2011

QUALITATIVE ANALYSIS

BY Mr. OJOK OYITE DAVID. ADILANG SECONDARY SCHOOL 11/7/2011

QUALITATIVE ANALYSIS
1. APPEARANCE OF THE SUBSTANCE.
Always note the physical properties of the substance e.g. appearance, colour, smell, & solubility in water. If the compound or its solution is colourless, it s most probable that the ions are those of group one, two, three & four e.g. Na+, K+, Ca2+ etc. If it s coloured, then a transition metal is deduced as follows; OBSERVATION Yellow colour. Green colour. Smell of ammonia. DEDUCTION Ferric salts, i.e. Fe3+ Ferrous or copper salts, Fe2+ or Cu2+ Ammonium salts, NH4+

Then if the substance is black, it s likely to be an oxide or sulphide of a transition metal or group (iv) metals.

2. SOLUBILITY IN WATER.
When a small solid sample is added to water in a test tube, the following should be noticed. If the sample does not dissolve in cold water warm a bit then refer to the table below. ANION CO32+ NO3+ SO42+ PO43+ SOLUBLE Na+, K+, NH4+. All The rest Na+, K+, NH4+ MODERATELY SOLUBLE --------------------------Ag+, Ca2+ -------------INSOLUBLE The rest ----------Pb2+, Ba2+, Ca2+ The rest.

3. ACTION OF HEAT ON SOLID SAMPLE.

Heat a small quantity of the solid gently & then very strongly in a dry glass tube until no further change occurs. Identify the gas(es) given off by their colour, smell, action on moist litmus & on burning/glowing splint. The deduction about the unknown may be obtained from the table below.

OBSERVATION Water vapor (steam). CO2 O2 NH3 SO2 NO2 Residue: (a) yellow hot, white cold (b) White hot, yellowish cold. (c) Black. (d) Sublimes.

DEDUCTION. Hydrated salts or hydrogen carbonate. CO32- or HCO3NO3- or MnO4NH4+ salt. SO42NO3- of heavy metals (not group one) ZnO. PbO. CuO. NH4+ salts.

4. RECORGNITION OF GASES.
Gases are usually given off when either a substance is heated or when a reagent reacts with a substance. Four easy tests serve to identify most of these. a) b) c) d) GAS Cl2 HCl NO2 SO2 NH3 CO2 H2 The colour of the gas. The smell of the gas. The action of the gas on the lighted splint. The action of the gas on a moist litmus paper. COLOUR SMELL Greenish Irritating Colourless, fumes in Irritating moist air Reddish brown Irritating Colourless Chocking Colourless Chocking Colourless None Colourless None ACTION ON SPLINT Extinguishes Extinguishes Splint burns Extinguishes Extinguishes Extinguishes Burns with blue flame, Pop sound with burning splint. ACTION ON LITMUS Red then bleached Red Red Red then bleached Blue Faint red. None.

CONFIRMATORY TEST FOR SOME GASES

 HCl; hold a moist stopper of a conc. ammonia bottle in the gas, dense white smoke of ammonium chloride is formed.  SO2; decolorizes dilute KMnO4 solution.  CO2; white ppt. with lime water.  NH3; turns moist red litmus blue.

5. TEST FOR THE METALIC IONS (CATIONS)

a) USING NaOH SOLUTION.
To the suspected solution is added NaOH drop wise until in excess, if no precipitate is formed, warm gently & test for ammonia. OBSERVATION DEDUCTION White ppt. formed with few drops of NaOH but soluble on adding excess Zn2+, Al3+ & NaOH. Pb2+ White ppt. formed with few drops & insoluble in excess NaOH. Mg2+, Ca2+. Green ppt. formed with few drops, insoluble in excess NaOH & turns brown on Fe2+ standing. White ppt. formed with few drops, insoluble in excess & quickly turns brown Al3+ black. Brown ppt. formed with few drops which is insoluble in excess NaOH. Fe3+ Blue ppt. formed with few drops & insoluble in excess NaOH. No ppt. with few drops & excess NaOH but evolves NH3 gas on warming. Cu2+ NH4+

b) USING AMMONIA SOLUTION, NH4OH.

To the solution is added ammonia solution drop wise till in excess. OBSERVATION DEDUCTION White ppt. forms with few drops & soluble in excess NH4OH to give a colourless Zn2+ , Ag+ solution. White ppt. forms with few drops & slightly soluble in excess ammonia. Al3+ White ppt. forms with few drops & insoluble in excess ammonia. Pb2+

A green ppt. forms with few drops, insoluble in excess & turns brown on Fe2+ standing. A brown ppt. forms with few drops & insoluble in excess ammonia. Fe3+ Blue ppt. forms with few drops soluble in excess ammonia to give a deep blue Cu2+ solution. No ppt. formed even with excess alkali Mg2+, Ca2+

NOTE;  Zn2+, Al3+ & Pb2+ dissolves in excess alkalis because of the formation of complex ions as follows.  Zn2+(aq) +2OH-(aq) -------------------------- Zn(OH)2(s), then
(White ppt.)

Zn(OH)2(s) + OH-(aq) ----------------------- Zn(OH)42-(aq)

(Excess) (Zincate ion)

 Al3+(aq) + OH-(aq) ---------------------------- Al(OH)3(s), then

(White ppt)

Al(OH)3(s) + OH-(aq) ------------------------- Al(OH)4-(aq)

(Excess) (Alluminate ion)

 Pb2+(aq) + OH-(aq) ---------------------------- Pb(OH)2(s), then (White ppt) . Pb(OH)2(s) + OH (aq) ------------------------ Pb(OH)42+(aq)
(Excess) (Plumbate ion)

 The presence of lead can be confirmed by carrying out the following tests; to the portion of the original solution of Pb2+ is added.  Dilute HCl, a white ppt. of PbCl2 is formed. Pb2+(aq) + 2Cl-(aq) ---------------------- 2PbCl2(s) (White ppt.)  Dilute H2SO4, a white ppt. is formed. Pb2+(aq) + SO42-(aq) -------------------- PbSO4(s) (White ppt.)  Potassium chromate solution, a yellow ppt. of lead chromate is formed Pb2+(aq) + CrO2-(aq) -------------------- PbCrO4(s) (yellow ppt.)

6. TEST FOR ANIONS;

ANION TEST CO32- (i) Heat the solid strongly. (ii) To the solid is added dilute HCl. NO3(i) Strongly heat the solid. (ii) Brown ring test; to the solution add freshly prepared solution of FeSO4, then carefully add conc. H2SO4 down the side of the test tube. (iii) Heat the solid mixed with copper turnings & conc. H2SO4. To the solution of sulphate is added, (i) Pb(NO3)2 solution & the mixture heated. OBSERVATION (i) CO2 gas evolves. (ii) CO2 gas evolves. (i) A brown fumes of NO2 forms. (ii) A brown ring forms at the interface. (iii) A brown fumes of NO2 forms.

SO42-

(i) A white ppt. of PbSO4 insoluble on heating. Pb2+(aq) + SO42-(aq) ------ PbSO4(s). (ii) BaCl2 solution in the presence of dilute HNO3 (ii) A white ppt. of BaSO4 forms Ba2+(aq) + SO42-(aq) ------ BaSO4 (iii) Ba(NO3)2 solution in the presence of dilute (iii) A white ppt. of BaSO4 is HNO3 formed Ba2+(aq) + SO42-(aq) ------ BaSO4(s) (iv) KI solution. (iv) A thick yellow ppt. of PbI2 is formed Pb2+(aq) + I-(aq) ------ PbI2(s) (i) To the solid chloride is added conc. H2SO4 (ii) To the solid chloride mixed with MnO2 is added conc. H2SO4 (iii) To the solution of chloride is added Pb(NO3)2 & the mixture heated. (i) Effervescence of HCl gas. (ii) A greenish-yellow Cl2 gas is given off. (iii) A white ppt. of PbCl2 is formed which dissolve on heating & reappears on cooling. Pb2+(aq) + 2Cl-(aq) ------ PbCl2(s) (iv) To the solution of chloride is added a few (iv) A white ppt. of AgCl is drops of AgNO3 solution in the presence of formed. Ag+(aq) + Cl-(aq) ------- AgCl(s) dilute HNO3

Cl-

E.g. 1; a substance Z contains two cations & a common anion, carry out the following tests to identify the cations & anion presence in substance Z. TEST 1. Place Two spatula ends full of Z in a boiling tube & add about 5cm3 of water. Shake the mixture vigorously & filter. Keep Both the residue & filtrate. 2. Divide the filtrate into 4 portions. (a). To the first portion add aqueous NaOH drop wise until in excess (b). To the second portion add NH4OH drops wise until in excess. OBSERVATION Filtrate is a solution. DEDUCTION colourless Probably Zn2+, Al3+, Pb2+ or NH4+ salt present. or Pb2+

Residue is a dirty white Zn2+, Al3+, present. solid

A white ppt. is formed which dissolve in excess NaOH to give a colourless solution. A white ppt. is formed which slightly dissolve in excess NH4OH. (c). To the third portion add 3 No observable change took drops of KI solution. place, (no yellow ppt.). (d). To the forth portion add 3 A white ppt. is formed. drops of dil. HNO3 followed by 3 drops of Ba(NO3)2 solution. (3). Wash the residue is with water & then dissolved in dilute HNO3. The residue dissolves to Then divide the resultant solution give a colourless solution. into 3 parts. (a). To the first part add NaOH A white ppt. is formed drops wise until in excess. soluble in excess to form a colourless solution. (b). To the second portion add A white ppt. insoluble in aqueous NH4OH drops wise until in excess is formed. excess (c). To the third portion add 3 A yellow ppt. is formed. drops of KI solution.

Probably Zn2+, Al3+ & Pb2+ present. Zn2+ absent, Al3+ & Pb2+ suspected. Pb2+ absent. Hence Al3+ presence confirmed. presence is SO42+ confirmed.

Probably Zn2+ or Pb2+. Present. Probably Zn2+ or Pb2+ presence. Pb2+ most likely present

Pb2+ confirmed.

Therefore from the observations & deductions made above, Z contains cations Al3+ & Pb2+ & the anion SO42Z is therefore a mixture of Al2(SO4)3 & PbSO4 salts.

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