Analytical Procedures for Cations Groups 4 & 5
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ScribdTranslationsAnalytical Procedures for Cations Groups 4 & 5
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ScribdTranslationsAnalytical March of Cations 4toand 5toGroup
Objectives
Carry out the systematic procedure of the analytical flow of cations of the
group 4 and 5, separately.
Apply the flame test identification method to certain ions.
Know your identification reagents.
2. Theoretical foundation
Cations of 4togroup
This group comprises the ions of the three alkaline earth metals: Ca, Sr and
Ba. The peculiarity of this group lies in that they are not precipitated by H.2S,
(NH4)2Sxand HCl, but they precipitate with ammonium carbonate (NH4(CO3)2) in
presence of ammonium hydroxide (NH)4OH).
The obtained precipitate contains the carbonates of those ions which are: BaCO3,
SrCO3and CaCO3These precipitates are soluble in dilute acids, due to this
CH is added3COOH 6 M for its complete dissolution. To separate the Ba ion.2+
in the form of a precipitate that contains said element, the reagent must be used
potassium chromate (K)2CrO4yellow in color whose pH is alkaline. To make
This separation is necessary for the acidic pH due to the CH.3COOH remains
approximately, for this reason a CH solution is added3COONH4for
to form a buffer system that will mitigate the increase in pH due to the
add the reagent K2CrO4.
The solution will turn orange due to the presence of the dichromate ion (Cr2O7) 2
which is formed in the presence of acid or pH<6, and a precipitate will be formed whose
reaction is:
2 2
Ba CrO
(ac)
BaCrO
4(ac) 4(s)
A1) When separating the precipitate formed by centrifugation and decantation, it should be
perform two tests: flame test and hydrogen identification reaction2SO4.
For this, it is necessary to dissolve the precipitate that supposedly contains
Barite, then add 6 M HCl until completely dissolved.
The call test consists of using a nichrome wire, previously
making a ring at one end of said wire and then dipping the end
folded in a solution of muriatic acid (commercial HCl), to later take it
to the hottest part of the flame until no coloration is observed in the
same.
The previous procedure aims to remove the impurities from said wire.
(only on the bent end). Once the wire has been cleaned, you
immerse in the solution of the isolated cation to be analyzed and the wire is taken
extreme) to the base the flame, in which, depending on the cation, one will appreciate a
specific coloration of the flame for a brief period of time.
Table No. 1 shows us the relationship of the flame color on the wire of
nicrome according to the solution of the cation to be analyzed:
Table No. 1
Element Color of the flame Observations
Na Yellow Persistent
K Violet Not very persistent,
sodium interferes
Ca Red brick The Ba interferes
Sr Orange-reddish Similar to Ca
Ba Light green Not very persistent,
Mr. interferes
Hg (Hg2+) Intense violet A sample is used of
HgCl2
Li Crimson Na and Ba interfere.
The above table shows us that, to analyze the Ba, it is necessary to remove the
traces of Mr that are in the separated precipitate, for this it is washed twice with
hot water to remove the Sr and thus avoid interferences. For the Barium, the
the coloration must be light green or lime green. If this coloration is not present, it
confirm that the Ba ion does not exist in the original solution of the cation march.
The other method to identify Ba is by adding to the solution of the precipitate of
Dissolved with HCl, a solution of H2SO46 M, in which a will be formed
white precipitate whose reaction is:
Barium Chloride2(ac) H2 SO4(ac) BaSO4(s) 2 HCl(ac)
The white precipitate BaSO4it is insoluble in water and diluted sulfuric acid. In
concentrated sulfuric acid dissolves.
A2) On the other hand, the separated solution of the BaCrO precipitate4, that contains
the Sr ions2+and Ca2+it is dealt with a procedure in order to convert them into
precipitates that contain carbonate and remove chromate and/or dichromate. It
dissolve the precipitate with a weak acid (CH3COOH) and is divided into 2 portions,
to analyze Sr and Ca separately.
Portion 1 (Mr): A saturated solution of CaSO is added.4, in which there will be
a slow reaction in cold, forming a precipitate that
supposedly contains SrSO4the precipitate is separated and dissolved
same with HCl, to then confirm the presence of the Sr ion2+through the test
of the flame (the coloration of the flame should be orange-reddish according to table No. 1).
Portion 2 (Ca): Mr should be removed.2+from this portion because it reacts
with ammonium oxalate ((NH4)2C2O4) and produces an identical precipitate in color
compared to that produced with Ca2+, this would lead us to erroneous results.
For example, we add the NH4OH y (NH4)2C2O4to the second portion without having
having taken the previous step and if we obtain a white precipitate, we could conclude that
wrong way, that there are Ca ions2+in the sample but that in reality the
the formed precipitate would be SrSO4and not CaCO3For this reason, H is added.2SO4,
forming both SrSO4like CaSO4as precipitates. These precipitates
they are separated from the solution and the Ca ion is identified2+.
Identification reaction of the Ca ion2+:
2 2
Ca C 2The
(ac)
CaC O
4(ac) 2 4(s)
Cations of 5togroup
This group of cations consists of Na ions.+, K+, Mg2+and the ammonium ion
(NH4+This last cation is included in this group because its compounds are
they resemble those of alkali metals, especially those of potassium. Although
magnesium is found in the alkaline-earth metals group in the periodic table,
it is included here because its carbonate does not precipitate due to solution of
ammonium carbonate ((NH4)2CO3) in the presence of NH4Cl and basic middle.
The solution containing only ions from group 5 is treated beforehand.
through a process aimed at evaporating the ammonium salts and preventing
interferences in the identification reactions. Once this is done, it is divided into
four equal portions:
Portion 1 (Mg): In this portion, Mg is investigated.2+with its reagent of
identification, the magneson (p-nitrobenzene-azo-resorcinol), resulting positive if
a blue precipitate appears in the presence of NaOH.
Portion 2 (Mg): This second method to investigate Mg2+use as reagent
sodium phosphate (Na2HPO4), which, in the presence of NH4Cl (for
prevent the precipitation of magnesium hydroxide) and NH3(ac), a occurs a
crystalline white precipitate with the formula Mg(NH4)PO4.6H2O (ammonium phosphate
hexahydrated magnesium) which is very poorly soluble in water.
Portion 3 (K): In the analysis of the K ion+ it is used as an identification reagent for
Hypochlorous Acid4(perchloric acid), forming a crystalline white precipitate of KClO4,
very poorly soluble in water and practically insoluble in ethyl alcohol, for this reason it is
this last reagent is added to better visualize the formed precipitate.
Portion 4 (Na): The identification reagent to investigate sodium is acetate.
from uranyl and magnesium (Blanchetierre reagent), forming a yellow precipitate
Yes, there is the presence of that ion.
Properties and hazards of the reagents used in the laboratory (NFPA)
Perchloric acid
Molecular formula: HClO4
Molecular weight: 100.46 g/mol
Physical-chemical properties:
- Physical state: oily liquid.
- Odorless
- Melting point: -19 °C
- 203 °C
- Specific gravity: 1.67
- Easily soluble in cold water
- It is unstable.
- Highly reactive with combustible materials, organic materials,
acids, alkalis.
Disodium phosphate anhydrous
Molecular formula: Na2HPO4
Molecular weight: 141.96 g/mol
Physical-chemical properties:
- Physical state: white solid.
- Odorless
- Melting point: 250 °C
- Specific gravity: 1.7
- Easily soluble in cold water.
- Stable compound.
- Reacts with oxidizing agents, acids, and alkalies.
c) Potassium chromate
Molecular formula: K2CrO4
194.19 g/mol
Physical-chemical properties:
- Physical state: yellow crystalline solid.
- No smell
- Melting point: 975 °C
- Specific gravity: 2.73
- Easily soluble in cold water, hot.
- Stable material under normal conditions.
- Reagent with combustible, organic materials.
ammonium oxalate
Molecular formula: (NH4)2C2O4
Molecular weight: 124.11 g/mol
Physical-chemical properties:
- Physical state: solid white odorless.
- Melting point: 70 °C (decomposes).
- Gravedad específica: 1.5
- Partially soluble in cold water.
- Stable material under normal conditions.
Calcium sulfate
Molecular formula: CaSO4
Molecular weight: 136.14 g/mol
Physical-chemical properties:
- Physical state: odorless crystalline solid.
- Melting point: 1450 °C.
- Specific gravity: 2.96
- Solubility in water: 0.21 g / 100 mL at 20 °C.
- Stable material under normal conditions.
- Reacts with oxidizing agents and acids.
Web references:
[Link] (pictograms)
Consulted bibliography:
