Setaram Instruments

Thermogravimetric analysis (TGA) and differential temperature analysis (DTA) were performed on a Setaram Instrumentation SETSYS Evolution - 1200. Samples were heated in flowing air (50 ml/min) from 20 to 900°C at 10°/min. 

Web http //www.brookhaven.co.uk/thanda.html E-mail info brookhaven.co.uk (SETARAM Instruments, etc.)... 

Figure 16.23 A 2D plate detector versus 3D Calvet detector designs, (a) A 2D plate detector with thermocouples under the two pans. Only the heat flow from the bottom of the pans Is measured, (b) and (c) 3D Calvet calorimetric sensors with arrays of thermocouples totally surrounding both the sample and reference chamber. Approximately 94% of the heat flow Is captured and measured using these sensors, (d) A Calvet detector with 10 thermocouples for the sample and 10 for the reference. (Courtesy of Setaram Instrumentation, SA, Caluire, France, www.setaram.com. Used with permission.)...

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. 

Pierre Lepariouer SETARAM Instrumentation, 7 Rue de I Oratoire, 69300 Caluire-et-Cuire, France, e-mail leparlouer setaram.com... 

The integral and differential enthalpies of displacement can be measured directly using calorimeters of the isothermal type. Such instruments either are produced and marketed by some manufacturers of high-performance calorimetric systems for different applications (e.g., SETARAM Instrumentation, LKB-ThermoMetric, TA Instruments, Microscal Ltd), or are home-mode prototypes based on original work carried out in university laboratories and therefore documented in considerable detail in scientiAc publications. This section focuses on the properAes of two calorimetry systems used by the author to study the compeAAve adsorpAon from dilute solution. 

Other instruments include the Calvet microcalorimeters [113], some of which can also run in the scanning mode as a DSC. These are available commercially from SETARAM. The calorimeters exist in several configurations. Each consists of sample and reference vessels placed in an isothermally controlled and insulated block. The side walls are in intimate contact with heat-flow sensors. Typical volumes of sample/reference vessels are 0.1 to 100 cm3, The instruments can be operated from below ambient temperatures up to 300°C (some high temperature instruments can operate up to 1000°C). The sensitivity of these instruments is better than 1 pW, which translates to a detection limit of 1 x 10-3 W/kg with a sample mass of 1 g. 

Equipment to be Used for the Analysis of Hazards The need for experimental thermodynamic and kinetic data is clear by now. The equipment designed to provide this information for the chemicals involved are described in Chapter 2, and include the DSC, DTA, ARC, Sikarex, SETARAM C-80, and DIERS technology. Kinetic data for the desired reaction are preferably obtained with instrumented bench-scale equipment such as the RC1. This type of equipment is discussed in Section 3.3. 

X-ray powder diffraction patterns were obtained on oriented film specimens [7] (2 to 45° 2 , Philips PW 1120, monochromatized CuKa radiation, continuous peak registration). BET surface area and the pore volume distribution were determined from Nj adsorption-desorption isotherms at 77 K (degassing at 393 K, lO" mbar, 5h Sorptomatic 1900, Carlo Erba Instruments). The IR-spectra were recorded on KBr wafers [4] with a Specord 80M spectrometer. The XPS (X-ray photoelectron spectroscopy) spectra were obtained with VG ESCALAB 200 MKII spectrometer equipped with a twin anode AIKa source (1486 eV). The thermogravimetric (TGA) analyses were carried out with a Setaram TG 85 thermobalance at a heating rate of 6 K min in a helium flow of 30 ml min . The chromium content of the samples was determined by EPMA (JEOL 840 scanning electron microscope) with energy dispersive spectrometer (EDS, Tracer Northern) and by AAS (atomic absorption spectroscopy, Perkin Elmer 3030) analyses. 

It should be noted that, in principle, all the flow calorimeters discussed here are capable of operating both in the gas/vapour phase and in the solution phase. However, the calorimeters manufactured by Setaram and Thermometric are generally used for solution-phase studies, whereas the Microscal instruments are designed specifically to facilitate gas/vapour-phase studies. For the purposes of this discussion, gaseous-phase flow calorimetry will centre around a consideration of the Microscal instruments, and solution-phase calorimetry will centre around the Setaram and Thermometric instruments. 

For TGA, a Setaram TGA-DTA 92 apparatus was used. Alternatively, a home-built apparatus was employed for TPD-MS. GC analysis was on a Chrompack CP-Sil-5 column, eventually coupled to a Fisons mass spectrometer. ESR spectra were recorded with a Bruker ESP-300 and a TE104 cavity at temperatures between 130 and 300 K. N2 sorption experiments were performed with an Omnisorp-100 instrument. The t-plot method was applied for the analysis of the pore volume. Solid state NMR spectra were recorded using a Bruker MSL 400 spectrometer at a resonance frequency of 100.61 MHz. Cross polarization was optimized with glycine as a reference. For the measurement of liquid samples, a Bruker AMX 300 system was used, operating at 300.13 and 75.47 MHz for iH and C, respectively. 

Whereas most fixed-cell instruments are power-compensation instruments (because it is possible to place heaters on the base of cells that are not removable), batch-cell instruments are available as either power-compensation or heat-flux designs. One design of a heat-flux, batch-cell instrument is the micro-DSC in (Setaram). The instrument consists of a calorimetric block into which two channels are machined. One channel holds the sample cell, the other holds the reference cell. At the bottom of each channel, between the cell and the block, is a plane-surfaced transducer. The transducers provide a thermal pathway between the cells and the block and are used to maintain the cells at a temperature identical to that of the block. The electrical signal produced by the transducer on the sample side is proportional to the heat evolved or absorbed by the sample. The temperature of the calorimetric block is maintained by a precisely thermostated circulating liquid. The liquid is raised in temperature by a separate heater and is cooled by a supply of circulating water. The precise control of the temperature of the circulating liquid allows scan rates of just 0.001°C min-1 to be attained and ensures that the calorimetric block is insulated from the surrounding environment. 

Thermal analyses (TG, DTG, DTA) of the n-Bu2NH-S APO-31 dried in air at 393K for 16 h were carried out in an oxidizing (air) atmosphere, using a computer assisted instrument (Setaram TG-DTA 92) under the following conditions sample size, 30g reference compound, a-alumina sample holder, Pt crucible heating rate, 10°C/min atmosphere, flowing air. 

Elemental composition of the calcined AIPO4 was determined by SEM-EDX (JEOL-JSM 6300, 20 kV). TG-DTA measurements were performed in flowing Ar (293-1173 K, 10 K min ) using a Setaram thermobalance Setsys-12. XRD patterns (CuK radiation) were developed in a Siemens D-5000 diffractometer. FT-Raman spectra were taken from compacted samples at 3600-200 cm (resolution 0.2 cm ), using a Perkin-Elmer System 2000 spectrometer. XPS were recorded on a Leybold-Heraeus LHS-10 spectrometer (at 10 Torr) using Al Ka radiation and a pass energy constant of 50 eV. A1, P and MAS-NMR spectra were recorded on a Bruker ACP-400 spectrometer. DRIFT spectra (4000-400 cm resolution 8 cm 256 scans) were recorded on a Bomem MB-100 FT-IR instrument equipped with an environmental chamber placed in a DRIFT attachment. DRIFT spectra were recorded for calcined materials (200 mesh size and diluted to 15 wt% KBr) previously vacuum-dried at 400 K for 24... 

A Setaram Titrys microcalorimeter was used for these experiments. This instrument is based on the C80 microcalorimeter described above, modified to allow continuous stirring of liquid samples. The pre-heated titrant is added to both sample and reference cells simultaneously using a programmable twin syringe pump. 

The state of copper in the prepared catalysts was studied by ESR spectroscopic technique and by thermal analysis in flow hydrogen medium. Experimental measurements were performed with a spectrometer ART-6 in X frequency bands analysis (u = 9010 MHz) and a thermoanalitical instrument SETARAM. 

A TG-DSC instrument capable of sub-ambient temperature operation has been available for a number of years, and is especially valuable in the study of systems containing moisture, or other volatiles. In this case, a DSC heat flux plate was adapted to allow it to be suspended from the thermobalance beam, instead of the pair of thermocouples shown in Figure 1. A completely different approach to TG-DSC is taken by SETARAM, in their TG-DSC 111 instrument. The sample and reference... 

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.)... 

The powders have been characterized by the following methods XRD with a Philips 1130 (CoKa radiation) diffractometer, simultaneous TG-DTG-DTA analyses with a Setaram TG92 instrument, FT- IR and FT-FIR spectroscopies with a Nicolet Magna 750 spectrometer, FT-Raman spectroscopy with a Bruker RFSIOO instrument. Surface area and porosity were performed at 77 K by the BET method. 

For highly sensitive nticrobalances (Thermo Cahn, Hiden, Mettler-Toledo, Rubotherm, Setaram, TA Instruments, VTI) only tiny amounts of sorbent materials are needed to measure gas adsorption equilibria. This is advantageous for investigations in newly developed sorbent materials where often only small amounts are available. However, results may be misleading as the sorbent sample used does not represent a statistically averaged sample of a techitical sorbent and thus may exhibit considerable statistical deviations. 

FIG. 6 Calorimetric curves of amorphous sucrose and cellobiose (both heated in sealed crucibles) c, Crystallization /, fusion d, decomposition. Instrument Setaram C80. (From Ref. 46.)... 

FIG. 10 Gelatinization and specific heat change of native wheat starch (water solution of 40% dry matter). Instrument Setaram Micro-DSC. (Adapted from Ref. 69.)... 

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. 

Setaram offers four different lines of DSC instrumentation based on a heat flux design using either a heat leak disk or a Calvet detector. The first DSC line, the DSC131, uses a heat leak or what Setaram terms a plate construction. This unit has an operating range of -170-700 C. The unit can be operated with 30- or 100-pL crucibles. 

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