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تحضير وتشخيص مركبات خماسية وسباعية غير متجانسة الحلقة لمشتقات الامينو بنزوثيازول == Synthesis And Identification of Five And Seven Membered Ring Heterocyclic Compounds of Amino Benzothiazole Derivatives
Author name:
علي فتاح ناصر الحسيني
Supervisor name:
فائز عبد الحسين عبد الرماحي
General topic:
Chemistry
Specific topic:
Chemistry
Degree:
Master
University:
University of Kufa - College Of Education For Girls - Chemistry Department
Language:
Arabic
University location:
Najaf
First pages:
25T1451 - p.pdf
Abstract:
تضمن الجزء الاول من البحث تحضير اربعة كواشف عضوية جديدة هي مشتقات ازو لمركب الباراكريزول وقد تم تشخيص الكواشف المحضرة من خلال اطياف الاشعة فوق البنفسجية - المرئية (UV - Vis) فضلا عن قياس اطياف الاشعة تحت الحمراء IR)) وتم اجراء قياسات نسب العناصر الدقيق ( | The first part of this study included perpetrating four new organic reagents which are derivatives of P - cresol. Its identification was done by UV - Vis spectrophotometer, IR and C. H. N. Depending on the results, we found the correspondence between the theoretical calculation and the experimental ones with a way to suggest the final structures of the prepared reagents. The purity of these reagents was tested through thin layer chromatography.The prepared reagents are : 1. 2[(4 - Methyl phenyl )azo] - 4 - Methyl phenol (MePAMP)2. 2[(4 - Chloro phenyl )azo] - 4 - Methyl phenol (CPAMP)3. 2[(4 - Methoxy phenyl )azo] - 4 - Methyl phenol (OMePAMP)4. 2[(4 - Nitro phenyl )azo] - 4 - Methyl phenol (NPAMP)The second part deals with the study of chromatographic behavior of organic prepared reagents dissolved in ethanol according to gas chromatography on stationary liquid phases as capillary columns with different polarities as zebron (FFAT) which is characterized with high polarity, silica fused (BP10) with a medium polarity and poly phenyl siloxine (OV - 5) that appears with low polarity.Gas chromatography was equipped with a flame ionization detector (FID) and the nitrogen as carrier gas with flow rate 30cm3min - 1 at different column temperatures ranged 100C increments depending on columns maximum operation temperature, column inlet temperature and detector temperature were higher than the separation column (25,50) 0C respectively.This investigation attempts to find the optimum conditions for the sequential separation were defined for the azo compounds of all capillary columns such as injection, applied pressure inlet of column, gas flow rate as well as the conditions of the efficient separation.The order of elution and resolution of compounds on various stationary liquid phases were normal chromatographic behavior which is decrease in specific retention volumes with increase of column temperature through the relationship between logarithm of specific retention volume for the studied compounds against reciprocal of absolute column temperature which is observed generally linear relation for all compounds on different liquid phases by using (Clausius - Clapeyron) , then calculate the thermodynamic parameters ?H0 , ?S0 and ?G from the slope and intercept respectively the negative values of partial molar enthalpy ?H0 of solutions indicate to highest interaction between liquid phases and separated compounds. The results show that the zebron (FFAT) consider the high negative value of ?H and the reaction was exothermic, on other hand the highest negative value of ?s means less random of solutes on some liquid phase , so it was more selective towards to prepared azo derivatives of p - cresol. Also calculated separation factor (RS),number of theoretical plate (N), equivalent highest of one theoretical plate (HETP) respectively for mixture of studied compounds on various liquid phases.The precision and accuracy of the prepared organic reagent (MePAMP) from 0.06% to 1.44% for (CPAMP) from 0.91% to 1.5%, (OMePAMP) from 0.03% to 1.42% and finally for (NPAMP) from 0.06% to 1.6%
