全固态酸度微电极组的设计与应用

以木犀草素为pH特性敏感物,碳纤维为导电基质,固体石蜡为粘合剂制成了木犀草素碳纤维酸度微电极,将该电极与自制导电凝胶型全固态微型Ag/AgCl电极和铂丝微电极联用,构成全固态酸度微电极组。 采用循环伏安法研究了该电极组对pH值为2.00~10.00的磷酸盐缓冲溶液有效酸度的响应,结果表明,循环伏安曲线上有一对可逆氧化还原峰,两峰的峰电势均随pH值呈线性变化,据此建立了方波伏安法测定溶液酸度的方法,氧化峰的峰电势(E_pa)与pH的线性回归方程为:E_pa(V)=-0.0567pH+0.603(r=0.999),体液中常见离子及蛋白质等不干扰测定。 该电极组微型、无毒、抗干扰能力强,应用于微量体表唾液和汗液酸度的测定,取得了令人满意的结果,为微量体液的实时、在体、现场检测提供了技术基础。     

微电极制备、表面修饰及活体/单细胞电分析应用

微电极是指至少在一维尺度上不大于25μm的电极。微电极由于尺寸小而具有一些常规电极无法比拟的性质,如具有电流密度高、响应速度快、欧姆压降(iR降)小、信噪比高等特点。微电极特殊的性质使其在电化学测试中具有独特的优点和重要性,并在分析化学、生物学及医学等方面得到了广泛应用,尤其在生命分析领域如在单细胞检测和活体分析中具有众多重要的应用。微电极的设计制备是微电极电化学发展应用的关键,目前涌现出的制备微电极的技术有电化学刻蚀法、电沉积法、自组装技术、化学镀层技术等,这些制备方法为快速制备微电极提供了可能性。本文综述了近年来微电极的研究进展,包括微电极的特点、分类、制备方法及其单细胞检测和活体分析方面的应用,最后提出了微电极面临的挑战与发展方向。     

银基微电极方波伏安法测定矿样中痕量铅镉

研究了银基质微电极的伏安特性，经与玻碳电极比较，具有灵敏度高、重现性好、分辨率强、线性范围宽、使用寿命长等优点。并克服了宏观电极的某些缺点，消除了充电电流的影响，基线平稳，峰形清晰。     

电热蒸发进样微波诱导等离子体原子吸收光谱法测定银和镉的研究

研究了以常压低功率氩微波诱导等离子体（ＭＩＰ）为原子化器的原子吸收光谱法（ＡＡＳ）测定银和镉。采用电热蒸发（ＥＴＶ）,浓Ｈ２ＳＯ４吸收去溶的进样方法。考察了微波前向功率,载气流量,去溶电压,去溶时间,蒸发电压,酸度对银,镉测定的影响。方法已用于试样分析。     

原子吸收法测定矿石中的银

以火焰原子化法测定银,一般常在强盐酸介质中进行,使银呈AgCl_4~3状态,便于测定。但此法对仪器侵蚀性较大。引入氯化钠或二乙烯三胺以有所益处,但溶液酸度仍在10％以上,而在火焰原子化系统中,测试溶液的酸度一般不宜超过5％。于氨性介质进行测定有其优点,但大量铁、锰的存在有干扰,结果偏低。采用银的硫代硫酸盐中性介质进行测定,条件较烦锁,且不易控制。我们试用硫脲络合银,在含有一定量铁盐存在的情况下,于低酸度介质中进行测定,取得良好效果。     

微电极上单核沉积的现场电化学原子力显微镜研究

用现场电化学原子力显微镜（ＥＣＡＦＭ）观察玻碳微电极上银单核电化学成核与生长的不同阶段的行为,结果表明银单核在玻碳边缘生成以（１００）面择优的晶粒,证实了成核过程强烈地信赖于玻碳棋底的状态,有成核历史的基底沉积多核,经特殊方法“清洗”的基底沉积单核,本工作首次把ＥＣＡＦＭ应用于微电极系统的研究,对微是极上的单核生长进行实时观察;同非现场测量进行比较,演示一种轩单晶微电极的可行方法。     

PVBS螯合树脂分离富集-火焰原子吸收法测定痕量银

建立了聚[4-乙烯苄基(2-羟乙基)硫醚]螯合树脂分离富集-火焰原子吸收法测定矿样中银的方法．考察了树脂粒度、吸附时间、银的起始浓度、酸度等对吸附性能的影响，试验了共存元素的干扰情况，用灰化法解脱，火焰原子吸收法检测，方法的检出限为0．004μg／ml，检测范围为0．010～1．0μg/ml，相对标准偏差为2.3％(n=3)，回收率为95～100％．此法可用于矿样中痕量银的测定．     

金在微电极上的电沉积研究

本工作利用微循环伏安法和阶跃电位法研究在ＡｕＣｌ３的酸性溶液中金在玻碳和铂微电极上的电沉积行为。结果表明，金在微电极上成核所需的过电位较高，但成核几率也高，在所研究的微电极尺寸范围内，金可形成大量的临界单核，且核的生长速率很快。铂微电极上金电沉积的Ｉ－ｔ曲线符合连续成核的模式。     

儿茶酚胺类神经递质的修饰微电极伏安法研究

本文用电化学方法在铂微盘电极的表面沉积一层铁氰化镍薄膜修饰微电极，对儿茶酚胺类神经递质具有明显的电催化作用，可有效地改善微电极伏安法检测的波形，提高分析检测的准确度和灵敏度，此法用于去甲肾上腺素针剂的样品检测，结果良好。     

氢化物发生—光度分析法连续测定砷锡

锗、砷、锡、锑等性质相近元素在用普通分光光度法测定时,存在着选择性差的问题,为实际分析及连续测定造成了困难。共价氢化物发生-银溶胶光度分析体系的建立和发展,基本解决了此类元素的选择性问题,也为同时或连续测定创造了条件。本文在原工作的基础上,借助于AsH_3和SnH_4在形成酸度上的差异,在高酸度(3.0mol/L HCI)溶液中使砷离子转变为AsH_3逸出分析后,再调节至微酸性(pH 4.5,CH_3COOH-CH_3COONa)产生SnH_4,而显色测定,     

N,O-羧甲基壳聚糖的合成和性质研究

采用多段升温法将壳聚糖改性,合成了取代度为1.84、平均分子量为3.08×105、等电点为7.28的N,O-羧甲基壳聚糖(CMC),分别用紫外光谱、红外光谱、荧光光谱对其结构进行了表征,并对其水溶液的Zeta电位、电导率、表面张力以及水分散体系中羧甲基壳聚糖微粒的粒径分布进行了研究.结果表明, N,O-羧甲基壳聚糖具有表面活性;介质的pH值和浓度对羧甲基壳聚糖溶液的稳定性有很大的影响.     

水性聚氨酯的制备及其性能的研究

本文以琥珀酸酐与三羟甲基丙烷反应,制得了含有羟基和羧基的酯类亲水性单体,并以此单体与ＴＤＩ和ＰＰＧ－１０００反应,制得了含有羧基的聚氨酯预聚体,在三乙醇胺水溶液中分散得到了水性聚氨酯（简称ＷＰＵ）。本文对预聚体的溶剂种类和用量,对乳胶粒的大小及形状的影响进行了研究,确认溶剂的用量越大,乳胶的粒径就越小;以丙酮作溶剂,乳胶粒为棒状或橄榄球状,而以丁酮为溶剂,得到的乳胶粒为圆球状。通过改变亲水单体的用     

Wastewater treatment using nanomaterial quaternary photocatalyst ZrCdPbO4 - Removal of colour pollutant by an eco friendly process

Pollution of environment is a major issue and has drawn attention of researchers throughout the globe. Water is polluted by various means like excretion of various industries and house releases, for example release of yarn, paper, and cloth industries etc. Present investigation consists of removal of such a pollutant. For this, synthesis of a novel quaternary nano particle sized photocatalyst ZrCdPbO₄ is carried and its characterization by different analytical techniques is also carried out. This is further used for removal of colour pollutants from the environment and Erythrosine-B is considered as a role model. Effect of various operational parameters like pH, concentration of dye, amount of photocatalyst, irradiation power etc. is studied, maximum degradation condition is extracted, and it is observed that reaction follows pseudo first order kinetics. Scavenger study suggests the participation of OH free radical in the reaction. Complete degradation of the dye in presence of light and photocatalyst is reported here by. Reusability of the photocatalyst is tested and is found to work up to five cycles efficiently.     

山东省主栽果树生殖器官中稀土与微量营养元素的相关性研究

通过对山东省5大类主栽果树20余个树种的花粉、种子和果实稀土与微量元素自然含量进行分析比较, 认为稀土(RE)与微量元素在各树种花粉中平均含量顺序为Fe＞Zn＞B＞Cu＞Mn＞RE, 种子中B＞Fe＞Zn＞Mn＞Cu＞RE, 果实中Fe＞B＞Zn＞Cu＞Mn＞RE. 各元素在各生殖器官中的自然分布因树种而有很大差异. 但基本规律类同, 即花粉＞种子＞果实. 花粉富集各种微量营养元素的能力都很强. 花粉和果实稀土与微量元素之间绝大多数呈正相关, 种子大多呈负相关, 但相关性均不显著.     

用计算全息法检测卡塞格林系统主镜

为实现对卡塞格林光学系统中的非球面主镜表面面形的高精度检测,设计了一种二元位相型计算全息图(CGH)。介绍了工作原理,对CGH的相位模型参数的优化设计、衍射次级分离以及台阶位置与深度计算等关键问题进行了讨论。通过引入虚拟玻璃的概念快速建立非球面检测模型,针对卡塞格林系统主镜中心开孔的特点,通过加入同轴载波实现了衍射次级的完全分离,相比目前常用的倾斜载波方法简化了相位量化复杂度,数值仿真计算出了最优的台阶深度,降低了加工难度。给出了相应的设计方法及实例,研制投产了CGH。测试得到主镜面形的均方根误差为0.018λ,并与传统补偿器结果(RMS=0.019λ)进行对比,两者测试结果吻合,验证了该设计与检测方法的正确性,该设计方法简单快捷,适用于卡塞格林光学系统主镜面形检测。     

聚苯胺薄膜电极上示差脉冲伏安法可逆波理论研究

本文提出了聚苯胺(PANI)薄膜电极上示差脉冲伏安法可逆波理论,经验证理论和实验结果相符合.     

微波消解-ICP-MS测定电镀污泥中的重金属

采用微波消解系统对某电镀污泥进行消解,利用ICP-MS对污泥中的重金属进行测定。称取制备后样品,置于消解罐中充分反应后,赶酸、定容后利用电感耦合等离子体质谱法进行测定。电镀污泥中的铬为18845.2mg/kg、镉为10.3mg/kg、镍为5200.0mg/kg、铅为189.7mg/kg、铜为3271.7mg/kg、锌为49632.6mg/kg。测定结果表明所检测项目工作曲线线性关系好,相关系数r均大于0.999。铬加标回收率在91.6～97.7%之间、镉加标回收率在92.0～97.0%之间、镍加标回收率在95.1～98.0%之间、铅加标回收率在94.3～95.2%之间、铜加标回收率在97.1～102%之间、锌加标回收率在96.3～98.7%之间,均满足相关测定要求。计算的潜在生态危害系数、潜在生态危害指数结果表明,电镀污泥中的铬、镉、铅、铜、锌为轻微生态危害,镍为强生态危害;潜在生态危害指数RI计算值为216.69,属于中等生态危害。     

Interaction of graphene with antipsychotic drugs: Is there any charge transfer process?

Antipsychotics represent an effective therapy for schizophrenia (a chronic mental disorder). Their benefits are related to the interaction of the drugs with dopamine D2 receptor (D2R). Antipsychotics are classified as agonists or antagonists. One of the working hypotheses is that there is a charge transfer process between the drugs and the receptors, which is different for agonists and antagonists. To have more insight into the nature of the interaction of these molecules and the differences between agonists and antagonists, we analyze the interaction of graphene with three molecules: dopamine, pramipexole (an agonist of dopamine), and risperidone (an antagonist of dopamine). The idea is to use graphene as a simple model to analyze the charge transfer process of these three drugs. Optimized structures, atomic charges, and Density of States results indicate that global charges of dopamine and pramipexole are similar, while for risperidone, it is more than double. Pramipexole is an agonist, and the charge transfer process is similar to that of dopamine. Risperidone is an antagonist, and the charge transfer process is different from dopamine. The charge transfer is more significant with risperidone than with dopamine, and this could be related to the mechanism of action. This is in agreement with the working hypotheses that establish that it is possible to distinguish between agonists and antagonists since they have different capacity to transfer charge.     

钾盐矿床中含石膏盐分析方法的研究

由于现行标准《岩石矿物分析规程》(DZG93-08)对含石膏钾盐样品分析方法的叙述较为粗略,同时没有国家一级有证标准物质进行质量监控,因此在测定含石膏钾盐样品时较为困难。本文讨论了溶矿温度、称样量、以及放置时间对含石膏钾盐样品溶解的影响。得出在称样量为0.5000g,水温80℃,放置时间为24小时,用电感耦合等离子体发射光谱法测定,以样品中各组分百分数加和、溶液中元素阴阳离子平衡以及加标回收实验进行数据质量监控。测试数据符合《地质矿产实验室测试质量管理规范》对钾盐样品分析质量的要求。     

Facile Electrochemical Hydrogenation and Chlorination of Glassy Carbon to Produce Highly Reactive and Uniform Surfaces for Stable Anchoring of Thiolated Molecules

Carbon is a highly adaptable family of materials and is one of the most chemically stable materials known, providing a remarkable platform for the development of tunable molecular interfaces. Herein, we report a two‐step process for the electrochemical hydrogenation of glassy carbon followed by either chemical or electrochemical chlorination to provide a highly reactive surface for further functionalization. The carbon surface at each stage of the process is characterized by AFM, SEM, Raman, attenuated total reflectance (ATR) FTIR, X‐ray photoelectron spectroscopy (XPS), and electroanalytical techniques. Electrochemical chlorination of hydrogen‐terminated surfaces is achieved in just 5 min at room temperature with hydrochloric acid, and chemical chlorination is performed with phosphorus pentachloride at 50 °C over a three‐hour period. A more controlled and uniform surface is obtained using the electrochemical approach, as chemical chlorination is observed to damage the glassy carbon surface. A ferrocene‐labeled alkylthiol is used as a model system to demonstrate the genericity and potential application of the highly reactive chlorinated surface formed, and the methodology is optimized. This process is then applied to thiolated DNA, and the functionality of the immobilized DNA probe is demonstrated. XPS reveals the covalent bond formed to be a C?S bond. The thermal stability of the thiolated molecules anchored on the glassy carbon is evaluated, and is found to be far superior to that on gold surfaces. This is the first report on the electrochemical hydrogenation and electrochemical chlorination of a glassy carbon surface, and this facile process can be applied to the highly stable functionalization of carbon surfaces with a plethora of diverse molecules, finding widespread applications.