微波等离子体炬耦合方式的研究

采用气动雾化连续进样、端视观测法,考察了微波等离子体炬原子发射光谱法中等离子体Ar线的背景发射以及Al,Mg,V等元素的信号发射强度随天线耦合连接点位置的不同而发生的变化.结果表明,当天线位于炬管顶端,即天线距离活塞3λ/4和λ/4时均能获得较好的等离子体,λ/4略好,信号发射强度和信背也较大,只是精密度略差一些.初步探讨了MPT炬管的电磁场结构.     

超声雾化进样微波诱导等离子体原子发射光谱法测定痕量磷的研究

本文提出了一种测定水溶液样品中痕量磷的微波诱导等离子体原子发射光谱法(MIPAES)。样品经超声雾化并去溶后引入等离子体。考查了Ar和He MIP中磷的发射光谱特性和一些实验参数对磷发射强度的影响。用Ar和He作工作气体时,检出限分别为0.03和0.0045μg/ml,方法的相对标准偏差小于5％。     

气相色谱-微波等离子体炬双检测器及其气相色谱的响应特性

提出并建立了气相色谱-微波等离子体炬(MPT)原子发射光谱和离子化双检测器系统. 以Ar气作为等离子体工作气体, O2气作为等离子体屏蔽气体, 同时获得了被测组分的原子发射和离子化信息, 并对不同种类有机化合物的相对响应系数及检出限进行了测定.     

Ar/O2低温等离子体处理对高密度聚乙烯-玻璃粘接性能的影响

Ar／O2低温等离子体处理的高密度聚乙烯(HDPE)膜，和硅烷化玻璃进行粘接。借助X光电子能谱仪(XPS)和衰减全反射红外光谱(ATP-FTIR)对Ar／O2等离子体处理的HDPE膜和硅烷化玻璃进行表面结构分析。研究不同等离子体处理时间、成层温度和成层时间对HDPE／APS-玻璃粘接效果的影响，考察HDPE膜的亲水性与其粘接性之间的关系，寻找HDPE／APS-玻璃最佳粘接条件。结果表明，在本实验条件下，实现了HDPE膜与玻璃之间的粘接，HDPE／APS-玻璃剥离粘接强度高达51．2N／cm。     

粒径对煤在H2/Ar等离子体中热解的影响

对粒径在H2／Ar等离子体煤热解制乙炔中的影响进行了研究，得到了煤的粒径与煤的裂解程度（转化率）、乙炔收率、乙炔在产品气体中摩尔分数和反应器壁结焦的关系，并且在考虑各种因素的制约下，对如何选择最佳粒径和粒径分布的问题进行了讨论。根据煤等离子体热解制乙炔反应器壁结焦的机理和煤粒径是影响反应器内结焦的重要因素，提出了进料粒径双峰分布缓解煤等离子体热解制乙炔装置结焦的新方法，实验证明该方法可行。     

低温等离子体处理天然纤维的ESR研究

低温等离子体表面改质技术,近年来在纤维加工领域的应用引起广泛注目。纤维、高分子材料经低温等离子体处理,在纤维基质中生成自由基。这些自由基同活性原子团一样,其中不稳定的自由基迅速重新结合,而稳定的自由基就残留在纤维基质中。本文研究了天然纤维棉、麻、羊毛和蚕丝分别在O_2、N_2、Ar、CO及CF_4气体中的低温等离子体表面改质处理,用ESR光谱测定了纤维基质中生成的自由基的相对强度,并讨论了热处理对自由基稳定性的影响。     

微波等离子体炬发射光谱法去溶系统性能的研究

用微波等离子体矩（MPT）作激发光源，等离子体的工作气体为氩气，研究了气动雾化进样去溶系统的工作参数对分析性能的影响，探讨了水冷凝与浓硫酸吸收二者协同去溶的相关性，结果表明，OH （Q1带，带头谱线为308.520nm）的发射强度即可判别样品去溶效果。     

低温等离子体对聚合物多孔膜的亲水化改性

综述了低温等离子体在聚合物多孔膜表面亲水化改性领域的研究与应用进展。在简要介绍等离子体技术的原理、方法的基础上,讨论了Ar、He、O2、N2、CO2、H2O、NH2和SO2等非反应性和反应性气体的等离子体表面处理,烷基醇、烷基胺、烯丙基醇和烯丙基胺等饱和及不饱和单体的等离子体沉积聚合,以及烯类单体的等离子体引发的接枝聚合等等离子体方法,对膜表面和膜孔壁的化学组成和形态结构、膜亲水性的获得及其时效性、膜水通量和蛋白质抗污染性等方面的影响。     

电感耦合等离子体-发射光谱分析中硫酸基体效应及抑制

研究了电感耦合等离子体-发射光谱分析中的硫酸基体效应及克服干扰的有效方法。对2%~20%范围内4种不同体积分数H2SO4溶液中30种元素的基体效应进行了观察,发现H2SO4对各元素的谱线发射强度均存在明显的抑制作用。实验证实体积分数5%乙酸可有效抑制H2SO4的基体效应,并建立了H2SO4溶液中痕量元素的电感耦合等离子体-发射光谱分析法。     

碱性氯化法破氰-碲共沉淀富集-电感耦合等离子体原子发射光谱法测定氰化退镀液中金含量

采用碱性氯化法氧化分解样品中氰化物,碲共沉淀法分离富集破氰溶液中的金,建立了电感耦合等离子体原子发射光谱法(ICP-AES)测定退镀液中金的分析方法. 在碱性条件下,使用次氯酸钠氧化分解退镀液中的氰化物,使其转化为二氧化碳和氮气,使用亚硫酸钠溶液中和破氰溶液中的余氯,消除氧化物对氰化物测试包的影响,可以简便快速判断退镀溶液破氰效果. 在3.6 mol/L盐酸介质中,12.5 mL碲溶液(2.5 g/L)和11.0 mL氯化亚锡溶液(1 mol/L)可定量沉淀5~500 μg金,50倍量的杂质元素不干扰测定. 金的质量浓度在0.05~25.00 mg/L范围内与其发射强度呈线性,线性回归方程为y=46.487x+0.343,相关系数r大于0.999 9,检出限为0.004 4 mg/L. 对实际样品进行准确度考察,测定结果的相对标准偏差(RSD, n=7)低于1.0%,加标回收率为96.9%~103.1%,实际样品测定结果与火试金法的对照结果一致性好.     

Sc2MgGa2 and Y2MgGa2

Scandium magnesium gallide, Sc₂MgGa₂, and yttrium magnesium gallide, Y₂MgGa₂, were synthesized from the corresponding elements by heating under an argon atmosphere in an induction furnace. These intermetallic compounds crystallize in the tetragonal Mo₂FeB₂‐type structure. All three crystallographically unique atoms occupy special positions and the site symmetries of (Sc/Y, Ga) and Mg are m2m and 4/m, respectively. The coordinations around Sc/Y, Mg and Ga are pentagonal (Sc/Y), tetragonal (Mg) and triangular (Ga) prisms, with four (Mg) or three (Ga) additional capping atoms leading to the coordination numbers [10], [8+4] and [6+3], respectively. The crystal structure of Sc₂MgGa₂ was determined from single‐crystal diffraction intensities and the isostructural Y₂MgGa₂ was identified from powder diffraction data.     

Zur Kenntnis der Dialkalimetalldichalkogenide β-Na2S2, K2S2, α-Rb2S2, β-Rb2S2, K2Se2, Rb2Se2, α-K2Te2, β-K2Te2 und Rb2Te2

On Dialkali Metal Dichalcogenides β-Na₂S₂, K₂S₂, α-Rb₂S₂, β-Rb₂S₂, K₂Se₂, Rb₂Se₂, α-K₂Te₂, β-K₂Te₂ and Rb₂Te₂ The first presentation of pure samples of α- and β-Rb₂S₂, α- and β-K₂Te₂, and Rb₂Te₂ is described. Using single crystals of K₂S₂ and K₂Se₂, received by ammonothermal synthesis, the structure of the Na₂O₂ type and by using single crystals of β-Na₂S₂ and β-K₂Te₂ the Li₂O₂ type structure will be refined. By combined investigations with temperature-dependent Guinier-, neutron diffraction-, thermal analysis, and Raman-spectroscopy the nature of the monotropic phase transition from the Na₂O₂ type to the Li₂O₂ type will be explained by means of the examples α-/β-Na₂S₂ and α-/β-K₂Te₂. A further case of dimorphic condition as well as the monotropic phase transition of α- and β-Rb₂S₂ is presented. The existing areas of the structure fields of the dialkali metal dichalcogenides are limited by the model of the polar covalence.     

Crystal Structures of [Bu2Sn(O2PPh2)2], [Ph2Sn(O2PPh2)2], and [PhClSn(O2PPh2)OMe]2. Raman Spectra of [Ph2Sn(O2PPh2)2] and [PhClSn(O2PPh2)OMe]2

[(n‐Bu)₂Sn(O₂PPh₂)₂] ( 1 ), and [Ph₂Sn(O₂PPh₂)₂] ( 2 ) have been synthesized by the reactions of R₂SnCl₂ (R=n‐Bu, Ph) with HO₂PPh₂ in Methanol. From the reaction of Ph₂SnCl₂ with diphenylphosphinic acid a third product [PhClSn(O₂PPh₂)OMe]₂ ( 3 ) could be isolated. X‐ray diffraction studies show 1 to crystallize in the monoclinic space group P2₁/c with a = 1303.7(1) pm, b = 2286.9(2) pm, c = 1063.1(1) pm, β = 94.383(6)°, and Z = 4. 2 crystallizes triclinic in the space group , the cell parameters being a = 1293.2(2) pm, b = 1478.5(4) pm, c = 1507.2(3) pm, α = 98.86(3)°, β = 109.63(2)°, γ = 114.88(2)°, and Z = 2. Both compounds form arrays of eight‐membered rings (SnOPO)₂ linked at the tin atoms to form chains of infinite length. The dimer 3 consists of a like ring, in which the tin atoms are bridged by methoxo groups. It crystallizes triclinic in space group with a = 946.4(1) pm, b = 963.7(1) pm, c = 1174.2(1) pm, α = 82.495(6)°, β = 66.451(6)°, γ = 74.922(6)°, and Z = 1 for the dimer. The Raman spectra of 2 and 3 are given and discussed.     

Electrochemical study of (NEt4)2Cl2FeS2MoS2 and (NEt4)2Cl2FeS2MoS2FeCl2

Summary The ability of [MoS₄]^2–, anions to be used as ligands for transition metal ions has been widely demonstrated, especially with Fe²⁺. The present study has been restricted to linear complexes such as (NEt₄)₂ [Cl₂FeS₂MoS₂] and (NEt₄)₂[Cl₂FeS₂MoS₂FeCl₂]. Their electrochemical properties are described: upon electrochemical reduction, these compounds yield MoS₂, as a black precipitate, and an iron complex in solution, assumed to be [SFeCl₂]^2–. The electrochemical reduction goes through two electron transfers, coupled with the breakdown of the molecular skeleton: a DISPl and an ECE mechanism. Depending on the solvent, the following equilibrium may be observed: [Cl₄Fe₂MoS₄]^2–[Cl₂FeMoS₄]^2–+FeCl₂. The equilibrium constant, K_D, was evaluated by differential pulse polarography. K_D is tightly related to the donor number of the solvent.     

Syntheses,Spectroscopic Studies,and Crystal Structures of Me2Sn(O2PPh2)2, Ph2Pb(O2PMe2)2, and Ph2Pb(O2PPh2)2

Me₂Sn(O₂PPh₂)₂ ( 1 ), Ph₂Pb(O₂PMe₂)₂ ( 2 ), and Ph₂Pb(O₂PPh₂)₂ ( 3 ) have been synthesized by the reactions of Me₂SnCl₂ or Ph₃PbCl with the corresponding diorganophosphinic acid in methanol. X‐ray diffraction studies show that the diorganophosphinate groups behave as double bridges between the metal atoms leading to polymeric ring‐chain structures with M₂O₄P₂ (M = Pb, Sn) eight‐membered rings. The organic groups bonded to the metal atoms are in trans‐position in the resulting octahedral arrangement around the metal atoms. The IR and the mass spectra were reported and discussed.     

Thermal decomposition of Me3SnO2PCl2, Me2Sn(O2PCl2)2 and Ph3SnO2PCl2

TG and DTA studies on Me₃SnO₂PCl₂, Me₂Sn(O₂PCl₂)₂ and Ph₃SnO₂PCl₂ were carried out under dynamic argon atmosphere. The results show that the decomposition proceeds in different stages leading to the formation of Sn₃(PO₄)₂ as a stable product. This compound was characterized by IR spectroscopy. Decomposition schemes involving reductive elimination reactions were proposed.     

The alkali hypophosphites KH2PO2, RbH2PO2 and CsH2PO2

The structures of the hypophosphites KH₂PO₂ (potassium hypophosphite), RbH₂PO₂ (rubidium hypophosphite) and CsH₂PO₂ (caesium hypophosphite) have been determined by single‐crystal X‐ray diffraction. The structures consist of layers of alkali cations and hypophosphite anions, with the latter bridging four cations within the same layer. The Rb and Cs hypophosphites are isomorphous.