Print ISSN: 1608-9391

Online ISSN: 2664-2786

Volume 16, Issue 8

Volume 16, Issue 8, Spring 2005, Page 1-211


Square Wave Voltammetric Method for the Determination of Substituted Oxadiazol in Aqueous Solution

Eman I. Ahmed; Sadallah T. Sulaiman

Rafidain Journal of Science, Volume 16, Issue 8, Pages 1-6

A rapid, sensitive and accurate method for the determination of substituted oxadiazol (I&II) has been developed based on the reduction of electroactive group (-C=S) at hanging mercury electrode by using square wave voltammetric technique. The reduction peaks obtained at –0.028 and –0.172 V Vs Ag/AgC1 fir compounds I & II respectively at pH 2 in Britton – Robinson buffer are recommended for the trace determination of these compounds. Regression analysis on standard curve indicated a linear relationship between peak current and concentration over the rang 1.2  10-6–2.5  10-5 M with a correlation coefficient of more than 0.98.

Spectrophotometric Determination of Sulphamethazine by the Diazotisation-Coupling Method with m-Aminophenol as the Coupling Agent-Application to Pharamaceutical

tmad A. Taha

Rafidain Journal of Science, Volume 16, Issue 8, Pages 7-14

A spectrophotometric method for the trace determination of sulphamethazine has been worked out. It is based on the reaction of sulphamethazine with sodium nitrite in acidic medium to form the corresponding diazonium salt. After removal of excess nitrite with sulphamic acid, the diazotised sulphamethazine is coupled with m-aminophenol fo form an intensely-yellow coloured, water-soluble and stable azo dye which shows maximum absorption at 457 nm. The plot of absorbance versus determinand concentration shows that Beer’s law is obeyed over the concentration range 5-150 g sulphamethazine/25 ml final volume, i.e., 0.2-6 ppm with a molar absorptivity of 4.8X104
l.mol-1.cm-1. The method has been applied to the assay of the drug in a tablet.

Synthesis of 1,2,4-Oxadiazolidine and Isoxazolidine Derivatives from Addition of Isocyanates and Alkenes to Nitrones

Namer S. Ezzat; Huda A. Basheer; Mohammad S. Al-Ajely

Rafidain Journal of Science, Volume 16, Issue 8, Pages 15-21

Some new heterocyclic compounds of 1,2,4-oxadiazolidine-5-one derivatives
[3a-m] were synthesized from the reaction of nitrone compounds with some isocyanates of amino acid esters in good yields.
The reaction of nitrone compounds with cyclooctene and tetrahydrophthalic anhydride gave oxazolidine derivatives [4a-d]. The synthesized compounds were formed via 1,3-cycloaddition reaction of isocyanates and alkenes to nitrones. The I.R. spectral data of the synthesized compounds were also discussed.

The Electrical Conductivity of a Mixture of Both Symmetrical and Unsymmetrical Complexes in Methanol At 25 °C

Banan A. Akrawi

Rafidain Journal of Science, Volume 16, Issue 8, Pages 22-34

We have measured the electrical conductivity of a mixture of both symmetrical and unsymmetrical complexes: {[Ni(en)3](N03)2} + {[Co(en)2Cl2]Cl} in methanol at 298K. The results are analysed using Lee-Wheaton equation. The equivalent conductivities have been compared with the experimental values at the best-fit values of (R) and they are found to be in a good agreement. Besides, we have calculated the ionic concentration, activity coefficient, transport number for each ion present in the solution.

Some Biochemical Studies on Serum of Duodenal Ulcer Patients Infected with Helicobacter pylori in Ninevah Governorate

Bahyj Y. Al-Khalil; Tareq Y. Ahmad; Layla A. Mustafa

Rafidain Journal of Science, Volume 16, Issue 8, Pages 35-44

The research was concerned with biochemical studies in serum of duodenal ulcer (DU) patients. The present study included (152) patients (105 males and 47 females), their ages ranged between (15-56) years, attending endoscopy unit of Al-Razzi General Teaching Hospital in Ninevah Governorate.
Blood samples from (152) DU patients, were collected for some biochemical parameters including alkaline phosphatase (ALP), glutamate pyruvate transaminase (GPT), urea, total protein, Immunoglobulins (Igs), and haemoglubin (Hb).
The results predicted that GPT, urea, total protein, IgG and complement C4 statistically showed no significant difference with H. pylori infection, while ALP, IgM, IgA, complement C3 and Hb showed significant differences.

Synthesis of New Derivatives for Substituted Malonamic Acids

Mohammad A. Sheat

Rafidain Journal of Science, Volume 16, Issue 8, Pages 45-53

A number of substituted malonamic acids derivatives were prepared by nucleophilic substitution reactions of substituted malonyl chlorides with phenyl carbamate followed by reaction of the products with water, alcohol and amine. The structures of the synthesized compounds were elucidated by physical and spectroscopic methods.

Nutritional Rickets in Northern Iraqi Children – Response to Vitamin D

Akram J. Ahmad; Samir B. Al-Mukhtar

Rafidain Journal of Science, Volume 16, Issue 8, Pages 54-59

alkaline phosphatase (ALP) and albumin was studied on twenty seven rachitic children aged 6-60 months who attended the outpatient department in Al-Khansa maternity and children's Hospital in Mosul during the period from July 2000 to April 2001 and were followed up 6-8 weeks after treatment by oral massive single dose of vitamin D . The radiological and biochemical characteristics of cases ware ascertained before and after therapy .The biochemical changes ware analyzed by student (t) test.
There was a significant increase in the level of serum calcium(p<0.006), phosphorus, and albumin (P<0.0001), with a significant decrease in the ALP activity after vitamin D therapy with no risk of hypercalcaemia (P< 0.0001).
In conclusion, ALP is the main test in the follow up of rachitic children ,also oral massive single dose of vitamin D is effective in reversal of BBP to normal levels with no risk of hypercalcaemia
Key words: Rickets, Calcium, Phosphorus, Albumin, Alkaline phosphatase, Biochemical Bone Profile, Vitamin D.

Diazotised p-Nitroaniline Reagent for the Determination of Trace Amounts of Salbutamol Sulphate in Aqueous Solution– Application to Pharmaceutical Preparations

Inaam A. Hamdon; Nabeel S. Othman

Rafidain Journal of Science, Volume 16, Issue 8, Pages 60-67

A simple, rapid and sensitive spectrophotometric method for the determination of micro amounts of salbutamol sulphate in aqueous solution has been developed. The method is based on the coupling of salbutamol sulphate with diazotised p-nitroaniline in basic medium to form a coloured mono azo dye which is stable, water- soluble and exhibits maximum absorption at 488 nm. Beer’s law is obeyed over the range 10–120 g of salbutamol sulphate in a final volume of 25 ml, i.e., 0.4–4.8 ppm with a molar absorptivity of 3.13104 l.mol.-1cm-1, a relative error of +1.80 to –3.40% and a relative standard deviation of +5.70 to +1.65%, depending on the concentration level. The proposed method does not require temperature control or solvent extraction and the method has been successfully applied to the determination of salbutamol sulphate in different types of pharmaceutical preparations, tablets and syrup.

Effect of Substituents Type on the Adsorption of Aromatic Carboxylic Acids and their Relation to Concentration, Temperature and pH

Emad A. Al-Hyali; Omar M. Ramadhan; Safwan A. Al-Dobone

Rafidain Journal of Science, Volume 16, Issue 8, Pages 68-79

The study involved investigation of the adsorption of aromatic carboxylic acids carrying various substituents such as OH, NH2 and SH. The effects of concentration, temperature and pH were induced. The results indicated that increasing the temperature from 15 to 30 oC reduces the adsorption ratio, while dilution of carboxylic acid solution to a little value showed high adsorptivity. This point is of a valuable interest because most of carboxylic acids as pollutants present in a minute amounts.
Effect of pH showed that the natural pH is the best condition for the removal which is arreptable for the treatment of industrial water. According to the literature we assumed that after one hour of extraction the system will be in equilibrium. Therefore, from this point we determined the thermodynamic functions for each system under investigation. The study revealed that the hydrogen bond present in the system and other attraction forces with the resonance have great effect on the adsoption.

Study of Charge Transfer Complexes of salicylidene aliphatic amines with Eu(fod)3 in cyclohexane by U. V. spectroscopy

Isam J. Al-Nuri; Sadallah T. Sulaiman; Layla M.N. Saleem

Rafidain Journal of Science, Volume 16, Issue 8, Pages 80-87

Salicylidene aliphatic amines in cyclohexane form 1:1 charge transfer complexes on addition of Eu(fod)3, indicated by the observation of a new band in their U.V. spectra located at longer wavelength (= 400 nm) and with low extinction coefficient. The coulorless solutions of Schiff-bases were changed to yellow on complexation with the shift reagent Eu(fod)3.
Equilibrium Constant values (K) for the complexes were obtained by applying Benesi-Hildebrand equation. The factores which affected the values of of K like the charge on N, O & C (ChN, ChO, ChC), steric energy, O-N distance, the dihedral angles (dh1 and dh2) were established computationaly and were inserted into an equation of multiple linear regression as independent variables with K as dependet variable:

K= -1288.806-1653.722ChN-40.197ChO-914.560ChC+507.207(O-N dist.)

From the equation it is seen that the most effective factor is ChN which means that increasing ChN causes more availability of the lone pair of electrons on nitrogen which facilitate the interaction with Eu(fod)3 and thus leading to higher K-value.

Application of -Radiolysed Natural Silica on the Fractionation of Virgin Olive Oil

Akram A. Mohammed

Rafidain Journal of Science, Volume 16, Issue 8, Pages 88-94

The study of -radiolysed natural Iraqi silica (Ninivite) as obtained from the main rocks indicated that as we increase the irradiation time, the ratio of amorphous silica to the crystalline one is increased. A significant effect is recognized when irradiation time approximately two hours. The radiation causes cleavage of the polymeric structure of the silica and produce monomeric silica of amorphous type. The application of the irradiated silica to the separation of virgin olive oil indicates a large difference between one fraction and another as shown by the amount of fractions and I.R. measurements. I.R. measurements indicate that olive oil contains fatty acids, fatty acid esters, phenols, alcohol and some other minor components.

Polarographic Measurement of Lactate Dehydrogenase Activity in Human Serum “Clinical Application

Hisham S. Hamdon; Talal S. Al-Najafi; Sadallah T. Sulaiman

Rafidain Journal of Science, Volume 16, Issue 8, Pages 95-99

The paper reports a sensitive and rapid method for the measurement of Lactate Dehydrogenase activity (EC 1.1.1.27) in human serum. The method is based on the polarographic measurement in the reduction of polarographic peak of NAD+ via the enzymatic reaction of LDH with lactate and NAD+.
The method was successfully applied to measure LDH activity in serum of normal and diseased individuals after the removal of albumin by zinc acetate method.

Synthesis of some Azo Compounds Derived from Substituted 4`-Aminosulfonanilides

Haiffaa Y. Hussain; Kawther H. Al-Naimi; Mohammad A. Al-Iraqi

Rafidain Journal of Science, Volume 16, Issue 8, Pages 100-106

The synthesis of azo compounds (9-11) has been achieved by reaction of diazonium salts of substituted 4`-aminosulfonanilides with some aromatic amines or phenols 4-Nitroaniline (1) is served as a synthon for 2,6-dibromo-4-nitroaniline (6). The compounds (1 and 6) undergo sulfonylation with methane- and 4-toluene sulfonyl chloride to give the corresponding sulfonanilides (2, 3, 7). The nitro group in these compounds is reduced to amino group to produce compounds (4, 5, 8). These compounds are diazotised to the corresponding diazonium salts, which are coupled with different aromatic amines or phenols to produce the azo compounds (9-11). The structure of the synthesized compounds has been confirmed on the basis of physical and spectral measurements

Coordination Compounds of Tin, Selenium and Bismuth. Complexes of Tin(IV), Selenium(IV) and Bismuth(III) with Schiff Bases

Amer A. Taqa

Rafidain Journal of Science, Volume 16, Issue 8, Pages 107-117

Tin, selenium and bismuth metal complexes containing Schiff bases ligands derived from ortho-benzaldehyde, dimethyl ketone, diethyl ketone and di(o-aminophenyl) disulphide have been prepared from the direct reaction of Schiff base and metals in 1:2 molar ratio to give:
Sn(SC6H4N=CHC6H4OCH3-o)4, Sn(SC6H4N=C(CH3)2)4, Sn(SC6H4N=C(CH2CH3)2)4, Bi(SC6H4N=CHC6H4OCH3-o)3, Bi(SC6H4N=C(CH3)2)3, SC6H4N=C(CH2CH3)2)3, Se(SC6H4N=CHC6H4O CH3-o)4, Se(SC6H4N=C(CH3) 2)4 and Se(SC6H4N=C(CH2CH3)2)4.
The reaction of the above metals with a mixture of iodine and Schiff bases give in (1:1:3) molar ratio the compounds SnI(SC6H4N=CHC6H4OCH3-o)3, SnI(SC6H4N=C(CH3)2)3, SnI(SC6H4N=C(CH2CH3)2)3, BiI(SC6H4N=CH-C6H4OCH3-o)2, BiI(SC6H4N=C(CH3)2)2, BiI(SC6H4N=C(CH2CH3)2)2, SeI(SC6H4N=CHC6H4 OCH3-o)3, SeI(SC6H4N=C(CH3)2)3 and SeI(SC6H4N=C(CH2CH3 )2)3. The compounds were characterized by microanalysis, infrared, UV/Visible spectroscopy and conductivity measurement.

Aging Effect in Different Aqueous Media on Thermal Stability of Epoxy Resin

Qais M. Abd Al-Hameed; Akram A. Mohamed

Rafidain Journal of Science, Volume 16, Issue 8, Pages 118-125

ABSTRACT
The present work deals with the influence of aging conditions on thermal stability of authentic epoxy resin exposed to different aqueous media. Thermogravimetric analysis (TGA) shows that epoxy samples cured at moderate temperatures are more stable in acidic media than the samples cured at higher temperatures. The complete decomposition temperature of the epoxy resin exceeds 4000C for samples cured at 250C then decreased gradually for samples cured at 32 and 480C respectively.

Approaches to the Synthesis of Tetracyclic Quinone System Related to Anthracyclinone

Abdul Hakeem T. Mahmood; Badie A. Ahmed

Rafidain Journal of Science, Volume 16, Issue 8, Pages 126-132

Synthesis of the tetracyclic quinone compound (10) is described. The synthetic route adopted involves: preparation of the precursor 2-(2’-methoxy carbonyl benzoyl) – 1,4-benzoquinone (7), Diels-Alder reaction of the later with cyclopentadiene, [1,5]-aroyl migration in the resulting adduct (8), and finally ring closure in (9).

Synthesis and Characterization of Some Zinc(II) and Cadmium(II) Complexes with Schiff Bases

Akram A. Mohammed

Rafidain Journal of Science, Volume 16, Issue 8, Pages 133-137

A number of zinc(II) and cadmium(II) complexes with two Schiff base ligands have been prepared. The ligands derived from the condensation of furfuraldehyde with butylamine (FBA) and hexylamine (FHA). The complexes which have the molar ratio of 1:2 (metal to ligand) had general formula [M(L)2]X2 (where M = Zn(II) or Cd(II) ; while X = Cl, NO3 or ½ SO ). The complexes were characterised by molar conductance measurements and the study of their infrared and ultraviolet absorption spectra, while zinc and cadmium contents were determined by standard procedures. These studies revealed the action of both ligands as neutral bidentate chelating ligands, formed complexes with tetrahedral structure

Synthesis and Characterization of Trinuclear Complexes and Adducts through Oxidative Addition Reaction of Thiuram Disulfide

Amena F. Al-Omari; Nabeel H. Buttrus

Rafidain Journal of Science, Volume 16, Issue 8, Pages 138-145

Selenium metal react with (RNHC(S)S)2 when (R = Ph or o-EtPh) in refluxing toluene to give the compounds [Se{RNHC(S)S}4] in high yields. The new trinuclear complexes were prepared by the reaction of [Se{RNHC(S)S}4] with some transition metal chloride salts in (1:2) molar ratio giving complexes of the general formula [M2Se{RNHC(S)S}4Cl4] where M = Co(II) and Ni(II). Adducts of these complexes with triphenyl phosphine and 1,10-phenanthroline were also prepared.
The new complexes and adducts were characterized by atomic absorption, infrared, UV-visible spectroscopy, conductivity and magnetic measurements.

Unexpected Products in the Synthesis of Tetracyclic Anthrone Systems

Abdul Hakeem T. Mahmood; Badie A. Ahmed

Rafidain Journal of Science, Volume 16, Issue 8, Pages 146-154

An unexpected bis-anthranol (11) was obtained in an attempt to synthesis 1,4-dimethxy anthrone (5a) as a precursor in the total synthesis of tetracyclic anthrone systems (7 and 8) related to anthracyclinones. Oxidative-demethylation of (11) to the corresponding quinone (12) gave the unexpected quinone methide (13). The structure of the latter and the other compounds were confined by spectroscopic measurements.

The Electrical Conductivity of Some Alkali Nitrates in Propanol-Water Mixtures at 298K

Ashur M. Dawod; Salem M. Khalil; Banan A. Akrawi

Rafidain Journal of Science, Volume 16, Issue 8, Pages 155-164

The electrical conductivity of some symmetrical (1:1) alkali nitrates in different percentages of propanol-water mixtures at 298K have been measured.
The results were analysed using Lee-Wheaton (LW) equation, that is based on a method of which involving definite sizes for the ions. The electrical conductivities of NaNO3, KNO3 and CsNO3 in propanol-water mixtures, were measured. The values of conductivity parameters, (Λo, Ka, and R) at the best fit values of the standard deviation σs(Λ) have been calculated

An Application of Lee-Wheaton Conductance Equation to Mixed (Symmetrical and Asymmetrical) Electrolytes in Methanol at Two Different Temperatures

Yaser O. Hameed; Banan A. Akrawi

Rafidain Journal of Science, Volume 16, Issue 8, Pages 165-175

The applicability of (LW) Lee-Wheaton equation is tested for three mixtures I-[Ni(phen)3]Cl2 + KBr, II-[Co(phen)3]Cl2 + KBr at 298.16K and III-[Co(phen)3]Cl2 + KBr at 308.16K. From the association constant KA and the ionic mobility λ° data for appropriate single electrolytes, detail information about the conductivity parameters are interpreted which have been affected by varying the temperature. A very good agreement is obtained between the experimental and calculated data. It is also found that (LW) equation is applicable to the salts and complexes, at different temperatures under studying.

The Effect of Proteinous Compounds from Myrtus communis L. Fruit on Some Biochemical Parameters in Mice

Tareq Y. Ahmad

Rafidain Journal of Science, Volume 16, Issue 8, Pages 176-185

Three compounds (A, B and C) were isolated by gel filtration chromatography of the precipitate produced by acetone precipitation of the aqueous extract of Myrtus communis L. fruits. Comparative molecular weights determination by gel filtration using standard proteins gave a value of 74990, 6310 and 620 dalton respectively. A single intraperitoneal injection of the isolated compounds (A, B and C) at a does of 77.5 mg/Kg was given to normal mice and some biochemical parameters were determined. The results of injection showed a significant decrease of serum glucose, cholesterol, triglycerides, total lipids level and glycogen content in liver tissues for both component A and B at different variation as compared to control group. However, compound C showed only a significant decrease in glycogen content in liver tissues.

Radical Behavior Produced in -Irradiated Alanine and Phenylalanine Amino Acids Aqueous Solutions

Khalid Y. Al-Yamoor; Azhar A. Abdul-Rahman

Rafidain Journal of Science, Volume 16, Issue 8, Pages 186-192

Radiolysis of alanine and phenylalanine in aqueous solutions containing NADH has been carried out at different gas saturation and pH. It has been found that the oxidation of NADH decreases by increasing pH. Also, it has been observed that the yield of NADH oxidation in N2-saturated aqueous solutions is higher than that observed in oxygenated irradiated solution. It is concluded that more oxidizing radicals are generated through the deamination process as a result of the electron addition on the ammo acid. The results also have shown that the yield of NADH oxidation is higher slightly in the case of alanine as compared to that in the case of phenylalanine.

Construction of Multi-Electrodes Electrochemical Detection System for Flow-Injection Analysis (FIA): Application to Cu1+/Cu2+ Couple

Amer Th. Al-Taee; Sadallah T. Sulaiman

Rafidain Journal of Science, Volume 16, Issue 8, Pages 193-200

A house-built multi-electrodes detector has been designed for flow-injection electrochemical analysis. The detection system constructed intwo part, the auxiliary electrode (1 mm diameter Pt wire), the working electrodes (5 mm diameter glassy carbon (GC)), 5 mm diameter graphite (GR) and 5 mm diameter poly pyrrole plated (PPPE) as conducting polymer) placed in one part where as the reference electrode (Ag/AgCl,sat. KC1) placed in the second part. These electrodes were fitted into a teflon body cell, as it is a good isolator and easy to machine. One can readily change the working electrodes from GC, GR or PPPE without taking the cell apart. The cell based on a conventional laminar flow or on a wall-jet mode of operation. Use of the cell is illustrated by determination of Cu1+/Cu2+ couple on the different working electrodes. The best results obtained using the conducting polymer with lowest detection limit 10-7 M (6.3 ppb as Cu+2 ion).

Flow Injection Analysis ( FIA) Technique as a Method for Determination of Hemoglobin (Total) Quantity

Amer Th. Al-Taee

Rafidain Journal of Science, Volume 16, Issue 8, Pages 201-211

A new method for the determination of Hemoglobin quantity in human blood serum based on Flow Injection Analysis ( FIA) was described . This method is relay on the decrease in the reduction peak of Potassium Ferricyanide K3[Fe(CN)6] which appeared at (-0.5V) vs. (Ag/AgCl, Sat. KCl) using Phosphate buffer (pH= 7.0) as a supporting and carrier solution. The method is sensitive and rapid. The procedure was successfully applied to the determination of Hemoglobin in various blood samples represent normal and different diseased cases such as: anemia, polysythemia. A comparison between the proposed method ( FIA) and colorimetric method was carried out using (36 samples), the relation was linear with a correlation coefficient (r= 0.9998).