Netzsch instrumentation

Figure 16.28 Hyphenated TGA-FTIR, showing the heated transfer line and heated IR gas cell. (Courtesy of Netzsch Instruments, Inc., Paoli, PA.)...

Figure 16.29 (Continued) (b) The Perseus TGA-DSC-FTIR system with a vertical arrangement of the FTIR and thermal analysis system, with no external transfer line. (Courtesy of NETZSCH Instruments, Inc., Burlington, MA, www.netzsch-hermal-analysis.com.)...

The mass spectrum of evolved gases (up to MWs of 1024 Da) can be obtained to provide identification of the structure with no condensation during transfer between the thermal analyzer and the mass spectrometer. (Courtesy of Setaram Instmmentation, SA, Caluire, France, www. setaram.com.) (b) A different commercial thermogravimetry (TG)-GC-MS system, showing the Netzsch TG 209 on the right, connected to a GC-MS via an external transfer line. (Courtesy of NETZSCH Instruments, Inc., Burlington, MA, www.netzsch-thermal-analysis.com.)... 

Websites with thermal analysis instruments and apphcations include TA Instruments, www.tainstru-ments.com Mettler Toledo, wwwjnt.com PerkinElmer, www.peikinetmer.com NETZSCH Instruments, www.netzsch-thermal-analysis.com Setaram Instrumentation, www.setaram.com Expert System Solutions, www.expertsystemsolutions.com Shimadzu Scientific Instruments, www.ssi.shimadzu.com Hitachi High Tech Science Corporation, www.hitachi-hitec-science.com and GE Healthcare Life Sciences, www.gelifesciences.com. 

Figure 3.2. Three examples of commercial thermobalances, including typical thermocouple placement (a) a top-loading model (courtesy of Netzsch Instruments) (b) a side loading model (courtesy of Mettler-Toledo) (c) a bottom-loading model (courtesy of TA Instruments).

Fig. 54. - Example of thermodilatometric data 1396J obtained by using tlic NETZSCH instrument TMA 402, which shows the actually measured curve (thin solid line) and simultaneously calculated data of the relative defoimation (solid points) by means of the Narayanaswam s model [400J. Right, there is the graph of the time dependence of thermodynamic temperature (thin solid line) and calculated fictitious temperature (solid points). Courtesy of Marie Cfiromcikovd and Marek Liska, Trenilin, Slovakia. ...

Laser flush method (scheme left) for the detentiination of diffusivity, commercially produced by the Netzsch instruments at different modes (LFA 427, 437 or 447) using various measuring set ups and sample arrangements (right). Insets show two MicroRash applications, upper the thermal diffusivity and parallel calculated conductivity (by the aid of Netzsch DSC 404, cf. Fig.85. for electrolytic iron and bottom that for oxide glass. 

Nitrogen adsorption was performed at -196 °C in a Micromeritics ASAP 2010 volumetric instrument. The samples were outgassed at 80 °C prior to the adsorption measurement until a 3.10 3 Torr static vacuum was reached. The surface area was calculated by the Brunauer-Emmett-Teller (BET) method. Micropore volume and external surface area were evaluated by the alpha-S method using a standard isotherm measured on Aerosil 200 fumed silica [8]. Powder X-ray diffraction (XRD) patterns of samples dried at 80 °C were collected at room temperature on a Broker AXS D-8 diffractometer with Cu Ka radiation. Thermogravimetric analysis was carried out in air flow with heating rate 10 °C min"1 up to 900 °C in a Netzsch TG 209 C thermal balance. SEM micrographs were recorded on a Hitachi S4500 microscope. 

Tel. 09287-881-0, Fax -44, at ngb.netzsch.com, www.ngb.netzsch.com Perkin-Elmer Instruments, 710 Bridgeport Ave, Shelton CT 06484-4794, USA, Perkin-01-203-925-4600, Fax -4654, www.perkinelmer.com, info perkinelmer.com Elmer Rheometric Scientific, Inc. One Possumtown Road, Piscataway NJ 08854, USA, Rheometric 01-732-560-8550, Fax 7451, www.rheometricscientific.com,www.rheosci.com. Scientific (formerly Omnitherm PL)... 

The following instruments and analytical techniques were used FT-IR Perkin-Elmer FTIR 1750, KBr pellets, Raman Bruker IFS 55 H, C and Si NMR spectroscopy Bruker WM 300, solvent rfa-DMSO, internal standard Si(CH3)4) TGA-MS Netzsch STA 429, coupled with a Balzers QMG 420 mass spectrometer. 

The amount of coke on the spent catalysts was evaluated by CHNS Carlo Erba Instrument) and TGA/DSC (Netzsch STA 409 C analyzer) measurements. 

The crystal phases in the glass-ceramics were determined by XRD analysis. All instruments were precisely and identically set to ensure a high precision to obtain the integral peak area. The microstructure of the fresh fractured cross section of the glass-ceramics was observed by SEM. The thermal expansion coefficient (TEC) was calculated from room temperature to 500 °C at a heating rate of 5°C/min in the dilatometry analyser (NETZSCH, DIL402PC). The flexural strength was determined in a 3-point bend test at a constant strain ratio of 0.5mm/min. 

The late 1970s saw Polymer Laboratories develop their DMTA using dual cantilever bending, which works well for most small. samples from -150 C to the onset of melt. Shear, tensile, torsion, and simple compression options followed, as did the complementary Di-clectric Thermal Analyser (DETA), and computers were used from 1982 to both control and analyze the data. Seiko Instruments copied this and tried to patent it. and others such as Netzsch, Perkin-Elmer, and TA Instruments looked very closely at this before launching their own. For comparative data and fast thermal scans they all can give good data, but for absolute modulus numbers most systems need to consider the frame compliance, sample end corrections, and relative dimensions, and hence only a limited range of sample dimensions can be used for accurate measurement of modulus in a particular mode of deformation. 

Disadvantages to the use of a separate transfer line and separate FTIR inclnde the need for a separate heater for the transfer line, hot or cold spots in an improperly heated line, leading to the possibility of contamination due to buildup of condensable gases in the transfer line. In addition, more linear bench space is required for side-by-side instruments. New instruments are now available with no separate transfer line between the thermal analysis system and the FTIR spectrometer. In the Netzsch Perseus TGA-DSC-FTIR system, a Bruker Optics ALPHA FTIR spectrometer is connected directly to the thermal analyzer in a vertical arrangement (Figure 16.29b). The built-in heated gas cell of the spectrometer is directly connected to the gas outlet of the furnace. No separate heating controller is needed. The low volume of the short gas path results in rapid response and is especially useful where condensable evolved gases are present. 

Relaxation transitions in polymer EPDM samples before and after the introduction of CNF in alternating load was studied using dynamic mechanical analysis (DMA) on the instrument Netzsch DMA 242C in a temperature range from -140 to 150°C. We used the special cooler CC 200 L running on liquid nitrogen to obtain low temperatures... 

Simultaneous differential thermal and gravimetric analysis (DTA/TG) were carried out in a Netzsch STA 409 instrument on the azeotropically dried samples. The measurements were performed either in air or in nitrogen (18 1 ), from room temperature to 1073K at a heating rate of 2K/min. 

Metder-Toledo Inti. HP DSC 1 NETZSCH-Geratebau DSC 204 HP Phonix TA Instruments Q20P ... 

FIG. 16 DTA curves of cellulose heated and burned under 25 bars of oxygen. High-pressure DTA 404 H instrument from Netzsch. (From Ref. 112.)... 

In addition to the description of the DSCs of the three best-known commercial manufacturers in the previous paragraphs, Netzsch, Setaram, Seiko Instruments, and Shimadzu are often encountered on the US market. These are all heat flux DSCs Perkin-Elmer is the only power compensation DSC manufacturer. 

Low-force tabletop instruments are offered by the traditional thermal analysis vendors Mettler Toledo, Netzsch, Perkin-Elmer, and TA Instruments as well as Seiko Instruments. Higher-force tabletop and floor model instruments are offered by Bose and OldbMetrovib. Rotational rheometers that also perform torsional shear measurements on solid samples are marketed by Reologica... 

Aspects of common DEA techniques are presented in the following paragraphs, with emphasis on the instrumentation that is likely to be used in a typical thermal analysis laboratory examples are Novocontrol Spectrometers (BDS), TA Instruments (DEA 2970, although the production of this instrument has been discontinued), and Polymer Laboratories (DETA, this instrument is not available any more either). Dielectrometers (Micromet Instruments, now owned by Netzsch), used for in-process cure monitoring of thermosets, operate on similar principles. Features of the sensitive thermally stimulated current technique, and its comparison to DEA, are also discussed. 

The diagram on the right middle displays the principle of the Netzsch DSC 404. This instrument is based on the classical design of a heat flux DTA and can be used for heat capacity measurements up to about 1700 K. With a related design (STA 409, see also Chapter 7), differential calorimetry and thermogravimetry can be carried out simultaneously. [The temperature range is 110 K to 2700 K with different furnaces the heating rate is 0.1 to 100 K/min noise is 100 /liK, and sample volume is 100-900 mm ]. 

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