2.2. Instrumentation
Elemental microanalyses of the separated solid chelates
for C, H, N and Cl were performed at the Microanalytical
center, Cairo University. The molar conductance of the
complexes in DMF was measured using Sybron-Barn-
stead conductometer (Meter-PM.6, E = 3406). Infrared
spectra were recorded on a Perkin-Elmer FT-IR type
1650 spectrophotometer. The spectra were recorded as
KBr pellets. The UV-vis absorption spectra were mea-
sured on a Shimadzu 3101pc spectrophotometer. The
molar magnetic susceptibility was measured on pow-
dered samples using the Faraday method. The diamag-
netic corrections were made by Pascal’s constant and
Hg[Co(SCN)4] was used as a calibrant. The mass spectra
were recorded by the EI technique at 70 eV using MS-
5988 GS-MS Hewlett-Packard instrument. The
H1NMR
spectra
were recorded using 300 MHz Varian-Oxford Mercury.
The thermal analyses were carried out in dynamic nitro-
gen atmosphere (20 mL·min
–1
) with a heating rate of
10˚C·min
–1
using Shimadzu TG-60H thermal analyzer.
XPD analyses were carried out by using Philips Analyti-
cal X-Ray BV, diffractometer type PW 1840. Radiation
was provided by copper target (Cu anode 2000 W) high
intensity X-ray tube operated at 40 KV and 25 mA. All
spectrophotometric measurements were preformed using
a Unicam UV-2 spectrophotometer using 10 mm quartz
cell and a blank solution as a reference. The pH measure-
ments were made using HANNA pH meter.