Abstract The basis of recently developed quantitative TG-MS analysis was used for the evaluation of TPD-MS measurements in order to characterize the changes in the surface chemistry of carbon cryogels after the oxidation/activation treatment. This methodology was applied to the analysis of partially pyrolysed carbon cryogels (400 °C), which were oxidized/activated in four different ways (phosphoric acid, Fenton like reaction, ammonium persulfate with sulfuric acid and nitric acid with hydrogen peroxide). The quantitative TPD-MS evaluation enables analysis of all the evolved gases during the sample heating (without the calibration of all gases) and distinguishes the carbonization process from the decomposition of the more thermally stable oxygen surface groups (analysis of the effect of oxidation/activation reagents). The activation by H3PO4 results in the hydrolysis and esterification of anhydrides, lactones and phenols and creation of phosphoric acid esters (C-O-P), which decompose into C3-P=O linkages with the CO evolution. All the oxidation treatments had a similar effect on the surface chemistry. The amounts of carboxylic acids and anhydrides increased significantly, while the amount of lactones and phenol groups decreased (oxidized into carbonyls). Application of TG-MS fundamentals to the evaluation of TPD-MS profiles from a wide range of samples allows determining all the gaseous products.

中文翻译：

---

低温热解碳质样品的氧表面基团分析

摘要 最近开发的定量 TG-MS 分析的基础用于评估 TPD-MS 测量，以表征氧化/活化处理后碳冷冻凝胶的表面化学变化。该方法用于分析部分热解的碳冷冻凝胶 (400 °C)，该凝胶以四种不同的方式（磷酸、类芬顿反应、过硫酸铵与硫酸和硝酸与过氧化氢）氧化/活化。定量 TPD-MS 评估能够分析样品加热过程中的所有逸出气体（无需校准所有气体），并将碳化过程与更热稳定的氧表面基团的分解区分开来（分析氧化/活化的影响）试剂）。H3PO4 的活化导致酸酐、内酯和酚的水解和酯化以及磷酸酯 (COP) 的产生，磷酸酯 (COP) 分解为 C3-P=O 键并伴随 CO 释放。所有的氧化处理对表面化学都有相似的影响。羧酸和酸酐的数量显着增加，而内酯和酚基的数量减少（氧化成羰基）。将 TG-MS 基础应用于评估来自各种样品的 TPD-MS 曲线可以确定所有气体产物。羧酸和酸酐的数量显着增加，而内酯和酚基的数量减少（氧化成羰基）。将 TG-MS 基础应用于评估来自各种样品的 TPD-MS 曲线可以确定所有气体产物。羧酸和酸酐的数量显着增加，而内酯和酚基的数量减少（氧化成羰基）。将 TG-MS 基础应用于评估来自各种样品的 TPD-MS 曲线可以确定所有气体产物。