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色谱/质谱联用技术分析测定贻贝中的多环芳烃 总被引:5,自引:0,他引:5
介绍了GC-MS联用技术-物质征离子选择法测定贻贝中多环芳烃的分析方法,并就定性定量离子的选择,以及方法的准确度和精密度进行了探讨。结果表明,本方法适用于海洋生物贻贝,牡蛎中PAHs的分析测定。 相似文献
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采用重量-容量法制备丙酮中除虫脲溶液标准物质。准确称量国家二级标准物质除虫脲溶解到色谱纯丙酮中,通过A级容量瓶定容至500 mL,摇匀后分装到2 mL安瓿瓶内共460瓶,每瓶为1 mL,保持低温迅速封口,配制过程中室温保持在(20±2)℃。采用液相色谱法进行均匀性、稳定性检验和定值结果验证。从样品中随机抽取16瓶进行均匀性检验,经F检验表明,在95%的置信区间范围内该标准物质均匀性良好;采用t检验对标准物质稳定性进行检验,标准物质在12月内稳定性良好。对该标准物质的不确定度进行了评定,研制的丙酮中除虫脲溶液标准物质定值结果为100μg/mL,相对扩展不确定度为2%(k=2)。结果表明,该标准物质均匀性与稳定性良好,量值准确,可用于日常分析检测中的方法评价和仪器校准。 相似文献
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Liping Fang Wei Wang Haiping Liu Henan Qiu Yaxian Zhao Bingwen Lu 《International journal of environmental analytical chemistry》2015,95(10):879-893
Two freshwater sediments certified reference materials (CRMs) for 16 polycyclic aromatic hydrocarbons (PAHs) have been developed by the Institute for Environmental Reference Materials (IERM) of Ministry of Environmental Protection (MEP) in China. The methodology for preparing the CRMs of PAHs in sediments is described in this paper. The collected natural sediment samples were air-dried, ground, homogenised, packed, sterilised and tested on stability and homogeneity. Homogeneity results showed that the between-unit variation was confirmed to be below 4.5% for each compound. Stability was assessed after storage of samples for 16 months at temperature less than 30°C and in shade. The certification of the natural sediment matrix CRMs for PAHs was based on the agreement of results using different analytical techniques including gas chromatography/mass spectrometry (GC/MS) and reversed-phase liquid chromatography (LC) by no less than eight collaborating laboratories including IERM. Results of the homogeneity showed that the calculated ubb′ was 0.9–2.5% for environmental river standard-4 (ERS-4) and 9–2.3% for environmental lake standard-1 (ELS-1), whereas stability results of total 16 PAHs indicated that the calculated urel,lts was 4.2% for ERS-4 and 2.2% for ELS-1. Certified values of 16 PAHs in ERS-4 varied from 8.5 to 167 μg/kg and ranged from 0.036 to 2.8 mg/kg in ELS-1.The good comparability, together with the independent confirmation of the assigned mass fraction by using different methods, confirmed that the CRMs are suitable for the method validation and quality control in soil or sediments analysis. 相似文献
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Patricia Navarro Luis Bartolomé Juan Carlos Raposo Olatz Zuloaga Gorka Arana Nestor Etxebarria 《Analytica chimica acta》2010,675(1):91-96
Due to high cost of certified reference materials (CRMs), reference materials (RMs) are preferred to check the method performance in environmental analysis. In this work, a laboratory reference material (LRM) was prepared and characterised to carry out the quality control in monitoring analysis of eight polycyclic aromatic hydrocarbons (PAHs) and nine trace metals in mussel tissue. Mussels were collected in a naturally polluted area. Before the reference material was bottled, the mussel tissue was stabilised by freeze-drying, ground and sieved. For the material characterisation, several statistical tests were applied to check the homogeneity of the analytes in the tissue, and a stability test was performed to study the effect of the storage temperature in the analyte concentration. Other characteristics such as specific density, moisture and lipid contents as well as particle size distribution of the material were determined. Although the LRM had a homogeneous distribution for all PAHs and almost all metals, the stability study showed different results at both storage temperatures studied. For both PAHs and trace metals, the material was suitable to assure the quality control of the analysis. 相似文献
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To confirm the method for preparing artificially spiked soil with polycyclic aromatic hydrocarbons (PAHs), we tested the homogeneity of PAHs in spiked soils, which were prepared by three different procedures, by using kaolin and ando soil. When the slurry of kaolin and acetone containing PAHs were evaporated by a rotary evaporator at 30 - 35 degrees C, the most homogeneous distribution of PAHs was obtained in the spiked soil. This procedure was applied to the preparation of PAH-spiked soil for natural soil (ando soil). Such spiked soils can be useful as the standard materials for standardization of the analytical methods for PAHs in the soil and sediment samples. 相似文献
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稀土矿石成分分析标准物质的研制 总被引:1,自引:0,他引:1
介绍两种稀土矿石成分分析标准物质的研制过程。采用X射线荧光光谱法检验标准物质的均匀性和稳定性,标准物质的均匀性和稳定性良好。由8家具有权威性的测试单位协同定值及对数据进行数理统计,确定了该标准物质的标准值及标准偏差。 相似文献
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Saioa Elordui-Zapatarietxe Ina Fettig Janine Richter Rosemarie Philipp Guido Vanermen Els Monteyne Gerard Boom Håkan Emteborg 《Accreditation and quality assurance》2016,21(2):113-120
We have prepared and evaluated three whole water test materials containing eight polycyclic aromatic hydrocarbons (PAHs), six polybrominated diphenyl ethers (PBDEs) and tributyltin (TBT) with respect to homogeneity and short-term stability. The test materials were used as samples in two inter-laboratory comparisons. The materials were composed of natural mineral water and model suspended particulate matter (SPM) containing the target compounds at ng L?1 levels. The expanded uncertainty of the estimated mass concentrations in the final test materials was obtained by combining contributions from the homogeneity, the stability and the model SPM characterization. The whole water materials were sufficiently homogeneous and stable at 4 °C for their intended use. In total, 12 out of 15 investigated target parameters could be assessed to be present with a relative combined expanded uncertainty below 25 %. The outcome of the two inter-laboratory comparisons confirmed the good quality of the test materials and the level of uncertainties associated with the estimated mass concentrations. These findings are an important contribution towards the development of whole water matrix reference materials certified for PAH, PBDE and TBT in support of the Water Framework Directive of the European Union. 相似文献
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A fiber coating from polyaniline (PANI) was electrochemically prepared and employed for solid phase microextraction (SPME) of some polycyclic aromatic hydrocarbons (PAHs) from water samples. The PANI film was directly electrodeposited on the platinum wire surface in sulfuric acid solution using cyclic voltammetry (CV) technique. The applicability of this coating was assessed employing a laboratory-made SPME device and gas chromatography with mass spectrometry (GC-MS) for the extraction of some PAHs from the headspace of aqueous samples. Application of wider potential range in CV led to a PANI with more stability against the temperature. The homogeneity and the porous surface structure of the film were examined by the scanning electron microscopy (SEM). The study revealed that this polymer is a suitable SPME fiber coating for extracting the selected PAHs. Important parameters influencing the extraction process were optimized and an extraction time of 40 min at 40 degrees C gave maximum peak area, when the aqueous sample was added with NaCl (20%, w/v). The synthesis of the PANI can be carried out conveniently and in a reproducible manner while it is rather inexpensive and stable against most of organic solvents. The film thickness of PANI can be precisely controlled by the number of CV cycles. The resulting thickness was roughly 20 microm after 20 cycles. At the optimum conditions, the relative standard deviation (RSD) for a double distilled water spiked with selected PAHs at ppb level were 8.80-16.8% (n = 3) and detection limits for the studied compounds were between 0.1-6 pg mL(-1). The performance of PANI was, also, compared with a commercial solid coated-based SPME fiber, carbowax/divinylbenzene (CW/DVB), under similar experimental conditions. 相似文献