光谱学与光谱分析, 2017, 37 (5): 1656, 网络出版: 2017-06-20  

电化学处理油田污水中微量H2O2的光谱分析

Spectrum Analysis of Trace Hydrogen Peroxide in Electrochemical Process
作者单位
1 长江大学化学与环境工程学院 湖北 荆州 434023
2 海洋石油高效开发国家重点实验室, 北京 100027
3 中海油研究总院, 北京 100027
摘要
电化学去除污水COD是一种高效绿色快速的方法。 在电化学法处理某油田含聚采油污水中, 产生活性中间体H2O2能间接氧化去除COD; 而电化学过程中产生的H2O2是很微量的, 常规方法难以检测和准确定量, 需要采用高灵敏度的测定方法检测H2O2, 用以指导电化学处理工艺控制过程; 而Ti(Ⅳ)与5-Br-PADAP(B)及H2O2在pH 1~1.5时能形成稳定的三元络合物Ti(Ⅳ)-B-H2O2, 该三元显色体系在561 nm附近有明显的吸收峰, 且H2O2浓度在0.2~10 μmol·L-1的范围内遵从Beer-Lambert Law, 因此可建立起用分光光度法检测电化学法处理污水过程中微量活性中间体H2O2的方法。 本文分别研究了5-Br-PADAP(B), Ti(Ⅳ)-B二元络合物, Ti(Ⅳ)-B-H2O2三元络合物体系的紫外光谱图, 提出了测定微量H2O2的方法。 该研究创新点在于: 通过紫外光谱图研究了影响Ti(Ⅳ)-B-H2O2三元络合物体系生成且稳定存在的因素是: 试剂加入顺序、 pH值、 无水乙醇用量、 加热温度及时间、 Ti(Ⅳ)-B配比及其用量等, 进而确定了准确检测和定量微量H2O2的实验条件为: 体系pH 1.0~1.5, 无水乙醇加量50%, 在50 ℃水浴锅中加热20 min, Ti(Ⅳ)与B溶液按等摩尔比混合, 药剂加入顺序为: H2O2溶液2 mL, 无水乙醇3 mL, 0.32 mol·L-1的HCL溶液1 mL, pH 1.5的缓冲溶液2 mL, Ti(Ⅳ)-B混合液2 mL, 用0.32 mol·L-1的HCL溶液定容至刻线。 该方法简便、 快速、 重现性好、 费用低, 灵敏度高, 在电化学处理污水过程的实际检测中获得了满意效果。
Abstract
Electrochemistry is an efficient, fast and green method for the COD removal of sewage. The electrochemical treatment process of sewage containing polymer in an oilfield produces some reactive intermediates such as H2O2 which can remove COD by indirect oxidation. It is very difficult to detect accurately and quantitatively with general methods because of the trace H2O2 in the process of electrochemistry. Thus, we need a method of high-sensitivity to measure the amount of H2O2 to guide the control process of electrochemical treatment; Ti and 5-Br-PADAP with H2O2 can form a stable colored ternary complex at pH 1~1.5, and there is an obvious absorption peak of this ternary color system at about 561 nm. Within the range of 02~10 μmol·L-1 H2O2 and sticking to Beer-Lambert Law, a method of spectrophotometry can be established for determination of trace reactive intermediates about H2O2 in the process of electrochemical treatment of sewage. The UV spectra of 5-Br-PADAP(B), binary complexes Ti(Ⅳ)-B and ternary complexes of Ti(Ⅳ)-B-H2O2 is studied and the determination method of trace H2O2 is proposed in this paper. Here are innovations of this paper: The factors of influencing the formation and stability of ternary complex system of Ti(Ⅳ)-B-H2O2 are the order of adding reagents, pH, the amount of anhydrous ethanol, heating temperature and time and the ratio and amount of Ti(Ⅳ)-B with UV spectroscopy. The experimental conditions for the accurate detection and quantification of trace H2O2 are obtained: pH 1.0~1.5, 50% of ethanol, heated in water bath at 50 ℃ about 20min, Ti(Ⅳ) and B solution mixed at the equal molar ratio, The order of adding reagents: 2 mL of various concentrations of these standards H2O2 solution, 3 mL of anhydrous alcohol, 1 mL of 0.32 mol·L-1 HCL, 2 mL of pH 1.5 HCl-KCl buffer solution, 2 mL of Ti(Ⅳ)-B solution to a 10 mL volumetric flask, and dilute with 0.32 mol·L-1 HCL solution to the mark line of volume. The method is easy, rapid, reproducible, cheap and high sensitive, and it obtains satisfying results in practical applications.

刘倩, 陈文娟, 靖波, 张健, 杨梦颖, 陈武, 尹先清. 电化学处理油田污水中微量H2O2的光谱分析[J]. 光谱学与光谱分析, 2017, 37(5): 1656. LIU Qian, CHEN Wen-juan, JING Bo, ZHANG Jian, YANG Meng-ying, CHEN Wu, YIN Xian-qing. Spectrum Analysis of Trace Hydrogen Peroxide in Electrochemical Process[J]. Spectroscopy and Spectral Analysis, 2017, 37(5): 1656.

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