Effect of Concentration on the Ionic Interaction between Polystyrene Sulfonate and Cationic Surfactant in Aqueous Solution

2018 ◽  
Vol 916 ◽  
pp. 24-29
Author(s):  
Agus Haryono ◽  
Muhammad Ghozali ◽  
Sri Budi Harmami ◽  
Yenny Meliana
Keyword(s):  
Aqueous Solution ◽  
Nmr Spectra ◽  
Polymer Concentration ◽  
Polystyrene Sulfonate ◽  
Ionic Interaction ◽  
Anionic Polymer ◽  
H Nmr ◽  
Sulfonation Degree ◽  
Polystyrene Waste

Polystyrene sulfonate (PSS) were prepared by sulfonation method of polystyrene using sulfuric acid. Abundant amount of polystyrene waste can be reused as a coagulant, membrane for polymer fuel cell and anionic-cationic polymer interactions. The characterization of PSS was carried out by using UV-Vis, Fourier transform infrared spectroscopy (FTIR), nuclear magnetic resonance (NMR) spectra, molecular weight and analysis of sulfonation degree. The degree of sulfonation was obtained at 94,18%. Ionic interaction between anionic polymer PSS and cetyltrimethylammonium bromide (CTAB) as cationic compound in aqueous solution were analyzed by using dynamic light scattering (DLS), conductometry and fluorimetry. Behavior of conductivity have been calculated the critical micelle concentration (cmc). The FTIR and 1H-NMR spectra showed the ionic interaction between PSS and CTAB. This ionic interaction can be controlled by changing the polymer concentration.

Tautomerization tendencies of 2-acetylcycloalkanones, 2-acetyl-1,3-cycloalkanediones, and cyclic β-keto esters of five- and six-membered rings

2001 ◽  
Vol 79 (4) ◽  
pp. 448-454 ◽  
Author(s):  
Antonio Rojas ◽  
Alfonso Perez-Encabo ◽  
Ignacio Herraiz-Sierra ◽  
Carlos A Blanco
Keyword(s):  
Aqueous Solution ◽  
Rate Constants ◽  
Nmr Spectra ◽  
Tautomeric Equilibrium ◽  
Concentration Effects ◽  
Keto Esters ◽  
H Nmr ◽  
Kinetics Studies ◽  
Dilute Aqueous Solution ◽  
C Nmr

NMR and kinetics studies of the tautomeric equilibrium of 2-acetylcycloalkanones, 2-acetyl-1,3-cycloalkanediones, and methyl 2-oxocycloalkanecarboxylates of five- and six-membered rings have been carried out. By comparing 1H NMR and 13C NMR spectra recorded in D2O–DOCD3 and CDCl3, with those results derived using a bromination kinetic procedure in dilute aqueous solution, information concerning tautomeric interconversion is provided. Some discussions considering ionisation equilibria and rate constants involved have also been considered. Solvent and concentration effects on keto-enol equilibria have also been discussed.Key words: 2-acetylcycloalkanones, 2-acetyl-1,3-cycloalkanediones, methyl 2-oxocycloalkanecarboxylates, equilibrium, tautomerization, ionization.

scholarly journals Preparation and Characterization of Styrene Bearing Diethanolamine Side Group, Styrene Copolymer Systems, and Their Metal Complexes

2018 ◽  
Vol 2018 ◽  
pp. 1-15 ◽  
Author(s):  
Aslışah Açıkses ◽  
Necmittin Çömez ◽  
Fatih Biryan
Keyword(s):  
Free Radical ◽  
Electrical Properties ◽  
Metal Complexes ◽  
Nmr Spectra ◽  
Side Group ◽  
Conductivity Measurements ◽  
H Nmr ◽  
Ft Ir ◽  
Polymerization Method

The two copolymer systems of styrene bearing diethanol amine side group and styrene were prepared by free radical polymerization method at 60°C in presence of 1,4-dioxane as solvent and AIBN as initiator. Their metal complexes were prepared by reaction of the copolymer used as ligand P(DEAMSt-co-St)L′′ and Ni(II) and Co(II) metal ions, which was carried out in presence of ethanol and NaOH at 65°C for 48 h in pH = 7.5. The structures of the copolymers used as ligand and metal complexes were identified by FT-IR, 1H-NMR spectra, and elemental analysis. The properties of the copolymers used as ligand and metal complexes were characterized by SEM-EDX, AAS, DSC, TGA, and DTA techniques. Then, the electrical properties of the copolymers and metal complexes were examined as a function of the temperature and frequency, and the activation energies (Ea) were estimated with conductivity measurements.

sHigh resolution 1H nuclear magnetic resonance studies of a flavine and its product with MoCl4

1977 ◽  
Vol 55 (4) ◽  
pp. 575-582 ◽  
Author(s):  
T. Roberie ◽  
N. S. Bhacca ◽  
J. Selbin
Keyword(s):  
Aqueous Solution ◽  
Nuclear Magnetic Resonance ◽  
Binding Sites ◽  
Nmr Spectra ◽  
Coupling Constants ◽  
Side Chain ◽  
Magnetic Resonance Studies ◽  
H Nmr ◽  
Metal Atoms ◽  
1H Nuclear Magnetic Resonance

The high resolution 1H nmr spectra of the substituted flavine, 3-N-methyltetraacetylriboflavine (3-Me-TARF), and its non-aqueous solution complexes with Gd(fod)3, Eu(fod)3, MoCl4, and MoCl4•2CH3(CH2)2CN, were studied in order to try to discern the binding sites of the flavine as it attaches to the molybdenum. Evidence was found that all three metal atoms, Gd(III), Eu(III), and Mo(IV), are attached in solution not only by the primary binding (chelating) sites of the flavine, viz., the O-4 and N-5 atoms, but also by an acetyl oxygen atom, at the C-4′ site of the ribityl side chain. 300 MHz spectra of the 3-Me-TARF have permitted the coupling constants for the side chain methine and methylene protons to be obtained.

Synthesis of low-symmetry subphthalocyanines with diverse functionalization patterns

2009 ◽  
Vol 13 (02) ◽  
pp. 203-214 ◽  
Author(s):  
David González-Rodríguez ◽  
Christian G. Claessens ◽  
Tomás Torres
Keyword(s):  
Molecular Modeling ◽  
Nmr Spectra ◽  
Careful Analysis ◽  
Complete Separation ◽  
H Nmr ◽  
Chromatographic Techniques ◽  
Structural Assignment ◽  
Isolation And Characterization ◽  
Low Symmetry

We report here on the synthesis, isolation and characterization of unsymmetrically substituted subphthalocyanines obtained from the mixed condensation of 4,5-substituted phthalonitriles and/or 4-substituted phthalonitriles in the presence of BCl 3. Compared to phthalocyanines, it is clear that the cone-shaped structure of subphthalocyanines facilitates the isolation of the different regioisomers formed by regular laboratory chromatographic techniques. However, we demonstrate that some factors, such as the solubility of the regioisomers formed or the intermolecular interactions between side chains, can sometimes impede their complete separation. We also show that the structural assignment of each regioisomeric compound can be performed by careful analysis of its 1 H NMR spectra and, in some cases, with the help of NOE NMR experiments and molecular modeling.

Enhanced the Negative Charges of Antheraea pernyi Silk Fibroin by Methylglyoxal Modification

2015 ◽  
Vol 1101 ◽  
pp. 307-313 ◽  
Author(s):  
Jing Li ◽  
Ceng Zhang ◽  
Yi Zhang ◽  
Yan Ni Yu ◽  
Jing Wan Luo ◽  
...  
Keyword(s):  
Aqueous Solution ◽  
Silk Fibroin ◽  
Nmr Spectra ◽  
Negative Charge ◽  
Controlled Drug Release ◽  
Side Chain ◽  
Antheraea Pernyi ◽  
H Nmr ◽  
Chemically Modified ◽  
Positively Charged

Antheraea pernyi silk fibroin has favorable biocompatibility, good bioactivity and controllable biodegradability, meeting the basic requirements of controlled drug release carriers. Enhancing the negative charge of silk fibroin could further increase the encapsulation and loading efficiency of positively charged drugs. In this study, Antheraea pernyi silk fibroin was chemically modified by methylglyoxal in aqueous solution. The electric charge properties of Antheraea pernyi silk fibroin were examined to characterize the modification, the results indicated that the isoelectric point of Antheraea pernyi silk fibroin decreased from 4.5 to 3.9, and the zeta potential reduced from-11.7 mV to-12.8 mV. Amino acid analysis and 1H-NMR spectra showed that arginine residue of Antheraea pernyi silk fibroin side chain was modified by methylglyoxal for enhancing negative charge of silk fibroin. These results suggested that methylglyoxal-modified Antheraea pernyi silk fibroin could be considered as a potential starting material in loading positively charged drugs.

Phenylsilane dehydrocoupling and addition to styrene catalyzed by (R-indenyl)Ni(phosphine)(methyl) complexes

2009 ◽  
Vol 87 (1) ◽  
pp. 280-287 ◽  
Author(s):  
Yaofeng Chen ◽  
Davit Zargarian
Keyword(s):  
Solid State ◽  
Nmr Spectra ◽  
Variable Temperature ◽  
Structural Parameters ◽  
Catalytic Cycle ◽  
Synthesis And Characterization ◽  
H Nmr ◽  
Solid State Structures ◽  
Indenyl Complexes

This report describes the synthesis and characterization of the Ni–Me complexes (R-indenyl)Ni(PR′3)Me (R = 1-i-Pr, 1-SiMe3, and 1,3-(SiMe3)2; R′= Me, Ph) and outlines their catalytic reactivities in the dehydrogenative oligomerization of PhSiH3 and its addition to styrene in the absence of initiators/activators. Observation of higher hydrosilylation activities for PPh3-based compounds featuring bulky substituents on the indenyl ligand confirms earlier suggestions that phosphine dissociation is an important component of the catalytic cycle for this reaction. In contrast, oligomerization of PhSiH3 is more facile with PMe3-based precursors and independent of the steric bulk of the indenyl ligand, implying that this reaction does not involve phosphine dissociation. These conclusions are consistent with the variable-temperature 1H NMR spectra of {1,3,-(SiMe3)2-indenyl}Ni(PR′3)Me and various structural parameters observed in the solid-state structures of {1,3,-(SiMe3)2-indenyl}Ni(PPh3)Me, {1,3,-(SiMe3)2-indenyl}Ni(PMe3)Cl, and {1-SiMe3-indenyl}Ni(PMe3)Me.Key words: nickel-indenyl complexes, hydrosilylation, hydrosilane oligomerization.

Synthesis and characterization of a series of 3-methyl-3-{3-[1-methyl-3-aryl-2-triazenyl]propyl}-1-aryl-1-triazenes and related compounds

2006 ◽  
Vol 84 (6) ◽  
pp. 831-842
Author(s):  
Jeff D Clarke ◽  
Shasta L Moser ◽  
Keith Vaughan
Keyword(s):  
Secondary Amine ◽  
Nmr Spectra ◽  
High Resolution Mass Spectrometry ◽  
Coupling Reaction ◽  
H Nmr ◽  
Methylene Groups ◽  
Related Series ◽  
Diazonium Coupling ◽  
Related Compounds

A series of diazonium salts has been coupled to both secondary nitrogen atoms of the bis-secondary amine, N,N′-dimethyl-1,3-propanediamine (MeNHCH2CH2CH2NHMe), to afford the new bistriazene series, the 3-methyl-3-{3-[1-methyl-3-aryl-2-triazenyl]propyl}-1-aryl-1-triazenes (9). These compounds have been fully characterized by IR and NMR spectroscopy, with supporting data from elemental analysis and high-resolution mass spectrometry. A limited number of model compounds in the N,N-dimethyl-N-{3-[1-methyl-3-aryl-2-triazenyl]propyl}amine series (10) have been synthesized to aid in the interpretation of the NMR spectra of the bistriazenes (9). A series of related compounds, the 3-ethyl-3-{(E)-4-[1-ethyl-3-aryl-2-triazenyl]-2-butenyl}-1-aryl-1-triazenes (11), have been synthesized by diazonium coupling with the bis-secondary amine N,N′-diethyl-2-butene-1,4-diamine (15), and the diazonium coupling reaction with trans-N,N′-dimethycyclohexane-1,2-diamine (19) has been used to prepare another related series of bistriazenes, the 3-methyl-3-{2-[1-methyl-3-aryl-2-triazenyl]cyclohexyl}-1-aryl-1-triazenes (12). The 1H NMR spectra of these compounds are complex because of the presence of two chiral centres in the cyclohexanediamine moiety; the diastereotopic protons of the methylene groups in the cyclohexane ring are clearly distinguished in the 500 MHz spectra of these compounds.Key words: triazene, bistriazene, synthesis, nuclear magnetic resonance, propanediamine, 1,4-diamino-2-butene, cyclohexanediamine.

scholarly journals Synthesis and characterization of π–extended “earring” subporphyrins

2018 ◽  
Vol 14 ◽  
pp. 1956-1960 ◽  
Author(s):  
Haiyan Guan ◽  
Mingbo Zhou ◽  
Bangshao Yin ◽  
Ling Xu ◽  
Jianxin Song
Keyword(s):  
Single Crystal ◽  
Aromatic Ring ◽  
Nmr Spectra ◽  
Ring Current ◽  
Synthesis And Characterization ◽  
Single Crystal Diffraction ◽  
X Ray ◽  
H Nmr ◽  
Single Crystal Structures

A π-extended “earring” subporphyrin 3 was synthesized from β,β′-diiodosubporphyrin and diboryltripyrrane via a Suzuki–Miyaura coupling and following oxidation. Its Pd complex 3Pd was also synthesized and both of the compounds were fully characterized by 1H NMR, MS and X-ray single crystal diffraction. The 1H NMR spectra and single crystal structures revealed that aromatic ring current did not extend to the “ear” in both of the two compounds. Their UV–vis/NIR spectra were recorded and the absorption of both compounds is extended to the NIR region and that the absorption of 3Pd is further red-shifted and more intense.

scholarly journals Synthesis and Characterization of Aza-Trimetalla Tetrahedranes

1996 ◽  
Vol 51 (11) ◽  
pp. 1621-1626 ◽  
Author(s):  
Max Herberhold ◽  
Uwe Bertholdt ◽  
Bernd Wrackmeyer
Keyword(s):  
Nitrogen Atom ◽  
Nmr Spectra ◽  
Chemical Shifts ◽  
Double Resonance ◽  
Synthesis And Characterization ◽  
Exchange Reactions ◽  
H Nmr ◽  
A Minor

The sulfimide complex Fe2(CO)6(μ-SNH) (1) reacts with Co2(CO)8 to form a 1:1 mixture of the known clusters FeCo2(CO)9(μ3-S) (2) and FeCo2(CO)9(μ3-NH) (3). The azatetrahedrane 3 may be used as a precursor for the synthesis of the new aza-trimetalla tetrahedranes Fe2Co(CO)9(μ-H)(μ3-NH) (5), CpMoFeCo(CO)8(μ3-NH) (6), CpNiFeCo(CO)6(μ3-NH) (7) and (CpNi)2Fe(CO)3(μ3-NH) (8) which were obtained from exchange reactions of 3 with Na2[Fe(CO)4], Na[CpMo(CO)3] and [CpNi(CO)]2. However, the reactions of 3 with Na2[Fe(CO)4] and Fe3(CO)12 gave Fe3(CO)9(μ-H)2(μ3-NH) (9) only as a minor product in addition to large amounts of Fe3(CO)9(μ-H)2(μ3-S) (10). The 1H NMR spectra of 3 and 5 - 9 show a broadened triplet for the NH proton between δ(1H) 8.21 and 9.53. Chemical shifts δ(14N) were determined most efficiently by heteronuclear 1H {14N} double resonance experiments. The δ(14N) values for aza-trimetalla tetrahedranes (-180 to -202) indicate delocalized bonding between the μ3-bridging nitrogen atom and the metal triangle.

scholarly journals Stimuli-responsive HBPS-g-PDMAEMA and its application as nanocarrier in loading hydrophobic molecules

2016 ◽  
Vol 12 ◽  
pp. 939-949 ◽  
Author(s):  
Yongsheng Chen ◽  
Li Wang ◽  
Haojie Yu ◽  
Zain-Ul-Abdin ◽  
Ruoli Sun ◽  
...  
Keyword(s):  
Aqueous Solution ◽  
Ph Value ◽  
Polymer Concentration ◽  
Nile Red ◽  
Stimuli Responsive ◽  
Guest Molecules ◽  
Drug Controlled Release ◽  
H Nmr ◽  
Vis Spectroscopy ◽  
Small Hydrophobic

The topic of stimuli-responsive nanocarriers for loading guest molecules is dynamic. It has been widely studied in applications including drug controlled release, smart sensing, catalysis, and modeling. In this paper, a graft copolymer (hyperbranched polystyrene)-g-poly[2-(dimethylamino)ethyl methacrylate] (HBPS-g-PDMAEMA) was synthesized and characterized by 1H NMR and GPC. It was observed that the star-like HBPS-g-PDMAEMA formed aggregates in aqueous solution. The influence of polymer concentration, ionic strength and pH value on the aggregates in aqueous solution was investigated by using UV–vis spectroscopy and DLS analysis. The results showed that size of aggregates was affected by a corresponding stimulus. In addition, the loading ability of HBPS-g-PDMAEMA aggregates was investigated by using pyrene or Nile red as the model guest molecules by using UV–vis and fluorescence spectroscopy. The results showed that HBPS-g-PDMAEMA aggregates were capable to encapsulate small hydrophobic molecules. These newly prepared HBPS-g-PDMAEMA nanocarriers might be used in, e.g., medicine or catalysis.

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