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1.
K. Heydorn 《Accreditation and quality assurance》1998,3(3):111-114
Stability tests are carried out on candidate reference materials in order to ascertain that the certification values continue
to be valid a reasonable time after completion of the certification analysis. These tests are also used for recommending storage
conditions, as well as the duration of storage before certification values need be rechecked. BCR (Community Bureau of Reference)
reference materials do not normally have an expiry date, but rely on stability monitoring throughout the lifetime of the certified
material. The 1997 version of the BCR Guidelines for the production and certification of reference materials does, however,
take into account the necessity of limiting the validity of a certification, when degradation of the material during storage
cannot be ignored. This paper discusses an example of significant degradation taking place between the time of completion
of the certification analysis and the issue of a formal certificate. Various options are presented together with an account
of their influence on the certified values and their uncertainties.
Received: 3 October 1997 · Accepted: 3 November 1997 相似文献
2.
Since the uncertainty of each link in the traceability chain (measuring analytical instrument, reference material or other
measurement standard) changes over the course of time, the chain lifetime is limited. The lifetime in chemical analysis is
dependent on the calibration intervals of the measuring equipment and the shelf-life of the certified reference materials
(CRMs) used for the calibration of the equipment. It is shown that the ordinary least squares technique, used for treatment
of the calibration data, is correct only when uncertainties in the certified values of the measurement standards or CRMs are
negligible. If these uncertainties increase (for example, close to the end of the calibration interval or shelf-life), they
are able to influence significantly the calibration and measurement results. In such cases regression analysis of the calibration
data should take into account that not only the response values are subjects to errors, but also the certified values. As
an end-point criterion of the traceability chain destruction, the requirement that the uncertainty of a measurement standard
should be a source of less then one-third of the uncertainty in the measurement result is applicable. An example from analytical
practice based on the data of interlaboratory comparisons of ethanol determination in beer is discussed.
Received: 5 October 2000 Accepted: 3 December 2000 相似文献
3.
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
4.
E. Vasileva S. Azemard J. Oh P. Bustamante M. Betti 《Accreditation and quality assurance》2011,16(8-9):439-447
A marine certified reference material (CRM), IAEA-452, prepared with scallop (Pecten maximus) sample was recently produced by the International Atomic Energy Agency (IAEA) and certified for trace elements and methyl mercury (MeHg). The Scallop (Pecten maximus) sample is commonly found and consumed seafood and is also used as bio-indicators for trace metal contamination in marine pollution studies. This paper presents the sample preparation methodology, material homogeneity and stability studies, evaluation of certification campaign results, the assignment of property values and their associated uncertainty. The reference values and associated expanded uncertainty for 9 trace elements (As, Cd, Cr, Cu, Fe, Hg, Mn, Pb and Zn) and MeHg in scallop sample are established. The informative value for one more element (Ni) is also given. The new CRM can be used for the development and validation of analytical methods for determination of trace elements and methyl mercury in seafood and also for quality assurance/quality control purposes. 相似文献
5.
Adriaan M. H. van der Veen Thomas P. J. Linsinger Andree Lamberty Jean Pauwels 《Accreditation and quality assurance》2001,6(6):257-263
To serve as a measurement standard, a (certified) reference material must be stable. For this purpose, the material should
undergo stability testing after it has been prepared. This paper looks at the statistical aspects of stability testing. Essentially,
these studies can be described with analysis of variance statistics, including variant regression analysis. The latter is
used in practice for both trend analysis and for the development of expressions for extrapolations. Extrapolation of stability
data is briefly touched upon, as far as the combined standard uncertainty of the reference material is concerned. There are
different options to validate the extrapolations made from initial stability studies, and some of them might influence the
uncertainty of the reference material and/or the shelf-life. The latter is the more commonly observed consequence of what
is called ’stability monitoring’.
Received: 6 October 2000 Accepted: 4 December 2000 相似文献
6.
C. S. Phinney K. E. Murphy M. J. Welch P. M. Ellerbe S. E. Long K. W. Pratt S. B. Schiller L. T. Sniegoski M. S. Rearick T. W. Vetter R. D. Vocke 《Fresenius' Journal of Analytical Chemistry》1998,361(2):71-80
The National Institute of Standards and Technology (NIST) has developed several Standard Reference Materials (SRMs) based
on human serum. NIST SRM 909b, Human Serum, is a lyophilized human serum material with concentrations for seven organic and
six inorganic analytes at two levels certified solely by definitive methods (DMs). This material provides the vehicle by which
high precision, high accuracy measurements made with DMs at NIST can be transferred through the measurement hierarchy to other
laboratories. Isotope dilution gas chromatographic-mass spectrometric (GC-IDMS) methods were applied to measure cholesterol,
creatinine, glucose, urea, uric acid, triglycerides, and total glycerides. Thermal ionization isotope dilution mass spectrometry
(TI-IDMS) was used for determination of lithium, magnesium, potassium, calcium, and chloride. In addition, chloride was determined
by coulometry, providing a comparison between two DMs. Sodium, which lacks a stable isotope that would permit isotope dilution
mass spectrometric (IDMS) measurement, was determined by gravimetry. SRM 909b includes certified values for total glycerides
and triglycerides, which were not certified in the previous lot of this material (SRM 909a). Improvement in uniformity of
vial fill weight in the production of SRM 909b resulted in smaller certified uncertainties over previous freeze-dried serum
SRMs. Uncertainties at the 99% level of confidence for relative expanded uncertainty (%) for certification of the organic
analytes on a mmol/L/g basis ranged from 0.44% for urea (level II) to 5.04% for glucose (level II). (In-house studies have
shown glucose to be a relatively unstable analyte in similar lyophilized serum materials, degrading at about 1% per year.)
Relative expanded uncertainties (99% C.I.) for certification of inorganic analytes on a mmol/L/g basis ranged from 0.25% for
chloride (level I) to 0.49% for magnesium (level II).
Received: 30 July 1997 / Revised: 24 October 1997 / Accepted: 31 October 1997 相似文献
7.
The element contents of Ag, Al, As, Be, Bi, Cd, Co, Cr, Fe, Mg, Mn, Ni, P, Pb, S, Sb, Se, Sn, Te, Ti, Zn and Zr in a pure
copper (99.5%) sample (CRM BAM-376) for use in spark emission and X-ray fluorescence spectrometry were certified and the certified
values are given. For Si, the certification has not yet been completed, the content of this element will be certified later.
The sample was produced and certified in collaboration with the Committee of Chemists of the GDMB Gesellschaft für Bergbau,
Metallurgie, Rohstoff- und Umwelttechnik. Data of the homogeneity testing and the certification campaign with 14 participating
laboratories using different analytical methods are reported.
Received: 3 February 1997/Revised: 21 February 1997/Accepted: 5 March 1997 相似文献
8.
P Robouch M Eguskiza M I Maguregui S Pommé J Pauwels 《Fresenius' Journal of Analytical Chemistry》2001,370(2-3):255-258
The main concern of producers of certified reference materials (CRM) is the preparation of high-quality products with demonstrated homogeneity and stability, combined with a well established set of certified characteristics. CRM producers must, furthermore, comply with other constraints imposed by the ISO Guide 34: production processes, production control, and certification analyses should be performed by expert laboratories, using validated protocols documented in their respective quality assurance manuals; laboratory mean values and the corresponding "expanded" uncertainties, must be used for the determination of the certified values, as recommended by the ISO Guide to the Expression of Uncertainties in Measurements (GUM); and when possible, traceability of the certified value to the SI units, using appropriately validated and/or primary methods, must be ensured. k0-NAA, i.e. neutron activation analysis with k0 standardization, is one of the analytical techniques implemented at the Reference Material Unit of IRMM; it meets the first two requirements. 相似文献
9.
The stability of pH and certified amounts of nitrate, ammonia, total soluble nitrogen, total soluble organic carbon, magnesium,
sodium, potassium and phosphorus obtained by extraction from air-dried (40 °C) soil samples by 0.01 mol/L CaCl2 solution during storage at –18 °C, 4 °C, ambient temperature, 40 °C and 70 °C was investigated in one calcareous soil and
one acid sandy soil. Even at storage times of 45 and 90 days, extractable amounts changed. Extractable amounts of P, NH4-N, total soluble N and soluble organic C increased even at a storage temperature of 40 °C. The pH was lower for samples stored
at a temperature of 70 °C and also the Mg concentration became lower at elevated storage temperatures after 45 days in both
soils. It is suggested that reference materials certified for values using unbuffered extractants should be stored at a temperature
not higher than 4 °C.
Received: 13 May 1997 / Revised: 16 July 1997 / Accepted: 18 July 1997 相似文献
10.
D. A. Becker 《Journal of Radioanalytical and Nuclear Chemistry》1993,168(1):169-183
The ASTM Task Group on Nuclear Methods of Chemical Analysis (E10.05.12) has conducted a trace element intercomparison among some of its members over the past two years. Eight non-NIST laboratories submitted data using nuclear techniques, with a total of 111 values for the apple leaves and 116 values for the peach leaves, on 46 and 50 elements, respectively. This intercomparison provided a unique opportunity for the analytical laboratories, because the analytical values submitted could be later compared to the NIST certified values. For the seven elements which were certified by NIST and had three or more intercomparison values, the results showed that: 1) 61% of all 56 intercomparison values submitted had results whose stated uncertainty overlapped the uncertainty limits of the NIST certified values, and 2) less than 6% of the intercomparison values had means which fell outside ±20% of the NIST values. In general, the intercomparison values submitted showed excellent agreement with the NIST values. However, many reported uncertainties accompanying intercomparison values appeared overly optimistic. 相似文献
11.
P. Robouch M. Eguskiza M. I. Maguregui S. Pommé J. Pauwels 《Analytical and bioanalytical chemistry》2001,370(2-3):255-258
The main concern of producers of certified reference materials (CRM) is the preparation of high-quality products with demonstrated homogeneity and stability, combined with a well established set of certified characteristics. CRM producers must, furthermore, comply with other constraints imposed by the ISO Guide 34: ·*production processes, production control, and certification analyses should be performed by expert laboratories, using validated protocols documented in their respective quality assurance manuals; ·*laboratory mean values and the corresponding “expanded” uncertainties, must be used for the determination of the certified values, as recommended by the ISO Guide to the Expression of Uncertainties in Measurements (GUM); and ·*when possible, traceability of the certified value to the SI units, using appropriately validated and/or primary methods, must be ensured. k0-NAA, i.e. neutron activation analysis with k0 standardization, is one of the analytical techniques implemented at the Reference Material Unit of IRMM; it meets the first two requirements. 相似文献
12.
A semi-preparative high-performance liquid chromatography process was evaluated as a tool to quantitatively determine the
purity or percentage mass fraction content (% m/m) of organic compounds. The method is simple and does not require the identification and subsequent quantitation of organic-related
structure impurities. A protocol was developed and tested on four reference materials certified for purity from 95% m/m to 99.3% m/m. Comparing the purity results of each certified reference material using the new approach with their respective certified
values showed no significant analytical bias. Semi-preparative high-performance liquid chromatography has proved the potential
to be a primary method directly traceable to mass with an uncertainty statement written down also in terms of mass with expanding
uncertainty ranging from 0.8% to 1.3% m/m compared to 0.3 to 2.0% m/m for the certified purity values at the 95% confidence interval. 相似文献
13.
A new reliable analytical method, "Monochromatic X-ray Excitation X-ray Fluorescence Spectrometry", has been proposed. For validating the method, trace elements in sediment certified reference materials were determined. In the method X-ray fluorescence spectra are measured for specimens and pure metals; in addition the mass-attenuation coefficients of the specimens for various X-ray wavelengths are also measured. The data are analyzed by the fundamental parameter method and the uncertainty of the analysis is evaluated. The obtained results were in satisfactory agreement with the certified values within their uncertainties. This method will be applicable to the certification of reference materials, in the field of which reliable results with uncertainty statements are required. 相似文献
14.
Nitroimidazoles have been applied in the past to poultry and pigs to treat protozoan diseases and to combat bacterial infections, but due to adverse health effects their use in food-producing animals has meanwhile been banned in the EU. The request for a certified reference material in a representative matrix was stipulated by the responsible Community Reference Laboratory and is underpinned by the need to improve the accuracy and comparability of measurement data and to establish metrological traceability of analytical results. The Institute for Reference Materials and Measurements (IRMM) has responded to this demand by developing and producing a new certified matrix reference material, ERM-BB124. This incurred lyophilised pork meat material was certified according to ISO guides 34 and 35 for the mass fractions of six nitroimidazole compounds. Processing of the frozen muscle tissue to the final material was accomplished by application of cutting, freeze-drying, mixing and milling techniques. Homogeneity and stability measurements were performed using liquid chromatography tandem mass spectrometry. The relative standard uncertainty due to possible heterogeneity showed to be below 1.8% for all analytes. Potential degradation during transport and storage was assessed by isochronous stability studies. No significant instability was detected at a storage temperature of −20 °C for a shelf-life of 2 years. The certified mass fraction values were assigned upon evaluation of the data acquired in an international laboratory inter-comparison involving 12 expert laboratories using different sample preparation procedures, but exclusively LC-MS/MS methods. Relative standard uncertainty contributions for the characterisation (between-lab variation of mean values) were found to be between 1.6 and 4.8%. Certified values for five analytes were in the range of 0.7 to 6.2 μg kg−1, with expanded relative uncertainties ranging between 7 and 14%. Dimetridazole could be certified as “<0.25 μg kg−1 with a probability of 95%”. All values are traceable to the International System of Units (SI). The material is intended to be used for method validation purposes (including trueness estimation) and for method performance assessment. 相似文献
15.
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
16.
J. Medved Vladimír Streko Jana Kubová Jozefa Polakoviová 《Fresenius' Journal of Analytical Chemistry》1998,360(2):219-224
Nine decomposition procedures for soil samples, such as via acid mixtures and fusion in open systems and microwave and autoclave
dissolution (in closed systems under elevated temperature and pressure) were assessed using certified soil reference materials.
The determination of various elements in solutions was performed by FAAS and ICP-OES and the results were compared with certified
values and with direct current arc OES analysis.
Received: 3 March 1997 / Revised: 30 May 1997 / Accepted: 3 June 1997 相似文献
17.
Josef Kratochvíla Bedřich Friedecký Marek Budina Ilona Šperlingová 《Accreditation and quality assurance》2007,12(3-4):146-150
In this paper, the creation of a certified reference material for urinary creatinine is described. We used the Jaffe method
and HPLC method for establishment of the certified value. Homogeneity tests are also described. We obtained material with
sufficient homogeneity, stability, and with certified value (expanded uncertainty, k=2 for CI 95%) (7.77±0.27) mmol·L−1. This material was consequently used for the interlaboratory comparison (EQA Czech Republic for clinical chemistry). Twenty-nine
percent of the participants obtained measurement results within the interval of the certified value ± expanded uncertainty,
while 85% of the participants obtained values inside the interval of the certified value ± target measurement uncertainty.
Direct use of the certified reference materials for method evaluation in EQA programs means a significant advance for monitoring
and documentation traceability of results in routine measurements. 相似文献
18.
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 相似文献
19.
The European Reference Laboratory of Air Pollution implements the static volumetric method for the preparation of nitrogen
monoxide and sulphur dioxide reference standard gas mixtures. According to the new ISO guide for the expression of uncertainty,
the uncertainty of these standards is up to 0.8% for nitrogen monoxide in the range 100 to 600 ppbv, and up to 0.4% for sulphur
dioxide in the range 200 to 400 ppbv. The values presented in the present paper suggest that there is a 95% probability of
the true value lying within the interval specified. To attain such low uncertainty values, the standard procedure for the
implementation of the static volumetric method must be rigorously followed, and instruments must be carefully maintained.
Received: 26 June 1997 · Accepted: 23 August 1997 相似文献