Ultrasound-assisted emulsification solidified floating organic drop microextraction for the determination of trace amounts of copper in water samples

A simple and efficient liquid-phase microextraction (LPME) technique was developed using ultrasound-assisted emulsification solidified floating organic drop microextraction (USAE-SFODME) combined with flame atomic absorption spectrometry, for the extraction and determination of trace copper in water samples. 1-(2-Pyridylazo)-2-naphthol (PAN) was used as chelating agent. Microextraction efficiency factors (including extraction solvent type, extraction volume, time, temperature, and pH), the amount of the chelating agent, and salt effect were investigated and optimized. Under the optimum extraction conditions, figures of merit of the proposed method were evaluated. The calibration graph was linear in the range of 20–600 mg·L⁻¹ with a detection limit of 0.76 mg·L⁻¹. The relative standard deviation (R.S.D) for ten replicate measurements of 20 and 400 mg·L⁻¹ of copper was 3.83% and 2.65%, respectively. Finally, the proposed method was applied to tap water, river water, and sea water, and accuracy was assessed through the analysis of certified reference water or recovery experiments.     

Atmospheric measurements of the halogenated hydrocarbons involved in global change phenomena

Chlorofluorocarbons and their replacement compounds are anthropogenic compounds of great environmental concern. For this reason monitoring their atmospheric mixing ratios on a worldwide scale is recommended. An analytical methodology for the simultaneous determination of selected chlorofluorocarbons and their replacement compounds has recently been developed. This methodology was applied in the analysis of actual air samples collected in remote and semi-remote areas located in the Northern and Southern Hemispheres. The concentration levels measured in the air samples collected in the two hemispheres are reported.     

Enrichment of elements in industrial waste incineration bottom ashes obtained from three different types of incinerators,as studied by ICP-AES and ICP-MS

The elemental composition of the industrial waste incineration bottom ash (IWIBA) samples collected from three different types of incinerator with different kinds of wastes were compared. The major-to-ultratrace elements in the IWIBA samples were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES) and inductively coupled plasma mass spectrometry (ICP-MS). As a result, ca. 40 elements in the concentration range from milligrams per gram to submicrograms per gram could be determined with relative standard deviations of less than 5%. The IWIBA sample from petrochemical wastes contained lower concentrations of the elements, because fewer mineral constituents were contained in the input waste materials. On the contrary, the elemental concentrations in the IWIBA sample from industrial solid wastes provided the highest values for most elements, while the elemental compositions of the IWIBA sample from food wastes were similar to those of municipal solid waste incineration bottom ash. In addition, it was found from the analytical results that the levels of various heavy metals such as Cr, Mn, Fe, Ni, Cu, As, Zr, Mo, Sb, Ba, and Pb were higher in the IWIBA samples than in municipal solid waste incineration bottom ash. The enrichment factors of the elements in the IWIBA samples were estimated from the analytical results to compare the elemental distributions in incineration bottom ashes in relation to their mining influence factors, which are the indices for human use of the elements.     

原子荧光光谱法测定汞的方法探讨

采用原子荧光光谱仪测定标准样品扇贝粉、土壤和水中的汞过程中,用固定液代替稀释液。结果表明,该方法减少系统误差,提高分析精密度,准确可靠,能满足食品、土壤和水中汞的监测。检出限为0．004μg/L,相对标准偏差为小于3．19％,回收率为95％～103％。     

L-半胱氨酸预还原-氢化物发生-原子荧光光谱法测定水中的锑

在稀H：sO。介质中,以L-半胱氨酸作预还原剂,用氢化物发生-原子荧光光谱法测定水中的锑。L-半胱氨酸的存在,改善了氢化物发生条件和增敏光谱测定信号,当在低酸度下发生锑的氢化物时,过渡金属离子的干扰显著地得到了抑制,灵敏度提高,方法的检出限为0．13μg／L,回收率为92．5％～106．5％。     

Releases of phosphate fertilizer industry in the surrounding environment: Investigation on heavy metals and polomum-210 in soil

Distribution of Cu,Zn,Pb,Cr,Ni,Mn concentrations and the activity of polonium-210 in the surrounding area of a phosphate fertilizer industry located on the eastern coast of the Mediterranean Sea has been determined.Nineteen sampling sites were distributed around the industrial zone on a surface area of about 100,000 m2.Atomic absorption spectroscopy and Alpha spectroscopy were used to quantify the heavy elements and polonium-210,respectively.Investigation on a particle scale was conducted by TEM and SEM coupled to EDX and X-ray cartography to determine the nature of heavy elements carders and their distribution.Heavy elements were mainly concentrated inside the particle size fraction ＜ 50μm.Their levels decreased with distance increasing from the industry.According to the reference soil,enrichment factors were about 10,15,32 and 100 times for Zn,Pb,Cu,and Cr,respectively inside the particle size fraction ＜ 50 μm on the closest sites to the industry.The main contaminant sources were transport and storage of row materials and the free release of phosphogypsum waste.Heavy elements were entrapped inside agglomerates of sulfates,phosphates and iron oxihydroxides in a diffused shape.Polonium-210 with an enrichment factor of about 56,showed the same behavior of the spatial distribution of the trace elements.     

水中铅的测定——流动注射氢化物原子吸收光谱法

目前水质分析部门对测定水中铅一般采用双硫腙比色法和原子吸收光谱法这两种方法,但都需要萃取、分离富集等繁琐的操作手段,分析时间长,用样品量大,有机溶剂污染环境等弊端。本文采用流动注射、氢化物原子吸收测定铅,它具有分析速度快、灵敏度等优点,回收率在95%-102%。     

湘江重点城市饮用水源地挥发/半挥发有机污染物调查与分析评价

采用气相色谱质谱仪（GC-MS）对湘江流域长沙、株洲、湘潭、岳阳等8个重点城市生活饮用源地水质中挥发/半挥发性有机物进行了分析,结果表明,8个重点城市饮用水源地水质中108种挥发和半挥发性有机物均未检出,含量均处在较低水平。对湘江流域有机污染物来源进行了调查分析,提出了加强有机污染物排放监测和控制管理,并定期对地表水中有机污染物进行监测的必要性。     

Improved preparation and identification of aristolochic acid-DNA adducts by solid-phase extraction with liquid chromatography-tandem mass spectrometry

Aristolochic acid (AA) is a known nephrotoxin and potential carcinogen, which can form covalent DNA adducts after metabolic activation in vivo and in vitro. A simple method for preparation and characterization of aristolochic acid-DNA adducts was developed. Four AA-adducts were synthesized by a direct reaction of AAI/AAII with 2’-deoxynucleosides. The reaction mixture was first cleaned-up and pre-concentrated using solid phase extraction (SPE), and further purified by a reversed-phase high performance liquid chromatography (HPLC). By the application of developed SPE procedure, matrices and byproducts in reaction mixture could be greatly reduced and adducts of high purity (more than 94% as indicated by HPLC) were obtained. The purified AA-DNA adducts were identified and characterized with liquid-electrospray ionization-quadrupole-time of flight-mass spectrometry (LC-ESI-Q-TOF-MS/MS) and LC-Diode array detector-fluorescence (LC-DAD-FL) analysis. This work provides a robust tool for possible large-scale preparation of AA-DNA adduct standards, which can promote the further studies on carcinogenic and mutagenic mechanism of aristolochic acids.     

原子吸收法测定水中锰的质量控制指标研究

通过全国17个省份69家实验室的监测数据分析,研究确定了原子吸收法测定水中锰的质量控制指标和重复性限、再现性限,建议控制值为：浓度在0。1～3mg／L范围内的标准样品,控制RSD≤4％,RSD≤10％,RD≤5％,RE≤±10％;浓度在0．01—25mg／L范围内的实际样品,控制RD≤7％;同时,建议加标回收率控制在90％～110％。