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Food Science and Technology

Faculty of Agriculture
Hasanuddin University

Analisa Kualitatif Kation


Andi Rahmayanti R
Outline
01 Pendahuluan

02 Analisa Kualitatif

03 Cation Analysis
Pendahuluan
Introduction
• Many problems in analytical chemistry
begin with the need to identify what is
present in a sample.
• This is the scope of a qualitative analysis,
examples of which include identifying the
products of a chemical reaction, screening
an athlete’s urine for the presence of a
performance-enhancing drug, or
determining the spatial distribution of Pb
on the surface of an airborne particulate.
• Much of the early work in analytical
chemistry involved the development of
simple chemical tests to identify the
presence of inorganic ions and organic
functional groups
• Analytical chemistry is the chemistry discipline concerned with
Qualitative the chemical composition of materials. Analytical chemistry
also is concerned with developing the tools used to examine
Analysis chemical compositions.
• Qualitative analysis deals with the detection of the nature of
the chemical species in a sample.
• Elemental qualitative analysis is used to separate and detect
cations and anions in a sample substance.

• Classical qualitative inorganic analysis is a method of analytical chemistry which seeks to


find elemental composition of inorganic compounds. It is mainly focused on detecting ions in
an aqueous solution, so that materials in other forms may need to be brought into this state
before using standard methods. The solution is then treated with various reagents to test for
reactions characteristic of certain ions, which may cause color change, solid forming and
other visible changes.
• Qualitative inorganic analysis is that branch or method of analytical chemistry which seeks to
establish elemental composition of inorganic compounds through various reagents.
CATION ANALYSIS

The procedure used to separate


and identify more than 20 common
metal cations from a single solution
consists of selectively precipitating
only a few kinds of metal ions at a
time under given sets of conditions.
Consecutive precipitation steps
become progressively less selective
until almost all of the metal ions are
precipitated,
Group Reaction
Base – Insoluble
Sulfides

Insoluble Insoluble
Chloriodes Carbonates or
Phospates

Acid – Insoluble Alkali Metals


Sulfides
Cation Analysis
Cation Analysis
Most metal chloride salts are soluble in water; only Ag+, Pb2+, and Hg22+ form chlorides that

1
precipitate from water. Thus the first step in a qualitative analysis is to add about 6 M HCl,
thereby causing AgCl, PbCl2, and/or Hg2Cl2 to precipitate. If no precipitate forms, then these
cations are not present in significant amounts. The precipitate can be collected by filtration or
Grup 1
centrifugation
Next, the acidic solution is saturated with H2S gas. Only those metal ions that form very insoluble
2 sulfides, such as As3+, Bi3+, Cd2+, Cu2+, Hg2+, Sb3+, and Sn2+, precipitate as their sulfide salts
under these acidic conditions. All others, such as Fe2+ and Zn2+, remain in solution. Once again,
the precipitates are collected by filtration or centrifugation
Grup 2
Ammonia or NaOH is now added to the solution until it is basic, and then (NH4)2S is added. This
3 treatment removes any remaining cations that form insoluble hydroxides or sulfides. The divalent
metal ions Co2+, Fe2+, Mn2+, Ni2+, and Zn2+ precipitate as their sulfides, and the trivalent metal Grup 3
ions Al3+ and Cr3+ precipitate as their hydroxides:
The next metal ions to be removed from solution are those that form insoluble carbonates and
4 phosphates. When Na2CO3 is added to the basic solution that remains after the precipitated
metal ions are removed, insoluble carbonates precipitate and are collected
Grup 4
A yellow flame that persists for at least 5 seconds confirms the presence of Na+1 . A pale violet
5 flame that persists at least 2 seconds confirms the presence of K+1 . Grup 5
Insoluble Chloriodes
• In the first group of cations, we include Silver(I), Mercury(I)and Lead(II) cations.
Before we begin, it is good to note that mercury(I) ions - or mercurous ions - are
NOT Hg+ but Hg22+.
• The group reagent is dilute Hydrochloric acid.
• When we pass dil. Hcl through the solution, we expect the precipitation of the
chlorides of the aforementioned cations. ANY Precipitation is nothing but a
chloride and the cation of the ppt. can not be any other than the three.
• If a presipitation is obtained, group I cations are confirmed. If not, we wll test the
solution for the presence of group II cations.
• Suppose we obtain a ppt on adding dil. HCl to the solution. It is inferred that the
cation in the solution is either Ag+, Hg22+ or Pb2+.
• Our goal now would be to distinguish between these three cations.
• Before we pass onto this section, please realize that dil. HCl was added to only a
part of the solution, taken in another testtube. The rest of the solution would be
preserved for use in other tsts should it be needed.
Acid-insoluble Sulfides
Next, the acidic solution is saturated with H2S gas. Only those metal ions that form very insoluble sulfides,
such as As3+, Bi3+, Cd2+, Cu2+, Hg2+, Sb3+, and Sn2+, precipitate as their sulfide salts under these acidic
conditions. All others, such as Fe2+ and Zn2+, remain in solution. Once again, the precipitates are collected by
filtration or centrifugation.

In the fume hood, add 10 drops of 1M Thioacetamide (CH3CS(NH2)) to each of the solutions from the
Precipitation of Group 1 Cations that did not form a precipitate in Step 1 of that procedure. In the fume hood,
heat each solution in a Hot Water bath for 10 minutes. This should allow the Thioacetamide to decompose into
Hydrogen Sulfide (H2S) and allow the Sulfide precipitates to form in an Acidic environment.

Base
. – Insoluble Sulfides
 Golongan III : membentuk endapan dengan NH4S
Co2+, Ni2+, Fe2+, Fe3+, Cr3+, Al3+, Zn2+, Mn2+

Insoluble Carbonates or Phospates


 Golongan IV : membentuk endapan dengan (NH4)2 CO3
◦Ca2+, Sr2+, Ba2+
Alkali Metals
 Tidak bereaksi dengan reagen golongan sebelumnya
◦Mg, Na, NH4+, Li,

Separation of cations
SAMPLE

Results Separ. of HM Selective Group


Ident. NH4+
verification by NH4HS reactions reaction HCl

Selective solution, filtrate precipitate


reactions group reaction AgCl, Hg2Cl2,
Na+, K+, Mg2+ H2SO4 PbCl2

solution, filtrate precipitate


additional group BaSO4, CaSO4,
reactions PbSO4
Thank you

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