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Impact of cryogenic grinding on iodine homogeneity in NIST SRM 1548a Typical Diet
Kameník, Jan ; Kučera, Jan
The reference material NIST SRM 1548a Typical Diet has a certified iodine mass fraction of 0.759±0.103 mg kg-1. The expanded uncertainty is rather large (relative value 13.6 %), thus the material does not provide strict requirements for quality control results. Milling of NIST SRM 1548a at the temperature of liquid nitrogen yielded free-flowing material. Iodine mass fraction in the original and cryo-ground materials was determined by epithermal neutron activation analysis (ENAA) and radiochemical neutron activation analysis (RNAA). The average and standard deviation from both methods was 0.73±0.03 mg kg-1 (20 values). The determined mass fraction was in a close agreement with the certified value of NIST SRM 1548a, thus iodine total content was not influenced by the milling procedure. In comparison to iodine mass fraction determined in the original NIST SRM 1548a 0.72±0.07 mg kg-1 (average ± standard deviation, 14 values), the standard deviation for cryo-ground material was considerably lower. The prepared quality control material sets up more stringent requirements on the validation and quality control procedures of the measurement of iodine mass fraction in such a composite food matrices. We believe that the iodine random inhomogeneity in the original NIST SRM 1548a is due to insufficient mixing of some iodine-rich component in the complex food matrices. Milling at the temperature of liquid nitrogen offers an effective option for production of future reference materials of this kind.
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IMPEDANCE MEASUREMENT OF GAS SENSORS WITH NICKEL(II)-AND COPPER(II)-OXIDE ACTIVE LAYERS
Horák, Pavel ; Khun, J. ; Vrňata, M. ; Bejšovec, Václav ; Lavrentiev, Vasyl ; Vacík, Jiří
Thin layers (90 nm) of nickel(II)- and copper(II)- oxide were deposited onto ceramic sensor substrates equipped with interdigital electrodes for signal reading. The deposition was carried out in two or three steps: (i) sputtering by means of Ar ion beam from pure (99.99%) metal targets, (ii) following thermal oxidation (400 degrees C for 5 h) in air, (iii) in some cases - sputtering of Pd catalyst to the surface. Then the impedance response of produced sensors (NiO, NiO+Pd, CuO, CuO+Pd) to 1000 ppm of hydrogen and 1000 ppm of methanol vapor was measured. Impedance measurements were performed in the frequency range from 40 Hz to 100 MHz. The obtained data were depicted in Nyquist representation (i.e. imaginary vs. real part of complex impedance). These diagrams have a character of one complete and one incomplete semicircle, each of them corresponding to a parallel RC-element. It was proved, that both NiO and CuO behave like p-type semiconductors; the sensor impedance increases on exposure to reducing gases. The best sensitivity was achieved on NiO+Pd sensor - during detection of hydrogen (1000 ppm) the real part of complex impedance measured at 40 Hz increased from 120 to 350 Omega.
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A comparative study of the total mercury determination in highly contaminated soils by AAS and RNAA methods
Sysalová, J. ; Kučera, Jan ; Zvěřina, O.
High total mercury (T-Hg) contents in soils, up to 25 mg kg−1, were determined by two independent methods: a one-purpose atomic absorption spectrometer AMA-254 (Advanced Mercury Analyser) with direct solid sampling, and radiochemical neutron activation analysis (RNAA), using sample masses of 10 mg to 25 mg and about 150 mg, respectively. An excellent agreement between results of both methods was obtained. For quality control (QC) purposes, NIST SRM 2711 Montana Soil and NIST SRM 2711a were analysed by both methods using the above sample masses. The results obtained were compared with the NIST certified values within the uncertainty margins, thus proving the accuracy of the procedures employed. It has been found that the cryogenic grinding used provided sufficiently representative and homogeneous samples. A test in which HgS was analysed by RNAA showed that even mercury present in sulfide form would be fully recovered using the procedures employed. For contents of T-Hg above the upper limit of the AMA-254 working range (500 ng), samples were firstly diluted with sea sand in the ratio 1:10 and homogenised well to get RSD below 5%. The dilution procedure was verified using the certified reference material ERM-CC580 Estuarine Sediment.
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Determination of reference values of element contents in certified reference material SWCNT-1 by INAA a PGAA
Kučera, Jan ; Sturgeon, R. E. ; Grinberg, P. ; Oflaz, R. ; Paul, R. L. ; Bennett, J. W. ; De Nadai Fernandes, E. A. ; Kubešová, Marie ; Bacchi, M. A. ; Stopic, A. J.
Instrumental neutron activation analysis with both relative and k-0 standardization was used in four experienced laboratories to determine element mass fractions in single-wall carbon nanotube certified reference material (CRM) SWCNT-1. Results obtained were evaluated using the NIST “Type B On Bias” approach and yielded consensus values in agreement with NRCC certified values for Fe, Co, Ni and Mo and provided mass fraction values for thirteen additional elements, namely Na, Mg, Al, K, Ca, Ti, V, Cr, Mn, Br, La, W and Au. In addition, prompt gamma neutron activation analysis was employed to determine mass fractions of H, B, Co, Ni, and Mo. Results of this work provide a basis for the establishment of reference values of element mass fractions in CRM SWCNT-1, thus expanding its usability for more accurate characterization and benchmarking of similar nanotechnology materials.
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NANOSTRUCTURE CHARACTERIZATION OF IN738LC SUPERALLOY FATIGUED AT HIGH TEMPERATURE
Petrenec, M. ; Strunz, Pavel ; Gasser, U. ; Heczko, Milan ; Zálešák, J. ; Polák, Jaroslav
The nanostructure of Inconel 738LC Ni-superalloy strengthened by trimodal Y precipitates distribution was investigated after Low Cycle Fatigue (LFC) loading at temperature 700°C. Different microscopic techniques as Scanning Electron Microscope (SEM) equipped with STEM detectro, transmission Kikuchi diffraction in the SEM, transmission electron microscope (TEM) in the bright field mode and high resolution transmission electron mciroscopes (HRTEM) in STEM mode were used for the characterization and quantification of superalloy nanostructure. The characteristic morphology of y precipitates was examined by ex-situ and in-situ Small Angle Neutron Scattering (SANS) at high temperatures. All adopted microscopic techniques indicate that the morphology of y precipitates distributed in the y matrix as recived state corresponds to two types, i.e. large cuboid-like precipitates with the size around 670 nm, and the spherical precipitates with the diameter 52nm. After eh LCF tests at temperature 700°C, the ex-situ SANS measurement yielded addititonal scattering intensities coming from another small y precipitetes with estimated size up to 10nm.
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NANOSTRUCTURE CHARACTERIZATION OF IN738LC SUPERALLOY FATIGUED AT HIGH TEMPERATURE
Petrenec, M. ; Strunz, Pavel ; Gasser, U. ; Heczko, Milan ; Zálešák, J. ; Polák, Jaroslav
The nanostructure of Inconel 738LC Ni-superalloy strengthened by trimodal γ’ precipitates distribution was investigated after Low Cycle Fatigue (LCF) loading at temperature 700°C. Different microscopic techniques as Scanning Electron Microscope (SEM) equipped with STEM detector, transmission Kikuchi diffraction in the SEM, transmission electron microscope (TEM) in the bright field mode and high resolution transmission electron microscopes in STEM mode were used for the characterization of nanostructure. The characteristic morphology of γ’ precipitates was examined by ex-situ and in-situ Small Angle Neutron Scattering (SANS) at high temperatures. All microscopic techniques indicate that the morphology of γ’ precipitates distributed in the γ matrix as received state corresponds to two types, i.e. large cuboid-like precipitates with the size around 670 nm, and the spherical precipitates with the diameter 52 nm. After the LCF tests at temperature 700°C, the ex-situ SANS measurement yielded additional scattering intensities coming from another small γ’ precipitates with estimated size up to 10 nm.
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Determination of iodine in biological materials by neutron activation analysis
Kučera, Jan
The advantages and disadvantages of various modes of neutron activation analysis (NAA), such as instrumental NAA (INAA), epithermal NAA (ENAA), and radiochemical NAA (RNAA) for iodine determination in biological materials, namely in food and diet samples are briefly reviewed. Examples are given of iodine determination in Asian diet samples by ENAA and RNAA. The accuracy of the results obtained was proved by analyses of numerous US NIST reference materials (RMs) of biological origin.
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