SHEHAL A HoLEY
SEMI - MICRO QUALITATIVE ANALYSIS OF SIMPLE INORGANIC SALT
CATIONS: Pb Hqcuca? Ag'. Fe?, Fe. [Link]?, Mn,Co. Sr, Ba Ma', NHA
ANIONS: CO,S , SO, SO,, NO,, NO,, Cl, Br . PO,3 CH,COO
PRELIMINARY TESTS
1. Note the state (amorphous or crystalline) and colour of
salt.
2. Test the solubility of the salt in the following
solutions:
i Water (cold and hot)
ii. Dilute HCl (cold and hot)
iii. Dilute HNO3 (cold and hot)
IDENTIFICATION OF ACID RADICALS (ANIONS)
This part is the classified into three
groups:
FIRST GROUP OF ACID RADICALS
The acid radicals involved in this group are carbonate(CO,), Sulphide(s),
Thiosuiphate(S,0,)and nitrate(NO,). The group reugent is diiute hydrochloric [Link](SO,).
EXPERIMENT OBSERVATION INFERENCE
Sait + dil. Hci
Effervescence or evolution of gases 1s group of acid radicas is presert.
(a) Colourless, odouriess gas turns lime water
milky The acid radicai may be Co or Hco
(b) Colourless with rotten eggs smell and turns
lead acetate paper black. Sulphide(s) is confirmed.
(c) Colourless gas with suffocating smell. Heat
and pass the gas through acidified KzCrz0, SO is confirmed.
solution. The solution turns green
(d) Colourless gas with suffocating smell with a
yellow ppt. of sulphur in the test tube. Heat and
pass the gas through acidified KzCr0, solution. S,0 is confirmed.
The solution turns dark blackish green.
(e) Colourless gas followed by brown gas and it
turns starch iodide paper blue. NO, is confirmed.
(f) Colourless qas with the smell of vinegar. The acid radical may be CHsCO0
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Tests to distinguish between CO, and HCO3
EXPERIMENT OBSERVATION INFERENCE
Salt + water, boil and pass the (a) Lime water does not turn milky. CO is confirmed.
gas through lime water HCO, is confirmed.
(b) Lime water turns milky.
Confirmation test for Acetate
EXPERIMENT OBSERVATION INFERENCE
Salt solution + Neutral FeCl; sol. Appearance of blood red colour. Acetate is confirmed
SECOND GROUP OF ACID RADICALS
The acid radicals involved in this group are Cl, Br and NO:. The group reagent is concentrated
sulphuric acid (H;SO4).
EXPERIMENT OBSERVATION INFERENCE
Effervescence with colourless or coloured gases 2nd group Acid radical is
present
(a) Colourless gas with a pungent smell and gives dense
Salt + white fumes when a glass rod dipped in ammonium The Acid radical may be Cl
Concentrated
hydroxide (NH,OH) is exposed.
H2SO, and heat
if necessary. (b) Brown gas and the solution is not blue. The acid radical may be Br
(c) Light brown gas and brown gas with pieces of copper
turnings and the solution turns blue in the test tube. The Acid radica! may be NO
Confirmation test for Chloride
EXPERIMENT OBSERVATION INFERENCE
(a) Chromyl - Chloride test: Salt + few
KzCr,0, crystals + conc. H2SO4 and heat. Red vapours are obtained.
Pass the vapours through the test tube
which contains NaOH solution. The solution turns yellow.
Chloride is confirmed.
To this yellow solution, add dilute
CH,COOH and lead acetate solution. Yellow ppt. is formed
(b) Silver Nitrate test: Salt solution + White ppt. is formed
AgNO solution + dilute HNO, which is soluble in NHOH. Chloride is confirmed.
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Confirmation test for Bromide
OBSERVATION INFERENCE
EXPERIMENT
(a) Globule Test: Aqueous solution of salt + two An orange-red globule is Bromide is confirmed.
drops of CCl, + 1ml chlorine water and shake obtained
well.
(b)Silver Nitrate test: Salt solution + AgNO3 A pale yellow ppt. slightly soluble Bromide is confirmed.
solution + dilute HNO3 NH,OH is obtained.
Confirmation test for Nitrate
OBSERVATION INFERENCE
EXPERIMENT
Brown ring test: Strong solution of the substance + 2 or A brown ring is formed
3 drops of conc. H2SO4, and cool. Add freshly prepared at the junction of two Nitrate is confirmed.
FeSO, solution on the sides of the test tube. liquids.
THIRD GROUP OF ACID RADICALS
The basic radicals involved in this group are SO4 and PO4
EXPERIMENT OBSERVATION INFERENCE
Test for Sulphate: Aqueous solution of salt + dilute A white ppt. insoluble in dilute Suiphate (SO4) is
HCI + BaCl, solution. HC! is obtained confirmed.
Ammonium - Molybdate Test: 2ml of soda extract A canary yellow precipitate is Phosphate (PO)is
dilute HNO, + Ammonium Molybdate solution. obtained. confirmed.
Soda extract to be prepared if the givensalt is partially soluble in water.
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ANALYSIS OF BASIC RADICALS OR CATIONS
This is classified into 6 groups. They are mentioned as below:
GROUP RADICALS GROUP REAGENTS
Pb? Ag Dilute Hydrochloric acid(HCI)
II
Pb² ,Hg ,cu ,Cd* Dilute HCI + HS gas.
III AI ,Fe?, Fe NH,CI(s) + NH,OH
IV Zn ,Mn? ,co? ,Ni?" NHCI(s) + NH,OH + H2S gas
Ca ,Sp2· ,Ba2 NH,CI(s) + NH4OH + (NH4) 2COs
VI Mg, NH4 -Nil
Preparation of Oriqinal solution: A suitable solvent found for the sait as given in the preliminary test. A
few drops are used as solution.
Test for NH Radicals: This test is carried out before starting the analysis for the basic radicals.
EXPERIMENT OBSERVATION INFERENCE
(a) Salt + NaOH solution and heat it.
Colourless gas with a pungent smell is
Expose a glass rod dipped in conc. obtained. NH4 may be present in the
Dense white fumes and moist red salt
HCl to the gas and moist red litmus
iitmus paper turns blue
paper.
(b) Original solution + Nesseler's Brown solution or ppt. is obtained
reagent. NH4 is confirmed.
FIRST GROUP OF BASIC RADICALS
The basic radicals of this group are Pb &Ag' .The group reagent is dilute HCl.
EXPERIMENT OBSERVATION INFERENCE
(1) Original solution + Dilute HCI White ppt. formed. May be Pb & Ag
Filter and add water to ppt. (a) ppt. dissolves in hot water. May be PL2"
and het (b) ppt. is insoluble in water. May be Ag*
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(2) Original solution + Potassium
(a) A yellow ppt. is formed Pb is confirmed.
Chromate solution.
(b) Abrick red ppt. is formed. Ag' is confirmed.
(3) Original solution + KCl sol. A yellow ppt. soluble in hot
water, on cooling reappears as
golden yellow spangles. Pb is confirmed.
ppt. obtained + water and The yellow ppt. is insoluble
heat it. in hot water.
SECOND GROUP OF BASIC RADICALS
The basic radicals of this group are Pb,Hg, Cu and Cd'.The group reagent is Dilute HCl + H;S gas.
EXPERIMENT OBSERVATION INFERENCE
Original solution Dilute HCI + (a)A Black ppt. is observed. May be Pb Hg & Cu?
H2S gas. ñay be Ca?
(b)A yellow ppt. is observed.
The identification of Pb, Hg, Cu and Ca' are as follows:
EXPERIMENT OBSERVATION INFERENCE
(a) Original solution + Potassium
Chromate. A yellow ppt. is observed. Pb is confirme.
Abluish white ppt. soluble in excess
(b)Original solution + NH,OH of NH OH is observed which gives May be Cue
rise to a deep blue solution.
(c) Original solution dil. acetic A chocolate red ppt. is observed.
acid * potassium Ferro cyanide sol. Cu is confirmed.
(d) Dissolve the black ppt. in aqua
regia + 1ml of distilled water, Awhite ppt. is observed which turns
grey. Hg is confirmed.
heat &add 2 drops of SnClz
(e) Original solution + dilute acetic
acid + HzS gas. Ayellow ppt. is formed. Cd' is confirmed.
Aqua regia is mixture of 3 drops of HCI + 1 drop of HNO3
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THIRD GROUP OF BASIC RADICALS
The basic radicals of this group are Al, Fe* and [Link] group reagent is NH Cl + NH,OH
EXPERIMENT OBSERVATION INFERENCE
(1) Original solution + (a) A white gelatinous ppt. is obtained. May be A|3
NH,CI(s) + NH4OH in (b) A dirty green ppt. is obtained May be Fe2
excesSS
(c) A reddish brown ppt. is obtained May be Fe
(a) White gelatinous ppt. soluble in excess of NaOH The basic radical is A3
is obtained which gives a colourless sol.
(2) Original solution +
(b) Dirty green ppt. insoluble in excess of NaOH The basic radical is Fe2
NaOH solution
(c) Reddish brown ppt. insoluble in excess of NaOH The basic radical is Fe
(3) Clear solution of
2(a) + solid NH4Cl and The white gelatinous ppt. reappears. AI` is confirmed.
heat
(4) Origiral solution +
acidified KMnO4 solution (a) The pink colour of KMnO4 is not discharged. Fe is confirmed.
which is added drop wise.
FOURTH GROUP OF BASIC RADICALS
The basic radicals of this group are Zn*, Mn, Co* & Ni".The group reagent is NHCI* NH_OH
And HeSg).
EXPERIMENT OBSERVATION INFERENCE
(a) a white ppt. is obtained May be Zn, Mn or Co?:
(1)Original solution + NH,CI(s)
+ NH OH in excess + H2s(9) (b) Buff or pale pink or flash coloured ppt. May be Mn?
soluble in dilute HCI is obtained.
(a) The white ppt. is soluble in excess of Zn is confirmed
(2) Original solution + NaOH NaOH giving a colourless solution.
solution+, (b) The white ppt. insoluble in excess of Mn is confirmed
NaOH but turns brown.
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