Iraqi National Journal Of Chemistry

The new azo reagent 4-[ (6-Bromo-2-benzothiazolyl ) azo] orcinol (6-BrBTAO)
was prepared by coupling reaction between (6-bromo-2-benzothiazolyl diazonium )
chloride with orcinol in alkaline solution. The reagent was examined by using
elemental analysis, UV-Vis, and infrared spectra. A sensitive and selective
spectrophotometric method is proposed for the rapid determination of copper (II)
using (6-BrBTAO), as anew spectrophotometeric reagent. The reaction between this
reagent and copper (II) is instantaneous at 497 nm (λmax) and pH=4 to form red
complex having a mole ratio 1 : 2 (metal : ligand) and the absorbance remains stable
for over 24 hr. Beer's law is obeyed in the range of (5-30) μg.ml-1 with molar
absorptivity (Є) = 149×103 L.mol-1.cm-1and a detection limit of 0.355μg.ml-1 The
precision and accuracy were obtained to be R.S.D%=0.59%,Re%=99.94% and Erel%= -0.006%.The method is successfully employed for the determination of copper(II)
in Amalgum dental filling Sampels .The most important interference were due to
Ni2+, Zn2+, Co2+, Cd2+, Pb2+, Ag1+, and Cr3+ and suitable masking agents were used.

A sensitive and economical spectrophotometric method has been
developed for the determination of chloranil in pure form. The method is based on the
reaction of chloranil as π-acceptor with resorcinol as π-donor to give highly coloured
complex species in aqueous solution which absorbs maximally at 495nm. Beer's law
is obeyed in the concentration range 2-24 µg ml-1 with high apparent molar
absorptivity of 10.03×103 l.mol-1 cm-1.

A simple, accurate, and rapid visible spectrophotometric method has been
developed for the determination of metformin in pure form, pharmaceutical
preparations and environmental water samples . The method is based on the reaction
of metformin with copper in alkaline solution in the presence of citrate ion to form a
violet colored chromogen with an absorption maximum at 570 nm. Beer’s Law was
obeyed in the range of 10-100 µg/ml with molar absorbitivity and Sandell,s
sensitivity of 1.656×103 L.mol.-1.cm-1 and 0.1 µg/cm2 respectively. The relative
standard deviation of the method was less than 2% and accuracy (average recovery )
was 100±1.4% .The optimum conditions for color development are described and the
proposed method has been successfully applied for the determination of metformin in
pharmaceutical preparations and water samples. The common excipients and additives
did not interfere in the proposed method.

Two novel enalapril maleate (ENM) ion selective electrodes were constructed
and used for the determination of ENM in its pure form and pharmaceutical
formulations. The electrodes were based on the use of the ion association complexes
of either phosphotungstic acid (PTA) or phosphomolybdic acid (PMA) as anions with
Enalapril cation in a PVC matrix plasticizers with di-butyl phthalate (DBP). The
results of these electrodes showed stability (life time 33 and 51 days), near Nernstian
response (slope 57.2 and 52.2 mV/decade ), low detection limit (1.3×10-7 and 4.2×10-7
M ) for DBP-ENM-PTA and DBP-ENM-PMA electrodes respectively. For both
electrodes the best concentration for internal filling solution was 1×10-3 M ENM and
the linear range was 1×10-5- 1×10-1 M. The electrodes were found to be usable within
the pH range 2.2 – 3.8 and 2.5 – 3.0 for the above mentioned electrodes. This study
also included the measurements of selectivity of these electrodes in the presence of
common cations, anions and some drug excipients. The KPot
J , i
found to be less than 1.
The electrodes were successfully applied for determination of ENM in pure form and
in tablet pharmaceutical preparation with recovery of not less than 98 %.

The aim of this research is showing the preparation of poly(Styrene-Co-Ethyl
acrylate) which obtained by a free radical initiation process for co-polymerization
between Ethlyacrylate and styrene with a mixing ratio (1:1) using benzoyl peroxide as
an initiator at (70°c) and (10% ) ratio of conversion. Conversion of the ester group of
the (CPS-EA) in to hydroxamic acid was carried out by treatment of (CPS-EA) with
hydroxyl amine hydrochloride in alkaline medium at (pH=13) using sodium
hydroxide. The poly hydroxamic acid was identified by (FT-IR) spectroscopy:
Sorption capacity (qe) of the metal ion (Fe3+) was determined This study also shows
the effect of initial (pH), temperature and time on the sorption capacity of (Fe3+ ) by
(PHA).The sorption capacity of (Fe3+) on to (PHA) resin which decrease as
temperature increases indicates that the sorption was exothermic process . The values
of (∆G°) was negative, showing that the sorption of (Fe3+) on to (PHA) resin is
spontaneous .

The work is concerned with the influence of different ethanol percentages in the
range (10-50)vol. % at fixed 25Cº temperature on the values of ionization constants
pKa for some acidic and basic imines . These imines are derived 3-acetyl and 4-acetyl
pyridines in a forms of syn or anti oxime and phenolic or amino Schiff bases ,
containing phenol and primary amine groups in ortho , meta and p-positions on the
aromatic ring of primary amine sides
The plots of pKa values of acids versus the dielectric constants (D) of different
alcoholic media show a different linear or curve shapes . These results were
interpreted and discussed in details in this topic .

In this research a new complexes have been prepared with some first transition
elements, which have ageneral formula [M(L1)2X2] (where M = Manganese (II),
iron(II) cobalt(II) nickel(II) copper (II) and zinc (II). L1 = ,-Diphenyl--hydroxy
thiourea X = Cl-, NO3-) Two types of metal salts were used (chloride and nitrate) for
preparation,The complexes have been characterized by metal analysis (metal 100%)
molar conductance measurements, magnetic susceptibility measurements, IR,
electronic spectral studies.

Two new bis-acylhydrazone where as 1,4-diacetylbenzene bis(4-hydroxy
benzoyl-hydrazone) (L1H2) and 1,4-diacetylbenzene bis(4-nitrobenzoylhydrazone)
(L2H2) ligands bearing two hydrazone side groups and their metal(II) complexes have
been synthesized and characterized by 1H-NMR,13C-NMR, elemental analysis, FT-IR
spectra, magnetic susceptibility measurements and UV-vis electronic absorption
spectra. The (L1H2, L2H2) ligands were synthesized by reacting 4
hydroxybenzohydrazide and 4-nitrobenzohydrazide with 1,4-diacetylbenzene,
respectively. The ligands (L1H2, L2H2) react with anhydrous metal(II) chlorides to
form polymeric dinuclear metal(II) complexes with general formula [{M2(Lx)2}n] with
a metal to ligand ratio of 1:1 when [x = 1, 2 ; M= Co(II), Ni(II), Cu(II), Zn(II),
Cd(II)]. In the complexes, the ligands act as dianionic tetradentate and coordination
takes place in the enol tautomeric form with the enolic oxygen and azomethine
nitrogen atoms while the phenolic hydroxyl and nitro groups of dihyrazone moiety do
not participate in coordination.

Rheumatoid arthritis is associated with an excess mortality from
cardiovascular disease(CVD) and this may be related to an atherogenic lipid profile.
This study was designed to identify whether there was a correlation between disease
activity and levels of different lipid fractions in early rheumatoid arthritis (ERA)
before used any treatment.
Thirty fife of ERA patients who met in Al-Sader medical city were included in
the study compared results with Forty fife apparently healthy individuals. In the
present study significant relationship exists between reduced high density lipoprotein –cholesterol (HDLC) and elevated C-reactive protein (CRP) p value was (<0.0001)
and elevated erythrocyte sedimentation rate (ESR) p value was (<0.005).Raised of
total cholesterol (TC) was associated with raised of both ESR and CRP (<0.0001),
(<0.0005) respectively. A significant relationship is demonstrated between elevated
ESR and CRP with raised low density lipoprotein –cholesterol (LDLC) (p<0.0001)
and (p<0.05) respectively. Non significant correlation of ESR with raised triglycerides
(TG) but significant correlation between CRP and serum TG.

A Cloud point extraction procedure was presented for preconcentration of
lead(11)and cadmium(11)ions in various samples after complexation by 2-[(Benzo
thiazolyl)azo]-4-benzyl phenol (BTABP) with lead and 2-[(3-Bromo phenyl)azo]-4,5
diphenylimidazole (BPADPI) with cadmium ions are quantitatively extracted in
Triton-x-100 Following separation ,5ml of 1,2Dichloroethane (1,2-DCE) was added
to surfactant -rich phase of lead and 5ml ethanol added for surfactant rich phase of
cadmium prior to its analysis by UV-Vis Spectrometry. The experimental conditions
such as pH, concentration of Triton-x-100, temperature, time of heating ,organic
solvent effect, stoichiometry for complex extracted, synergism, when evaluated in the
proposed method was applied for the determination of lead(II) and cadmium(II) in
different samples .

Starting compound (2,6-dimethyl-4-phenyl-3,5-diethoxy carbonyl -1,4
dihydropyridine)(1) has been prepared by treating (2mole) from ethylacetoacetate
with benzaldehyde, which reacted with (2mole) hydrazine hydrate and ethanol to give
hydrazide derivative(2), then converted hydrazide group to oxadiazole and triazole
rings by reacted with (2mole) from carbon disulphide and potassium hydroxide to
give compound(3) and with (2mole) from carbon disulphide and potassium hydroxide
then (2mole) from hydrazine hydrate to give compound (4). hydrazide derivative (2)
also reacted with P-nitrobenzaldehyde and P-chlorobenzaldehyde to give (5) and (6)
respectively.

Chelation polymers for transition metals were prepared by copolymerization of
Allopurinol, a known drug for the treatment of gout and hyperuricaemia, with
ethylendiaminetetraacetic acid (EDTA) or cyclohexyldiaminetetraacetic acid (CDTA).
The prepared condensed polymers were characterized by using the following
spectrometric techniques: UV-visible, 1H-NMR and FT-IR. Their thermal behavior
were studied by using thermogravimetric analysis, The intrinsic viscosities in DMF
were calculated, and their % swelling in water was measured at 30°C.Their softening
point were measured, Also the carboxylic acid functional groups content were
measured by acid-base titration.
When they were polymerized with as a diamine drug compound; these new drug
polymers were modified with metal ions as good ligand, which could be complexes
with many poison metal ions.