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1
Content available remote Experimental and analytical procedures for the ToF-SIMS measurement data of membranous structures
Skalska Magdalena E., Durak-Kozica Martyna
Bio-Algorithms and Med-Systems
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2023
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Vol. 19, no. 1
64--68
EN
Time-of-flight secondary ion mass spectrometry (ToF-SIMS) is a powerful analytical technique with great application potential in biomolecular matter research. SIMS measurements performed on biological samples, due to their complex structure and the content of many small and large atomic molecular compounds, suffer very rich and complex mass spectra of particles, which characterise the content and physio-chemical properties of examined samples. The proper description and understanding of features appearing in the spectra and, consequently, the final data confirming or rejecting the hypothesis put forward in the experiment, largely depend on the experimenter’s correct understanding of the technique itself and its limitations, knowledge of the tested material and its appropriate preparation. These issues mean that obtaining the right answer to the questions posed in the research hypothesis requires not only the correct conduct of experiments but also the appropriate processing of post-experimental data. This study aims to demonstrate the impact of various analytical and experimental procedures applied to reach proper conclusions from TOF-SIM measurements. These are different types of data normalization, the selection of a so-called region of interest (ROI), the selection of representative secondary ions and specific quantification methods, including a combination of experimental parameters. All these aspects were checked and discussed based on the results of the analysis of pancreatic β cells placed in a PBS solution on silicon wafers.
2
Content available remote Nowe podejście do badania śladów w kryminalistyce
Szynkowska M. I., Osingłowska K., Pawlaczyk A., Palińska K., Marcinek M., Rogowski J., Czubak A., Parczewski A.
Przemysł Chemiczny
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2013
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T. 92, nr 6
1125--1133
3
Content available remote Charakterystyka materiału włóknistego z zastosowaniem metod XRF, XPS, SEM oraz ToF-SIMS
Kubacki J., Mańka M., Balin K., Miros A.
Materiały Ceramiczne
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2013
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T. 65, nr 4
424--428
PL
W pracy przedstawiono wyniki badań przemysłowych materiałów termoizolacyjnych z wykorzystaniem technik spektroskopowych i mikroskopowych. Przeprowadzone badania miały na celu scharakteryzowanie struktury i składu chemicznego materiału włóknistego używanego do produkcji wełny mineralnej. Analiza składu chemicznego wykazała obecność azotu, krzemu, glinu, żelaza, sodu, magnezu i wapnia na poziomie kilku procent atomowych, oraz tlenu i węgla na poziomie kilkudziesięciu procent atomowych. Wyniki badań uzyskane metodami XRF oraz XPS wykazały odwrócony stosunek koncentracji atomowej tlenu i węgla. Określona została średnica włókien. Otrzymane z widm masowych mapy chemiczne wykazały homogeniczny rozkład pierwiastków dla pojedynczych włókien. Otrzymane wyniki stanowią bazę do zaplanowania eksperymentów wiążących skład chemiczny surowców, służących do produkcji wełny mineralnej, z właściwościami cieplnymi wyrobów finalnych.
EN
This paper presents the results of industrial investigations of thermal insulation materials by using spectroscopic and microscopic techniques. The goal of this study was to characterize a structure and chemical composition of fibrous material used in production of mineral wool. Analysis of the chemical composition showed the presence of nitrogen, silicon, aluminium, iron, sodium, magnesium and calcium at the level of a few atomic percent, and several atomic percent of carbon and oxygen. The results obtained by XRF and XPS methods showed an inverted value of atomic concentration for oxygen and carbon. The mean diameter of a single fibre was determined. The homogeneous distribution of chemical elements within an individual fibre was determined from a chemical map obtained by SIMS. The obtained results form the basis for planning experiments aimed at finding a relationship between chemical composition of the materials used for production of mineral wool and the thermal properties of final products.
4
Content available ToF-SIMS studies of the surface of Pd/ZrO2-TiO2 catalyst used in the hydrodechlorination process
Grams J., Góralski J., KLeczewska J., Szczepaniak B., Paryjczak T.
Polish Journal of Chemical Technology
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2007
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Vol. 9, nr 3
81-85
EN
Time-of-flight secondary ion mass spectrometry (ToF-SIMS) was used in order to obtain the information about the surface composition of Pd/ZrO2-TiO2 catalyst and to estimate the changes in the concentration of particular components on its surface during the hydrodechlorination of CCl4. The results demonstrated that the hydrodechlorination process led to the increase in the concentration of chlorine and the drop in the amount of surface accessible palladium, while the quantity of Pd-Cl bounds did not change considerably. It suggested that the presence of ZrO2 protected the surface of the studied catalyst against the formation of PdCI2.
5
Content available Surface characterization of different particles arising as a result of coal combustion process in selected power plants from Central Poland using ToF-SIMS
Grams J., Bawolak K.
Polish Journal of Chemical Technology
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2007
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Vol. 9, nr 4
77-80
EN
The aim of this work was the ToF-SIMS investigations of different particles arising as a result of a coal combustion process in selected power plants from Central Poland. The chemical composition and distribution of particular compounds on the studied surfaces were determined. Moreover, the ratio of the quantity of aromatic and aliphatic hydrocarbons adsorbed on the surface of the particles was estimated. A qualitative analysis of the studied samples demonstrated the presence of a big number of various compounds, including heavy metals such as Pb, Cd and As on the investigated surfaces. In the prevailing number sample components were distributed non-homogenously on the surface and the larger areas richer in a certain type of ions were observed.
6
Content available Application of the TOF-SIMS and SEM-EDS methods to assess the influence of dusting from a phosphate waste deposal place based on hair analysis
Szynkowska M.I., Leśniewska E., Pawlaczyk A., Rogowski J., Paryjczak T.
Polish Journal of Chemical Technology
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2007
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Vol. 9, nr 4
85-90
EN
In this work, scanning electron microscopy with energy dispersive X-ray spectrometry (SEM-EDS) and the time-of-flight secondary ion mass spectrometry (TOF-SIMS) were used to study the particles present on the hair surface of the inhabitants of Wislinka (people environmentally exposed due to the closeness of a dump) in order to obtain the information about the possible influence of dusting from a phosphate waste deposal place. Additionally, the morphology and the composition of fresh phosphogypsum were analyzed. Waste phosphogypsum is formed in the process of a wet phosphoric acid production and there is still a problem with its storage. A thorough understanding of the composition and chemistry of phosphogypsum seems to be necessary to evaluate its environmental impact comprehensively. The results obtained from these two techniques turned out to be complementary and revealed the information expected.
7
Content available remote Zastosowanie spektroskopii TOF-SIMS w charakterystyce katalizatorów Pd/SiO2 otrzymanych metodą zol-żel
Karski S., Ludomirska I., Proga H., Szynkowska M.I., Witońska I., Kłonkowski A.M., Kledzik K.
Przemysł Chemiczny
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2006
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T. 85, nr 1
33-37
PL
Zbadano wpływ warunków preparatyki katalizatorów Pd/SiO2 otrzymanych metodą zol-żel na ich aktywność i selektywność w procesie redukcji aldehydu krotonowego. Do analizy powierzchni katalizatora użyto spektrometru TOF– SIMS, co umożliwiło wizualizację powierzchni, określenie składu chemicznego oraz segregację warstw powierzchniowych katalizatora w zależności od temperatury kalcynacji i redukcji, i w konsekwencji dobranie optymalnych warunków preparatyki.
EN
Catalyst activity and selectivity were tested in the redn. (100°C/2 hrs.) of crotonaldehyde satd. vapors in 0.03 l. H2/ min in relation to the 5%Pd/SiO2 prepn. history, esp. to calcination at 300, 500, or 700°C in Ar and at 300 or 500°C in H2 just before the reaction. The 500 and 300°C, resp., resulted in Pd distributed uniformly on the SiO2 surface, a factor crit. for catalyst’s high activity. TOF-SIMS found CH3+, CH3O+, C2H5, and SiCH3+ on the catalyst surface, but calcination at 500 or 700°C removed most of the org. fragments. The H2-treatment at 500–700°C, resulted in Pd clusters nonuniformly distributed (TOF–SIMS) on the surface and in a less active catalyst.
8
Content available remote Surface characterization of palladium catalysts using time-of-flight secondary ion mass spectrometry (ToF-SIMS)
Grams J., Góralski J., Szczepaniak B., Paryjczak T.
Polish Journal of Chemical Technology
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2006
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Vol. 8, nr 2
106-108
EN
This paper presents potentialities of time-of-flight secondary ion mass spectrometry in surface characterization of palladium catalysts destined for hydrodechlorination reaction. The secondary ion mass spectra collected from the surface of the analyzed catalysts allowed to obtain useful information regarding surface composition, presence of contaminants and interactions between particular surface components. Moreover, the amount of Cl containing species formed on the catalyst surface during hydrodechlorination reaction was also estimated.
9
Analiza składu chemicznego obszaru przejściowego w układzie DLC/Si
Staryga E., Rogowski J., Knapik M., Jarzyńska D., Cłapa M.
Elektronika : konstrukcje, technologie, zastosowania
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2006
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Vol. 47, nr 11
12-14
PL
Warstwy diamentopodobnego węgla są atrakcyjnym materiałem ze względu na dużą twardość, odporność chemiczną oraz właściwości elektryczne. Właściwości fizykochemiczne warstw DLC są ściśle związane z warunkami i parametrami procesu osadzania, dlatego też istotne jest zbadanie składu chemicznego warstw oraz ich struktury w zależności od parametrów wytwarzania. Badania składu chemicznego warstw wykonano przy użyciu spektrometrii mas jonów wtórnych TOF-SIMS. Warstwy DLC osadzono na gładkich podłożach krzemowych przy użyciu techniki RF PCVD (13,56 MHz). Warstwy nakładane były przy różnych wartościach ujemnego potencjału autopolaryzacji z zakresu od -60 V do -420 V. Zarejestrowano widma masowe i profile głębokościowe dla powierzchni, objętości i obszaru granicznego układu DLC/Si. W składzie chemicznym warstwy DLC, oprócz węgla, zarejestrowano wodór i tlen. Uzyskane profile głębokościowe wskazują na obecność zanieczyszczeń takich jak żelazo i chrom w obszarze granicznym pomiędzy podłożem a warstwą DLC.
EN
Diamond-like carbon (DLC) films attract considerable interest due to their mechanical hardness, chemical inertness, optical transparency and electrical properties. Those properties are highly influenced by the deposition parameters and in turn should be correlated with chemical composition and structure of the DLC films. In this study the Time-of-Flight Secondary Ion Mass Spectrometry (TOF-SIMS) was used to analyze chemical composition of DLC films deposited at various preparation parameters. The DLC films were deposited on flat Si substrates using Radio Frequency Plasma Chemical Vapour Deposition (RF PCVD 13.56 MHz) method. Deposition of samples was carried out using various negative self-bias voltage of electrode between -60 V and -420 V. Both surface and bulk chemical composition was analyzed for all samples by recorded surface mass spectra and depth profiles respectively.
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