X-RAY PHOTOELECTRON SPECTROSCOPY
Equipment: Electronic spectrometer ESCALB MkII of the English company Vacuum Generators (now part of Thermo Electron Corporation) purchased in 1986.
Method of analysis: X-ray Photoelectron Spectroscopy (XPS), also known as ESCA (Electron Spectroscopy for Chemical Analysis).
This is a surface-sensitive non-destructive method that provides quantitative information about the chemical state of all elements except hydrogen and helium. XPS provides information about the composition of the top 10 atomic layers of the surface of the analyzed sample for elements from lithium to uranium. Additionally, information about the chemical state of the analyzed elements is obtained.
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ELECTRON PARAMAGNETIC RESONANCE
Equipment:
- JEOL JES – FA100 EPR spectrometer, operating in the X-range with the capability of measurements in two temperature ranges: from 325 K to 425 K and from 125 K to 325 K.
- BRUKER ER200 D-SRC spectrometer, operating in the X and Q range; attachment for operation at temperatures in the range of 100-500 K and 3.8-300 K; ENDOR attachment at a frequency of 0.5-36 MHz.
- ADANI PS100X ‘mini’ EPR spectrometer operating in the X-range with an attachment for temperature variation in the range of 100-500 K.
Analysis method: Electron Paramagnetic Resonance spectroscopy, also known as Electron Spin Resonance.
Objects of investigation with EPR spectroscopy are stable or short-lived free radicals – natural or induced as a result of external influences (ionizing radiation, thermal treatment, etc.); transition metal ions such as Cu(II), Mn(II), Cr(III,V), V(IV), Fe(III), Co(II), etc. The method is characterized by high absolute sensitivity – it can detect up to 10^-10-10^-12 paramagnetic particles, corresponding to a concentration of 10^-11-10^-12 mol/l. Since it only detects paramagnetic objects, EPR spectroscopy is highly selective and works without prior sample preparation. The method is fast, non-destructive, and uses small sample volumes.
INFRARED SPECTROSCOPY
Equipment: Nicolet 6700 FTIR (Fourier Transform Infrared) spectrometer from Thermo Electron Corporation, purchased in 2009. Attachments for recording transmission, diffuse reflectance, and spectra in the attenuated total reflection mode are available. It is also equipped with a detector for operation in the far-infrared region.
Analysis Method: Infrared Spectroscopy – registers vibrational spectra. The method is sensitive to the functional groups in the investigated materials.
Non-destructive Method – the analyzed system is preserved in the state prior to the analysis. Applicable under a wide range of experimental conditions – applicable under significant changes in experimental conditions during the research, allowing measurements of catalytic processes at pressures up to 7 MPa. Informative Method – provides information about the composition of the substance, properties of the catalyst, participants in the reaction, surface compounds, and reaction products.
SPECIFIC SURFACE AREA
Equipment: Quantachrome Nova 1200e analyzer
Analysis Method: Gas adsorption is a suitable technique for characterizing porous materials. Low-temperature adsorption is based on the Brunauer-Emmett-Teller (BET) theory. Based on the obtained data from adsorption measurements, specific surface area according to BET, pore volume, and average pore diameter can be determined. Additionally, the distribution of micro- and mesopores by size can be assessed using various methods.
MÖSSBAUER SPECTROSCOPY
Equipment: Mössbauer spectrometer – WissEl – Wissenschaftliche Elektronik GmbH. The spectrometer is equipped with:
- Radioactive source of 57Co isotope for the investigation of iron-containing materials.
- Cryostat for capturing spectra of samples at liquid nitrogen temperatures.
- High-temperature attachment for capturing spectra of samples at temperatures in the range of 25 to 800°C.
- Cell for in situ Mössbauer spectroscopy in a reaction environment.
- RiKon-5 conversion electron detector, WissEl.
Analysis Method: Mössbauer spectroscopy is used to obtain data on the qualitative and quantitative composition of iron-containing crystalline, low-crystalline, and amorphous phases, as well as their degree of dispersity. It is one of the best techniques for studying relaxation phenomena such as superparamagnetism, collective magnetic excitation, and electron exchange.
X-RAY DIFFRACTION
Equipment: X-ray Diffractometer “TUR-M62” with PC control of the goniometer HZG-3
Analysis Method: X-ray diffraction (XRD) is a non-destructive analytical technique that provides in-depth information about crystalline samples, including the identification and determination of the morphology of crystalline phases, determination of crystal structure, crystal symmetry, textural effects, effective size of crystallites, and structural defects. It also allows for the assessment of the crystalline-to-amorphous ratio (% crystallinity). Suitable objects for investigation include inorganic and organic materials, minerals, corrosion products, etc.
TEMPERATURE PROGRAMMED REDUCTION AND DESORPTION
Equipment: DSC 111, Setaram, 1982
The DSC 111 (SETARAM) is a versatile instrument. It is to the physical-chemistry laboratory, to quality control, to industrial process studies and so on… It may be adapted to the user’s needs:
Analysis Method:
– isothermal or variable temperature measurement in wide temperature range(150-1100K);
– gas-solid reaction (oxidation – reduction, TPO, TPR) and heterogeneous catalysis;
– studies of the structure transformations and changes, phase diagrams, purity control, specific heat and polymerization.
GAS CHROMATOGRAPHY
Equipment: Gas Chromatograph by Agilent Technologies model 7890A configured to work with a single hyperbolic quadrupole mass-selective detector with electron impact ionization Agilent 5975C; automatic injector 7683B for 8 samples with a volume of up to 2 ml; capillary split/splitless injector with full electronic (digital) control of gas flows. In addition to the mass-selective detector, it is equipped with a flame ionization detector with full electronic control of all gases, optimized for operation only with capillary columns.
Analysis Method: Gas chromatography is a method for analyzing gas and liquid mixtures by separating and identifying the components of the respective mixture. When using the flame ionization detector for identifying compounds in the mixture, witnesses are required, and the characteristic parameter is the retention time of the compound. For the mass-selective detector, this is not necessary because identification is done immediately after the analysis based on the obtained mass spectrum and data from the computer library. Quantitative analyses are also possible after building calibration curves.
The apparatus is configured for the analysis of liquid samples only.
TRANSLATION: DIFFERENTIAL SCANNING CALORIMETRY
Equipment: Differential Scanning Calorimeter 111 manufactured by Setaram, 1982
Analysis Method: Brief Description: DSC is an autonomous and complex apparatus. It is suitable for physical-chemical laboratories, quality control, industrial process studies, etc. It can be adapted to the users’ needs:
– Measurements at constant and variable temperature in a wide temperature range (150 – 1100 K);
– Investigation of gas-solid reactions (oxidation-reduction, TPO, TPR) and heterogeneous catalysis;
– Study of structural transformations and changes, phase diagrams, purity control, specific heats, and polymerization.
ULTRAVIOLET AND VISIBLE REGION SPECTRA
TOTAL ORGANIC CARBON
Equipment: Total Organic Carbon Analyzer for water – TOC Analyzer Manufacturer: Shimadzu, Japan Model: TOC VCSH
Analysis Method: Catalytic complete oxidation of carbon-containing organic and inorganic compounds over a platinum catalyst at 680˚C
Method Sensitivity: Range from 4 ppm to 10,000 ppm (mg C/L)
OZONE TITRATION
Equipment: Ozone generator BMT 803 N – Germany. The generator has an ozone production capacity of 8 g/hour. The working gas is oxygen. Ozone analyzer BMT 964 – Germany. Operating range – 2-600 g/m3.
Analysis Method: Ozone is one of the most powerful oxidants with an oxidation potential of 2.07 V. It oxidizes all metals (except Pt, Au, and Ir) and non-metals to their highest oxidation states. It has a strong disinfectant action against viruses, bacteria, microbes, spores, fungi, etc. Under normal conditions, ozone rapidly oxidizes paraffins and unsaturated compounds and destructs polymers.
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