原子捕集-导数火焰原子吸收光谱法测定中草药中的微量锌

提出了原子捕集－导数火焰原子吸收光谱法，考察了捕集管位置，火焰状态、冷却水流量、捕集时间、导数测量系统灵敏度档等实验条件对灵敏度的影响。在测量系统20mV/min灵敏度档下，捕集5min，特征浓度为0．037ng/mL，较常规火焰原子吸收光谱法提高了1243倍。     

离子交换—原子捕集火焰原子吸收光谱法测定炼铝母液铝土矿中镓

在文中所述条件下，原子捕集２～４ｍｉｎ，在０～２５μｇ．ｍｌ＾－１范围内Ｃａ吸光度（Ａ）与Ｇａ浓度（ＣＧ）呈线性关系，Ｇａ的原子捕集灵敏度较常规法提高１８倍，为了消除大量Ａｌ，Ｎａ及其它盐类对测定的干扰，采用阴离子交换树脂进行分离，在水溶液中直接测定了炼铝母液，工厂废水，铝土矿中μｇ．ｇ＾－１级Ｇａ，准确度，精密度令人满意。     

开缝石英管原子捕集原子吸收光谱法测定银

试验了空气和乙炔流量、缝管高度、捕集时间、溶液介质等对银灵敏度的影响。结果表明,分别用不同的乙炔流量进行原子捕集与释放可获得最高灵敏度。捕集1min,测得银的特征浓度为8.1×10~(-4)μg·ml~(-1),比常规火焰原子吸收法的灵敏度提高62倍,变异系数2.8％,本法测定了牡蛎中的银。     

石墨炉原子吸收光谱无标样分析法的研究：Ⅳ.实际样品的分析

以有机基体改进剂、管壁原子化、热解涂层石墨管、峰面积积分吸收信号、Ｄ２灯或Ｚｅｅｍａｎ效应扣除背景，有效地控制和消除了海水基体对Ｃｄ，Ｃｏ，Ｃｒ，ＣｕＭｎ，ＮｉＰｂ等元素的干扰。在此前提下，用ＧＦＡＡＳ无标样分析汉分析了实验海水样品中的痕量元素，与极谱法及间接火焰原子吸收法测得的结果相符，测得质控海水样品的结果与标准值亦很吻合，而且检出限和回收率都达达到要求。     

单缝石英管原子捕集原子吸收光谱法测定了水中碲

研究了单缝石英管贫焰捕集－脉冲富焰释放原子捕集原子吸收光谱法测定碲的条件和线性范围;用Ｘ射线衍射分析得碲以Ｔｅ４Ｏ１１形式捕集,探讨了捕集、释放机理。测定质量浓度为２０μｇ／Ｌ的碲（Ⅵ）时,捕集１ｍｉｎ后测得特征质量浓度为１．７６×１０＾－３ｍｇ／Ｌ,比常规ＦＡＡＳ法提高１１３倍,相对标准偏差为２．６％,已用于饮用水样中痕量碲的测定。     

缝管原子捕集初探

本文针对九种元素初步探索了缝管捕集原子吸收的各种参数影响,给出缝管捕集法与常规火焰法的灵敏度、精密度对比结果。并进行了单缝管、双缝管及微量进样的比较实验。该法用于测定自来水和啤酒样品中的Cd、Cu、Pb、Zn,取得结果较为满意。     

缝管原子捕集原子吸收光谱法测定维生素B12

本文研究了Ａｌ２Ｏ２涂层的开缝石英管原子捕集法测定ＣＯ的条件并通过测ＣＯ间接测定维生素Ｂ（１２）。结果表明，在优化条件下Ｃｏ的特征浓度为８×１０（－３）μｇ·ｍＬ（－１），比常规火焰原子吸收法的灵敏度提高８倍。采用本法测定腺苷辅酶维生素Ｂ（１２）中ＶＢ（１２）的含量，相对标准偏差１．１％，加标回收率９８．２～１００．４％。     

单缝石英管原子捕集原子吸收光谱法测定水中碲

研究了单缝石英管贫焰捕集－脉冲富焰释放原子捕集原子吸收光谱法测定碲的条件和线性范围;用Ｘ射线衍射分析得碲以Ｔｅ４Ｏ１１形式捕集,探讨了捕集、释放机理。测定质量浓度为２０ μｇ／Ｌ的碲（Ⅵ）时,捕集１ｍ ｉｎ 后测得特征质量浓度为１．７６×１０－ ３ ｍ ｇ ／Ｌ,比常规ＦＡＡＳ法提高１１３ 倍,相对标准偏差为２．６％ ,已用于饮用水样中痕量碲的测定。     

原子捕集火焰原子吸收法测定水中镉

采用自制原子捕集装置，选择了镉在不锈钢管上捕集的合适条件，使测镉的灵敏度比常规火焰原子吸收法提高了116倍。应用于工业废水中痕量镉的测定，获得满意结果。     

塞曼石墨炉原子吸收光谱法直接测定血液中痕量铝

采用偏振塞曼原子吸收法，以Ｃａ作基体改进剂，注入热解涂层石墨管中，直接测定用ＯＰ溶液稀释血液样品中的痕量铝，有效地消除了血液基体的干扰，克服了铝的记忆效应，从而提高了方法的测定灵敏度、重现性和准确度。     

Dispersion-corrected DFT study on the carbon monoxide sensing by B<Subscript>2</Subscript>C nanotubes: effects of dopant and interferences

Electrical sensitivity of a boron carbon nanotube (B₂CNT) was examined toward carbon monoxide (CO) molecule by using dispersion-corrected density functional theory calculations. It was found that CO is weakly adsorbed on the tube, releasing energy of 3.5–4.1 kcal/mol, and electronic properties of the tube are not significantly changed. To overcome this problem, boron and carbon atoms of the tube were substituted by aluminum and silicon atoms, respectively. Although both Al and Si doping make the tube more reactive and sensitive to CO, Si doping seems to be a better strategy to manufacture CO chemical sensors due to the higher sensitivity without deformation of nanotube structure after adsorption procedure. Moreover, it was shown that some interference molecules such as H₂O, H₂S and NH₃ cannot significantly change the electronic properties of B₂CNT. Therefore, the Si-doped tube might convert the presence of CO molecules to electrical signal.     

Pd掺杂的纳米晶a-Fe2O3基CO敏感元件

采用共沉淀法制备了掺杂Pd和其它元素的纳米晶α-Fe2O3粉体,并制作了厚膜型CO敏感元件.用XRD、TEM和比表面积测定技术对合成的粉体进行了表征,考察了掺杂元素的种类和含量及焙烧温度对敏感元件的灵敏度的影响.结果表明,掺杂5％Sn4+和1％Pd2+,在450℃焙烧的α-Fe2O3对CO的气敏性最佳.     

Synthesis of Tin Oxide Through Thermal Decomposition of Sn2 （NH4）2 （ C2 O4 ）3 and Its Gas Sensing Property

Nanocrystalline tin oxide samples were prepared by using Sn2 （NH4 ）2 （C2O4）3 as the precursor. The thermal decompositions were respectively conducted at 250,450 and 650 ℃. TG-DTA, XRD, TEM, FTIR were used to characterize the samples. The indirect heating sensors by using these materials as sensitive bodies were fabricated on an alumina tube with Au electrodes and platinum wires. Sensing properties of these sensors were investigated. It was found that the tin oxide sample obtained by thermal decomposition at 450 ℃ has a higher sensitivity to C2H5OH and a higher selectivity to hexane and ammonia than those obtained via the conventional precipitate method and the working temperatures needed were greatly decreased.     

The use of graphite cups for introducing solid samples with an electrothermal atomizer

Because of difficulties in quantitatively transferring accurately weighed solid microsamples into electrothermal atomizer tubes, various materials were investigated for their suitability as cups or carriers. Plastics, ‘ashless’ papers and cellulose acetates, though theoretically completely destructible at the ashing step, were found to have two principal disadvantages: they contribute comparatively high and variable blank values of many common elements; the residues left in the tube after atomization of solid metal and refractory samples lead to inaccuracy of reading and to much shortened tube life.Graphite cups not only overcome these problems but have the positive advantage that their use results in a usefully higher sensitivity for the elements investigated.Some brief examples of the use of graphite cups are quoted, but it is emphasized that the method of calibration must still be carefully checked. The reasons for the improved sensitivity of the graphite cup method and its relationship to the L'vov ‘platform’ method are discussed.     

The oxygen-shielded air-acetylene flame in emission analysis

Flame-emission studies have been made on 18 elements in the inner zone of an oxygen-shielded air-acetylene flame. The shielded flame gave higher emission sensitivity that that of the C(2)H(2)N(2)O flame for Cu and Tl, and comparable sensitivity for a number of other elements, but poorer sensitivity for elements forming stable refractory oxides in flames. The inner zone of the shielded flame has low emission-background and high flame-temperature, permitting good analytical sensitivity to be obtained with relatively low-resolution optical equipment.     

化学气相传输法分离二元混合重稀土氧化物

稀土气态配合物;化学气相传输法分离二元混合重稀土氧化物     

XANES研究Al2O3包覆LiNi0.4Co0.2Mn0.4O2材料的稳定性

采用溶胶凝胶水解法在LiNi0.4Co0.2Mn0.4O2(NCM)表面包覆了0.5 wt%Al2O3.透射电镜(TEM)表明在NCM表面形成了均匀的Al2O3包覆层;分别采用恒电位极化及热重分析(TG)研究了包覆前后NCM的析氧特性;采用X射线吸收近边结构谱(XANES)研究了包覆前后O的电子结构.结果表明,包覆后的NCM析氧量更少;Al2O3包覆使得NCM表面层中与金属3d轨道杂化的O比例减少,而更稳定的、与金属4sp轨道杂化的O比例增加.这些因素导致Al2O3包覆后的NCM更加稳定、安全性更高.     

Detection of H2O2 released from TiO2 photocatalyst to air.

H2O2 generated and released from TiO2 photocatalysts to the gas phase was detected. A flow-through cell packed with TiO2-coated glass beads was irradiated with UV light, and the gas flowing out of the cell was flushed through a collecting solution containing 2,2'-azino-bis(3-ethylbenzothiazoline-6-sulforic acid) diammonium salt (ABTS) and peroxidase. Oxidative coloration of ABTS was observed only in the absence of catalase, indicating the presence of H2O2 in the gas. The quantum yield of the H2O2 generation was estimated to be > 1 x 10(-7). The detected amount of H2O2 decreased as the TiO2 thickness decreased. H2O2 was not detected when dry air or nitrogen was used.     

Electrochemically controlled in-tube solid phase microextraction

We report a new in-tube solid phase microextraction approach named electrochemically controlled in-tube solid phase microextraction (EC in-tube SPME). This approach, which combined electrochemistry and in-tube SPME, led to decrease in total analysis time and increase in sensitivity. At first, pyrrole was elctropolymerized on the inner surface of a stainless steel tube. Then, the polypyrrole (PPy)-coated in-tube SPME was coupled on-line to liquid chromatography (HPLC) to achieve automated in-tube SPME–HPLC analysis. After the completion of EC-in-tube SPME–HPLC setup, the PPy-coated tube was used as working electrode for uptake of diclofenac as target analyte. Extraction ability of the tube in presence and in absence of applied electrical field was investigated. It was found that, under the same extraction conditions, the extraction efficiency could be greatly enhanced by using the constant potential. Important factors are also optimized. The detection limit (S/N = 3) and precision were 0.1 μg L⁻¹ and 4.4%, respectively.     

New benchmark for water photooxidation by nanostructured alpha-Fe2O3 films

Thin films of silicon-doped Fe2O3 were deposited by APCVD (atmospheric pressure chemical vapor deposition) from Fe(CO)5 and TEOS (tetraethoxysilane) on SnO2-coated glass at 415 degrees C. HRSEM reveals a highly developed dendritic nanostructure of 500 nm thickness having a feature size of only 10-20 nm at the surface. Real surface area determination by dye adsorption yields a roughness factor of 21. XRD shows the films to be pure hematite with strong preferential orientation of the [110] axis vertical to the substrate, induced by silicon doping. Under illumination in 1 M NaOH, water is oxidized at the Fe2O3 electrode with higher efficiency (IPCE = 42% at 370 nm and 2.2 mA/cm2 in AM 1.5 G sunlight of 1000 W/m2 at 1.23 VRHE) than at the best reported single crystalline Fe2O3 electrodes. This unprecedented efficiency is in part attributed to the dendritic nanostructure which minimizes the distance photogenerated holes have to diffuse to reach the Fe2O3/electrolyte interface while still allowing efficient light absorption. Part of the gain in efficiency is obtained by depositing a thin insulating SiO2 interfacial layer between the SnO2 substrate and the Fe2O3 film and a catalytic cobalt monolayer on the Fe2O3 surface. A mechanistic model for water photooxidation is presented, involving stepwise accumulation of four holes by two vicinal iron or cobalt surface sites.