Linseis Couplings Overview
12Pages

With the coupling of a thermal balance and a gas analyzer like a FTIR spectrometer (Fourier Transform Infrared) or a Quadrupole-Mass-Spec-trometer a very powerful analytical instrumentation is used which gives information from the thermal balance (TGA) or simultaneous thermal analyzer (STA) as well as from the spectrometer simultaneously. The optional Pulse-Analysis injects an exactly predetermined amount of gas into the Thermobalance (TGA) or Simultaneous Thermal Analyzer (STA). This enhances the measurement possibilities significantly. Typical coulings for simultaneous measurements are: •...

racteristic vibrations which are either typical for a certain functional ionization detectors (FID) and thermal conductivity detectors (TCD). group (CO, COOR etc.) or for a particular compound (so called “fingerprint-region” of the spectra from 1500 – 500cm-1). Spectra libraries are helpful during spectra interpretation. Coupling to TGA and STA is a valuable tool especially in analysis of The coupling of the thermal analyser with the spectrometer/chromato- organic compounds (polymers etc.). graph can be done by different means: • Heated transfer capillary (FTIR, GCMS, GC, MS) Mass...

Mass spectrometry (MS) is an analytical technique to measure the mass of atoms or molecules of a gas e.g. evaporated from a sample material which has been heated up. The spectra are used to determine the elemental or isotopic signature of a sample, the masses of particles and of molecules, and to elucidate the chemical structures of molecules, such as peptides and other chemical compounds. Mass spectrometry works by ionizing chemical compounds to generate charged molecules or molecule fragments and measuring their mass-to-charge ratios. The QMS - quadrupole mass spectrometer coupling device...

The combination of thermal analysis with mass spectroscopy is a very powerful method to identify and quantify the components of the raw material and it is also a tool for the simulation of the manufacturing process of building materials. The components of cement raw material are: mixture of ceramic components (gypsum, calcium carbonate, etc.) and also organic components. The picture shows the simultaneous thermogravimetry (TG) combined with differential scanning calorimetry (DSC) and mass spectroscopy (MS). The mass spectrometry allows the identification of the evolved gases from the...

The Fourier transform infrared spectroscopy (FTIR) is a technique which is used to obtain an infrared spectrum of absorption, emission, • Research balance (different models) with TG or simultaneous TG/DSC photoconductivity or Raman scattering of a solid, liquid or gas. An FTIR spectrometer simultaneously collects spectral data in a wide spectral • High precision Nicolet FTIR spectrometer (different model available). range. This confers a significant advantage over a dispersive spectro- • Temperature range -170°C up to + 1750°C Three separate heating meter which measures intensity over a...

Analysis using thermogravimetry and FTIR Cement is an inorganic, non-metallic material. Together with water it The additives can be identified and quantified with thermal analysis. hardens and afterwards it stays also hard under water. Portland ce- The first step shows the evolved water from the CaSO4 di-hydrate to ment consists of limestone, clay and/or sand. The additives gypsum, CaSO4 half-hydrate. The second step is the conversion of the CaSO4 anhydrite etc. influence the setting time of the cement. Impurities in half-hydrate to the CaSO4 anhydrite. The evolved water can also be the raw...

Due to the limitation of the input pressure of the MS, the sample gas for the QMS. Since this aperture is inside the hot zone of the furnace, must be taken after the pressure controller (at ambient pressure). So, condensation of the out gassings can’t take place. Since between the only substances which can pass through the cold trap can be analyzed. aperture and the ion-source of the QMS a vacuum of app. 1e-5mbar exists, condensation there is impossible also. The outgassings of the sample are passed to the QMS-analyzer direct- The sniffer is placed directly above the sample. This is...

During heating samples often undergo phase transitions and/or weight tions or weight loss due to decomposition by liberation of volatile com- change due to evaporation of solvents and/or chemical reactions. The- pounds. Analysis of these evolved gases can give valuable information se changes can be detected by thermal analysis: calorimetric tech- about the sample composition and reaction pathways for decomposi- niques (DTA and DSC) give information about the heat involved in these tion. As thermal analysis gives no information about the nature of the processes and thermogravimetry (TG)...

Thermal decomposition of latex 100 90 At 370° synthetic rubber decomposes into some monomer parts. The main parts limonene and isoprene can be identified using STA com- bined with GC-MS. The STA signal shows mass loss and enthalpie and a bigger one, where the samller one can be identified by mass change at 372°. At the same time the GC shows two peaks, a smaller spectrometrie as isoprene and the bigger one as limonene. Relative Intensity

Possible Techniques: Advantages of the optical In-Situ window: • FTIR: Fourier Transform Infrared Spectroscopy: Measurement of • No cooling / modification of the measuring gas (for example no basic and trace gas components until ppm range (for example H2O, out-condensation, no transition reaction, no equilibrium shift) CO2, CO, H2S...). Polar Molecules are necessary. • Many materials with high condensation temperature for exam- • Raman-Spectroscopy: Measurement of basic gas components. Also ple alkali metals (Na, K and their combinations) are now able to be not polar molecules like H2 or N2...

LINSEIS GmbH Vielitzerstr. 43 95100 Selb Germany Tel.: (+49) 9287–880 - 0 Fax: (+49) 9287–70488 E-mail: info@linseis.de LINSEIS Inc. 109 North Gold Drive Robbinsville, NJ 08691 USA Tel.: +01 (609) 223 2070 Fax: +01 (609) 223 2074 E-mail: info@linseis.com Products: DIL, TG, STA, DSC, HDSC, DTA, TMA, MS/FTIR, In-Situ EGA, Laser Flash, Seebeck Effect Services: Service Lab, Calibration Service