Comparative Study on Reactive Extraction of Nicotinic Acid with Amberlite LA‐2 and D2EHPA

Abstract

The comparative study of reactive extraction of nicotinic acid with Amberlite LA‐2 and D2EHPA in three solvents with different polarity indicated that the extractant type and solvent polarity control the extraction mechanism. Thus, the reactive extraction with Amberlite LA‐2 in low‐polar solvents occurs by means of the interfacial formation of an aminic adduct with 3 or 2 extractant molecules. If solvents with higher polarity are used, each reactant participates with one molecule to the interfacial reaction. The mechanism of reactive extraction with D2EHPA involves in all cases the formation of a salt as the product of the interfacial reaction between one molecule of each reactant.     

Solid Phase Extraction and Preconcentration of Trace Heavy Metal Ions in Natural Water with 2,2′‐Dithiobisaniline Modified Amberlite XAD‐2

Abstract

A solid phase extraction and preconcentration methodology utilizing a new chelating resin is described for the separation of Cd, Ni, Co, Cu, and Zn. The chelating resin matrix was prepared by covalently linking 2,2′‐dithiobisaniline synthesized from 2‐aminothiophenol with the benzene ring of polystyrene‐divinylbenzene resin Amberlite XAD‐2 through a –N?N– group. Its adsorption and preconcentration behavior for Cd, Ni, Co, Cu, and Zn in aqueous solution was studied using batch and column procedures in detail. The newly designed resin quantitatively adsorbs Cd, Ni, Co, Cu, and Zn above pH 5.0. Subsequent elution with 2 M HCl readily strips the sorbed metal ions from the resin. The sorption capacity is 360, 230, 170, 200, and 150 mol g^?1 for Cd, Ni, Co, Cu, and Zn, respectively. Their preconcentration factors are 80–200. The time for 80% sorption was less than 10 min for all five metal ions. The effects of electrolytes on the preconcentration were also investigated with the recoveries >95%. The procedure was validated by analysis of a standard reference river sediment material (GBW 08301 China). The developed method was successively utilized for the determination of Cd, Ni, Co, Cu, and Zn in tap water and river water by flame atomic absorption spectrometry (FAAS) after column SPE and preconcentration. The 3σ detection limits for these metal ions were found to be 0.10, 0.34, 0.42, 0.16, and 0.52 g L^?1, respectively. The relative standard deviation was <10% for the determination of 10 g each of Cd, Ni, Co, Cu, and Zn in a 100 mL water sample.     

Enantioselective Extraction of Racemic Mandelic Acid by Di(2‐ethylhexyl) Phosphoric Acid and Tartaric Acid Derivatives as Mixed Complex Chiral Selectors

The distribution behavior of mandelic acid (MA) enantiomers was examined in a two‐phase system containing di(2‐ethylhexyl) phosphoric acid (D2EHPA) with two tartaric acid derivatives as complex chiral selectors in n‐octanol. Factors affecting the extraction were investigated, including the structure and concentration of tartaric acid as well as the concentration of D2EHPA and D,L‐MA. The results showed that both the distribution ratio and enantioselectivity were greatly improved by using a complex chiral selector rather than using the tartaric acid derivative by itself. Finally, it was found that the formation of mixed complex chiral selectors by mixing two tartaric acid derivatives with D2EHPA can improve the capacity of enantioselective extraction.     

Extraction of 4‐Hydroxycinnamic Acid from Aqueous Solution by Emulsion Liquid Membranes

Abstract

This work reports a study of 4‐hydroxycinnamic acid extraction by emulsion liquid membranes. The effect of the presence of additives in the membrane phase on solute permeation was tested. The membrane with 2 wt.% of isodecanol, 2 wt.% of ECA4360J, and Shellsol T as diluent was selected to examine the permeation of 4‐hydroxycinnamic acid. The modeling of solute extraction was done by taking into account the mass transfer in the external phase and globule, and the reaction between the diffusing component and the stripping reagent. The agreement between the calculated results and the experimental data was found satisfactory.     

Study on Mechanical Properties and Crystallization Behavior of Polypropylene and Its Blends Modified by β Crystalline Form Nucleating Agent

The influence of β crystalline form nucleating agent (β nucleator) on the mechanical properties of homo-polymerized polypropylene (PPH), random-copolymerized polypropylene (PPR), block-copolymerized polypropylene (PPB), and PPH/PPR/PPB blends was studied. Polarized optical microscopy (POM), differential scanning calorimetry (DSC), and wide angle X-ray diffraction (WAXD) were used to characterize the crystalline morphology and behavior. The results indicated that α crystalline form of polypropylene (PP) had transformed to β crystalline form by adding 0.5% β nucleator; in the meantime, the toughness of PP and its blends was enhanced. That is, 0.5% β nucleator helped to improve the notched impact strength of PPH, PPR, and PPH/PPR/PPB blends by 130%, 40%, and 40%, respectively, without losing the tensile strength and flexural strength.     

Synthesis and Metal‐ion Binding Properties of New N2S4O2‐ and N2S5O2‐Donor Macrocycles

Abstract

Synthetic procedures for new mixed‐donor macrocycle compounds were reported. The macrocyclic compounds were used in solvent extraction metal picrates such as Ag⁺, Hg²⁺, Cd²⁺, Zn²⁺, Cu²⁺, Ni²⁺, Mn²⁺, Pb²⁺, and Co²⁺. The metal picrate extractions were investigated at 25±0.1°C with the aid of UV‐visible spectrometry. It was found that 6,7,9,10,12,13,23,24‐octahydro‐19H,26Hdibenzo[h,t](1,4,7,13,16,22,10,19) dioxatetrathiadiazasiclotetracosine‐20,27(21H,28H)‐dione showed selectivity towards Ag⁺, Hg²⁺, and Cd²⁺ among the other metals. The extraction constants (Log K_ex) and complex compositions were determined for the Ag⁺ and Hg²⁺ complexes for this compound and 9,10,12,13,23,24,26,27,29,30‐decahydro‐5H,15H‐dibenzo‐[h,w][1,4,7,13,16,19,25‐,10,22] dioxapentathiadiazacycloheptacosine‐6,16(7H,17H)‐dione.     

Three New Metal–Organic Polymers Based on Flexible 3-(4-(Carboxymethoxy) Phenyl) Propanoic Acid: Crystal Structures, Luminescent and Magnetic Properties

Three new metal–organic coordination complexes, [Zn₂L(bpp)₂Cl₂] _n (1), [ZnL(bipy)] _n (2), [NiL(bipy)(H₂O)] _n (3), have been synthesized through hydrothermal reactions of flexible 3-(4-(carboxymethoxy)phenyl) propanoic acid(H₂L) with different pyridyl-containing 1,3-bis(4-pyridyl)propane(bpp) or 4,4′-bipyridine(bipy) ligand, and they are characterized by elemetal analysis and single-crystal X-ray diffraction techniques. Complex 1 has a 2-D layer supramolecular network composed of 1-D distorted trapezoidal chains via C–H···π stacking interactions. Complex 2 displays a 2-D lattice-shaped layer structure. Complex 3 has three kinds of O–H···O intermolecular hydrogen bonds, exhibiting a 3-D supramolecular framework. The luminescent properties of complex 1 and 2 have indicated the mixture characteristic of intraligand and ligand-to-ligand charge transition. The magnetic property of 3 has shown the ferromagnetic coupling between Ni²⁺ ions.