Analaysis Cation & Anion
Analaysis Cation & Anion
Analaysis Cation & Anion
TITLE
B.
PURPOSE
confirmatory tests are required. The detection of a particular ion in a sample that
contains several ions is somewhat more difficult, because the presence o the other
ions may interfere with the test. This problem can be circumvented by precipitating,
thereby removing, the disturbing ions from solution prior to testing for the particular
ion. The successful analysis of a mixture containing large number of ions centres
upon the systematic separation of the ions into groups containing only a few ion. It is
much simpler task to work with 2 or 3 ions than with 10 or more. Ultimately, the
separation of cations depends upon the difference in their tendencies to form
precipitates, or to form complex ions.
One of the best and well known separation scheme, outlined below, was first
described by R. Fresenius in 1841, though in the course of time modifications were
introduced. In this system cations are classified into five groups on the basis of their
behavior against some reagents, called group-reagents. By the systematic use of these
reagents one can decide about the presence or absence of groups of cations, and can
also separate these groups for further examination. The group reagents used for the
classification of most common cations are hydrochloric acid, hydrogen sulfide,
ammonium sulfide, and ammonium carbonate. Classification is based on whether a
cation reacts with these reagents by the formation of precipitates or not. It can
therefore be said that classification of the most common cations is based on the
differences of solubility of their chlorides, sulfides, and carbonates. The five groups
of cations and the characteristics of these groups are as follows:
Group 1
Cations of this group form precipitates with dilute hydrochloric acid. Ions
of this group are lead (II), mercury (I), and silver (I). Rationale: Softest acids react
strongly enough with a borderline base to precipitate in acid solution
Group 2
The cations of this group do not react with hydrochloric acid, but form
precipitates with hydrogen sulfide in dilute mineral acid medium. Ions of this
group are mercury (II), copper (II), bismuth (III), cadmium (II), tin(II), tin(IV),
arsenic(III), arsenic(V), antimony(III), and antimony(V). The first four form the
Analysis Cation And Anion
sub-group 2/a and the last six the sub-group 2/b. While sulfides of cations in
Group 2/a are insoluble in ammonium polysulfide, those of cations in Group 2/b
are soluble. Rationale: Soft acids react with a very soft base.
Group 3
Cations of this group do not react either with dilute hydrochloric acid, or
with hydrogen sulfide in dilute mineral acid medium. However they form
precipitates with ammonium sulfide in neutral or ammoniacal medium. Cations of
this group are iron (II), iron (III), cobalt (II), nickel (II), manganese (II),
chromium (III), aluminum (III), and zinc (II). Rationale (1): ZnS, NiS, FeS as
sulfides, i.e. borderline acids bind to a very soft base, when the pH is adjusted so
as to weaken the M(OH2)nm+ hydrated cation. Rationale (2): Fe(OH)3, Cr(OH)3,
Al(OH)3 precipitate because these are hard acids reacting with the hard base OH-.
As acidic cations, they will tend to precipitate when the pH is equal to the pKa.
These are all hard cations, and therefore prefer the hard base OH
Group 4
Cations of this group do not react with the reagents of Groups 1, 2, and 3.
They form precipitates with ammonium carbonate in the presence of ammonium
chloride in neutral medium. Cations of this group are calcium (II), strontium (II),
and barium (II). Rationale: These are weakly acidic (Bronsted definition) cations.
The carbonates are insoluble because of the favorable lattice energy when the
weakly basic carbonate ion reacts with these cations, since the cation and anion
are both doubly charged and similar in size.
Group 5
Common cations, which do not react with reagents of the previous groups,
form the last group of cations, which includes magnesium(II), lithium(I),
sodium(I), potassium(I), and ammonium(I) ions. Rationale: These are weakly
acidic (Bronsted definition) cations. The carbonates are insoluble because of the
Analysis Cation And Anion
favorable lattice energy when the weakly basic carbonate ion reacts with these
cations, since the cation and anion are both doubly charged and similar in size.
ANION :
Qualitative analysis is a method used for identification of ions or compounds
in a sample. In many cases, qualitative analysis will also involve the separation of
ions or compounds in a mixture. Examples of qualitative tests would include ion
precipitation reactions (solubility tests) or chemical reactivity tests. The separation of
ions is easily achieved by taking advantage of their solubility properties
To facilitate the analysis process, it is often useful to put ions that react in
similar ways and follow similar chemical reaction patterns into groups. For example,
it may be useful to group ions based on their solubility properties. Some anions such
as halides and sulfates are insoluble in lead containing solutions while remaining
soluble in iron or copper containing solutions. Therefore, anions can be roughly
classified into groups according to their solubility in a particular solution. The
reactions used to form groups of anions are referred to in this lab protocol as
classification reactions. The individual anions in each group are then separated and
identified using different reactions often referred to as confirmatory reactions.
Having become familiar with the characteristic reactions of anions, one may
be able to identify an unknown material using simple chemical tests and separations.
In this process, called inorganic qualitative analysis, one deals with the detection and
identification of the elements that are present in a sample of material. Frequently this
is accomplished by making an aqueous solution of the sample and then determining
which anions and anions are present on the basis of chemical and physical properties.
If a sample contains only a single anion, their identification is a fairly simple and
straightforward process, although to distinguish between two anions that have similar
chemical properties is not easy and in this instance additional confirmatory tests are
required. The detection of a particular ion in a sample that contains several ions is
somewhat more difficult, because the presence o the other ions may interfere with the
test. This problem can be circumvented by precipitating, thereby removing, the
disturbing ions from solution prior to testing for the particular ion. The successful
analysis of a mixture containing large number of ions centres upon the systematic
separation of the ions into groups containing only a few ion. It is much simpler task
to work with 2 or 3 ions than with 10 or more. Ultimately, the separation of anions
depends upon the difference in their tendencies to form precipitates, or to form
complex ions.
The methods available for the detection of anions are not as systematic as
those which have been described above for cations. No really satisfactory scheme has
yet been proposed which permits the separation of the common anions into major
groups, and the subsequent unequivocal separation of each group into its independent
constituents; however, it is possible to detect anions individually in most cases, after
perhaps a 1-2 stage separation. It is advantageous to remove all heavy metals from the
sample by extracting the anions through boiling with sodium carbonate solution;
heavy metal ions are precipitated out in the form of carbonates, while the anions
remain in solution accompanied by sodium ions.
The following scheme of classification of anions has been found to work well
in practice; anions are divided into four groups on the basis of their reactions with
dilute hydrochloric acid and of the differences of solubility of their barium and silver
salts.
The four groups of anions and the characteristics of these groups are as
follows:
Group 1
Visible change, gas evolution and/or formation of a precipitate, with dilute
hydrochloric acid. Ions of this group are carbonate, silicate, sulfide, sulfite, and
thiosulfate.
The first group of anions to be separated will be those that precipitate in the
presence of calcium ions, Ca+2. Sulfate ions, SO4-2, and carbonate ions, CO3-2,
precipitate, that is they form a solid, when mixed with an aqueous solution
containing Ca2+ ions. The net ionic equations representing the reactions occurring
are shown below:
Ca+2(aq) + SO4-2(aq) CaSO4(s)
Equation 1
Equation 3
Equation 4
Group 2
The anions of this group do not react with hydrochloric acid, but form
precipitates with barium ions in neutral medium. Ions of this group are sulfate,
phosfate, fluoride, and borate.
When mixed with dilute sulfuric acid, and heated, the nitrite ion, NO2-, forms
red-brown nitrogen dioxide gas and nitrate ion. This is a confirmatory reaction,
since only one ion is involved.
2NO2-(aq) NO(aq) + NO3-(aq)
Equation 5
Equation 6
precipitate is formed, it will not dissolve on addition of acid. The Ag + ion solution
used in this experiment is aqueous silver nitrate solution, the only silver salt that
is soluble in water. Net ionic equations:
Ag+(aq) + Cl-(aq) AgCl(s)
Equation 7
Equation 8
Equation 9
Confirmatory reactions that distinguish between the three halide ions and
identify each are based on a redox process. All three halides can act as reducing
agents and in the process are oxidized to their diatomic elemental forms. Their
relative reducing strength is as follows: I- >Br- > Cl-. When coupled with a strong
oxidizing agent such as aqueous Cl2 (chlorine water), bromide and iodide ions
will undergo oxidation. If chloride reacts with chlorine it will produce chloride
and chlorine. While this may happen, it is easier to say that no reaction occurs
Cl2(aq) (colorless) + Cl- (aq) (colorless) No Reaction
Equation 10
Equation 11
(aq)
If Cl- ion is present in the solution, without any other halide, the chlorine
water will remain colorless. Therefore, this test verifies the presence of Cl - ion
only if the classification test produced a silver precipitate that did not dissolve in
acid. After addition of colorless chlorine water to a colorless solution of either
bromide or iodide, the solution will change color to yellow-brown, since
elemental iodine and bromine impart such color to water. This test, however, does
not distinguish between the two ions. One more step is necessary. It is not a
reaction, but a physical process of extraction with hexane of the solution obtained
Analysis Cation And Anion
upon addition of chlorine water. A small volume of hexane is added to the yellowbrown halide solution. A pink or purple hexane layer (the top layer) after
extraction indicates that the initial solution contained I- ion. A yellow to brownorange hexane layer indicates that the initial solution contained Br- ion. The
actual shade of the hexane layer depends on the concentration of the halogen (a
higher concentration of the halogen produces a darker shade).
Group 4
Common anions, which do not react with reagents of the previous groups,
form the last group of anions, which includes nitrite, nitrate and chlorate ions.
Nitrate ion does not directly produce any precipitates (remember the solubility
rules?) nor does it produce any gaseous products in an acidic environment.
However, upon reduction by Fe2+ ion it forms a characteristic brown gas,
nitrogen dioxide. As with nitrite, the reaction is considered a confirmatory one.
The equations for the reactions involved are as follows:
NO3-(aq) + 4H+(aq) + 3Fe2+(aq) NO(aq) + 3Fe3+(aq) + 2H2O(l) Equation 13
2NO(g) (colorless) + O2(g) 2NO2(g) (red-brown)
Equation 14
A specific test reagent, ideally, possesses a specific reaction with each type of
anion. The reagent might react with one anion to provide a distinguishing product,
but not with the other anions in the mixture. The color of precipitate formed and
the reaction of the precipitate formed with dilute acid or identity of gas liberated
gives us definitive proof of the unknown anion in the solution.
There are three main solution tests and these are also confirmatory tests for
specific anions:
Test reagents
The principles that are employed in the identification of cations can also be
applied to the analysis of anions. The qualitative detection of anions in a sample
depends on the distinctive solubility properties of particular salts of the ions and
specific chemical reactions that are (ideally) unique to a particular ion.
10
D.
Materials
Tools
Sample
Beaker Glass
Aquades
Test Tube
HCl 6 M
Rack
H2O2 3%
Tripot
HCl 2 M
Burner
NH4Cl 2 M
Spatula
NH4OH
Kassa
Ammonium Oxalate
Clamp
b. Anion
Materials
Tools
Unknown Solution
Test tube
Na2CO3 concentrate
Burner
AgNO3
Tripot
Kassa
Clamp
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E.
PROCEDURE
a. General Procedure of Cation
12
Analyt
Filtrate for
Analyte for
Mixed it well
Added 15 drops of NH4OH, drop by drop
Stirred
Analyte Contain of
White
Precipitate
Ca2+ Present
13
Unknown
-
Precipitate
Filtrate
-
Preparation Solution
- Added AgNO3
White Precipitate
Cl- exist
-Added NH3
Dissolve
14
F.
EXPERIMENT RESULT
a.
No.
Cation Ca2+
Procedure of Experiment
Experiment
Result
Hypothesis /
Reaction
Conclusion
15
Before:
Sampl
- Sample: colorless
Thinned with
aquades
Analyt
- Adde
d 5 drops of solution
into test tube
Added 5 drops of
water
Added 2 drops of
HCl 6 M
Stirred
Washed substances
that stick on the wall
with water
Filtrate for
Added 6 drops of
H2O2 3%
Added 2 drops of
HCl 2 M
Boiled until reach
volume 1-2 drops
Cooled dawn
Added 6 drops of
HCl 6 M
Evaporated
Analyte for
Added 4 drops of
NH4Cl 2 M
Mixed it well
Added 15 drops of
NH4OH, drop by
drop
Stirred
Analyte Contain of
- Water : colorless
- HCl
: colorless
- H2O2
: colorless
- NH4Cl : colorless
- NH4OH : colorless
- Ammonium
Oxalate (NH4)2S :
yellow
After:
- Sample + aquades:
colorless solution
(sample solution)
- Sample solution +
water: colorless
solution
- Sample solution +
water + HCl:
colorless solution
(filtrate for
procedure II)
First, we
made a hypothesis that the
sample which
is given
contain of
cation Mg2+,
Ba2+, and
Ca2+. When
we add 1-2
drops of
ammonium
oxalate, it
forms white
precipitate.
Because
calcium
oxalate
(CaC2O4) will
be form after
adding of
ammonium
oxalate.
CaCO3(s)+
H2O(l)
Separation of
calcium with
other cation
based on the
solubility of
CaC2O4 salt
which cant
dissolve on
the water,
hence the
other cation is
easy to
dissolve. If
theres white
precipitate in
calcium,
CaC2O4 will
be form when
adding
(NH4)2C2O4.
Solution made
in base
condition to
prevent the
solubility of
oxalate salt.
Ca(OH)2(aq) +
CO2(g)
Ca(OH)2(aq) +
- Filtrate 2 + H2O2:
colorless solution
2HCl(aq)
- Filtrate 2 + H2O2 +
HCl: colorless
solution
2H2O
Ca2+ +
CaCl2(aq)+
(COO)22-
16
Added 2 drops of
NH4OH
Added 2 drops of
Ammonium Oxalate
White
Precipitate
17
b. Anion ClNo
Procedure of Experiment
Experiment
Result
Hypothesis / Reaction
Conclusion
Making Preparation
Before:
- Unknown
solution:
colorless
- Na2CO3
concentrate:
colorless
- AgNO3:
colorless
After:
- Unknown
solution +
Na2CO3:
colorless filtrate
and white
precipitate
- Supply
Solution +
AgNO3: White
precipitate
Unknown solution
+AgNO3: white
precipitate
Ag+ + Cl- AgCl(white)
Na2CO3 + CaCl2
CaCO3 + 2NaCl
There is white
precipitate
after adding
AgNO3 so the
anion of Cl- is
proven.
Unknown
Solution
- Heated with
Na2CO3
Precipitateconcentrate
Filtrate
2.
Preparation Solution
Na2CO3 + 2 AgNO3
2 NaNO3 + Ag2CO3
NaCl + AgNO3
AgCl white +
NaNO3
AgCl + 2NH3
[Ag(NH3)2]+ + Cl-
White Precipitate
Cl- exist
-Added NH3
Dissolve
18
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oxalate compounds. The function of ammonium oxalate for precipitate Ca. Therefore,
we conclude that the sample contains cations Ca2+
Ca2+ + (COO)22- Ca(COO)2
Ca2+ + C2O4 CaC2O4(s)
ANALYSIS OF ANION
Analyte is colorless and the shape is like jelly. To know there is anion on
analyte, the first step that we have done is adding saturated Na 2CO3 to the reaction
tube which contain of analyte so it formed colorless solution. The purpose of adding
Na2CO3 is to dissolve the anion on the analyte , with analyte CaCl 2 (Ca is our cation)
that have been found so the equation that will be happen is :
Na2CO3 + CaCl2 CaCO3 + 2NaCl
The next step is heating the reaction tube, it purpose to faster the reaction that
occur or in other case it can give the activation energy to the solution, so the reaction
which didnt take place in the beginning because less of activation energy, through of
heating the reaction can be occur.
The third step is separation between precipitate and filtrate, it purpose to
remove the other substance which may be react with reagent to be added later. And
the fourth steps is adding AgNO3 and filtrate, it purpose to difference between Cl- and
Br-.
Na2CO3 + 2 AgNO3 2 NaNO3 + Ag2CO3
CO32- ion is precipitated when ionic displacement occurs..
In this experiment Cl- ion would be formed white precipitate and Br- ion
would be formed yellow precipitate.
NaCl + AgNO3 AgCl white + NaNO3
The last step is dissolve the precipitate into NH3 it purpose to keep the
possibility of a substance that
precipitate too, so that if the substance is reacted with NH3, AgCl will react while
AgCN not react, so that when the precipitate dissolved in NH 3 it can be concluded
that of the analyte anion is Cl-. The reaction is:
AgCl + 2NH3 [Ag(NH3)2]+ + ClAnalysis Cation And Anion
20
H.
CONCLUSION
I.
21
: M2+ + S2- MS
with M2+ = Zn2+, Co2+, Ni2+
Group V
22
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J. REFERENCE
http://www.inc.bme.hu/en/subjects/inchem/sillabus/129-145.pdf Accessed on
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December 2nd 2013 at 15:05
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Accessed
on Monday, December 2nd 2013 at 15:38
http://www2.ucdsb.on.ca/tiss/stretton/chem3/lab_24_intro_qa_theory.html Accessed
on
Monday, December 2nd 2013 at 16:15
http://chemist-try.blogspot.com/2013/01/analisa-kualitatif-reaksi-identifikasi.html
Accessed on Monday, December 2nd 2013 at 17:55
http://www.crescent.edu.sg/crezlab/Webpages/AnionLabManual01.htm Accessed on
Monday, December 2nd 2013 at 17:58
http://www.inc.bme.hu/en/subjects/inchem/sillabus/129-145.pdf Accessed on
Monday,
December 2nd 2013 at 15:05
http://sunny.moorparkcollege.edu/~chemistry/chemistry_1B_labs/experiment_twelve.
pdf
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http://www.slcc-science.org/chem/labs/chem1225/1225experiment07.pdf Accessed
on
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Svela, G. 1985. VOGEL Buku Teks Analisis Anorganik Kualitatif Makro dan
Semimakro. Edisi ke 5. Jakarta: PT. Havery Indah.
Achmad, Hiskia. 2012. Kimia Analitik Kualitatif. Bandung:PT. Citra Aditya Bakti.
Tim.2013.Panduan Praktikum Kimia Analitik I Dasar-Dasar Kimia Analitik.
Surabaya:Jurusan Kimia FMIPA UNESA
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ATTACHMENT
PICTURE
EXPLANATION
Unkown solution (clear like gel)
26
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