This article describes the synthesis of a liquid crystalline curing agent 4,4′-bis-(4-amine-butyloxy)-biphenyl (BABB), and its application as a curing agent for the epoxy resin (DGEBA) in comparison with normal curing agent, 4,4′-diaminobiphenyl (DABP). BABB was investigated with polarized optical microscopy, differential scanning calorimetry, and small-angle X-ray scatting, and the results showed that BABB displayed smectic liquid crystalline phase. The curing behaviors of DGEBA cured with BABB and DABP were studied by using differential scanning calorimetry (DSC), polarized optical microscopy (POM), and dynamic mechanical analysis (DMA). The results indicated that BABB showed a higher chemical reactivity than DABP. The kinetics was studied under isothermal conditions using an isoconversional method, and the isothermal DSC data can be fitted reasonably by an autocatalytic curing model. The nematic droplet texture was observed for the resulting polymer network of DGEBA/BABB system, while the DGEBA/DABP system showed an isotropic state. The storage modulus of DGEBA/BABB system was enhanced in comparison with DGEBA/DABP system because of the formation of LC phase, whereas the glass transition temperatures decreased because of the introduction of flexible spacer group.
This article described the synthesis and mesomorphic behavior transition of a novel liquid crystalline (LC) epoxy resin 4-(2,3-epoxypropoxy)biphenyl,4″-(2,3-epoxypropoxy)phenyl-4′carboxylate (EBEPC), which combined a hydroxyl benzoic aromatic ester and biphenol rigid-rod group. EBEPC showed a clear nematic schlieren texture under curtain conditions. The reaction kinetics of EBEPC cured by 4,4′-diaminodiphenyl-methane (DDM) was studied by using an isoconversional method under isothermal conditions with differential scanning calorimetry (DSC). The isothermal DSC data can be fitted reasonably by an autocatalytic curing model. Smectic phases had been observed in the EBEPC/DDM curing system. The results of DSC showed that the formation of the LC phase had pronounced influence on the curing reaction.
Authors:Rong Zhang, Yongde Yue, Rimao Hua, and Wen Yan
The phthalate esters (PAE) are ubiquitous in the environment because of the widespread use of plastic products. Reports of their harm to the environment and to human beings are increasing. This paper reports, for the first time as far as we are aware, use of HPTLC to separate and quantify PAE. The HPTLC assay enables separation of four PAE-dimethyl phthalate (DMP), diethyl phthalate (DEP), di-
-butyl phthalate (DBP), and bis-(2-ethylhexyl) phthalate (DEHP), priority pollutants listed by EPA- and qualitative and quantitative analysis of the compounds in water. The factors affecting the separation were investigated, including use of different stationary and mobile phases, different methods of development, humidity, and presaturation, or not, of the plate. The method was evaluated with water fortified at 5, 1, and 0.5 μg L
. It was then applied to detection of the compounds in water from Lake Chaohu. The assay was fully validated and shown to be sensitive (LOD ≤7 ng, LOQ 0.1 μg L
on HPTLC plates), accurate (recovery ≥80%), and precise (intra-day variation ≤8.7%, interday variation ≤6.7%). The results obtained by extraction using different solvents were compared. It was shown that dichloromethane was suitable for extraction of the four target substances from water.
Authors:Feng Tang, Shimei Ge, Yongde Yue, Rimao Hua, and Rong Zhang
A high-performance thin-layer chromatographic method has been developed for determination of four carbamate residues in vegetables. The method uses two mobile phases on silica gel 60 F
GLP HPTLC layers, and detection at
= 243 nm and 207 nm, the average wavelengths of maximum adsorption of pirimicarb and methomyl, and carbaryl and carbofuran, respectively. Recovery of 1.0–5.0 mg kg
of the four mixed carbamates from wax gourd and potatoes was 70.05–103.7%. The accuracy and precision of the method were confirmed by means of fortification experiments.
Authors:Shimei Ge, Feng Tang, Yongde Yue, Rimao Hua, and Rong Zhang
Residues of three pyrethroids in spiked vegetables have been analyzed by HPTLC with two mobile phases in a twin-trough chamber and in horizontal chambers. The spots were detected at
= 203 nm and the greatest detection sensitivity for the three pyrethroids was 10 ng. Recovery after fortification at 0.5–5.0 mg kg
was from 70.20 to 108.5%. The relative standard deviation was 1.59–27.94%.
Authors:Qing Guo, Yan Huang, Yu-Ying Zhang, Li-Rong Zhu, and Bao-Long Zhang
A new homologous series of curing agents (LCECAn) containing 4,4′-biphenyl and n-methylene units (n = 2, 4, 6) were successfully synthesized. The curing behaviors of a commercial diglycidyl ether of bisphenol-A epoxy (E-51) and 4,4′-bis(2,3-epoxypropoxy)biphenyl (LCE) by using LCECAn as the curing agent have been investigated by differential scanning calorimetry (DSC), respectively. The Ozawa equation was applied to the curing kinetics based upon the dynamic DSC data, and the isothermal DSC data were fitted using an autocatalytic curing model. The glass transition temperatures (Tg) of the cured epoxy systems were determined by DSC upon the second heating, and the thermal decomposition temperatures (Td) were obtained by thermogravimetric (TG) analyses. The results show that the number of methylene units in LCECAn has little influence on the curing temperatures of E-51/LCECAn and LCE/LCECAn systems. In addition, the activation energies obtained by the dynamic method proved to be larger than those by the isothermal method. Furthermore, both the Tg and Td of the cured E-51/LCECAn systems and LCE/LCECAn systems decreased with the increase in the number of methylene units in LCECAn.
Authors:Xue Zhi-Len, Tan Ming-Guang, Zhang Jia-Din, and Bao Jin-Rong
The determination of calcium in yttrium oxide through the40Ca(α, p)43Sc reaction was studied, using a post-irradiation radiochemical separation procedure. The half-life of43Sc was determined to be 3.87 hr. The chemical recovery was about 70%. The detection limit was about 10 ppb, for a 30 min irradiation
at an alpha-particle beam current of 1 μA (Eα=13.4 MeV) and γ−γ coincidence counting (background counts being<1, cpm), with counting starting at 4 hours after the end
of irradiation. Four samples of a batch of yttrium oxide (A.R.) were analyzed, and found to contain 13.9±1.0 ppm of calcium.
Authors:Yang Yan-Zhao, Sun Si-Xiu, Zhang Lei, Yang Yong-Hui, and Bao Bo-Rong
The liquid-liquid extraction of uranium(VI) from aqueous nitric acid with bis(octylsulfinyl)methane (BOSM) has been studied
over a wide range of conditions. The extracted species appear to be UO2(NO3)2·2BOSM. It was found that the extraction increased with increasing nitric acid concentration up to 8.5 mol/l and then descreased.
Extraction also increased with increasing extractant concentration. The influence of temperature and salting-out agent concentration
on the extraction equilibrium has also been investigated, and the enthalpy of the extraction reaction was estimated.
Authors:Mao Jia-Jun, Chen Yu-De, Zhang Gui-Rong, and Zhou Zu-Ming
A study on the synergistic extraction of uranium(VI) from nitric acid media with double-chelating agent systems 1-phenyl-3-methyl-4-benzoyl-pyrazolone-5 (PMBP) plus thenoyltrifluoroacetone (TTA), and 1-phenyl-3-methyl-4-benzoyl-pyrazolone-5 plus 1-phenyl-3-methyl-4-trifluoroacetyl-pyrazolone-5 (PMTFP) is described. Some synergistic effects have been observed. The experimental results suggest that the composition of synergistic complex species is UO2PMBP·TTA and UO2PMBP·PMTFP, respectively. The equilibrium constants for these synergistic extractions are calculated by three methods and the mechanism and the regularity of extraction are discussed as well.
Authors:Rong Zhang, Yongde Yue, Rimao Hua, Feng Tang, Haiqun Cao, and Shimei Ge
In this work we have studied the separation of a mixture of the sulfonylurea herbicides (metsulfuron-methyl, chlorsulfuron, bensulfuron-methyl, tribenuron, chlorimuron-ethyl) by HPTLC on silica gel F
plates, with two different mobile phases. We also studied the effect of humidity on the separation. Bensulfuron-methyl added to tapwater at levels of 5, 10, and 20 µg kg
were determined after extraction by LC
SPE. Detection limits of the method are given.