GROUP III Flowchart

GROUP III FeS(s), Fe2S3(s), NiS(s) 12 M HCl 16 M HNO3

Sulfur

Fe

2+ 3+ 2+ , Fe , Ni 6 M NH3 3% H2O2

Fe(OH)3(s) brown 6 M HCl 0.1 M KSCN

2+ Ni blue 6 M CH3COOH Na(CH3COO) 1% HDMG

2+ [Fe(SCN)] blood red

Ni(DMG)2(s) bright red

Cation Qualitative Analysis __________________________________________________________________

PART III: Cation Group III Separation of Cation Group III 40. To 4 mL of the solution saved from step 23, add 5 drops of 6 M HCl. 41. Add 1.5 mL of 6 M NH3. Stir. Using pH paper, check for pH = 9. If not, add 6 M NH3 dropwise, with stirring, until the resulting suspension has a pH = 9. 42. Add 15 drops of 1 M thioacetamide and heat the mixture in a hot water bath in the hood for 10 minutes. 43. Centrifuge and decant, saving both the supernatant and precipitate. Label and save the supernatant solution for the analysis of Group IV (step 62). Save the precipitate for Cation Group III analysis in the next step. Cation Group III Analysis Dissolution of Cation Group III 44. Add 1 mL of deionized water to the precipitate. _______________________________________________________________________
CAUTION The concentrated HCl and HNO3 used in step 45 is highly corrosive, and can cause severe damage to eyes, skin, and clothing. In case of skin contact, immediately wash the area with large amounts of water.

45. Add 10 drops of 12 M HCl and 5 drops of 16 M HNO3 and gently boil in the hood for 5 minutes or until a clear (not colorless) solution is formed. 46. Add 1 mL of deionized water. 47. Discard any sulfur. 48. Save the solution which now contains Fe3+ and Ni2+ for the next step. Separation of the Fe3+ and Ni2+ Cations 49. To the solution (from step 48) add 6 M NH3 dropwise, with stirring, until the solution is just alkaline. Check with litmus paper. 50. Add 1 additional mL of 6 M NH3. 51. Add 10 drops of 3% hydrogen peroxide (H2O2), with stirring. 52. Heat the solution in a hot water bath in the hood for 1-2 minutes to coagulate any Fe(OH)3 precipitate. 53. Let the solution stand undisturbed for 5 minutes. 54. Centrifuge and decant saving both the supernatant and precipitate. Save the supernatant solution to test for Ni2+ (step 58). Save the precipitate to test for Fe3+ in the next step.

Cation Qualitative Analysis __________________________________________________________________

Confirmation of the Fe3+ Cation 55. To dissolve the precipitate from step 54, add 1 mL of 6 M HCl, with stirring. 56. Add 2 drops of 0.1 M KSCN. 57. Record your observations. The formation of a blood-red solution produced by the thiocyanatoiron(III) complex ion, [Fe(SCN)]2+, indicates the presence of the iron(III) cation (Fe3+). Confirmation of the Ni2+ Cation 58. To the supernatant solution from step 54 add 6 M CH3COOH dropwise, with stirring, until the solution is acidic. Check with litmus paper. 59. Add solid Na(CH3COO) in small portions, with stirring, until the solution is saturated. 60. Add 5 - 10 drops of 1% dimethylglyoxime solution. 61. Record your observations. The formation of a bright-red precipitate indicates the presence of the nickel(II) cation (Ni2+).

Cation Qualitative Analysis Group III Name____________________ CHEZ 102L Section_____ Date _______ Unknown # _____ Cation Report: Fe2+/3+ Ni
2+

(circle one) Present Absent (15 pts) Present Absent (15 pts)

GRADE

100

85

70