ICP－AES法分析水质的探讨

本文用ＩＣＰ－ＡＥＳ（电感耦合等离子体－原子发射光谱法）测定水中Ａｌ、Ｂ、Ｂａ、Ｂｅ、Ｃａ、Ｃｄ、Ｃｏ、Ｃｒ、Ｃｕ、Ｆｅ、Ｍｇ、Ｍｏ、Ｍｎ、Ｎｉ、Ｐｂ、Ｓｒ、Ｖ、Ｚｎ等１８种微量元素。方法简便、快速，只将样品简单酸化，即可测定。方法检出限为０．０００５－０．５μｇ／ｍＬ。相对标准偏差＜１８％     

ICP—AES法测定锌及其化合物中的杂质元素

采用样品溶解后直接测定及氢氧化钇共沉淀将锌与被测杂质元素分离后测定相结合，研究了锌及其化合物中Ａｇ，Ｃｏ，Ａｌ，Ｎｉ，Ｆｅ，Ｃｕ，Ｃｄ，Ｃｒ，Ｍｎ，Ｉｎ，Ａｓ，Ｐｂ，Ｓｎ，Ｓｂ，Ｂｉ等１５个杂质元素的ＩＣＰ－ＡＥＳ测定方法，相对标准偏差１．６－８．１％。     

中药方剂煎煮液中ICP—AES法同时测定16个元素

本文提出了用硝酸－过氧化氢对中药方剂煎煮液进行处理，ＩＣＰ－ＡＥＳ法对煎煮液中Ｌｉ，Ｎａ，Ｂｅ，Ｃａ，Ｓｒ，Ｂａ，Ｍｇ，Ｃｕ，Ｃｏ，Ｎｉ，Ｚｎ，Ｍｎ，Ｃｄ，Ｆｅ，Ｃｒ，Ｖ１６个元素进行同时测定的方法，该方法简单，快速，准确度高，所测元素的加标回收率均在８５～１０３％之间，样品分析结果满意。     

La1.85-xSr0.15+xCu1-xMxO4(M = Cr, Mn, Fe, Co, Ga, Al)体系的输运性质研究

利用Ｘ－光衍射,电阻率和电势等实验手段,系统地研究了Ｌａ１．８５－ｘＳｒ０．１５＋ｘＣｕ１－ｘＭｘＯ４（Ｍ＝Ｃｒ,Ｍｎ,Ｆｅ,Ｃｏ,Ｇａ ａｎｄ Ａｌ）体系的结构和输运性质。结果表明;所有的三阶离子掺杂都能在较低的掺杂浓度下抑制超导电性,并且引起金属到绝缘体的转变。磁性离子和非磁性离子掺杂引起显著不同的热电势变化,并用ｄ－ｐ杂化态的变化和局域自旋散射来进行分析讨论。     

MAl2O4：Eu^2＋,RE^3＋,长余辉发光性质的研究

研究鳞石英结构碱土铝酸盐ＭＡｌ２Ｏ４：Ｅｕ＾２＋,ＲＥ＾＋（Ｍ＝Ｍｇ,Ｃａ,Ｓｒ,Ｂａ：ＲＥ＝Ｙ,Ｌａ,Ｃｅ,Ｐｒ,Ｎｄ,Ｓｍ,Ｇｄ,Ｔｂ,Ｄｙ,Ｈｏ,Ｅｒ,Ｔｂ,Ｄｙ,Ｈｏ,Ｅｒ,Ｔｍ,Ｙｍ,Ｙｂ,Ｌｕ）的荧光及长余辉发光性质。其发光由Ｅｕ＾２＋的４ｆ－５ｄ跃迁产生。ＲＥ＾３＋作为辅助激离子,提供合适的陷阱能级。即使用ＲＥ＾３＋的特性波长激发,在ＭＡｌ２Ｏ４：Ｅｕ＾３＋的发光中也观察不到ＲＥ＾３     

ICP—AES法测定人体血清中的Al,Be,Cu,Mn,Mo,V

建立了用ＩＣＰ－ＡＥＳ同时测定人体血清中的Ａｌ，Ｂｅ，Ｃｕ，Ｍｎ，Ｍｏ，Ｖ等六种元素的方法。在我们的设备上，检出限对Ａｌ，Ｃｕ，Ｍｏ为１－３μｍｏｌ／Ｌ，而对Ｂｅ，Ｍｎ，Ｖ为０．１－０．３μｍｏｌ／Ｌ。这六种元素的回收率在１００±２０％之间。     

新型（Pb,Cd）—1222相化合物的制备,结构和电学性质

本成功地合成了一系列新型Ｐｂ－１２２２相层状铜氧化物（Ｐｂ０．５Ｃｄ０．５）（Ｓｒ０．９Ｒ０．１）２（Ｒ‘０．７Ｃｅ０．３）２Ｃｕ２Ｏｚ，Ｒ＝Ｒ’＝Ｙ，Ｐｒ，Ｓｍ，Ｅｕ，Ｇｄ，Ｄｙ，Ｈｏ以有（Ｒ，Ｒ‘）＝（Ｌａ，Ｅｕ），Ｓｍ，Ｇｄ），（Ｓｍ，Ｅｕ），（Ｌａ，Ｇｄ），（Ｅｕ，Ｇｄ），（Ｎｄ，Ｄｙ），（Ｎｄ，Ｙ），（Ｎｄ，Ｅｒ）。     

ICP－AES测定核纯海绵锆中17个杂质元素方法的研究

应用ＩＣＰ－ＡＥＳ法，对核纯海绵锆中１７个杂质元素的测定进行了试验研究。取样量１００ｍｇ时，Ａｌ、Ｃａ、Ｃｏ、Ｃｒ、Ｃｕ、Ｆｅ、Ｍｇ、Ｍｎ、Ｍｏ、Ｎｉ、Ｐｂ、Ｓｎ、Ｔａ、Ｔｉ、Ｖ、Ｙ和Ｚｎ的测定范围是１０μｇ／ｇ—３２００μｇ／ｇ。回收率为９５．２％—１０６．５％。     

ICP－AES法测定人体血清中的Al、Be、Cu、Mn、Mo、V

建立了用ＩＣＰ－ＡＥＳ同时测定人体血清中的Ａｌ、Ｂｅ、Ｃｕ、Ｍｎ、Ｍｏ、Ｖ等六种元素的方法。在我们的设备上，检出限对Ａｌ、Ｃｕ、Ｍｏ为１～３μｍｏｌ／Ｌ，而对Ｂｅ、Ｍｎ、Ｖ为０．１～０．３μｍｏｌ／Ｌ。这六种元素的回收率在１００±２０％之间。     

TBP色层分离－ICP／AES法测定锆铀铒合金中十七个微量杂质元素和铒

本法对锆铀铒合金中十七个微量杂质元素和铒的测定进行了较系统的实验研究。取样１００ｍｇ时，Ａｌ、Ｃａ、Ｃｏ、Ｃｒ、Ｃｕ、Ｆｅ、Ｍｇ、Ｍｎ、Ｍｏ、Ｎｉ、Ｐｂ、Ｓｎ、Ｔａ、Ｔｉ、Ｖ、Ｙ和Ｚｎ的测定范围为３０～３２００μｇ／ｇ，Ｅｒ为０．２～３．２％，回收率为９４～１０８％，ＲＳＤ（ｎ＝８）为０．２～２．１％。     

The influence of a probe on the optical path of atomic absorption spectrometer with a graphite tube atomizer

We have studied the influence on the atomic absorption signal of the obscuring of the transmission beam by a probe for the two-stage atomization in a graphite tube atomizer. The following parameters were varied: the thickness of the probe (0.5–1.0 mm), its displacement from the optical axis of the spectrometer (up to 2 mm), the diameter of the transmission beam (1.3–4.0 mm), the slit width of the monochromator, and the shape of the intensity distribution over the cross section of the beam emitted either by a hollow cathode lamp, or a deuterium lamp, or an electrodeless lamp. We have shown that, using a probe with a thickness that is optimal for the two-stage atomization (1 mm), it is possible to register analytical absorption signals from 28 chemical elements out of 56 (except Hg), which can be determined in graphite atomizers, with a maximal sensitivity and with no optical interference. The remaining elements can be determined with a lower sensitivity because of the necessity to lower the temperature of the secondary atomization.     

石墨炉内石墨探针表面上的原子化机理研究 Ⅳ钒的原子化机理

本文通过X-射线衍射分析(XRD),扫描电子显微镜分析(SEM),化学分析光电子能谱分析(ESCA),并结合原子吸收测量,研究了钒在普通石墨管中石磨探针表面上发生的固相化学反应。结果表明,钒化合物在灰化阶段即可转化为热稳定性较高的碳化物,原子化的最后步骤为碳化物的热分解。     

石墨管涂覆-塞曼效应石墨炉原子吸收法测定土壤和沉积物中钡

样品使用硝酸-氢氟酸-高氯酸湿法消解,在0.015 mol·L-1硝酸介质中,采用自制涂钨石墨管,塞曼效应背景校正技术石墨炉原子吸收法测定了土壤和沉积物中的钡。经涂钨处理的石墨管表面形成了稳定的碳化钨层,有效避免了在原子化过程中待测元素钡与石墨管直接接触形成难熔碳化物,大幅度提高了检测的灵敏度和精密度,显著延长了石墨管使用寿命。碳化钨为间充型碳化物,在高温下可以产生较强的还原性氛围,可在一定程度上避免土壤和沉积物中常见的高浓度基体成分在原子化阶段生成难熔的氧化物而干扰钡的测定。氢氧化钙分子带背景干扰可以通过稀释法消除。该法测定土壤和沉积物中钡操作简便, 快速;检出限为4.2×10-10 g·g-1。环境样品中钡测定的相对标准偏差范围为2.0％～6.5％, 测定标准土壤的相对偏差均小于5％。     

Energy expression of the chemical bond between atoms in metal oxides

The chemical bond between atoms in metal oxides is expressed in an energy scale. Total energy is partitioned into the atomic energy densities of constituent elements in the metal oxide, using energy density analysis. The atomization energies, ΔE_M for metal atom and ΔE_O for O atom, are then evaluated by subtracting the atomic energy densities from the energy of the isolated neutral atom, M and O, respectively. In this study, a ΔE_O vs. ΔE_M diagram called atomization energy diagram is first proposed and used for the understanding of the nature of chemical bond in various metal oxides. Both ΔE_M and ΔE_O values reflect the average structure as well as the local structure. For example their values vary depending on the vertex, edge or face sharing of MO₆ octahedron, and also change with the overall density of binary metal oxides. For perovskite-type oxides it is shown that the ΔE_O value tends to increase by the phase transition from cubic to tetragonal phase, regardless of the tilting-type or the 〈1 0 0〉 displacement-type transition. The bond formation in spinel-type oxides is also understood with the aid of the atomization energies. The present approach based on the atomization energy concept will provide us a new clue to the design of metal oxides.     

Electrothermal atomization of a substance with fractional condensation of the element being determined on a probe

This paper describes a method of electrothermal atomization with a fractional condensation of the elements being determined on a refractory probe with the aim of decreasing the matrix influences on the atomic-absorption signal. In the course of primary atomization of the sample, the probe is placed over the dosing port of a tubular atomizer. The internal argon flow directs the vapor to the probe for the condensation of the elements being determined. The matrix vapors volatilize. Then the probe is inserted into the atomizer for evaporation of the elements and analytical signal recording. It has been shown that this technique makes it possible to decrease the influence of sodium chloride and potassium sulfate on the absorption of Ag, Cd, Pb, and Au by a factor of 50–20,000 as compared to the atomization from the atomizer wall. In the case of Au, this decrease is comparable to the level attained under the conventional conditions of a stabilized temperature furnace with a platform, a modifier, and a background corrector based on the Zeeman effect, while for the other elements its efficiency is 1.5–40 times higher.__________Translated from Zhurnal Prikladnoi Spektroskopii, Vol. 72, No. 1, pp. 124–128, January–February, 2005.     

悬浮进样探针原子化石墨炉原子吸收法测定地质样品中铍的研究

本应用探针恒温原子化技术，系统研究了铍的分析性能，比较了不同类型石墨管和探针材料的测定效果。应用固体悬浮进样，直接测定了地质样品中的痕量铍，方法的ＲＳＤ为３．３￣５．２％，检测限为５．１×１０＾－１２ｇ铍。     

Spatial structure of absorbing vapor in a transversely heated graphite atomizer with a probe

The dynamics of the spatial structure of absorbing layers of silver atoms and molecules and condensed particles of sodium chloride and potassium sulfate in a transversely heated graphite atomizer during atomization of these substances from a platform and evaporation of their condensate from a tungsten probe is investigated by shadow spectral visualization. The fractional probe atomization significantly decreases the spatial inhomogeneities of absorbing layers, the level of nonselective absorption, and the suppression of atomic absorption. As a result, the photometric error decreases. The use of a probe made it possible to increase the maximum amounts of sodium chloride and potassium sulfate allowable for interference-free atomic absorption analysis in a silver sample from 100 to 4000 μg and from 20 to 750 μg, respectively. These values exceed by a factor of 5–8 the acceptable levels in the generally accepted procedure of atomization from a platform with the Pd-Mg modifier.     

Structure of precursors of complex oxides of rare-earth elements prepared by solvent thermolysis

X-ray diffraction and electron microscopy were used to study the structural states of precursors of borates LuBO₃, YBO₃, and EuBO₃, garnets Lu₃Al₅O₁₂ and Y₃Al₅O₁₂, and perovskites LuAlO₃ and LaAlO₃ prepared by solvent thermolysis from a nitric-acid solution or an ammonium nitrate melt solution of simple oxides and nitrates of rare-earth elements. The precursors are mainly found to be amorphous. In some cases, small amounts of non-reacted initial oxides and nitrates are observed to be in an amorphous matrix.     

结构参数变化对内混式喷嘴雾化性能的影响作用

通过对比6种结构参数不同的环形内混式喷嘴的雾化平均直径的变化规律,研究了喷嘴结构变化对雾化性能的 影响规律。结果表明,混合腔宽度、内喷嘴缩进长度、出口流程均对喷嘴雾化性能造成明显影响,而不同的混合腔长度、 气体及液体的喷入方式则基本上不影响雾化性能。     

燃烧法合成碳纳米管的实验方案设计

碳纳米管是一种新型的碳材料,其合成方法多种多样。燃烧法是一种新兴的合成方法,燃烧过程提供用于碳纳米管生长的高温环境,同时也提供足够的烃原料。目前,用于合成碳纳米管的原料包括气体燃料和液体燃料,火焰类型主要有层流扩散火焰、逆流扩散火焰和预混火焰等。影响炭纳米管火焰合成的因素主要有气体成分,温度,催化剂,燃氧比和采样条件。我们采用甲烷扩散火焰用于实验研究炭纳米管的合成条件。实验系统包括扩散火焰喷嘴,混和段,质量流量计,取样探针和基板,气源。内径5 mm的喷嘴与内径100 mm的钢筒同轴。实验测得在气量为0．20 SLM时火焰高度为 3．5 cm。涂覆有催化剂的基板水平朝下置于火焰中采样,并将采集的样品进行电镜分析。本文还对燃烧法合成碳纳米管的机理进行了分析。