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51.
建立自动石墨消解-电感耦合等离子体质谱法(ICP-MS)同时测定左氧氟沙星胶囊中铅、铬、砷、镉、锡、铝、铁7种金属元素含量的方法。以HNO3-H2O2()体积比为1∶1为消解体系,采用自动石墨消解法消解左氧氟沙星胶囊样品,消解液除酸后,用5%硝酸溶液定容至50 mL,采用电感耦合等离子体质谱法对消解液进行测定,以内标法定量。铅、铬、砷、镉、锡、铝、铁的质量浓度在0.05~20.0μg/mL范围内与质谱响应值成良好的线性关系,相关系数均大于0.998,方法检出限为0.119~1.323μg/kg。样品加标回收率为91.2%~105.5%,测定结果的相对标准偏差为1.67%~3.46%(n=6)。该方法样品前处理简单,检出限低,测定结果准确,适用于左氧氟沙星胶囊等沙星类抗生素中多种金属元素残留的测定。 相似文献
52.
Wei Xu Dr. Karoly Kozma Tianxiang Sha Yi-Jen Wu Prof. May Nyman Prof. Michael M. Lerner 《Chemistry (Weinheim an der Bergstrasse, Germany)》2020,26(36):8101-8104
The alkaline earth metals (M=Mg, Ca, Sr, and Ba) exhibit a +2 oxidation state in nearly all known stable compounds, but MI dimeric complexes with M−M bonding, [M2(en)2]2+, (en=ethylenediamine) of all these metals can be stabilized within the galleries of donor-type graphite intercalation compounds (GICs). These metals can also form GICs with more conventional metal (II) ion complexes, [M(en)2]2+. Here, the facile interconversion between dimeric-MI and monomeric-MII intercalates upon the addition/removal of en are reported. Thermogravimetry, powder X-ray diffraction, and pair distribution function analysis of total scattering data support the presence of either [M2(en)2]2+ or [M(en)2]2+ guests. This phase conversion requires coupling graphene and metal redox centers, with associated reversible M−M bond formation within graphene galleries. This chemistry allows the facile isolation of unusual oxidation states, reveals M0→M2+ reaction pathways, and present new opportunities in the design of hybrid conversion/intercalation materials for applications such as charge storage. 相似文献
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S. Paszkiewicz A. Szymczyk Z. Špitalský M. Soccio J. Mosnáček T. A. Ezquerra Z. Rosłaniec 《Journal of Polymer Science.Polymer Physics》2012,50(23):1645-1652
Nanocomposites based on poly(ethylene terephthalate) (PET) and expanded graphite (EG) have been prepared by in situ polymerization. Morphology of the nanocomposites has been examined by electronic microscopy. The relationship between the preparation method, morphology, and electrical conductivity was studied. Electronic microscopy images reveal that the nanocomposites exhibit well dispersed graphene platelets. The incorporation of EG to the PET results in a sharp insulator‐to‐conductor transition with a percolation threshold (?c) as low as 0.05 wt %. An electrical conductivity of 10?3 S/cm was achieved for 0.4 wt % of EG. The low percolation threshold and relatively high electrical conductivity are attributed to the high aspect ratio, large surface area, and uniform dispersion of the EG sheets in PET matrix. © 2012 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys, 2012 相似文献
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AbstractIn this work, an effective method was developed to prepare novel PEO-b-PPO-b-PEO (EPE)/α-cyclodextrin (α-CD) supramolecular hydrogels containing exfoliated graphite nanoplates (xGNPs) by mixing an aqueous solution of α-CD with an aqueous dispersion of xGNPs at the presence of amphiphilic EPE copolymer. The EPE copolymer played three important roles in the preparation process: (1) as an exfoliating agent to break expanded graphites into xGNPs under ultrasonication, (2) as a dispersant to stabilize xGNPs in the aqueous solution, and (3)as a component to form the inclusion complexes with α-CD. The resultant xGNPs/EPE/α-CD hybridized hydrogels were characterized by scanning electron microscopy, wide-angle X-ray diffraction, differential scanning calorimetry, and Fourier transform infrared spectroscopy, which confirmed not only the formation of supramolecular hydrogel structure but also the homogenous dispersion of xGNPs in the hydrogel matrix. It was found that the existence of xGNPs can accelerate the speed of gel formation in comparison with that of the native EPE/α-CD hydrogel. Additionally, the water-retention ability and the release behavior of vancomycin hydrochloride for the xGNPs/EPE/α-CD hybridized hydrogels were investigated. 相似文献
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The flammability and the thermal oxidative degradation kinetics of expandable graphite (EG) with magnesium hydroxide (MH) in flame‐retardant polypropylene (PP) composites were studied by limiting oxygen index (LOI), UL‐94 test, and thermogravimetric analysis (TGA). The results show that EG is a good synergist for improving the flame retardancy of PP/MH composite and the effect is enhanced with decreasing EG particle size. The Kissinger method and Flynn‐Wall‐Ozawa method were used to determine the apparent activation energy (E) for degradation of PP and flame retarded PP composites. The data obtained from the TGA curve indicate that EG markedly increases the thermal degradation temperature of PP/MH composites and improves the thermal stability of the composites. The kinetic results show that the values of E for degradation of flame retarded PP composites is much higher than that of neat PP, especially PP/MH composites with suitable amount of EG, which indicates that the flame retardants used in this work have a great effect on the mechanisms of pyrolysis and combustion of PP. 相似文献
56.
通过对石墨氧化、酯化,将聚乙烯亚胺耦合接枝到氧化石墨表面,制备聚乙烯亚胺改性氧化石墨(PEI-GO).通过FTIR、XRD、TEM、RS和XPS等对合成材料进行表征,并研究了其对水中的Cr(Ⅵ)吸附和脱附性能.表征结果表明,聚乙烯亚胺成功嫁接到氧化石墨上,其氨基含量为4.36 mmol·g-1.PEI-GO对水中Cr(Ⅵ)具有很好的吸附性能,吸附等温线符合Freundlich方程,吸附动力学可用拟二级动力学方程来描述.PEI-GO对水中Cr(Ⅵ)的吸附随pH的升高而降低.阴离子的存在降低吸附剂对Cr(Ⅵ)的吸附,不同阴离子的影响大小顺序为PO43- >SO42- >NO3- >Cl-.XPS结果表明,PEI-GO对Cr(Ⅵ)的去除是吸附-化学还原耦合作用的结果.经4次脱附再生循环,PEI-GO对Cr(VI)仍具有较高吸附量,表明该吸附剂再生性好,可循环使用. 相似文献
57.
用化学共沉淀法和原位乳液聚合法分别制备了镍锌铁氧体(NixZn1-xFe2O4)、Ni0.7Zn0.3Fe2O4/膨胀石墨(NZF/EG)二元复合物及其聚苯胺(PANI)包覆的三元复合物(NZF/EG/PANI)。用现代测试技术表征了样品的组成、结构、形貌和电磁性能。结果表明,NZF粒子较好地嵌入到EG的层间,PANI对NZF/EG的包覆效果良好;三元复合物的磁性能随磁性组分含量的减小而减弱,而电导率与EG和PANI的导电性及其相对含量相关联;复合物的电磁损耗性能优良,其中三元复合物优于二元复合物。含PANI 70wt%的NZF/EG/PANI三元复合物,制样厚度分别为1.5、2.0和2.5 mm时,其反射损耗峰值(有效带宽)分别为-19.99 dB(5.82 GHz),-20.33 dB (4.08 GHz)和-25.28 dB(3.67 GHz),具有优良的电磁波吸收效果。 相似文献
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Operational instability from processes occurring at the anode during the production of aluminum in the commercial Hall‐Héroult process may lead to an increase in undesirable fluorocarbon emissions, higher energy use, and shorter plant life. One contribution to this instability may be the possible formation of a fluorocarbon film at the electrode interface. Here, the surface composition of graphite anodes after electrolysis in molten NaF–AlF3–CaF2 at 990 °C is investigated for evidence of fluorocarbon formation using C K‐edge near edge X‐ray absorption fine structure. Fluorocarbon is identified on an anode surface after prolonged anode effect (very high overpotential with increased cell resistance) and also on an anode surface after normal electrolysis without anode effect. This provides evidence that fluorocarbon formation may occur prior to anode effect lowering the surface tension of the anode and therefore resulting in dewetting to contribute to the onset of the anode effect. Confirmation that such compounds form furthers our understanding of electrochemical reactions of graphite with fluoride and of the fundamental processes that occur in an aluminum smelter cell. Copyright © 2013 John Wiley & Sons, Ltd. 相似文献