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一种改进的在过硫酸盐存在下测定碳水化合物的苯酚-硫酸法。

An improved phenol-sulfuric acid method for the determination of carbohydrates in the presence of persulfate.

机构信息

Tianjin Key Laboratory of Pulp and Paper, Tianjin University of Science and Technology, Tianjin 300457, PR China; Guangxi Key Laboratory of Clean Pulp & Papermaking and Pollution Control, College of Light Industry and Food Engineering, Guangxi University, Nanning 530004, PR China; Hangzhou Specialty Paper Industry Co. Ltd., Hangzhou 311407, PR China.

Tianjin Key Laboratory of Pulp and Paper, Tianjin University of Science and Technology, Tianjin 300457, PR China.

出版信息

Carbohydr Polym. 2020 Jan 1;227:115332. doi: 10.1016/j.carbpol.2019.115332. Epub 2019 Sep 12.

Abstract

Advanced oxidation processes (AOPs) based on activated persulfate have received extensive attention for sludge pretreatment. Persulfate (PS) is a persistent oxidant and the excess persulfate in the sludge affects the carbohydrate analysis using the traditional phenol-sulfuric acid method. In this study, an improved phenol-sulfuric acid method was developed for the determination of carbohydrates in the presence of persulfate, and a critical procedure was introduced before the conventional determination with the assistance of the chemical pretreatments. The best reagent was screened from four reductants (i.e. NaS, KI, NaSO and NaSO) and two free-radical scavengers (i.e. phenol and benzoic), and the optimal conditions were determined based on the monosaccharides (i.e. glucose, galactose and mannose) and the polysaccharides in different EPS fractions from two activated sludges. The results showed that NaSO was the best reagent for chemical pretreatment due to redox reaction, high selectivity and colorless oxidation product, and the others were not suitable as pretreatment reagents mainly since the reaction products affect the final spectral analysis. Besides, the optimal NaSO concentration for eliminating the impact of PS was 150 mmol/L, and the relative deviation of measurement is less than 5% if the PS concentration was on more than 100 mmol/L, regardless of the kinds of carbohydrates. Compared with the anthrone-sulfuric acid method and the sulfuric method, the improved phenol-sulfuric acid method has a great advantage for determining the carbohydrate concentration in the presence of PS.

摘要

基于过硫酸盐的高级氧化工艺 (AOPs) 在污泥预处理方面受到了广泛关注。过硫酸盐 (PS) 是一种持久性氧化剂,污泥中过量的过硫酸盐会影响传统苯酚-硫酸法测定碳水化合物的结果。本研究开发了一种在过硫酸盐存在下测定碳水化合物的改良苯酚-硫酸法,并在常规测定前引入了一个关键步骤,借助化学预处理。从四种还原剂(即 NaS、KI、NaSO 和 NaSO)和两种自由基清除剂(即苯酚和苯甲酸)中筛选出最佳试剂,并根据两种活性污泥中不同 EPS 组分中的单糖(即葡萄糖、半乳糖和甘露糖)和多糖确定最佳条件。结果表明,由于氧化还原反应、高选择性和无色氧化产物,NaSO 是最佳的化学预处理试剂,而其他试剂则不适合作为预处理试剂,主要是因为反应产物会影响最终的光谱分析。此外,如果 PS 浓度高于 100mmol/L,消除 PS 影响的最佳 NaSO 浓度为 150mmol/L,测量的相对偏差小于 5%,而与碳水化合物的种类无关。与蒽酮-硫酸法和硫酸法相比,改良苯酚-硫酸法在测定 PS 存在下的碳水化合物浓度方面具有很大的优势。

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