Instrumentation, differential scanning

Fourier Transformation Infrared (FT-IR) spectra were recorded using a Peridn-Elmer RX-1 spectrometer with KBr pellet from 4,000 to 400 cm . The H NMR and NMR speetra were acquired at 300 MHz on a Bruker-300 spectrometer with 1% tetra-methylsilane (TMS) as an internal standard. The DSC analysis was carried out with a Qj series TA instruments differential scanning calorimeter using 5-7 mg of the sample crimped in alumininm pans at a heating rate of 10°C/min and nnder nitrogen atmosphere with a flow rate of 40 ml/mia The MW reactions were carried out in a Milestone Ine., laboratory MW system with a frequency of 2,450 MHz and controllable power system (max 1,000 W). A 50 ml (diameter 5 cm) Teflon reaction vessel was used. The temperature and time of the reaction were controlled by pre-programmed Easywave software system. 

Tg values for NOA 63 (and composites thereof) cured to varying extents were measured using a TA Instruments Differential Scanning Calorimeter (DSC) model 2920 using heating/cooling rate of 10 C/min under nitrogen atmosphere. A PerkinElmer Dynamic Mechanical Analyzer (DMA) 7e was run in tensile mode at an... 

Electrophoretic methods of separation of LD Tsoenzymes have become routine in clinical laboratories. Efforts are now being made to standardize the methodologies used for LD isoenzymes, particularly by Rosalki (38). The preferred methods are based on electrophoresis on a solid medium, so that the several bands may be scanned instrumentally. Differential isoenzyme inhibition with urea or other inhibitors is based on the fact that the heart LD isoenzyme is more resistant to inhibition than other isoenzymes. However, the analyst then has the problem of allocating the observed degree of inhibition between the different isoenzymes of a given sample, a problem that has not been resolved satisfactorily thus far. Hence, differential inhibition is not as reliable for isoenzyme separation as is electrophoresis. 

Anonymous. Software for Oscillating Differential Scanning Calorimeter. Horsham, Seiko Instruments 1995. 

Figure 2. Comparison of the Differential Scanning Calorimetry (DSC) thermograms of the homopolymer HB and various block copolymers to that of the LDPE. Weight of each polymer sample is indicated in the parentheses. The instrument range is 2 mcal/s for all the runs.

Measurements of differential scanning calorimetry (DSC) were obtained on a TA Instruments 2910 thermal analysis system (Fig. 2). Samples of approximately 1-2 mg were accurately weighed into an aluminum DSC pan, and covered with an aluminum lid that was crimped in place. The samples were then heated over the range of 20-140 °C, at a heating rate of 10 °C/min. Valproic acid was found to boil at 227 °C. 

Safety studies of the graphite anode samples were performed using a Perkin-Elmer Differential Scanning Calorimeter (DSC, model Pyris 1) instrument. The temperature scanning rate was 10 C/min over a temperature range of 50 to 375°C. 

X-ray diffraction studies are usually carried out at room temperature under ambient conditions. It is possible, however, to perform variable-temperature XPD, wherein powder patterns are obtained while the sample is heated or cooled. Such studies are invaluable for identifying thermally induced or subambient phase transitions. Variable-temperature XPD was used to study the solid state properties of lactose [20], Fawcett et al. have developed an instrument that permits simultaneous XPD and differential scanning calorimetry on the same sample [21], The instrument was used to characterize a compound that was capable of existing in two polymorphic forms, whose melting points were 146°C (form II) and 150°C (form I). Form II was heated, and x-ray powder patterns were obtained at room temperature, at 145°C (form II had just started to melt), and at 148°C (Fig. 2 one characteristic peak each of form I and form II are identified). The x-ray pattern obtained at 148°C revealed melting of form II but partial recrystallization of form I. When the sample was cooled to 110°C and reheated to 146°C, only crystalline form I was observed. Through these experiments, the authors established that melting of form II was accompanied by recrystallization of form I. 

If the observed AH is positive (endothermic reaction), the temperature of the sample will lag behind that of the reference. If the AH is negative (exothermic reaction), the temperature of the sample will exceed that of the reference. Owing to a variety of factors, DTA analysis is not normally used for quantitative work instead, it is used to deduce temperatures associated with thermal events. It can be a very useful adjunct to differential scanning calorimetry, since with most instrumentation DTA analysis can be performed in such a manner that corrosive... 

Adiabatic calorimeters are complex home-made instruments, and the measurements are time-consuming. Less accurate but easy to use commercial differential scanning calorimeters (DSCs) [18, 19] are a frequently used alternative. The method involves measurement of the temperature of both a sample and a reference sample and the differential emphasizes the difference between the sample and the reference. The two main types of DSC are heat flux and power-compensated instruments. In a heat flux DSC, as in the older differential thermal analyzers (DTA), the... 

ARC = Accelerating Rate Calorimeter (Columbia Scientific Instrument Corp.) DSC = Differential Scanning Calorimeter DTA = Differential Thermal Analysis RC1 = Reactor Calorimeter (Mettler-Toledo Inc.) RSST = Reactive System Screening Tool (Fauske and Associates) VSP = Vent Size Package (Fauske and Associates) ... 

A variety of techniques have been used to determine the extent of crystallinity in a polymer, including X-ray diffraction, density, IR, NMR, and heat of fusion [Sperling, 2001 Wunderlich, 1973], X-ray diffraction is the most direct method but requires the somewhat difficult separation of the crystalline and amorphous scattering envelops. The other methods are indirect methods but are easier to use since one need not be an expert in the field as with X-ray diffraction. Heat of fusion is probably the most often used method since reliable thermal analysis instruments are commercially available and easy to use [Bershtein and Egorov, 1994 Wendlandt, 1986], The difficulty in using thermal analysis (differential scanning calorimetry and differential thermal analysis) or any of the indirect methods is the uncertainty in the values of the quantity measured (e.g., the heat of fusion per gram of sample or density) for 0 and 100% crystalline samples since such samples seldom exist. The best technique is to calibrate the method with samples whose crystallinites have been determined by X-ray diffraction. 

A differential scanning calorimeter (DSC), Dupont Instrument, Model DSC2910, was used to determine the glass transition temperatures. Thermo-gravimetric analyses were carried on a thermogravimetric analyzer (TGA), TA Instruments, Model Hi-Res TGA 2950. 

Instrumentation. UV/Visible spectra were collected on a Perkin-Elmer Lambda 4 spectrophotometer. IR spectra were collected on a Perkin-Elmer 1640 spectrophotometer. NMR spectra were taken on a Nicolet NT-200 spectrometer. Differential scanning calorimetry was run on a Perkin-Elmer DSC-4 unit, equipped with a system 4 microprocessor controller and a 3600 data station. Elemental analyses were run by the Purdue microanalysis laboratory in the Department of Chemistry at Purdue University and by Huffman Labs (Golden, CO). Lignin group analysis techniques are described in references 19-21. 

Differential scanning calorimetry is primarily used to determine changes in proteins as a function of temperature. The instrument used is a thermal analysis system, for example a Mettler DSC model 821e. The instrument coupled with a computer can quickly provide a thermal analysis of the protein solution and a control solution (no protein). The instrument contains two pans with separate heaters underneath each pan, one for the protein solution and one for the control solution that contains no protein. Each pan is heated at a predetermined equal rate. The pan with the protein will take more heat to keep the temperature of this pan increasing at the same rate of the control pan. The DSC instrument determines the amount of heat (energy) the sample pan heater has to put out to keep the rates equal. The computer graphs the temperature as a function of the difference in heat output from both pans. Through a series of equations, the heat capacity (Cp) can be determined (Freire 1995). 

Characterization of Fats and Waxes by Differential Scanning Calorimetry , Instrument News 17(1), 8-9 (1966) 75) G.T. Afanas ev. 

Interest in the use of calorimetry as a routine diagnostic or analysis tool has gained significant momentum only in the last 50 years. This interest has lead to the development of popular procedures such as differential thermal analysis (DTA) and differential scanning calorimetry (DSC). A wide variety of solution calorimetric techniques exist today. These techniques include thermometric titration, injection and flow emhalpimetry. The major growth of commercial instrumentation for calorimetry has occurred to address applications in routine analysis and the rapid characLerizaiion of materials. 

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