Group III Cations

y Al3+, (Cd2+), Co2+, Cr3+, Fe2+ and Fe3+, Mn2+, Ni2+, Zn2+ y Precipitated in 0.1 M H2S solution at pH 9 y Ions that form sulfides which are insoluble in basic solution. The reagents are similar to these of the 2nd group, but separation is conducted at pH of 8 9

C-1

Decantate from B-1:
add 1ml 5% thioacetamide (C2H5NS) and heat in hot water bath for at least 5 min.

add 1ml 15M NH3 and stir up the precipitate heat mixture for 5 min in hot water bath separate the precipitate and wash it w/ H2O

C-2

Precipitate from C-1:

add 10 drops HCl and stir

separate immediately and as resid e / 4 drops 1 HCl

save centrif gate for C-7

C-3

Residue from C-2: heat in hot water bath discard sulfur residue
boil the solution and add 6 3 until it becomes slightly basic to litmus

dilute solution to 1ml and divide into 3 arts

C-4
1st part of solution from C-3:

Red precipitate: Ni+2

add 1 drop DMG (dimethylglyoxime) and let it stand for 1 min

C-5

2nd part of solution from C3:
acidify with 1M HCl and add several crystals of NH CNS

Blue precipitate: Co+2

add equal volume of acetone and agitate the mixture

C-6
3rd part of solution from C-3: acidify with M CH3COOH and add several large crystals of KNO3

Yellow precipitate: Co+3

warm the mixture

C-7
Solution from C-2: transfer to a casserole, add 1ml of M HNO3 then evaporate the solution to moist residue add drops freshly prepared 3% H2O2 to mixture and heat in hot water bath for 5 min add M NaOH until precipitate forms -no precipitate: part D

add 10 drops NaOH in excess

separate the mixture and wash residue with 10 drops H2O+1 drop M NaOH

centrifuge

save centrifugate for C-12

Casserole
y Porcelain, Casserole Dish

high-temperature vessel for melting, ashing or drying samples

C-8
Residue from C-7: 1ml M HNO3 and 2 drops 1M NaNO3 stir and heat in a warm water bath Centrifuge, separate and discard any residue that remains heat to boiling then cool and divide into 3 parts

C-9
1st part of solution in C-8: add NaBIO3 and 2 drops M HNO3

Purple solution: Mn+2

C-10
2nd part of solution in C-8:

Red solution: Fe+3

add 10 drops of 0.2M KSCN

C-11
3rd part of solution in C-8:

Blue solution: Fe+3

add 2 drops of 0.2M K Fe(CN)

C-12
Centrifugate in C-7: add M CH3COOH until it is acid to litmus and add 23 drops of acid in excess add M NH3 until the solution is distinctly alkaline to litms precipitate: add M CH3COOH until dissolved white gelatinous precipitate: separate and reserve decantate for C-13

add 2 drops aluminon reagent and enough 1M (NH )2CO3 to make it basic

Red: Al+3

no precipitate: C13

C-13
Divide solution in C12 to 2 parts:

1st part: add 1M CH3COOH until acid turns to litmus then 2 drops of Pb(OAc)2

Yellow Precipitate: Cr+3
then add 10 drops 1M HCl and 5 drops 0.1M K Fe(CN)

Gray-green precipitate: Zn+2

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2nd part: add 5 drops 5% thioacetanide and heat in hot water bath

add M HCl to precipitate until it dissolves

Sources
y Introduction to Qualitative Analysis http://chemistry.about.com/library/weekly/aa091 001a.htm y Porcelain, Casserole Dish, Laboratory Supplies

http://www.labdepotinc.com/Category_Deta ils~id~30 .aspx

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