The new accreditation standard ISO/IEC 17025: 1999 requires laboratories to estimate the uncertainty of
measurement.
“I used to be uncertain – now I’m not so sure”
Uncertainty does not inspire confidence, but from an analytical laboratory perspective, uncertainty defines the range of the values that could reasonably be attributed to an analytical result. Uncertainty arises as a
result of random effects, such as short-term fluctuations in temperature, relative humidity and power source
variations or a result of systematic effects, such as instrumental drift between calibrations. When laboratories
report uncertainty it gives a quantitative indication of the quality of the analytical results, and it allows the
user of the result to:
- Assess its reliability.
- Assess the confidence that can be placed on a result, when comparing it with a limiting value
defined in a specification or regulation.
- Compare analytical results e.g., from different laboratories.
- Assess the “fitness for purpose” of the result.
The complexity involved in estimation of uncertainty of measurement in the case of testing varies
considerably from one test field to another and also within one field itself. A less metrologically rigorous
process than that which can be followed for calibration can also often be used. Clause 5.4.6.2 of ISO/IEC
17025 allows for these factors. The degree of rigor needed in an estimation of uncertainty of measurement
depends on factors such as:
- Requirement of the test method.
- Requirement of the client.
- There are narrow limits on which decisions conformance to a specification are based.
If the test method is well recognized (ASTM, ISO) and specifies limits to the values of the major sources of
uncertainty of measurement, and specifies the form of presentation of calculated results, the laboratory is
considered to have satisfied this clause by following the test method and reporting instructions. Clause
5.4.6.3 states that uncertainty components/budgets are a combination of many factors that may include, but
are not limited to:
- Sampling – where in-house or field sampling form part of the specified procedure, effects such
as random variations between different samples and any potential for bias in the sampling
procedure.
- Storage conditions – where test sample is stored prior to analysis, the storage conditions may
affect the analytical result.
- Properties and condition of item being tested.
- Equipment used – limits of accuracy of instruments used in the measurement process i.e.,
analytical balance.
- Analytical method used – assumed stoichiometry, reagent purity, instrument settings, blank
correction.
- Reference standards.
- Reference materials.
- Environmental conditions.
- Calibration.
- Operator effects.
- Known physical characteristics of components such as, coefficient of thermal expansion. These
often can be looked up in engineering and scientific handbooks.
- Data processing.
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Uncertainty of measurement comprises, in general, many components. Some of these components may be estimated on the basis of the statistical distribution of the results of series of measurements and can be characterized by experimental standard deviations, and are called Type A evaluation. The Type A can be applied when several independent observations have been made for one of the input quantities under the same conditions of measurement. If there is sufficient resolution in the measurement process, there will be an observable scatter or spread in the values obtained. In this case, the standard uncertainty is the experimental standard deviation of the mean that follows from an averaging procedure or an appropriate regression analysis. |
Estimates of other components can only be based on experience or other information, and are called Type B evaluation. Values belonging in this category may be derived from:
- Previous measurement data.
- Experience with or general knowledge of the behaviour and properties of relevant materials and instruments.
- Manufacturer’s specifications.
- Data provided in calibration and other certificates.
- Uncertainties assigned to reference data taken from handbooks.
The measurement uncertainty for a given calibration is the combination of all the type A and type B components of the uncertainty budget. |