ANALYTICAL SEPARATION MARCH OF ANIONS OF THE 2ND, 3RD AND 4TH GROUP

1. General Objectives

Separate the anions and identify the anions of the second, third, and fourth group.

2. Theoretical framework

For the analysis of salts or mixtures of salts, procedures must be applied to

analysis of cations and furthermore, all anions must be investigated. Although not
there is an orderly procedure for the separation or identification of anions,
as there are for cations, however to test for the presence of anions one
they must follow defined steps.
The absence of certain ions can be tested with a single test, eliminating
thus the need to conduct individual tests for those discarded ions.
Common anions can be divided into three groups:

1. Chloride group: forms salts with silver ions, which are insoluble in
diluted nitric acid. According to Ray Brumblay, the selected chlorides are: Cl--,
I- , and S2-.
2. Sulfate group: forms salts with barium or calcium ions, which, with
exception of BaSO4They are soluble in diluted nitric acid but insoluble in water.
selected ions are: sulfate (SO4),, sulfite-2 (SO32-), phosphate (PO4-3),
2-
arsenate (AsO43-borate (BO2-carbonato (CO32-), chromate (CrO4), oxalate(C 2O4 ) y
2-

fluoride (F) ).
-

3. The anions of a third group do not form insoluble salts with any of the ions.
of silver, barium, or calcium. These anions are: acetate (C2H3O2-) nitrate (NO3), -and nitrite
(NO2-Due to nitrate ion being the most common of these soluble ions, this group is referred to as
denomination group of nitrates.

3. Experimental part

a. Observations

The solution shows a transparent yellowish color.

By adding Zn(NO3)2a white precipitate was observed.
Water washing, centrifugation and decantation were performed. 5 drops of 6M HCl were added and
immediately covered the mouth of the test tube with a square of paper
previously moistened filter with Pb(CH3COO2. After about 2 minutes, it
he observed a dark brown circle on the filter paper.
Then the solution was separated into two parts:
5 drops of FeCl were added to the first part.30.2 M. A blue precipitate was observed.
intense.
5 drops of FeSO were added to the other part.40.2 M. A blue precipitate was observed.
celestial, clearer than the previous one.
When we added silver nitrate, a slightly yellow precipitate was observed.
-When NH was added35M can be centrifuged and a precipitate can be observed (AgBr and
AgI) and a solution, to this last one HNO is added.36M until acidity is observed
a white precipitate.
To the precipitate (AgBr and AgI) add 3 drops of ammonium sulfide, then
Centrifuging and decanting will reveal a black precipitate, which will be discarded.

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Zinc is added to the remaining solution (NO3)2after centrifuging and decanting
A white precipitate will be observed, which will be discarded.
Carbon tetrachloride and water are added to the remaining solution of this last step.
of chlorine, a purple color will be observed, if more chlorine water is added, it
you will observe an orange color.
In the recognition of the acetate anion, a characteristic fruit smell is noted.
For the permanganate anion, it was observed that when crystals of FeSO are added4.7H2O
the coloration changed from purple to yellow.
When the nitrate was analyzed, the addition of the reagents resulted in a final
brown ring that divided two phases.

b.Chemical equations

+¿ → H 2S g ( )

2−¿+2 H ¿
S¿

2+¿ L e a d S u l f i d e (s)
H 2S+Pb¿

Fe(CN)
3+¿ → F e 4 [ Fe( CN6) ]3(s)
4−¿+ 4Fe¿
[¿¿6]¿
3¿
(Prussian blue)

4−¿
¿
3+¿+[Fe ( CN )6 ]
3−¿ I r o n ¿
¿
2+¿+[Iron( CN )6 ]
Fe ¿
Subsequently:
Fe(CN)
( CN6) ]3(s)
3+¿ → F e 4 [ Iron
4−¿+4Fe¿
[¿¿6]¿
3¿
(Turnbull blue)

AgCl: white precipitate

Silver chloride(ac)+ 2NH3(ac) Ag (NH3)2Cl(ac)

Ag (NH3)2Cl(ac) 2HNO3(ac)AgCl(s)+2NH4NO3(ac) Kps=1.8x10-10

white precipitate

Br-bromine ion

ZnBr2(ac) + Cl2(ac)+I2(ac)Br2+ 2 ZnCl2(ac)+ I2(ac)orange solution

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 I- iodine ion

ZnBr2(ac)+ Cl2(ac) + I2(ac)Br2+ 2 ZnCl2(ac)+ I2(ac)(purple solution)

CH3COO-(ac) + H2SO4 (continued)CH3carboxylic acid group(ac)+ HSO4-(ac)

CH3COOH(ac)+ C2H5OH(ac)CH3COO.C2H5(v)+ H2O(l)

MnO4-(ac)+ 5 Iron2++ 8H+ 5 Fe3++ Mn2+(ac)+ 4 H2O(l)

2 NO3-(ac)+ 4 H2SO4 (continued)+ 6 Fe2+(ac)→6 Fe3+(ac)+2 NO(g)+ 4 SO4-(ac)+ 4 H2O(l)

Fe2+(ac)+ NO(g) Iron Nitrosyl2+(ac)

c. Process diagram

Identification of anions of the second group

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Identification of the anions of the third group

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Identification of anions of the fourth group

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d.Conclusions

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The dark brown circle observed on the filter paper was a precipitate of PbS.
which confirms the presence of sulfide ions S2-.
The dark blue precipitate was iron (III) cyanide, also called blue of...
Prussia, which confirms the presence of hexacyanoferrate ions of iron (III).
The sky blue precipitate turned out to be iron (III) ferrocyanide, also called blue.
from Turnbull. Although it has the same formula as Prussian blue, the difference is in
the name, since it was once believed that the precipitate had the formula
Fe3[Fe(CN)6]2hexacyanoferrate of iron (II), there lies the difference in the name.
The presence of the chloride ion can be confirmed by the formation of a
white precipitate, which will be silver chloride.
The presence of the iodide ion can be confirmed by a violet coloration of
our solution, which contains iodide, thanks to the release of iodine after
add chlorine water and shake with 0.5mL of tetrachloride.
The presence of the bromide ion can be confirmed by an orange coloration.
from our solution, which contains bromide, thanks to the release of bromine after
add chlorine water and shaking with 0.5mL of tetrachloride.
The recognition of the acetate anion can be carried out due to the formation of
ethyl acetate (CH3COO.C2H5that is recognized by its pleasant fruity smell.
By adding iron(II) sulfate to the permanganate, it acts as an oxidizing agent.
and iron (II) appears which gives the observed yellow color as a consequence of
the simultaneous reduction of permanganate.
In the contact area of the two liquids that were poured into the solution, a
brown ring that is given due to the formation of [Fe(NO)]2+This allows to recognize
that the nitrate was indeed present in the solution. This test could not be performed if
there would have been halogens since they interfere in the reactions, the same happens with the
chromates, sulfites, cyanides and others that must be removed before the recognition of
nitrate anion.

4.Questionnaire

1. Create a flow diagram to identify chloride ions in a sample.

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2. Complete the following chemical reaction:

2NO3 4H3 O   2Br

2 HBr + 2 HNO3+ 4 H2O

What is a coordination complex?

InchemistryA complex is referred to as an entity that is formed by a

association that involves two or more components linked by a type oflink
chemical, thecoordinating linkwhich is usually a little weaker than
acovalent bondtypical.
Historically, the term complex is primarily used for
describe that type of molecular structure that is usually formed
by a central atom (which is often acationmetallicthat is located
linked to an ordered array of other groups of atoms that surround it
callsligands. This last meaning is also known as entity of
coordination.
The term is also used to refer to a huge number of structures.
unstable or metastable that act as intermediaries in different
reactions; therefore it is preferable to always use a more suitable term whenever possible.
explanatory to refer to these compounds. In this sense, the term complex is
much wider, but less precise. In inorganic chemistry, for example, it
prefers to use the term coordinating entity instead of complex.

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4.Dar 5 ejemplos de complejos indicando sus nombres.

K4[Fe(CN)6potassium hexacyanoferrate (II)

[Co(H2O)6]Cl2hexaaquacobalt(II) chloride

[Cu(NH3)4]SO4tetramminecopper(II) sulfate

CoBr2(en)2Dibromobis(ethylenediamine)cobalt(III) chloride

[Pt(NH3)4] [PtCl6tetrammineplatinum(II) hexachloroplatinate(IV)

5. Bibliography

Books:

Atkins, P.
Chang, R. (2012). Chemistry. Mexico City: McGraw Hill.
Vogel, A. (1983). Qualitative Analytical Chemistry. Buenos Aires: Kapelusz

Articles:

-Guide to practical work in analytical chemistry 2010. National University of

Catamarca, Argentina.

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