火焰原子吸收光谱法研究五种螯合剂对染镉小鼠睾丸中镉钙铁锌浓度的影响

采用火焰原子吸收光谱法分别对染镉小鼠和N-对羟甲苯甲基-D-葡糖二硫代氨基甲酸钠(HBGD)、N-苯甲基-D-葡糖二硫代氨基甲酸钠(BGD)、二乙基二硫代氨基甲酸钠(DDTC)、二巯基丙醇(BAL)、乙二胺四乙酸(EDTA)等五种螯合剂治疗组小鼠睾丸中镉、钙、铁、锌等金属浓度进行了测定和研究.结果表明:镉染毒(Cd 2.5 mg·kg-1,腹腔注射)后,小鼠睾丸中镉、钙、铁、锌等金属浓度显著高于对照组(p＜0.05),染镉30 min后用各螯合剂治疗(0.400 mmol·kg-1,腹腔注射),24 h后除EDTA外,其余螯合剂能明显降低睾丸中镉的浓度并抑制钙、铁、锌浓度的增加(p＜0.05);染镉24 h后注射各螯合剂,治疗24 h后,HBGD、BGD和DDTC显著降低了小鼠睾丸中各金属浓度(p＜0.05);提示HBGD和BGD有望成为染镉中毒的理想解毒剂.     

Second derivative spectrophotometric method for simultaneous determination of cobalt, nickel and iron using 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol

A simple, sensitive and rapid derivative spectrophotometric method using 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (5-Br-PADAP) has been developed for simultaneous determination of Co(II), Ni(II) and Fe(II) which have very similar chemical behavior and appear together in many real samples. The complexes of all these metal ions with 5-Br-PADAP were formed immediately at pH 7.0 ammonium acetate buffered solution and were stable for at least 24 h. Second derivative spectra were selected for evaluation, because working wavelength determination was more precise and spectral overlap was less than in the ordinary and first derivative spectra. Three wavelengths at which the complexes exhibit extremum ²D values for Co(II), Ni(II) and Fe(II) were selected as analytical wavelengths, i.e., 640, 600 and 740 nm, respectively. Calibration curves drawn with zero-to-peak values at mentioned wavelengths were linear between 80 and 2000 ng ml⁻¹ for each metal ion. Concentrations of Co(II) and Ni(II) were calculated from the total ²D values and the sum of the linear equations for these three cations at 640 and 600 nm, after Fe(II) assay by making use of the ²D value at 740 nm. Limits of detection (LOD) for Co(II), Ni(II) and Fe(II) were 2.7, 13.9 and 3.0 ng ml⁻¹, respectively. The method has been applied to tool steel and heater resistance wire samples successfully.     

Partial Oxidation of Methane to Synthesis Gas over Hexaaluminates LaMAl11O19-δ catalysts

A series of M-substituted hexaaluminates LaMAl11O19-δ (M=Fe, Co, Ni, Mn, and Cu)were prepared and characterized by XRD, XPS, TPR and TGA techniques, respectively. They exhibited different reducibility and catalytic activity for partial oxidation of methane (POM) to synthesis gas. Among the LaMAl11O19-δ samples, LaNiAl11O19-δ showed the best catalytic activity for the topic reaction and selectivity for synthesis gas at 780 ℃ for 2 h. The conversion of CH4 was over 99.2%, and the product selectivity for both CO and H2 was above 90.3%.     

压力、温度和晶粒尺寸对Fe-N合金的合成及结构的影响

在 1× 1 0 - 3 Pa～ 4 GPa的压力和 5 80～ 930 K温度范围内 ,利用高压技术并结合机械球磨 ,研究了压力、温度和晶粒尺寸对α-Fe与非晶 BN的固态反应的影响 .发现高压和晶粒细化可以极大地促进α-Fe和非晶 BN的固态反应过程 ,α-Fe与非晶 BN发生固态反应的临界晶粒尺寸约 8nm.压力和温度对反应产物及其晶体结构有明显影响 .2 GPa和 80 0 K时 ,反应产物为具有正交结构的 Fe-N新相 ;在 3～ 4 GPa和 690～80 0 K时 ,可形成单一ε-Fex N合金相 ;而在 4 GPa和 930 K以上 ,反应产物由 Fe-N合金相转变为 Fe3B相     

Fe(0)催化三氯乙酸烯丙酯的环化反应研究

通过对Fe(O)催化烯烃自由基环化反应的研究，发现以Fe(O)为催化剂催化三氯 乙酸烯丙酯分子内自由基环化反应可以高化学选择性得到五元环内酯产物，反应中 不需加入配体。和大多数自由基反应一样，反应温度与催化剂用量对该反应的转化 率和产率有着很大的影响。     

Mo/Fe3O4(111)表面对燃煤烟气汞吸附的密度泛函研究

利用CASTEP软件包采用密度泛函理论计算研究了过渡金属Mo掺杂Fe_3O_4(111)Fe_(tet)表面对Hg~0、HgCl和HgCl_2的吸附特征,分析了Mo掺杂前后Fe_3O_4(111)Fe_(tet)表面上不同汞物种的吸附形态。结果表明,Mo掺杂Fe_3O_4(111)Fe_(tet)表面对HgCl和HgCl_2为化学吸附,而对Hg~0的吸附为物理吸附;与纯净表面相比,HgCl在Mo原子掺杂表面上的吸附能提高了40%-66%。HgCl_2在纯净Fe_3O_4(111)Fe_(tet)表面形成"M"形结构;而掺杂Mo原子后,由于Cl原子与Mo原子之间更强的相互作用,使得HgCl_2发生了完全解离,两个Cl原子分别与Mo原子和Fe原子成键吸附在表面,Hg脱附。相关研究结果可为脱除燃煤烟气中的汞提供一定的理论指导。     

Evaluation of digestion procedures for the determination of iron and zinc in biscuits by flame atomic absorption spectrometry

An evaluation is made of different digestion methods for the determination of iron and zinc in biscuits prior to flame atomic absorption analysis. For the initial studies, microwave digestion was enough (using hydrogen chloride and nitric acid 3:1, v/v, at 180 °C and 600 W) to provide comparable accuracy, precision, digestion time and non-critical handling of reagents to dry-ashing and wet digestion (using different acid mixtures) and also to a simple acid treatment at room temperature. Although, after a simple microwave digestion, the spiked recoveries were found around 96–102%, to reduce the digestion time and for simplicity we worked on wet acid treatments. The results showed that acid-only treatment is not enough to digest the samples without adding ethanol, which was found necessary to digest organic residue at room temperature. The method was validated by comparison of the data found for commercial biscuit samples through using the proposed procedure and the AOAC official reference spectrophotometric method. Fe concentration in the different biscuits (such as petit beurre, baby biscuits, etc.) ranged from 1.21 to 15.96 mg/100 g while Zn concentration ranged from 0.58 to 2.50 mg/100 g depending on biscuit type. The highest concentration of Fe was in baby biscuits and these biscuits were about thirteen times richer in Fe than petit beurre biscuits.     

Fe、Mn掺杂六铝酸镧的微乳液制法及性能研究

以TX-100/正己醇/环己烷组成的反相微乳液为媒介，采用反相微乳 共沉淀法制备系列金属掺杂的六铝酸镧催化剂。用BET、XRD进行物性表征, 以甲烷燃烧为探针反应考察了催化剂的催化活性。结果表明，反相微乳液合成催化剂的最佳成晶温度可降至1100℃。 LaMx Al12－x O19－α 中M的最佳掺杂数为1(x1)。单金属Mn的存在可以降低甲烷的起燃温度，使催化剂具有良好的低温活性；单金属Fe掺杂的六铝酸镧催化剂具有较低的完全转化温度；而Fe、Mn共同掺杂的LaMnFeAl-10O19－α催化剂具有低、高温活性和高温稳定性。100h稳定性运转的转化率始终保持在99.7％，无失活现象。     

H2O−D2O solvent isotope effect in the volume behavior of some high-charge high-size electrolytes

The apparent molar volumes V of KCl, BaCl₂, K₂SO₄, LaCl₃, Co(en)₃Cl₃ [Tris(ethylenediamine)cobalt(III) chloride], K₃Co(CN)₆, K₃Fe(CN)₆, K₄Fe(CN)₆, and Ba₃[Co(CN)₆]₂ have been determined at 25°C in both light and heavy water. The V values in D₂O are systematically lower and increase more rapidly with salt concentration than the V in H₂O. The volume of transfer from H₂O to D₂O as well as the partial molar volume at infinite dilution in both solvents have also been calculated. These results together with literature values for other electrolytes were used to estimate both of these quantities for D₂O solutions of individual ions. The predictions of ion hydration models and ion-ion interactions are compared with experimental observations.     

模板组装Fe纳米线阵列及其微结构

铝在硫酸溶液中经直流阳极氧化,得到多孔铝阳极氧化膜(AAO). 以AAO膜为模板,通过交流电沉积的方法,在AAO模板孔内成功组装了Fe纳米线.TEM分析表明,Fe纳米线的长度约为2.5 μm,其长度分布十分均匀；粗细均匀,直径约为25 nm. XRD实验分析证实,所制备的Fe纳米线为α-Fe.选区电子衍射（SAED）实验分析表明,α-Fe纳米线具有单晶结构.