标准物质在检测实验室质量控制中的应用

【】 本文介绍了检测中使用标准物质进行质量控制的重要意义,分别在盲样测试、期间核查和质量控制图应用方面提出了使用标准物质进行质量控制的三种方法,并通过在实验室获得的检测数据对上述应用方法作了实例说明,对检测实验室应用标准物质进行质量控制工作具有指导意义。     

酶标分析仪波长标准物质的研制

以硫化锌为高折射材料和冰晶石为低反射材料,利用真空镀膜技术、光学极值法检测膜厚技术镀制了窄带全介质干涉滤光片,K9玻璃为薄膜保护层,采用切割、粗磨、精磨、抛光、镀膜等光学工艺制得酶标分析仪波长标准物质,经均匀性、稳定性考核合格后,由紫外可见近红外分光光度计标准装置对标准物质定值。研制的酶标分析仪波长标准物质定制结果扩展不确定度为0.7 nm(k=2),使用方便,量值准确、稳定,技术指标满足酶标分析仪波长示值误差及重复性检定/校准工作的需要。     

Intralaboratory Quality Control of Chemical Analysis with Reference Materials at Disposal

In this problem-oriented article, regarding the author's experience, a review of the methods of intralaboratory quality control based on systematic analysis of reference samples (control materials) is given. The requirements imposed on reference samples are briefly considered. The principles of selection of an inspection plan and the requirements on the evaluation period of statistical characteristics are formulated. The techniques for graphically representing the results of intralaboratory control and the algorithms for detecting out-of-control analytical processes are considered. Control charts for average values and ranges or charts for cumulative sums and geometric (exponentially weighted) moving averages are recommended as the main or auxiliary graphical representation, respectively. Westgard rules and the simplest rules for ranges are recommended as the main algorithms for revealing out-of-control analytical processes. Multivariate statistical process control methods, which are recommended for use in the cases of a great number of simultaneously determined factors, are briefly discussed.     

焦炭特性及成分分析用标准物质的研制

介绍焦炭特性及成分分析用标准物质的研制过程。对标准物质进行了均匀性检验和稳定性考察,8家权威实验室用准确可靠的方法参与协作定值,确定了22个项目的标准值和扩展不确定度。粒度分析和成分分析结果表明该标准物质均匀性良好,在5年内性质稳定。     

化肥成分分析系列标准物质研制

研制了尿素、磷酸氢二铵、氯化钾、高氮磷低氯复合肥、高氮低氯复合肥、高钾硫基复合肥、高钾中氯复合肥、高磷低氯复合肥和平衡型硫基复合肥系列化肥标准物质,样品严格按照相关标准要求进行采集、加工制备、均匀性检验、稳定性检验,由15家不同行业的权威实验室进行协作定值,并对不确定度进行评定。结果表明,样品粒度分布满足样品加工要求,具有良好的均匀性和稳定性。本系列化肥标准物质共定值45项元素(指标),包括N、P_2O_5、水溶性P_2O_5、有效性P_2O_5、K_2O、S、Cl、As、Hg、Cr、Cd、Cu、Pb、Zn、Ni、B、Se、Ge、Fe、Na、Ca、Mg、Al、Ti、V、Mn、Co、Sr、Mo、Ba、Y、La、Ce、Pr、Nd、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu,量值准确可靠、不确定度范围评估合理,符合国家一级标准物质的要求。研制的9个化肥化学成分标准物质定值的元素含量梯度范围合理,填补了国内复合肥料标准物质空白,可为化肥样品分析质量控制、实验室仪器校准、分析方法和实验室检测能力验证与评价提供基础技术支撑。     

铝合金化学成分标准物质的研制

介绍铝合金化学成分标准物质的研制过程。采用中频感应电炉熔炼法制备了铝合金化学成分标准物质候选物,并对标准物质候选物的均匀性和稳定性进行了考察。选择6家具有资质的实验室对研制的标准物质中各化学成分进行协作定值,并对各元素定值的不确定度进行评定。结果表明,在95%的置信区间内标准物质均匀性良好,经过13个月稳定性考察试验,标准物质稳定性良好。Si,Fe,Cu,Mn,Mg,Ti,Cd,V,Zr,B,Sn,Zn的定值结果分别为0.013 8%,0.012 5%,2.868%,0.185%,0.014 0%,0.082 8%,0.041 7%,0.032 9%,0.031 4%,0.003 8%,0.003 4%,0.025 6%,定值结果的相对扩展不确定度为1.4%~9.0%(k=2)。研制的标准物质达到相关技术要求,可用于该类铝合金材料的质量控制。     

化肥成分分析系列标准物质研制

研制了尿素、磷酸氢二铵、氯化钾、高氮磷低氯复合肥、高氮低氯复合肥、高钾硫基复合肥、高钾中氯复合肥、高磷低氯复合肥和平衡型硫基复合肥系列化肥标准物质,样品严格按照相关标准要求进行采集、加工制备、均匀性检验、稳定性检验,由15家不同行业的权威实验室进行协作定值,并对不确定度进行评定。结果表明,样品粒度分布满足样品加工要求,具有良好的均匀性和稳定性。本系列化肥标准物质共定值45项元素(指标),包括N、P₂O₅、水溶性P₂O₅、有效性P₂O₅、K₂O、S、Cl、As、Hg、Cr、Cd、Cu、Pb、Zn、Ni、B、Se、Ge、Fe、Na、Ca、Mg、Al、Ti、V、Mn、Co、Sr、Mo、Ba、Y、La、Ce、Pr、Nd、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu,量值准确可靠、不确定度范围评估合理,符合国家一级标准物质的要求。研制的9个化肥化学成分标准物质定值的元素含量梯度范围合理,填补了国内复合肥料标准物质空白,可为化肥样品...     

在环境科学与生命科学研究中广泛应用的元素形态分析研究进展

按测试方法分类,包括电化学分析方法、毛细管电泳法,分子活化分析法,计算机模拟以及以气相色谱、高效液相色谱,流动注射等为基础的联用技术,对近lO年来广泛应用于环境与生命科学的国内外元素形态分析研究进展进行了综述。     

New Data on Sixteen Reference Materials Obtained by INAA

We report instrumental neutron activation analysis results for 15 elements (K, Fe, Sc, Cr, Co, Zn, As, Rb, Sb, Cs, Ba, Hf, Ta, Th, and U) in 16 geochemical reference samples, namely SDC-1, SCo-1, SGR-1, STM-1, RGM-1, BIR-1, MAG-1 and BHVO-1 from USGS (United States Geological Survey, Reston), Soil-5, Soil-7 and SL-1 from IAEA (International Atomic Energy Agency, Vienna), and GSS-1, GSS-4, GSS-7, GSR-2 and GSR-3 from IGGE Institute of Geophysical and Geochemical Prospecting, People's Republic of China), The results are compared with literature values. In general our results agree well with recommended or proposed values.     

New Arctic Marine Sediment Certified Reference Material for Elemental Analysis

A multi-elemental certified reference material (CRM) based on Arctic marine sediment was prepared and labeled GBW 07481. Approximately 4.5?kg of the sediment was collected during the third Chinese Arctic Expedition. The sediment was processed in procedures that included air drying, debris removal, drying, and milling. The final product contained particles that were generally smaller than 74?;m representing 99% of the total mass. The powder was poured into clean 10-mL brown glass vials and a total of 300 vials were obtained. The homogeneity and stability were preliminarily investigated to assess the suitability of the marine sediment as a candidate CRM. The candidate material was demonstrated to be suitable for this purpose; and hence the certification project was accomplished with nine reputable laboratories. More than 10 reliable analytical methods, including inductively coupled plasma-mass spectrometry (ICP-MS), inductively coupled plasma-atomic emission spectrometry (ICP-AES), and x-ray fluorescence (XRF), were used for analyzing the sediment for 68 elements. The results should be useful for assessing the analytical accuracy of major, minor, and trace elements in marine sediments. Therefore, the CRM is expected to play an important role in Arctic geochemical surveys and environmental assessment.     

The UK National Marine Analytical Quality Control Scheme

 The approach to analytical quality control adopted for the UK National Marine Analytical Quality Control Scheme is described. The Scheme began in 1991 and is in its fifth year of operation. The aim of the programme of work is to ensure adequate control over the accuracy of analysis, such that the aims of the UK National Marine Monitoring Plan are satisfied. The results of interlaboratory tests for the determination of nutrients in water samples and metals, organic compounds in waters, sediments and biological samples are summarised. Received: 7 October 1996 Accepted: 27 February 1997     

Fifteenth International Symposium on Biological and Environmental Reference Materials (BERM-15)

Accreditation and Quality Assurance -     

中药质量控制与安全性评价中的分析化学

本文论述了中药现代化实施中进行质量控制的“5P”(GAP、GCP、GLP、GMP、GSP)系统工程 ;结合本实验室近年来以“5P”指导中药质量控制与安全性评价所做的一些工作 ,阐明了将分析化学应用于中药质量控制与安全性评价的策略与方法 ,提出了分析化学在中药现代化系统工程及重大科学问题的解决中所能发挥的重要作用。