• OF THE • HYDROGEN SULFIDE GROUP OBJECTIVES 1. Observe the colors of the products formed in the reactions. 2. Develop a systematic method that will identify the ions in an unknown solutions through the application of chemical tests. PROCEDURE • ANALYSIS OF GROUP IIA CATIONS
5-1. Evaporate almost to dryness 1mL of the unknown
solution. Add 1 drop of 12M HCl and 39 drops of water, 10 drops of 10% thioacetamide, and heat in a water bath. Saturate again with H2S to complete precipitation. Centrifuge, decant and discard the centrifugate. 5-2. Precipitate: PbS, HgS, CuS, Bi2S3, CdS, As2S3, Sb2S3, Sb2S5, SnS, SnS2
Note the color of the precipitate. Add 8 drops of
3M NaOH and saturate with H2S. Centrifuge and decant the centrifugate. 5-3. Precipitate contains Cu subgroup: CuS, CdS, PbS, Bi2S3 Refer to the analysis of the copper sub – group (IIA cations) 5-4. Centrifuge contains Sn sub – group: Na2HgS2,Na3SbS4 ,Na3AsS4, Na2SnS3 Refer to the analysis of Tin subgroup (IIB cations) B. ANALYSIS OF GROUP IIA CATIONS
5-3 Precipitate contains : CuS , Cds, PbS,
and Bi2S3 Dissolve in hot 3M HNO3. Centrifuge and decant. 5-3-1. Precipitate S Discard 5-3-2. Centrifuge contains: Pb2+, Bi3+, Cu2+, and Cd2+.
Transfer to a casserole. Add 3 drops conc. H2SO4.,
evaporate until dense white fumes(SO3) appear and only 2-3 drops of liquid remain . Cool and dilute with 1mL water. Stir and transfer to a centrifuge tube. Rinse casserole with 5 drops water and add washings to the solution. Centrifuge and decant. 5-3-3. Precipitate PbSO4 Dissolve in 10 drops of sat. NH4CH3COO and heat. Add 1 drop of conc. HAc and 2 drops 1M K2CrO4. Yellow precipitate confirms Pb2+. 3+ 2+ 2+. 5-3-4. Centrifugate contains: Bi ,Cu ,Cd Make the solution basic by addition of conc. NH3 and add an excess of 3 drops . Centrifuge. 5-3-5. Precipitate : Bi(OH)3 Add 10 drops or more of freshly prepared sodium stannite solution. Immediate blackening of the precipitate confirms Bi3+. 5-3-6 Centrifugate: Cu(NH ) 2+, Cd(NH ) 2+. 3 4 2+ 3 4 a. Deep blue solution confirms Cu .a portion acidified with HAc, and add K4Fe(CN)6. 2+ Reddish brown ppt. confirms Cu . b. A portion acidified with 2+. HAc saturate with H2S. Yellow ppt. confirms Cd C. ANALYSIS OF TIN SUB- GROUP (IIB) CATIONS 5-4. Centrifugate contains Sn sub group: Na2HgS2, Na3SbS4, Na3AsS4, Na2SnS3. Add 3M HCl until solution is barely acid. Heat. Centrifugate and discard centrifugate. Add 10 drops of conc. HCl . Heat for 1 min. and centrifuge. 5-4-1 Centrifugate : Sb3+ Sn2+ Divide into three equal portions: a. To the one portion add an equal volume of 3M HCl. Place a piece of Mg ribbon and any precipitate formed. Add 4 drops sat. HgCl2 to the clear soln. White to gray precipitate confirms presence of Sn2+. b. To the 2nd portion add equal volume of water and 3+. 3M H2C2O4. Pass H2S. Orange ppt. confirms Sb .
Add 1 drop of the centrifugate to the surface of a clean
silver coin. Place a small piece of tin on the coin. Black deposit insoluble in indicates Sb3+ NaOBr 5-4-2 Precipitate; As2S3, HgS Add 6M NaOH. Centrifuge and decant. 5-4-3. Precipitate; HgS Dissolve with aqua regia(1:3 parts conc nitric acid and conc hydrochloric acid) a. Take 5 drops and add to it 2 drops SnCl2. 2+ white ppt to black ppt. confirms Hg . b. Take another 5 drops and add 2 drops 6M HCl on copper coin. Let it stand, wash, wipe dry. A silver 2+ white deposit (amalgam)confirms Hg 3+. 5-4-4. Centrifugate : As Add 5 drops 0.5M AgNO 3. If precipitation occurs, discard residue. Add 15 drops of 2.5M NaCH3COO. Reddish 3+. brown ppt. confirms As