Mixture of Anions

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Experiment#2

Determination of anions in a binary salt mixture.

Introduction:

Salt analysis is the qualitative analysis of actions and anions present in a given pure
inorganic salt or in a mixture. The salt analysis involves a series of chemical reaction steps
that helps in identifying a salt and its constituent ions.

Binary salts are a mixture of salts which is composed of ions of different elements on eof
which is a metal and the other is nonmetal. For example Sodium iodide, NaI is composed of
sodium ions Na+ (metal) and iodide ions I- (nonmetal).

Theory:

Qualitative analysis is carried out through the reactions which are easily perceptible to our

senses such as sight and smell. Such reactions involve:

(a) Formation of a precipitate

(b) Change in color

(c) Evolution of gas etc.

Systematic analysis of an inorganic salt involves the following steps:

(i) Preliminary examination of solid salt and its solution.

(ii) Determination of anions by reactions carried out in solution (wet tests) and confirmatory
tests.

Two basic principles of great use in the analysis are:

(i) The Solubility product; and

(ii) The Common ion effect.

When ionic product of a salt exceeds its solubility product, precipitation takes place. Ionic
product of salt is controlled by making use of common ion effect.

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BROMIDE NITRATE
Aim

To identify the anionic radicals present in an inorganic mixture of anionic salts by performing
various tests.

Theory:

In bromide nitrate there are two salts bromide and nitrate. As the two radicals in this
experiment, Br- and NO-3 are acidic radicals or anions. We use test of acidic radicals for the
estimation of these ions.

Apparatus:

• Test tubes
• Test tube Holder
• Test Tube stand
• Pipette
• Measuring Cylinder
• Beakers
• Bunsen Burner

Chemicals:

• Reagents (Dilute H2SO4, Conc. H2SO4),


• AgNO3 solution,
• NH4OH solution,
• Dilute HNO3 acid,
• KMnO4,
• CS2,
• FeSO4 Solution,
• Diphenylamine (C12H11N),
• NaOH Solution,
• Aluminum foil

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Procedure:

Tests For Bromide

Experiment Observations Inference


Dry Tests:
Action of dilute Acid

Salt + dilute H2SO4 No reaction. Cl–, Br–, I–, CH3COO–, NO3–


& C2O42– may be present.
Action of conc. Acid
Took 0.1 g of salt in a test Reddish brown gas with a Bromide (Br–) or Nitrate
tube and 3-4 drops of conc. pungent odor and Brown (NO3– )may be present.
H2SO4. fumes evolved.

Wet Tests:

Took 0.1 g of salt and a pinch Intense brown fumes are Br is present.
of MnO2 in a test tube. evolved.
Added 3-4 drops conc.
H2SO4 and heat.
Salt solution+ BaCl2 solution No ppt. Nitrate (NO3–) is also
present.
Confirmatory Tests:
Silver nitrate test
Salt soln. + AgNO3 soln. Yellow ppt. are formed. Br– is present.

Ppt. + NH4OH solution Not dissolved completely. Br– is present.

Ppt. + dilute HNO3 acid. Completely dissolved. Br– is confirmed.


Layer Test
Salt soln. + CS2 + KMnO4 + Orange color layers are Br– is confirmed.
dilute H2SO4 + shake well. formed.

Tests For Nitrate

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Dry Tests:
Action of dilute Acid

Salt + dilute H2SO4 No reaction. Cl–, Br–, I–, CH3COO–, NO3–


& C2O42– may be present.
Action of conc. Acid
Took 0.1 g of salt in a test White fumes with pungent Bromide (Br–) or Nitrate
tube and 3-4 drops of conc. smell. (NO3– )may be present.
H2SO4.

Wet Tests: No Precipitates. Nitrate (NO3–) may be


Salt solution+AgNO3 present.

Nitrate (NO3–) may be


Salt solution+BaCl2 solution. No Precipitates. present.

Confirmatory Tests:

Brown Ring test


Took 1 mL of salt solution in A dark brown ring is formed Nitrate (NO3–) is confirmed.
water in a test tube. Added 2 at the junction of the two
mL conc. of H2SO4 and solutions.
mixed thoroughly. Cool the
mixture under the tap. Added
freshly prepared ferrous(II)
sulphate (FeSO4) solution
along the sides of the test
tube without shaking.
Ring test
Took 1mL salt solution in Dark blue ring is formed. Nitrate (NO3–) is confirmed.
test tube, added few drops of
diphenylamine (C12H11N)
and conc.sulphuric acid
(H2SO4)

Salt soln. + Aluminum foil Ammonia smell. Nitrate (NO3–) is confirmed.


pieces + NaOH Solution +
heat.

Result:

The given anionic mixture of salts contains Potassium Bromide (KBr) and Sodium
Nitrate (NaNO3).

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OXALATE CHLORIDE
Aim
To identify the anionic radicals present in an inorganic mixture of anionic salts by performing
various tests.

Theory:

In Oxalate chloride there are two salts oxalate and chloride. As the two radicals in this
experiment, C2O2-4 and Cl- are acidic radicals or anions. We use test of acidic radicals for the
estimation of these ions.

Apparatus:

• Test tubes
• Test tube Holder
• Test Tube stand
• Pipette
• Measuring Cylinder
• Beakers
• Bunsen Burner

Chemicals:

• Reagents (Dilute H2SO4, Conc. H2SO4),


• AgNO3 solution,
• NH4OH solution,
• Dilute HCl
• KMnO4

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• K2Cr2O7
• Lead Acetate,
• Lime water
• Acetic Acid
• BaCl2
• CaCl2

Procedure:

Tests For Oxalate

Experiment Observations Inference


Dry tests:
Action of dil.acid
Original salt + dil.H2SO4 No reaction. Cl- - may be present,Br-,I- ,
Action of conc. acid NO-3 , C2O4 -2 , CH3COO.

Original salt + conc. H2SO4 Colorless gas burns the Cl- ,Br-,I- , NO-3 , C2O42- ,
+ heat. flame bluish color appeared. CH3COO-may be present.

Pass the gas through lime Milky colour of water C2O4 -2 may be present.
water. prepared.

Wet Tests:
Original salt soln + BaCl2 White precipitates are C2O4 -2may be present.
soln. formed.
Add above soln. in 2 test
tubes.
One containing dil. HCl Vapours dissolved. C2O4 -2 may be present.
other contain acetic acid. Vapours not dissolved.

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Confirmatory Tests:

O.S+ CaCl2 soln. White precipate C2O4 -2 is confirmed.

Add above soln. in 2 test Ppts dissolved on heating. C2O4 -2 is confirmed.


tubes. One containing dil.
HCl other contain acetic Not dissolved.
acid.

O.S + dil. H2SO4 + heat + Purple colour vanishes. C2O4 -2 is confirmed.


KMnO4 soln. dropwise
added in soln.

Tests for Chloride


Experiment Observation Inference
Dry Tests:
Took a pinch of given salt in No reaction. Cl–, Br–, I–, CH3COO–, NO3–
test tube then added dilute & C2O42– may be present.
H2SO4 in it.
Cl–, Br–, I–, CH3COO–, NO3–
0.1g Salt + 1ml conc. H2SO4 Fumes evolved. & C2O42– may be present.

Wet Tests:

Above salt solution + dipped Irritating gas with white Cl– may be present.
glass rod of NH4OH solution fumes evolved.
brought close to the brim of
test tube.
Silver nitrate Test Cl– is confirmed.
White precipitates formed.
Took salt solution in a test
tube and added AgNO3 Cl– is confirmed.
solution in it. Ppt. dissolved.
Precipitates + NH4OH
solution.

Confirmatory Tests:

Orange ppts. are formed. Cl– is confirmed.


Chromyl chloride Test
Salt + conc. H2SO4 +
K2Cr2O7 (powdered
Yellow colored ppts. are Cl– is confirmed.
potassium dichromate).
formed.
Above soln. + NaOH soln. +
lead acetate soln.

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