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Standard Test Method for Temperature Calibration of Thermogravimetric Analyzers 热重分析仪温度校准的标准试验方法
发布日期: 2021-07-01
1.1 本试验方法描述了热重分析仪在25°C至1500°C温度范围内的温度校准,适用于商用和定制仪器。该校准可通过使用熔点标准或磁转换标准来完成。 1.2 热重分析中的重量变化曲线受多种影响,其中一些影响是试样支架组件和大气的特性,而不是试样的特性。不同仪器的温度测量点、材料性质、尺寸和包装、样本容器的几何形状和组成、熔炉的几何形状和设计、温度传感器和显示刻度的准确性和灵敏度都有所不同。这些都会导致测量温度的差异,可能超过20℃ °C。此外,一些样品架组件将显示测量温度随样品尺寸或加热/冷却速率或两者的变化。 由于标准化样品架或热天平几何形状既不实用也不可取,因此可以通过测量熔融或磁性(居里点)转变温度与标准参考温度的偏差来校准仪器。该偏差可作为后续测量的校正项。 1.3 本试验方法假设仪器的指示温度在两点校准定义的范围内呈线性,并且该线性已得到验证。这两个校准温度应尽可能接近要进行的实验测量。 1.4 本试验方法描述了使用任何类型天平对热重分析仪进行温度校准的两个程序。程序A使用熔点标准进行校准。程序B使用磁转换标准进行校准。 1.5 通过这些程序生成的数据可用于使用一个或多个值来校正仪器的温度标度- 或两点温度校准程序。 1.6 以国际单位制表示的数值应视为标准值。本标准不包括其他计量单位。 1.7 本标准并非旨在解决与其使用相关的所有安全问题(如有)。本标准的用户有责任在使用前制定适当的安全、健康和环境实践,并确定监管限制的适用性。 1.8 本国际标准是根据世界贸易组织技术性贸易壁垒(TBT)委员会发布的《关于制定国际标准、指南和建议的原则的决定》中确立的国际公认标准化原则制定的。 ====意义和用途====== 5.1 热重分析仪用于表征广泛的材料。在大多数情况下,热重测量中指定的一个期望值是试样质量发生显著变化的温度。 因此,所有视质量变化曲线的温度轴(横坐标)必须通过直接读取温度传感器或通过调整编程器温度来精确校准,以匹配所需温度范围内的实际温度。在后一种情况下,这是通过使用熔点或磁转换标准来实现的。 5.2 本试验方法允许仪器温标数据的实验室间比较和实验室内相关性。
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. ====== Significance And Use ====== 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.
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归口单位: E37.01
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