水质常量分析中固体标准物质的研制及质量控制

主要介绍固体标准物质的研制过程,包括标准物质的混合比设计,混合后均匀性检验,标准物质的定值方法、稳定性的周期检验以及应用质控图的方式对分析进行分析过程的质量控制。     

五氯酚、对硝基酚、对甲基酚环境标准样品的研制

化学纯的五氯酚经纯化处理后得到高纯物质,对硝基酚、对甲基酚选用进口高纯物质;采用重量法配制,以甲醇作为标准样品溶剂,经过均匀性、稳定性检验和多家高水平的实验室用气相色谱、液相色谱等方法定值、数理统计检验,给出了标准样品的标准值和不确定度.     

室内空气污染监测用氨标准样品研究

根据中国对室内空气污染监测的实际需要,介绍了室内空气污染监测用氨标准样品的研制方法,包括试剂的验证、均匀性和稳定性检验、分析定值和测定数据的统计检验等方面。氨标准样品采用重量法制备,用纳氏试剂分光光度法对样品进行均匀性和稳定性研究,并进行不确定度评估。研究结果表明,氨标准样品的均匀性良好,室温条件下可稳定18个月以上;在全面分析不确定度来源的基础上,定值结果为0.494 mg/L,不确定度小于3%。与美国同类标准物质进行比对分析,结果具有可比性。可用于氨测定的质量控制、分析方法评价以及实验室能力验证等方面。     

牡蛎生物环境标准样品的研制

文章对我国环境保护系统研制出用于海洋和江河水域环境监测的牡蛎生物环境标准样品的一些情况做了详细介绍;尤其对牡蛎环境标样的制备过程,牡蛎标样的作用,均匀性、稳定性检测和分析定值进行了较为充分的论述。     

三氯甲烷中有机磷农药混合标准样品的研制

确立了三氯甲烷中有机磷农药混合标准样品的制备、分析和定值方法，进行了标准样品的均匀性检验、稳定性监测及协作定值数据的不确定度评价。结果表明，三氯甲烷中有机磷农药混合标准样品的均匀性良好，至少在18个月的时间内稳定。     

实验室质量控制的探讨

对校准曲线的检验、加标回收率分析和标准物质对比等三个方面进行了讨论,分析了实验室质量控制中存在的问题,提出了改进意见。     

臭氧前驱体物监测用氮气中多组分VOCs气体标准物质的研制

介绍了瓶装1μmol/mol臭氧前驱体物监测用氮气中57组分挥发性有机物(VOCs)气体标准物质的研制过程,该气体标准物质严格按照《气体分析 校准用混合气体的制备 第1部分:称量法制备一级混合气体》(GB/T 5274.1-2018)所规定的配制气体标准物质的方法采用称量法制备。建立了GC-MS联用结合选择离子扫描(SIM)的分析方法,研究了目标化合物在气瓶中的均匀性和稳定性。57种目标化合物完全满足美国环保署光化学评估监测站(PAMS)关于臭氧前驱体物VOCs在线监测的技术要求。将气体标准物质分别送至中国环境监测总站和英国国家物理实验室(NPL)进行比对分析,结果良好,表明研制的气体标准物质具有较好的压力均匀性和稳定性,符合使用要求。相对扩展不确定度为5%(k=2),使用有效期为1年,取得国家二级标准物质证书,证书编号为GBW(E)083966。     

苯系物环境标准样品的研制

苯系物标准样品包括苯、甲苯、乙苯、二甲苯和异丙苯.用气相色谱、质谱、付立叶红外确定化合物纯度,重量法配制,经均匀性、稳定性、多家定值、数理统计检验确定标准样品的标准值和不确定度.     

硫化物溶液标准物质的研究

研究了硫化钠配制标准溶液不稳定的原因,制备出稳定一年的硫化物溶液标准物质.它均匀,定值结果准确,浓度范围50～100μg/ml(S2-计).     

海洋沉积物基质多环芳烃标准参考物质的原料样品制备研究

海洋沉积物基质多环芳烃(PAHs)标准参考物质是海洋环境沉积物监测分析中质量控制和质量保证的重要保障。由于缺少对相关原料样筛选研究,目前我国尚未有自主制备的海洋沉积物基质PAHs标准参考物质。通过海洋沉积物原始数据调研、定点筛查、实验室间验证等手段,对江苏近岸海域海洋沉积物原料样进行筛选研究。结果表明,连云港赣榆某入海口点位的海洋沉积物样品∑PAHs的质量分数为413μg/kg,该样品各粒径中的PAHs质量分数分布均匀,精密度能够满足我国海洋沉积物环境监测质量控制需求,可以为进一步制备海洋沉积物PAHs标准参考物质提供技术支持。     

Preparation and evaluation of candidate certified reference materials (CRMs) for nutrients in seawater

Certified reference materials (CRMs) are an essential part of the quality assurance (QA) necessary for the reliable analytical measurement of nutrients in seawater. The CRMs currently available for these analyses are not matrix matched to marine samples. QUASIMEME routinely produces test materials for the nutrients in seawater and nutrients in estuarine water and low-salinity open water Laboratory Performance Studies (LPS) that are both homogeneous and stable. QUASIMEME, in conjunction with Eurofins Scientific, Denmark have produced two reference materials (RMs). The homogeneity testing and preliminary stability studies were carried out by QUASIMEME, and the results are presented in this article. Participants of the QUASIMEME LPS who demonstrated satisfactory long-term performance for the analysis of nutrients in seawater and nutrients in estuarine water and low-salinity open water were invited to take part in the certification exercise. Twenty laboratories returned data, a summary of which is also presented. The certification and long-term stability testing and additional data analysis were carried out by Eurofins Scientific, Denmark, and are outwith the scope of this article and not reported here. Eurofins Scientific, Denmark have marketed these RMs as part of their range of VKI Reference Materials (further information is available from eurofins@eurofins.dk).     

硫化物水样的稳定性研究

对硫化钠水样的制备及其稳定性进行了研究和讨论,找到一种长期稳定保存硫化钠标准溶液及硫化物标准样品的有效方法。     

我国环境标准样品发展及应用

环境标准样品广泛应用于我国的环境监测活动中,为监测数据的一致性、可比性和准确性提供了重要的技术支撑。该文综述了环境标准样品发展及应用现状,根据国外环境标准样品体系分析了我国环境标准样品体系存在的问题,并对环境监测工作中环境标准样品应用问题提出了相关建议,为环境监测工作者认识和使用环境标准样品提供了指导。     

Two fish bile reference materials certified for PAH metabolites

Environmental pollution with polycyclic aromatic hydrocarbons (PAHs) from pyrogenic or petrochemical sources is a matter of concern in many aquatic ecosystems. For field monitoring purposes, PAH metabolite levels in fish bile samples can be used as biomarkers of exposure, but previously there were no reference materials for analytical method validation or quality control. In this paper we describe the preparation and certification of two fish bile materials. BCR 720 is a pure bile material from sediment-exposed flounder (Platichthys flesus) and BCR 721 is a pure bile material from oil-exposed plaice (Pleuronectes platessa). Homogeneity and stability tests were carried out and a group of 12 expert laboratories was assembled for the certification measurements. The methods applied were liquid chromatography with fluorescence detection or gas chromatography with mass spectrometric detection. In BCR 720 three PAH metabolites were certified: 1-hydroxyphenanthrene, 1-hydroxypyrene and 3-hydroxybenzo[a]pyrene. In BCR 721 1-hydroxypyrene was certified. The fourth target compound, 2-hydroxynaphthalene, could not be certified, but the results obtained are listed. The major findings from earlier feasibility studies and recommendations for the optimal use of the reference materials are also included.     

X射线荧光光谱法测定土壤样品中铅的不确定度评定

用实例对X射线荧光光谱法测定土壤样品中铅的不确定度进行了评定.测量结果的不确定度由仪器综合稳定性、制样、标准物质、回归工作曲线、重复测量等所引入的不确定度分量组成.在对各个不确定度分量进行量化的基础上,通过合成得到测量结果的标准不确定度,再乘以95%置信概率下的扩展因子2,得到测量结果的扩展不确定度.     

标准物质在环境应急监测定量分析中的作用

以环境空气中挥发性有机物(VOCs)监测为例,比较分析了标准物质在应急监测、实验室定量分析,以及应急监测定量、半定量分析中的作用。结果表明,在有标准物质进行定量校准时,应急监测方法和实验室标准分析方法的定量结果具有可比性;在无标准物质进行半定量分析时,应急监测结果可能存在较大误差。提出,在需准确定量的应急监测中应使用标准物质进行校准,以保证监测结果的准确性。     

A new organic-rich soil reference material certified for its EDTA- and acetic acid- extractable contents of Cd, Cr, Cu, Ni, Pb and Zn, following collaboratively tested and harmonised procedures

There is an increasing requirement for assessment of the bioavailable metal fraction and the mobility of trace elements in soils upon disposal. One of the approaches is the use of leaching procedures, but the results obtained are operationally defined; therefore, their significance is highly dependent on the extraction protocol performed. So, for this type of study, there is a need for reference materials that allow the quality of measurements to be controlled. This paper describes the steps involved in the certification of an organic-rich soil reference material, BCR-700, for the EDTA- and acetic acid-extractable contents of some trace elements, following collaboratively tested and harmonised extraction procedures. Details are given for the preparation of the soil, homogeneity and stability testing, analytical procedures and the statistical selection of data to be included in the certification.     

Evaluation of old landfills--a thermoanalytical and spectroscopic approach

Abandoned landfills and dumps, where untreated waste materials were deposited in the past, are a main anthropogenic source of relevant gaseous emissions. The determination of stability is a crucial target in the context of landfill risk assessment. FTIR spectroscopy and simultaneous thermal analysis in association with multivariate statistical methods were applied to landfill materials in order to get information on the kind of waste and its reactivity. The spectral and thermal patterns are fingerprints of the material. Industrial waste and the material from a 5-year-old reactor landfill were distinguished from the defined classes of mechanically-biologically treated ("MBT") waste and 30 to 40-year-old stable landfills containing municipal solid waste and construction waste ("LF") by a classification model based on soft independent modeling of class analogy (SIMCA). Degradation experiments were carried out with the fresh material originating from one MBT plant that was subjected to aerobic and anaerobic conditions in lab-scale reactors. These samples were compared to samples of one reactor landfill and to the landfill fraction from the MBT plant to demonstrate the efficiency of the biological pretreatment before final disposal. Prediction models that are based on spectral or thermal characteristics and the corresponding reference analyses were calculated by means of a partial least squares regression (PLS-R). The developed models of the biological oxygen demand (BOD) and the dissolved organic carbon (DOC) were based on spectral data, the models of the total organic carbon (TOC) and total nitrogen (TN) were based on thermal data (heat flow profiles and mass spectra of combustion gases). Preliminary results are discussed. The enthalpy of the materials decreases with progressing mineralization, whereas the enthalpy of the remaining organic matter increases. The ratio of the enthalpies was used as an indicator of stability. Selected samples comprising old landfills, a recent reactor landfill, MBT landfills and MBT materials were classified according to the calculated ratios.     

Certification of the extractable contents of Cd, Cr, Cu, Ni, Pb and Zn in a freshwater sediment following a collaboratively tested and optimised three-step sequential extraction procedure

Sequential extraction procedures have been used during the last decades to study and determine trace element mobility in aquatic sediments. However, the results obtained are operationally defined and, therefore, the significance of the analytical results is related to the extraction scheme used. So, there is a need for suitable reference materials for this type of study to enable the validation of the methodologies and to control the quality of the measurements. This paper describes the preparation of a sediment reference material, BCR-701, the homogeneity and stability studies and the analytical work performed for the certification of the extractable contents of some trace elements, following a collaboratively tested and optimised sequential (three-step) extraction procedure. The paper contains all the results and gives the methods used to certify the extractable contents (mass fractions expressed as mg kg-1 on a dry matter basis) of Cd, Cr, Cu, Ni, Pb and Zn in all steps. Moreover, indicative values are given for the aqua regia extractable contents of the six elements in the sediment and the residue obtained after sequential extraction.     

Application of laser-based ion mobility (IM) spectrometry for the analysis of polycyclic aromatic compounds (PAC) and petroleum products in soils

The capability of laser-based IM spectrometry to detect PAC and petroleum products (oils) in model matrices, laboratory reference (LR) materials and in real-world contaminated soil samples was demonstrated. Quantitative IM investigations of PAC-doped PVC films yielded detection limits in the ppm range for single PAC. The potential of IM spectrometry for in situ analysis was demonstrated by the analysis of PAC-containing certified reference (CR) material, and of petroleum product-containing LR materials and real-world soil samples. The calibration of IM signals obtained from oil-doped LR materials was also possible, and detection of oils with concentrations below 100 mg kg(-1) was achieved. The in situ analysis of real-world contaminated soils with the IM and LIF techniques was in good accordance with ex situ reference investigations.