光电发射光谱法测量不确定度的评定

近几年来,我国开展了宣贯实施《测量设备的计量确认体系》以及《测量过程控制》,其中要求对测量不确定度进行全面评定,用以作为保证测量结果可靠的依据。这样,我国计量学界自20世纪50年代以来所形成的至今基本上没有改变的习惯概念和数据的处理完成及测量结果的表达方式面临着一个颇大的必须接受的变革。光电发射光谱法作为冶金行业主要的检测方法,其测量结果不确定度的评定显得尤为重要[1]。1测量方法依据GB/T 7999-2000《铝及铝合金光电(测光法)发射光谱分析方法》,将加工好的试样用激发系统激发发光,经分光系统色散成光谱,对选用的内标…     

直读光谱法测量镁合金中锰含量的测量不确定度评定

根据GB/T13748.21-2009镁及镁合金化学分析方法(光电直读发射光谱分析方法测定元素含量)对镁合金中锰元素含量进行了分析,对锰含量测量的不确定度来源进行了分析,并对测量过程中产生的不确定度进行了评定.此外,指出了该方法影响锰元素测量不确定度的主要原因,以期为镁合金中锰元素含量的光谱分析提供参考.     

光电发射光谱法测定碳素钢中硅含量的测量不确定度评定

讨论了光电发射光谱法测定碳素钢中硅含量的各种不确定度因素,提供了不确定度评定过程所需各参数的采集和计算方法,评定了硅含量的测量不确定度.     

火花直读光谱法对铝合金中各元素含量测量结果的不确定度评定

分析了火花直读光谱法测定铝合金中Si、Fe、Cu、Mg、Mn、Zn、Cr、Ti元素含量测量结果的不确定度来源,对不确定度分量进行了评定与计算,Si、Fe、Cu、Mg、Mn、Zn、Cr、Ti测量结果的相对扩展不确定度分别为2. 9%、2. 5%、2. 6%、2. 7%、2. 6%、2. 6%、2. 5%、2. 7%(包含因子k均为2).     

火焰原子吸收光谱法测定镁及镁合金中镉含量不确定度评定

采用火焰原子吸收光谱法测定镁及镁合金中镉含量,对测定结果不确定度进行评定.建立数学模型,分析不确定度来源,计算合成标准不确定度和扩展不确定度.当镁及镁合金中镉含量为0.00418％时,其扩展不确定度为0.00034％(k=2).火焰原子吸收光谱法测定镁及镁合金中镉含量不确定度主要来源于样品称量、样品消解溶液定容、标准工...     

电感耦合等离子体原子发射光谱法测定燃料油加氢精制催化剂中铂含量的不确定度评定

评定电感耦合等离子体原子发射光谱法测定燃料油加氢精制催化剂中贵金属铂含量的测量不确定度.电感耦合等离子体原子发射光谱法测量不确定度主要来源于测量重复性、标准工作曲线拟合、天平称量以及标准溶液配制和稀释4个分量,其中测量重复性和标准工作曲线拟合对合成不确定度的贡献最大.结果表明,当燃料油加氢精制催化剂中贵金属铂含量为0....     

红外吸收法测定碳含量的测量不确定度评定

对CCS-140型高频感应炉燃烧红外吸收法测定碳含量的不确定度进行了评定,分析了测量不确定度的主要来源,包括仪器的精密度引入的不确定度,标准物质标准值的不确定度,试样称量的不确定度,以及坩埚、助熔剂等引起的空白不确定度。当碳含量为0.366%时,测量结果的扩展不确定度为0.010%。     

蒸馏法测定化肥中氮含量的测量不确定度评定

对蒸馏法测定化肥中氮含量的测量不确定度进行了评定。分析了蒸馏法测定化肥中氮含量的不确定度的主要来源,通过数学模型对各不确定度分量进行了评定,采用蒸馏法测定化肥中氮含量的扩展不确定度为0．07％。     

红外吸收法测定钢中碳量的测量不确定度评定

对高频炉燃烧.红外吸收法测定钢中碳含量的测量不确定度来源进行了详细的分析,建立了合理的数学模型,概述了物质称量、标准物质认定值、测量的重复性等等各主要的不确定度分量的评定方法,对高频炉燃烧.红外吸收法测定钢中碳含量的测量不确定度进行了仔细的评定,给出了扩展不确定度,并就其对钢中碳含量测量结果的影响进行了深入的探讨.     

Simultaneous determination of the constituents in Al-Ge-Si alloys by inductively coupled plasma atomic emission spectrometry

An accurate method for determination of the constituents Ge, Si, In and Mg in Al–Ge–Si based compact alloys and foil materials by ICP atomic emission spectrometry is developed. The material samples were dissolved in nitric acid–hydrofluoric acid. Optimum parameters for the simultaneous measurement of the constituent elements are worked out. To compensate the time determined sensitivity fluctuations the analytical signal was corrected by a special procedure of external standardization.     

Simultaneous determination of the constituents in Al-Ge-Si alloys by inductively coupled plasma atomic emission spectrometry

An accurate method for determination of the constituents Ge, Si, In and Mg in Al-Ge-Si based compact alloys and foil materials by ICP atomic emission spectrometry is developed. The material samples were dissolved in nitric acid-hydrofluoric acid. Optimum parameters for the simultaneous measurement of the constituent elements are worked out. To compensate the time determined sensitivity fluctuations the analytical signal was corrected by a special procedure of external standardization.     

原子荧光法测定水中砷的不确定度评定

评定原子荧光法测定水中砷的不确定度.结合原子荧光法原理和相关实验流程,根据JJF 1059.1—2012《测量不确定度评定与表示》建立原子荧光法测定水中砷的不确定度测量模型,对整个测定过程中的不确定度来源进行分析.测量不确定度的主要来源包括:取样体积、样品定容体积、由标准曲线上查得砷浓度、样品稀释、重复性测定,分别进行...     

电感耦合等离子体原子发射光谱法测定工业电解质中钙、镁、锂

工业电解质中微量元素钙、镁、锂对电解槽的正常运行非常重要。本文采用高氯酸加热挥发除氟,以盐酸(1 1)溶解残渣,选用Ca317.9nm、Mg297.5nm、Li670.7nm作为分析谱线,考察了样品处理方法、共存元素干扰对测定结果的影响。建立了电感耦合等离子体原子发射光谱法测定工业电解质中钙、镁、锂的方法。结果表明：不同的电解质因其所含氧化铝的不同会有部分不溶杂质,但对微量元素的测定影响很小,可以忽略不计。共存元素铝和钠不干扰微量元素的测定。按照试验方法对2个电解质标准样品进行了测定,其测定值与标准值吻合。同时对不同电解槽的工业电解质样品进行了分析,其结果的相对标准偏差(RSD,n=11)在0.69%-5.68%之间,满足生产分析的需要。     

Determination of calcium, iron and magnesium in rabbit arteries by inductively coupled plasma atomic emission spectrometry

Regional variations in arterial concentrations of Ca, Mg and Fe may influence susceptibility to atherosclerosis. However, investigation of such hypotheses requires the availability of a sensitive, reliable method for the determination of elements in small arterial samples. These biologically important elements are determined in rabbit arteries by inductively coupled plasma atomic emission spectrometry (ICP-AES). Arterial samples (aorta and iliac arteries) are collected from 4- and 6- to 7-month-old rabbits fed rabbit chow. Closed-vessel microwave acid digestion is used to prepare the samples. The accuracy of the method is tested with a NIST bovine liver (1577b) standard reference material, and the amount of each metal found is within the reported uncertainty in the certified concentration. Also, the recovery from artery samples spiked with 0.5 μg of each metal is nearly 100% (96-105% Ca, 93-105% Fe, and 92-104% Mg). The simultaneous multielement detection of Ca, Fe and Mg at levels more than 1000-fold higher than the detection limit, in arterial samples weighing as little as 5 mg, suggests that this method may be applicable to very small clinical samples or arterial samples from very small animals.     

Evaluation of the solid sampling technique for the determination of aluminium in biological materials by atomic absorption and atomic emission spectrometry

Summary Results for the determination of aluminium in several biological materials by atomic absorption and atomic emission spectrometry using the solid sampling technique in connection with a constant temperature furnace are given. A comparison was made with a dissolution procedure and good agreement was generally obtained. With the solid sampling technique it was possible to calibrate against aqueous standards and to achieve a precision of better than 10% r.s.d. for NBS 1577a Bovine Liver and IAEA H-4 Animal Muscle, providing that the sample mass was greater than 1.3 mg and that the peak area was evaluated. Laboratory air and the solid sampling procedure were identified as possible sources of contamination.

---

Auswertung der Feststofftechnik für die Bestimmung von Aluminium in biologischen Materialien durch AAS und AES

     

Determination of tungsten by direct current plasma atomic emission spectrometry

The determination of tungsten in steels and alloys with the three-electrode direct current plasma (DCP) “spectrajet” was investigated. The relative intensities of 17 spectral lines of tungsten and several possible interfering lines of its concomitants are listed. WI 400.875 nm is normally best suited, because the background produced by iron and acid is low and easily compensated for by using a blank solution. The limit of detection c_l in steels is 2 × 10^?3% W for 10 $\text{mg}\text{ml}$ of sample. The line W I 407.436 nm is preferred in the presence of much titanium. For the purpose considered the DCP provides about the same power of detection as the more expensive inductively coupled plasma (ICP), but its observation zone is less well buffered against influences from the matrix.     

Evaluation of measurement uncertainties for the determination of total metal content in soils by atomic absorption spectrometry

In this work estimation of measurement uncertainties associated with the total metal content in soils was done by an intralaboratory approach based on method validation and quality control data, and using two certified reference materials (CRM). CRM and soil samples were analyzed following procedures based on the methods that are applied to silicate materials. All elements were determined by atomic absorption spectrometry following a quality assurance program previously established. Quality control actions were implemented in order to provide reliable data. The precision under within-laboratory reproducibility conditions was estimated from triplicate analysis. The trueness component was determined as recovery of the analyte from CRMs: soil sample, SO-2 and river clay sediment, LGC 6139. Combined measurement uncertainty was expressed in terms of precision and recovery uncertainties and the later further split on CRM replicate analysis and uncertainty of the certified value components. The results obtained are critically discussed on the basis of the different contributions. For the selection of the reference material, the CRM dependent terms are critically compared in order to fulfill specific requirements. Electronic supplementary material  The online version of this article (doi:) contains supplementary material, which is available to authorized users.