双语化学辞典Chem Lexicon
技术 · 分析化学 · 热分析 Analytical chemistry · Thermal analysis

热重分析Thermogravimetric analysis

拼音Pinyin rè zhòng fēn xī 别名Also TGA;热重法;TG;TGA;thermogravimetry;TG

定义Definition

热重分析是在程序控温下连续测量样品质量随温度(或时间)变化的热分析技术,用于研究物质的热稳定性、分解过程、脱水、氧化、吸附和组成。

Thermogravimetric analysis continuously measures a sample's mass as a function of temperature or time under a controlled temperature programme. It is used to study thermal stability, decomposition, dehydration, oxidation, adsorption and composition.

原理与仪器Principle and instrument

热重分析仪核心是高灵敏度的热天平(可达 0.1 μg),样品放在坩埚中,在设定的气氛(氮气、氩气、空气或氧气)下以一定速率(常用 10 °C/min)升温。所得热重曲线(TG)显示质量损失台阶,其一阶导数(DTG)的峰对应最大失重速率温度。常与差示扫描量热法(DSC)同步联用(TG-DSC),或与红外、质谱联用分析逸出气体。

At its heart is a sensitive thermobalance, reading to about 0.1 μg; the sample sits in a crucible and is heated at a set rate, commonly 10 °C/min, in nitrogen, argon, air or oxygen. The TG curve shows steps of mass loss, and peaks in its first derivative (DTG) mark temperatures of fastest loss. It is often run simultaneously with DSC (TG-DSC) or coupled to infrared or mass spectrometry to identify evolved gases.

经典示例A classic example

一水合草酸钙 CaC₂O₄·H₂O 的热重曲线有三个台阶:约 100–200 °C 失去结晶水(失重 12.3%),约 400–500 °C 分解为 CaCO₃ 并放出 CO(19.2%),约 600–800 °C 分解为 CaO 并放出 CO₂(30.1%)。它常被用作热重仪器的校准标准。

Calcium oxalate monohydrate, CaC₂O₄·H₂O, loses mass in three steps: water of crystallisation at about 100–200 °C (12.3%), CO on decomposing to CaCO₃ at about 400–500 °C (19.2%) and CO₂ on decomposing to CaO at about 600–800 °C (30.1%). It is often used to calibrate thermogravimetric instruments.

由来与应用Origin and applications

1915 年日本东北大学的本多光太郎制造了第一台热天平。1950 年代起商品化仪器出现。TGA 用于测定高分子的热分解温度和填料含量、药物和晶体的结晶水与溶剂含量、催化剂积碳量、煤和生物质的水分灰分挥发分、金属有机框架的热稳定性、锂电池材料的组成,以及研究反应动力学。

Kotaro Honda at Tohoku University built the first thermobalance in 1915, and commercial instruments appeared from the 1950s. TGA measures decomposition temperatures and filler content of polymers, water and solvent of crystallisation in drugs and crystals, coke on catalysts, moisture, ash and volatiles in coal and biomass, thermal stability of metal–organic frameworks and the composition of battery materials, and is used in kinetic studies.

反应Reactions

CaC2O4·H2O ⟶ CaC2O4 ⟶ CaCO3 ⟶ CaO

分别放出 H₂O、CO、CO₂。

Releasing H₂O, CO and CO₂ in turn.

CuSO4·5H2O ⟶ CuSO4·3H2O ⟶ CuSO4·H2O ⟶ CuSO4

五水硫酸铜分步脱水

Stepwise dehydration of copper sulfate pentahydrate

年表Timeline

  • 1915

    本多光太郎制造热天平

    Honda builds the thermobalance

  • 1950s

    商品化热重分析仪出现

    Commercial TGA instruments appear