原子荧光光谱法测定谷子中硒含量的测量不确定度评定

硒是与人体健康密切相关的微量元素,2003年国家发布了经修订后的国家标准GB/T5009.93-2003<食品中硒的测定>.但有关硒测定中不确定度评定的报道不多,本试验以谷子为样品.采用GB/T5009.93-2003推荐的氢化物原子荧光法(AFS)测定样品中硒含量,依据JJF1059-1999<测量不确定度评定与表示>进行不确定度分析和评定.     

玩具重金属分析不确定度的评定

参照我国计量技术规范JJF1059-1999《测量不确定度的评定与表示》及有关方法,对玩具重金属分析不确定度进行了评定,获得玩具中可溶性汞、锑、砷、硒、铅、铬、镉、钡八种有害元素分析相对扩展不确定度在4.5%~23.5%之间。证明该方法能满足实验认证认可对测量不确定度的要求。     

HG-AFS法测定地质样品中微量硒的不确定度评定

通过氢化物发生-原子荧光光谱法(HG-AFS)对地质样品中的硒进行测定,对测定结果的不确定度来源进行分析,评定不确定度的分量。结果表明,该方法测量不确定度引入的最主要来源有两项:硒标准溶液配制过程和重复性测量样品。因此在实际分析过程中,应提高分析人员检测技能和规范操作,保证测定结果的准确性和可靠性。当测试样品中硒的含量为0.1631μg/g时,其扩展不确定度(k=2)为0.0081μg/g。     

玩具重金属分析不确定度的评定

参照我国计量技术规范JJF1059—1999《测量不确定度的评定与表示》及有关方法，对玩具重金属分析不确定度进行了评定，获得玩具中可溶性汞、锑、砷、硒、铅、铬、镉、钡八种有害元素分析相对扩展不确定度在4．5％～23．5％之间。证明该方法能满足实验认证认可对测量不确定度的要求。     

CMM形状测量任务的不确定度分析与评定

研究了坐标测量机(CMM)形状测量任务的不确定度评定问题,实现了CMM形状测量的不确定度快速、可靠地评定。给出了测量不确定度评定与表示指南(GUM)和蒙特卡洛随机抽样两种不确定度合成方法,平面度测量实验验证了不确定度评定方法的可行性,实验结果表明:GUM确定的不确定度精度意义不可靠,扩展不确定度相对于实际情况扩大了11.1%; 解决CMM形状测量任务的不确定度评定问题,具有较强的典型性和代表性,可有效地应用于解决其他精密仪器的不确定度评定问题。     

氦气分析检测中不确定度评定

依据JJF1135-2005<化学分析测量不确定度评定>,对氦气分析检测中的不确定度进行了评定,分析了各不确定度分量,并通过建立气相色谱外标法测量结果不确定度的数学模型 ,计算了其测量结果的相对合成标准不确定度和扩展不确定度.     

测量不确定度评定的应用分析

<正>本文将对测量不确定度评定在实验室日常工作中的各种应用进行分析比较,总结梳理各种应用中测量不确定度评定和表示的相同及不同之处,从而为实验室测量不确定度评定工作理清思路,在评定不确定度工作中能够统筹兼顾,提高工作效率。一、实验室认可中的校准和测量能力(CMC)评估与计量标准考核中的测量不确定度评定两者既有相同点,又有不同之处。相同点主要表现为:分析不确定度的来源相同,评定方法基本相同。     

测量不确定度概念的理解

本文以测量误差与测量不确定度的定义解析,了解两者的区别,在概念上加深对测量不确定度的理解;通过介绍测量不确定度A类和B类评定方法的异同点,使检测人员初步认知测量不确定度的评定方法,为今后开展测量不确定度的评定工作打下基础。     

采样计数法测量信号频率的不确定度

介绍了用数字化采样计数法评价周期信号频率时,测量结果的不确定度分析和评定过程,讨论了影响测量不确定度的几个主要误差来源;给出了减小测量不确定度的主要措施;在一组实际评价例子上,给出了其不确定度分析和评定结果,该过程及结论可应用信号频率的测量不确定度评定。     

测量不确定度概念的理解

本文以测量误差与测量不确定度的定义解析,了解两者的区别,在概念上加深对测量不确定度的理解;通过介绍测量不确定度A类和B类评定方法的异同点,使检测人员初步认知测量不确定度的评定方法,为今后开展测量不确定度的评定工作打下基础。     

石墨炉原子吸收法直接测定饮用水中的铍

采用石墨炉原子吸收法,使用热解涂层石墨管,加上硝酸镁作基体改进剂,直接测定水中的铍。     

原子吸收法测定白酒中铅和锰的方法改进

目的:本文以简化操作步骤,改进实验方法为目的,着重研究利用原子吸收光谱法直接测定白酒中的铅和锰。方法:直接对样品进行稀释,用火焰原子吸收法测定锰。以磷酸氢二铵为基体改进剂,用石墨炉原子吸收光谱法测定铅。结果:该方法操作简单快速,减少了试剂用量,而且精密度和准确度都能满足实验要求。结论:该方法是可行的,值得推广使用。     

石墨炉原子吸收法测定洗涤剂中砷含量

建立了石墨炉原子吸收光谱法测定洗涤剂中砷含量的方法。采取硝酸及高氯酸法处理样品,加入基体改进剂硝酸镍,应用石墨炉原子吸收光谱法测定砷。结果表明,测定一次回归方程为Y=0.0012X+0.0009,相关系数r=0.9994。检出限为0.16 ug/L,回收率为92.9%～101.4%,相对标准偏差为1.42%～3.18%。该方法具有快速、准确、灵敏度高等优点,适用于洗涤剂中砷含量的检测。     

石墨炉原子吸收光谱法测定超高纯试剂中钙的研究．

研究了超高纯试剂异丙醇中痕量钙的石墨炉原子吸收光谱测定法。制定了石墨炉原子吸收光谱法测定痕量钙的分析程序，试样经挥发浓缩，采用标准曲线法测定；还确定了仪器最佳工作条件，原子化条件等，研究了共存离子的干扰，回收试验及实测样品等。同时将石墨管用氯氧化锆进行适当的处理，并控制合适的仪器操作条件及升温程序，即可提高石墨炉原子吸收法测钙的灵敏度，获得了较满意的结果。     

Separation and preconcentration of cadmium ions using octadecyl silica membrane disks modified by methyltrioctylammonium chloride

A simple and selective method for the determination of cadmium in water samples by FAAS after solid phase extraction has been developed. The method is based on the sorption of cadmium as CdI(4)(2-) on octadecyl silica membrane disks modified by cationic surfactant of methyltrioctylammonium chloride in the pH range of 1-8. The sorbed cadmium is then eluted with 10ml of 1moll(-1) nitric acid in ethanol and is measured by flame atomic absorption spectrometry. The influence of flow rates of eluent and sample solution, iodide concentration and amount of surfactant in retention and elution of cadmium from disks was also investigated. A preconcentration factor of 100 was achieved by passing 1000ml of sample through the membrane disk. The limit of detection (LOD) of cadmium was found to be 0.014ngml(-1). Precision at 2.5mugl(-1) was 1.2% (n=8). The method was successfully applied to the determination of cadmium in some natural water samples. The accuracy was assessed through recovery experiment, independent analysis by graphite furnace atomic absorption spectrometry, and analysis of certified reference waters.     

石墨炉原子吸收光谱法测定水样消解研究

本文采用硝酸-过氧化氢的消解体系,对石墨炉原子吸收法测定水样中痕量重金属含量过程中样品消解环节进行研究,认为通过严格控制使用的试剂和消解过程,能够提高样品分析的准确度和精密度,同时样品加标回收率结果也比较满意。     

基于不确定度评价对稻米中镉元素分析标准物质高精度定值方法的比较

通过对稻米中镉含量测定的3种典型方法(石墨炉原子吸收光谱法(GFAAS)、电感耦合等离子体质谱法(ICP-MS)和同位素稀释电感耦合等离子体质谱法(ID-ICP-MS))测量不确定度分量来源、类型、贡献进行系统分析比较,为稻米镉分析标准物质高精度定值方法的选择和定值的过程控制提供依据.研究结果显示,GFAAS、ICP-...     

Evaluation of various digestion procedures for trace element contents of some food materials

The levels of trace elements in different types of food material consumed in Turkey were determined by flame and graphite furnace atomic absorption spectrometry. Food samples were digested with dry ashing, wet ashing and microwave digestion procedures in this study. The microwave digestion procedure was chosen for the digestion of all the food samples because it required shorter time and made higher recovery (specially for Se). Fe, Cu, Mn, Zn, Al and Se were determined by flame and graphite furnace atomic absorption spectrometry, respectively. Relative standard deviations (RSD) were found below 10%. The accuracy of the procedure was confirmed by certified reference materials. Moreover, this procedure was easier to use when compared with dry and wet digestions.     

Study on solid phase extraction and graphite furnace atomic absorption spectrometry for the determination of nickel, silver, cobalt, copper, cadmium and lead with MCI GEL CHP 20Y as sorbent

A solid phase extraction and graphite furnace atomic absorption spectrometry (GFAAS) for the determination of nickel, silver, cobalt, copper, cadmium and lead with MCI GEL CHP 20Y as sorbent was studied. Trace amounts of chromium, nickel, silver, cobalt, copper, cadmium and lead were reacted with 2-(2-quinolinil-azo)-4-methyl-1,3-dihydroxidobenzene (QAMDHB) followed by adsorption onto MCI GEL CHP 20Y solid phase extraction column, and 1.0molL(-1) HNO(3) was used as eluent. The metal ions in 300mL solution can be concentrated to 1.0mL, representing an enrichment factor of 300 was achieved. The recoveries of analytes at pH 8.0 with 1.0g of resin were greater than 95% without interference from alkaline, earth alkaline and some metal ions. When detected with graphite furnace atomic absorption spectrometry, the detection limits in the original samples were 1.4ngL(-1) for Cr(III), 1.0ngL(-1) for Ni(II), 0.85ngL(-1) for Ag(I), 1.2ngL(-1) for Co(II), 1.0ngL(-1) for Cu(II), 1.2ngL(-1) for Cd(II) and 1.3ngL(-1) for Pb(II). The validation of the procedure was performed by the analysis of the certified standard reference materials, and the presented procedure was applied to the determination of analytes in biological, water and soil samples with good results (recoveries range from 89 to 104%, and R.S.D.% lower than 3.2%. The results agreed with the standard value or reference method).     

石墨炉原子吸收法直接测定饮用水中的铍、镍、钡

采用石墨炉原子吸收法,使用热解涂层石墨管,加上硝酸镁作基体改进剂,直接测定水中的痕量铍、镍、钡。测定钡时采用原子化阶段不停气,通以10mL/min的流量;测定完成后,再使用“清除温度”空烧1～2次处理,可消除记忆效应的影响。