Iraqi National Journal Of Chemistry

This study included the extraction and separation of palladium(II) from its aqueous solutions, by
using swelled polymer crown ether (PDB18C6), and included the following:
After studying the factors that affect the extraction process for palladium ion in order to
find the ideal conditions, it was found that; the palladium ion (II) is extracted when (pH=7), and the
extraction percentage reaches its highest value (E%=91). It was noticed that, the extraction of
palladium ion was impossible from high concentration [0.5M-3.0M] of the acidic medium (HCl ,
H2SO4 , HNO3), but gave extraction percentage (E%=63-64) at the concentration [0.01M] of the
same acid. The percentage extraction of palladium from the alkaline medium (KOH , NaOH) was
very low at [1.0M-3.0M], and it became (E%=51-48) at the concentration [0.01M]. It was found
from experiments that the best shaking time was (60) minutes. It was also found that when adding
ethanol, the best extraction percentage for palladium II was (E%=92), when the volume of ethanol
(20±1Co )in the aqueous phase was (40%V/V) at a temperature
The extraction of palladium from natural medium salts (KCl , NaCl) and medium salt (NH4Cl)
has reached highest (E%-69), (E%=80), at the (1.5M) concentration of both NaCl and KCl,
respectively, and (E%=80) at the (0.01M) concentration of NH4Cl. The selectivity of saturated solid
crown ether polymer towards the extraction of palladium(II) ion, in the present of positive ions
(Li+ ,Na+ ,K+ ,Rb+ ,Ba+2 ,Sr+2 ,Ca +2 ,Cd+2 ,Ni+2 ,Mg+2 ) and presence negative ions
(F− ,Br− ,Cl− ,I− ) , was also studied.
The effect of temperature and thermodynamics functions on the process of extraction of
palladium(II) ions was studied, and it appeared that the extraction enthalpy ΔHex , has a positive
value, which means that the extraction process is endothermic. The free energy for extraction
ΔGex showed a negative value while its entropy ΔSex showed a positive value at all temperature
degrees, which means that the reaction is instantaneous.The separation of copper from palladium ions was carried out on a chromatographic column
filled with the substance (Polydibenzo-18crown-6), which was treated previously with (2.0M) KOH
solution, and using the same solution as a mobile phase to elute Pd (II) first. The process was
performed on eight batches, each batch contained (10ml) from the mobile phase, copper was
recovered from the column, using (1.0M) HCl in five batches, each (10ml) flow-rate was 1ml/min.

Cyprinus carpio were exposure to three sublethal concentrations of zinc 0.05, 0.1
and 1 mg/l ZnCl2 as well as control treatments, during periods of ( 1, 7, 14 and 21) days of
exposure. Concentration levels of zinc were determined in gills, liver, and kidney and
muscle tissues. The highest concentration was recorded in the liver, kidney and gills tissues
respectively for higher exposure concentration of zinc during (14 and 21) days of
experiment, while, the muscle tissue was accumulated lower values of zinc in comparison
with control samples.

A simple and selective spectrophotometric method is described for the
determination of p-aminophenol and m-aminophenol alone and in admixture. The
analysis is based on the reaction of tetracyanoethylene reagent with the above amines in
basic aqueous solution of sodium hydroxide forming two products having absorption
bands at λmax at 350 nm for p-aminophenol and at 466 and 350 nm for m-aminophenol.
Beer's law is obeyed in the range of 1-24 μg/ml for p-aminophenol at 350 nm and 2-34nm
for m-aminophenol at 466nm. The determination of amines in admixture is mainly
depended on the measurement of absorbances of complexes using two identical sets of
solutions, each at its λmax and under its respective optimised conditions. The accuracy
(average recovery %) are 99.66 % and 100.51 % for p-aminophenol and m-aminophenol
respectively with precision (RSD) less than 1.7 % for the two components in admixture

Three new organic heterocyclic azo dyes compounds which containing 4,5–diphenyl
imidazole group which were ( 6–NO2BTADI ) , ( 6–MBTADI ) and (6–MeBTADI ) have been
synthesized . The complexes of these reagents have been prepared with the metal ions Co (II) ,
Ni(II) and Cu(II) and were spectrally studied after fixing the optimum conditions. The study was
complated by investigating the UV–Vis spectra for solutions of forming complexes between
reagents and metal ions for a wide range of optimum pH at ( pH = 3.5 – 9.0 ) and the molar
concentrations that obey Lambert – Beer's law .
The mole ratios method of the metal: Ligand (M:L) has showed 1: 2 for all the prepared
complexes.The solutions of all these complexes prepared in the ethanol showed a bathochromic
shift in the visible spectral region, related to π →π * transitions of the semiaromatic ring
formed by the chelational coordination between the metal ions and the reagents.
The reagents and their complexes were characterized by C.H.N, IR spectra, UV-Vis
spectra, molar conductance measurements, magnetic susceptibility measurements and stability
constant. Flame atomic absorption and emission spectrophotometer was used to determine the
percents of the metal ion in the prepared complexes. The results are explained in the light of
these analysis.

In this study, the removal of cationic dye basic blue and neutral red dye used in the aqueous
solutions with zeolite was investigated as a function of ionic strength, pH and temperature.
Adsorption process was attained to the equilibrium within 1 h.
The adsorbed amount of two dyes basic blue and neutral red dye increased with increasing
ionic strength, but decreased with increasing temperature and pH. Adsorption of cationic
dye basic blue and neutral red dye was investigated by using uv-visible technique.
The Freundlich and Dubinin- Rasdushkevich (D-R) isotherm equations were applied to the
data and values of parameters of these isotherm equations were calculated.
The mean energy of adsorption E, was also calculated from the adsorption energy constant
Keng. It’s Value determined from the D-R isotherm equation. Finally thermodynamic
functions ΔG, ΔS and ΔH, were calculated by using Freundlich isotherm.

This study focus upon the determination of deposited lead on the surface area of plant
leaves spreaded in Mukalla streets, the most crowded traffics. Samples of plant leaves from
highway roads were studied as a control. Lead was analyzed spectrophotometrically by
using dithiozone method. Determined levels of lead for control samples(50 samples) were
in the range 0.0234-0.1032 μg/g dry weight with a mean value of 0.0384 μg/g, in October
Q. the range was 0.028-0.115 μg/g dry weight with a mean value of 0.0537 μg/g. In
Sharge Q. the range was 0.0237-0.1032 μg/g dry weight with a mean value of 0.0512 μg/g,
while in Mukalla Q. the rang was 0.0172-0.1247 μg/g dry weight with a mean value of
0.0532 μg/g . The main source of atmospheric pollution by lead in Mukalla is the waste
from exhaust of the petroleum fuel automobile

Flow injection spectrophtometric method was described for the trace
determination of chloramphenicol. This method depends upon the reduction of the nitro
group of the chloramphenicol to the amino group using Zn- reductor mini-column, then
diazotization of the amino group with nitrous acid and coupling with 8-hydroxyquinoline
in alkaline medium to give an intense water soluble and stable azo dye with a maximum
absorption obtained at a wavelength of 485 nm. The linear calibration curve was applied
in the range of (0.5- 50 μg ml-1). The relative standard deviation was estimated as ≤ 1.4%
for (30 μg ml-1) chloramphenicol solution of 10 successive injections. This method was
found to be easy, simple, reproducible, high precession and very sensitive for the
determination of chloramphenicol in pure form and in pharmaceutical preparations
comparing with British pharmacopoeia method.

This study is concerned with the adsorption of Crystal violet from solution on the surface of
kaolin. UV-spectrophotometric technique has been used to produce quantitative adsorption data
at different conditions of contact time, ionic strength, pH and temperature.
The calculated data were in accordance with Freundlich equation and the adsorption isotherms
are of S-curve type according to Giles classification. The results obtained show that adsorption
process follows the first order rate expression.
The adsorption phenomenon was examined as a function of temperature (20, 30, 55 oC). The
extent of adsorption of Crystal violet on the Kaolin was found to increase with
increasing temperature (endothermic process). The basic thermodynamic functions have also
been calculated.
The amount of dye adsorbed on the clay at different pH values showed an increase in the
following order pH 7< 8.1<10.5<11.9.
The adsorption process is affected by the electrolyte concentration. The results indicated an
decrease in adsorption of crystal violet in the presence of sodium hydrochloride

Photocatalytic degradation of acetic acid over zinc oxide suspended as a
photocatalyst was done , under irradiation with ultraviolet light .
The photocatalytic degradation of the acid was followed by using (IR) spectroscopy ,
which exhibits reduction in the intensity of absorption of carboxyl group of the acid .
The remaining quantity of the acid was determined by spectrophotometric method by
using a standard calibration curve of standard solutions of the acid . The reaction was
done at three different temperatures293,298,and 303 K. The effect of temperature on the
rate of reaction used in the estimation of activation energy for the reaction according to
Arrhenius plot , the activation energy was about (22)kJ . mol-1 . Langmuir kinetic model
was applied for the reaction , it used in the estimation of an approximate adsorption
equilibrium constant which was about (1.8 × 10-4 l . mol-1) . Rate constant for the
reaction was calculated by plotting of invers of rate of the reaction versus invers of
concentration of the used acid which was equal to (4.5 × 10-6) sec-1 .

Natural Iraqi mineral clays treated chemically by base using sodium hydroxide and
grafting with chromium trioxide by using thermal analysis, infrared ,ultraviolet and high
performance liquid chromatography .Result indicate that this sample have physical and
structural properties evaluated their scientific and economic utilization to be applied in
fraction processes as adsorbent to separate Iraqi heavy crude oils into their simple component

A new ligand 2-[(6-Nitro-2-benzothiazolyl)azo]-4,6-dimethylphenol (6-NBTADMP = HL) has
been synthesized by coupling diazotized 2-amino-6-nitrobenzothiazole with 2,4-dimethylphenol in
alkaline alcoholic solution. Metal complexes have the general formula [FeL2], [CoL2]Cl . H2O,
[NiL2], [CuL H2O]Cl, [ZnL2], [CdL2]. H2O, [PdLCl], and [AgL H2O] . H2O, were synthesized
from thiazolylazo ligand and metal chloride ( sulfate for Fe(II) and nitrate for Ag(I) ) in 1:1 molar
ratio (metal:ligand) for Cu(II) , Pd(II) and Ag(I) and 1:2 for the rest metal ions. Based on elemental
analysis, molar conductivity, magnetic susceptibility data, IR and UV-Vis spectra. The data show
that the ligand coordinates to the metal ion νia phenolate O, azo N and with thiazole N atoms. All
complexes are insoluble in water but these are soluble in common organic solvents such as acetone,
DMF and DMSO. According to results obtained the geometry for the complexes was suggested.

This research consists of the synthesis of some Schiff bases the following types:
1, 3 - Bis - (2-hydroxy-benzylidene) - thiourea = (L1)
1, 3 – Bis - (2-hydroxy-benzylidene) - urea = (L2)
The complexation of these ligands with some of transition metal ions (Zn+2 , Cd+2, and
Hg+2).The Schiff bases together with their corresponding prepared transition metal
complexes have been characterized on the bases of their (C.H.N) elemental analysis, IR,
UV-VIS, and atomic absorption. Molar conductivity measurement and melting point of
prepared complexes were measured. Their structures were propose according to the obtained
results.

7-Chloro-2- methyl thio-2-N-ethyl carbazato, 2N-acetyl tyrosyl hydrazido 4,5-
dioxo pyrano [ 3, 4-e ] - 1, 3-oxazine -4, 5-dione [2] , 2, 7-di(N-ethyl carbazato) 4,5-
dioxo pyrano [ 3, 4-e ] - 1, 3-Oxazine -4, 5-dione [3] and, 7- chloro 2N-acetyl amino
acid hydrazido , 2N-benzoyl amino acid Hydrazido-4,5-dioxo pyrano [3, 4-e]-1,3-
oxazine 4, 5-dione [4] were synthesized by standard methods. The pyrano -1, 3-oxazine
[1] was prepared from condensation of two moles of malonyl chloride with methyl or
benzyl thiocyanate. Spectroscopic characteristics (IR, NMR) of the pyrano -1, 3-oxazine
derivatives are presented and discussed

Serum total protein (S.T.P.), aspartate aminotransferase (AST), alanine
aminotransferase (ALT), albumin, and serum total bilirubin are of biological and chemical
importance in the diagnosis and follow up in different diseases. A variety of changes in the
concentration of these substances with the time of storage were found with time. This
research studied the possible changes in the concentration of these substances with time.
The results showed a decrease in all the biochemical substances that measured in the
research and the amount of decrease depends on the time. The decrease depends on the
chemical type of each parameter. Aminotransferases enzymes showed the most significant
changes with storage are noticed in enzymes.
It was found a negative relationship between the storage time and each of the
measured biochemical parameters in serum. The changes in serum total bilirubin explained
by the possible effect of light on the chemical transformation of bilirubin into lumirubin.
Serum proteins, especially enzymes, decrease due to the possible denaturation caused by
freezing and thawing processes. It is recommended that the analysis should be done
immediately after blood aspiration. If the sample delayed then the results should corrected
according to the ratios that obtained in this work.

This study evaluated the total thiols group(-SH), total serum protein, albumin
concentration and vitamin E, as well as peroxynitrite in serum as a parameter of
peroxidative stress for patients with β– thalassemia major, transfusion dependent,
compared with healthy controls. We found that the levels of total thiols and total protein
are significant decreased, while the albumin concentration slightly decreased in patients
compared with controls where as the depletion of the vitamin E concentration in serum
of patients is accompanying the increasing of peroxynitrite levels. The results suggest
that the measurement of peroxidative product matched with evaluation of antioxidants,
may be a simple measure of iron toxicity in thalassemia.