Metal ions whose sulfides develop color were separated from each other by paper chromatography using a solution of ammonium sulfide (commercial reagent, JIS first class grade chemical) as a developing solvent.
Antimony, tin and arsenic ions migrated with the solvent as their thionates, whereas other ions remained at the original point as their sulfides. Therefore ions of antimony, tin and arsenic were separated from other metal ions by a solution of ammonium sulfide (colorless).
It is rather difficult to separate tin from antimony by paper chromatography. However the separation was completed by using a mixed solution of ammonium polysulfide and pyridine, regardless of their oxidation numbers.
The sample solution contains 5 mg of each metal ion in 1 m
l of 6
N HCl.
One microliter of the sample solution was spotted with a capillary tube 1 cm apart from the end of filter paper (Toyo Roshi, No. 50).
The paper was developed up to 5 cm by the ascending technique for 30 minutes. The volume ratio of ammonium polysulfide to pyridine was 2 : 3. The paper was dried at room temperature, and then the spots of antimony and tin appeared as their sulfides. The
Rf values of antimony(III, V) and tin(II, IV) are 0.28 and 0.94.
Arsenic can be separated from tin by the same procedure as antimony separated from tin. The
Rf values of arsenic(V), arsenic(III) and tin(II, IV) are 0.12, 0.36 and 0.94, respectively.
When a small amount of 2, 4, 6-collidine was added in the solvent, antimony can be separated from arsenic. The sample solution contains 2 mg of antimony(III, V) with tin(II, IV) and 5 mg of arsenic(III, V) as each metal ion in 1 m
l of 6
N HCl.
The paper was developed up to 7 cm by the ascending technique for 60 minutes. The solvent used was ammonium polysulfide, pyridine and 2, 4, 6-collidine in a 35 : 55 : 10 volume ratios. The spot of antimony was in contact with that of arsenic(III) but can be distinguished by their color of sulfides.
Consequently, a mixed solution of ammonium polysulfide and pyridine was effective for the paper chromatographic separation of antimony, tin and arsenic ions.
View full abstract