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Experiment 5

• REACTION AND ANALYSIS


• 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