【国外标准】 Standard Test Method for Temperature Calibration of Thermogravimetric Analyzers

5.1 Thermogravimetric analyzers are used to characterize a broad range of materials. In most cases, one of the desired values to be assigned in thermogravimetric measurements is the temperature at which significant changes in specimen mass occur. Therefore, the temperature axis (abscissa) of all apparent-mass-change curves must be calibrated accurately, either by direct reading of a temperature sensor, or by adjusting the programmer temperature to match the actual temperature over the temperature range of interest. In the latter case, this is accomplished by the use of either melting point or magnetic transition standards.5.2 This test method permits interlaboratory comparison and intralaboratory correlation of instrumental temperature scale data.1.1 This test method describe the temperature calibration of thermogravimetric analyzers over the temperature range from 25 °C to 1500 °C and is applicable to commercial and custom-built apparatus. This calibration may be accomplished by the use of either melting point standards or magnetic transition standards.1.2 The weight change curve in thermogravimetry results from a number of influences, some of which are characteristic of the specimen holder assembly and atmosphere rather than the specimen. The variations from instrument to instrument occur in the point of measurement of the temperature, the nature of the material, its size and packing, the geometry and composition of the specimen container, the geometry and design of the furnace, and the accuracy and sensitivity of the temperature sensor and displaying scales. These all contribute to differences in measured temperatures, which may exceed 20 °C. In addition, some sample holder assemblies will show variations of measured temperature with sample size or heating/cooling rate, or both. Since it is neither practical nor advisable to standardize sample holders or thermobalance geometries, instruments may be calibrated by measurement of the deviation of a melting or magnetic (Curie point) transition temperature from the standard reference temperature. This deviation can be applied as a correction term to subsequent measurements.1.3 This test method assumes that the indicated temperature of the instrument is linear over the range defined by a two-point calibration and that this linearity has been verified. These two calibration temperatures should be as close to the experimental measurements to be made as possible.1.4 This test method describes two procedures for temperature calibration of thermogravimetric analyzers using any type balance. Procedure A uses melting point standards for calibration. Procedure B uses magnetic transition standards for calibration.1.5 The data generated by these procedures can be used to correct the temperature scale of the instrument by either a positive or negative amount using either a one- or two-point temperature calibration procedure.1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.7 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.1.8 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.