共沉淀分离富集—电感耦合等离子体原子发射光谱法测定高纯氧化？…

提出了以Ｌａ（ＯＨ）３为共沉淀剂，对高纯氧化钨中的痕量金属杂质元素经共沉淀预分离富集后进行ＩＣＰ－ＡＥＳ测定的分析方法，探讨了影响杂质元素回收率和钨残留量的若干因素，确定了合适的分离富集条件，合成试样和标准样品的测试结果表明，Ｂｉ，Ｃａ，Ｃｄ，Ｃｏ，Ｃｕ，Ｆｅ，Ｍｇ，Ｍｎ，Ｎｉ，Ｐｂ，Ｓｂ，Ｓｎ，Ｔｉ等元素能被定量分离回收，回收率和精密度均令人满意。     

磷酸三丁酯色层分离—电感耦合等离子体原子发射光谱法测定U3Si2

本法对Ｕ３Ｓｉ中２２个微量杂质元素的测定，进行了较系统的实验研究，取样１００ｍｇ时，Ａｌ、Ｃａ、Ｃｄ、Ｃｒ、Ｃｕ、Ｆｅ、Ｈｆ、Ｉｎ、Ｍｇ、Ｍｎ、Ｍｏ、Ｎｂ、Ｎｉ、Ｐｂ、Ｓｎ、Ｔａ、Ｔｉ、Ｖ、Ｙ、Ｚｎ和Ｚｒ的测定范围５μｇ／ｇ－８００μｇ／ｇ，回收率为９４％－１０５％，ＲＳＤ（ｎ＝８）０．４％－１．２％。     

微晶萘固相萃取分离富集及ICP—AES测定Cu,Mn的研究

报道以微晶萘作吸附载体的固相萃取分离及ＩＣＰ－ＡＥＳ测定Ｃｕ，Ｍｎ的新方法，详细研究了溶液酸度，试剂浓度，萘用量及共存离子对待测物回收率的影响，考查了加入适量的Ｃｏ＾２＋，对富集痕量Ｃｕ＾２＋Ｍｎ＾２＋辅助作用，本法用于生物样品马尾藻及小牛肝中Ｃｕ，Ｍｎ的测定，分析结果与标准值吻合。     

端视ICP-AES法测定钕铁硼永磁材料中常量及微量元素

报道了用高灵敏度的电感耦合等离子体原子发射光谱法（ＩＣＰ－ＡＥＳ）直接测定钕铁硼永磁材料中常量、少量及微量元素：Ｎｄ、Ｆｅ、Ｃｏ、Ｂ、Ｌａ、Ｃｅ、Ｐｒ、Ｄｙ、Ｇｄ、Ｓｍ、Ａｌ、Ｍｎ、Ｃａ、Ｍｇ、Ｇａ和Ｓｉ的分析方法。选择了合适的分析线，研究了基体元素Ｎｄ、Ｆｅ、Ｃｏ对被测杂质元素分析线的光谱干扰，采用基体匹配与背景扣除法进行校正。各被测元素的检出限为０．５～３０μｇ／Ｌ，回收率为９２～１１０％，相对标准偏差小于７％。本法已用于钕铁硼产品的快速检验，并获得了满意的结果。     

不同产地高良姜无机元素含量的比较

用等离子体发射光谱法测定了三个不同产地高良姜的元素含量，在２７种被测元素中，除Ａｓ、Ｂｅ、Ｃｒ、Ｍｏ、Ｐｂ、Ｓｂ、Ｔｌ７种元素未被检出外，三个产地的高良姜均含有Ａｇ、Ａｌ、Ｂ、Ｂａ、Ｃａ、Ｃｄ、Ｃｏ、Ｃｕ、Ｆｅ、Ｍｇ、Ｍｎ、Ｎａ、Ｎｉ、Ｓｅ、Ｓｉ、Ｖ、Ｚｎ、Ｋ、Ｐ、Ｓ２０种元素，湛江产的高良姜大多数元素的含量要高于其它两地。Ｚｎ和Ｍｎ两种人体必需微量元素的含量较丰富。     

FIA活性碳纤维在线富集水样中痕量元素及ICP－AES检测

本文研究了新型吸附材料－活性碳纤维的在线分离富集特性，用ＦＩ活性碳纤维填充的锥形柱，实现痕量金属元素Ｚｎ、Ｐｈ、Ｎｉ、Ｃｏ、Ｃｄ、Ｍｎ的在线富集。经ＨＮＯ３洗脱后．由ＩＣＰ－ＡＥＳ检测，测定速率达３０样／ｈ，检出限（ｎｇ／ｍＬ）分别为：０．４（Ｚｎ）、４．０（Ｐｈ）．０．９（Ｎｉ）、０．４（Ｃｏ）、０．４（Ｃｄ）、０．７（Ｍｎ），富集柱可使用多次。     

沉淀分离ICP—AES测定铅锭中Te,Cr,Co,Ni杂质元素

采用硫酸沉淀分离基本元素铅后，ＩＣＰ－ＡＥＳ直接测定铅锭中Ｔｅ、Ｃｒ、Ｃｏ、Ｎｉ杂质元素。试验证明在本文提供的条件下Ｓｅ会以ＰｂＳｅＯ３的形式与ＰｈＳＯ４共沉淀，而Ｔｅ、Ｃｒ、Ｃｏ、Ｎｉ等待测元素则保留在溶液中。待测元素加标回收率在８６．４％￣１０８．４％之间。     

PIA活性碳纤维在线富集水样中痕量元素及ICP—AES检测

本文研究了新型吸附材料－活性碳纤维的在线分离富集特性，用ＦＩ活性碳纤维填充的锥形柱，实现痕量金属元素Ｚｎ、Ｐｂ、Ｎｉ、Ｃｏ、Ｃｄ、Ｍｎ的在线富集。经ＨＮＯ３洗脱后，由ＩＣＰＡＥＳ检测，测定速率达３０样／ｈ，检出限（ｎｇ／ｍＬ）分别为：０．４（Ｚｎ）、４．０（Ｐｂ），０．９（Ｎｉ）、０．４（Ｃｏ）、０．４（Ｃｄ）、０．７（Ｍｎ），富集柱可使用多次。     

（PSF—PDMS—PHS）n／PSF共混物的相容性及表面组成

利用ＤＳＣ、ＤＭＡ、ＴＥＭ和ＸＰＳ对［ＰＳＦ－ＰＤＭＳ－ＰＨＳ］ｎ／ＰＳＦ共混物的相容性及表面组成进行了研究．结果表明，ＰＤＭＳ在共混物表面的富集与ＰＳＦ均聚物和［ＰＳＦ－ＰＤＭＳ－ＰＨＳ］ｎ中硬段的相容性有关；ＰＤＭＳ在相容的共混物体系表面的富集与对应的多嵌段共聚物组成基本相近；不相容共混物体系表面ＰＤＭＳ的富集程度相对较高，当共混物本体中有机硅含量从１％增至５％，表面层ＰＤＭＳ的含量迅速增加，可达到嵌段共聚物中ＰＤＭＳ的含量．     

菊花微量及宏量元素分析

用ＩＣＰ－ＡＥＳ法测定了药用野菊花和抗白菊及６种人工栽培菊花中Ａｓ，Ｂ、Ｂａ、Ｃａ、Ｃｄ、Ｃｏ、Ｃｕ、Ｆｅ、Ｍｇ、Ｍｎ、Ｍｏ、Ｎｉ、Ｐｂ、Ｓｅ、Ｓｉ、Ｖ、Ｚｎ、Ｐ、Ｓ、Ｋ等元素的含量。结果表明：（１）菊花中Ｃａ、Ｍｇ、Ｐ、Ｓ、Ｋ含量很高，Ｂ、Ｆｅ、Ｍｎ、Ｚｎ也有较高的含量；（２）野菊花中Ｂ、Ｃａ、Ｆｅ、Ｍｇ含量较其他品种高、，抗白菊中Ｍｎ、Ｓｅ、Ｓ含量高地其他品种；（３）代栽培的菊花Ｋ、Ｐ含量高于     

Solid sampling electrothermal atomic absorption spectrometry for analysis of high-purity tungsten trioxide and high-purity tungsten blue oxide

A solid sampling ETAAS method for the direct determination of Ca, Co, Cr, Cu, Fe, K, Mg, Mn, Na, Ni and Zn in high-purity tungsten trioxide and tungsten blue oxide powders using a modern spectrometer with transversely heated graphite tube and a solid sampling system is described. The extremely high background caused by the vaporizing tungsten oxides could be eliminated by the reduction to tungsten metal using hydrogen as purge gas during pyrolysis. Quantification of all elements was performed using calibration curves measured with aqueous standard solutions. The analyte contents determined were between 0.033 (Cu) and 12.6 (Fe) μg/g for tungsten trioxide and between 0.001 (Co) and 0.5 (Na) μg/g for tungsten blue oxide. The accuracy was checked by comparing the results with those obtained by ETAAS in analysis of HF/HNO₃ sample digests and by other methods. Extremely low limits of detection being between 0.07 (Mg, Na, Zn) - 2 (Ni) and 0.01 (Mg, Na, Ni) - 1.7 (Fe) ng/g for tungsten trioxide and tungsten blue oxide, respectively, could be achieved due to almost complete freedom of blank and unusually high applicable sample amounts (5–15 mg for tungsten trioxide and 5–70 mg for tungsten blue oxide).     

仲钨酸铵水热法制备WO3及其表征

仲钨酸铵水热法制备WO3及其表征;仲钨酸铵（APT）;正交设计;WO3;水热     

WO3纳米管的模板法制备及表征

0引言 WO3纳米材料具有光致变色、电致变色、气致变色等特性,可用于光学信息和储存显示器、pH值探测器、气敏传感器、灵敏窗口等[1,2];并且在太阳能的储存与利用、光电转换、光催化降解大气和水中的污染物等方面有着广阔的应用前景[3,4],成为近几年重点研究的半导体材料之一.以前纳米WO3的制备主要集中在薄膜上,其薄膜的制备工艺已经相当成熟,主要包括蒸发法、溅射法、CVD法、喷涂法、阳极氧化法、溶胶-凝胶法等[3].     

一种新的WO3纳米管的制备方法

一维纳米材料因可用来构造高性能纳米器件的结构单元而成为纳米材料研究的热点．目前的研究重点集中在材料的制备和结构性能表征方面,已发展了多种制备方法,主要有模板法、V-L-S法、L-L-S法和V-S法等,其中阳极氧化铝(AAO)模板法是制备一维材料的好方法．AAO模板的制备工艺已相当成熟,     

镍修饰WO3膜光电化学氧化水的研究

在强碱性溶液中低电压低电流条件下在W基底上经阳极氧化得到致密WO3层,而后在酸性条件下在WO3表面经光辅助电化学还原沉积镍,所获得的复合电极具有优异的光电化学氧化水的活性和稳定性.SEM,EDX,XPS和TEM等表征表明复合电极中具有体心立方结构的W基底经阳极氧化形成了具有单斜结构的WO3层,表面修饰的镍物种以Ni(OH)2形式存在.光电化学实验表明WO3层对可见光具有良好的光响应,表面修饰镍后,光电氧化水的起始电位显著降低,电极的稳定性也得以提高.     

Preparation and characterization of WO3 from ammonium paratungstate via hydrothermal method

Tungsten trioxide powder has been prepared from ammonium paratungstate via hydrothermal method using orthogonal and mono-level design of experiments. The effects of preparation process on particle size, specific surface area, crystal form and crystalline morphology of the tungsten trioxide was investigated by TEM and XRD etc. It was found that the optimum conditions of the preparation are hydrothermal crystallization for 8 h at 180°C, followed by vacuum drying at 45°C and calcination at 500°C for 2 h. The blank reference experiment shows that hydrothermal crystallization treatment favors the formation of hexagonal tungsten trioxide, and the tungsten trioxide powder sample prepared by this method has a high degree of crystallinity. __________ Translated from Chinese Journal of Applied Chemistry, 2005, 22(8) (in Chinese)     

Phase transitions in tungsten trioxide at low temperatures

Capacitance and electrical resistivity measurements have been made on stoichiometric and on oxygen-deficient tungsten trioxide crystals from 4.2 to 300°K. X ray oscillation and rotation photographs were made on single crystals of both materials near 200°K and near 300°K. Capacitance and resistivity anomalies identify phase transitions near 40, 65, 130, 220, and 260°K in stoichiometric WO₃. Resistivity anomalies occur near 80, 130, 220, and 260°K in oxygen-deficient tungsten trioxide. Capacitance measurements suggest that the transformation at 130°K of a low-temperature phase to a high-temperature phase of stoichiometric WO₃ is associated with a doubling of thec-parameter of the unit cell. Resistivity measurements establish probable conduction mechanisms in each phase of stoichiometric and of oxygen-deficient tungsten trioxide, and show that oxygen-deficient tungsten trioxide undergoes a semiconductor-to-metal transition near 220°K. Electronic phenomena that do not appear to be associated with structural phase transformations are observed near 16°K in stoichiometric WO₃.     

One‐step electrodeposition of amorphous carbon films containing WO3 with high conductivity and good wettability

Tungsten trioxide‐incorporated hydrogenated amorphous carbon (WO₃/a‐C:H) films have been fabricated on a single‐crystal silicon wafer by liquid phase electrodeposition using methanol as carbon source and tungsten carbonyl as incorporated reagent. The morphology, composition and structure of the films have been investigated by SEM, XPS, Raman scattering spectroscopy, Fourier transform infrared spectroscopy (FTIR) and Transmission electron microscope (TEM), respectively. The effects of WO₃ incorporation on the electrical and wetting properties were studied in detail. The characterization results showed that tungsten trioxide nanocrystalline particles with diameters in the range of 10–20 nm were homogenously embedded in the amorphous carbon films. Also, the electrical conductivity and wetting ability of the films were strongly improved due to the contribution of the tungsten trioxide. Copyright © 2010 John Wiley & Sons, Ltd.     

The energy of crystallographic shear plane formation in reduced tungsten trioxide

The free energy of crystallographic shear (CS) planes in reduced tungsten trioxide has been considered in a semiquantitative fashion. The CS planes are treated as chemical defects in the tungsten trioxide structure and the energy to create such defects is considered to be largely due to enthalpy contributions due to chemical bond breaking. An assessment of this enthalpy term for the various CS plane types known in the tungsten oxide based CS phases is made and the results are then used to explain the experimentally observed CS plane microstructures in binary and ternary tungsten oxide CS phases.     

Synthesis of Mesoporous Tungsten Trioxide with Crystalline Pore Wall at Low Hydrothermal Temperature

Well-ordered hexagonal mesoporous tungsten trioxide with crystalline pore walls were synthesized at low hydrothermal temperature by using cationic quaternary ammonium gemini surfactants as structure-directing agents and sodium tungstate dihydrate (Na₂WO₄·2H₂O) as a precursor. The effects of alkyl chain length of gemini surfactants, hydrothermal temperature and molar ratio of tungsten to gemini surfactants have been investigated in detail. The strong self-assembly ability of gemini surfactants, strong electrical interaction between gemini surfactants and tungsten trioxide, and solvent extraction strategy contributed together to the coexistence of WO₃ mesostructures and crystalline pore walls.