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The need for quality assessment of anthropogenic impact on environmental pollution is increasing due to discharge from various industries, the use of chemicals in agriculture and the consumption of fossil fuels. Diminishing resources such as natural waters used for the cultivation of agricultural products, plant and animal habitats are under severe pollution pressure and are at constant risk. Several parameters, such as Pb, Cd, Ni, Hg were listed by Water Framework Directive in Directive(2008/105/EC) in the priority substances. Cadmium and Hg were identified as priority hazardous substances whereas As is an important contaminant for its potential toxicological and carcinogenic effects. An inter-comparison study is organised in EURAMET TC-MC in order to demonstrate the capability participants for measuring five elements in river water. The participants carried out measurements for analytes: Pb, Cd, Ni and As as mandatory elements, and Se as an optional one. Participants were asked to perform the measurements with respect to the protocol provided. To reach the main text of this paper, click on Final Report. Note that this text is that which appears in Appendix B of the BIPM key comparison database https://www.bipm.org/kcdb/.
The final report has been peer-reviewed and approved for publication by the CCQM, according to the provisions of the CIPM Mutual Recognition Arrangement (CIPM MRA).
We present here the design and characterization of a set of spectral calibration beads. These calibration beads are intended for the determination and regular control of the spectral characteristics of fluorescence microscopes and other fluorescence measuring devices for the readout of bead-based assays. This set consists of micrometer-sized polymer beads loaded with dyes from the liquid Calibration Kit Spectral Fluorescence Standards developed and certified by BAM for the wavelength-dependent Determination of the spectral responsivity of fluorescencemeasuring devices like spectrofluorometers. To cover the wavelength Region from 400 to 800 nm, two new near-infrared emissive dyes were included, which were spectroscopically characterized in solution and encapsulated in the beads. The resulting set of beads presents the first step towards a new platform of spectral calibration beads for the determination of the spectral characteristics of fluorescence instruments like fluorescence microscopes, FCM setups, and microtiter plate readers, thereby meeting the increasing demand for reliable and comparable fluorescence data especially in strongly regulated areas, e.g., medical diagnostics. This will eventually provide the basis for standardized calibration procedures for imaging systems as an alternative to microchannel slides containing dye solutions previously reported by us.
The inter-instrument, inter-laboratory, and long-term comparability of fluorescence data requires the correction of the measured emission and excitation spectra for the wavelength- and polarization-dependent spectral irradiance of the excitation channel at the sample position and the spectral responsivity of the emission channel employing procedures that guarantee traceability to the respective primary standards. In this respect the traceability chain of fluorometry is discussed from a radiometrists point of view. This involves, in a first step, the realization of the spectral radiance scale, based on the blackbody radiator and electron storage ring, and the spectral responsivity scale, based on the cryogenic radiometer and their control via key comparisons of the national metrology institutes. In a second step, the characterization including state-of-the art uncertainties of the respective source and detector transfer standards such as tungsten strip lamps, integrating sphere radiators, and trap detectors used to disseminate these radiometric quantities to users of spectroscopic techniques is presented.
The present study addresses the capability of measurement of relative particle number concentration by scanning electron microscopy for model bimodal silica and gold samples prepared in the frame of the European research project “nPSize - Improved traceability chain of nanoparticle size measurements” as candidate reference nanoparticles.
An international interlaboratory comparison of the measurement capabilities of four National Metrology Institutes (NMIs) and one Designated Institute (DI) in the determination of the chemical composition of thin Fe-Ni alloy films was conducted via a key comparison (K-67) of the Surface Analysis Working Group of the Consultative Committee for Amount of Substance. This comparison was made using XPS (four laboratories) and AES (one laboratory) measurements. The uncertainty budget of the measured chemical composition of a thin alloy film was dominated by the uncertainty of the certified composition of a reference specimen which had been determined by inductively coupled plasma mass spectrometry using the isotope dilution method. Pilot study P-98 showed that the quantification using relative sensitivity factors (RSFs) of Fe and Ni derived from an alloy reference sample results in much more accurate result in comparison to an approach using RSFs derived from pure Fe and Ni films. The individual expanded uncertainties of the participants in the K-67 comparison were found to be between 2.88 and 3.40 atomic %. The uncertainty of the key comparison reference value (KCRV) calculated from individual standard deviations and a coverage factor (k) of 2 was 1.23 atomic %.
Isotope amount ratios of krypton were measured on subsamples from one large batch of high purity krypton separated from the atmosphere. Synthetic mixtures of enriched krypton isotopes were used to calibrate the measurements with small uncertainties. The result is a primary isotopic gas standard (PIGS) IRMM-2030 with certified values for isotope ratios, isotopic composition, and molar mass of krypton with small combined uncertainties uc, evaluated according to the ISO/BIPM Guide (GUM). It is commercially available from IRMM-Geel or from MESSER (Duisburg, D). The certified krypton isotope amount ratios in the PIGS IRMM-2030 are as follows: n(78Kr)/n(84Kr)=0.006 232 5(55), n(80Kr)/n(84Kr)=0.040 107(17), n(82Kr)/n(84Kr)=0.203 43(12), n(83Kr)/n(84Kr)=0.201 79(11), and n(86Kr)/n(84Kr)=0.303 205(59) with expanded uncertainty U=kuc and coverage factor k=2. The molar mass of Kr in this sample is M(Kr)=83.798 02(16) g/mol. These values are in good agreement with published measurements of atmospheric krypton but have smaller combined uncertainties and are calibrated by means of synthetic isotope mixtures. The values of the PIGS are traceable to the SI. Measurements of isotope amount ratios of krypton in other samples can be linked to SI using this PIGS.
In Germany a system of primary amount of substance standards for elemental analysis is being developed, which forms the material´s basis for the National Standards for element determination. The metrological concept and technical approach is briefly described. The objective of traceability in chemistry, in this case for elemental determination, is illustrated on the example of copper.
The application of metrology in chemical analysis is today hampered by psychological and practical barriers. The argumentation is based on the differences in physical and chemical metrology, which arises mainly from the objects of the measurements. The term measurement is discussed in the realm of analytical chemistry with a special focus on the inherent relation between chemical identification and determination as well as the consequent use of the concept of traceability and uncertainty.