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1.
S. Küppers 《Accreditation and quality assurance》1997,2(1):30-35
Any analytical data is used to provide information about a sample. The "possible error" of the measurement can be of extreme
importance in order to have complete information. The measurement uncertainty concept is a way to achieve quantitative information
about this "possible error" using an estimation procedure. On the basis of the analytical result, the chemist makes a decision
on the next step of the development process. If the uncertainty is unknown, the information is not complete; therefore this
decision might be impossible. The major problem for the in-process control (IPC) procedure is that not only the repeatability
but also the intermediate precision (which expresses the variations within laboratories related to different days, different
analysts, different equipment, etc.) has to be good enough to make a decision. Unfortunately, the statistical information
achieved from one single analytical run only gives information about the repeatability. This paper shows that the estimation
of the measurement uncertainty for IPC is a way to solve the problem and gives the necessary information about the quality
of the procedure. An example demonstrates that an estimate of uncertainty based on the standard deviations of an analytical
method gives a value similar to one based on the standard deviations obtained from a control chart. Therefore, the estimation
is both a very useful and also a very cost-effective tool. Though measurement uncertainty cannot replace validation in general,
it is a viable alternative to validation for all methods that will never be used routinely.
Received: 24 May 1996 Accepted: 10 August 1996 相似文献
2.
3.
M. Buzoianu 《Accreditation and quality assurance》2000,5(6):231-237
In practice there are three aspects that need to be considered in order to achieve the required traceability according to
its definition: the 'stated reference', the 'unbroken chain of calibrations' and the "stated uncertainty". For a certain chemical
result, each of these aspects highly depends on the measurement uncertainty, both on its magnitude and how it was estimated.
Therefore, the paper describes the experience of the Romanian National Institute of Metrology in estimating measurement uncertainty
during the certification of reference materials (RMs), in metrological activities (calibration, pattern approval, periodical
verification, etc.), as well as during the analytical measurement process. Practical examples of estimation of measurement
uncertainty using RMs or certified reference materials are discussed for their applicability in spectrophotometric and turbidimetric
analysis. Use of the analysis of variance to obtain some additional information on the components of measurement uncertainty
and to identify the magnitude of individual random effects is described.
Received: 12 November 1999 / Accepted: 25 February 2000 相似文献
4.
In the EURACHEM/CITAC draft ”Quantifying uncertainty in analytical measurement” estimations of measurement uncertainty in
analytical results for linear calibration are given. In this work these estimations are compared, i.e. the uncertainty deduced
from repeated observations of the sample vs. the uncertainty deduced from the standard residual deviation of the regression.
As a result of this study it is shown that an uncertainty estimation based on repeated observations can give more realistic
values if the condition of variance homogeneity is not correctly fulfilled in the calibration range. The complete calculation
of measurement uncertainty including assessment of trueness is represented by an example concerning the determination of zinc
in sediment samples using ICP-atomic emission spectrometry.
Received: 9 February 2002 Accepted: 17 April 2002 相似文献
5.
A protocol has been developed illustrating the link between validation experiments, such as precision, trueness and ruggedness
testing, and measurement uncertainty evaluation. By planning validation experiments with uncertainty estimation in mind, uncertainty
budgets can be obtained from validation data with little additional effort. The main stages in the uncertainty estimation
process are described, and the use of trueness and ruggedness studies is discussed in detail. The practical application of
the protocol will be illustrated in Part 2, with reference to a method for the determination of three markers (CI solvent
red 24, quinizarin and CI solvent yellow 124) in fuel oil samples.
Received: 10 April 1999 / Accepted: 24 September 1999 相似文献
6.
A strategy is presented for applying existing data and planning necessary additional experiments for uncertainty estimation.
The strategy has two stages: identifying and structuring the input effects, followed by an explicit reconciliation stage to
assess the degree to which information available meets the requirement and thus identify factors requiring further study.
A graphical approach to identifying and structuring the input effects on a measurement result is presented. The methodology
promotes consistent identification of important effects, and permits effective application of prior data with minimal risk
of duplication or omission. The results of applying the methodology are discussed, with particular reference to the use of
planned recovery and precision studies.
Received: 28 October 1997 · Accepted: 17 November 1997 相似文献
7.
V. J. Barwick S. L. R. Ellison M. J. Q. Rafferty R. S. Gill 《Accreditation and quality assurance》2000,5(3):104-113
A protocol has been developed illustrating the link between validation experiments and measurement uncertainty evaluation.
The application of the protocol is illustrated with reference to a method for the determination of three markers (CI solvent
red 24, quinizarin and CI solvent yellow 124) in fuel oil samples. The method requires the extraction of the markers from
the sample matrix by solid phase extraction followed by quantification by high performance liquid chromatography (HPLC) with
diode array detection. The uncertainties for the determination of the markers were evaluated using data from precision and
trueness studies using representative sample matrices spiked at a range of concentrations, and from ruggedness studies of
the extraction and HPLC stages.
Received: 10 April 1999 · Accepted: 24 September 1999 相似文献
8.
T. Drglin 《Accreditation and quality assurance》2003,8(3-4):130-133
A validation procedure based on the ISO/IEC 17025 standard was used to demonstrate the long-term stability of a calibration
process and to assess the measurement uncertainty of a standard test method for optical emission vacuum spectrometric analysis
of carbon and low-alloy steel (ASTM E 415–99a). The validation was used to provide documented evidence that the selected method
fulfils the requirements and that the method is ”fit for purpose”. A test for drift was applied to determine statistically
whether the analytical results vary systematically with time. The accuracy and traceability of the optimised method were tested
by an analysis of closely matched matrix certified reference materials (CRMs). The measurement uncertainty estimations took
account of the precision study, the bias and its uncertainty, and the qualification of uncertainties not considered in the
overall performance studies.
Received: 2 November 2002 Accepted: 2 January 2003
Acknowledgement The author expresses gratitude to Dr. Aleš Fajgelj for helpful discussions during the 3rd Central European Conference on Reference Materials and Measurements.
Presented at CERMM-3, Central European Reference Materials and Measurements Conference: The function of reference materials
in the measurement process, May 30–June 1, 2002, Rogaška Slatina, Slovenia
Correspondence to T. Drglin 相似文献
9.
A procedure for estimation of measurement uncertainty of routine pH measurement (pH meter with two-point calibration, with
or without automatic temperature compensation, combination glass electrode) based on the ISO method is presented. It is based
on a mathematical model of pH measurement that involves nine input parameters. Altogether 14 components of uncertainty are
identified and quantified. No single uncertainty estimate can be ascribed to a pH measurement procedure: the uncertainty of
pH strongly depends on changes in experimental details and on the pH value itself. The uncertainty is the lowest near the
isopotential point and in the center of the calibration line and can increase by a factor of 2 (depending on the details of
the measurement procedure) when moving from around pH 7 to around pH 2 or 11. Therefore it is necessary to estimate the uncertainty
separately for each measurement. For routine pH measurement the uncertainty cannot be significantly reduced by using more
accurate standard solutions than ±0.02 pH units – the uncertainty improvement is small. A major problem in estimating the
uncertainty of pH is the residual junction potential, which is almost impossible to take rigorously into account in the framework
of a routine pH measurement.1
Received: 11 August 2001 Accepted: 22 February 2002 相似文献
10.
11.
R. Kadis 《Accreditation and quality assurance》1998,3(6):237-241
Simple in principle, the evaluation of uncertainty, especially in chemical analysis, is not a routine task and needs great
care to be correct. This can be seen, particularly, from an examination of the EURACHEM Guide, Quantifying Uncertainty in Analytical Measurement (1995), which is the most important document on the subject. The examination reveals, in the author's opinion, a shortage
of correctness in some principal details of the uncertainty estimation process as presented in worked examples in the Guide,
and the author has therefore formulated some "in pursuit of correctness" rules for estimating uncertainty. The rules and respective
comments are concerned with the following items: (1) choosing an appropriate distribution function in type B evaluation of
uncertainty, (2) the necessity for consideration of separate contributions to the combined uncertainty, and (3) taking account
of actual influence factors in the uncertainty estimation process. Furthermore, the problem of estimation of conditional versus
overall uncertainty is touched upon in connection with comparative trials where only internal consistency of results is required.
Received: 29 January 1998 · Accepted: 10 February 1998 相似文献
12.
The current situation in the pharmaceutical industry is discussed, when the traceability of measurement (analytical) results to certified values of pharmacopoeial reference standards is required, without evaluating their uncertainties. It is shown that the evaluation of measurement uncertainty is necessary for understanding the level of confidence of the analytical results and their comparability, particularly during preparation and characterisation of the reference standards.Papers published in this section do not necessarily reflect the opinion of the Editors, the Editorial Board and the Publisher. Apart from exceptional circumstances, they are not submitted to the usual referee procedure and go essentially unaltered. 相似文献
13.
M. Buzoianu 《Accreditation and quality assurance》1998,3(8):328-334
The need for reliability of measurements supporting legal decisions in environmental policy or medical diagnosis and treatment
is well known and widely accepted. This prerequisite can be met only by ensuring that legal measurements are accurate and
traceable to national or international standards. Consequently, an outline of the organizational structure of the Romanian
National Institute of Metrology (INM) for ensuring uniformity, consistency and accuracy of all measurements including legal
measurements performed in chemical laboratories is presented. Since reliable measurements can only be accomplished within
an appropriate traceability chain, the experience of the INM in identification and evaluation of measurement uncertainty in
legal activities concerning the environment and health is reviewed. Practical examples of measurement uncertainty evaluation
in spectrophotometric determination of five analytes, commonly determined in environmental and clinical chemistry are described.
The implications of measurement uncertainty for interpretation of regulatory compliance are discussed.
Received: 3 January 1998 · Accepted: 9 June 1998 相似文献
14.
Dean A. Flinchbaugh L. F. Crawford David Bradley 《Accreditation and quality assurance》2001,6(12):493-500
A model is presented that correlates historical proficiency test data as the log of interlaboratory standard deviations versus
the log of analyte concentrations, independent of analyte (measurand) or matrix. Analytical chemistry laboratories can use
this model to set their internal measurement quality objectives and to apply the uncertainty budget process to assign the
maximum allowable variation in each major step in their bias-free measurement systems. Laboratories that are compliant with
this model are able to pass future proficiency tests and demonstrate competence to laboratory clients and ISO 17025 accreditation
bodies. Electronic supplementary material to this paper can be obtained by using the Springer LINK server located at http://dx.doi.org/
10.1007/s007690100398-y.
Received: 31 March 2001 Accepted: 11 September 2001 相似文献
15.
Quality assurance in analytical measurement 总被引:2,自引:0,他引:2
The peculiarities of analytical measurement require to check characteristics of the error (its components) of the obtained
analysis results to assure the quality of the measurements. This article deals with the various quality assurance procedures
and algorithms which are used to check the quality indices, i.e. the accuracy, reproducibility, certainty and repeatability
of analytical measurements: These procedures include: laboratory rapid control; Intra-laboratory statistical control (statistical
selection control by alternative attribute, statistical selection control by quantity method of periodic check of the analysis
procedure for conformity to the specified requirements) and external control (inter-laboratory control checks, inter-laboratory
comparison tests, and intra-laboratory control algorithms carried out by the appropriate supervisory body.) in the separately
taken laboratory. The respective algorithms, control plans and control requirements, specified according to the different
control aims and assurance tasks, enable the quality and certianty of analytical information obtained in laboratories in Russia
to be assured.
Received: 9 November 1998 / Accepted: 24 November 1998 相似文献
16.
The new traceability system of measurement standards based on the Japanese Measurement Law has been established since November
1993. Some reference materials such as metal standard solutions, pH standard solutions and standard gas mixtures are included
in the system together with relevant physical quantities. In this system, primary measurement standard instruments or primary
reference materials are designated by the regulation for each quantity. For the practical dissemination of each quantity,
accreditation of calibration bodies is recognized by the steering committee under the supervision of the government. In the
course of assessment of a candidate calibration body, the concepts of ISO/IEC Guide 25 and ISO/IEC Guide 58 are effectively
introduced. For the estimation of reliability, the concept of how to introduce the statistical approach is effectively considered.
The method of uncertainty evaluation described in the ISO document entitled "Guide to the expression of uncertainty in measurement"
is adopted. 相似文献
17.
Irina Ekeltchik Elena Kardash-Strochkova Orna Dreazen I. Kuselman 《Accreditation and quality assurance》2002,7(10):412-416
Dependence of the uncertainty of a pH measurement result on the quality of buffers (i.e. the uncertainty of their certified
pH values) at different levels of instrumental uncertainty (pH-meter, etc.) was simulated using the Monte Carlo method and
regression analysis. The contribution of the instrumental standard uncertainty (in the studied range from 0.1 to 1 mV) to
the uncertainty of the pH measurement result is negligible, if the standard uncertainties of the pH buffers exceed 0.04 pH
(e. g. for in-house buffers). It is shown how the choice of pH-meter and buffers should be correlated in order to meet the
required uncertainty of a pH measurement result in a sample under analysis. The results of the simulation were compared with
experimental data obtained from calibrations of a pH/ion-meter with a hydrogen working electrode (Radiometer PHM-240) and
with a glass electrode (Metrohm 744). Buffers of different quality (National Institute for Standards and Technology standard
reference materials, certified Radiometer buffers and Merck CertiPUR buffers) were used for the calibrations. The uncertainties
of the experimental results are close to the predicted ones obtained by the simulation.
Received: 16 June 2002 Accepted: 19 July 2002
Presented at the 14th International Conference of the Israel Society for Quality, 18–21 November 2002, Jerusalem, Israel
Correspondence to I. Kuselman 相似文献
18.
An analytical result is not considered to be complete without a statement of the measurement uncertainty associated with
it. Evaluation of measurement uncertainty is therefore an essential part of every determination. In the present study the
measurement uncertainty of the result of determination of selenium in the reference material Seronorm Trace Elements Serum
was studied. The combination of a digestion procedure using sulfuric acid, V2O5 in H2SO4 and hydrogen peroxide and the continuous flow approach of hydride generation atomic fluorescence spectrometry (HG-AFS) detection
was used for selenium determination. The total uncertainty budget was calculated with the help of the GUM Workbench program,
in which computations follow the rules of the ’ISO guide to the expression of uncertainty in measurement’. The major sources
of uncertainty were found to be due to the recovery of the procedure, measurement of peak heights and the purity of Na2SeO3. A selenium mass fraction of 77.1±4.8 ng/g (with a coverage factor of 2.1, 95% probability) was determined, which is comparable
with the recommended value of 80 ng/g.
Received: 13 September 2002 Accepted: 23 December 2002
Acknowledgements We would like to thank Tinkara Buˇcar, B.Sc. for useful discussions and the IAEA Vienna, for financial support of the project
11553/RO.
Presented at CERMM-3, Central European Reference Materials and Measurements Conference: The function of reference materials
in the measurement process, May 30–June 1, 2002, Rogaška Slatina, Slovenia
Correspondence to V. Stibilj 相似文献
19.
Marc Priel 《Accreditation and quality assurance》2009,14(5):235-241
Since the advent of the Guide to the expression of Uncertainty in Measurement (GUM) in 1995 laying the principles of uncertainty
evaluation numerous projects have been carried out to develop alternative practical methods that are easier to implement namely
when it is impossible to model the measurement process for technical or economical aspects. In this paper, the author presents
the recent evolution of measurement uncertainty evaluation methods. The evaluation of measurement uncertainty can be presented
according to two axes based on intralaboratory and interlaboratory approaches. The intralaboratory approach includes “the
modelling approach” (application of the procedure described in section 8 of the GUM, known as GUM uncertainty framework) and
“the single laboratory validation approach”. The interlaboratory approaches are based on collaborative studies and they are
respectively named “interlaboratory validation approach” and “proficiency testing approach”. 相似文献
20.
R. J. N. Bettencourt da Silva M. Filomena G. F. C. Camões João Seabra e Barros 《Accreditation and quality assurance》1998,3(4):155-160
Every analytical result should be expressed with some indication of its quality. The uncertainty as defined by Eurachem ("parameter
associated with the result of a measurement that characterises the dispersion of the values that could reasonably be attributed
to the, . . ., quantity subjected to measurement") is a good tool to accomplish this goal in quantitative analysis. Eurachem
has produced a guide to the estimation of the uncertainty attached to an analytical result. Indeed, the estimation of the
total uncertainty by using uncertainty propagation laws is components-dependent. The estimation of some of those components
is based on subjective criteria. The identification of the uncertainty sources and of their importance, for the same method,
can vary from analyst to analyst. It is important to develop tools which will support each choice and approximation. In this
work, the comparison of an estimated uncertainty with an experimentally assessed one, through a variance test, is performed.
This approach is applied to the determination by atomic absorption of manganese in digested samples of lettuce leaves. The
total uncertainty estimation is calculated assuming 100% digestion efficiency with negligible uncertainty. This assumption
was tested.
Received: 3 November 1997 · Accepted: 2 January 1998 相似文献