碳糊电极阳极溶出法测定中药甘草中桑色素

用碳糊电极阳极溶出法测定桑色素的含量。在0.15mol·L-1NH4Cl 氨水缓冲溶液的介质中富集120s,桑色素在+0.10V(vs.SCE)左右出现阳极溶出峰。其峰电流的大小与桑色素的浓度呈线性关系。线性范围为4.00×10-6～1.40×10-5mol·L-1,相关系数为0.9996,检出限可达1.00×10-6mol·L-1,回收率为99.87%～102.01%。此法不用汞电极,灵敏度高,操作方便、快捷,成功地用于甘草提取物中桑色素的测定。     

铋(Ⅲ)-桑色素极谱络合吸附波的研究

在0.25 mol/L HCl底液中,用单扫极谱法得到了灵敏的铋(Ⅱ)-桑色素络合吸附波,其检测下限达5.0×10~(-9)mol/L。用其测定了锰盐中的痕量铋。测得电活性络合物组成为:铋(Ⅱ):桑色素=1:1,条件稳定常数1gμ=5.0。电极反应为吸附络合物中Bi(Ⅱ)还原为Bi(Hg)。测得电极反应转移系数α=0.42,表面电化学反应的标准速率常数k_s=12.7s~(-1)。     

Resonance Rayleigh scattering determination of trace amounts of Al in natural waters and biological samples based on the formation of an Al(III)-morin-surfactant complex

A novel method for the determination of trace amounts of Al(III) based on resonance Rayleigh scattering (RRS) has been developed. In the presence of some surfactants, Al(III) can react with morin and form an Al(III)-morin-surfactant complex, which results in the enhancement of RRS intensity and the appearance of the corresponding RRS spectral characteristics. Their maximum scatter peaks are at 476 nm for the cetyltrimethylammonium bromide (CTAB) system, 489 nm for the cetylpyridinium chloride (CPC) system, 474 nm for the Triton X-100 system, and 473 nm for the Tween-20 system. The enhanced RRS intensity is directly proportional to the concentration of Al(III). The detection limits are in the range of (0.50-1.2)×10⁻⁷ mol l⁻¹ depending on the surfactant. The characteristics of RRS spectra of the complexes, the optimum conditions of these reactions and the influencing factors have been investigated. The method has high selectivity, and was successfully applied to the determination of Al(III) in natural and biological samples. Furthermore, according to different complexation capacity of Al(III)-morin-CTAB system under two pH conditions, speciation analysis of Al(III) in natural waters was explored. The labile monomeric Al fraction (mainly inorganic Al, Al_i) is determined at acidic pH and the total monomeric Al fraction (Al_a) is determined at alkaline pH. The results are in agreement with those obtained by Driscoll’s 8-hydroxyquinoline extraction-ion exchange method.     

铝（Ⅲ）—桑色素—含氧有机溶剂荧光体系的研究

本文系统研究了醇、酮等7种含氧有机溶剂对铝-桑色素络合物荧光反应的溶剂化效应。研究发现,上述有机溶剂对荧光体系均有增敏作用,以乙醇的效果最佳,使络合物的荧光强度增加6倍多。据此,本文建立了测定微量铝的高灵敏度荧光分析方法,线性范围为0～1.0μg/10ml,检测限为1.6×10~(-9)g/ml。用所建立的方法对化学试剂中的微量杂质铝进行了测定,结果令人满意。并对有机溶剂化效应的机理作了探讨。     

Phenyliodine(III) Diacetate/I2-Mediated Domino Approach for Pyrrolo[1,4]Thiazines and 1,4-Thiazines by a One-Pot Morin Rearrangement of N,S-Acetals

An efficient domino transformation using a phenyliodine(III) diacetate (PIDA)/I₂ combination towards Morin 1,4-thiazine compounds has been developed starting from N,S-acetals. The latter leads to “one-step” regioselective methylene insertion without the need for traditional sulfoxide intermediates in good yields. The reaction involves easily accessible N,S-acetals obtained from cost-effective basic ketones and cysteamine as starting materials. This process ultimately leads to 1,4-thiazines related to natural product and fused derivatives necessary for further QSAR study.     

Morin transition suppression in Polycrystalline 57Hematite (α-Fe2O3) exposed to 56Fe(II)

We used the isotope selectivity of ⁵⁷Fe Mössbauer spectroscopy to investigate changes in the magnetic properties of polycrystalline hematite exposed to ferrous iron (Fe(II)). We found that sorption of ⁵⁶Fe(II), followed by interfacial electron exchange, alters the bulk magnetic properties of ⁵⁷hematite. After reaction with ⁵⁶Fe(II), we observed partial suppression of the Morin transition of ⁵⁷hematite to below 13 K. This is significantly lower than the Morin temperature (T _M) of ～230 K measured for isotopically enriched polycrystalline ⁵⁷hematite, as well as the T _M of 264?±?2 K reported for normal polycrystalline hematite.     

桑色素络合荧光分光光度法测定中药材中铝的含量

以桑色素为络合剂,采用荧光分光光度法测定了10种中药材中铝的含量。结果表明,样品中铝在0.25~2.50μmol/L的范围内荧光强度与含量呈良好的线性关系(r=0.999 3),该法准确、简便,适用于中药材中铝含量的测定。各中药材之间对铝的累积存在明显差异亦应引起重视。     

Phase Transitions of Ruthenium-Doped Iron Oxide Studied by 57Fe Mössbauer Spectroscopy at Elevated Temperatures

Hyperfine Interactions - The 57Fe Mössbauer spectra recorded in situ from 5% ruthenium-doped maghemite show parameters typical for maghemite up to 600 K and a hyperfine field distribution...     

ILEEMS: Methodology and Applications to Iron Oxides

ILEEMS is the acronym for Integral Low-energy Electron Mössbauer Spectroscopy. In this variant of Mössbauer spectroscopy the low-energy electrons, E < ～15 eV, emitted by the probe nuclei in the absorber are counted as a function of source velocity. As a consequence of their low energy, the detected electrons' origin lies within a very thin surface layer with thickness of a few nanometers and consequently, ILEEMS is a useful technique to examine surfaces of Fe-containing substances. In a first part of this paper the authors briefly describe the design of a home-made ILEEMS equipment allowing the temperature of the investigated sample to be varied between 77 K and room temperature. The second part of this contribution deals with a selection of results obtained from ILEEMS spectra for various Fe oxides. In particular, the following items are covered: (1) surface versus bulk Morin transition in small-particle and near-bulk hematite, α-Fe₂O₃; (2) bulk and thin-film magnetite, Fe₃O₄; (3) ferrihydrite, 5Fe₂O₃·9H₂0, goethite, α-FeOOH, and lepidocrocite, γ-FeOOH, all to some extent in relation to their morphology. Interesting and intriguing findings concerning the surface properties of these oxides were obtained and it is argued that the results encourage more systematic research in this and related fields using the surface-sensitive ILEEMS technique.     

VSM and Mössbauer study of nanostructured hematite

In the present work, we have synthesized nanostructured hematite samples using chemical precipitation method. The crystal structure and the grain size of the samples were studied using XRD. The zero field cooled and field cooled magnetization curves of the samples were recorded in the temperature range from 300 to 10 K. The variations of Morin transition temperature and blocking temperature with the grain size of the samples were investigated. The hysterics curves of the samples were recorded and the samples showed a superparamagnetic nature at room temperature whereas, at 10 K the samples showed open hysteresis curves. The sample with smaller grain size showed higher value of coercivity compared to samples with larger grain size. Mössbauer spectra of the samples were recorded and the grain size dependence on Mössbauer parameters was investigated.