Carbon black was functionalized by gas-phase oxidation using nitric acid vapor at 150 °C, and temperature-programmed desorption (TPD) and temperature-programmed reduction (TPR) experiments were performed in a plug-flow reactor to analyze the decomposition mechanisms of oxygen-containing surface groups by monitoring evolved H₂O, CO₂, and CO quantitatively. Subsequent TPD measurements detected an enrichment of acidic surface groups with increasing duration of the HNO₃ functionalization from 2 h to 24 h. A significant amount of H₂O was released during the TPD experiments, yielding H₂O evolution profiles which were deconvoluted into two Gaussian peaks at 162 °C and 228 °C. The combined analysis of the CO₂ and H₂O profiles indicates that desorbed H₂O originates from chemisorbed water bound to carboxylic acid groups and from condensation reactions of carboxylic acids and phenols. Phenols and carbonyls were found to be reduced selectively by H₂ during TPR, generating a pronounced H₂O peak at 650 °C. A new peak in the CO₂ evolution profile appeared at 575 °C in reducing atmosphere, which is assigned to the hydrolysis of anhydrides and lactones with subsequent decomposition. Thus, taking H₂O into account is mandatory for a complete quantitative analysis of the decomposition mechanisms occurring during TPD and TPR experiments.

在150  °C下使用硝酸蒸气通过气相氧化功能对炭黑进行功能化，并在活塞流反应器中进行了程序升温脱附（TPD）和程序升温还原（TPR）实验，以分析氧气的分解机理通过定量监测放出的H ₂ O，CO ₂和CO来确定含碳的表面基团。随后的TPD测量发现，随着HNO ₃功能化持续时间从2小时增加到24小时，酸性表面基团的富集。在TPD实验过程中释放了大量H ₂ O，产生了H ₂ O演化曲线，在162  °C和228时解卷积为两个高斯峰 ℃。对CO ₂和H ₂ O分布图的组合分析表明，解吸的H ₂ O源自与羧酸基团结合的化学吸附水以及羧酸和酚的缩合反应。在TPR过程中，酚和羰基被H ₂选择性还原，在650 °C时产生明显的H ₂ O峰 。在还原气氛中，在575 °C时，CO ₂释放曲线出现了一个新的峰，该峰 与酸酐和内酯的水解以及随后的分解有关。因此，取H ₂对于TPD和TPR实验期间发生的分解机理的完整定量分析，必须考虑到O。