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Solid phase extraction (SPE) methods based on multiple extractions have been developed to overcome matrix interferences in the charge-based fractionation analysis of As, Cr, Mo, Sb, Se and V leached from cement-based materials. Disposable SPE tubes packed with 500 mg strong anion-exchange (SAX) or strong cation-exchange (SCX) sorbents were used to extract the anionic and cationic species of the elements, respectively. The multiple extractions were based on the percolation of a small sample volume (5.0 mL) through a series of identical ion-exchange tubes. For most of the elements, more than 90% of the anionic species were extracted from a sample containing up to 16 g L−1 NO3− by passing the aliquot through five identical SAX tubes. Percolating a sample aliquot through three identical SCX cartridges gave more than 99% retention for Cr(III) from leachates containing a high concentration of interfering metal cations. The anionic and cationic analytes showed only slight non-specific adsorption on the SCX and SAX sorbents, respectively, except for V(V) on the SCX sorbent. A condition was established for the quantitative elution of the retained analytes from the ion-exchange sorbents with 1.0 mol L−1 HNO3. The multiple ion-exchange SPE procedures were validated using spike recovery tests. The methods were used to determine the anionic and cationic fractions of the target elements in concrete leachates covering a broad range of pH (3.8-13.4). The elements were found to exist predominantly as anions in the alkaline and neutral leachates. A high fraction (85%) of cationic Cr was detected in the most acidic leachate (pH 3.8). 相似文献
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Amphiphilic urethane acrylate hydrogels having heterophasic gel structure: swelling behaviors and mechanical properties 总被引:1,自引:0,他引:1
Amphiphilic urethane acrylate hydrogels containing ionic group (dimethylopropionic acid, DMPA) were prepared by varying the
molecular weight of the soft segment (polyether type, PTMG) and type of diisocyanate, and their swelling behaviors and mechanical
properties were examined. They showed amphiphilic property due to the hydrophilic ionic groups and hydrophobic polyethers
comprising the urethane acrylate network. Heterophasic gel structure could be found for the hydrogels prepared in water, but
not for the hydrogels in organic solvent (1,4-dioxane), through scanning electron microscopy. Because of this heterophasic
gel structure, they were able to take in a large amount of water as well. The hydrophobic interaction generated by the polyether
soft segments between urethane acrylate network chains decreased the degree of swelling, however, increased reversibly the
tensile strengths at equilibrium swelling state. MDI-based hydrogel showed low swelling ratio and high tensile strength because
of its ordered hard domain structure. These amphiphilic urethane acrylate hydrogels showed salt- and pH-dependent swelling
behaviors.
Received: 26 September 1997 Accepted: 24 December 1997 相似文献
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Renata Biegelmeyer Rafael Schröder Douglas F. Rambo Roger R. Dresch João L. F. Carraro Beatriz Mothes B 《Natural product research》2016,30(23):2734-2737
The purpose of this work was to study the cytotoxic effects of marine sponge Polymastia janeirensis, which has been observed in the field to release an orange substance that is toxic to fish. The result showed that aqueous extract (pH 7.0) was highly cytotoxic to glioma (U87) and neuroblastoma (SHSY5Y) cancer cell lines (IC50 < 1.0 μg/mL). In addition, this extract showed potent antioxidant and procoagulant (decreased the clotting time by 1.7-fold) activities. Interestingly, the cytotoxic effects were pH-dependent since the viability of the cancer cells was not affected with the extract (pH 5.5). The close similarity between the aqueous extract (pH 7.0) and the orange liquid that is released by the sponge indicates that this potential chemical defence of P. janeirensis deserves further investigation. 相似文献
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Shweta GuptaSandip Chavhan Krutika K. Sawant 《Colloids and surfaces. A, Physicochemical and engineering aspects》2011,392(1):145-155
Adefovir dipivoxil (ADV) is an anti-viral drug having low bioavailability due to low permeability and pH dependent solubility. In this study, self-nanoemulsifying drug delivery systems (SNEDDS) of ADV were developed with the objective of increasing its bioavailability by enhancing its intestinal permeability and minimizing the effect of pH. Preliminary screening was carried out to select oil, surfactant and co-surfactant. Ternary phase diagrams were constructed to identify the area of nanoemulsification. The nanoemulsion system selected from the phase diagram was transformed into solid-SNEDDS (S-SNEDDS) by lyophilization using D-mannitol as cryoprotectant. The formulations were characterized for transmittance, globule size, polydispersity index, zeta potential, cloud point, robustness to dilution, effect of pH and temperature, microscopic properties, in vitro and ex vivo drug release parameters. The liquid SNEDDS (L-SNEDDS) showed mean globule size of 110 ± 10 nm while mean globule size of 150 ± 16 nm was obtained with S-SNEDDS. The formulations were found to be robust to dilution and showed cloud point at 80-85 °C. TEM and SEM studies of nanoemulsion reconstituted from S-SNEDDS demonstrated the spherical shape and size of the globules. Results of DSC and XRD studies confirmed that the drug was incorporated in the S-SNEDDS. No significant difference was observed in the globule size within physiological variations of pH and temperature. The in vitro and ex vivo drug release from ADV SNEDDS was found to be significantly higher in comparison to that from plain drug suspension, irrespective of pH. Thus, SNEDDS were found to be instrumental in reducing the effect of pH variability of ADV and improving the release performance of ADV, indicating their potential to improve the oral bioavailability and thus the therapeutic efficacy of ADV. 相似文献
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Mesay Mulugeta Grethe Wibetoe Christian J. Engelsen Alemayehu Asfaw 《Analytical and bioanalytical chemistry》2009,393(3):1015-1024
Analytical methods have been developed for the simultaneous determination of hydride-forming (As, Sb) and non-hydride-forming
(Cr, Mo, V) elements in aqueous samples of a wide pH range (pH 3–13). The methods used dual-mode (DM) sample introduction
with ICP-AES and ICP-MS instruments. The effect of selected experimental variables, i.e., sample pH and concentrations of
HNO3, thiourea, and NaBH4, were studied in a multivariate way using face-centered central composite design (FC-CCD). Compromised optimum values of
the experimental parameters were identified using a response optimizer. The statistically found optimum values were verified
experimentally. The methods provided improved sensitivities for the hydride-forming elements compared with the respective
conventional nebulization (Neb) systems by factors of 67 (As) and 64 (Sb) for ICP-AES and 36 (As) and 54 (Sb) for ICP-MS.
Slight sensitivity improvements were also observed for the non-hydride-forming elements. The limits of detection (LOD) of
As and Sb were lowered, respectively, to 0.8 and 0.9 μg L−1 with the DM-ICP-AES system and to 0.01 and 0.02 μg L−1 with the DM-ICP-MS system. The short-term stabilities of both methods were between 2.1 and 5.4%. The methods were applied
for the analysis of leachates of a cement mortar material prepared in the pH range 3–13. The elemental concentration of the
leachates determined by the two DM methods were statistically compared with the values obtained from Neb-ICP-MS analysis;
the values showed good agreement at the 95% confidence level. Quantitative spike recoveries were obtained for the analytes
from most of the leachates using both DM methods.
Figure Schematic of the dual-mode sample introduction system used in combination with ICP-AES and ICP-MS for the simultaneous determination
of hydride and non-hydride-forming elements 相似文献
18.
Dada B. Shaikh Mahmood D. Aljabri Dinesh N. Nadimetla Shailesh S. Birajdar Mohammad Al Kobaisi Rajesh S. Bhosale Frank Antolasic Sidhanath V. Bhosale Sheshanath V. Bhosale 《Helvetica chimica acta》2021,104(8):e2100011
Design, synthesis and characterization of novel (2S)-2-[7-(2-aminoethyl)-1,3,6,8-tetraoxo-3,6,7,8-tetrahydrobenzo[lmn][3,8]phenanthrolin-2(1H)-yl]propanoic acid ( 1 ) bolaamphiphile, which combine naphthalene diimide (NDI) appended with l -alanine at one end of imide and ethylenediamine at the other end. An l -alanine bearing NDI-based asymmetric bolaamphiphile self-assembled at various pH ranging from 2 to 10 forms a variety of supramolecular nanostructures. The UV-Vis and emission spectroscopic techniques employed for the optical and photophysical properties study of bolaamphiphile 1 at various pH values. It was revealed that the change in pH alters both the optical and photophysical properties of bolaamphiphile 1 . Theoretical calculations used to investigate the electronic properties of the bolaamphiphile 1 . Dynamic light scattering experiments displayed formation of aggregates in solution and scanning electron microscopy (SEM) was used to visualize the nanostructures formed on silicon wafers. Furthermore, the X-ray diffraction was used to determine the nanostructure's packing properties i. e. crystalline/amorphous. Experimental circular dichroism (CD) spectroscopy results inferred and revealed the induction of chirality into the supramolecular systems, which was shown to be pH dependent. This study clearly demonstrates the manipulation of pH can control/tune chiral supramolecular structures and provide future methods for the development of chiral recognition and catalysis study. 相似文献
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Chengjuan Li Suna Wang Xianxi Zhang Jianmin Dou Dacheng Li 《Journal of solid state chemistry》2011,184(7):1581-1590
Six complexes based on a flexible tripodal ligand H3TTTA (2,2′,2″-[1,3,5-triazine-2,4,6-triyltris(thio)]tris-acetic acid) have been hydrothermally synthesized and structurally characterized. X-ray single-crystal diffractions reveal that they have rich structural chemistry: mononuclear, [Zn(HTTTA)(2,2′-bpy)(H2O)3]n (1); dimeric metallamacrocycle, [Zn(HTTTA)(2,2′-bipy)(H2O)]n (2) and [Cd(HTTTA)(2,2′-bipy)(H2O)·H2O]n (3); two-dimensional networks with binodal (3,6)-connected CdI2 topology based on linear trinuclear M3(μ2-CO2)4(μ2-CO2)2 SBUs (Secondary Building Units), [M3(TTTA)2(2,2′-bipy)2(H2O)m·nH2O]n (M=Zn·4, m=0, n=4; Cd·5 and Mn·6, m=2; n=2). The value of pH and the metal ions has large influences on the resulting structures. The flexible tricarboxylic acid exhibits four coordination modes from monodentate to μ6-bridge. Fluorescence and magnetic properties of the complexes have also been investigated in details. 相似文献
20.
WU Xiao-Yuan LU Can-Zhong ZHAO Zhen-Guo CHEN Shan-Ci KUANG Xiao-Fei XIE Yi-Ming 《结构化学》2008,27(9):1109-1118
Three novel inorganic-organic hybrid materials, [Cu(imi)2(H2O)(MoO4)]n 1, [Cuz(imi)3(MoO4)E]n.nH2O 2 and [Cu3(imi)2(OH)2(MoO4)2]n 3 (imi = imidazole), were synthesized and characterized by X-ray single-crystal structure determination. 1 crystallizes in orthorhombic, space group Pca21 with a = 13.382(4), b = 8.527(2), c = 9.622(3)A, V = 1098.0(5) A^3 Z = 4, C6H10CuMoN4O5, Mr = 377.66, Dc = 2.285 g/cm^3, F(000) = 740,μ(MoKa) = 3.095 mm^-1, the final R = 0.0256 and wR = 0.0722 for 1896 observed reflections with I 〉 2σ(I). 2 crystallizes in monoclinic, space group P2t/c with a= 11.170(2), b = 7.8244(15), c = 22.631(4)A, β = 115.790(7)°, V = 1780.9(6)A^3 Z = 4, C9H14Cu2Mo2N6O9, Mr = 669.24, Dc= 2.496 g/cm^3, F(000)=1295,μ(MoKa) = 3.792 mm^-1, the final R = 0.0225 and wR = 0.0615 for 3838 observed reflections with I 〉 2σ(I). 3 crystallizes in monoclinic, space group P21/c with a = 5.5599(19), b = 23.771(8), c = 7.3044(18)A , β = 129.356(16)°, V = 746.5(4)A^3, Z = 2, C6H10Cu3Mo2N4O10, Mr = 680.71, Dc = 3.029 g/cm^3, F(000) = 650,μ(MoKa) = 5.900 mm^-1, the final R = 0.0215 and wR = 0.0524 for 1620 observed reflections with I 〉 2σ(I). 相似文献