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PL
Weryfikacja prawnie dopuszczalnych zawartości formaldehydu w materiałach tekstylnych i skórzanych obecnych na światowym rynku wymaga dobrze opracowanych i zwalidowanych metod analitycznych, najlepiej ujętych w normach międzynarodowych. W tej pracy zaprezentowano metody oznaczania formaldehydu wolnego w środkach pomocniczych dla garbarstwa oraz dwóch zdefiniowanych operacyjnie form formaldehydu w próbkach artykułów włókienniczych i skórzanych. Oznaczanie formadehydu ekstrahowalnego jest kluczowe dla zapewniania bezpieczeństwa kontaktu ze skórą użytkownika, natomiast oznaczanie formaldehydu emitowalnego jest szczególnie ważne dla oceny zagrożenia rakotwórczego na drodze inhalacyjnej. Popularyzacja oraz dalsze rozpowszechnienie znormalizowanych procedur analitycznych powinno przyczynić się do likwidacji luki informacyjnej dotyczącej zawartości formaldehydu w artykułach włókienniczych i skórzanych dostępnych na krajowym rynku i tym samym poprawy poczucia bezpieczeństwa chemicznego konsumentów.
EN
Verification of legally permissible formaldehyde levels in textile and leather products available on the global market requires well-developed and validated analytical methods, preferably included in international standards. This paper presents methods for determining free formaldehyde in tanning auxiliaries and two operationally defined forms of formaldehyde in samples of textile and leather articles. The determination of extractable formaldehyde is crucial for ensuring the safety in contact with the user’s skin, while the determination of emittable formaldehyde is particularly important for assessing the carcinogenic risk by inhalation. The promotion and further dissemination of the standardised analytical procedures should help to close the information gap regarding the formaldehyde content in textile and leather articles available on the domestic market, thereby improving consumers’ sense of chemical safety.
EN
Within the framework of the EuroGO-SHIP Project, an experiment on the long-term preservation of nutrients in seawater samples was conducted in May 2023 using high-salinity, low-nutrient continental shelf waters from the Gulf of Trieste. Sample comparison included filtered and non-filtered samples, preserved by both freezing and pasteurization techniques. The results indicated that neither of these methods is individually ideal for the long-term (6- and 12-month) preservation of seawater samples, although freezing is less affected by experimental biases than pasteurization. Syringe filtration (0.22 µm pore size MCE filters) can cause the breakage of plankton cells and the release of nitrogen into the samples, whereas pasteurization can cause the remineralization of dissolved organic phosphorus and the release of phosphorus and silicate from marine particulate matter. Experimental results indicated that the best preservation method should be chosen depending on the biogeochemical characteristics of the marine system studied.
PL
Dla ochrony konsumentów przed ekspozycją na metale ciężkie obecne w wyrobach tekstylnych i skórzanych wprowadzono szereg regulacji prawnych. W prestiżowych eko-certyfikatach zostały określone progowe zawartości przynajmniej najbardziej toksycznych metali ciężkich (As, Cd, Hg i Pb). Jednakże nawet najlepiej sformułowane regulacje prawne nie mogą zapewnić pełnej ochrony użytkowników tych artykułów. Niezbędna jest kontrola analityczna, dysponująca zestawem dobrze opracowanych i zwalidowanych procedur analitycznych wykorzystujących współczesne techniki instrumentalne. Takie warunki spełniają procedury analityczne ujęte w normach, najlepiej międzynarodowych lub europejskich (ISO i EN). W tej pracy omówiono procedury analityczne opisane w normach ISO oraz EN i wdrożonych do zbioru Polskich Norm. Aby przybliżyć czytelnikom tę tematykę, omówienie norm badań poprzedzono krótką charakterystyką wykorzystywanych technik instrumentalnych. Zaprezentowane postępowania analityczne umożliwiają oznaczanie całkowitej zawartości metali ciężkich oraz oznaczanie ich frakcji biodostępnej.
EN
To protect consumers from exposure to heavy metals present in textile and leather products, many legal regulations have been introduced. Prestigious eco-certificates specify the threshold levels for at least the most toxic heavy metals (As, Cd, Hg and Pb). However, even the best-formulated legal regulations cannot provide full protection for users of these articles. Analytical control with a set of well-developed and validated analytical procedures using modern instrumental techniques is essential. Such conditions are met by standardized analytical procedures preferably published in ISO and EN standards. This paper discusses analytical procedures described in ISO and EN standards and implemented in the set of Polish Standards. To better familiarize readers with this topic, the discussion was preceded by a brief description of the instrumental techniques used. The presented analytical procedures make it possible to determine the total content of heavy metals and their bioaccessible fraction.
EN
A rapid and simple method for the determination of stearic acid and 12-hydroxystearic acid in PEG-60 hydrogenated castor oil by high performance liquid chromatography with evaporative light scattering detection was established. The oil sample was first pretreated by alkaline hydrolysis. The analysis was performed on a Zhongpu Develop XD-C18 column (250mm 3 4.6 mm, 5 μm) with gradient elution of methanol and 1% acetic acid aqueous solution at a flow rate of 1.2 mL$min1 and a column temperature of 40 8C. The drift tube temperature of the evaporative light scattering detection system was set at 40 8C, and the pressure of carrier gas (N2) was 337 kPa. The regression equation revealed a good linear relation (r 5 0.9993–0.9995) during the test ranges (119.1–1190.7 μg$mL1 for 12-hydroxystearic acid, 10.7–107.4 μg$mL1 for stearic acid). The detection limits of 12-hydroxystearic acid and stearic acid were 1.1 and 2.5 μg$mL1, the limits of quantitation were 3.2 and 7.4 μg$mL1, respectively. And the mean recoveries were 101.5 and 101.0%, the corresponding relative standard deviations (RSDs) were 2.1 and 2.8%, respectively. The RSDs corresponding to repeatability (n 5 6) were both less than 1.7% in terms of precision. As to the stability, the test results remained stable after 8 h at room temperature (RSDs were both less than 2.6%). The developed method showed high sensitivity, recovery, repeatability and stability, which indicated that the method could be applied as a quality evaluation method for the determination of stearic acid and 12-hydroxyoctadecanoic acid in PEG-60 hydrogenated castor oil.
EN
The article presents the results of a theoretical study, the purpose of which was to analyze the basic principles of development of volitional qualities of student youth as a holistic systemic individual psychological characteristics in the process of physical culture and sports. Scientific novelty lies in the theoretical substantiation of volitional qualities of students in the process of physical culture and sports, it is in the process of physical education clearly defines the goals and content of activities, tools and methods that affect the development of determination, perseverance, endurance, determination, courage, ie. form a habit of showing the willful efforts of young people. The concept of „will” from the point of view of philosophers, psychologists and teachers is described. The modern definition of will is consistent with the fact that it is a conscious self-regulation of human activities, which provides overcoming obstacles and difficulties on the way to his goal. It is noted that in the process of physical education a necessary condition for the formation of the child’s will is to master the techniques, increase the level of physical fitness. At the same time, psychological and pedagogical methods of stimulation should be taken into account: praise, awards and other techniques that increase students’ interest in classes and contribute to a significant increase in selfconfidence. The volitional efforts in the process of physical culture and sports activities are analyzed and five of their types are distinguished: volitional efforts at muscular tensions; volitional efforts under stress; volitional efforts when performing actions to overcome fatigue; strong-willed efforts aimed at adhering to the regime; volitional efforts are aimed at overcoming feelings of fear.
PL
W artykule przedstawiono wyniki teoretycznego badania, którego celem była analiza głównych zasad rozwoju siły woli uczniów, jako całościowych, systemowych cech indywidualno-psychologicznych, w procesie wychowania fizycznego i sportu. Nowatorstwo naukowe polega na badaniu teoretycznego ugruntowania siły woli uczniów w procesie wychowania fizycznego i sportu. To właśnie w procesie wychowania fizycznego, cele i treści działań, środki i metody, wpływają na realizację celów kształcenia wytrwałości, wytrzymałości. Determinacja, odwaga są jasno określone, tj. tworzą nawyk okazywania młodym ludziom silnej woli. Pojęcie „woli” jest scharakteryzowane z punktu widzenia filozofów, psychologów i nauczycieli. Współczesna definicja woli jest zgodna z faktem, że jest to świadoma samoregulacja przez osobę swoich działań, zapewniająca pokonywanie przeszkód i trudności na drodze do celu. Zwraca się uwagę, że w procesie wychowania fizycznego warunkiem koniecznym kształtowania się woli dziecka jest opanowanie różnych technik, służących podnoszeniu poziomu sprawności fizycznej. Jednocześnie należy wziąć pod uwagę psychologiczne i pedagogiczne metody stymulacji: pochwały, nagrody i inne metody, które zwiększają zainteresowanie uczniów zajęciami, przyczyniając się do znacznego wzrostu pewności siebie. Przeanalizowano wysiłki wolicjonalne w procesie kultury fizycznej i aktywności sportowej, wyróżniając pięć ich typów: wysiłek wolicjonalny podczas napięcia mięśniowego; wolicjonalne wysiłki podczas zwracania uwagi; wolicjonalne wysiłki podczas wykonywania działań, mających na celu przezwyciężenie zmęczenia; dobrowolne wysiłki, ktore mają na celu utrzymanie reżimu; wysiłki wolicjonalne służące przezwyciężeniu uczucia strachu.
6
Content available remote Woltamperometryczne oznaczanie tymolu w preparatach farmaceutycznych
PL
Opracowano prostą, szybką i czułą metodę woltamperometrycznego oznaczania tymolu w farmaceutykach. Podstawą badań jest proces jego utleniania na mikroelektrodzie platynowej w lodowatym kwasie octowym zawierającym acetonitryl (20% obj.) oraz 0,1 mol/L chloranu(VII) sodu jako elektrolit podstawowy. Uzyskano liniową odpowiedź sygnału woltamperometrycznego (DPV) w szerokim zakresie stężeń 0,5-1105 mg/L, przy niskiej wartości granicy wykrywalności wynoszącej 0,05 mg/L. Analizę ilościową przeprowadzono metodą wielokrotnego dodatku wzorca.
EN
Content of thymol in pharmaceutical preparations was detd. by differential pulse voltammetry at a Pt microelectrode (25 μm diam.) in a mixt. of glacial AcOH and MeCN (8:2 by vol.) with 0.1 M NaClO₄. A good accuracy and precision of the DPV method was achieved and its usefulness in routine anal. was confirmed.
EN
A rapid and simple UPLC-MS/MS method was developed to determine toddalolactone in mouse blood and applied to measure the pharmacokinetics of toddalolactone in mice. Blood samples were first preprocessed by ethyl acetate liquid-liquid extraction. Oxypeucedanin hydrate (internal standard, IS) and toddalolactone were gradient eluted from a UPLC BEH C18 column using a mobile phase consisting of acetonitrile and water (0.1% formic acid). Using electrospray ionization (ESI) as the ionization source, multiple reaction monitoring was used to detect the precursor and product ions of m/z 309.2 and 205.2, respectively, for toddalolactone and of m/z 305.1 and 203.0 for IS, respectively, for quantitative detection. A calibration curve was run over the concentration range of 5–4,000 ng/mL (r > 0.995). The matrix effects ranged from 93.5 to 98.4%, and the recovery was higher than 77.3%. The precision was less than 13%, and the accuracy ranged from 90.9 to 108.4%. The developed UPLC-MS/MS method was successfully used for measuring the pharmacokinetics of toddalolactone in mice after oral (20 mg/kg) and intravenous administration (5 mg/kg), and the absolute bioavailability of toddalolactone was 22.4%.
EN
Narciclasine is a 7-hydroxy derivative of lycorisidine. It was the first alkaloid isolated from the stem of narcissus (Amaryllidaceae) in 1967. Six mice were given narciclasine (5 mg/kg) by intravenous administration. A UPLC-MS/MS method was developed to determine narciclasine in mouse blood. Tectorigenin (internal standard, IS) and narciclasine were gradient eluted by mobile phase of methanol and 0.1% formic acid in a BEH C18 column. The multiple reaction monitoring (MRM) of m/z 308.1→248.1 for narciclasine and m/z 301.1→286.0 for IS with an electrospray ionization (ESI) source was used for quantitative determination. The calibration curve ranged from 1 to 6,000 ng/mL. The accuracy was from 92.5 to 107.3%, and the matrix effect was between 103.6 and 107.4%. The developed UPLC-MS/MS method was successfully applicated to a pharmacokinetic study of narciclasine in mice after intravenous administration (5 mg/kg).
EN
Eugenitin is a non-volatile chromone derivative which is always found in dried flower buds of Syzygium aromaticum L. (Merr.) & L.M. Perry. Until now, there were no reports about the pharmacokinetics of eugenitin in biological fluids. A UPLC-MS/MS method developed to determine eugenitin in mouse blood. The blood samples were prepared by protein precipitation with acetonitrile. Chrysin (internal standard, IS) and eugenitin were gradient eluted by mobile phase of acetonitrile and water (0.1% formic acid) in a BEH C18 column. The multiple reaction monitoring (MRM) of m/z 221.1→206.0 for eugenitin and m/z 255.1→152.9 for IS with an electrospray ionization (ESI) source was used for quantitative detection. The calibration curve ranged from 0.5 to 500 ng/mL (r > 0.995). The accuracy ranged from 98 to 113%, the precision was less than 12%, and the matrix effect was between 86 and 94%, the recovery was better than 81%. The developed method was successfully used for pharmacokinetics of eugenitin in mice after intravenous (5 mg/kg) and oral (20 mg/kg) administration, and the absolute availability of eugenitin was 12%.
10
EN
The variety of the chemical forms of phosphorus compounds occurring in plant tissues, accompanied by the complexity of the chemical composition of plants as the analytical matrices, are the reasons why there is no one, the best answer, how those individual substances may be determined qualitatively and quantitatively. Interestingly, if the subject of determination is the total phosphorus content, the spectrum of effective methods and techniques seems to be impressive. However, in case of spectrophotometric measurements and classical variants of absorption (FAAS) or emission (ICP-AES/ ICP-OES) spectrometry techniques, it is necessary at first to isolate various phosphorus forms from the matrix, and then to mineralize them prior determination. The development of combined methods e.g. ETV-ICP- AES or HR-ETAAS, does allow the isolation of the phosphorus analyte and its detection in a kind of “one step” analytical procedure, directly in plant tissues. Similar benefits, while maintaining the sensitivity of determinations, are brought by the use of XRF, SIMS or nanoSIMS - more expensive techniques of imaging the presence of phosphorus in biological matrices. In turn, the application of nuclear magnetic resonance spectroscopy, especially the 31P NMR technique is thought to be the most universal approach. Using this technique and being aware of higher limit of detection, it is possible to determine various plant phosphorus compounds qualitatively and quantitatively, at the same time.
PL
W trzeciej części cyklu artykułów dotyczących zginanych ścian murowanych, obciążonych prostopadle do ich powierzchni [5, 6] omówiono sposoby analizy tego rodzaju konstrukcji, w tym założenia dotyczące warunków brzegowych modeli ścian jednowarstwowych i szczelinowych. Przedstawiony został również sposób określania wartości momentów zginających przyjęty w normie PN-EN 1996-1-1.
EN
In the third part of the series of articles on bent masonry walls, loaded perpendicular to their surfaces [5, 6], methods of analysis of this type of structure are discussed, including assumptions regarding the boundary conditions of single-leaf and cavity wall models. The method of determining the values of bending moments adopted in the PN-EN 1996-1-1 standard is also presented.
PL
Przedstawiono algorytm oznaczania grubości warstw nawierzchni drogowych metodą georadarową, zapewniający uzyskanie możliwie największej dokładności przy minimalizacji liczby odwiertów koniecznych do wykonania. Zastosowanie algorytmu umożliwia zredukowanie błędów oznaczeń grubości bez wykonywania odwiertów z ±30 do ±10% rzeczywistej grubości, tj. do mieszczących się w zakresie tolerancji pomiarowej metody georadarowej.
EN
The article presents an algorithm for determining the thickness of road pavement layers using GPR method which allows to obtain the highest possible accuracy while minimizing the number of drillings required. Presented algorithm allows to reduce errors in road pavement layers thickness determination using the GPR method without drilling from ± 30% to ± 10% of the actual thickness, i.e. to the GPR method tolerance range.
EN
The subject of the wind tunnel tests is a steel chimney 85 m high of cylindrical - type structure with a grid-type curtain structure situated at its upper part. The model of the upper part of the chimney made in the scale of 1:19 was equipped with 3 levels of wind pressure measurement points. Each level contained 24 points connected with pressure scanners. On the base of the pressure measurements, both mean and instantaneous aerodynamic drag and side force coefficients were determined. Next wind gust factors for these two wind action components were determined. Moreover, for each pressure signal Fast Fourier Transform was done. Mean wind action components were also determined using stain gauge aerodynamic balance. Obtained results make possible to conclude that the solution applied in the upper part of the designed chimney is correct from building aerodynamics point of view. Some minor vortex excitations were observed during model tests of the upper part of the chimney. The basic dynamic excitation of this part of the chimney is atmospheric turbulence.
PL
Przedmiotem badań w tunelu aerodynamicznym był stalowy komin wysokości 85 m, o konstrukcji cylindrycznej z umieszczoną w górnej części konstrukcją siatki osłonowej. Model górnej części komina wykonany w skali 1:19 został wyposażony w 3 poziomy punktów pomiarowych ciśnienia wiatru. Każdy poziom zawierał 24 punkty połączone ze skanerami ciśnienia. Na podstawie pomiarów ciśnienia wyznaczono średni i chwilowy współczynnik oporu aerodynamicznego oraz współczynniki siły bocznej. Następnie określono współczynniki porywów wiatru dla tych dwóch składowych działania wiatru. Ponadto dla każdego sygnału ciśnienia wykonano szybką transformację Fouriera. Średnie składowe siły działania wiatru zostały również określone przy użyciu wagi aerodynamicznej. Uzyskane wyniki pozwalają stwierdzić, że rozwiązanie zastosowane w górnej części projektowanego komina jest poprawne z punktu widzenia aerodynamiki budowli. Podczas badań modelowych górnej części komina praktycznie nie zaobserwowano wzbudzeń wirowych. Podstawowym wzbudzeniem dynamicznym tej części komina są turbulencje atmosferyczne.
14
Content available remote Pharmacokinetics and bioavailability of liensinine in mouse blood by UPLC-MS/MS
EN
Liensinine is a bisbenzyltetrahydroisoquinoline alkaloid extracted from lotus (Nelumbo nucifera GAERTNER., Nelumbonaceae), especially in its embryo loti “Lien Tze Hsin” (green embryo of mature seed). A rapid and simple UPLC-MS/MS method was developed to determine liensinine in mouse blood and its application to a pharmacokinetic study. The blood samples were preprocessed by protein precipitation using acetonitrile. Midazolam (internal standard, IS) and liensinine were gradient eluted by mobile phase of methanol and water (0.1% formic acid) in a Waters UPLC BEH C18 column. The multiple reaction monitoring of m/z 611.3 → 206.1 for liensinine and m/z 326.2 → 291.1 for IS with an electrospray ionization (ESI) source was used for quantitative detection. The calibration curve ranged from 0.5 to 400 ng/mL (r > 0.995). The accuracy ranged from 92.2 to 108.2%, the precision of intra-day and inter-day was less than 14%, and the matrix effect was between 100.0% and 109.6%, the recovery was better than 71.0%. The developed UPLC-MS/MS method was successfully used for a pharmacokinetic study of liensinine in mice after oral (5 mg/kg) and intravenous administration (1 mg/kg), and the absolute availability of liensinine was 1.8%.
EN
This study focused on developing an effective and environmentally friendly method to measure ligustrazine in rat serum by using polymer monolith micro-extraction (PMME) technique. A poly (methacrylic acid-ethylene glycol dimethacrylate) material was used to extract ligustrazine through hydrophobic and ion-exchange interaction. Qualitative and quantitative analysis was performed by a liquid chromatography and tandem mass spectrometry. After optimization of several PMME conditions, the developed method exhibited excellent extraction performance to the ligustrazine. Good linearity was acquired ranging from 10 to 2,000 ng mL−1, and the limit of detection of the proposed method was 0.14 ng mL−1. The recoveries measured by spiking three different concentrations in rat serum ranged from 82.6 to 95.3%, and excellent precision was found with relative standard deviations (RSDs) less than 8.3% for intra-day and 9.7% for inter-day, respectively. At last, the applicability of the method was further confirmed through continuous monitoring of ligustrazine in rat serum after dosing of ligustrazine tablets to rats.
EN
The analyzed organosilicon derivatives of electrostatically stabilized silanates belong to a group of pentacoordinated compounds. These derivatives are:1-(N-morpholiniomethyl)spirobi(1-sila-2,5-dioxacyclopentan-3-on)at,1-(N-morpholiniomethyl)spirobi(1-sila-2,5-dioxa-4-methylcyclopentan-3-on)at,1-(N-morpholiniomethyl)spirobi(1-sila-2,5-dioxa-4-(i-propyl)cyclopentan-3-on)at. In the course of the work, the extraction process and optimization of conditions for separation and determination of a mixture of electrostatically stabilized silanates were carried out using capillary isotachophoresis. Proper leading electrolytes were elaborated developed and the terminating electrolyte:4,4’-bis[(1-morpholiniomethyl)spirobi(1-sila-2,5-dioxacyclopentan-3-on)at] was proposed. The extraction process involved the use of three stationary phases: octadecyl, octyl and phenylpropyl. The highest recovery values, approx. 94%, were obtained on the phenylpropyl column. The optimum time of analysis by the isotachophoretic technique did not exceed 12 min. The developed method of separation and determination of electrostatically stabilized silanates expands the possibility of research on biological activity of this group of compounds in aqueous solutions and surface water vegetation.
PL
Zastosowanie technologii MALDI i technik elektromigracyjnych w analizie mikrobiologicznej może stać się kamieniem milowym w diagnostyce i analizie zakażeń.
EN
Due to the development of alternative propulsion systems, there is a need for LNG tanker turbine propulsion plants to regain their competitiveness. Previous research revealed effective methods to increase the thermal efficiency of the steam cycle based on quality assessment, and it was proposed that the latent heat of the main turbine exhaust steam could be recovered. Research was carried out for the steam cycle using regenerative heat exchangers fed by steam jet injectors. In this paper, an algorithm to determine the operating parameters of steam jet injectors, and the calculation results for different drive steam parameters are presented. The obtained results will be used as input parameters for further heat balance calculations of the proposed regenerative steam cycles.
EN
The article presents a simulation method for determining the minimum safe pull of tugs assisting in port manoeuvres. The method can be used to determine the relationship between the minimum safe pull, understood as the tension on the line, of the assisting tugs and the overall length, cargo capacity or net capacity of ships manoeuvring in a given port under allowable hydrometeorological conditions. The method was verified through simulated tests of gas tankers’ entry, turning and berthing at the LNG terminal of Świnoujście.
EN
A new method for determination of positive realizations of given transfer matrices of linear continuous-time linear systems is proposed. Necessary and sufficient conditions for the existence of positive realizations of transfer matrices are presented. A procedure for computation of the positive realizations is proposed and illustrated by an example.
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