Analysis of a Solution Containing One Inorganic Compound A. Detection of the Basic Constituent 1.

Add 1 drop of 2M HCl A precipitate is formed - Ag group. Add few drops more of HCl till precipitation is complete, centrifuge. Pipet > dilute with water > Boil > Dissolve > Add K2CrO4 > Yellow ppt > LEAD Insoluble > Decant > Add NH4OH > Dissolve > SILVER Ppt blackens > MERCUROUS No ppt > #2 2. Add 10 drops of 10% thioacetamide and boil in a water bath for 10 mins. Ppt is produced - H2S group. Add 1M NaOH and Na2S, warm. Ppt is insoluble - Cu subgroup Yellow ppt - Cd2+. Add K4Fe(CN)6 > White ppt > CADMIUM Black or brown ppt - Bi2+, Pb2+, Cu2+ Add K2CrO4 > Yellow ppt > LEAD Add NaOH & Na2SnO2 > blackening of ppt > BISMUTH Blue solution > Add K4Fe(CN)6 > reddish brown ppt > COPPER Ppt is soluble - Sn subgroup Black ppt - Hg2+. Add Na2SnO2 > White ppt turning gray > MERCURIC Orange ppt - Sb3+ > Drop metallic Sn > Black ppt, insoluble in NaOBR > ANTIMONY Yellow ppt - As+3, Sn+2/+4 Add HCl and Mg ribbon, boil (2-3 mins), filter, add HgCl2 to the filtrate > white/gray ppt > TIN Add 1mL of NH4OH & H2O2, warm on a water bath (2-3 mins), evaporate, dissolve the residue in 1mL of water & conc. HNO3, add 2 mL of (NH4)2MoO4 > warm > yellow ppt > ARSENIC No ppt > #3 3. Add 10 drops of 6M NH4Cl & 10 drops of 12M NH4OH. Ppt is formed - trivalent cations of (NH4)2S group White ppt - Al+3 > Add 10 drops of NH4CH3COO & aluminon rgt, mix and make alkaline w/ 6M NH4OH > Red ppt > ALUMINUM Grayish green - Cr+3 > Add 1M NaOH, H2O2 till green, boil (5 mins), replacing the water which evaporates, cool, acidify w/ 6M CH3COOH, add Pb(CH3COO)2 > Yellow ppt > CHROMIUM Reddish brown - Fe3+ > Add K4Fe(CN)6 > Blue ppt > FERRIC No ppt formed > add 10% thioacetamide > ppt formed - Zn+2, Mn+2, Co+2, Ni+2 White ppt > ZINC

Flesh-colored/salmon ppt - Mn+2 > Add 6M HNO3 & NaBiO3 > Violet colorization > MANGANESE Black ppt - Co+2, Ni+2 Pink sol'n - Co+2 > Add 1mL of KNO2, acidify w/ 6M CH3COOH > Yellow ppt > COBALT Green sol'n - Ni+2 > dimethylglyoxime(C4H8N2O2) rgt, make w/ 6M NH4OH > Red ppt > NICKEL Still no ppt > #4 4. Add Na2CO3. White ppt - Alkaline earth group Add 2-3 drops of 6M CH3COOH & 5 drops of K2CrO4 > Yellow ppt > BARIUM No ppt, make alkaline w/ 6M NH4OH & 1 drop of C2H5OH > Yellow ppt - Sr+2 > flame test > carmine-red flame colorization > STRONTIUM Add 1mL of water, 5 drops of K2C2O4 & 2-3 drops of 6M CH3COOH > White ppt > CALCIUM Add 10 drops of 6M NH4Cl, 10 drops of Na2HPO4, make alkaline w/ 6M NH4OH > white crystalline ppt > MAGNESIUM No ppt > #5 5. Still no ppt - Alkali group Add 1mL of 1M NaOH, heat > evolution of NH3 - Ammonium salt > Add Nessler's rgt > Orange ppt > AMMONIUM Add 1mL of Na3Co(NO2)6 > Yellow ppt > POTASSIUM Add 1mL of K2H2Sb2O7 > White crystalline ppt > SODIUM Flame test > Carmine red flame > LITHIUM B. Detection of the Acid Constituent 6. Determine the group which the acid constituent belongs Add 1-2 drops of 1M AgNO3 > ppt formed > add 10 drops of 6M HNO3 > doesn't dissolve > boil for a minute Add 1-2 drops of 1M BaCl2 > ppt formed > add 10 drops of 6M HNO3 > doesn't dissolve > boil for a minute 7. Produced a ppt with AgNO3 insoluble in 6M HNO3, no ppt w/ BaCl2 - Group 1 Orange ppt - Fe(CN)6-3 > Add 1-2 drops of FeSO4 > Blue ppt > FERRICYANIDE Yellow ppt - Br- & I Add 1mL of CHCl3 (or CH2Cl2), 10 drops of 6M HNO3 & KMnO4 a drop at a time till the aq sol'n has acquired a pink coloration, shake. Reddish brown coloration (or dichloromethane) layer > BROMIDE Violet layer > IODIDE White ppt - Cl-, CN-, Fe(CN)6-4, SCN-, ClO- (through elimination process) Add 1-2 drops of FeCl3 > blue coloration > FERROCYANIDE

Blood red colorization > THIOCYANATE Add 6M CH3COOH (a drop at a time till acidic), add 1mL of Pb(CH3COO)2, heat, stand for 5 mins > Brown ppt > HYPOCHLORITE Add 1M NaOH till alkaline, add a few drops of FeSO4, 1 drop of FeCl3, heat to boiling, cool & acidify w/ HCl > Blue ppt > CYANIDE *if all of the above tests are negative*, add Hg2(NO3)2 in (Add 1M NaOH till alkaline, add a few drops of FeSO4, 1 drop of FeCl3, heat to boiling, cool & acidify w/ HCl) > White ppt > CHLORIDE 8. Produced a precipitate w/ AgNO3 soluble w/ HNO3, BaCl2 also produced a ppt - Group 2 Black ppt - S-2. Acidify w/ 6M HCl > evolution of H2S gas > blackens Pb(CH3COO)2 paper > SULFIDE Ppt is white rapidly changing to brown or black - H2PO2- > Add 1mL of 6M NaOH, boil for 1 min., acidify strongly w/ HNO3 & (NH4)2MoO4, heat > Yellow > HYPOPHOSPHITE White ppt - NO2- & CH3COO Add 3M H2SO4 > evolution of brown gas > NITRITE Add 1mL of conc. H2SO4, add 5 drops of C2H5OH, warm > evolution of gas with a fruity odor > ACETATE 9. Produced a ppt w/ AgNO3 soluble w/ HNO3, BaCl2 also produced a ppt soluble w/ HNO3 Group 3 Acidify w/ HCl > SO2 gas evolved, solution remains clear - SO3-2 > add 3-5 drops of BaCl2 & few drops of HCl to re-dissolve the ppt, filter (if not completely dissolved), add 1 mL of bromine water & boil for 1-2 mins > white ppt > SULFITE Effervescence is produced but the gas evolved is odorless > expose a lime water to the issuing gas > white ppt in the lime water > CARBONATE (in an evap. dish) Add 1mL if conc. H2SO4 & 3mL of CH3OH, stir, set on fire > Green flame coloration > BORATE Add CaCl2 till precipitation is complete, then acidify w/ 6M CH3COOH > White ppt insoluble in CH3COOH > OXALATE Add CaCl2 till precipitation is complete, then acidify w/ 6M CH3COOH > White ppt soluble in CH3COOH - C4H4O62- > Add CH3COOH & acidify w/ CH3COOH > white crystalline ppt > TARTRATE CaCl2 has produced no ppt w/o adding 6M CH3COOH > boil for 1-2 mins. > white ppt > (C6H5O73-) CITRATE 10. Produced a colored ppt w/ AgNO3 soluble in HNO3 & BaCl2 has produced a white ppt soluble in HNO3 - Group 4 Reddish brown ppt w/ AgNO3 - AsO4-3 & CrO4-2 Add drops of conc. HCl, 5 drops of KI & 2-3 drops of starch sol'n > blue coloration > ARSENATE Add a few drops of Pb(CH3COO)2 > yellow ppt > CHROMATE

Yellow ppt w/ AgNO3 - PO4-3 & AsO3-3 Add 10 drops of NH4Cl, 1mL of magnesia mixture, and an excess of NH4OH > stand for 10 mins. > white crystalline ppt > PHOSPHATE Acidify w/ HCl and pass H2S > Yellow ppt > ARSENITE White ppt readily turning black w/ AgNO3 - S2O3-2 > add few drops of iodine sol'n > immediate discoloration of the iodine solution > THIOSULFATE 11. No ppt produced w/ AgNO3 and BaCl2 - Group 5 Add 1mL of conc. H2SO4 & copper wire > warm > evolution of brown > (NO3-) NITRATE Add 2-3 drops of KNO2, acidify w/ HNO3 > White ppt > (ClO3-) CHLORATE 12. No ppt w/ AgNO3, BaCl2 produced a white ppt insoluble in HNO3 - Group 6 Add few drops of Pb(CH3COO)2 & 1-2mL of NH4CH3COO sol'n > warm > white ppt soluble in NH4CH3COO > (SO4-2) SULFATE Add several drops of CaCl2 > white slimy ppt difficulty soluble in HCl and HNO3 but soluble in CH3COOH > FLUORIDE