SEMI MICRO QUALITATIVE ANALYSIS OF SIMPLE INORGANIC SALT _______________________________________________________________

CATIONS: Pb2+ ,Hg2+ ,Cu2+ ,Cd2+ , Ag+ , Fe2+ , Fe3+ , Al3+ , Zn2+ , Mn2+ , Co2+ , Sr2+ , Ba2+ , Mg2+ , NH4+ ANIONS: CO32- , S2- , SO32- , SO42- , NO2- , NO3- , Cl- , Br2- , PO43- , CH3COO-

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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)

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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(CO32-), Sulphide(S2-), Sulphite(SO32-), Thiosulphate(S2O32-) and nitrate(NO2-). The group reagent is dilute hydrochloric acid. EXPERIMENT Salt + dil. HCl OBSERVATION Effervescence or evolution of gases (a) Colourless, odourless gas turns lime water milky (b) Colourless with rotten eggs smell and turns lead acetate paper black. (c) Colourless gas with suffocating smell. Heat and pass the gas through acidified K2Cr2O7 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 K2Cr2O7 solution. The solution turns dark blackish green. (e) Colourless gas followed by brown gas and it turns starch iodide paper blue. (f) Colourless gas with the smell of vinegar. INFERENCE 1st group of acid radicals is present. The acid radical may be CO32- or HCO3Sulphide(S2-) is confirmed.

SO32- is confirmed.

S2O32- is confirmed.

NO2- is confirmed. The acid radical may be CH3COO-

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Tests to distinguish between CO32- and HCO3EXPERIMENT Salt + water, boil and pass the gas through lime water OBSERVATION (a) Lime water does not turn milky. (b) Lime water turns milky. Confirmation test for Acetate EXPERIMENT Salt solution + Neutral FeCl3 sol. OBSERVATION Appearance of blood red colour. INFERENCE Acetate is confirmed INFERENCE CO32- is confirmed. HCO3- is confirmed.

The acid radicals involved in this group are Cl-, Br- and NO3- . The group reagent is concentrated sulphuric acid (H2SO4). EXPERIMENT OBSERVATION Effervescence with colourless or coloured gases (a) Colourless gas with a pungent smell and gives dense white fumes when a glass rod dipped in ammonium hydroxide (NH4OH) is exposed. (b) Brown gas and the solution is not blue. (c) Light brown gas and brown gas with pieces of copper turnings and the solution turns blue in the test tube. Confirmation test for Chloride EXPERIMENT (a) Chromyl Chloride test: Salt + few K2Cr2O7 crystals + conc. H2SO4 and heat Pass the vapours through the test tube which contains NaOH solution. To this yellow solution, add dilute CH3COOH and lead acetate solution. OBSERVATION Red vapours are obtained. The solution turns yellow. Yellow ppt. is formed Chloride is confirmed. INFERENCE INFERENCE 2nd group Acid radical is present The Acid radical may be Cl-

SECOND GROUP OF ACID RADICALS

Salt + Concentrated H2SO4 and heat if necessary.

The acid radical may be BrThe Acid radical may be NO3-

(b) Silver Nitrate test: Salt solution + AgNO3 solution + dilute HNO3

White ppt. is formed which is soluble in NH4OH.

Chloride is confirmed.

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Confirmation test for Bromide

EXPERIMENT
(a) Globule Test: Aqueous solution of salt + two drops of CCl4 + 1ml chlorine water and shake well. (b)Silver Nitrate test: Salt solution + AgNO3 solution + dilute HNO3

OBSERVATION
An orange-red globule is obtained A pale yellow ppt. slightly soluble in NH4OH is obtained.

INFERENCE
Bromide is confirmed.

Bromide is confirmed.

Confirmation test for Nitrate

EXPERIMENT
Brown ring test: Strong solution of the substance + 2 or 3 drops of conc. H2SO4, and cool. Add freshly prepared FeSO4 solution on the sides of the test tube.

OBSERVATION
A brown ring is formed at the junction of two liquids.

INFERENCE
Nitrate is confirmed.

THIRD GROUP OF ACID RADICALS

The basic radicals involved in this group are SO42- and PO43- .

EXPERIMENT
Test for Sulphate: Aqueous solution of salt + dilute HCl + BaCl2 solution. Ammonium Molybdate Test: 2ml of soda extract 1 + dilute HNO3 + Ammonium Molybdate solution.

OBSERVATION
A white ppt. insoluble in dilute HCl is obtained A canary yellow precipitate is obtained.

INFERENCE
Sulphate (SO42-) is confirmed. Phosphate (PO43-) is confirmed.

Soda extract to be prepared if the given salt 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
I II III IV V VI Pb
2+

RADICALS
Pb2+ ,Ag+ ,Hg
2+

GROUP REAGENTS
Dilute Hydrochloric acid(HCl)
2+

,Cu

2+

,Cd ,Ni
+

Dilute HCl + H2S gas. NH4Cl(s) + NH4OH NH4Cl(s) + NH4OH + H2S gas NH4Cl(s) + NH4OH + (NH4) 2CO3 -Nil-

Al3+ ,Fe2+ , Fe3+ Zn

2+

,Mn Mg

2+

,Co

2+

2+

Ca2+ ,Sr2+ ,Ba2+

2+

, NH4

Preparation of Original solution: A suitable solvent is found for the salt as given in the preliminary test. A few drops are used as solution. Test for NH4+ Radicals: This test is carried out before starting the analysis for the basic radicals.

EXPERIMENT
(a) Salt + NaOH solution and heat it. Expose a glass rod dipped in conc. HCl to the gas and moist red litmus paper. (b) Original solution + Nesselers reagent.

OBSERVATION
Colourless gas with a pungent smell is obtained. Dense white fumes and moist red litmus paper turns blue Brown solution or ppt. is obtained

INFERENCE
NH4+ may be present in the salt

NH4+ is confirmed.

FIRST GROUP OF BASIC RADICALS

The basic radicals of this group are Pb2+ & Ag+ .The group reagent is dilute HCl.

EXPERIMENT
(1) Original solution + Dilute HCl Filter and add water to ppt. and heat

OBSERVATION White ppt. is formed. (a) ppt. dissolves in hot water. (b) ppt. is insoluble in water.

INFERENCE May be Pb2+ & Ag+ May be Pb2+ May be Ag+

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(2) Original solution + Potassium Chromate solution. (3) Original solution + KCl sol.

(a) A yellow ppt. is formed. (b) A brick red ppt. is formed. A yellow ppt. soluble in hot water, on cooling reappears as golden yellow spangles. The yellow ppt. is insoluble in hot water.

Pb2+ is confirmed. Ag+ is confirmed.

ppt. obtained + water and heat it.

Pb2+ is confirmed.

SECOND GROUP OF BASIC RADICALS

The basic radicals of this group are Pb2+, Hg2+, Cu2+ and Cd2+.The group reagent is Dilute HCl + H2S gas.

EXPERIMENT
Original solution + Dilute HCl + H2S gas.

OBSERVATION
(a)A Black ppt. is observed. (b)A yellow ppt. is observed.

INFERENCE
May be Pb2+ Hg2+ & Cu2+ May be Cd2+

The identification of Pb2+, Hg2+, Cu2+ and Cd2+ are as follows:

EXPERIMENT
(a) Original solution + Potassium Chromate. (b)Original solution + NH4OH (c) Original solution + dil. acetic acid + potassium Ferro cyanide sol. (d) Dissolve the black ppt. in aqua regia 2 + 1ml of distilled water, heat & add 2 drops of SnCl2 (e) Original solution + dilute acetic acid + H2S gas.

OBSERVATION
A yellow ppt. is observed. A bluish white ppt. soluble in excess of NH4OH is observed which gives rise to a deep blue solution. A chocolate red ppt. is observed. A white ppt. is observed which turns grey. A yellow ppt. is formed.

INFERENCE
Pb2+ is confirmed. May be Cu2+ Cu2+ is confirmed. Hg2+ is confirmed.

Cd2+ is confirmed.

Aqua regia is mixture of 3 drops of HCl + 1 drop of HNO3

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THIRD GROUP OF BASIC RADICALS

The basic radicals of this group are Al3+, Fe2+ and Fe3+ .The group reagent is NH4Cl + NH4OH

EXPERIMENT
(1) Original solution + NH4Cl(s) + NH4OH in excess

OBSERVATION
(a) A white gelatinous ppt. is obtained. (b) A dirty green ppt. is obtained (c) A reddish brown ppt. is obtained (a) White gelatinous ppt. soluble in excess of NaOH is obtained which gives a colourless sol.

INFERENCE
May be Al3+ May be Fe2+ May be Fe3+ The basic radical is Al3+ The basic radical is Fe2+ The basic radical is Fe3+ Al3+ is confirmed.

(2) Original solution + NaOH solution

(b) Dirty green ppt. insoluble in excess of NaOH (c) Reddish brown ppt. insoluble in excess of NaOH

(3) Clear solution of 2(a) + solid NH4Cl and heat (4) Original solution + acidified KMnO4 solution which is added drop wise.

The white gelatinous ppt. reappears.

(a) The pink colour of KMnO4 is not discharged.

Fe3+ is confirmed.

FOURTH GROUP OF BASIC RADICALS

The basic radicals of this group are Zn2+, Mn2+, Co2+ & Ni2+.The group reagent is NH4Cl + NH4OH And H2S(g). EXPERIMENT (1) Original solution + NH4Cl(s) + NH4OH in excess + H2S(g) OBSERVATION (a) a white ppt. is obtained (b) Buff or pale pink or flash coloured ppt. soluble in dilute HCl is obtained. (a) The white ppt. is soluble in excess of NaOH giving a colourless solution. (b) The white ppt. insoluble in excess of NaOH but turns brown. INFERENCE May be Zn2+, Mn2+ or Co2+ May be Mn2+ Zn2+ is confirmed Mn2+ is confirmed

(2) Original solution + NaOH solution+.

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(3) Dissolve the 1(a) in aqua regia, evaporate to Dryness, add 1ml of distilled water and divide the resultant product into two parts. Part (1) + 1 ml of amyl alcohol + 100 mg of solid NH4SCN and stir it. Part (2) + 5 drops of dimethyl glyaxime reagent + NH4OH. A Blue colour in the alcohol layer is obtained. A pink ppt. is obtained. Co2+ is confirmed

Ni2+ is confirmed.

FIFTH GROUP OF BASIC RADICALS

The basic radicals of this group are Ca2+, Sr2+ & Ba2+ .The group reagent is NH4Cl(s) + NH4OH and (NH4)2 CO3.

EXPERIMENT (1) Original solution + NH4Cl(s) + NH4OH in excess + (NH4)2 CO3 solution. (2) Dissolve the white ppt. obtained in small amounts of dilute acetic acid. Divide the solution in three parts. Part (1) + Potassium chromate solution. Part (2) + Calcium Sulphate Sol. and heat. Part (3) + Ammonium exalate solution. (3)Flame tests: Make a paste of the given salt with few drops of Conc. HCl in a watch glass. Heat a Pt. wire in non luminous flame till no colour is imparted to the flame. Dip the Pt. wire in the paste and hold it in the flame.

OBSERVATION (a) A white ppt. is obtained.

INFERENCE May be Ca2+, Sr2+ or Ba2+

A yellow ppt. is obtained. A thin white ppt. is obtained. A white ppt. is obtained. (a) Apple green coloured flame is obtained. (b) Crimson red coloured flame is obtained. (c) Brick red coloured flame is obtained,

May be Ba2+ . May be Sr2+ . May be Ca2+ . Ba2+ is confirmed. Sr2+ is confirmed. Ca2+ is confirmed.

SIXTH GROUP OF BASIC RADICALS

EXPERIMENT (1) Original solution + excess of NH4OH + Ammonium Hydrogen Phosphate. OBSERVATION A white ppt. is obtained. INFERENCE Mg2+ is confirmed.

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