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I.
Introduction
Precipitation reactions happen throughout our lives even without noticing it
and they are considerably important in different fields. The preparation of
sodium bicarbonate is made through precipitation reactions. The deterioration
of the tooth enamel which can lead to tooth decay, the production of barium
sulphate to diagnose digestive tract disorders are also governed by
precipitation reactions (Chang, 2010).
According to Chang (2010), the solubility product constant or Ksp is the
product of the molar concentrations of the constituent ions, each raised to the
power of its stoichiometric coefficient in the equilibrium equation. K sp follows
the general equation
Ksp = [An+]x [Bm-]y
The solubility quotient or ion product Q determines if precipitate would form
and is of the equation
Q = [An+]xo [Bm-]yo
According to Atkins & Beran (1992), just as the reaction quotient was used to
determine the shift of the equilibrium, the comparison of the Q and Ksp
determines if a precipitate will form.
If Q>Ksp, there are excess ions which makes the solution
supersaturated and precipitation will occur.
If Q=Ksp, the solution would be saturated and in equilibrium thus no
precipitation will occur.
If Q<Ksp, the solution has very few ions making it unsaturated and no
precipitation will occur.
An application of the solubility product constant would be the
qualitative analysis which involves simply identifying the presence or
absence of cations and anions in a given solution (Brown & Lemay,
1985).
After the separation of the first four groups of cations, the Group D
cations, will be precipitated and be separately identified. This group of
cations include Cu2+, Mg2+, Ni2+, Zn2+, and Cd2+.
II.
Materials
A. Reagents
CC1 (Cations of Groups D-E from Group C Analysis)
Concentrated HNO3
6M HCl
6M NH3
0.1M K4Fe (CN) 6
1% dimethylglyoxime (DMG)
6M CH3COOH
Solid Na2S2O3
0.1M Na2HPO4
6M NaOH
0.2M Na2S
Distilled water
B. Apparatus and Equipment
Centrifuge Tubes
Test Tubes
Centrifuge
Hot plate
Water bath
Ice
Stirring Rod
Watch Glass
Red and Blue Litmus Paper
Pasteur pipets
III.
Procedure
Ten drops of CC1 from the analysis of the Group C cations have been
obtained and was heated to dryness over low heat. It was cooled then
6 drops of concentrated HNO3 was added then it was heated to dryness
again. After cooling, 5 drops of 6M HCl was added to dissolve the
residue formed. The solution was transferred quantitatively to a
centrifuge tube using distilled water and was labelled as CD1.
One drop of CD1 was used to test the presence of the Cu 2+ ion. The pH of
the solution was determined using litmus paper. 6M NH 3 was added until the
solution became neutral. Two drops of 6M acetic acid was added to make the
solution slightly acidic. Three to four drops of 0.1M K 4Fe (CN) 6was added to
confirm the presence of the Cu2+ ion. The presence of the Cu2+ ion was confirmed
upon formation of cupric hexacyanoferrate (II) which is a maroon precipitate.
One drop of CD1 was used to test the presence of theNi 2+ ion. The pH of
the solution was determined using litmus paper. 6M NH 3 was added until the
solution became basic. 10-15 drops of the confirmatory reagent 1%
dimethylglyoxime was added. Upon addition of DMG, the formation of a cherry
red-nickel dimethylglyoxime was observed which confirms the identity of Ni 2+ ion.
The remainder portion of CD1 was used to test the remaining Group D ions
including Mg2+, Zn2+, and Cd2+. 6M NH3 was added to make the solution neutral
then 2 drops of 6M CH3COOH was added to make it slightly acidic. A crystal
(about 0.2-0.3 g) of solid Na2S2O3 was added afterwards. The solution was heated
it a boiling water bath for 10 minutes and was cooled afterwards in an ice-water
bath. It was then centrifuged and decanted. The precipitate was labelled as PD1
and the centrifugate was labelled as CD2.
CD2 was used to determine the presence of the Mg 2+ ion. 6M NH3 was
added to make it basic and six to eight drops of 0.1M Na 2HPO4 was added. It was
left to stand for several minutes and centrifugation followed shortly. The
presence of a white precipitate of magnesium ammonium phosphate confirms
the presence of the Mg2+ ion upon addition of sodium hydrogen phosphate.
50 drops of 6M NaOH was added to PD1 using a Pasteur pipet. It was
stirred, centrifuged, and decanted afterwards. The centrifugate was labelled as
CD3 and the precipitate was labelled as PD2.
CD3 was used to determine the presence of the Zn 2+ ion in the solution.
6M acetic acid was added to the solution until it became slightly acidic. Four
drops of the confirmatory agent 0.1 M K 4Fe(CN)6 was added under the fumehood.
The presence of a white precipitate of Zn 2Fe(CN)6 upon addition of potassium
hexacyanoferrate (II) confirms the presence of the Zn 2+ ion.
PD2 was washed twice with 10 drops of distilled water. Six drops of 6M HCl
was added to the solution and was stirred and centrifuged. Upon decantation,
the centrifugate was labelled as CD4 and the precipitate was labelled as PD4 but
was discarded.
CD4 was used to test the presence of the Cd 2+ ion. Two centrifuge tubes
each containing three drops of CD4 was used. In the first centrifuge tube, 6M NH 3
was added until the solution became neutral. Two drops of 6M acetic acid was
added to make the solution slightly acidic. Five drops of the confirmatory reagent
potassium hexacyanoferrate (II) was added and led to the formation of a white
precipitate of Cd2Fe(CN)6 which confirms the presence of the Cd 2+ ion. In the
second centrifuge tube, 6M NH3 was added to make the solution neutral. Five
drops of the confirmatory reagent 0.2M Na 2S was added to further confirm the
presence of the Cd2+ ion. The presence of the Cd2+ ion can be confirmed upon
formation of a yellow precipitate of CdS.
IV.
V.
Data/Observations
Discussion
Precipitation reactions happen throughout our lives even without noticing it
and they are considerably important in different fields. The preparation of
sodium bicarbonate is made through precipitation reactions. The deterioration
of the tooth enamel which can lead to tooth decay, the production of barium
sulphate to diagnose digestive tract disorders are also governed by
precipitation reactions (Chang, 2010).
According to Chang (2010), the solubility product constant or Ksp is the
product of the molar concentrations of the constituent ions, each raised to the
power of its stoichiometric coefficient in the equilibrium equation. K sp follows
the general equation
Ksp = [An+]x [Bm-]y
(l)
(aq)
The presence of the Mg2+ ions can be confirmed upon addition of Na2HPO4 to
produce MgNH4PO4 which is a white precipitate. The blue supernatant can be
explained due to the presence of unreacted Cd 2+, Zn2+, and Cu2+ which forms
complex ion formation with NH3. The reactions upon determination of Mg2+ are as
follows:
H3O+ (aq) + NH3(aq) (double headed arrow) NH4+ (aq) + H2O
(l)
Mg2+ (aq) + NH4+(aq) +HPO42- (aq) + OH-(aq) (double headed arrow) MgNH4PO4 (s) + H2O
(l)
(s)
(aq)
(g)
+ 2H2O
(l)
There are two ways to confirm the presence of Cd 2+ ions. Addition of sodium
sulfide forms a yellow precipitate CdS or a white precipitate will form upon
addition of potassium hexacyanoferrate (II):
Cd2+ (aq) + S2-(aq) (double headed arrow) CdS
(s)
equilibrium involves OH- ions, the addition of hydroxide ions to the solution will
decrease the solubility if the hydroxide-forming ion. Upon addition of an acid, the
generation of H3o+ ions decreases the number of OH- ions which means a shift of
the equilibrium to the right increasing the solubility of the hydroxide-forming ion
(Atkins & Beran, 1992).
VI.
VII.
Conclusion
The Group D cations readily precipitate out as hydroxides and oxides
soluble in ammonia but insoluble in sodium hydroxide upon addition of
HNO3 and HCl. The addition of basic solutions decreases the solubility
of the hydroxide forms of the Group D cations while the addition of
acidic solutions increases the solubility of the hydroxide forms of the
Group D cations.
Literature Cited/Bibliography