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431.
Simultaneous determination of trace migration of phthalate esters in honey and royal jelly by GC–MS
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Jinhui Zhou Yitao Qi Hongmei Wu Qingyun Diao Feifei Tian Yi Li 《Journal of separation science》2014,37(6):650-657
A simple, rapid, and reliable liquid–liquid extraction coupled to GC–MS method was developed and validated for the quantification of 22 phthalate esters (PAEs) in honey and royal jelly. Instrument parameters for GC–MS were tested to obtain the satisfactory separation between 22 PAEs with high sensitivity. The extraction procedure was optimized in order to achieve the best recovery. The following criteria were used to validate the developed method: linearity, LOD, lower LOQ, precision, accuracy, matrix effect and carry‐over. Correlation coefficients were >0.999 by applying the linear regression model based on the least‐squares method with a weighting factor (1/x). The intra‐ and interday precision were within 12.7% in terms of RSD, and the accuracy was within ?11.8% in terms of relative error. The mean extraction recoveries ranged between 80.1 and 110.9% for honey and royal jelly. No significant matrix effect and carry‐over for PAEs were observed for the analysis of honey and royal jelly samples. A total of 20 real samples were analyzed for a mini‐survey using the developed method. Seven PAEs in honey samples and five PAEs in royal jelly samples were found, indicating potential contamination with several PAEs. 相似文献
432.
设计并合成了一种交叉共轭的(cross-conjugated)缺电子型聚合物单体——二溴代噻吩[2,3-b]并噻吩-吡咯[3,4-c]并吡咯(DPPTTZ)二酮,并将其分别与噻吩(T)、硒吩(Se)和N-甲基吡咯(Py)的双锡试剂进行共聚反应,获得了一类新的供体-受体(D-A)型共轭聚合物光电材料.这类材料分子的最高占有轨道(HOMO)能级较低,因此其光电器件具有较高的开路电压(Voc),稳定性好.此外,它们在紫外-可见光区有较宽的吸收,最大吸收位于波长620 nm附近;能带隙(band gap)小,分别为1.86 e V(p DPPTTZ-T)、1.83 e V(p DPPTTZ-Se)和1.85 e V(p DPPTTZ-Py).器件初步测试结果表明,上述聚合物与PC71BM组成的本体异质结聚合物太阳能电池Voc在0.68~0.81 V之间,能量转化效率(PCE)最高达3.05%(p DPPTTZ-T). 相似文献
433.
A simple and sensitive chemiluminescence method was developed for the determination of fenfluramine. The chemiluminescence signal arising from the reaction between alkaline luminol and N‐bromosuccinimide was found to be greatly enhanced by fenfluramine in the presence of gold nanoparticles. But fenfluramine alone slightly inhibited the CL signal of N‐bromosuccinimide‐luminol in the absence of gold nanoparticles. The experimental parameters that affected the chemiluminescence signal were thoroughly investigated. Under the optimum experimental conditions, the enhanced chemiluminescence intensity was proportional to the concentration of fenfluramine in the range of 0.005‐1.0 mg/L. The detection limit was 0.9 μg/L fenfluramine with a relative standard deviation of 2.5% for 0.1 mg/L fenfluramine solution (n = 11). The method was applied to the determination of fenfluramine in some weight‐reducing tonics and in spiked human urine. A possible CL reaction mechanism was proposed. 相似文献
434.
435.
大气边界层的风洞模拟 总被引:8,自引:1,他引:8
本文通过比较大气边界层与不同比尺的模型实验,研究了风洞模型实验中的比尺效应。结果表明,大气边界层粗糙高度的比尺应当和边界层厚度比尺相等。边界层厚度的比尺在200~400之间时可以得到最好的速度分布的相似性,表面压强分布主要依赖于边界层比尺而与建筑物几何比尺关系不大。如果正确选择了粗糙高度比尺,扩散系数比尺和边界层厚度比尺相同。 相似文献
436.
An experimental study was conducted to investigate the heat transfer characteristic of a vertical copper plate with rectangular micro-channels. In this research, Cu/R141b nanofluids were used as the working fluid. Three different volume concentrations—0.001, 0.01, and 0.1 %—of Cu nanoparticles with an average diameter of 20 nm dispersed in R141b were prepared. Experiments were performed to measure thermal resistance of the microchannel surface under a steady operating pressure range of 0.86 × 105 Pa to 2 × 105 Pa. Thermal resistance weakened with addition of nanoparticles into the base fluid. The maximum reduction effect of the thermal resistance was 50 %, which corresponds to 0.01 % volume concentration of nanofluid at low operating pressure. The operating pressure significantly affects thermal performance of the microchannel surface. This paper also studied heat transfer characteristics for a Cu nanoparticle-coated surface with rectangular microchannels, which were produced by heating in different volume concentrations from 0.001 to 0.1 %. Nanoparticle layer on the micro-channel surface is responsible for enhanced heat transfer of nanofluids with 0.001 and 0.01 % volume concentrations. 相似文献
437.
利用低官能度的丙烯酸酯单体进行全息液晶/聚合物光栅的制备, 获得了具有聚合物支撑形貌的光栅结构. 由于这种光栅内部不存在液晶微滴, 当作为分布反馈式激光器的谐振腔时, 可以有效降低光栅内部的散射损失(<4%), 降低激光腔损耗. 此外, 选用的高折射率单体提升了光栅的折射率调制量, 增强了光栅的反馈增益. 在以上两种因素的共同作用下, 采用染料DCM为激光工作物质, 以532 nm的Nd:YAG脉冲激光器作为抽运光源, 最终获得了中心波长为635 nm, 转化效率为1.2%的高性能激光, 在以阈值能量0.8 μJ/pulse抽运下获得激光线宽0.3 nm, 较之国内外同类激光器的报道, 在阈值、线宽、转化效率三方面均有不同程度提升. 相似文献
438.
The quantum Fourier transform (QFT) is a powerful tool in quantum computing. The main ingredients of QFT are formed by the Walsh-Hadamard transform H and phase shifts P(·), both of which are 2×2 unitary matrices as operators on the two-dimensional 1-qubit space. In this paper, we show that H and P(·) suffice to generate the unitary group U(2) and, consequently, through controlled-U operations and their concatenations, the entire unitary group U(2n) on n qubits can be generated. Since any quantum computing algorithm in an n-qubit quantum computer is based on operations by matrices in U(2n), in this sense we have the universality of the QFT. 相似文献
439.
A simple, mild and green approach has been developed for the synthesis of asymmetrical heterobiaryls under the irradiation of visible light without any oxidants and promoting reagents through using Pd/CeO2 nanocomposite photocatalyst. This method tolerates considerable functional groups such as electron-donating groups and electron-withdrawing groups through C-C cross-coupling. 相似文献
440.
Pd/Amberlyst-45催化剂催化水相中苯酚选择性加氢制环己酮(英文) 总被引:1,自引:0,他引:1
环己酮是重要的有机化工原料和工业溶剂,是制造尼龙、己内酰胺和己二酸的主要中间体,环己酮的绿色生产工艺受到人们关注.目前全世界环己酮年产量接近900万吨,但环己酮生产仍主要以环己烷为原料,采用富氧空气氧化为环己基过氧化氢,再在铬酸叔丁酯催化剂作用下分解为环己醇和环己酮的混合物,然后经一系列蒸馏精制后得到环己酮、工艺复杂、能耗高,而且设备腐蚀、环境污染及安全问题严重.因此,大量工作正致力于新工艺和新催化剂研究,其中光催化氧化、分子筛催化氧化和金属氧化物催化氧化等都有相关报道,同时还有学者开发了其它环己酮制备新方法,如环己烯水合法、苯加氢法、环己醇氧化法和苯酚加氢法等.苯酚直接选择性加氢合成环己酮研究具有重要意义.苯酚加氢通常有两种工艺,气相加氢和液相加氢,由于液相加氢具有无需将反应物汽化、能耗较低和催化剂反应活性高等优势而受到广泛关注.但是目前大量文献报道的苯酚加氢过程仍需要高温条件且较易产生环己醇和环己烷等副产物,大部分催化反应需在有机溶剂中进行,因此如何提高环己酮选择性,减小环境影响成为近年来的热门课题.在过去数年中,人们筛选了大量催化剂,其中Pd催化剂具有较高活性和目的产物选择性,因为其对羰基表现出较低的催化活性.研究还发现,催化剂载体对苯酚加氢产物分布有重要影响,酸性载体或酸性助剂的加入均能提高苯酚转化率和环己酮选择性,可能的原因是催化剂表面可与苯酚羟基形成O-H…π强相互作用,使苯酚分子更容易吸附在载体表面,而一旦苯酚经催化加氢生成环己酮,由于失去羟基与载体表面相互作用,环己酮更容易从载体表面脱附,从而避免过度加氢生成环己醇,同时酸性位点可以增强Pd的电子密度,提高催化加氢活性.另外,通过添加助剂也可有效改善催化剂性能.然而,到目前为止,通过单一的一种催化剂仍然很难同时实现苯酚的高转化率和环己酮的高选择性.因此,开发新催化剂和简便的生产工艺对环己酮高效高质量生产具有重要意义.本文使用一种多孔、不易溶解的酸性离子交换树脂Amberlyst-45(A-45)为载体,采用简单的浸渍工艺制备了一系列不同Pd负载量的Pd/A-45催化剂,详细考察了催化剂在水相中对苯酚选择性加氢制环己酮的催化活性和选择性,包括反应温度、催化剂用量、反应时间和Pd负载量等对反应活性的影响及催化剂重复使用情况,并且与传统的SiO_2,ZnO,MgO,Al_2O_3和活性炭负载的Pd催化剂进行对比.研究发现,Pd/A-45催化剂在温和反应条件(40-100℃,0.2-1 MPa)下具有极高的催化活性和选择性,在适宜的反应条件下苯酚转化率达到100%,环己酮选择性高于89%.进一步分析由不同活性金属负载量制备的不同粒径Pd/A-45催化剂的活性规律发现,苯酚加氢生成环己酮是一个结构敏感型反应,其中Pd颗粒尺寸为12-14 nm时更有利于环己酮生成. 相似文献