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1.
A series of calcium silicate hydrate (C–S–H)-polymer nanocomposite
(C–S–HPN) materials were prepared by incorporating poly(acrylic
acid) (PAA) into the inorganic layers of C–S–H during precipitation
of quasicrystalline C–S–H from aqueous solution. The as-synthesized
C–S–HPN materials were characterized by X-ray fluorescence (XRF),
X-ray diffraction (XRD), scanning electron microscopy-energy dispersive spectroscopy
(SEM-EDS), Fourier-transform infrared (FTIR) spectroscopy, thermogravimetric
analysis (TG) and differential scanning calorimetry (DSC). The XRD analysis
of C–S–HPN materials suggest the intermediate organizations presenting
intercalation of PAA within C–S–H and exfoliation of C–S–H.
The SEM micrographs of C–S–H, PAA and C–S–HPN materials
with different PAA contents exhibit the significant differences in their morphologies.
The effect of the material’s composition on the thermal stability of
a series of C–S–HPN materials along with PAA and C–S–H
were studied by TG, DTA and DSC. Three significant decomposition temperature
ranges were observed on the TG curves of all C–S–HPN materials. 相似文献
2.
Dianxue Cao Xue Cao Guiling Wang Lin Wu Zhanshuang Li 《Journal of Solid State Electrochemistry》2010,14(5):851-855
Mg–Li–Al–Sn and Mg–Li–Al–Sn–Ce alloys were prepared using a vacuum induction melting method. Their electrochemical oxidation
behavior in NaCl solution was investigated by means of potentiodynamic and chronoamperometric measurements. The surface morphology
after discharge was examined using scanning electron microscopy. Utilization efficiency was estimated with a mass-loss method.
The results indicated that Mg–Li–Al–Sn has a higher discharge current density but lower utilization efficiency than Mg–Li–Al–Sn–Ce.
The typical utilization efficiency after continuous discharging at constant potential of −1.0 for 2 h is 65% and 70% for Mg–Li–Al–Sn
and Mg–Li–Al–Sn–Ce, respectively. The utilization efficiency decreased with the increase of anodic potential. Both alloys
have similar self-discharge rate in NaCl solution at open-circuit potential. 相似文献
3.
Jakubowska N Polkowska Z Kujawski W Konieczka P Namieśnik J 《Analytical and bioanalytical chemistry》2007,388(3):691-698
The analysis of volatile organic compounds in samples of biological fluids characterized by complex matrices is highly challenging.
This paper presents a comparison of the results obtained in this field using three solvent-free techniques: thin-layer headspace
with autogenous generation of liquid sorbent (TLHS) and membrane separation of the trace substances (pervaporation, PV), both
of which are coupled to direct aqueous injection gas chromatography–electron capture detection (TLHS–DAI–GC–ECD and PV–DAI–GC–ECD),
as well as conventional static headspace analysis followed by GC analysis with ECD detection (HS–GC–ECD). Basic validation
parameters of the HS–GC–ECD, TLHS–DAI–GC–ECD and PV–DAI–GC–ECD procedures were calculated for water and urine samples. The
calibration curves for all procedures were linear within the concentration range examined. The intermediate precisions of
the procedures were good and reached about 10% (for all analytes) for HS–GC–ECD and TLHS–DAI–GC–ECD. The poorest results were
obtained for PV–DAI–GC–ECD: about 20% for all analytes. The lowest method detection limits were obtained for the TLHS–DAI–GC–ECD
procedure: below 0.0022 μg/L for all analytes. The enrichment factors did not differ significantly between water and urine
samples, indicating little or no matrix effect in all procedures. 相似文献
4.
S. C. Mojumdar L. Raki N. Mathis K. Schimdt S. Lang 《Journal of Thermal Analysis and Calorimetry》2006,85(1):119-124
A non-ionic polymer (poly(vinyl
alcohol) (PVA)) has been incorporated into the inorganic layers of calcium
silicate hydrate (C–S–H) during precipitation of quasicrystalline
C–S–H from aqueous solution. C–S–H and a C–S–H-polymer
nanocomposite (C–S–HPN) material were synthesized and characterized
by X-ray fluorescence (XRF), energy dispersive spectroscopy (EDS), 29Si
magic angle spinning nuclear magnetic resonance (29Si
MAS NMR) and 13C cross-polarization nuclear magnetic
resonance (13C CP NMR) spectroscopy, atomic force
microscopy (AFM), thermal conductivity, thermogravimetric analysis (TG) and
differential thermal analysis (DTA). Thermal conductivity of PVA, C–S–H
and C–S–HPN material was studied in the temperature range 25–50°C.
C–S–HPN materials exhibited the highest thermal conductivity at
25 and 50°C. The thermal conductivity increases from 25 to 50°C are
7.03, 17.46 and 14.85% for PVA, C–S–H and C–S–HPN
material, respectively. Three significant decomposition temperature ranges
were observed on the TG curve of C–S–HPN material. 相似文献
5.
Several calcium silicate hydrate (C–S–H)-polymer nanocomposite
(C–S–HPN) materials have been prepared by incorporating poly(acrylic
acid) (PAA) into the inorganic layers of C–S–H during precipitation
of quasicrystalline C-S-H from aqueous solution. The synthetic C–S–HPN
materials were characterized by X-ray fluorescence (XRF), X-ray diffraction
(XRD), Fourier-transform infrared (FTIR) spectroscopy, scanning electron microscopy/energy
dispersive spectroscopy (SEM-EDS), thermogravimetry (TG), differential thermogravimetry
(DTG) and differential scanning calorimetry (DSC). The XRD peaks of C–S–HPN
materials suggest the intermediate organizations presenting both intercalation
of PAA and exfoliation of C–S–H. The SEM images of C–S–H
and C–S–HPN materials with different PAA contents exhibit the
significant differences in their morphologies. Effects of the material compositions
on the thermal stability of series of C–S–HPN materials along
with PAA and C–S–H has been studied by TG, DTG and DSC. Three
significant decomposition temperature ranges were observed on the TG curves
of all C–S–HPN materials. 相似文献
6.
Zou Hantao Yi Changhai Wang Luoxin Liu Hongtao Xu Weilin 《Journal of Thermal Analysis and Calorimetry》2009,97(3):929-935
Thermogravimetric (TG), differential thermal analysis (DTA) and thermal degradation kinetics, FTIR and X-ray diffraction (XRD)
analysis of synthesized glycine–montmorillonite (Gly–MMT) and montmorillonite bound dipeptide (Gly–Gly–MMT) along with pure
Na–MMT samples have been performed. TG analysis at the temperature range 25–250 °C showed a mass loss for pure Na–MMT, Gly–MMT
and Gly–Gly–MMT of about 8.0%, 4.0% and 2.0%, respectively. DTA curves show the endothermic reaction at 136, 211 and 678 °C
in pure Na–MMT whereas Gly–MMT shows the exothermic reaction at 322 and 404 °C and that of Gly–Gly–MMT at 371 °C. The activation
energies of the first order thermal degradation reaction were found to be 1.64 and 9.78 kJ mol−1 for Gly–MMT and Gly–Gly–MMT, respectively. FTIR analyses indicate that the intercalated compounds decomposed at the temperature
more than 250 °C in Gly–MMT and at 250 °C in Gly–Gly–MMT. 相似文献
7.
Summary The simultaneous quantitation of acids and sugars as their trimethyl silyl (TMS) derivatives has been extended in order to
identify and quantitate the simple acid and sugar constituents in the hydrolyzates of various immunostimulant, water-soluble
polysaccharides obtained from various Basidiomycetes, such as Armillariella mellea, Auricularia auricula-judae, Coriolus versicolor,
Flammulina velutipes, Fomes fomentarius, Ganoderma applanatum, Ganoderma lucidum, Pleurotus ostreatus, Schizophyllum commune,
Trametes hirsuta. Optimum hydrolysis conditions, performed with 2 M trifluoroacetic acid (TFAA) for five hrs, proved the presence
of several sugars and acids with maximum recovery. (i) the total sugar/sugar alcohol content of polysaccharides varied between
20- and 65% and consisted of arabitol (0.01–10.2%), arabinose (0.09–1.3%), ribose (0.2–1.8%), fucose (0.3–1.2%), mannitol
(0.01–5.3%), sorbitol (0.01–0.05%), galactiol (0.04%), fructose (0.08–0.8%), galactose (0.9–29%), glucose (10–53%), uronic
acids (0.14–3.7%), sucrose (0.03–2%), trehalose (0.2–1%), cellobiose (0.01–0.6%), maltose (0.2–1.9%), other disaccharides
(0.2–8%). (ii) The total of acids varied from 1.5 to 30% including o-phosphoric (1.3–19%), malic (0.08–4.7%), citric (0.08–4.7%),
isocitric; (3%) and C16−C18 fatty acids (1–6%). 相似文献
8.
Jerzy Jurczyk Rafał Sitko Beata Zawisza Franciszek Buhl Ewa Malicka 《Mikrochimica acta》1999,132(1):41-47
A simple and quick method of durable samples preparation by the thin layer method through direct digesting of the analysed
material on the substrate has been presented. Four- and three-component mono- and polycrystals have been analysed. Standards
have been used in calibration containing: Cr, Co, Ni, Cu, Zn, Ga, Se, Sb, Yb. To improve the correlation between the concentration
and the fluorescent radiation models of mathematical corrections have additionally been used: multiple linear regression,
Lucas-Tooth-Pyne model (L. T. P.) and de Jongh model (d. J.).
Statistical parameters: detection limits for 0.5 mg samples: Cr–0.041%, Co–0.034%, Ni–0.042%, Cu–0.053%, Zn–0.054%, Ga–0.057%,
Se–0.057%, Sb–0.113%, Yb–0.077%. Correlation coefficients: simple regression 0.9946–0.9997, multiple regression 0.9974–1.0000,
L. T. P. 0.9993–1.0000, d. J. 0.9995–1.0000.
Received August, 1, 1998. Revision March 25, 1999. 相似文献
9.
Geoff Rayner-Canham 《Foundations of Chemistry》2011,13(3):223-232
As part of a series of contributions on patterns in the periodic table, the relationships among the transition metals are
examined here in a systematic manner. It is concluded that the traditional method of categorizing transition elements by group
or by period is not as valid as by using combinations thereof. From chemical similarities, it is proposed that the transition
metals be considered as the [V–Cr–Mn] triad; the [Fe–Co–Ni–Cu] tetrad; the [Ti–Zr–Hf–Nb–Ta] pentad; the [Mo–W–Tc–Re] tetrad;
and the [Ru–Os–Rh–Ir–Pd–Pt–Au] heptad. Silver does not fit neatly in anywhere and is better linked with thallium. 相似文献
10.
Complexes of cell–THPC–urea–ADP with transition metal ion Co2+ and lanthanide metal ions such as La3+, Ce4+, Nd3+ and Sm3+ have been prepared. The thermal behavior and smoke suspension of the samples are determined by TG, DTA, DTG and cone calorimetry.
The activation energies for the second stage of thermal degradation have been obtained by following Broido equation. Experimental
data show that for the complexes of cell–THPC–urea–ADP with the metal ions, the activation energies and thermal decomposition
temperatures are higher than those of cell–THPC–urea–ADP, which shows these metal ions can increase the thermal stability
of cell–THPC–urea–ADP. Moreover, these lanthanide metal ions can more increase thermal stability of samples than do the transition
metal ion Co2+. The cone calorimetry data indicate that the lanthanide metal ions, similar to transition metal Co2+, greatly decrease the smoke, CO and CO2 generation of cell–THPC–urea–ADP, which can be used as smoke suppressants. 相似文献
11.
1,2,4-triazole-3-one (TO) and guanidine nitrate (GN) have the potential to be used as alternative gas-generating agents. To
obtain a better understanding of thermal decomposition properties of TO/GN mixtures, sealed cell differential scanning calorimetry,
thermogravimetry–differential thermal analysis–infrared spectroscopy (TG–DTA–IR), and thermogravimetry–differential thermal
analysis–mass spectrometry (TG–DTA–MS) were carried out. The endothermic peak and onset temperatures of TO/GN mixtures were
lower than those of individual TO and GN. TG–DTA–IR and TG–DTA–MS showed that the mass of TO/GN mixtures decreased with heat
generation and N2 evolved as the major gas during thermal decomposition. The interaction between TO and nitric acid from the dissociation of
GN is proposed for the thermal decomposition of TO/GN mixtures. 相似文献
12.
S. F. Malysheva N. K. Gusarova N. A. Belogorlova A. M. Nalibayeva S. V. Yasko N. A. Chernysheva S. I. Verkhoturova G. K. Bishimbayeva B. A. Trofimov 《Russian Journal of General Chemistry》2020,90(2):229-234
Bis(polyfluoroalkyl) chlorophosphites and polyfluoroalkyl dichlorophosphites react easily with secondary amines (from –40 to –22°C, 1–3 h, CH2Cl2) in the presence or absence of triethylamine to form the corresponding bis(polyfluoroalkyl) diorganylamidophosphites or bis(diorganylamido) polyfluoroalkyl phosphites in the yield of up to 74%. Bis(polyfluoroalkyl) diorganylamidophosphites were also synthesized from diorganylamidodichlorophosphites and polyfluoroalkanols (–25 to –22°C, 2 h, Et3N–CH2Cl2) with a yield of 56–60%. 相似文献
13.
C. Perruchot M. M. Chehimi M. Delamar E. Cabet-Deliry B. Miksa S. Slomkowski M. A. Khan S. P. Armes 《Colloid and polymer science》2000,278(12):1139-1154
Thin chloride-doped polypyrrole films (PPyCl) were deposited chemically onto untreated and silane-treated planar glass plates
from aqueous solutions. The organosilanes used to treat the glass substrates were methyltriethoxysilane (Cl), propyltrimethoxysilane
(C3), octyltrimethoxysilane (C8) and aminopropyltriethoxysilane (APS). The decreasing order of hydrophobic character of silane-treated
glass slides, as measured by water contact angle measurements, was glass–APS ≅ glass–C8 > glass–C3 > glass–C1 > glass. X-ray
photoelectron spectroscopy was used to determine the surface chemical composition of the glass plates before and following
coating with the silane coupling agents and/or the PPy thin layer, respectively. The attenuation in intensity of the glass
Na1
s
peak enabled the average thickness of the various organosilane overlayers to be estimated. Atomic force microscopy showed
that the morphology of the organosilane overlayers was islandlike. The domains have a structure which depends upon the nature
of the organosilane in question. Scanning electron microscope images showed that the morphology of the PPyCl thin films was
homogeneous when coated onto glass–APS and glass–C8, but wrinkled at the surface of glass, glass–C1 and glass–C3 plates. Qualitative
peel tests using 3M adhesive tape showed very good adhesion of PPyCl to the glass–APS substrate, whereas adhesion was fairly
poor in the case of glass–PPy and PPy–alkylsilane–glass interfaces. The results of this multitechnique study suggest that
hydrophobic interactions are important to obtain homogeneous and continuous thin PPy films, but Lewis acid–base interactions
are the driving forces for strong and durable PPy–glass adhesion.
Received: 3 January 2000/Accepted: 19 May 2000 相似文献
14.
Mol HG Rooseboom A van Dam R Roding M Arondeus K Sunarto S 《Analytical and bioanalytical chemistry》2007,389(6):1715-1754
The ethyl acetate-based multi-residue method for determination of pesticide residues in produce has been modified for gas
chromatographic (GC) analysis by implementation of dispersive solid-phase extraction (using primary–secondary amine and graphitized
carbon black) and large-volume (20 μL) injection. The same extract, before clean-up and after a change of solvent, was also
analyzed by liquid chromatography with tandem mass spectrometry (LC–MS–MS). All aspects related to sample preparation were
re-assessed with regard to ease and speed of the analysis. The principle of the extraction procedure (solvent, salt) was not
changed, to avoid the possibility invalidating data acquired over past decades. The modifications were made with techniques
currently commonly applied in routine laboratories, GC–MS and LC–MS–MS, in mind. The modified method enables processing (from
homogenization until final extracts for both GC and LC) of 30 samples per eight hours per person. Limits of quantification
(LOQs) of 0.01 mg kg−1 were achieved with both GC–MS (full-scan acquisition, 10 mg matrix equivalent injected) and LC–MS–MS (2 mg injected) for
most of the pesticides. Validation data for 341 pesticides and degradation products are presented. A compilation of analytical
quality-control data for pesticides routinely analyzed by GC–MS (135 compounds) and LC–MS–MS (136 compounds) in over 100 different
matrices, obtained over a period of 15 months, are also presented and discussed. At the 0.05 mg kg−1 level acceptable recoveries were obtained for 93% (GC–MS) and 92% (LC–MS–MS) of pesticide–matrix combinations. 相似文献
15.
The poly(glycidyl methacrylate) adsorbents P(GMA–EDMA) and P(GMA–DVB) were synthesized by the radical suspension–polymerization
method and farther coupled by oligo-β-cyclodextrin (CDP) to obtain P(GMA–EDMA)–CDP and P(GMA–DVB)–CDP. The synthesized polymeric
media were characterized by Fourier transform infrared (FTIR) spectrometer, scanning electron microscopy, and BET surface
area. The adsorption of puerarin from aqueous solution onto the four media, i.e., P(GMA–EDMA), P(GMA–DVB), P(GMA–EDMA)–CDP,
and P(GMA–DVB)–CDP, was studied. An enhanced adsorption of puerarin apparently presented on grafted media. The interaction
between the polymeric media and the puerarin was researched by FTIR. The result shows that the adsorption efficiency on P(GMA–DVB)–CDP
driven by multiple weak interactions is much higher than that on P(GMA–EDMA) driven by hydrogen bonding interaction only and
on P(GMA–DVB) or P(GMA–EDMA)–CDP driven by two interactions. 相似文献
16.
Ahmed A. Abd El-Raady Nasr E. Fouad Mohamed A. Mohamed Samih A. Halawy 《Monatshefte für Chemie / Chemical Monthly》2002,133(10):1351-1361
Summary. Selective decomposition of ethanol was used as a test reaction at 350°C to evaluate the catalytic activity of two Al–Mg–O
mixed oxides prepared by two different methods (wet impregnation and coprecipitation). The catalyst precursors were examined
by TG and DTA and were calcined between 500–900°C for 5 h in air. The surface area of all catalysts was measured by N2 sorption using the BET method. The total acidity and basicity were determined by TPD using pyridine and formic acid. The
catalysts were characterized by XRD analysis. It was found that the preparation method of Al–Mg–O catalyst has a great effect
on the selective decomposition of ethanol. Al–Mg–O (I) catalysts, prepared by wet impregnation, were more selective towards
ethene formation during dehydration of ethanol. This is ascribed to their high total surface acidity. On the other hand, Al–Mg–O
(II) catalysts, prepared by coprecipitation, were highly selective in the oxidative dehydrogenation of ethanol to yield acetaldehyde.
This could be attributed to their high concentration of basic sites. In addition, the production of traces of diethyl ether
was also observed (three times more for Al–Mg–O (II) than for Al–Mg–O (I)).
Corresponding author. E-mail: shalawy99@yahoo.com
Received October 12, 2001. Accepted (revised) January 7, 2002 相似文献
17.
Ultrasonic slurry sampling electrothermal vaporization dynamic reaction cell inductively coupled plasma mass spectrometry
(USS–ETV–DRC–ICP–MS) for the determination of Cr, Cd and Pb in several plastic samples, using NH4NO3 as the modifier, is described. The influences of the instrumental operating conditions and the slurry preparation technique
on the ion signals are investigated. A reduction in the intensity of the background at signals corresponding to chromium masses
(arising from matrix elements) was achieved by using NH3 as the reaction cell gas in the DRC. The method was applied to determine Cr, Cd and Pb in two polystyrene (PS) samples and
a polyvinyl chloride (PVC) sample using two different calibration methods, namely standard addition and isotope dilution.
The results were in good agreement with those for digested samples analyzed by ultrasonic nebulization DRC–ICP–MS. The precision
between sample replicates was better than 17% with the USS–ETV–DRC–ICP–MS method. The method detection limits, estimated from
standard addition curves, were about 6–9, 1–2 and 8–11 ng g−1 for Cr, Cd and Pb, respectively, in the original plastic samples. 相似文献
18.
This study reports in detail the results of systematic large-scale theoretical investigations of the acidic dimeric structural
units (D–E, E–F, F–G, and G–H) and pentamer D–E–F–G–H (fondaparinux) of the glycosaminoglycan heparin, and their anionic forms.
The geometries and energies of these oligomers have been computed using HF/6–31G(d), Becke3LYP/6–31G(d), and Becke3LYP/6–311+G(d,p)
methods. The optimized geometries indicate that the most stable structure of these units in the neutral state is stabilized
via a system of intramolecular hydrogen bonds. The equilibrium structure of these species changed appreciably upon dissociation.
Water has a remarkable effect on the geometry of the anions studied. Because of high negative charge, the solvent effect also
resulted in an appreciable energetic stabilization of biologically active anionic forms of these glycosaminoglycans. The stable
energy conformations around glycosidic bonds found for dimers and pentamer investigated are compared and discussed with the
available experimental X-ray structural data for the structurally related heparin-derived pentasaccharides in cocrystals with
proteins. 相似文献
19.
Ruixia Gao Junjie Zhang Xiwen He Langxing Chen Yukui Zhang 《Analytical and bioanalytical chemistry》2010,398(1):451-461
We report the use of nanospheres prepared by coating silica with molecularly imprinted polymer (MIP) for sulfamethoxazole
(SMO). The resulting SiO2–SMO–MIP nanoparticles have highly improved imprinting and adsorption capacity, and can be used for separation and determination
of sulfonamides in eggs and milk. In the synthesis, monodispersed SiO2 nanoparticles (Si–NP) of diameter 80 nm were amino-modified by reaction with 3-aminopropyltriethoxylsilane. The acryloyl
monolayer was then grafted onto the amine-modified Si–NP. Finally, the MIP films were coated on to the surface of Si–NP by
the copolymerization of the vinyl end groups with functional monomer (acrylamide), cross-linking agent (ethylene glycol dimethacrylate),
initiator (azo-bis-isobutyronitrile), and template molecule (sulfamethoxazole). The resulting SiO2–SMO–MIP–NP were characterized by transmission electron microscopy, scanning electron microscopy, and Fourier transform infrared
spectrometry. The adsorption properties were demonstrated by equilibrium rebinding experiments and Scatchard analysis. The
results showed that the binding sites of the SiO2–SMO–MIP were highly accessible, and the maximum adsorption capacity of the SiO2–SMO–MIP for SMO was 20.21 mg g−1. The selectivity of the SiO2–SMO–MIP–NP obtained was elucidated by using SMO and structurally related sulfonamides. The results indicated that the SiO2–SMO–MIP had significant selectivity for SMO. The feasibility of removing SMO and sulfadiazine (SDZ) from food samples was
proved by use of spiked milk and eggs. A method for the separation and determination of trace SMO and SDZ in milk and egg
samples was developed, with recoveries ranging from 69.8% to 89.1%. 相似文献
20.
Liviu V. Costea Vasile N. Bercean Valentin Badea Klaus Gerdes Ulrich Jordis 《Monatshefte für Chemie / Chemical Monthly》2006,8(2):737-744
1H-3-Methyl-4-ethoxycarbonyl-5-(benzylidenehydrazino)pyrazoles are key intermediates in obtaining various heterocyclic systems
including pyrazolotriazoles. We present the voltammetric behavior of these compounds in nonaqueous media, with the following
para substituents grafted on the benzene ring: –N(CH3)2, –OH, –OCH3, –F, –Cl, –CF3, –NO2, as well as of the novel compounds with –Br, –I, and –SCH3 in the para position, in order to elucidate the influence of the various substituents on the mechanism of anodic oxidation. 相似文献