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ANALYTICAL CHEMISTRY LAB MANUAL 1-Qualitative Analysis

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ANALYTICAL CHEMISTRY LAB MANUAL 1-Qualitative Analysis ANALYTICAL LABORATORY MANUAL I QUALITATIVE ANALYSIS OF ANIONS –CATIONS ANKARA UNIVERSITY, FACULTY OF PHARMACY DEPARTMENT OF ANALYTICAL CHEMISTRY TABLE OF CONTENTS 1) QUALITATIVE ANALYSIS OF ANIONS................................................................................... 2 1.1. Identification of chloride ion (퐂퐥 −) ............................................................................ 2 1.2. Identification of sulfate ion (퐒퐎ퟒퟐ −) ........................................................................ 2 1.3. Identification of nitrate ion (푵푶ퟑ −) .......................................................................... 3 1.4. Identification of carbonate ion (푪푶ퟑퟐ −) .................................................................. 3 1.4.1. By adding acid .......................................................................................................... 3 1.5. Identification of ortophosphate ion (퐇퐏퐎ퟒퟐ −) ........................................................ 4 2+ + + + 2) GROUP V CATIONS (Mg , Na , K , NH4 ) ........................................................................... 6 + 2.1. Ammonium (NH4 ) ...................................................................................................... 7 2.2. Magnesium (Mg2+) ....................................................................................................... 7 2.3. Sodium (Na+ ) ............................................................................................................... 7 2.4. Potassium (K+) .............................................................................................................. 7 3) SEPARATION OF GROUP IV AND GROUP V CATIONS ......................................................... 8 4) GROUP IV CATIONS (Ba2+, Ca2+, Sr2+) .................................................................................. 9 5) GROUP III CATIONS (Fe3+, Al3+, Cr3+, Ni2+, Co2+, Mn2+, Zn2+) ............................................. 10 6) GROUP II CATIONS (As3+, Sb3+, Sn2+, Hg2+, Cu2+, Cd2+, Pb2+, Bi3+) ...................................... 12 7) GROUP I CATIONS (Ag+, 퐇퐠ퟐퟐ + ve Pb2+) ........................................................................ 15 7.1. Ag+ .............................................................................................................................. 15 7.2. Pb2+ ............................................................................................................................ 16 2+ 7.3. Hg2 ........................................................................................................................... 17 1 1 drop of liquid is supposed to be 0.05 mL so that 20 drops of liquid is 1 mL. 1) QUALITATIVE ANALYSIS OF ANIONS − 2− − 2− 3− Cl , SO4 , NO3 , CO3 and PO4 each have specific identification reactions so they can be identified in the mixtures containing these anions. That is why there is no need for a separation step for their identification tests. In qualitative analysis of anions, the reactants should be added drop by drop and directly into the solution in the test tube (not on the wall of the tube). 1.1. Identification of chloride ion (퐂퐥−) 1.1.1. With silver nitrate (AgNO3) − 2− 2− 3− Preliminary info: In neutral solutions, Cl , SO4 , CO3 and PO4 all reacts with AgNO3 to precipitate as silver salts. When HNO3 is added to this solution, all these silver salts except for − silver chloride (AgCl) dissolves. So for identification test of Cl , HNO3 should be added to the solution to prevent Ag2CO3, Ag3PO4, Ag2SO4 salts from precipitation. Procedure: To 0.5 mL of sample in a test tube, add 7 drops of HNO3 and 1 drop of AgNO3. The white precipitate is AgCl and the formation of this precipitate indicates there is Cl− ion in the sample. − − Cl + AgNO3 → AgCl(s) + NO3 In order to confirm that this precipitate is AgCl, 20 drops of NH4OH is added to the same test tube. The white precipitate dissolves because AgCl salt forms a complex with NH3. + − AgCl(s) + 2NH3 → [Ag(NH3)2] + Cl Add 15 drops of HNO3 into the solvated complex and a white precipitate is re-constituted. + Because with the addition of HNO3, the silver diammine complex ( [Ag(NH3)2] ) decomposes and re-precipitates as AgCl. + − + − [Ag(NH3)2] + Cl + 2HNO3 → 2NH4 + 2NO3 + AgCl(s) ퟐ− 1.2. Identification of sulfate ion (퐒퐎ퟒ ) 1.2.1. With barium chloride (BaCl2) 2− 2− 3− Preliminary info: In neutral solutions, SO4 , CO3 and PO4 reacts with BaCl2 to precipitate as barium salts. When a mineral acid is added to this solution, these barium salts except for 2− barium sulfate (BaSO4) dissolve. So for identification test of SO4 , a mineral acid should be added to the solution to prevent BaCO3, Ba3(PO4)2 salts from precipitation. 2 Procedure: To 0.5 mL of sample in a test tube, add 7 drops of HNO3 and 1 drop of BaCl2, respectively. The 2− white precipitate is BaSO4 and the formation of this precipitate indicates the presence of SO4 ion in the sample. 2− − SO4 + BaCl2 → BaSO4 (s) + 2 Cl − 1.3. Identification of nitrate ion (푵푶ퟑ ) Preliminary info: Diphenylamine, which is a colorless reactant, oxidizes to blue-violet colored − diphenyl benzidine violet in presence of an oxidant such as NO3 . This reaction occurs in acidic medium. Procedure: To 0.5 mL of sample in watch glass, add 1 drop of diphenylamine solution. In the contact surface of two liquids, blue color appears. The blue color may disaappear after a while. (The diphenylamine solution given in the laboratory has been prepared with H2 SO4 by the laboratory personnel. So there is no need to add acid into the watch glass.) ퟐ− 1.4. Identification of carbonate ion (푪푶ퟑ ) 1.4.1. By adding acid Procedure: To 2 mL of sample in a test tube, add 1 mL of acid (for example CH3COOH, HCl, HNO3) all at 2− once. The formation of gas bubbles indicate the presence of CO3 in sample and the releasing gas is CO2. The formation of gas bubbles can be accelerated by shaking the test tube. 2− − CO3 + 2CH3COOH → 2CH3COO + H2O + CO2(g) 1.4.2. With BaCl2 2− This test does not prove the existence of CO3 . It will help you to understand why you need 2− to acidify the medium when you perform SO4 identification test with BaCl2. Procedure: To 1 mL of sample in a test tube, add 1 drop of BaCl2. The white precipitate might be barium carbonate (BaCO3). In order to confirm that it is BaCO3, add 7 drops of HNO3 and observe the dissolving precipitate which releases CO2. 2− − CO3 + BaCl2 → BaCO3(s) + 2 Cl + 2+ BaCO3(s) + 2H → Ba + H2O + CO2(g) 3 1.4.3. With AgNO3 2− This test does not prove the existence of CO3 . It will help you to understand why you need − to acidify the medium when you perform Cl identification test with AgNO3. Procedure: To 1 mL of sample in a test tube, add 1 drop of AgNO3. The white precipitate might be silver carbonate (Ag2CO3). In order to confirm that it is Ag2CO3, add 7 drops of HNO3 and observe the dissolving precipitate which releases CO2. 2− − CO3 + 2AgNO3 → Ag2CO3(s) + 2NO3 + + Ag2CO3(s) + 2H → 2Ag + H2O + CO2(g) ퟐ− 1.5. Identification of ortophosphate ion (퐇퐏퐎ퟒ ) 1.5.1. With ammonium molybdate ((NH4)2MoO4) Procedure: To 0.5 mL of sample in a test tube, add 5 drops of HNO3 and 5 drops of (NH4)2MoO4. Heat to 40°C in water bath for 5 minutes. The yellow precipitate is ammonium phosphomolybdate 2− ((NH4)3(MoO3)12PO4) and the formation of this precipitate indicates the presence of HPO4 ion in the sample. 2− HPO4 + 12(NH4)2MoO4 + 23HNO3 + − → (NH4)3(MoO3)12PO4(s) + 21NH4 + 23NO3 + 12H2O 1.5.2. With BaCl2 2− This test does not prove the existence of HPO4 . It will help you to understand why you need 2− to acidify the medium when you perform SO4 identification test with BaCl2. Procedure: To 1 mL of sample in a test tube, add 1 drop of BaCl2. The white precipitate may be barium hydrogen phosphate (BaHPO4) and the formation of this precipitate may indicate the presence 2− of HPO4 . When 7 drops of HNO3 is added into this tube, the white precipitate disappears because BaHPO4 is dissolved in acidic medium. 2− − HPO4 + BaCl2 → BaHPO4(s) + 2 Cl + 2+ BaHPO4(s) + 2H → Ba + H3PO4 4 1.5.3. With AgNO3 2− This test does not prove the existence of HPO4 . It will help you to understand why you need − to acidify the medium when you perform Cl identification test with AgNO3. Procedure: To 0.5 mL of sample in a test tube, add 1 drop of AgNO3. The yellow precipitate is silver 2− phosphate (Ag3PO4) and the formation of this precipitate indicates the presence of HPO4 . When 7 drops of HNO3 is added into this tube, the yellow precipitate disappears because Ag3PO4 is dissolved in acidic medium. 2− − HPO4 + 3AgNO3 → Ag3PO4(s) + 2NO3 + HNO3 + + Ag3PO4(s) + 3H → 3Ag + H3PO4 5 2+ + + + 2) GROUP V CATIONS (Mg , Na , K , NH4 ) There is not a common precipitating agent for the group V cations. Sodium and potassium are alkali metals. + + NH4 is also classified in the group V because the compounds containing NH4 have similar properties with alkali metals. Magnesium is an alkaline earth metal, but it does not precipitate with the common precipitating agent of group IV. Therefore, it is also classified in the group V. The salts of colourless anions and group V cations are colourless and have ionic bonds. Therefore, most of them are soluble in water and this is why group V cations don’t have a common precipitating agent. Important points: If acidity or alkalinity of a solution is stated, it must be controlled by litmus paper. Litmus paper must not be contacted with the tube. Care should be taken that the solution which is splashed from the tube can also change the color of the litmus
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