This work reported on the thermal decomposition of ammonium perchlorate activated by addition of NiO nanocrystals with different
surface areas. NiO samples were characterized by X-ray diffraction (XRD), transition electron microscope (TEM), Brunauer-Emmett-Teller
(BET) technique, Fourier transform infrared spectroscopy (FTIR), and Raman spectroscopy. With increasing annealing temperature,
the surface areas of NiO samples reduced from 108.6 to 0.9 m2 g−1. The catalytic activities of NiO nanocrystals on the thermal decomposition of ammonium perchlorate were investigated by thermogravimetric
analysis (TG) coupled with differential thermal analysis (DTA). With addition of NiO nanocrystals, thermal decomposition temperature
of AP decreased greatly. Larger surface areas of NiO nanocrystals promoted the thermal decomposition of AP.
CuO nanocrystals of different surface areas were prepared. All samples were characterized by X-ray diffraction, transition
electron microscope, thermogravimetry, Brunauer-Emmett-Teller technique, Fourier transform infrared spectroscopy, and Raman
spectroscopy. CuO nanocrystals showed a stable monoclinic structure. With increasing surface areas, the surface hydration
became significant, which is followed by shifts in infrared frequencies and Raman phonon modes. CuO nanocrystals were explored
as an additive to catalytic decomposition of ammonium perchlorate (AP). AP decomposition underwent a two-stage process. Addition
of CuO nanocrystals led to a downshift of high-temperature stage towards lower temperatures.
Two rapid, sensitive and reproducible methods for the determination of baclofen(BAL) in urine and plasma based on high-performance liquid chromatography (HPLC) with UV-vis and fluorescent detection, respectively, were developed for the first time using a new synthesized fluorescent label, 6-oxy-(N-succinimidylacetate)-9-(2′-methoxycarbonyl) fluorescein (SAMF). The optimal derivatization yield was achieved in borate buffer (pH 8.0) for 15 min at room temperature (25 °C). With a mixture of methanol and water containing 5 mmol L−1 sodium citrate buffer (pH 5.0) as mobile phase, BAL was determined at λ = 455 nm with UV-vis detection and at λex/λem = 488/520 nm with FD detection. The detection limits are 1.065 × 10−3 mg mL−1 and 1.065 × 10−2 mg mL−1 with HPLC-UV-vis and HPLC-FD, respectively. The proposed method has been successfully applied to the analysis of BAL in human urine and plasma samples. The established method is rapid (15 min of derivatization process and 10 min of chromatographic run), reproducible and sensitive.
Synthesis, characterization and thermal analysis of polyaniline (PANI)/ZrO2 composite and PANI was reported in our early work. In this present, the kinetic analysis of decomposition process for these
two materials was performed under non-isothermal conditions. The activation energies were calculated through Friedman and
Ozawa-Flynn-Wall methods, and the possible kinetic model functions have been estimated through the multiple linear regression
method. The results show that the kinetic models for the decomposition process of PANI/ZrO2 composite and PANI are all D3, and the corresponding function is ƒ(α)=1.5(1−α)2/3[1−(1-α)1/3]−1. The correlated kinetic parameters are Ea=112.7±9.2 kJ mol−1, lnA=13.9 and Ea=81.8±5.6 kJ mol−1, lnA=8.8 for PANI/ZrO2 composite and PANI, respectively.
A reversed-phase high-performance liquid chromatographic method was developed for the first time to simultaneously determine salicin and eight flavonoids in leaves of Salix matsudana, that is salicin, luteolin-7-O-glucoside, myricetin, apigenin-3′-oxyethyl-7-O-glucoside, rutin, quercetin, luteolin, kaempferol and apigenin. The separation of these compounds was achieved on a reversed phase C18 column (250 × 4.6 mm, 5 μm), with linear gradient of methanol in 0.2% phosphoric acid solution with a flow rate of 1.0 mL/min with UV detection at 246 nm. The calibration curves for the determination of all analytes showed good linearity over the investigated ranges (r > 0.999). The % relative standard deviation (% RSD) values were less than 0.34%, and the recoveries were between 95.79% and 99.94%. The values of luteolin-7-O-glucoside, salicin, myricetin, apigenin-3′-oxyethyl-7-O-glucoside, rutin, quercetin, luteolin, kaempferol, and apigenin were 1.0 μg g−1, 20.0 μg g−1, 32.9 μg g−1, 2.0 μg g−1, 29.5 μg g−1, 6.0 μg g−1, 1.0 μg g−1, 3.5 μg g−1, and apigenin was not found in the sample. This developed method can be used for evaluating the quality of different plant materials.
The flux of cold neutrons that is obtainable from various high energy netron sources is studied for a particular model of
a cold neutron source when the cold moderation region of the apparatus is at 20, 70, and 298K. The maximum flux obtained with
a californium-252 source was 2.7·10−3 cold neutron per (cm2·second (source neutron)). This flux was obtained when the cold moderation region of the apparatus was at 20K and when the
thermal moderator is either polyethylene or trimethylbenzene and the cold moderator is polyethylene. This flux should allow
sensitive prompt and delayed neutron activation analysis measurements.
Authors:J.R. Li, D.X. Li, L. Li, W.L. Deng, L.S. Ding, H.X. Xu, and Y. Zhou
A rapid and sensitive ultraperformance liquid chromatography-multiple reaction monitoring-multi-stage/mass spectrometry (UPLC-MRM-MS/MS) method has been developed for simultaneous quantification of salvianolic acid B and tanshinone IIA of salvia tropolone tablets in dog plasma. This was achieved by performing quantification using the MRM acquisition with two channels of MRM-MS/MS and MS full scan for more accuracy qualitative results, and the fragmentation transitions of m/z 295→249, 191 for tanshinone IIA and m/z 297→279, 251 for IS in positive mode, m/z 717→519, 321 for salvianolic acid B and m/z 295→267, 239 for IS in negative mode were selected. The UPLC separation was achieved within 3 min in a single UPLC run. Linear calibration curves were obtained over the concentration range of 10 pg/mL−1 ng/mL for tanshinone IIA and 100 pg/mL−1 for salvianolic acid B. Lower limit of quantitation (LLOQ) was 10 pg/mL and 100 pg/mL for tanshinone IIA and salvianolic acid B, respectively. The inter-day and intra-day precision (relative standard deviation, RSD) in all samples were less than 8.21%, and the recoveries were over 85.9% for both tanshinone IIA and salvianolic acid B. The two channels of MRM with MS full scan approach could provide both qualitative and quantitative results without the need for repetitive analyses and resulted in the reduction of further confirmation experiments and analytical time. The pharmacokinetic study of the two active components of salvia tropolone tablets following oral gavage administration of dogs was thus explored with this method.
Authors:Y. Li, G. Fei, H. Xingen, L. Ruisen, and L. Zhen
Enthalpies of dilution at 298.15 K of aqueous solutions of THF and 1,4-dioxane have been determined using flow microcalorimetry.
The results obtained were used to determine the homotactic enthalpic interaction coefficients that characterize pair interactions
of THF and 1,4-dioxane in aqueous solution. These are briefly discussed from the point of view of intermolecular interaction
between the hydrated solute species.
Authors:L. Li, X. Wang, J. Shen, L. Zhou, and T. Zhang
Adsorption microcalorimetry has been employed to study the interaction of ethylene with the reduced and oxidized Pt-Ag/SiO2catalysts with different Ag contents to elucidate the modified effect of Ag towards the hydrocarbon processing on platinum
catalysts. In addition, microcalorimetric adsorption of H2, O2, CO and FTIR of CO adsorption were conducted to investigate the influence of Ag on the surface structure of Pt catalyst.
It is found from the microcalorimetric results of H2and O2adsorption that the addition of Ag to Pt/SiO2leads to the enrichment of Ag on the catalyst surface which decreases the size of Pt surface ensembles of Pt-Ag/SiO2catalysts. The microcalorimetry and FTIR of CO adsorption indicates that there still exist sites for linear and bridged CO
adsorption on the surface of platinum catalysts simultaneously although Ag was incorporated into Pt/SiO2. The ethylene microcalorimetric results show that the decrease of ensemble size of Pt surface sites suppresses the formation
of dissociative species (ethylidyne) upon the chemisorption of C2H4on Pt-Ag/SiO2. The differential heat vs. uptake plots for C2H4adsorption on the oxygen-preadsorbed Pt/SiO2and Pt-Ag/SiO2catalysts suggest that the incorporation of Ag to Pt/SiO2could decrease the ability for the oxidation of C2H4.
The dilution enthalpies of D-mannitol and D-sorbitol in aqueous sodium chloride solution at various concentrations have been determined by isothermal microcalorimetry
at 298.15 K. The homogeneous enthalpic interaction coefficients over a quite large range of concentration of aqueous sodium
chloride solutions have been calculated according to the excess enthalpy concept. The results show that enthalpic pairwise
interaction coefficients (h2) of D-mannitol and D-sorbitol are positive in aqueous sodium chloride solution and become more positive with increase of the concentration of
sodium chloride. The results are interpreted in terms of the different conformations of the two polyols, solute-solute and
solute-solvent interactions involved by solvent effects.