Russian Journal of Applied Chemistry, 2013, Vol. 86, No. 8, pp. 1152−1160.
Pleiades Publishing, Ltd., 2013.
Original Russian Text © M.I. Degtev, O.N. Popova, A.A. Yuminova, 2013, published in Zhurnal Prikladnoi Khimii, 2013, Vol. 86, No. 8, pp. 1174−1182.
AND INDUSTRIAL INORGANIC CHEMISTRY
Organic-Solvent-Free Systems with Phase
Separation as Efﬁ cient and Safe Systems
for Extraction of Metal Ions
M. I. Degtev, O. N. Popova, and A. A. Yuminova
Perm State National Research University, Perm, Russia
Received June 25, 2013
Abstract—The possibilities of using organic-solvent-free extraction systems with phase separation, based on
antipyrine derivatives, are examined. Ionic associates with tin(II) and tin(IV) anionic complexes and mixed che-
lates of indium with antipyrine and sulfosalicylic acid are extracted into the organic phase. The suggested systems
show promise for the recovery and determination of macro- and microamounts of indium, tin(II), and tin(IV) ions.
Among diverse extraction methods for recovery and
separation of metal ions, the methods based on organic-
solvent-free systems are preferable. Such systems not
only ensure high distribution ratios of the complexes, but
are also safe and environmentally friendly.
Antipyrine (AP) and its derivatives, diantipyrylalkanes
(DAAs), are well-known organic reagents [1, 2]. Despite
success achieved in classical two-phase extraction with
these reagents, this process has a major drawback: the use
of organic solvents, which are volatile, inﬂ ammable, and
dangerously explosive; furthermore, some of them are
toxic and hazardous for the nature and human.
The use of systems with phase separation in which
water is the only liquid component can solve this problem.
Among such systems are aqueous solutions of polyeth-
ylene glycol or other water-soluble polymers with an
inorganic salting-out agent [3, 4], and also of organic
bases and acids [5, 6].
Antipyrine, which is readily soluble in water, and
its condensed derivatives are of interest as bases, and
benzoic (BA), salicylic (SA), sulfosalicylic (SSA), and
other acids are of interest as acids for this purpose. In
this work, we considered systems with phase separation,
based on these reagents, and studied the phase formation
in these systems and the extraction of some metal ions
(In, Sn, Pb) with them.
We used such organic bases as AP, diantipyrylmethane
(DAM), and propyl- (PDAM), butyl- (BDAM), isobutyl-
(IBDAM), and hexyldiantipyrylmethane (HDAM) (all
analytically pure). The reagents (R) were synthesized
by the procedure described in . Benzoic, salicylic,
sulfosalicylic, hydrochloric, and sulfuric acids were of
analytically pure grade. The inorganic salts KCl, NH
, and Na
, used as salting-
out agents, were also of analytically pure grade.
Indium solutions (0.1 M) were prepared by dissolv-
ing a weighed portion of In
grade) in 0.25 M H
, and those of tin(II), tin(IV), and
lead(II), by dissolving a weighed portion of SnCl
O in 2 M НCl or of Pb(NO
water. The metal ion concentrations were determined by
complexometric titration .
Experiments on phase separation in the systems or-
ganic base–organic acid–hydrochloric or sulfuric acid–
water were performed in 20-mL calibrated test tubes
with ground-glass stoppers. The test tubes were charged
with a weighed portion of benzoic or salicylic acid (2.5 ×