Purpose: To use the L25 Taguchi orthogonal array for optimizing the three main solvothermal parameters that affect the synthesis of metal-organic frameworks-5 (MOF-5). Methods: The L25 Taguchi methodology was used to study various parameters that affect the degree of crystallinity (DOC) of MOF-5. The parameters comprised temperature of synthesis, duration of synthesis, and ratio of the solvent, N,N-dimethyl formamide (DMF) to reactants. For each parameter, the volume of DMF was varied while keeping the weight of reactants constant. The weights of 1,4-benzodicarboxylate (BDC) and Zn(NO3)2.6H2O used were 0.390 g and 2.166 g, respectively. For each parameter investigated, five different levels were used. The MOF-5 samples were synthesized using the solvothermal reaction method, and successful synthesis was confirmed with x-ray diffraction (XRD), microscopy, Fourier transform infrared spectroscopy (FTIR) and energy-dispersive x-ray spectroscopy (EDS). The DOC obtained via XRD served as a parameter of objective quality. Results: The optimum conditions that gave the highest DOC were synthesis temperature of 130 °C, duration of 60 h, and a vehicle volume of 50 mL, with optimum Brunauer-Emmett-Teller surface area (BET -SA) of 800 m2/g. All the three synthesis parameters significantly influenced the DOC of the synthesized MOF-5 (p < 0.05). Sub-optimal conditions resulted in distorted MOFs, products that deviated from MOF-5 specifications, or MOF-5 with low DOC. Conclusion: Based on DOC and BET-SA, the best conditions for synthesis of MOF-5 when using Taguchi OA, were temperature of 130 °C, duration of 60 h, and a DMF volume of 50 mL.
MCA has gained a reputation for being a very useful statistical method for determining the association between two or more categorical variables and their graphical description. For performance this method, we must calculate the singular vectors through (SVD). Which is an important primary tool that allows user to construct a low-dimensional space to describe the association between the variables categories. As an alternative procedure to use (SVD), we can use the (BMD) method, which involves using orthogonal polynomials to reflect the structure of ordered categorical responses. When the features of BMD are combined with SVD, the (HD) is formed. The aim of study is to use alternative method of (MCA) that is appropriate with order
... Show MoreABSTRACT. The reaction between benzil and hexamethylenediamine formed a new ligand [L], [(1Z,3Z)-2,3-diphenyl-5,6,7,8,9,10-hexahydro-1,4-diazecine], of the type [N2], was synthesized by the condensation reaction through Schiff base reaction between benzil and hexamethylenediamine. The new Schiff base ligand reacts with Mnп, Niп and Coп metal ions to give the complexes with the general formula: [M(L)Cl2]. The elemental investigations have been used to analyze the ligand and its complexes by CHN, FT-IR, UV-Vis, TLC, mass spectrum, melting point with the study of biological activity to the formed compounds. From the data obtained, the proposed molecular structure adopts square planar structure about the metal ions. The study reveals
... Show MoreComplexes of Co(II),Ni(II),Cu(II) and Zn(II) with mixed ligands of phenylalanine (L) and tributylphosphine (TBPh) were prepared in aqueous ethanol with (2:1:1) (M:L:TBPh). The prepared complexes were characterized using flame atomic absorption,(C.H.N)Analysis, FT.IR and UV-Vis spectroscopic methods as well as magnetic susceptibility and conductivity measurements. In addition biological activity of the phenylalanine and complexes against two selected type of bacteria were also examined. Some of the complexes exhibit good bacterial activities. From the obtained data the octahedral structure was suggested for all prepared complexes.
The synthesis of new substituted cobalt Phthalocyanine (CoPc) was carried out using starting materials Naphthalene-1,4,5, tetracarbonic acid dianhydride (NDI) employing dry process method. Metal oxides (MO) alloy of (60%Ni3O4 40%-Co3O4 ) have been functionalized with multiwall carbon nanotubes (F-MWCNTs) to produce (F-MWCNTs/MO) nanocomposite (E2) and mixed with CoPc to yield (F-MWCNT/CoPc/MO) (E3). These composites were investigated using different analytical and spectrophotometric methods such as 1H-NMR (0-18 ppm), FTIR spectroscopy in the range of (400-4000cm-1), powder X-rays diffraction (PXRD, 2θ o = 10-80), Raman spectroscopy (0-4000 cm-1), and UV-Visib
... Show MoreFour mixed ligand complexes were prepared from 1,10-phenanthroline (Phen), 5-chlorosalicylic acid (CSA), and anthranilic acid (Anthra) dissolved in aqueous ethanol at a ratio of (1:1:1:1) M: Phen:CSA: Anthra, M(II)= Cu, Zn, Cd, and Hg. The prepared compounds were analyzed by flame atomic absorption, FT—IR, UV-Vis, and spectroscopic methods, as well as conductivity measurements and magnetic properties. After analyzing the prepared compounds using the acquired data, the complexes formed by mixing ligands were concluded to adopt an octahedral geometry. That study has been conducted to test the inhibitory effectiveness of the complexes (1,10-Phenanthroline (Phen), 5-Chlorosalicylic acid (CSA), Na[Cu(Phen)(CSA)(Anthra), Na[Zn(Phen)(CSA)(Anthr
... Show MoreSalicylaldehyde was reacting with 2-amino benzoic acid to produce the Schiff base ligand benzoic acid 2-salicylidene (L). The prepared ligand was identified by Microelemental Analysis, FT.IR and UV-Vis spectroscopic techniques. A new complexes of Co(II),Ni(II),Cu(II) and Zn(II) with Schiff base was prepared in aqueous ethanol with a (1:1) M:L. The prepared complexes were characterized using flame atomic absorption, (C.H.N) Analysis, FT.IR and UV-Vis spectroscopic methods as well as magnetic susceptibility and conductivity measurements. Biological activity of the ligand and complexes against three selected types of bacteria were also examined. Some of the complexes exhibit good bacterial activities. From the obtained data the tetrahedral str
... Show MoreOrtho amino hydrazobenzene (L) has been prepared from the reaction of ortho amino phenyl thiol with phenyl hyrazan in mole ratio(1:1). It has been characterized by elemental analysis (C, H, N), IR, UV–Vis. The complexes of the bivalent ions (Co, Ni, Cu, Zn, Pd, Cd, Hg and Pb) and the trivalent (Cr) have been prepared and characterized too. The structural have been established by elemental analysis(C,H,N), IR , UV – Vis spectra , conductivity measurements , atomic absorption and magnetic susceptibility . The complexes showed characteristic behaviour of octahedral geometry around the metal ion and the( N,N) ligand coordinated in bidentate modeexcept with pd showed square planer. ? ,kf , ?max for the complexes were estimated too .
... Show MoreThis study is included the preparation of two tetradentate amide-thiol proligands of the general structure [H2Ln], [where; (n = (1–2)]. The ligands [H2L1] and [H2L2] have been prepared from the reaction of the cyclic thioester 2-oxo-1, 4-dithiacyclohexane (compound 1) and 3-chloro-2-oxo-1, 4 dithiacyclohexane (compound 2) with 2-aminomethanepyridine in (1:1) ratio respetively. The reaction was carried out in chloroform at room temperature and under N2 atmosphere. Structural formula of these two ligands have been reported.
Four mixed ligand complexes were prepared from 1,10-phenanthroline (Phen), 5-chlorosalicylic acid (CSA), and anthranilic acid (Anthra) dissolved in aqueous ethanol at a ratio of (1:1:1:1) M: Phen:CSA: Anthra, M(II)= Cu, Zn, Cd, and Hg. The prepared compounds were analyzed by flame atomic absorption, FT-IR, UV-Vis, and spectroscopic methods, as well as conductivity measurements and magnetic properties. After analyzing the prepared compounds using the acquired data, the complexes formed by mixing ligands were concluded to adopt an octahedral geometry. That study has been conducted to test the inhibitory effectiveness of the complexes (1,10-Phenanthroline (Phen), 5-Chlorosalicylic acid (CSA), Na[Cu(Phen)(CSA)(Anthra), Na[Zn(Phen)(CSA
... Show MoreOrtho amino hydrazobenzene (L) has been prepared from the reaction of ortho amino phenyl thiol with phenyl hyrazan in mole ratio(1:1). It has been characterized by elemental analysis (C, H, N), IR, UV–Vis. The complexes of the bivalent ions (Co, Ni, Cu, Zn, Pd, Cd, Hg and Pb) and the trivalent (Cr) have been prepared and characterized too. The structural have been established by elemental analysis(C,H,N), IR , UV – Vis spectra , conductivity measurements , atomic absorption and magnetic susceptibility . The complexes showed characteristic behaviour of octahedral geometry around the metal ion and the( N,N) ligand coordinated in bidentate modeexcept with pd showed square planer. ? ,kf , ?max for the complexes were estimated too . ? for Co
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