Author name:
احمد سعدون عباس وتوت
Supervisor name:
قاسم حسن كاظم | عباس نور محمد
Abstract:
Chapter One : explaining illustration of the importance of surfactants uses and types, and also known on cloud point extraction method in analytical chemistry , selection methods of its surfactant , phase mechanisms of its method and factor affecting on its . It also involves briefly review on the modern research of the cloud point extraction and applications for the determination of zinc, chromium, lead, cadmium, arsenic and organic compound (drugs) such as Doxycycline Hyclate and Furosemide . | Chapter Two : involved known on different instrumental techniques used , general apparatus and chemicals used in the cloud point extraction in the present work under study. The full analytical procedures for CPE which have been designed for the determination of analytes (elements and drugs) under study were made in the present work. | Chapter Three : contains the results and discussion including for the separation and preconcentration. First part , included separation and determination on nano gram amount for the metal ions which selected under study of an extraction method used surfactants environmental friendly and ability for its determination by preconcentration in a small volume of the surfactant rich phase and also its methods doesn't used the organic solvent that high expensive and toxicity , the second part include for the ability of determination of its drugs under study by its ion selected in part one and obtained a very low limit of detection, very high sensitivity and a high value of enrichment factors by using cloud point extraction joined with spectroflurimetric technique . | First part of chapter three, included the use of Doxycycline Hyclate (DOX-HYC) as an complexing agent for the establishment of ions-drug complex of Cr(III), Zn(II) and Cr(VI) in alkaline medium. This reaction was form by presence of a non-ionic surfactant in solution, in place of complexes organic reagents which have used in CPE in large field . Furosemide as an complexing reagent, on the other hand, was used for the formation of ion-drug complex Cd(II), As(III) and Pb(II) in acidic medium as a hydrophobic molecule suitable for its separation and preconcentration by CPE. Therefore , a spectrofluorimetric study for the determination of its ions to be exact (Cr(III),Zn(II) and Cr(VI)) of these forms in CPE system at λex. and λem. were 415nm and 511 nm respectively. Different boundaries have been optimized such as pH effective , surfactant amount, organic drug concentration, equilibration temperature and incubation(heating) time. | Under its optimum conditions , results showed that the enrichment factor of 70.42, 43.00 and 84.22 were achieved for each Cr(III),Zn(II) and Cr(VI) species respectively. The linear calibration curve at a linear range for Cr(III) was 0.025-1.0 ng mL-1 with detection limit of 0.0034 ng mL-1, for Zn(II) was 10.0-100.0 ng mL-1 with detection limit of 0.182 ng mL-1, and for Cr(VI) was 0.1-1.0 with detection limit of 0.0019 ng mL-1. The precision for (n=7) at 0.1, 50 and 0.5 ng mL-1 Cr(III),Zn(II) and Cr(VI) were of 2.40% , 0.63 % and 1.41% . Because of the lowest detection limit obtained , the developed method was applied for the determination micro amounts of Cr(III),Cr (VI) and Zn(II) in tap water , R.O and honey samples respectively. The proposed method is compared statistically with GFAAS technique in our laboratory using paired t-test , F test and the results have shown that no significant differences at p=0.05 in accuracy and precision. | On the other hand , this proposed method was used for determination of nano gram amounts of Pb(II), As(III) and Cd(II) using cloud point extraction technique . This method involved the formation of an ion - complex between its ions and Furosemide drug (FUR) in acidic solution and the complex is extracted into the non-ionic surfactant (Triton X-114) at optimum conditions. The surfactant-rich phase which contains ions-complex is dissolved with solvent and the solution was measured spectrofluorimeterically at λex and λem = 363 and 409 nm respectively. The effects of the several variables which affect the CPE efficiency are optimized and the thermodynamic study was also examined for all complexes in a non-ionic surfactant under study. The enrichment factor of 62.44, 149.00 and 42.34 for each Pb(II), As(III) and Cd(II) respectively obtained leading to detection limits of 0.0953, 0.0000892 and 0.321 ng mL-1 in aqueous solution for each Pb(II), As(III) and Cd(II) respectively . | The concentrations range obey Beers law of 1.25-15.0 , 0.01-0.1 and 6.75-50.0 ng mL-1 for each Pb(II), As(III) and Cd(II) respectively. The precision for (n=7) at 5, 0.08 and 10 ng mL-1 Pb(II), As(III) and Cd(II) were of 1.96% , 1.52 % and 1.73% . The developed method was used for the determination of its ions in honey, and for Pb(II) and Cd(II) in powder and liquid milk samples, and the results were compared statistically with HGAAS, and GFAAS technique using paired t-test and F -test at p=0.05 concluding there are no significant differences in accuracy and precision. | The second part of this chapter includes, a new spectroflurimetric method has been developed for the determination of its drugs, ( Doxycycline Hyclate and Furosemide) by cloud point extraction system. These determinations were obtained under the optimum conditions and the concentration for the selected drugs were measured using spectroflurimetic at each λem. It was found that the enrichment factors of 74.87, 93.47 and 172.69 for Doxy-Zn(II), Cr(III) and Cr(VI) were achieved leading to the very low limit of detection of 2.2×10-8, 1.3×10-9 and 1.1×10-9 ng mL-1 respectively. While for the complexes of Furo-Pb(II), As(III) and Cd(II) were 111.32, 184.33 and 166.80 respectively, were achieved leading to the low limit of detection of 1.1×10-9, 1.4×10-11 and 2.5×10-11 ng mL-1 respectively . | The established method showed linear calibrations in the range for Doxy-Zn(II), Cr(III) and Cr(VI) were 2.0×10-6 -2.0×10-3 , 1.0×10-7 -1.0×10-3 and 2.0×10-7 -2.0×10-3 ng mL−1 respectively. Also for Furo-Pb(II), As(III) and Cd(II) were 1.0×10-7 -1.0×10-3 , 2.0×10-9 -2.0×10-4 and 2.0×10-9 -2.0×10-4 ng mL−1 respectively .The quantum yield for all complexes that extracted in surfactant rich phase were calculated .The developed method was applied for the determination of the Doxycycline Hyclate in blood serum samples |
