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Annemarie A. M. L. Huijbrechts Junrong Huang Henk A. Schols Barend van Lagen Gerben M. Visser Carmen G. Boeriu Ernst J. R. Sudhölter 《Journal of polymer science. Part A, Polymer chemistry》2007,45(13):2734-2744
New reactive unsaturated starch derivatives, 1‐allyloxy‐2‐hydroxy‐propyl‐starches (AHP‐starches), were synthesized by the reaction of waxy maize starch (WMS) and amylose‐enriched maize starch (AEMS) with allyl glycidyl ether in a heterogeneous alkaline suspension containing NaOH and Na2SO4. The degree of substitution (DS) was determined by 1H NMR spectroscopy, and a DS of 0.20 ± 0.01 was found for both AHP‐WMS and AHP‐AEMS, respectively. The AHP derivatives of WMS and AEMS were further characterized with 1H and 13C NMR. It was shown that the AHP substitution was located on the C‐6 hydroxyl group of the glucose residues in the starch. The substitution pattern of the AHP groups along the polymer chain was randomly clustered, as determined by enzymatic digestion using pullulanase, α‐amylase, and amyloglucosidase, followed by matrix‐assisted laser desorption/ionization time‐of‐flight mass spectrometry analysis of the digestion products. With X‐ray diffraction and scanning electron microscopy, no changes in the granular morphology and crystallinity between the unmodified starches and AHP‐starches were detected. © 2007 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 45: 2734–2744, 2007 相似文献
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In this work, determination of selenium in various water samples was done by using hydride generation atomic absorption spectrometry. The most appropriate values of HCl concentration, NaBH4 concentration, NaOH concentration, flow rate of argon and flow rate of waste solution were determined. The optimum concentration of the HCl, NaBH4 and NaOH solutions were found to be 7.0 mol L?1, 1.0% and 0.75%, respectively. The optimum flow rate of Ar gas and waste solution were also found to be 100.9 mL min?1 and 4.0 mL min?1, respectively. Values of LOD and LOQ were calculated separately for total Se and Se(IV). LOD and LOQ values were calculated 0.56 μg L?1, 1.87 μg L?1 for total Se and 0.72 μg L?1, 2.40 μg L?1 for Se(IV), respectively. The precision was evaluated by relative standard deviation (RSD%) was found to be 3.5% for total Se and 3.1% for Se(IV) (n = 11). A standard reference material (NIST 1643e) was used in order to check the accuracy of the proposed method. There was a good agreement between certified and found values for standard reference material. The method was applied to the analysis of total Se and Se(IV) concentrations in tap water samples collected from the various regions of Mu?la. Proposed method showed spike recovery ranges from 92% to 116% in water samples. 相似文献
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Voloshin Ya. Z. Varzatskii O. A. Vorontsov I. I. Antipin M. Yu. Lebedev A. Yu. Belov A. S. Strizhakova N. G. 《Russian Chemical Bulletin》2004,53(1):92-98
Nucleophilic substitution of chlorine atoms in the iron(ii) hexachloride clathrochelate on treatment with thiolate anions afforded hexafunctionalized tris-dioximate complexes with the pendant n-butyl-, n-octylsulfide, silatrane, and captopryl functionalizing groups. These complexes were characterized by elemental analysis, IR, UV-Vis, 1H and 13C NMR, and 57Fe Mössbauer spectroscopies, and plasma-desorption mass spectrometry. The crystal and molecular structures of the n-butylsulfide and silatrane clathrochelates were established by X-ray diffraction analysis. Cyclic voltammetry study demonstrated that the Fe2+/Fe3+ redox process of the encapsulated iron ion is responsible for the electrochemical behavior of the prepared compounds in solution. 相似文献
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Critical concentrations of α-(1→3)-D-glucan L-FV-Ⅱ from Lentinus edodes were studied by viscometry andfluorescence probe techniques. The dependence of the reduced viscosity on concentration of the glucan in 0.5 mol/L NaOHaqueous solutions with or without urea showed two turning points corresponding to the dynamic contact concentration c_s andthe overlap concentration c~* of the polymer. The values of c_s and c~* were found to be 1×10~(-3) g cm~(-3) and 1.1×10~(-2) g cm~(-3),respectively, for L-FV-Ⅱ in 0.5 mol/L NaOH aqueous solutions. The two critical concentrations of L-FV-Ⅱ in 0.5 mol/LNaOH aqueous solutions were also found to be 1.2×10~(-3) g cm~(-3) fbr c_s and 9.2×10~(-3) g cm~(-3) for c~* from the concentrationdependence of phenanthrene fluorescence intensities. The overlap concentration c~* of L-FV-Ⅱ in 0.5 mol/L NaOH aqueoussolutions was lower than that of polystyrene with same molecular weight in benzene, owing to the fact that polysaccharidetends to undergo aggregation caused by intermolecular hydrogen bonding. A normal viscosity behavior of L-FV-Ⅱ in 0.5 mol/L urea/0.5 mol/L NaOH aqueous solutions can still be observed in an extremely low concentration range at 25℃. 相似文献
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Bibekananda Das P. K. Choudhury 《Journal of polymer science. Part A, Polymer chemistry》1967,5(4):769-777
Molecular parameters of sodium cellulose xanthate in NaOH solution have been determined by means of light scattering and viscometry. The effect of the degree of substitution on the molecular configuration of sodium cellulose xanthate has been studied for three series of samples of varying degree of substitution. The expansion factor has been determined from the expression due to Orofino and Flory. The effective bond length b and the ratio of the unperturbed dimension to the dimension assuming free rotation of the chain units (R?o2/R?f2)1/2, have also been determined. It is concluded that sodium cellulose xanthate in dilute solution is a loosely coiled molecule, comparable to other cellulose derivatives in chain stiffness. 相似文献
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Toshiaki Yoshioka Tomohito Kameda Shogo Imai Masahiko Noritsune Akitsugu Okuwaki 《Polymer Degradation and Stability》2008,93(10):1979-1984
The wet dechlorination treatment of poly(vinylidene chloride) (PVDC) was evaluated at atmospheric pressure in a solution of NaOH in ethylene glycol (EG), as a function of NaOH concentration, temperature, and solvent. Hydroxide ion from NaOH was required for dechlorination with EG acting solely as a solvent. The wet treatment exhibited significantly enhanced dechlorination efficiency over traditional thermal techniques, with a reaction efficiency as high as 92.8% in 1.0 M NaOH at 190 °C. Dechlorination reactions of PVDC in both NaOH/EG and NaOH/H2O were expressed by an apparent first-order reaction. At 190 °C, the apparent rate constant in 1.0 M NaOH/EG was approximately 1.4 times larger than in 1.0 M NaOH/H2O, with an apparent activation energy of 82.8 kJ mol−1, indicating that the reaction proceeded under chemical control. The degree of dechlorination increased with increasing reaction temperature, favouring the elimination of HCl over the hydroxyl substitution of chloride. 相似文献
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The cellulose solvent dimethylsulfoxide/tetrabutylammonium fluoride trihydrate (TBAF·3 H2O) was studied as reaction medium for the synthesis of benzyl cellulose (BC) by treating the dissolved polymer with benzyl
chloride in the presence of solid NaOH or aqueous NaOH solution. BC samples with degree of substitution (DS) between 0.40
and 2.85 were accessible applying different molar ratios. The studies show that both the TBAF·3 H2O concentration and the molar ratio of the reagents to repeating unit influence the DS. The solubility of the BC synthesized
in a different way, however, of comparable DS is different. Structural analyses were carried out by means of FTIR-, 1H- and 13C NMR spectroscopy. SEC measurements revealed polymer aggregation in samples of low DS synthesized in a solvent containing
9.0% TBAF·3 H2O. At higher concentration of TBAF·3 H2O in the solvent, the BC samples obtained do not form aggregates. BC of high DS is crystalline and shows thermotropic liquid
crystalline behavior as analyzed by means of DSC. Melting point and degradation temperature are not related to the DS. 相似文献
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Ewa Rudnik G. Matuschek N. Milanov A. Kettrup 《Journal of Thermal Analysis and Calorimetry》2006,85(2):279-284
Thermal behaviour of different starch derivatives, i.e. starch esters
and ethers having degree of substitution (DS) in the range of 0.02–0.18
were studied. Potato, maize and wheat starches were used. Measurements were
carried out by coupled thermal analysis/ mass spectrometry method (STA-MS)
in air atmosphere.
The major DTG peak during the investigation
for starch derivatives is observed below 300°C. The mass loss up to a
temperature of 300°C is about 50%. The most abundant ions found areH2O+
and CO2
+. For the studied
starch derivatives with a low degree of substitution (DS<0.18) no correlation
was found between thermal stability and the level of substitution regardless
of the nature of substitution. 相似文献
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Liang Zhao Ke Feng Baosheng Wang 《International journal of environmental analytical chemistry》2013,93(12):931-939
A sensitive and simple method of ion-exchange resin separation and graphite-furnace atomic absorption spectrometry (GFAAS) detection was proposed for the determination of inorganic vanadium species. Methylene Blue (MB) was used as a chelating agent of V(V) for ion-exchange separation. The complex of V(V) and MB could be trapped by ion-exchange resin at pH 3.0 and eluted by 1.0?mol?L?1 NaOH. The vanadium species was determined subsequently by GFAAS. The concentration of V(IV) was calculated by subtracting the V(V) concentration from the total concentration of vanadium. Under the optimized experimental conditions, the detection limit of V(V) is 0.48?µg?L?1 with RSD of 2.6% (n?=?5, c?=?2.0?µg?L?1). In order to verify the accuracy of the method, a certified reference soil sample was analyzed, and the results obtained were in good agreement with the certified values. The range of recovery for V(IV) and V(V) was 97.8–99.3% and 101.7–103.6%, respectively. The proposed method was applied to the speciation analysis of vanadium in lake-water samples. 相似文献
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Susanta Kumar Borthakur Pabitra Kumar Kalita Sukanya Borthakur 《Journal of heterocyclic chemistry》2020,57(3):1261-1265
A series of novel 3,7-diphenyl-7-amino[1,3]-thiazolo[3,2-a]pyrimidine-6-nitrile derivatives 3 were synthesized by refluxing 2-amino-4-phenyl-1,3-thiazole 1 and arylidinemalononitrile 2 in propanol using NaOH as catalyst. Various synthesized products were characterized by 1H NMR, mass spectrometry (MS), infrared (IR), and elemental analysis. Antifungal activities of the synthesized compounds were done by testing against Rhizoctonia solani and Drechslera orazae, two fungal pathogens causing diseases on rice crops. 相似文献
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Aggregation properties of hydrophobized hyaluronan with different molecular weights and degrees of substitution were studied using pyrene and perylene as fluorescence probes. Both probes in contrast to native biopolymer confirmed aggregation of modified hyaluronan. The critical aggregation concentration (cac) was determined by the pyrene I1/I3 and perylene fluorescence intensity method. The cac value varied both with the molecular weight and the degree of substitution and was between 0.610 and 0.003 g·L?1. Pyrene polarity scale confirmed formation of hydrophobic domains. 相似文献
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A facile divergent synthesis of a phosphorus-containing dendron containing 1,5-diaminonaphthalene is described. The phosphorus-containing dendron, functionalized with a 1,5-diaminonaphthalene unit at the core and phenolic OH groups grafted at the periphery, has been accomplished in a versatile, simple fashion, using Schiff's condensation and nucleophilic substitution reactions with POCl3, 3-hydroxy-benzaldehyde, 4-hydroxy-benzaldehyde, and 3-amino-phenol iteratively. The structures of intermediate dendrons were characterized by infrared, NMR (1H, 13C, and 31P), liquid chromatography–mass spectrometry, and C, H, N analysis. The structure of the final dendron (6) was confirmed by infrared, NMR (1H, 13C, and 31P), matrix-assisted laser desorption/ionization time-of-flight mass spectrometry, and C, H, N analysis. The thermal stability and degradation of the resulting final dendron was checked by thermal gravitometric analysis/differential thermal analysis. 相似文献
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Bernard Bertino Ghera Qiongzhi Wu Antoine Leydier Anthony W. Coleman 《Journal of inclusion phenomena and macrocyclic chemistry》2009,64(3-4):367-371
The synthesis of a series of five para-acyl-calix[9]arenes has been achieved with total substitution as shown by MALDI-TOF mass spectrometry. All compounds form stable monolayers at the air–water interface, with apparent molecular areas between 200 and 330 Å2. 相似文献
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Zofia Kowalewska 《Spectrochimica Acta Part B: Atomic Spectroscopy》2011,66(7):546-556
For the first time, high-resolution molecular absorption spectrometry with a high-intensity xenon lamp as radiation source has been applied for the determination of sulphur in crude oil and petroleum products. The samples were analysed as xylene solutions using vaporisation in acetylene-air flame or in an electrothermally heated graphite furnace. The sensitive rotational lines of the CS molecule, belonging to the ?ν = 0 vibrational sequence within the electronic transition X1∑+ → A1П, were applied. For graphite furnace molecular absorption spectrometry, the Pd + Mg organic modifier was selected. Strong interactions with Pd atoms enable easier decomposition of sulphur-containing compounds, likely through the temporal formation of PdxSy molecules. At the 258.056 nm line, with the wavelength range covering central pixel ± 5 pixels and with application of interactive background correction, the detection limit was 14 ng in graphite furnace molecular absorption spectrometry and 18 mg kg−1 in flame molecular absorption spectrometry. Meanwhile, application of 2-points background correction found a characteristic mass of 12 ng in graphite furnace molecular absorption spectrometry and a characteristic concentration of 104 mg kg−1 in flame molecular absorption spectrometry.The range of application of the proposed methods turned out to be significantly limited by the properties of the sulphur compounds of interest. In the case of volatile sulphur compounds, which can be present in light petroleum products, severe difficulties were encountered. On the contrary, heavy oils and residues from distillation as well as crude oil could be analysed using both flame and graphite furnace vaporisation. The good accuracy of the proposed methods for these samples was confirmed by their mutual consistency and the results from analysis of reference samples (certified reference materials and home reference materials with sulphur content determined by X-ray fluorescence spectrometry). 相似文献
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Daniel M. Knauss Jack T. Bender 《Journal of polymer science. Part A, Polymer chemistry》2002,40(17):3046-3054
The phthalide ring was examined as an activating group for nucleophilic aromatic substitution. The proposed mechanism by which activation occurs is through a ring opening of the phthalide ring to form a Meisenheimer‐like σ complex. 3,3‐Bis(4‐fluorophenyl)phthalide was synthesized and examined under different reaction conditions to determine its suitability for polymer formation. Semiempirical calculations at the PM3 level suggested that 3,3‐bis(4‐fluorophenyl)phthalide is only moderately activated, whereas 1H, 13C, and 19F NMR spectroscopy suggested that the monomer was not sufficiently activated for nucleophilic aromatic substitution. However, low‐molecular‐weight polymers (number‐average molecular weight < 7000 g/mol) were produced from bisphenol A, hydroquinone, and phenolphthalein. The polymers were characterized by gel permeation chromatography, matrix‐assisted laser desorption/ionization time‐of‐flight mass spectrometry, NMR spectroscopy, and differential scanning calorimetry. The polymers displayed relatively high glass‐transition temperatures. © 2002 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 40: 3046–3054, 2002 相似文献
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Tatsuro Ouchi Masaharu Inamura Akinobu Kobayashi Minoru Imoto 《Journal of polymer science. Part A, Polymer chemistry》1981,19(10):2561-2569
The polymerization of vinyl monomer initiated by poly-p-vinylphenol (PVPh) in NaOH aqueous solution was carried out at 85°C with shaking. Methyl methacrylate (MMA) was polymerized, whereas styrene and acrylonitrile were not. PVPh, which is dissociated into phenolate form (PVPh?Na+) in NaOH aqueous solution, was effective for the polymerization. The effects of the amounts of MMA, PVPh, NaOH, and H2O on the conversion of MMA were studied. The rate of polymerization of MMA increased with an increase in the molecular weight of PVPh-Na. The overall activation energy was estimated as 54 kJ mol?1. The polymerization proceeded through a radical mechanism. The addition of tetra-n-butylammonium bromide increased the rate of polymerization. 相似文献
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M. A. Vershinin A. B. Burdukov Z. A. Starikova V. V. Novikov Ya. Z. Voloshin 《Russian Chemical Bulletin》2011,60(12):2510-2517
A free-radical substitution for the chlorine atoms with the 1,4-dioxan-2-yl fragment in the tris-dichloro-substituted dioximate iron(II) clathrochelate is accompanied by the oxidative dioxane ring opening as a side process. The compound obtained was characterized by elemental analysis data, 1D and 2D 1H and 13C{1H} NMR spectroscopy (in solution), MALDI TOF mass spectrometry, as well as by single-crystal X-ray diffraction. 相似文献
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T. Bantan R. Milačič B. Mitrović B. Pihlar 《Analytical and bioanalytical chemistry》1999,365(6):545-552
The possibilities for speciation of low molecular weight aluminium organic acid complexes (LMW-Al) in plant sap were investigated by applying a combination of various chromatographic and spectroscopic techniques. The behavior of different LMW-Al complexes was investigated in synthetic aqueous solutions on anion and cation exchange fast protein liquid chromatography (FPLC) columns with inductively coupled plasma – atomic emission spectrometry (ICP-AES) or electrothermal atomic absorption spectrometry (ETAAS) detection. Plant sap of Sempervivum tectorum with a high concentration of Al (9.3 μg cm–3) and Sansevieria trifasciata with an appreciably lower Al concentration (0.065 μg cm–3) were analyzed. The speciation study in plant sap indicated that the species present in these samples, existed as negatively charged LMW-Al complexes which were eluted at the retention time typical for Al-citrate and Al-aconitate. In order to identify Al binding ligands eluted under the chromatographic peak analysis by electrospray ionization (ESI)-MS technique using Z spray ion source were also applied. The predominant LMW-Al negatively charged complexes in Sempervivum tectorum and Sansevieria trifasciata were found to be Al-citrate and Al-aconitate. It was shown that other LMW organic acids do not form complexes with Al in the samples studied. 相似文献