红外分光光度计检定不确定度评定

以JJF 1059.1–2012为依据,对红外分光光度计计量检定的不确定度进行评定。分析了检定过程中波数示值误差及透射比示值误差不确定度的重要来源,包括测量重复性、标准物质等引入的不确定度分量。对各不确定度分量进行分析计算,波数示值误差测量结果的扩展不确定度U=1.1 cm–1,k=3。透射比示值误差测量结果的相对扩展不确定度U rel=0.2%,k=2。     

示差扫描量热计示值误差测量不确定度评定

采用示差扫描量热(DSC)法测定热分析标准物质的熔化温度和熔化热,对示值误差的测量不确定度进行评定.建立示值误差的测量模型,分析不确定度来源,计算各不确定度分量,最终合成标准不确定度和扩展不确定度.铟、锌的温度示值误差的扩展不确定度分别为0.34、0.62℃(k=2),热量示值误差的相对扩展不确定度均为1.2％(k=2...     

大气采样器计量标准的测量不确定度

对大气采样器计量标准的测量不确定度来源如计量标准、流量示值误差、流量重复性、温度计示值误差进行了分析和评定,计算得合成标准不确定度和扩展不确定度分别为0.65%和1.30%.对测量不确定度的合理性进行了验证.     

红外法测量钢铁中碳硫示值误差不确定度的评定

依据国家标准方法对不同类型大量台件的红外碳硫分析仪进行检定与测试,采用国家一级或二级标准物质对仪器进行校准,在此过程中获得大量的数据．根据拟订的示值误差数学模型,分别给出输入量的A类或B类不确定度评定结果,按照国际通行方法进行不确定度的合成与扩展,最终得到红外法测量示值误差不确定度的判断。不确定度的大小是评定一种测量方法能力优劣的指标。     

固体进样总有机碳分析仪校准方法

建立固体进样总有机碳分析仪的校准方法.根据仪器原理及使用情况,选取线性、示值误差、重复性作为仪器的主要计量特性,并探讨各个计量特性的校准方法.用该方法对某型号的仪器进行校准,得线性相关系数为0.998,示值误差为0.86％,重复性为0.39％,并对示值误差测量结果不确定度进行了评定,扩展不确定度为0.94％(k=2)....     

冶金分析仪器检定/校准中若干问题的探讨

对冶金分析仪器检定/校准中若干问题进行了探讨,包括计量标准、示值误差异常值的判断、不确定度、检定/校准项目、元素和测量范围等。计量人员用标准物质检定/校准仪器可以保证仪器测量结果的溯源,而实验室"自检定/自校准"不具备溯源性;示值误差的测量次数和测量数据的一致性需要利用统计规则进行判断,而不能直接取平均值作为测量结果;进行检定/校准结果的不确定度评定时,重复性引入的不确定度分量可以预先评估,评定检出限不确定度意义不大,实验室在进行一次测量时,一定程度上可以直接引用校准证书上的不确定度。校准的项目、元素和范围超出检定规程或者校准规范的要求时,计量机构需要进行方法确认及不确定度的评定。     

基于光学法的化学需氧量实时测定仪校准方法

针对一种基于光学法的化学需氧量实时测定仪,提出了一种校准方法.其校准项目与技术指标包括示值误差不大于10％,重复性不大于3％,示值稳定性不超过10％.对仪器示值误差测量结果不确定度进行评定,得到相对扩展不确定Urel=2％(k=2).采用有证标准物质或配制成系列浓度的化学需氧量标准溶液进行校准,将化学需氧量实时测定仪的...     

比色法余氯在线分析仪校准方法

建立比色法余氯在线分析仪的校准方法。比色法余氯在线分析仪的校准包括仪器示值误差、测量重复性和示值稳定性3个项目。根据实验数据,结合各仪器的出厂技术指标要求,综合分析得出比色法余氯在线分析仪的计量性能指标：示值误差在±10%内,重复性不大于3%,示值稳定性在±10%内。示值误差测量结果的相对扩展不确定度为2.8%。该方法可用于评价比色法余氯在线分析仪的计量特性。     

总磷测定仪校准方法

建立总磷测定仪的校准方法。介绍了总磷测定仪的工作原理。总磷测定仪的校准包括温度示值误差和温场均匀性、消解时间示值误差、仪器示值误差、测量重复性、示值稳定性5个项目。利用实验数据确定了总磷测定仪的技术指标:温度示值误差不超过±2℃,温场均匀性不大于3℃,消解时间示值误差为不超过±2%,仪器示值误差为不超过±10%,仪器重复性为不大于5%,示值稳定性为不超过±8%FS。该方法可用于总磷测定仪的校准,保证测量数据的准确可靠。     

石油产品微量残炭测定仪的校准

通过分析石油产品微量残炭测定仪的工作原理,参考相应的国家技术规范,建立石油产品微量残炭测定仪的校准方法,提出了示值误差、重复性等校准项目。采用残炭值为2.03%的油品残炭标准物质对石油产品微量残炭测定仪进行校准,其示值误差为0.04%,重复性为0.03%,对石油产品微量残炭测定仪示值误差测量结果的不确定度进行了评定,其扩展不确定度为0.15%(k=2)。该校准方法切实可行,可用于石油产品微量残炭测定仪的校准。     

Nuclear analytical application of thermionic mass spectrometry

Summary The relative uncertainty on the isotope abundance ratio measurements of uranium and plutonium samples by means of thermionic mass spectrometry at the Central Bureau for Nuclear Measurements (CBNM) in Geel, Belgium, has decreased to a level of about 2 · 10^–4.The improvement was mainly achieved through the preparation of synthetic isotope mixtures of uranium and plutonium, to a relative uncertainty of 0.01% (computed on a 2s basis) on the ratios of isotopes with major abundances. This allowed to determine some error sources more precisely, such as: — isotope fractionation, — non-linearity of the ion beam current measuring system.As a consequence CBNM is able to prepare certified uranium isotopic reference materials (U IRM's) for distribution, with a relative uncertainty of 0.07% (computed on a 2s basis) on the²³⁵U isotope abundance and to provide reference values on samples for the (European) Interlaboratory Measurement Evaluation Programmes (REIMEP).

---

Nuklearanalytische Anwendung der Thermionen-Massenspektrometrie

     

气相色谱–质谱法测定食用植物油中短链脂肪酸的测量不确定度评定

采用气相色谱–质谱法(GC–MS)测定食用植物油中短链脂肪酸含量,对测量结果的不确定度进行评定,探讨提高测量准确度的方法。依据方法建立数学模型,分析得出不确定度主要来源于样品制备过程、计量器具的使用、标准溶液配制、测量设备、人员读数误差、方法回收率,计算各不确定度分量,得到相对标准不确定度和扩展不确定度。结果表明,当食用植物油中短链脂肪酸测定结果为13.1 mg/kg时,其扩展不确定度为1.8 mg/kg(k=2)。测量设备、标准溶液配制过程引入的不确定度较大,应在实验过程中予以控制和关注。     

薄层色谱扫描仪波长示值误差校准方法

目前我国没有薄层色谱扫描仪国家检定规程,一些地方或部门标准中的波长示值误差项目计量方法可操作性不强。通过对比现有标准,提出了一种薄层色谱扫描仪波长示值误差计量方法。该方法利用计量单位使用的钬玻璃波长滤光片作为计量标准器,操作步骤与样品测试类似,波长示值误差的扩展不确定度为0.6 nm(k=2),满足校准要求。该法降低了计量操作难度,可作为计量人员的参考依据。     

冷原子荧光测汞仪检定结果的不确定度

依据JJG548-2004对冷原子荧光测汞仪进行检定时,检定结果的不确定度主要来源于仪器的线性误差、检测限、重复性和标准物质浓度。对各不确定分量进行了评定和计算,求得合成标准不确定度和扩展不确定度分别为0.033ng/mL和0.066ng/mL(k=2)。     

Validation of multi-element isotope dilution ICPMS for the analysis of basalts

In this study we have validated a newly developed multi-element isotope dilution (ID) ICPMS method for the simultaneous analysis of up to 12 trace elements in geological samples. By evaluating the analytical uncertainty of individual components using certified reference materials we have quantified the overall analytical uncertainty of the multi-element ID ICPMS method at 1–2%. Individual components include sampling/weighing, purity of reagents, purity of spike solutions, calibration of spikes, determination of isotopic ratios, instrumental sources of error, correction of mass discrimination effect, values of constants, and operator bias. We have used the ID-determined trace elements for internal standardization to improve indirectly the analysis of 14 other (mainly mono-isotopic trace elements) by external calibration. The overall analytical uncertainty for those data is about 2–3%.In addition, we have analyzed USGS and MPI-DING geological reference materials (BHVO-1, BHVO-2, KL2-G, ML3B-G) to quantify the overall bias of the measurement procedure. Trace element analysis of geological reference materials yielded results that agree mostly within about 2–3% relative to the reference values. Since these results match the conclusions obtained by the investigation of the overall analytical uncertainty, we take this as a measure for the validity of multi-element ID ICPMS.     

Uncertainties of mercury determinations in biological materials using an atomic absorption spectrometer – AMA 254

 The method is based on catalysed ignition of a sample portion in a flow of oxygen, capture of mercury by an amalgamator and measurement of the mercury vapour's absorbance after thermic release from the amalgamator. Three powdered food samples, a certified reference material (CRM) human hair and a reference material (RM) urine (liquid) were measured in the first range of the instrument (the possible contents determined according to our measurement procedure were 0.0003–0.5 ppm). The calibration function used was a line passing through the origin. The combined standard uncertainties of the mercury determinations were computed from uncertainty components of five quantities: absorbance of the sample, absorbance of the sample blank, slope of the calibration line, correction factor of the abscissa axis, and mass or volume of the sample. The most important uncertainty component is the uncertainty of the sample absorbance measurement which amounts to 52% of the determination uncertainty at the minimum (RM urine) and about 90% at the maximum (in our laboratory homogenized powdered food samples; analysis of variance showed their homogeneity to be insufficient). The results of the CRM and RM analyses do not indicate a significant systematic error for this determination. The relative expanded uncertainty (coefficient was 2) of the determination increases from 9 to 13% for the insufficiently homogenized samples with decreasing mercury content (range of 0.004–0.03 ppm); higher homogeneity of samples results in a decrease of the expanded uncertainty, e.g. 4.6% for the liquid sample (RM urine). Received: 26 April 1999 / Accepted: 30 August 1999     

ICP-OES测定钒矿石中五氧化二钒的测量不确定度评定

介绍了电感耦合等离子体发射光谱法(ICP-OES)测定钒矿石中五氧化二钒测重不确定度的评定万法.建立了测量过程中各不确定度分量的数学模型,对不确定度来源进行了分析,并对不确定度分量进行量化.当钒矿石中五氧化二钒含量为0.419％时,其扩展不确定度为0.0070％(k=2).     

国家标准方法测定锌精矿中锌的不确定度评定

对沉淀分离EDTA滴定法测定锌精矿中锌含量的测量不确定度来源进行了分析,并对EDTA标准溶液的滴定度、试样的质量、滴定体积、测定过程随机误差等不确定度分量进行了分析和量化,合成标准不确定度和扩展不确定度分别为0.20%和0.40%。     

一种全自动光度滴定仪

报道了改装７２１型分光光度计为光度滴定仪并联用８０３１单片微机构成一台全自动光度滴定仪，在单片机的控制下，实现取样，加试液，搅拌，开关光门，调零，调参比，滴定，测吸光度，数据处理，显示结果并打印，排除废液，冲洗滴定池等操作过程的全自动化，约１１０ｓ可完成一次测定，误差〈０．２％，ＲＳＤ〈１．５％，测定快速，准确，重复性好，可胜任在线监测工作，也可作常规滴定分析。