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Qualitative analytical chemistry I experiments

Qualitative Analysis
of
The Group Iv Cations

Wimbo triono
3315081900

University of Jakarta
I. Purpose

1. Separating the group IV cations from sample

2. Indentifying the group IV cations use specific reagent

3. Knowing chemical properties of group IV cations

II. Basic of theory

The cations in group IV have rather less distinctive chemical


properties than do the other cations we have studied, so their
detection depends, in some cases, more on physical than on
chemical behavior. Barium and calcium are separated by
precipitation of their carbonates under slightly basic condition.
Barium most of the common barium salts are soluble in water or
dilute strong acids and are colorless in solution. The main exception
is the sulfate, BaSO4, a finely divided white powder which is
essentially insoluble in all common reagents. Barium chromate,
BaCrO4, is insoluble in acetic acid but will dissolbe in solution of
strong acids. The oxalate and phosphate are soluble in acidic
system at a pH of 3 or less. Barium hydroxide is a strong base and is
moderately soluble in water. Barium exist in its compounds
essentialy only in the +2 state and is not reducible to the metal in
aqueous systems.

Calcium salts are typically soluble in water or dilute acids. Like


barium, calcium does not form many common comples ion.
Although the hydroxide is less soluble than Ba(OH)2, it will not
precipitate in amonia. Calcium oxalate, CaC2O4, is white and not
appreciably soluble in acetic acid, but it will dissolve in dilute strong
acid solutions. Calcium in its compounds occurs in the +2 state, and
the ion is very difficult to reduce to the metal.

III. Instruments and materials

• Instruments * Material

1. Pipete 1. NH4Cl

2. Beaker glass 2. NH4OH


3. Semimicro test tube 3. (NH4)2CO3

4. Centrifuge tube 4. CH3COOH

5. K2CrO4

6. C2H5OH

IV. Procedure

Sample
+ NH4Cl
+ NH4OH
Precipitate +(NH4)2CO3
+CH3CO
OH Identificatio
Precipitate n

Filtrate
+NH4O
H
+C2H5
Filtrat
OH Identificatio
n
Precipitate
The next group Identificatio
cations n
Filtrate

V. Data of experiments

Sample Result
NH4Cl + NH4OH+ (NH4)2CO3 A white precipitate*
• Precipitate*
+ CH3COOH Soluble
+ K2CrO4 An orange precipitate**, an
orange liquid*
• Precipitate** (Identification
Ba) Soluble
+ HCl A white precipitate
+ H2SO4
• Filtrate*
+ NH4OH A white precipitate***
+ C2H5OH
• Precipitate (Identification Soluble
Ca) A white precipitate
+ HCl
+ (NH4)2C2O4 A white precipitate
• Filtrate (Identification Sr)
+ NH4OH

VI. Analysis of data

Process separation the group IV cations must be in pH 9 condition


to prevent sedimentation of the magnesium (if the magnesium
presence in sample). In order to make condition in pH 9, the buffer
pH 9 solution added to the sample before separation. The group IV
cations are separated from the sample by precipitation of their
carbonates under slightly basic condition use (NH4)2CO3 as reagent
of these group. A white precipitate in experiments indicates the
presence of the group IV cations in sample. Precipitate Centrifuge
and decant liquid which may contain other cations into beaker glass.

Ba2+ + Sr2+ + Ca2+ + 3(NH4)2CO3 -> BaCO3S + SrCO3S + CaCO3S +


NH+

The acetic acid and potassium chromate added into the


precipitate of the group IV cations in order to confirmation the
presence of barium. Strontium and calcium will dissolve but barium
will precipitate as its chromate. An orange precipitate from
experiments indicates the presence of barium. Precipitate centrifuge
and decant liquid which may contain strontium and calcium into test
tube. To confirm again the presence of barium, an orange
precipitate dissolved by HCl and H2SO4 added into solution. Based
on experiment, a white precipitate established the presence of
barium in sample.

Ba2+ + SO42- -> BaSO4S


Liquid from separation of barium added ammonium and etanol in
order to separate strontium with calcium. The important thing
before separate strontium and calcium is addition acetic acid when
confirmation the presence of barium cannot be excess. Strontium
will not precipitate in acid condition. NH4OH will make precipitate of
strontium as its hydroxide. Etanol used as catalyst in this reaction.
Centrifuge and decant the liquid which may contains calcium into
test tube.

Sr2+ + 2NH4OH -> Sr(OH)2S + 2NH4+

A white precipitate indicate the presence of strontium and to


make sure the presence of strontium, precipitate dissolved in HCl
and added (NH4)2C2O4. A white precipitate established the
presence of strontium in sample.

Sr2+ + (NH4)2(COO)2 -> Sr(COO)2S + 2NH4+

Filtrate from separation of strontium and calcium used to


identification calcium in sample. (NH4)2(COO)2 add into filtrate to
confirm the presence of calcium. A white precipitate from
experiment established the presence of calcium.

Ca2+ + (NH4)2(COO)2 -> Ca(COO)2S + 2NH4+

Based on analysis, sample contains the group IV cations.

VII. Task

Write all of chemical equations from each step

1. Ba2+ + Sr2+ + Ca2+ + 3(NH4)2CO3 -> BaCO3S + SrCO3S + CaCO3S +


NH+

2. 2 CrO42- + CH3COOH -> Cr2O72- + 2CH3COO- + H2O

3. Ba2+ + SO42- -> BaSO4S

4. Ca2+ + (NH4)2(COO)2 -> Ca(COO)2S + 2NH4+

5. Sr2+ + (NH4)2(COO)2 -> Sr(COO)2S + 2NH4+

6. Sr2+ + 2NH4OH -> Sr(OH)2S + 2NH4+


VIII. Conclusion

1. Process separation the group IV cations must be in pH 9


condition to prevent sedimentation of the magnesium

2. Identify barium use sulfate acid and chromate establish the


presence of barium in sample

3. IdentifyStrontium use ammonium oxalate establish the


presence of barium in sample

4. Identify barium use ammonium oxalate establish the presence


of barium in sample

5. Separating strontium and amonium use etanol as catalyst

6. Sample contains the group IV cations

IX. Bibliography

Darsati, Siti, dkk. 1999. Dasar-Dasar Kimia Analitik. Bandung:


FMIPA UNJ

Haryadi, W. 1990. Ilmu Kimia Analitik Dasar. Jakarta: Gramedia

Khopkar, SM. 1990. Konsep Dasar Kimia Analitik. Jakarta: UI Press

Oktaviani, Isnania, P. 2008. Laporan Praktikum KA I. Jakarta: UNJ

Vogel. 1979. Analisis Anorganik Kualitatif Makro dan Semimikro.


Jakarta.: PT Kalman Media Pustaka