药用滑石粉酸中可溶物中杂质元素的分析及探讨

目的:通过能谱扫描电镜与ICP-AES的联合应用,考察滑石粉酸中可溶物项目控制的必要性与可行性。方法:通过扫描电子显微镜/X-射线能谱仪(SEM/EDS)对滑石粉酸中可溶物的主要金属元素构成进行分析,并采用电感耦合等离子体原子发光光谱法(ICP-AES)定量测定酸中可溶物中的钙、镁、铁等主要金属元素杂质。结果:扫描电子显微镜/X-射线能谱仪(SEM/EDS)发现滑石粉酸中可溶物普遍存在镁元素,但现行各国药典中均未对可能存在的酸溶性镁盐进行控制。增加ICP-AES测定法,对滑石粉酸中可溶的钙、镁、铁进行考察,并经方法学验证,方法可行。结论:(1)不同来源的滑石粉,酸中可溶物的金属元素含量构成比例有所不同,有必要对酸中可溶物进行控制;(2)ICP-AES可对滑石粉酸中可溶物的钙、镁、铁等主要金属元素杂质进行质量控制及评价。

Field Measurement of NO2 and RNO2 by Two-Channel Thermal Dissociation Cavity Ring Down Spectrometer

A two-channel thermal dissociation cavity ring down spectroscopy （CRDS） instrument has been built for in situ, real-time measurement of NO2 and total RNO2 （peroxy nitrates and alkyl nitrates） in ambient air, with a NO2 detection limit of 0.10 ppbv at 1 s. A 6-day long measurement was conducted at urban site of Hefei by using the CRDS instrument with a time resolution of 3 s. A commercial molybdenum converted chemiluminescence （Mo-CL） instrument was also used for comparison. The average RNO2 concentration in the 6 days was measured to be 1.94 ppbv. The Mo-CL instrument overestimated the NO2 concentration by a bias of ＋1.69 ppbv in average, for the reason that it cannot distinguish RNO2 from NO2. The relative bias could be over 100% during the afternoon hours when NO2 was low but RNO2 was high.

Spectroscopic Diagnostic of Spark Discharge Plasma at Atmospheric Pressure

The emission of CuInSe2-based spark discharge plasma at atmospheric pressure in air has been investigated by optical emission spectroscopy method. The plasma was formed by action of the high voltage pulse generator （with nanosecond pulse） on the corresponding electrodes （CulnSe2 compound）. The emission characteristics have been obtained for the spark discharge plasma at 3 mm interelectrode distance. It was established that the spark discharge plasma radiation was determined by decay products of the compound from which electrodes were made. The most suitable spectral lines for plasma diagnostics is atomic copper lines in the visible spectrum and atomic indium lines in UV （ultraviolet） and visible spectrum.

Preparation and luminescence properties of europium complex with α-naphthylacetic acid incorporated in silica matrix by sol-gel method

Europium ternary complex of Eu(NNA) 3(NNA=α-naphthylacetic acid) was embedded in silica matrix at different ratios by sol-gel method. The luminescence properties of silica composites were studied by comparing them with those of corresponding pure complex by means of excitation, emission spectra and lifetimes. The fluorescence lifetime was prolonged when the pure complex was incorporated in silica matrix. The relative fluorescence intensity and fluorescence lifetimes increased simultaneously with the increase of (Eu(NNA) 3.)

Distribution,fractionation,and contamination assessment of heavy metals in offshore surface sediments from western Xiamen Bay,China

Surface sediment samples were collected at 21 offshore sites in western Xiamen Bay, Southeast China. Total concentrations of Li, V, Cr, Co, Ni, Cu, Zn, St, Mn, Pb, Ba, Fe, and Ti were determined by inductively coupled plasma-optical emission spectrometry; Hg was determined by atomic fluorescence spectrometry. A modified BCR sequential extraction procedure was used to extract fractions of the above elements. Concentrations of Pb, Cr, and Hg at most sites met the primary standard criteria of Marine Sediment Quality except site S12 for Pb and S7 for Cr, while concentrations of Zn at 17 sites and Cu at seven sites exceeded the criteria. The mean concentration of Hg was three times higher than the background, with a possible source being the Jiulong River. Fe, Ti, Ba, Co, V, and Li dominated the residual phase, mainly from terrestrial input. Ni, Cr, Pb, and Hg in the non-residual phase varied largely between sites. Sr, Mn, Cu, and Zn were mainly in the non- residual fraction. Most sites showed considerable ecological risk; exceptions were site S7 （very high） and sites S10, S11, and S14 （moderate）. Cu showed moderate-to-high pollution and Pb exhibited no-to-low pollution, while other metals had a non-pollution status according to their ratios of secondary phase to primary phase （RSP）. Results of two assessment methods showed moderate pollution and a very high ecological risk for Cu, Zn, Ni, and Cr at site S7, which might be due to the local sewage treatment plant.

稀土铕-芳香羧酸-邻菲罗啉三元有机配合物的合成、表征及发光性能

分别以4种芳香羧酸—对甲基苯甲酸(PMBA)、对氯苯甲酸(PCBA)、对溴苯甲酸(PBr BA)、对氨基苯甲酸(PABA)—作为第一配体,邻菲罗啉(phen)为第二配体,采用溶剂热法合成了4种稀土铕离子(Eu3+)的三元有机配合物。通过元素分析、红外光谱、热重分析等手段确定配合物的化学结构,结果表明,4种配合物的组成可表示为Eu L3phen·H2O(L=PMBA、PCBA、PBr BA、PABA),芳香羧酸配体和邻菲罗啉均与稀土Eu3+配位;铕配合物在318℃以上才开始出现明显失重,表明其具有良好的热稳定性。研究了4种芳香羧酸配体对紫外光的吸收性能。通过荧光光谱研究了配合物的发光性能,4种配合物均发出Eu3+的特征荧光,5D0→7F2电偶极跃迁发射峰强度顺序为:Eu(PBr BA)3phen·H2O>Eu(PMBA)3phen·H2O>Eu(PCBA)3phen·H2O>Eu(PABA)3phen·H2O;其国际照明委员会(CIE)色坐标均落在红光区域,能发出纯正的红光。

STUDY ON THE DETERMINATION OF TRACE Fe(Ⅲ) BY THIN LAYER RESIN PHASE SPECTROPHOTOMETRY

A method to determine Fe（Ⅲ） by thin layer resin phase spectrophotometry has been developed in this paper. The colored complex formed by Fe（Ⅲ） and 1,2-benzendiol is concentrated on the 717^# resin, then Fe（Ⅲ） can be determined directly by making thin layer. The method is sensitive with a apparent molar absorption of 4.8×10^4L/mol.cm, which is 16 times higher than that of liquid phase spectrophotornetry, most coexisting ions do not influence the determination. The detection limit for Fe（Ⅲ） is 1.47μg/L with the precision of 3.3% [n=6, 7μg/50mL Fe（Ⅲ）]. The calibration curve is linear in the range of 0-25μg/50mL. The preposed method was applied to the determination of Fe（Ⅲ） in water sample with satisfactory results.

Occurrence and distribution of dissolved tellurium in Changjiang River estuary

With the implementation of the GEOTRACES program, the biogeochemical cycle and distribution of tellurium （Te） in marine environments are becoming increasing environmental concerns. In this study, the concentration of dissolved Te in the Changjiang （Yangtze） River estuary and nearby waters was determined in May 2009 by hydride-generation atomic fluorescence spectrometry to elucidate the abundance, dominant species, distribution, and relationship with environmental factors. Results show that： （1） dissolved Te was low owing to its low abundance in the Earth＇s crust, high insolubility in water, and strong affinity to particulate matter; （2） Te（IV） and Te（VI） predominated in surface water. Te（VI） was the dominant species in bottom water, and Te（IV） was the minor species; （3） Horizontally, resulting from low phytoplankton metabolism and the weak reduction from Te（VI） to Te（IV） in the shore, Te（IV） was concentrated in the central zone instead of the coastal region. However, Te（VI） was abundant near the mouth of the Changjiang River where the Changjiang water is diluted and in the area to the south where the Taiwan Warm Current invaded. In the adsorption-desorption process, Te（IV） was negatively related to suspended paniculate matter （SPM）, indicating that it was adsorbed by particulate matter. While for Te（VI）, the positive correlation with SPM suggested that it was desorbed from the solid phase. In the estuary, dissolved Te had a negative correlation to salinity. However, it deviated from the dilution line in high-salinity regions due to the invasion of the Taiwan Warm Current and the mineralization of organic matter. The relationship between Te（IV） and SPM nutrients indicated that it was more bioavailable and more related to phosphorus than to nitrogen. Progress in the field is slow and more research is needed to quantify the input of Te to the estuary and evaluate the biochemical role of organisms.

Study on Microcavity Organic Light-emitting Devices Containing Negative Refractive Index Dielectric Layer

A new structure containing negative refractive index dielectric layer（NRlDL） is introduced into microcavity. The properties of the new mierocavity organic light-emitting devices（MOLEDs） are investigated. In the experiment, the transfer matrix method is adopted. The dependence of reflectance and transmittance on the refractive index and thickness of NRIDL are analyzed in detail. Compared with the electroluminescence spectra of non-NRIDL diodes, the line widths of the spectra of the MOLEDs are narrower and all the peaks enhance. The results show that the new structure is beneficial to improve the performance and reduce the thickness of microcavity devices.

Quick Fluorescence Method for the Distinguishing of Vegetable Oils

This paper presents the possibilities offered by fluorescence spectroscopy for the identification of vegetable oils such as soybean, sunflower, flax, walnut, corn, almond, sesame, olive and pumpkin oils. The probes under study have been excited with two types of sources： a laser diode （LD） and light-emitting diodes （LEDs） emitting in the UV and in the visible range. Total luminescence spectra were recorded by measuring the emission spectra in the range 350-720 nm at excitation wavelengths from 375 to 450 nm. The excitation-emission matrices have been obtained and two basic fluorescence regions in the visible have been outlined. On this basis the fluorescence spectra of the oils have been subdivided into three categories depending on the prevalence of the fluorescence maxima. The samples show differences in their fluorescence spectra. The latter fact shows that fluorescence spectroscopy can be used for the quick identification of edible oils. The fatty acid, the tocopherol, the beta-carotene and chlorophyll contents in the analyzed oils have been studied. It is shown that some of the types of oils differ significantly from each other by the first derivatives of their fluorescence spectra. There also exist color differences between the groups of vegetable oils under study.

Determination of Cadmium in TSP, PM10 in urban areas by hydride generation atomic fluorescence spectrometry

In this paper, two different diameter particles （TSP, PM10） were collected by TH-16A four-channels classification air sampler. The samples were treated by HNO3. Analysis of cadmium was carried out by hydride generation atomic fluorescence spectrometry （HG-AFS） method, and distribution proportions of elements in four phases were calculated. This method was based on the reaction of cadmium with 1.5% （m/v） KBH4 solution and 0.5% KOH（m/v） solution to form the hydride gas in medium of 2% （v/v） HCl. The detection limit for cadmium as low as 0.008μg/L was obtained. The lineally correlation coefficient was 0.99992. The relative standard deviation （n=5, C=1.00μg/L） was 3.26%. The proposed method was applied for the determination of cadmium in atmosphere aerosol samples and the recoveries in the range of 95-102.2% were obtained. This method was simple, rapid, less matrix interference and high sensitivity.

高聚物发光方法的进展

高聚物发光方法研究迄今只有十几年的历史,而其应用几乎已广泛深入到高分子科学的各个领域。尤其在高聚物构象、形态及动态方面的?究已取得显著成功。高聚物发光方法是以高分子链所固有的、或向高分子体系引入的发光“探针”(probe)

Preliminary Assessment of Total Mercury in Bulk Precipitation around Olkaria Area, Kenya

Geothermal power plants are receiving increasing attention as regards the mobilization of mercury （Hg） to the environment. Hg is a trace element that may be present in the geothermal fluid, but due to its volatility, it is transferred mainly into the vapor phase. Hence, it may be mostly discharged to the atmosphere with the non-condensable gases. Olkaria geothermal field hosts 3 geothermal power plants. In this area Hg deposition fluxes have not been studied. Concentrations and wet deposition fluxes of total mercury （T-Hg） were determined from April 2009 to May 2010 at 2 sites in this field. Event-based precipitation samples were collected using fabricated bulk precipitation samplers. Samples were treated according to trace metal protocol and analyzed by cold vapor atomic fluorescence spectrometry （CVAFS）. This paper thus reports the first ever determination of T-Hg concentrations and fluxes in precipitation. The T-Hg concentration in samples ranged from 0.002-0.0602 μg/L at the two sites, however, the volume-weighted mean concentration and wet deposition flux were 0.01974 and 0.02884μg.L^-1 and 0.0167-1.45 μg.m2 during the study period. The annual volume-weighted mean wet deposition fluxes of T-Hg for 2 sites were 13.74 and 19.83 μg.m-2.yr-1 with an average flux of 16.785μg.m-2.yr-1. Hg concentrations and the Hg fluxes in precipitation showed seasonal trends being lowest in the short-rains and highest in the long rains. The concentrations of T-Hg for the 2 sites is negatively correlated with the precipitation depth （r2 = 0.26 ＆ r2 = 0.0065）, suggesting that scavenging of particle-bound mercury from the atmosphere is an important mechanism contributing to mercury in rainwater. Mean Hg concentrations in precipitation at the study sites were comparable to the ranges reported for Canada and the USA by the Mercury Deposition Network （MDN）.

Adsorption of Chromium （VI） onto Activated Carbon Modified with KMnO4

The adsorption capacity of activated carbon modified with KMnO4 （potassium permanganate） for Cr（VI） from aqueous solution was investigated. The modified activated carbon was characterized by SEM （scanning electron microscopy）, FT-IR （Fourier transform infrared spectrometer）, and N2 adsorption/desorption tests. Adsorption of Cr（VI） from aqueous solution onto the activated carbon was investigated in a batch system. In the present study, the effect of various parameters such as pH, contact time and initial concentration on the adsorption capacity were determined by ICP-AES （inductively coupled plasma atomic emission spectrometry）. The Cr（VI） adsorption on the activated carbon conforms to the Langmuir and Freundlich isothermal adsorption equation. The rates of adsorption were found to conform to pseudo-second order kinetic. The modified activated carbon can be an effective adsorbent for Cr（VI） from the aqueous solution.

一种新型金属铱(Ⅲ)有机配合物的光谱特性研究

针对一种合成的新型金属铱(Ⅲ)有机配合物的光谱特性进行了研究。实验中,该配合物的配体为苯基喹啉和异丁基酰苯胺。紫外—可见吸收光谱研究表明,该配合物分别在225 nm、267 nm、339 nm以及460 nm附近出现较强吸收峰,其中在320 nm～580 nm范围内,存在着单线态和三线态的金属铱到配体的电荷跃迁。发光光谱测试表明,随着溶液中(二氯甲烷作为溶剂)该新型金属铱(Ⅲ)有机配合物浓度的增加,溶液的发光光谱峰值位置不断发生红移。当处在460 nm激发波长下,溶剂二氯甲烷发光光潜没有出现明显的峰值强度。排除了溶剂对发光光谱测量的影响,直接测量山该配合物在606 nm附近有强的金属三线态磷光发射。因此,该配合物有望成为一种可用于有机电致发光领域的新型磷光材料。

Preparation,characterization and photocatalytic performance of Mo-doped ZnO photocatalysts

A series of Mo-doped ZnO photocatalysts with different Mo-dopant concentrations have been prepared by a grind- ing-calcination method. The structure of these photocatalysts was characterized by a variety of methods, including N2 physical adsorption, X-ray diffraction （XRD）, scanning electron microscopy （SEM）, Fourier transform infrared （FT-IR） spectroscopy, photoluminescence （PL） emission spectroscopy, and UV-vis diffuse reflectance spectroscopy （DRS）. It was found that Mo6＋ could enter into the crystal lattice of ZnO due to the radius of MO6＋ （0.065 nm） being smaller than that of Zn2＋ （0.083 nm）. XRD results indicated that Mo6＋ suppressed the growth of ZnO crystals. The FT-IR spectroscopy results showed that the ZnO with 2 wt.% Mo-doping has a higher level of surface hydroxyl groups than pure ZnO. PL spectroscopy indicated that ZnO with 2 wt.% Mo-doping also exhibited the largest reduction in the intensity of the emission peak at 390 nm caused by the recombi- nation of photogenerated hole-electron pairs. The activities of the Mo-doped ZnO photocatalysts were investigated in the pho- tocatalytic degradation of acid orange II under UV light （2 = 365 nm） irradiation. It was found that ZnO with 2 wt.% Mo-doping showed much higher photocatalytic activity and stability than pure ZnO. The high photocatalytic performance of the Mo-doped ZnO can be attributed to a great improvement in the surface properties of ZnO, higher crystallinity and lower recombination rate of photogenerated hole-electron （e-/h＋） pairs. Moreover, the undoped Mo species may exist in the form of MoO3 and form MoO3/ZnO heterojunctions which further favors the separation of e/h＋ pairs.