Anodic stripping voltammetry of antimony at unmodified carbon electrodes

Antimony is an element of significant environmental concern, yet has been neglected relative to other heavy metals in electroanalysis. As such very little research has been reported on the electroanalytical determination of antimony at unmodified carbon electrodes. In this paper we report the electrochemical determination of Sb(III) in HCl solutions using unmodified carbon substrates, with focus on non-classical carbon materials namely edge plane pyrolytic graphite (EPPG), boron doped diamond (BDD) and screen-printed electrodes (SPE). Using differential pulse anodic stripping voltammetry, EPPG was found to give a considerably greater response towards antimony than other unmodified carbon electrodes, allowing highly linear ranges in nanomolar concentrations and a detection limit of 3.9?nM in 0.25?M HCl. Furthermore, the sensitivity of the response from EPPG was 100 times greater than for glassy carbon (GC). Unmodified GC gave a comparable response to previous results using the bare substrate, and BDD gave an improved, yet still very high limit of detection of 320?nM compared to previous analysis using an iridium oxide modified BDD electrode. SPEs gave a very poor response to antimony, even at high concentrations, observing no linearity from standard additions, as well as a major interference from the ink intrinsic to the working electrode carbon material. Owing to its superior performance relative to other carbon electrodes, the EPPG electrode was subjected to further analytical testing with antimony. The response of the electrode for a 40?nM concentration of Sb(III) was reproducible with a mean peak current of 1.07?µA and variation of 8.4% (n?=?8). The effect of metals copper, bismuth and arsenic were investigated at the electrode, as they are common interferences for stripping analysis of antimony.     

氧化程度对微细鳞片可膨胀石墨结构及膨胀性的影响

以平均粒径为19.71μm的天然微细鳞片石墨为原料,通过化学氧化法制备了具有不同氧化程度的可膨胀石墨,采用XRD、FTIR、Raman、SEM等对可膨胀石墨的结构与膨胀性进行了表征。结果表明：当氧化程度较低时制得的微细鳞片可膨胀石墨由石墨、石墨层间化合物和氧化石墨三相组成;随着氧化程度的增加,氧化石墨相含量与可膨胀石墨结构无序程度逐渐增高,石墨层间化合物相含量先增加后减少,石墨相含量则逐渐降低;氧化促使HSO₄^-或SO₄^2-插入石墨层间,插入层间的HSO₄^-或SO₄^2-量是决定可膨胀石墨膨胀容积的关键因素,制备的微细鳞片膨胀石墨的膨胀容积可达65.9mL·g^-1。     

膨胀石墨负载钯纳米颗粒催化六价铬还原反应

采用高分子辅助的浸渍还原法,制备得到膨胀石墨(EG)负载的纳米钯催化剂(Pd-EG),采用X射线衍射(XRD)、透射电子显微镜(TEM)、X射线光电子能谱(XPS)等手段对催化剂组成、结构、形貌和价态进行了表征,并考察了Pd-EG催化剂在六价铬还原反应中的活性.结果表明,催化剂中纳米钯颗粒均匀分散在膨胀石墨上,平均粒径为4.37 nm,金属负载量质量分数为0.446%.该催化剂对六价铬还原反应具有良好的催化性能,可将六价铬完全转化为三价铬,在pH=4.0及45℃条件下反应转化频率(TOF)达到3186 h-1;催化剂经过多次重复使用后的活性仍保持稳定.     

氮掺杂氧化石墨催化苄胺氧化

酰胺类化合物是重要的化工原料和生物医药合成的中间体,但其制备大部分需要使用贵金属催化剂,因此,发展廉价金属乃至非金属催化剂具有重大意义.本文使用化学气相沉积法合成了氮掺杂的层状氧化石墨材料,并将其应用于苄胺氧化反应中,实现了液相中酰胺合成的非金属催化过程.在水相中可以活化氧气较高产率地生成亚胺化合物N-苄亚甲基苄胺,并且成功实现了在氨水反应介质中高转化率和选择性地生成苯甲酰胺.此外,对反应中的影响因素进行了逐一研究,并从多方面探究了该反应中氨水的作用以及反应最可能的历程,提出了一条经过包括亚胺在内的多个中间产物的反应路径.本工作对于研究碳氢键的活化过程以及拓宽碳催化领域进行了有益的尝试.     

石墨烯包覆天然球形石墨作为锂离子电池的负极材料，是否需要乙炔黑导电剂？

我们通过包覆炭化的方法制备得到了石墨烯包覆的天然球形石墨(G/SG)材料,并使用扫描电子显微镜、X射线衍射仪以及多种电化学测试手段考察了不同石墨烯含量的复合材料的形貌结构及电化学性能。我们发现,在不添加乙炔黑(AB)的情况下,G/SG复合材料表现出较高的首次库伦效率,很好的循环稳定性和高倍率性能。当石墨烯包覆量为1%时,材料50次循环后的可逆容量可与添加10%AB的天然石墨电极(SG)等同;当石墨烯包覆量为2.5%时,材料的比容量完全高于添加10%AB的石墨电极。材料电化学性能的改善归因于石墨烯的包覆。一方面,石墨烯的柔软可变性可以保证天然石墨颗粒在充放电过程中的结构完整性,从而有效改善材料的循环稳定性;另一方面,石墨烯的存在提高了电极的导电性,促进更好导电网络的形成。因此,石墨烯包覆天然球形石墨材料中,石墨烯不仅是活性物质,也发挥导电剂的作用。当添加5%的乙炔黑时,在50 mA·g^-1电流循环50次后,5%G/SG电极的可逆容量从381.1 mAh·g^-1提高到404.5 mAh·g^-1,在1 A·g^-1电流时可逆容量从82.5 mAh·g^-1提高到101.9 mAh·g^-1,这表明G/SG电极仍然需要乙炔黑导电剂。乙炔黑颗粒填充在复合材料的空隙中,通过点接触的形式连接到G/SG颗粒,与石墨烯协同作用形成了更加有效的导电网络。尽管石墨烯包覆和乙炔黑添加对天然石墨电极具有积极的影响,例如增加了天然石墨电极的导电性和储锂性能(包括可逆容量,倍率性能和循环性能),但随着石墨烯或乙炔黑的增加,电极密度通常会降低。因此,在实际应用中应考虑石墨负极材料的质量和体积容量的平衡。这些结果对天然石墨的进一步商业应用具有重要意义。我们的工作为天然石墨电极在锂电池中的电化学行为提供了一种新的认识,并且有助于制备更高性能的负极材料。     

Local Structure Analysis and Modelling of Lignin-Based Carbon Composites through the Hierarchical Decomposition of the Radial Distribution Function

Carbonized lignin has been proposed as a sustainable and domestic source of activated, amorphous, graphitic, and nanostructured carbon for many industrial applications as the structure can be tuned through processing conditions. However, the inherent variability of lignin and its complex physicochemical structure resulting from feedstock and pulping selection make the Process-Structure-Property-Performance (PSPP) relationships hard to define. In this work, radial distribution functions (RDFs) from synchrotron X-ray and neutron scattering of lignin-based carbon composites (LBCCs) are investigated using the Hierarchical Decomposition of the Radial Distribution Function (HDRDF) modelling method to characterize the local atomic environment and develop quantitative PSPP relationships. PSPP relationships for LBCCs defined by this work include crystallite size dependence on lignin feedstock as well as increasing crystalline volume fraction, nanoscale composite density, and crystallite size with increasing reduction temperature.     

Nickel and Tungsten Bimetallic Nanoparticles Modified Pencil Graphite Electrode: A High-performance Electrochemical Sensor for Detection of Endocrine Disruptor Bisphenol A

In this work, an economically viable, very low cost, indigenous, ubiquitously available electrochemical sensor based on bimetallic nickel and tungsten nanoparticles modified pencil graphite electrode (NiNP-WNP@PGE) was fabricated for the sensitive and selective detection of bisphenol A (BPA). The NiNP-WNP@PGE sensor was prepared by a facile electrochemical one step co-deposition method. The prepared nanocomposite was morphologically characterized by scanning electron microscopy (SEM), energy dispersive X-ray (EDX), X-ray diffraction (XRD), electrochemically by cyclic voltammetry (CV), and electrochemical impedance spectroscopy (EIS). The proposed sensor displayed high electrocatalytic activity towards electro-oxidation of BPA with one irreversible peak. The fabricated sensor displayed a wide detection window between 0.025 μM and 250 μM with a limit of detection of 0.012 μM. PGE sensor was successfully engaged for the detection of BPA in bottled water, biological, and baby glass samples.     

Development of Pen-type Portable Electrochemical Sensor Based on Au-W Bimetallic Nanoparticles Decorated Graphene-chitosan Nanocomposite Film for the Detection of Nitrite in Water,Milk and Fruit Juices

The development and fabrication of a simple, portable, and sensitive detection tool to precisely monitor nitrite level is of growing importance in electrochemistry research, given the strong interest in the protection of drinking water quality, treatment of wastewater, food production, and control of remediation processes. This work describes the fabrication of a simple, cost-effective, pen-type electrochemical sensor based on bimetallic gold and tungsten nanoparticles electrochemically decorated on graphene-chitosan modified pencil graphite electrode (PGE) for the trace detection of nitrite in real samples. The prepared nanocomposite was characterized using XRD, SEM, and EDS. The electrochemical behavior of the sensor was evaluated by cyclic voltammetry (CV) and impedance electrochemical spectroscopy (EIS). Results revealed that the proposed sensor displayed excellent electrocatalytic activity towards electro-oxidation of nitrite with an irreversible redox reaction. The AuNPs-WNPs@Gr-Chi/PGE sensor exhibited excellent analytical performance with a wide linear range from 10 to 250 μM towards nitrite. The LOD and LOQ were calculated to be 0.12 μM and 0.44 μM, respectively. The designed electrochemical sensor was successfully applied for the detection of nitrite in water, milk, and natural fruit juice samples.     

Sensitive,Accurate and Selective Determination of Cd(II) Using Anodic Stripping Voltammetry with in-situ Hg-Bi Film Modified Pencil Graphite Electrode After Magnetic Dispersive Solid Phase Microextraction

This paper describes a novel approach to detect Cd(II) using the combination of the differential pulse anodic stripping voltammetry and magnetic nanoparticle based dispersive solid phase microextraction as an efficient, green and accurate method. Currents of Cd(II) increased linearly in the range from 75 to 2000 ng L⁻¹ Cd(II) with a detection limit of 21.6 ng L⁻¹. The RSD values of 2.6 and 6.0 % for 1.00 and 0.10 μg L⁻¹ respectively showed that proposed method has an acceptable repeatability. Recovery values between 92.3 and 98.6 % showed that this approach can be successfully used for determination of Cd(II) in water samples.     

原子吸收光谱分析法测定补钙剂中钙含量

利用石墨炉原子吸收分光光度计对两种葡萄糖酸钙口服液中的钙进行了检测,分析了口服液中钙的含量。该方法准确便捷,为特定溶液样品中各种微量元素的检测提供了一条很好的途径。