氢化物—石墨炉原位富集原子吸收光谱法测定痕量锑

本文对标示问题进行了研究，自行设计了氢化物发生器，采用以石墨炉两端输入氢化物方式，载气流向用活塞控制，大幅度减少原子化阶段石墨炉内氢气分压，提高了锑的灵敏度，对氢化锑的石墨炉表面分解沉积和原子化机理进行了讨论，方法有于矿泉水和自来水痕量锑的测定，结果令人满意，锑的特征浓度为３０ｐｇ／０．００４４Ａ。     

氢化物发生-原子荧光法直接测定锑及其化合物中的硒和铋

通过研究在不同酸度下Sb5+对Se,Bi的干扰情况,发现在高酸度下,Sb对Se,Bi的干扰明显减弱,并结合锑在不同价态发生氢化反应的差异性,建立了不需通过任何化学分离而直接测定锑及其相关产品中的微量硒和铋的方法,并用于实际样品的分析.方法对实际样品加标回收率在95%～105%之间,检测下限(含量)硒和铋分别为0.00004×10-2mg@L-1和0.0001×10-1mg@L-1,对实际样品分析精度分别为RSD(Se)=2.4%(含量为0.00169×10-2mg@L-1时),5.4%(含量为0.00056×10-mg@L-1时)和RSD(Bi)=5.0%(含量为0.00024×10-2mg@L-1时),1.3%(含量为0.00229×10-2mg@L-1时),完全满足实际样品分析的要求.     

Synthesis of nanoscale antimony particles

For the search of new negative electrodes of Li-ion batteries, a low-temperature method has been developed for the preparation of nanoscale antimony particles which uses an alkoxide-activated sodium hydride as reducing agent of antimony pentachloride. X-ray diffraction and TEM studies confirm the obtaining of amorphous Sb nanoparticles dispersed in an organic matrix. ¹²¹Sb Mössbauer spectroscopy gives evidence for the occurrence of interactions between antimony and the matrix. These interactions are modified by the washing treatments.     

氢化物-原子荧光法测定锑精矿中痕量砷、汞的研究

研究了氢化物发生-原子荧光光谱测定锑精矿中痕量砷汞的分析方法,并对溶样方法及共存元素的干扰进行了研究。发现用王水溶解样品完全,砷汞溶出量最大;加入硫脲-抗坏血酸后,锑精矿中干扰元素的干扰基本消除;通过加入酒石酸抑制基体锑的水解,从而不需通过化学分离,直接测定锑精矿中的痕量砷汞,并用于实际样品的测定。方法的检出限分别为：砷0.220 ng·mL-1, 汞 0.002 ng·mL-1, 相对标准偏差(RSD% n=11)分别为1.47%和0.52%,回收率分别为94.0%～103.0%和98.7%～102.8%。方法具有快速、准确、灵敏度高等优点。     

氢化物发生-原子荧光光谱法测定塌陷湖水中的总锑

建立氢化物发生-原子荧光光谱法测定塌陷湖水体中总锑的分析方法,研究了酸度、硼氢化钾的浓度及其他因素对水体中总锑测定的影响,优化仪器的工作条件,选择5%的盐酸作载流,2%的硼氢化钾作还原剂。结果表明该法线性范围为0—30μg/L,最低检出限为0.29μg/L,加标回收率96.7%—110.0%,对标准溶液测定RSD<2%(n=20),该方法灵敏度高,准确度好,能满足水质分析的要求。     

氢化物发生-原子荧光光谱法测定化探样品中砷、锑、铋和汞的注意事项

针对氢化物发生-原子荧光光谱法测定化探样品中砷、锑、铋和汞的空白、试样制备和分离、干扰、污染、设备和配件故障等同题,分析并总结出应注意的事项和解决方法.     

Simultaneous Determination of Trace Arsenic and Antimony in Fomes Officinalis Ames with Hydride Generation Atomic Fluorescence Spectrometry

A robust, accurate and sensitive analytical procedure was developed for the simultaneous determination of trace arsenic and antimony in fomes officinalis ames by hydride generation atomic fluorescence spectrometry. The parameters were studied systematically, such as acid concentration of the reaction medium, flow rate of the carrier gas and shield gas, the atomizer of height, etc. Ascorbic acid, potassium iodide and thiourea were used as reducer or masking agents to enhance the generation efficiency of the volatile species of As and Sb. In the presence of thiourea, potassium iodide and ascorbic acid, the influences of some coexisting elements on the determination of arsenic and antimony were investigated.     

微波消解-氢化物发生-原子荧光光谱法测定三氧化二锑中砷

以微波消解分解样品,减少了样品前处理的时间,避免了挥发组分的损失。氢化物发生原子荧光光谱法测定三氧化二锑中砷含量,系统地研究了微波消解、氢化物发生的最佳条件。在此条件下测定砷,得出该方法的检出限为0.35μg/L,相对标准偏差小于5%,加标回收率为91.2%—100.3%。     

氢化物发生-双道原子荧光光谱法同时测定中药中不同形态的砷和锑

建立了一种氢化物发生-双道原子荧光光谱法同时测定中药中As(Ⅲ),As(Ⅴ),Sb(Ⅲ)和Sb(Ⅴ)的方法。对实验条件进行了优化,在最佳工作条件下,砷和锑的检出限分别为0.090 3和0.057 8 μg·L-1,RSD分别为2.01%和1.39%。将本法成功应用于中药样品的形态分析,As(Ⅲ)和As(Ⅴ)的回收率分别为90.8%～98.2%和89.2%～102.0%,Sb(Ⅲ)和Sb(Ⅴ)的回收率分别为89.7%～102.0% 和90.3%～110.0%。     

溶剂萃取非水介质氢化物发生-无色散原子荧光光谱法测定痕量锑

本文提出了用乙醇作为NaBH_4的溶剂,APDC-MIBK萃取,有机相氢化物发生原子荧光光谱法测定水样中痕量锑的新方法。与已报道的二甲基甲酰胺(DMF)作为NaBH_4的溶剂相比较,乙醇具有价廉、无毒性以及荧光背景小和可以在较低酸度下发生氢化物的特点。对非水介质氢化物发生法的推广应用具有一定的实用价值。     

原子荧光法测定刺五加不同部位中的砷、锑、汞、硒

采用微波消解处理样品,建立了氢化物发生-原子荧光法测定刺五加不同部位中的As, Sb, Hg, Se的分析方法。在最佳工作条件下,Se, Sb, Hg, Se的浓度与荧光强度均呈现良好的线性关系。砷的检出限为0.068 ng·mL-1,RSD为1.05%;锑的检出限为0.155 ng·mL-1,RSD为1.32%;汞的检出限为0.014 ng·mL-1,RSD为2.03%;硒的检出限为0.052 ng·mL-1,RSD为2.34%。并选用标准物质人发(GBW07601)对测定方法的准确度进行考察,该方法灵敏、快速准确。实验结果表明,刺五加不同部位中As, Sb, Hg, Se的含量有所差异。As, Hg和Se主要在叶中含量较高,锑在根中的含量高于其他部位。     

超声波辅助提取-HG-ICP-AES法测定中草药雷公藤中可溶态Sb(Ⅲ)和Sb(Ⅴ)

本文建立了用超声波辅助提取,氢化物发生-电感耦合等离子体原子发射光谱法测定中草药雷公藤中可溶态Sb(Ⅲ)和Sb(Ⅴ)的分析方法。研究了超声波辅助提取的影响因素、锑形态分离的最佳pH值、仪器工作条件对锑氢化物发生的影响及五价锑的还原条件,探讨了共存离子对锑测定的干扰及消除方法。Sb(Ⅲ)和Sb(Ⅴ)的检出限分别为0.3和2.4 μg·L-1, 相对标准偏差分别为3.9%和4.5%,样品加标回收率为93%～105%。     

Chemical reactivity and thermal stability of nanometric alkali metal hydrides

The chemical reactivities of nano-NaH particles were compared with those of the commercial ones in three test reactions. Large specific surface areas of these nanoparticles are the main factor for their extremely high reactivity in comparison with their commercial counterpart when these particles are used as a chemical reagent. However, when nano-NaH is used as a cocatalyst with Cp₂TiCl₂, activated surface with high surface energy seems to be the main factor for its high catalytic activity. The thermal stability and chemical reactivity of nanoparticles of lithium hydride, sodium hydride and potassium hydride have been studied. The average particle sizes of lithium, sodium and potassium hydrides before heat treatment are 22, 23 and 19 nm, respectively. Catalytic hydrogenation of olefins and hydrodechlorination of chlorobenzene were employed as test reactions for the chemical reactivities of these nanoparticles treated at different temperatures. The nanoparticles grow with the increase of heat treatment temperature, and the BET specific surface areas decrease simultaneously. An activation of the nanometric hydride surface is evident via the heat treatment under suitable temperatures.     

FLAPW calculations of the EFG in semimetallic arsenic and antimony under varying pressure

The variation of the electric field gradient (EFG) at nuclear sites with pressure in semimetallic arsenic and antimony has been calculated using the full-potential linearized augmented plane wave (FLAPW) method. The results are compared with NQR data, which are available up to a pressure of 2 GPa. The calculated EFG depends sensitively on the values of the lattice parameters used. A theoretical investigation of the relationship between c/a and the internal parameter z, using FLAPW methods, has been carried out and compared with available X-ray diffraction data for arsenic and antimony. For antimony, the FLAPW calculations give results which are consistent with the experimental pressure variation of both the lattice parameters and the EFG. In the As case, the use of theoretical values of z leads to good agreement with the measured pressure variation of the EFG. This revised version was published online in August 2006 with corrections to the Cover Date.     

火焰原子吸收法连续测定氧化锑中铅、铜、铁含量

确立了火焰原子吸收测定氧化锑中铅、铜、铁含量的方法,探讨了样品的前处理、酸度、及共存元素的干扰情况,确定了各元素测定的最佳条件,回收率在95.4％-112.1％之间,精密度RSD%不大于5.9％,该方法能满足氧化锑中铅、铜、铁元素的测定。     

阳离子金黄锑染料的合成及其光谱研究

本文以阳离子金黄三氯化锑为原料,合成了阳离子金黄染料,并对该产物进行了锑含量的测定,测定了产物的可见光吸收光谱和红外光谱。     

Structure and Properties of Self-Organized 2D and 3D Antimony/Carbon Composites

The conditions of synthesis of antimony/carbon composites by interlayer self-assembly from colloidal solutions and melts are discussed. The morphology and the structure of these composites are examined. The potential to produce composites of 2D and 3D morphologies is demonstrated. The 2D composite has a multilayer graphene structure with submicron antimony inclusions, while the 3D composite has a spheroidal shell structure with a deformed film-shell with carbon nanoinclusions. The difference in properties of these composites is demonstrated: the 2D composite is conductive, while the 3D composite has a nonlinear current–voltage characteristic that indicates the emergence of novel functional properties of the spheroidal antimony/carbon composite. A model of exfoliation of the layered precursor with covalent interlayer coupling is proposed. This model provides an explanation for the experimentally observed nonlinear hydrodynamic processes in the colloidal antimony solution.     

Application of Mössbauer spectroscopy to follow the incorporation of antimony into calcium— halophosphate phosphors. I

Mössbauer spectroscopy provides us with the possibility of following the incorporation of antimony activators into halophosphate phosphors activated with antimony and manganese and to identify their positions in the crystal lattice. The conditions of the applicability of the method have been elaborated and a series of measurements have been performed on samples taken at different phases of the phosphor preparation, both for fluorapatites and chlorapatites respectively, activated with antimony and manganese.     

氢化物发生-原子荧光光谱法直接测定土壤水溶态Sb(Ⅲ)和Sb(Ⅴ)

在HCl介质中,Sb(Ⅲ)和Sb(Ⅴ)在氢化物发生过程中的化学反应效率不同,通过测定经还原剂还原后和还原前Sb的荧光强度,求解联立方程计算出Sb(Ⅲ)和Sb(Ⅴ)的含量,据此建立了氢化物发生-原子荧光光谱法直接测定土壤水溶态Sb(Ⅲ)和Sb(Ⅴ)方法,操作简便,实用性强。考察了HCl浓度和KBH₄浓度对Sb(Ⅲ)和Sb(Ⅴ)测定灵敏度的影响以及共存元素的干扰情况,并比较了两种还原剂对Sb(Ⅴ)的还原效果。方法检出限为Sb(Ⅲ)1.11 ng·g-1 ,Sb(Ⅴ)1.57 ng·g-1。加标回收试验表明方法准确、可靠。     

ICP-AES法直接测定钢中微量砷、锡、锑

采用ICP-AES法直接测定钢中微量砷、锑、锡的含量。优选了试样溶解方式，最佳分析谱线及仪器工作参数，检出限为砷0.0004%、锑0.0005%、锡0.0003%，方法准确、简便。