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Stanovení prvkového složení drog neutronovou aktivační analýzou pro zjišťování jejich původu - studie proveditelnosti
Kučera, Jan ; Kameník, Jan ; Sabol, J. ; Šesták, B. ; Kolář, P. ; Roman, M.
Analyzovali jsme pět vzorků heroinu a pět vzorků kokainu zachycených na území České republiky metodou instrumentální neutronové aktivační analýzy (INAA). Alespoň v jednom z analyzovaných vzorků heroinu jsme stanovili 16 stopových prvků, ve vzorcích kokainu se jednalo o 9 stopových prvků. Pozoruhodné rozdíly až v rozmezí několika řádů, jsme zjistili v obsazích prvků Na, Cl, Cr, Zn a Br, zejména ve vzorcích heroinu. Přesnost výsledků INAA jsme prokázali simultánní analýzou certifikovaného referenčního materiálu NIST SRM 1547 Peach Leaves. Výsledky stanovení stopových prvků v heroinu jsme porovnali s výsledky zahraničních autorů. Dosažené výsledky ukazují na vysoký potenciál metody INAA pro prvkovou charakterizaci drog za účelem zjištění jejich původu, způsobu výroby a čištění či způsobu ředění pro konečné uživatele. Pokládáme za účelné pokračovat v analýzách většího množství vzorků s konečným cílem vytvoření databáze prvkového složení vzorků zkonfiskovaných na území ČR, která by později mohla být rozšířena ve spolupráci se zahraničními protidrogovými a policejními orgány v mezinárodním měřítku.
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Polymeric nanofibrous scaffolds reinforced with diamond and ceramic nanoparticles for bone tissue engineering
Bačáková, Lucie ; Pařízek, Martin ; Staňková, Ľubica ; Novotná, Katarína ; Douglas, T.E.L. ; Brady, M. A. ; Kromka, Alexander ; Potocký, Štěpán ; Stránská, D.
Three types of nanofibrous scaffolds were prepared by electrospining: (1) poly(lactide-co-glycoside) (PLGA) scaffolds reinforced with 23 wt.% of diamond nanoparticles (DNPs), (2) poly(L-lactide) (PLLA) scaffolds with DNPs in concentration ranging from from 0.4 wt.% to 12.3 wt.%, and (3) PLLA scaffolds with 5 wt.% or 15 wt.% of hydroxyapatite (HAp) nanoparticles. The diameter of the nanofibers ranged between 160 and 729 nm. The nanofibers with nanoparticles were thicker and the void spaces among them were smaller. Mechanical properties of the nanoparticle-loaded scaffolds were better, as demonstrated by a rupture test in scaffolds with DNPs and by a creep behavior test in scaffolds with HAp. On PLGA scaffolds with DNPs, the human osteoblast-like MG-63 cells adhered in similar numbers and grew with similar kinetics as on pure PLGA scaffolds. Human bone marrow mesenchymal stem cells grew faster and reached higher population densities on PLGA-DNP scaffolds. However, on PLLA-based scaffolds, the activity of mitochondrial enzymes and concentration of osteocalcin in MG-63 cells decreased with increasing DNP concentration. On the other hand, the metabolic activity of MG-63 cells and content of osteocalcin in these cells were positively correlated with the HAp concentration in PLLA scaffolds. Thus, PLGA nanofibers with 23 wt% of DNPs and PLLA nanofibers with 5 and particularly 15 wt.% of HAp seem to be promising for bone tissue engineering.
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Vliv kryogenního mletí na homogenitu jódu v NIST SRM1548a 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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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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Applications of self-assembled 2D polystyrene nanosphere arrays
Domonkos, Mária ; Ižák, Tibor ; Demo, Pavel ; Kromka, Alexander
In this study nanosphere lithography (NSL) is demonstrated to be a low-cost, parallel and material independent fabrication process for creating periodic arrays of nanostructures using self-assembled nanospheres as templates. SA is the most feasible way to fabricate 2D or 3D colloidal crystals on large areas. After the mask preparation NSL uses different steps of plasma etching and deposition processes. The resulting patterned nanostructures have a wide range of applications in many important areas such as photonics, antireflection, surface wetting, biological and chemical sensing, solar cells, etc. This study focuses on an overview of applications of 2D colloidal crystals. First, structuring of substrate surfaces and the creation of various nano-objects (nanotips, nanopillars, nanocones) is shown. Next, direct growth of patterned structures (graphene nanomesh and diamond structures) is pointed out.
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Microscopic characterization of graphene material and electronic quality across neighbouring, differently oriented copper grains
Čermák, Jan ; Yamada, T. ; Ganzerová, Kristína ; Rezek, Bohuslav
We study graphene grown across the boundary of three such grains having bright, medium, and dark color in reflection. Raman micro-spectroscopy proves presence of mostly a monoor bi-layer graphene on all the grains. Yet intensity of Raman 2D band is grain-dependent: highest at the darkest grain and lowest at the brightest one. Contrary, conductive atomic force microscopy detects the highest conductivity at the brightest grain and the lowest current at the darkest grain. This is attributed to dominant electrical current path through graphene and underlying oxide thickness of which also depends on the type of copper grain. We correlate and discuss the results with view to better understanding of graphene growth and electronic properties on large area copper substrates.
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Reactive ion etching of polystyrene microspheres
Domonkos, Mária ; Ižák, Tibor ; Štolcová, L. ; Proška, J. ; Kromka, Alexander
This article gives a brief insight also into the principle of the nanosphere lithography and various plasma systems focusing on their properties and applicability for a subsequent topographical modification of surfaces prepared by NS lithography. In the experimental part of this study we present a successful manipulation of microspheres by reactive ion etching (RIE). A self-assembled monolayer close-packed array of monodisperse polystyrene microspheres is used as the primary template. The polystyrene microspheres (PM) were processed in capacitively coupled radiofrequency plasma (CCP) RIE system. The influence of process conditions on the PM geometry is systematically studied by scanning electron microscopy. The process conditions are controlled by varying radiofrequency power, total pressure, composition of the gas mixture (ratio O2:CF4) and process duration.
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Nedestruktivní stanovení dusíku v biologických a jiných materiálech fotonovou aktivační analýzou
Krausová, Ivana ; Mizera, Jiří ; Chvátil, David ; Krist, Pavel ; Řanda, Zdeněk ; Kučera, Jan ; Štursa, Jan
Byl vyvinut postup instrumentální gama aktivační analýzy (IGAA) pro stanovení dusíku v biologických materiálech. Stanovení je založeno na měření nespecifického anihilačního záření gama o energii 511 keV emitovaného 13N, který je produktem fotojaderné reakce 14N(γ, n)13N a je čistým pozitronovým zářičem. Metoda IGAA umožnila stanovení dusíku pod úrovní 1 hmotnostního procenta ve vybraných biolgických referenčních materiálech - NIST RM 8433 Corn Bran, 1547 Peach Leaves, 8414 Bovine Muscle, and 1577b Bovine Liver. Optimalizovaný postup byl také použit pro stanovení dusíku v práškových nanodiamantech pro lékařské účely.
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