水质凯氏氮标准样品的研究

提出了水质凯氏氮标准样品的研究方法。在研究过程中，完成了样品的配制、均匀性、稳定性等工作。经过多家实验室协作定值，确定了样品的标准值及不确定度，并提供使用。     

甲醇气体标准样品的研制

介绍了甲醇气体标准样品的制备和定值方法,考察采用重量法制备氮气中甲醇标准气体样品的重现性、标准气体的均匀性和稳定性.试验表明,甲醇气体标准样品在气瓶内均匀性良好,在12个月研制期间没有不稳定趋势.摩尔分数为149.2×10-6甲醇气体标准样品,扩展不确定度为3%,能够满足环境污染源废气中甲醇气体监测的要求.     

7种指示性多氯联苯混合标准样品量值不确定度研究

分析并评估了异辛烷中7种指示性多氯联苯(PCBs)混合标准样品的量值不确定度。通过分析PCBs纯品中结构相似物、水分、无机物等杂质的含量,采用质量平衡法对PCBs纯品的纯度进行了定值。结果显示,7种指示性PCBs纯品的纯度为98.24%~99.92%,纯度不确定度为0.08%~1.28%。采用称量-容量法制备了各组分浓度均为50.0 μg/mL的异辛烷中7种指示性PCBs混合标准样品,全面分析了各组分的量值不确定度来源,主要包括样品配制、均匀性和长期稳定性等引入的不确定度。结果表明,该标准样品中,7种指示性PCBs组分的合成扩展不确定度为0.7~1.7 μg/mL。该标准样品量值准确且具有计量溯源性,可为我国PCBs相关国际履约监测和新污染物监测提供有效支撑。     

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。     

砷、汞、镉质控混合水样的配制

本文讨论了质控混合水样的配制方法,叙述了质控样品的均匀性、稳定性试验及定值的原则和方法,详实地列出了有关统计检验方法。在现有实验室条件下,可以配制出满足监测工作需要的质量控制样品。     

农药厂周边有机磷农药在生物体中残留的检测方法研究

测定南京某农药厂附近大米、蔬菜及肉类中11种有机磷农药含量，通过使用气相色谱/质谱联用的方法，建立GC／MS定性定量分析方法，检出限达到0．05μg／kg（肉类）和0．1μg／kg（大米和蔬菜），回收率均符合测定要求。环境样品监测结果显示，大米和蔬菜中有机磷农药的含量高于肉类中的含量，说明在大米和蔬菜表面残留的农药量要高于进入生物体体内的含量。南京蔬菜样品中有机磷农药高于常州蔬菜样品，说明农药厂对蔬菜表面残留农药量有影响。不同的有机磷农药在不同的介质中，检出情况不一样，说明不同的环境介质对有机磷农药的保留水平不一样。     

苯胺环境标准样品研制中紫外分光光度法的应用

研究了苯胺弱酸性水溶液的紫外吸收特性,并将研究结果运用于苯胺水质标准样品的研制。用紫外分光光度法对标准样品进行均匀性、稳定性和定值测定,从而简化了分析手续,取得了良好的分析结果     

气相色谱法测定土壤中37种有机磷农药残留

采用气相色谱法测定土壤中37种有机磷农药,当取样量为10 g时,37种有机磷农药方法检出限为0. 002～0. 015 mg/kg,测定下限为0. 008～0. 060 mg/kg。低含量加标样品中有机磷农药的加标回收率为72. 8%～104%,相对标准偏差为4. 2%～13. 8%;中含量加标样品中有机磷农药的加标回收率为71. 5%～101%,相对标准偏差为4. 3%～13. 5%;高含量加标样品中有机磷农药的加标回收率为74. 6%～109%,相对标准偏差为6. 8%～14. 6%。该方法灵敏度高、分离效果好、重现性好,能够满足土壤中37种有机磷农药残留检测的要求。     

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.     

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。     

能力验证中总硬度标准品均匀性及稳定性分析

研究用氯化钙和硫酸镁配制总硬度标准品的均匀性和稳定性,根据《能力验证样品均匀性和稳定性评价指南》(CNAS-GL03:2006),随机抽取样品进行检验。结果表明,4种浓度的样品在p H值2,室温25℃时,样品内和样品间均无显著性差异,样品均匀性合格,在一年内稳定性较好。     

牡蛎中多环芳烃(PAHs)标准物质的研制

介绍了牡蛎中多环芳烃标准物质的研究、制备方法 ,进行了均匀性检验、稳定性检验 ,统计计算了检验结果 ,基本确定主要参数。检验结果表明 ,研制的牡蛎中难降解有机物标准物质均匀 ,在一年保存期间内稳定 ,可用于海洋环境监测中     

水质二硝基甲苯环境标准样品的研制

报道了水和废水环境监测所用水质二硝基甲苯环境标准样品的研制情况。其中对水质二硝基甲苯环境标准样品的作用、样品的制备、均匀性测定、稳定性考察以及定值分析等方面做了较详细的介绍。     

Homogeneity and stability study of the candidate reference material Adamussium colbecki for trace elements

The preparation of a new candidate certified reference material (CRM) for trace elements based on the antarctic bivalve Adamussium colbecki(IRMM 813) was carried out by the Istituto Superiore di Sanità(ISS, Rome, Italy) in cooperation with the Institute for Reference Materials and Measurements, Joint Research Centre of the European Commission (EC-JRC-IRMM), in the frame of the Italian National Programme of Research in Antarctica (Programma Nazionale di Ricerca in Antartide, PNRA). Samples were collected at Terra Nova Bay (Ross Sea) during the 2000-2001 expedition in Antarctica. The preparation of a material suitable for certification was performed by the EC-JRC-IRMM. Measurements for homogeneity and short-term stability tests were carried out by ISS. The elements selected for the certification project were As, Cd, Cu, Cr, Fe, Mn, Ni and Zn. For the above-mentioned tests, the determination of the elements of interest was performed on samples mineralised by microwave-assisted acid digestion. The analytical techniques employed to this end were inductively coupled plasma atomic emission spectrometry (ICP-AES) and inductively coupled plasma dynamic reaction cell quadrupole mass spectrometry (ICP-DRC-Q-MS). The candidate material was shown to be fit for purpose with regard to homogeneity and short-term stability, thus allowing the following phases of the certification project to be undertaken, in the first place the selection of expert laboratories for the accomplishment of the certification campaign.     

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。     

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).     

Effects of sampling techniques on physical parameters and concentrations of selected persistent organic pollutants in suspended matter

This study focusses on the effect of sampling techniques for suspended matter in stream water on subsequent particle-size distribution and concentrations of total organic carbon and selected persistent organic pollutants. The key questions are whether differences between the sampling techniques are due to the separation principle of the devices or due to the difference between time-proportional versus integral sampling. Several multivariate homogeneity tests were conducted on an extensive set of field-data that covers the period from 2002 to 2007, when up to three different sampling techniques were deployed in parallel at four monitoring stations of the River Rhine. The results indicate homogeneity for polychlorinated biphenyls, but significant effects due to the sampling techniques on particle-size, organic carbon and hexachlorobenzene. The effects can be amplified depending on the site characteristics of the monitoring stations.     

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.