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EN
The research paper presents the conducted tests for determination of fuel content in a synthetic lubricating oil used in aviation engines. The authors applied infrared spectroscopy for quantitative determination of Jet A-1 aviation fuel content in ester-based synthetic oil used in the engines of Polish Armed Forces aircraft. The obtained results were compared with the results of tests conducted using the technique that employs acoustic surface wave measurement.
PL
W artykule przedstawiono przeprowadzone badania zawartości paliwa w syntetycznym oleju smarowym eksploatowanym w silnikach lotniczych. Zastosowano technikę spektroskopii w podczerwieni do ilościowego oznaczenia zawartości paliwa lotniczego typu Jet A-1 w syntetycznym oleju na bazie estrów, eksploatowanym w silnikach statków powietrznych Sił Zbrojnych Rzeczpospolitej Polskiej. Porównano otrzymane wyniki z wynikami badań otrzymanymi z zastosowaniem techniki wykorzystującej pomiar akustycznych fal powierzchniowych.
EN
In this research, the solid-state method was utilized to synthesize LaFeO3 powders, with La2O3 and Fe2O3 being employed as precursor materials. The prepared samples were calcined at different temperatures 800°C, 900°C, 1000°C, 1100°C, 1200°C and 1300°C for 4h to study phase stability. The thermal effect on structural and morphological properties was reported. The X-ray diffraction results confirmed the pure phase in its orthorhombic configuration at 1200°C and 1300°C, which was confirmed by Rietveld’s analysis. Scanning electron microscopy coupled with Energy-dispersive X-ray spectroscopy was employed to analyze the surface morphology and compositional characteristics. In addition, the samples were analyzed by Fourier Transform Infrared Spectroscopy. The thermal behavior of the product was investigated through the utilization of thermogravimetric analysis.
EN
We describe construction and investigation results of optical trace gas sensor working in the 3.334-3.337 μm spectral range. Laser spectroscopy was performed with a multipass cell. A setup was elaborated for detection of ethane at the 3.3368035 μm absorption line. Analysis of the gas spectra and the experiment have shown that, beside C2H6, the sensor is suitable for simultaneous detection of methane, formaldehyde and water vapor. Due to nonlinearity of the laser power characteristic we decided to detect the fourth harmonic of signal. Additional laser wavelength modulation was applied for optical interference suppression. In result, the precision of ethane detection of approximately 80 ppt has been achieved for the averaging time of 20 seconds. Long-term stability as well as the measurement linearity have also been positively tested. The system is suitable for detecting potential biomarkers directly in human breath.
EN
Transformers are crucial elements in the transmission and distribution of electrical energy. The importance of diagnosing these equipments are two-fold: (1) the necessity of service reliability and (2) the likelihood to avoid economic and environmental concerns. Under service conditions, the electrical and thermal stresses or chemical contaminants may degrade the insulation oil inside the transformer and cause incipient failures or reduce its service life. Partial discharges well recognized to be among the most common stresses that can lead to slow but steady degradation of insulating oil in transformers. The present work aims at understanding the influence of low energy electrical discharge on mineral oil based on two spectroscopic methods: FTIR spectroscopy and Frequency Domain Spectroscopy (FDS). An electrical fault has been created by continuous discharge of 10 kV on the surface of various oil samples according to the ASTM D6180. From the FDS results, it was found that the amount of charge carriers and moisture increased with the aging time elapsed that influences the conduction phenomena and in turn, increases the dissipation factor. These results are confirmed by the FTIR results, which show that the intensity of the peak absorbance of the C–H and C-C functional group decreased with aging. The application of these two methods may help monitoring the condition of oil. A combined FTIR and FDS measurements highlighted the correlations between modifications in electrical properties and changes in the chemical structure of the oil under electrical accelerated ageing.
PL
Wykonano syntezę 1-propylo-2-nitroguanidyny (PrNQ) wg oryginalnie zmodyfikowanej metody (podanej przez Davisa i Luce w 1927 r.), pozwalającej otrzymywać jednorazowo ok. 160 g produktu o czystości wystarczającej do dalszych badań. Strukturę cząsteczki PrNQ potwierdzono techniką magnetycznego rezonansu jądrowego (NMR). Temperatura topnienia PrNQ wyznaczona techniką skaningowej kalorymetrii różnicowej (DSC) wynosiła 99°C przy szybkości ogrzewania 1°C/min. Rozkład egzotermiczny następuje w tych warunkach w temperaturze ok. 200°C. Wyniki badania wrażliwości na bodźce mechaniczne uzyskane dla PrNQ wskazują, że jest to materiał o odporności zbliżonej do jednego z najmniej wrażliwych materiałów wybuchowych, jakim jest 1,3,5-triamino-2,4,6-trinitrobenzen (TATB). Wykazano, że czysta PrNQ może być formowana metodą prasowania na zimno oraz techniką odlewania.
EN
The synthesis of 1-propyl-2-nitroguanidine (PrNQ) was performed, according to an originally modified procedure, and ca. 160 g of PrNQ was obtained in a single run. The purity of it is sufficient for further research. The structure of PrNQ molecule has been confirmed by using nuclear magnetic resonance spectrometry (NMR). The melting (99°C) and decomposition (200°C) points were determined by using differential scanning calorimetry (DSC) at a heating rate of 1°C/min. Mechanical sensitivity tests showed that PrNQ is an nergetic material with impact sensitivity similar to the sensitivity of one of the least-sensitive explosives, i.e., 1,3,5-triamino-2,4,6-trinitrobenzene (TATB). It has been shown that PrNQ can be elaborated by cold pressing or melt-cast technique.
EN
Twin-screw extrusion is a crucial method for the direct inserting of carbon micro- and nanomaterials into a polymer matrix using a dry procedure. The study aimed to determine the influence of the parameters of the twin-screw extruder plasticizing system on the dispersion homogeneity and distribution of graphite filler in the polylactide polymer matrix and overall quality of the composite. As a filler, a graphite micropowder with a 5 μm lateral size of platelets was used at concentration of 1 wt.%. Three configurations of screws with different mixing intensity and various types segments were considered in the extrusion experiments. Morphology and chemical structure of the obtained composites were examined using scanning electron microscopy (SEM), Fourier transform infrared spectroscopy – attenuated total reflectance (FTIR-ATR) and Raman spectroscopy. Differential scanning calorimetry (DSC) and melting flow rate measurements (MFR) were used to asses thermal and rheological properties of the composites. Samples of the polylactide/graphite composites were also subjected to mechanical tests. The results show that the selection of the mechanical parameters of twin-screw extruder plasticizing system plays a key role in the preparation of the homogeneous PLA/graphite composites. Incorrect selection of the screw geometry results in poor mixing quality and a significant deterioration of the mechanical and thermal properties of the composites. Optimised mixing and extrusion parameters can be the starting point for the design of efficient twin-screw extruder plasticizing system for fabrication of PLA composites with carbon nanotube and graphene fillers.
PL
W artykule przedstawiono wyniki badań polskich kwantowych laserów kaskadowych w układach laserowej spektroskopii absorpcyjnej do wykrywania amoniaku. Parametry laserów zdeterminowały zastosowanie dwóch konfiguracji układów eksperymentalnych: z wnęką optyczną oraz z przestrajaniem wewnątrz-impulsowym. Uzyskane rezultaty potwierdziły, że emitowane przez nie promieniowanie o długości fali ok. 9,12 µm umożliwia wykrywanie amoniaku i uzyskanie granicy wykrywalności 50 ppb.
EN
The article presents the results of research on the use of Polish quantum cascade lasers for the detection of ammonia by laser absorption spectroscopy. The parameters of these lasers determined the use of two configurations of experimental systems: with an optical cavity and with intra-pulse tuning. The obtained results confirmed that the radiation emitted by them, at a wavelength of approx. 9.12 µm, enables the detection of ammonia and a detection limit of 50 ppb.
EN
Reactivity of (3-aminopropyl)trimethoxysilane with cellulose. The paper presents the results of tests for the reactivity of (3-aminopropyl)trimethoxysilane (APTMOS) with cellulose. The cellulose was treated with aqueous ethanolic solution of silane in two concentration: 5% and 20%. The reactivity of APTMOS with cellulose was analysed using instrumental methods: attenuated total reflectance Fourier transform infrared spectroscopy, atomic absorption spectrometry and elemental analysis. In the FTIR spectra of silane-treated cellulose, the bands of Si-O, Si-C and N-H bonds were detected. The analysis of silicon and nitrogen concentration in treated cellulose confirmed the presence of silane in cellulose structure. The presented results indicate that APTMOS forms chemical bonds with cellulose.
PL
Reaktywność 3-(aminopropylo)trimetoksysilanu z celulozą. W pracy przedstawiono wyniki badań reaktywności 3-(aminopropylo)trimetoksysilanu (APTMOS) z celulozą. Celuloza była traktowana etanolowym roztworem silanu w dwóch stężeniach, wynoszących 5 i 20%. Reaktywność APTMOS z celulozą była analizowana z wykorzystaniem metod instrumentalnych, w tym spektroskopii osłabionego całkowitego odbicia w podczerwieni z transformacją Fouriera, atomowej spektroskopii absorpcyjnej oraz analizy elementarnej. W widmach FTIR celulozy poddanej działaniu silanu obserwowano pasma pochodzące od wiązań Si-O, Si-C i N-H. Analiza stężenia krzemu i azotu w modyfikowanej celulozie potwierdziła obecność silanu w strukturze celulozy. Przedstawione wyniki wskazują, że APTMOS tworzy wiązania chemiczne z celulozą.
EN
Organosilanes in wood protection – chemical analysis of wood and cellulose treated with MTMOS. The paper presents the results of methyltrimethoxysilane (MTMOS) reactivity with Scots pine wood and cellulose. The lignocellulosic material after treatment with ethanolic solution of MTMOS was analysed using instrumental methods – atomic absorption spectrometry (AAS) and attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR). The analysis of silicon concentration in treated material indicated the presence of silane in structure of wood and cellulose. The bands characteristic of vibrations of the silicon-carbon and silicon-oxygen originating from MTMOS molecule were observed in the spectra of modified materials, which confirmed the reactivity of silane with wood and cellulose. Moreover, the chemical analysis indicated that MTMOS exhibited higher reactivity to cellulose than to pine wood.
PL
Organosilany w ochronie drewna – analizy chemiczne drewna i celulozy traktowanej MTMOS. W pracy przedstawiono wyniki badań reaktywności metylotrimetoksysilanu (MTMOS) z drewnem sosny zwyczajnej oraz celulozą. Materiał lignocelulozowy po działaniu etanolowego roztworu MTMOS był analizowany z wykorzystaniem metod instrumentalnych – AAS oraz ATR-FTIR. Analiza stężenia krzemu w impregnowanym materiale wskazuje na obecność silanu w strukturze drewna i celulozy. Charakterystyczne pasma dla drgań krzem-węgiel oraz krzem-tlen, pochodzące z cząsteczki MTMOS obserwowane w widmach modyfikowanych materiałów potwierdzają reaktywność silanu z drewnem oraz celulozą. Ponadto, analiza chemiczna wykazała, że MTMOS wykazywał wyższą reaktywność wobec celulozy niż drewna sosny.
EN
A reaction of [3-(2-aminoethylamino)propyl]trimethoxysilane with wood and cellulose – chemical analyses. The paper presents tests results for [3-(2-aminoethylamino)propyl]trimethoxysilane (AATMOS) reactivity with cellulose and Scots pine wood. The tested material was treated with ethanolic solution of aminosilane and analyzed using instrumental methods, including elemental analysis, atomic absorption spectrometry and infrared spectroscopy. The results of the chemical analysis indicated that [3-(2-aminoethylamino)propyl]trimethoxysilane exhibited reactivity with both cellulose and pine wood. In addition, AATMOS-treated cellulose showed a higher content of silicon and nitrogen and more significant changes in FTIR spectra than the treated wood, suggesting that AATMOS showed a higher reactivity to cellulose than to wood.
PL
Reakcja [3-(2-aminoetyloamino)propylo]trimetoksysilanu z drewnem i celulozą – analizy chemiczne. W pracy przedstawiono wyniki reaktywności [3-(2-aminoetyloamino)-propylo]trimetoksysilanu (AATMOS) z celulozą i drewnem sosny zwyczajnej. Badany materiał traktowano etanolowym roztworem aminosilanu i analizowano z wykorzystaniem metod instrumentalnych, takich jak: analiza elementarna, atomowa spektrometria absorpcyjna i spektroskopia w podczerwieni. Uzyskane wyniki wskazują, na reaktywność [3-(2-aminoetyloamino)propylo]trimetoksysilanu zarówno z celulozą jak i drewnem sosny. Ponadto, celuloza traktowana AATMOS charakteryzowała się większą zawartością krzemu i azotu oraz intensywniejszymi zmianami w widmach FTIR w porównaniu do impregnowanego drewna, co sugeruje, że AATMOS wykazuje większą reaktywność do celulozy niż do drewna.
EN
Differential scanning calorimetry (DSC) and infrared spectroscopy (FT-IR) techniques were applied to analyze polymer type and its content in wood-plastic composites (WPC). Methods of analysis were developed on the basis of commercial and laboratory made WPC samples with different content of polypropylene (PP) and high-density polyethylene (HDPE). Polymer melting temperature was used to determine its type and melting enthalpy value was used to determine polymer content in the sample. The method was rewarding, both in qualitative and quantitative way. The absorption bands from FT-IR spectra (1508 cm-1, i.e., aromatic skeletal vibration of lignin and 1455 cm-1, i.e., CH2 bending for polypropylene) were chosen to determine polymer content. Calibration curve obtained on the basis of measurements made on laboratory prepared samples with different polymer content was elaborated. Determination of polymer type with FT-IR was unequivocal, while determination of its content may cause troubles in case of samples with lower polymer content.
PL
Techniki kalorymetrii różnicowej (DSC) oraz spektrofotometrii w podczerwieni (FT-IR) zastosowano do analizy jakościowej i ilościowej kompozytów polimerowo-drzewnych (WPC). Metodykę analiz opracowano w odniesieniu do próbek WPC, komercyjnych i przygotowanych w laboratorium. Wyznaczoną wartość temperatury topnienia polimeru wykorzystano do określenia jego typu, natomiast wartość entalpii topnienia do określenia jego zawartości w kompozycie. Opracowana metoda okazała się skuteczna, zarówno do analizy jakościowej, jak i ilościowej. Pasma absorpcyjne zarejestrowane w podczerwieni przy liczbach falowych 1508 cm-1 (drgania szkieletowe pierścieni aromatycznych lignin) i 1455 cm-1 (drgania deformacyjne grupy CH2 w polipropylenie) zastosowano do wyznaczania zawartości polimeru. Na podstawie pomiarów próbek WPC sporządzonych w laboratorium przygotowano krzywe kalibracyjne. Stwierdzono, że na podstawie widm FT-IR można jednoznacznie określić rodzaj polimeru w kompozycie oraz oznaczyć jego zawartość, jednak w wypadku niewielkiego udziału może to być problematyczne.
EN
Gem has long been chased because of its cultural and historical significance and beauty, and the identification and evaluation of its structural features have also been paid attention to. Plum blossom jade and emerald were identified and analyzed by means of the conventional detection method, infrared spectroscopy and X-ray powder diffraction analysis. The results showed that plum blossom jade with black and brown background and red, white and brown amygdaloid body spots had a diameter of 1–10 mm, a relative density of 2.69–2.75 g/cm3 and a refractive index of 1.52–1.55, and its minerals contained water molecules, quartz, low albite, anorthoclase and andesite. It was observed that emerald was green, greasy, glassy, transparent, with a relative density of 2.66–2.78 g/cm3 and 1.58 refractive index, and its minerals contained water molecules; there were two kinds of arrangement in crystal channels. The main mineral component of emerald was beryl, and its purity was high.
EN
The article presents the process of fault location in the HDR-rhr engine EGR system based on the characteristics obtained in the conditions of traction measurements using the ESI Tronic 2.0 program. The measurements were obtained using the licensed BOSCH KTS540 diagnostic tester. In the process of diagnostic inference the PWM signal coefficient has been analyzed in relation to the level of boost pressure, mass variability and air temperature in the intake system (based on MAF data) and EGR valve positioning for variable angular positions of the accelerator pedal. Analysis of the characteristics allowed for proper identification of faults previously stored in the system with OBDII error codes. Attention was paid to the issue of sediment formation in the EGR valve channels as a result of using diesel oil with the participation of biocomponents. Sludge analysis was carried out in a certified laboratory using infrared spectroscopy methods. Conclusions have been drawn for the presence of non-oxidized components of organic origin precipitated in the channels of the EGR system.
PL
W celu uzyskania danych na temat charakterystyki morfologicznej i właściwości fizykochemicznych danego przedmiotu wykonanego z tworzyw sztucznych (lub gumy) powszechnie wykorzystywane są takie techniki, jak: spektroskopia w podczerwieni, różnicowa kalorymetria skaningowa, analiza termograwimetryczna, analiza dynamicznych właściwości mechanicznych, chromatografia żelowa czy skaningowa mikroskopia elektronowa.
EN
Four infrared spectroscopic techniques - photoacoustic (PAS), diffuse reflectance (DRS), attenuated total reflectance (ATR) and transmission (TS) - were evaluated for the qualitative analysis of the biochar obtained from willow feedstock during pyrolysis. Increase in pyrolysis temperature resulted in more aromatic and carbonaceous structure of biochars. These changes could easily be detected from Fourier transform infrared (FT-IR) spectral differences. The comparison of the spectra obtained by the four FT-IR techniques allowed to conclude that there are differences in the spectra acquired using different IR technique caused by different signal acquisition. PAS and ATR were the best techniques used in order to obtain spectra with smooth and sharp peaks, in contrast to TS, where bands were less-separated. DRS turned out to be the weakest of all techniques, due to poor spectral quality and poor separation of the bands.
PL
Zagadnienie sekwestracji CO2 w betonie w procesie karbonatyzacji nabiera w ostatnim czasie coraz większego znaczenia. Wynika to z faktu, iż coraz częściej zarówno konstrukcja, jak również zastosowane materiały są analizowane pod kątem ich całkowitego śladu węglowego. W artykule przedstawiono wyniki badań procesu karbonatyzacji betonu SCC C30/37 w formie gruzu betonowego frakcji 8 – 31,5 mm w komorze karbonatyzacyjnej przez okres 56, 112 i 168 dni. Próbki zostały poddane analizie spektrofotometrycznej FTIR (Fourier Transformation Infrared Spectroscopy). Następnie próbki badane przez 168 dni poddane zostały analizie termicznej TG/DTA (Thermogravimetric/Differential Thermal Analysis) w celu określenia ilości zaabsorbowanego CO2. Otrzymane wyniki zostały odniesione do maksymalnej teoretycznej ilości zaabsorbowanego CO2 wg normy PN-EN 16757-07.
EN
Issue of CO2 sequestraion in the carbonation process has become a crucial problem. This is due the fact, that construction and applied materials are analyzed in the terems of their total carbon footprint. Resutls of research on carbonation of SCC (Self-Compacting Concrete) C30/37 in the form of concrete rubble, in fraction 8 – 31,5 mm, kept for 56, 112 and 168 days have been presented in the paper. Samples were investigated with FTIR (Fourier Transformation Infrared Spectroscopy) analysis. Next, samples kept for 168 days were analyzed with thermal analysis TG/DTA (Thermogravimetric/Differential Thermal Analysis) to determine the amount of absorbed CO2. The obtained results were referred to the formula for the maximum theoretical CO2 uptake according to PN-EN 16757-07.
PL
Opracowanie prezentuje wybrane metody spektroskopowe i ich zastosowanie do badań obiektów biologicznych, takich jak: białka, kwasy tłuszczowe i komórki. Wśród omówionych metod znajdują się: spektroskopia w podczerwieni, spektroskopia Ramana, spektroskopia magnetycznego rezonansu jądrowego, spektrometria mas oraz spektroskopia sił atomowych. Wszystkie prezentowane wyniki uzyskane zostały w laboratoriach BioNanoParku.
EN
The paper presents selected spectroscopic methods and their application for the study of biological objects, such as proteins, fatty acids and cells. The discussed methods include: infrared spectroscopy, Raman spectroscopy, nuclear magnetic resonance spectroscopy, mass spectrometry and atomic force spectroscopy. All the presented results were obtained in BioNanoPark laboratories.
EN
Shock impact-produced mineral alterations in two thin sections of the recently found Csátalja H4 ordinary chondrite meteorite are compared. Peak positions of Raman and infrared spectra of mineral clasts show peaks shifted in wavenumber relative to unshocked reference minerals, and both peak shifts and FWHM values seem to correlate to each other. In the less shocked thin section (Csátalja-1) a more monomineralic and homogeneous composition indicate shock pressures of <15 GPa, while the more shocked Csátalja-2 indicates shock pressure in the 15–17 GPa range. The highest identified infrared peak position shifts range between –48 and +28 cm–1 with peak broadening between 60–84 cm–1 in the case of the feldspars, which, together with sulphide globules, were produced by the shock itself. Feldspar spectra could be detected only by FTIR spectroscopy, but in most cases (above the S3 shock level) the mixed type of the pyroxene-feldspar spectra (both peaks in the same spectra) is in agreement with the shock-produced secondary feldspars. These grains are located around crystalline borders, and probably formed by selective melting, due to shock annealing. In reconstruction of the shock history, an early fragmentation by a lower shock effect and a later increased shock level-related vein and melt pocket formation occurred, with subsequent shock annealing; temporal reconstruction of the shock event is possible only in part. The joint usage of Raman and infrared spectroscopy provided useful insights into the shock-produced changes and their spatial inhomogeneity, while shocked feldspar could be better detected by infrared than by the Raman method.
PL
W artykule przybliżono metodę spektroskopii w podczerwieni. Omówiono zasadę metody, techniki pomiaru, sposoby przygotowania próbek do badań. Podano przykłady zastosowań tej techniki w analizie wyrobów lakierowych obejmujących identyfikację, monitorowanie różnych procesów fizykochemicznych zachodzących w powłokach oraz analizę ilościową.
EN
The article presents the method of infrared spectroscopy. The principle of the method, measurement technique, methods of sample preparation for testing are discussed. Examples of applications of this technique in the analysis of coatings including identification, monitoring of various physicochemical processes occurring in coatings and quantitative analysis are given.
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