unknown sample provided by the
instructor.
The researchers used only 3 mL of the known
sample and incorporated it in a centrifuge tube. The
sample was then introduced with 6M HCl to precipitate
the ions. The sample was then centrifuged and to
complete the precipitation, the researchers added an
excess amount of 6M HCl and then centrifuged again to
separate the precipitate. The supernatant was discarded,
and the precipitate was washed with 3 mL of deionized
water, this was again centrifuged, and the supernatant
was kept in another tube for the confirmation of the lead
ion presence.
The precipitate left in the tube was then
introduced with 3 mL of deionized water and was heated
in a boiling water bath that produced a white precipitate.
The precipitate was left to resettle, and the researchers
separated the supernatant and precipitate via decantation.
The supernatant was combined with the washings.
The combined washings and supernatant were
then used for the confirmation of lead ions via
precipitation. Potassium chromate was used to
precipitate the ions and the solution produced a cloudy
yellow coloration. The precipitate after settling was then
dissolved using 6M NaOH in a fume hood.
To the precipitate from earlier, was washed
with deionized water and the washings were discarded.
Ammonia was then introduced to the precipitate and it
resulted the immediate blackening of the precipitate,
deionized water also was incorporated, and this solution
was centrifuged. The supernatant was then placed in a
separate tube and 6M nitric acid was added to the
supernatant which resulted to the formation of white
precipitate.
After performing the control analysis, the
unknown sample provided was then analyzed for its
identity. The unknown sample was analyzed like the
known sample.
The researchers used 3 mL of of the unknown
solution introducing it in a centrifuge tube, the ions in the
sample was then precipitated with 6M HCl and then a
cloudy white solution formed. This solution was then
centrifuged, the supernatant was discarded, and the
precipitate was washed with deionized water. This
washing was kept. The washed precipitate was heated in
a water bath with 3 mL deionized water introduced. This
created a cloudy solution and was then centrifuged. The
supernatant was combined with the washing after
centrifuging for the analysis of lead ion presence in the
sample.
The precipitate was then treated with 6M of
ammonia and 2 mL of deionized water. This resulted in
the immediate blackening of the precipitate. This
solution was centrifuged, and the supernatant was
separated, this supernatant was then treated with 6M
nitric acid, but no reaction was observed.
 To the washings and the kept supernatant, the precipitate formed is believed to be lead chromate. Lead
researchers analyzed it to confirm the lead ion presence (II) chromate is less soluble that lead (II) chloride with
with the addition of potassium chromate. This addition approximately 2 × 10-5 g/100 mL from lead (II)
only resulted in the yellow coloration of the solution chloride’s solubility; 1 g/100mL at room temperature.
without any visible precipitation and reaction. (Gilreath, 1954) The reaction involved for the formation
The results of the analysis done by the of lead (II) chromate is:
researchers are discussed in the next part, wherein it
would explain the reactions that took place in the Pb++ + CrO4 − ↔ PbCrO4
experiment.
Equation 3.1 Formation of Lead (II) Chromate
3.0 RESULTS AND DISCUSSION
This precipitate formed was then dissolved with
The researchers successfully performed the 6M NaOH as lead (II) chromate is easily dissolved with
experiment and the analysis of the cations performed the reagent, with the product shown in Figure 3.1. The
lead the identification of the ions in the unknown sample. reaction takes place as lead (II) chromate decomposes
For the control, the known solution was made from the into a mixture of sodium chromate and plumbite
mixture of the nitrate solutions of silver, lead and (Atomistry, 2012).
mercury. This sample was then analyzed, firstly by
precipitating it with 6M of hydrochloric acid. The
hydrochloric acid is used to precipitate the ions as it
converts the nitrates into insoluble chlorides. (Gilreath,
1954) the precipitation indicates the presence of the
chlorides in the sample. This was then centrifuged and
was introduced with an excess amount of hydrochloric
acid to the solution to complete the precipitation of the
ions.
Although there is precipitation involved in the
experiment, note that lead (II) chloride has a large
solubility than of the silver chloride and mercury (II)
Figure 3.1 Confirmation of lead ion presence in the
chloride (Gilreath, 1954). Lead is separated from the
known sample
solution by washing of the precipitate with deionized
water. As lead has a higher solubility in water than silver
The precipitate from the separation of the ions
and mercury, the washing of the precipitate was used to
was used for the confirmation of silver and mercury (II)
test for the confirmation of the lead ion.
ions in the sample. The precipitate was then again
The washing was treated with potassium
washed to prevent lead ion interference during the
chromate and a formation of a cloudy yellow solution
analysis. The residue left was then treated with ammonia
that predicted the presence of lead (II) chromate. The
to dissolve the silver chloride to form a silver ammonia
complex ion: (University of Massachusetts Amherst,
2011)
AgCl(s) + 2NH3 ↔ [Ag(NH3 )2+ ](aq) + Cl− (aq)
Equation 3.2. Reaction of silver chloride with
ammonia
From the introduction of ammonia in the
sample, the blackening of the residue was observed,
shown in Figure 3.2, indicating the presence of the
mercury ions in the sample. This reaction took place as
the ammonia reacted with the mercury (II) chloride. A
redox reaction happened forming mercury and mercuric
aminochloride. A mercurous ion was oxidized to the
mercuric state and the other was reduced to mercury
(Gilreath, 1954) with the equation shown below:
Hg 2 Cl2 + 2NH3 ↔ HgNH2 Cl + NH4 + + Cl−
Equation 3.3 Reaction of mercury (II) chloride with
ammonia
Figure 3.2 Confirmation of mercury (II) ions in the
known solution
With the mercury ion presence was confirmed,
the dissolved silver chloride was then again precipitated
with 6M nitric acid under the fume hood. A visible
precipitation or white precipitate was formed upon
addition as shown in Figure 3.3. This precipitation was
due to the silver ammonia complex ion was destroyed
and then the formation or precipitation of silver chloride
occurred with the equation below;
Ag(NH3 )2 + + Cl− + 2H2 O+
↔ AgCl + 2NH4 + + 2H2 O
Equation 3.4 Reaction of Silver Ammonia Complex
Ion with Nitric Acid, Reprecipitation of silver
chloride.
Figure 3.3 Confirmatory test for silver ion presence
from the prepare known solution
For the unknown sample, the researchers took
3mL of the unknown sample provided by the instructor.
The analysis pushed through like the analysis of the
known sample. The precipitation took place. The
precipitate was then washed twice, and the washings
were used to confirm the presence of lead ions. Upon
addition of potassium chromate, there was no reaction Figure 3.5 Confirmation of mercury (II) ion presence in
observed, thus indicating that lead chromate was not the unknown sample
present in the unknown sample as shown in Figure 3.4 This solution was then centrifuged and was
supernatant was separated, this supernatant was treated
with nitric acid under the fume hood, but no reaction
occurred or was observed by the researcher indicated that
silver ions were not present in the unknown sample. The
reaction in the tube was as shown in Figure 3.6.

Figure 3.4 Confirmation of Lead ions presence in

the unknown sample

The precipitate was then treated with ammonia

and the immediate blackening of the precipitate was
observed as shown in Figure 3.5. This indicated the
presence of mercury ions in the provided unknown
Figure 3.6 Confirmatory test for silver ion presence
sample.
from the provided unknown solution.

4.0 CONCLUSION

The experiment was performed successfully by

the researchers and determined that the ions in the known
solution contained the three ions from the Group I. The
analysis for this known sample was made to be the
control or to be compared with the analysis of the
unknown provided sample from the instructor.
From the tedious analysis of the unknown
sample, the researchers confirmed that the ions present
in the sample was only mercury (II) ions from the
blackening of the residue observed upon the addition of
ammonia to the residue.
 The researcher suggests that these confirmatory
tests made should be done in a systematic manner
without omitting any steps in the given instructions from
the manual to prevent misidentification of the present
ions in the sample. This paper could also serve as a guide
for those who are to perform the qualitative analysis for
the Group I Cations due to the preparation and analysis
for a known sample.

5.0 REFERENCES

Atomistry. (2012). Normal Lead Chromate, PbCrO4.

Retrieved from Atomistry:
http://lead.atomistry.com/normal_lead_chroma
te.html
Bradley, T. (1920). Qualitative Chemical Analysis For
Students of Pharmacy. Philadelphia: Lea &
Febiger.
Gilreath, E. S. (1954). Qualitative Analysis Using
Semimicro Methods. New York: McGraw-Hill
Book Company, Inc.
University of Massachusetts Amherst. (2011). Silver Salt
Equilibrium and LeChatlier’s Principle
(check). Retrieved from University of
Massachusetts Amherts: Chemistry:
https://lecturedemos.chem.umass.edu/equilibri
a15_5.html