四君子汤和四物汤微量元素含量研究

通过了解中药“四君子汤”和“四物汤”中微量元素含量的异同,研讨了微量元素和中医“气血”理论之间的关系。实验表明,“四君子汤”和“四物汤”在微量元素的含量方面,有一定的类同和差异。该现象同中医的“气血”理论有非常相像的地方。同时发现中药中的微量元素在煎煮过程中,并不是同想象的一样匀速进入药液,而是不同的元素在不同的时间段不同的批次进入药液,这也提示中药煎法理论有一定依据。由于目前做的实验还少,本实验留下很多问题和疑点,值得进一步做有关的实验和研究。     

可移动式微量氧分析仪检定装置研制

研制一种新型可移动式微量氧分析仪检定装置。该装置由标准气体、零点气、脱氧纯化器、减压阀、调节阀、4通阀、5通阀、不锈钢管路、流量控制系统、移动平台等组成。该装置气密性好,15 min内可将装置内氧气浓度由20.9%降至不大于0.1μmol/mol,对于0~10μmol/mol的微量氧分析仪检定结果的扩展不确定度为Urel=1.7%FS(k=2)。该装置满足气体标准物质的连续切换和在线检定的需要,检定时间短,结果准确可靠,可为在线式和非在线式微量氧分析仪的量值溯源提供有效保障。     

Quantification of several atmospheric gases from high resolution infrared solar spectra obtained at the south pole in 1980 and 1986

Simultaneous total column amounts of a number of minor and trace atmospheric gases above the South Pole in December 1980 and December 1986 have been deduced from analysis of high resolution solar absorption spectra recorded (by F. J. M. and F. H. M.) from Amundsen-Scott South Pole Station. These spectra also contain some limited information on the vertical profiles of the observed atmospheric gases.The data sets were recorded with a Bomem Michelson-type interferometer and analyzed with a spectral least-squares fitting procedure, utilizing the best available spectroscopic line parameters and absorption cross sections. Because the same instrument, line parameters, and analysis method have been used in analyzing the December 1980 and December 1986 data sets, the precision in comparing the column amounts from these two dates is rather high, about 10–20% for the stronger absorbing gases. For this reason, it has been possible to quantify or determine upper limits for differences between the December 1980 and December 1986 total column amounts, of a number of atmospheric gases including O₃, N₂O, HNO₃, CO₂, CH₄, and CF₂C_{1 2} (CFC 12). In addition, vertical column amounts for a number of atmospheric gases covered only in the December 1986 observations have been derived, including HC1, NO, NO₂, and C₂H₆. Some of these results will be discussed here. The HC1 measurements are especially interesting since the observed amounts are higher than expected from observations made at lower latitudes in the northern and southern hemispheres.     

THEiEARLY JINNING JUVENILE CONTINENTAL CRUST TRANSFORMATION TYPE GRANITOIDS FROM SOUTHERN ANHUI PROVINCE, CHINA

It is considered that the early Jinning period granitoids from southern Anhui Province belong to the continental crust transformation (S) type and have their own characteristics which are different from those for general continental crust transformation type granitoids. They were formed at the early stage of the late Proterozoic era when that region was at an island-arc stage of the continental margin environment. By that time the continental crust was just formed and had a nature of juvenile crust. It is this juvenile crust that determined a series of characteristics of that type granitoids and made them a relatively independent rock type. They are the products formed by the continental crust in a certain stage of development.     

Nanometer-sized zirconium dioxide microcolumn separation/preconcentration of trace metals and their determination by ICP-OES in environmental and biological samples

A new method is proposed using a microcolumn (20 mm × 2.0 mm) packed with nanometer-sized zirconia as solid-phase extractor for the separation/preconcentration of Mn, Cu, Cr, Zn, Ni and Co prior to their determination by inductively coupled plasma optical emission spectrometer (ICP-OES) in environmental samples. The factors affecting the separation and preconcentration of analytes such as pH, sample flow rate and volume, eluent concentration and volume were determined, interfering ions were studied, and the optimal experimental conditions were established. The adsorption capacity of nanometer-sized ZrO₂ for Mn, Cu, Cr, Zn, Ni and Co was found to be 1.3, 1.3, 1.7, 2.0, 3.9 and 1.5 mg g⁻¹, respectively. The detection limits of the method were 12, 58, 24, 2, 7 and 36 ng L⁻¹, respectively, with a preconcentration factor of 25. The precision of this method was 1.7% (Mn), 2.9% (Cu), 5.9% (Mn), 3.8% (Mn), 6.2% (Mn) and 4.3% (Mn) with 9 determinations of 10 ng mL⁻¹ of target analytes, respectively. The method was successfully applied to the determination of trace metals in lake water, dried fish samples, certified reference materials of human hair and milk, and provided satisfactory results.     

Analysis of organic pollutants in water at trace levels using fully automated solid-phase extraction coupled to high-performance liquid chromatography

Summary A method has been developed for the determination of trace levels of 32 pesticides, 19 explosives and 16 polycyclic aromatic hydrocarbons (PAH) in water in three individual steps. Solid-phase enrichment (SPE) is coupled to high-performance liquid chromatography (HPLC) with a fully automated system. The organic pollutants are enriched on reusable cartridges packed with adsorbent materials: pesticides and explosives on a mixed bed of divinylbenzene-ethylvinylbenzene copolymers (LiChrolut EN^?) and perfluorinated polyethylene (PolyF^?), and polycyclic aromatic hydrocarbons on C₁₈-modified silica (Zorbax^? ODS1). Thermally assisted desorption (TAD) has been shown to increase the recovery of analytes significantly. As all enriched analytes are transferred to the detector, only fifty millilitres of sample is needed for each single on-line analysis, compared with at least a litre for conventional methods. The separation of the enriched organic analytes is performed on specialized HPLC columns based on reversed-phase materials. The limits of detection of the system employed were found to be below 100 ng L⁻¹. Use of fluorescence detection for the polycyclic aromatic hydrocarbons resulted in limits of detection in the upper pg L⁻¹ range. Thek values, number of theoretical plates, the recovery rates and the limits of detection of this method for fast screening of organic pollutants from three fifty-millilitre aqueous samples are described. Presented at the 21^st ISC held in Stuttgart, Germany, 15^th–20^th September, 1996     

野生与种植青海川西獐牙菜中微量元素的测定

为了对比野生与种植青海川西獐牙菜中微量元素的变化,分别采集野生川西獐牙菜与种植青海川西獐牙菜种子采收前后的全植株,采用原子吸收光谱仪测定了其铜、锌、铁、锰、钴等微量元素含量。结果表明,野生川西獐牙菜较种植青海川西獐牙菜中微量元素含量高,种植川西獐牙菜在成熟种子采收后较采收前(花果期)铁、锰、钴、锌等元素含量高。     

人体血清中痕量铜的PAN分光光度法的测定研究

研究了用Cu2 -1-(2-吡啶偶氮)-2-萘酚(PAN)分光光度法测定人体血清中痕量铜的最佳条件。在HCl-KCl溶液介质中,十二烷基苯磺酸钠存在下,其表观摩尔吸光系数为1.42×104 L.mol-1.cm-1,Cu2 含量在0~2μg/mL范围服从比尔定律,检测限为0.5μg/dm3。操作简便、快速,该法可用于人体血清中痕量铜的测定。     

Analysis of microgram amounts of particulate material by simultaneous multiwavelength AES

A unique simultaneous emission spectrograph is utilized to perform qualitative and quantitative analysis on trace quantities of solid particulates. The atomic emission spectroscopic system consists of a direct current plasma source and an echelle spectrograph with a charge injection device detector, enabling the system to simultaneously measure the wavelength range from 220 nm to 520 nm with 0.02 nm resolution at 300 nm. Monitoring all wavelengths simultaneously allows the qualitative and quantitative determination of most major and minor constituent in a trace quantity of sample with little prior knowledge about the sample. The ability to perform qualitative and quantitative analysis on particulates is demonstrated by evaluating NBS certified coal fly ash, as well as a sample taken from the respirator air filter at an acute care unit in a hospital.Presented in part at the 1989 European Winter Conference on Plasma Spectrochemistry, Reutte, Austria     

Practical limitations of capillary gas chromatography

Glass capillary gas chromatography is a high resolution separation method which allows the qualitative and quantitative analysis of even complex mixtures, which may contain many components–also isomeric–in a wide range of volatilities, polarities and concentrations. The principal limitation of gas chromatographic application is given by an insufficient volatility of the species to be separated. Elevated temperatures have to be applied if the application range is to be extended and to achieve steep peak profiles, i.e. low detection limits at high resolution. The use of elevated temperatures is limited, of course, by the temperature stability of both the solvent (stationary liquid and support) and the solutes. The problems of trace analysis for low volatility compounds at high resolution and its limitational parameters regarding sampling, separation and detection are discussed. The applicability of glass capillary columns in this field is influenced by the following parameters: tailing behaviour; irreversible adsorption of polar and decomposition of unstable solutes; thermal stability of stationary liquid (including the support deactivation); separation efficiency and sample capacity (film thickness). Multidimensional gas chromatography using capillary columns coupled either with a packed or another capilllary column for preseparations may be applied with advantage in the analysis of complex mixtures.