“…Subsequent measurements using high-quality 5.0-MHz crystals, the second prototype instrument, and computer data acquisition under programmed temperature conditions showed the variation between successive heating cycles to be on the same order as the noise in a single background or about 1 to 2 times the digitization error for the frequency. At 1-s acquisition times, the error was [2][3][4][5] Hz while at 0.1-s acquisition times the error was 10-20 Hz. The background data were subjected to least-squares curve fitting of first through fifth orders.…”
Section: Resultsmentioning
confidence: 98%
“…Thermogravimetry (TG) has developed into an important analytical technique since its introduction by Honda in 1915 (1). Recent applications have been extensively reviewed in this journal (2,3) and have included studies of the decomposition of polymers (4,5), flame retardancy (6), oil stability (7,8), and the volatility of compounds in addition to more classical studies of minerals and precipitates (2,3). A large portion of the use of TG has been in the routine screening of materials by industry, and much of this has been documented primarily in the technical applications literature.…”
A piezoelectric crystal thermogravimetric analyzer Is described which allows analysis of microgram samples at rates up to 100 °C/min. Samples are deposited as films from solution In a volatile solvent. The variation in frequency as a function of crystal temperature Is measured and subtracted
“…Subsequent measurements using high-quality 5.0-MHz crystals, the second prototype instrument, and computer data acquisition under programmed temperature conditions showed the variation between successive heating cycles to be on the same order as the noise in a single background or about 1 to 2 times the digitization error for the frequency. At 1-s acquisition times, the error was [2][3][4][5] Hz while at 0.1-s acquisition times the error was 10-20 Hz. The background data were subjected to least-squares curve fitting of first through fifth orders.…”
Section: Resultsmentioning
confidence: 98%
“…Thermogravimetry (TG) has developed into an important analytical technique since its introduction by Honda in 1915 (1). Recent applications have been extensively reviewed in this journal (2,3) and have included studies of the decomposition of polymers (4,5), flame retardancy (6), oil stability (7,8), and the volatility of compounds in addition to more classical studies of minerals and precipitates (2,3). A large portion of the use of TG has been in the routine screening of materials by industry, and much of this has been documented primarily in the technical applications literature.…”
A piezoelectric crystal thermogravimetric analyzer Is described which allows analysis of microgram samples at rates up to 100 °C/min. Samples are deposited as films from solution In a volatile solvent. The variation in frequency as a function of crystal temperature Is measured and subtracted
The review summarizes the current state, outlook and development of the field of thermal analysis, emphasizing the study of thermal effects as the basis of all other methodologies. Heat and its understanding intertwines throughout the entire civilization from the Greek philosophers through the middle ages to today’s advanced technological era. The foundations of the field of thermal analysis, where heat acts as its own agent, date back to the nineteenth century, and the calorimetric evaluation of heat fluxes became the basis. It views the processes of calibration and rectification specifies the iso- and noniso- degrees of transformation, explains the role of the equilibrium background, which is especially necessary in kinetics. It introduces a new concept of thermodynamics with regard to the constancy of first derivatives and discusses the role of standard temperature and its non-equilibrium variant—tempericity. It describes the constrained states of glasses and assesses the role of dimensions in material science. Finally yet importantly, it deals with the influence of thermoanalytical journals, their role in presenting unusual results, and discusses the role of the dissident science. It also describes the level and influence of adequate books and finally describes discussions and perspectives, i.e. where to look better interpretation for and what is the influence of current over-sophisticated devices.
A novel continuous-flow apparatus for on-line kinetic studies of (bio)chemical solution-phase processes by electrospray ionization mass spectrometry (ESI-MS) is described. The device is based on two concentric capillaries. Fluid is released from the inner capillary into the intercapillary space, where it mixes with solution flowing through the outer capillary, thus initiating the reaction of interest. Gas-phase analyte ions are formed near the tip of the outer capillary by pneumatically assisted ESI. This setup allows the mixer to be placed directly within the ion source, thus providing a minimal dead volume of ~8 nL. Time-resolved data can be recorded in both "spectral" and "kinetic" modes. In the former case, the position of the inner capillary is fixed at various points, such that entire mass spectra can be recorded for selected reaction times. For experiments in kinetic mode, the mass spectrometer monitors the signal intensity at selected m/z values, while the inner capillary is continuously pulled back, thus providing intensity-time profiles for specific reactive species. A theoretical framework is developed that allows the measured kinetics to be analyzed by taking into account the effects of laminar flow within the reaction capillary. Failure to take these effects into account results in erroneous rate constants. Studies on the demetalation kinetics of chlorophyll reveal that the apparatus can reliably measure rate constants up to at least 100 s-1. This represents a substantial improvement over previous ESI-MS-based kinetic methods. Spectral mode experiments on the refolding of ubiquitin show the changing proportions of denatured and tightly folded protein subpopulations in solution. When monitored in kinetic mode, the refolding process was found to proceed with a rate constant of 5.2 s-1.
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