Rafidain Journal of Science

Complexes of the type [Cu(B`SCH)(AH)](NO3)2 and [Cu(B`SC)(A)] have been prepared in neutral and basic mediam, respectively, (where AH= substituted salicylic acid: salicylic acid-SA and o-acetylsalicylic acid-OASA and 3,5-dinitrosalicylic acid-DNSA or 5-aminosalicylic acid-ASA or 5-sulphosalicylic acid-SSA; A=deprotonated form of the AH ligand; B`SCH=benzoin semicarbazone; B`SC=deprotonated form of the ligand B`SCH).The prepared complexes were characterized by copper ion determination, relative molecular weight determination, magnetic and molar conductance measurements, infrared and electronic spectral data.
The effect of γ-rays have been studied on the aqueous solutions of the complexes under conditions where the hydroxyl radicals were scavenged by 10-3 M sodium formate in presence of dinitrogen gas at room temperature (25 ± 2 oC). Results indicated that copper (II) was reduced to copper (I) and a charge transfer between metal ion and ligands in some complexes were noticed. Some complexes have been completely decomposed while others did not affect by the radiolysis.

Tin metal react with bis (thiophosphoryl) disulfide in refluxing toluene to give the compound tetrakis- (o,o′-diethyl dithiophosphate) tin(IV). [Sn{S2P(EtO)2}4], through an oxidative addition reaction. Tri and pentanuclear complexes of general formulas [Sn{S2P(EtO)2}4(MCl2)n], and a mixed valance Sn(II) and Sn(IV) compound of general formula [Sn3{S2P(EtO)2}4Cl4], M=Co(II), Ni(II) or Cu(II),n=2,4 were prepared by a direct reaction of MCl2.6H2O, (M=Co,Ni), CuCl2.4H2O and SnCl2.2H2O with the tin compound. The complexes of the general formula [Sn3{S2P(EtO)2}4Cl4(MCl2)2],were prepared from the reaction of [Sn3{S2P(EtO)2}Cl4] and MCl2.6H2O (M=Co,Ni) and CuCl2.4H2O. The prepared were characterized by atomic absorption, IR and UV/Vis spectroscopy, conductivity and magnetic measurments.

A simple and sensitive spectrophotometric method for the assay of sulphadiazine (SDA) in aqueous medium is described, the method is based on the formation of a yellow coloured azo dye from the diazotisation of SDA followed by a coupling reaction with histidine in alkaline medium of sodium hydroxide. The intensity of absorbance for the resulting yellow azo dye was measured at 423 nm and the azo dye was stable at least for 55 minutes. Beer’s law is obeyed in the concentration range of 10 – 240 g of SDA in a final volume of 25 ml, with a molar absorptivity of 1.75104 L.mol-1.cm-1, a relative error of +0.34 to +0.44% and a relative standard deviation of 0.34 to 0.87%, depending on the concentration level of SDA.
The method has been successfully applied for the assay of SDA in burn cream and in a veterinary injectable solution.

Chalcones (1,3-diaryl-2-propen-1-ones) (1-13) were prepared using Claisen-Schmidt condensation, while Schiff bases (N-arylidene benzylamines) (14-20) were produced by the condensation of benzyl amine with substituted benzaldehydes. Schiff bases were added through 1,3-anionic cycloaddition to the double bond of chalcones under phase-transfer catalysis conditions to afford the corresponding heterocycles (pyrrolidines 21-30).
Spectral methods were used to support the structures of the new products, while the suggested mechanisms were investigated depending on the spectral identification as well as some theoretical parameters such as heat of formation (H.F) and steric energy (S.E). The biological activity of some reactants and some final products had been tested through its effects on two kinds of bacteria.

The research was concerned with chemical analysis of the gastric juice in duodenal ulcer patients caused by Helicobacter pylori infection. The study included (25) patients (13 males and 12 females) attending endoscopy unit of Salam General Hospital where gastric juice was taken. Also gastric juice from (25) normal healthy subjects (13 from males and 12 females) as control were collected for chemical analysis. The chemical analysis of gastric juice included measurement of electrolytes (Na+, K+, Ca+2 and Cl-) lactate, glucose, total lipids, iron in addition to conductivity and viscosity. The results of statistical analysis predicted significant differences in the levels of sodium, chloride, iron, lactate, glucose and conductivity in gastric juice of duodenal ulcer male patients infected with H. pylori in comparison to control male. However, potassium, calcium, total lipids and viscosity showed non significant difference. Females patients, however, showed significant differences for sodium, iron, calcium, lactate, glucose, total lipids and viscosity while potassium, chloride and conductivity showed non significant differences in comparison with healthy females.

In the present investigation, some new 1,3,4-oxadiazole derivatives have been prepared starting from readily available thymol. The reaction of thymol with ethylbromoacetate afforded the ethyl ester (1). Treatment of the latter with hydrazine hydrate yielded the corresponding hydrazide (2).
2,5-Disubstituted-1,3,4- oxadiazole (3a-h) were obtained by the reaction of the hydrazide with substituted benzoic acid in the presence of phosphorous oxychloride.
The structure of the new synthesized compounds were confirmed by spectral and physical means.

Salicylidene aniline and its substituents form 1:1 charge transfer complexes with the lanthanide shift reagent Pr(fod)3 in cyclohexane indicated by the observation of a new band in their U.V. spectra located at longer wavelength (λmax = 430 nm) and with its low extinction coefficient. The colourless solutions of Schiff’s-bases were changed to yellow on complexation with Pr(fod)3.
Equilibrium constant values (K) for the complexes were calculated by applying Benesi-Hildebrand equation at different temperatures, and the thermodynamic parameters ΔH, ΔS and ΔG were obtained. Negative values of ΔG indicates that the complexation occurs spontaneously.
Application of Hammet equation on K values for the para substituents show straight line with negative slope indicating that the electron donating groups enhances the reaction of complexation.

In the present study we have measured the electrical conductivity of some potassium halides (KCl, KBr and KI) in methanol at different temperatures (298-318°K). The conductivity parameters (R, Ka and Λ°) have been calculated by using Lee-Wheaton equation. The thermodynamic parameters (ΔH, ΔG and ΔS) are also calculated for these salts.
For the three electrolytes, and at any temperature, it is found that both Λo and Ka increase with increasing temperature following the order:
Λo KCl > Λo KBr > Λo KI While KaKCl < KaKBr < KaKI The overall distance parameter (R) is inversely proportional with temperature.

In the present work, the synthesis of some new fused heterocyclic rings derived from 3-benzofuranone was achieved. 3-Benzofuranone (1) was prepared by the action of polyphosphoric acid on phenoxyacetic acid. 3-Benzofuranone was treated with benzaldehyde and furfural in alkaline medium to afford 2-arylidene-3-benzofuranone (aurones) (2, 3). The reactions of the synthesized aurones with hydrazine hydrate, phenyl hydrazine, hydroxylamine hydrochloride, acetamide, urea and thiourea gave substituted pyrazoline (4, 5), 3-phenyl pyrazoline (6, 7), isoxazole (8, 9), 2-pyridinone and pyrimidin-2-one(thione) (12-15) respectively fused with 3-benzofuran. The structures of the synthesized compounds were confirmed by IR and physical methods.

An easy and extremely sensitive square wave voltammetric method for the determination of coenzyme Q10 has been evolved. The method is based on the direct measurement of the reduction peak current of the coenzyme Q10 at (-0.20 V)[(Ep) versus the Ag/AgCl reference electrode) at (pH = 7.3) and (25C). The magnitude of the reduction peak current (at Ep) has been found to be related to the concentration of the coenzyme over the range of (8.8 x 10-8 – 5.4 x 10-7 M) (r = 0.9893) and the relative standard deviation of the method at the (1.3 x 10-7 M) [113 ppb] level is ( 3.9 %) [n (number of samples) = 6]. The presence of albumin with CoQ10 causes a large depression in the reduction peak current of the coenzyme and its (Ep) moves to (-0.18 V).

A simple, rapid and sensitive spectrophotometric method for the determination of sulphacetamide sodium (SAS) was described. The method based on the oxidative coupling reaction of trifluoperazine hydrochloride (TFP) with SAS using ammonium ceric sulphate (ACS) as oxidizing agent in acidic medium to form a water soluble product, that is stable and has a maximum absorption at 560 nm. Beer’s law is obeyed in a concentration range of 1-22 g.ml-1 SAS with a molar absorptivity of 7.0103 L.mol-1 .cm-1, a relative error of –0.56 to +2.33% and a relative standard deviation of 2.56 to 4.56% depending on the concentration of SAS. The proposed method has been successfully applied to the determination of SAS in various ophthalmic preparations.

The electrical conductivity of trans – dichloro bis(ethylenediamine) cobalt (III) chloride [Co(en)2Cl2] Cl has been measured in (methanol + water), (ethanol + water) and (isoproponal + water) at different percentages and at 298K. The conductivity parameter, o (equivalent conductivity at infinite dilution, Ka; (association constant) and R the (distance parameter) between the ions were calculated by using Lee – Wheaton equation for symmetrical electrolytes.
The Walden product ( ) found to be not constant for the three media which describe as to the change of ion-solvation and of the solvent structure.

This paper deals with the extraction of a pigment (Malvidin-3-fructoside) from the Iraqi Kurdistan grape (Vitis vinifera L.). The extracted pigment was purified using physical methods including different chromatographic techniques (TLC, PC, PTLC and HPLC). The pure extracted pigment was identified using different techniques such as infrared (IR), ultraviolet (UV), 1H-NMR, 13C-NMR and CHN analysis.
The isolated pigment from grape was suggested to be very useful indicator for acid-base titration due to good precision and accuracy compared with commercial indicators such as methyl orange, methyl red and phenolphthalein. This pigment was also used in the preparation of indicator paper.