Spectroscopic investigation of trace levels Pd (II)‎ and Pd (IV)‎ using the ligand (H2L)‎, H2L=N', N''-bis [(1E)‎-1-(2-pyridyl)‎ ethylidene] ethanedihydrazide

Other Title(s)

الدراسة المطيافية لتحديد التراكيز القليلة للبلاديوم (II)‎ و البلاديوم (IV)‎ باستخدام ن', ن"-ثنائي [ (1E)‎-1-(2-بيريديل)‎ ايثيليدين] إيثان ثنائي الهيدرازايد

Dissertant

al-Zubi, Jafar Hashim Muhammad

Thesis advisor

Zaytun, Muhammad

University

Mutah University

Faculty

Faculty of Science

Department

Department of Chemistry

University Country

Jordan

Degree

Master

Degree Date

2016

English Abstract

In a try to find a simple, fast, accurate, and inexpensive method to differentiate between Pd(II) and Pd(IV) ions in an aqueous solution, the organic complexing agent N', N''-bis[(1E)-1-(2-pyridyl)ethylidene]ethane dihydrazide (H2L) ligand was synthesized and used to study complexation with Pd(II) and Pd(IV) in two ways: (i) Formation of soluble colored complexes employing low concentration levels of ligand and metal cations were obtained when a solution of the ligand was added to either Pd(II) or Pd(IV) ions at pH = 5- 5.5, formation of each of the complexes (Pd(II)- H2L and Pd(IV)- H2L) was accompanied by a characteristic emission and absorption spectra.

The ligand imposes a distinct emission and absorption peak(s) for each ion that could be used to characterize and identify it.

The Pd(IV)- H2L was characterized by an emission peak at 500 nm and an absorption peak at 420 nm while the Pd(II)- H2L has two absorption shoulders at 450 and 480 nm and two emission shoulders at 440 and 470 nm.

The ligand was further applied as a reagent for the spectrophotometric determination of Pd(IV) and Pd(II) ions.

The method was based on the color reaction of each ion with the H2L ligand.

Beer's law was valid over the concentration range 0.1- 6 ppm and a pH of 5- 5.5 was selected as the optimum pH for each of the soluble complexes (Pd(II)-H2L and Pd(IV)- H2L).

The reaction time between the metal ion and the ligand was found to be 60 and 80 min for Pd(II)- H2L and Pd(IV)- H2L, respectively.

The molar absorbtivity, sensitivity, and detection limit were 1.38 x 103 L.mol-1.cm-1, 1.38 x 103 L.

mol-1, and 1.17 x 10-6 mol.

L-1 for Pd(II)- H2L complex and were 4.36 x 103 L.

mol-1.cm-1, 4.36 x 103 L.

mol-1, and 4.86 x 10-7 mol.

L-1 for the Pd(IV)- H2L complex.

The relative standard deviation (RSD) was calculated to be 1.35% and 1.33% for Pd(II)- H2L and Pd(IV)- H2L complexes. (ii) Reflux for 45 min a mixture of the ligand H2L with either of the metal cations Pd(II) or Pd(IV) in 2- propanol/ water (5:1) (v/v) produced solid powders corresponding to the formation of the complexes Pd(II)- H2L (yellow) and Pd(IV)- H2L (pale yellow).

The complexes were characterized by FTIR, elemental analysis, and by comparing the 1H- NMR of the free ligand to that of the synthesized solid complexes.

Main Subjects

Chemistry

No. of Pages

71

Table of Contents

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Language

English

Data Type

Arab Theses

Record ID

BIM-731644