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N.Sh. Lebedeva et al. / Spectrochimica Acta Part A 70 (2008) 939–942
The IR spectra of the nujol mulls and thin crystalline films
in the range from 400 to 4000 cm−1 were recorded on a FT-
IR spectrometer Perkin-Elmer 2000 and from 50 to 650 cm−1
on a FT-IR spectrometer Bruker IFS 66 s. The appropriate thin
crystalline films were prepared by evaporation of solvent from
the solution of ZnTPhP·1,4-dioxane–CCI4 on the KBr and CsI
plates. The evaporation of the volatile solvent leads to con-
siderable losses of 1,4-dioxane. To compensate these losses,
the solid films were treated with the liquid 1,4-dioxane a few
times.
Fig. 4. Scheme of “chair”(a) and “bath”(b) forms of free 1,4-dioxane.
under vacuum at 320–350 K during several days. The electronic
absorption spectra agree well with the data published earlier
[14].
References
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The samples of the crystallosolvates of ZnTPhP with 1,4-
dioxane were prepared by the ZnTPhP dissolving in excess of
1,4-dioxane. Then the solution was heated up to boiling temper-
ature, and the solvent excess was removed after cooling by flow
of air.
The thermochemical investigations were performed using
differential scanning calorimeter SETARAM TG-DSC 111 (in
nitrogen atmosphere, the reference substance is Pb), Du Pont
reference substance is In) and thermoanalytical set (in air, the
reference substance is Al2O3) [6]. As an example, a DSC curve
of the crystallosolvate of ZnTPhP with 1,4-dioxane is presented
in Fig. 1. To observe the solvent evaporation process at non-
isothermal conditions, a heating rate of 0.6 ◦C min−1 was used.
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