高效液相色谱法检测蒽醌法生产过氧化氢工作液中有效蒽醌  

Determination of the Effective Anthraquinones in Hydrogen Peroxide Working Fluid Produced by Anthraquinone Process with HPLC

作　　者：潘景凤 胡芳 刘清海 PAN Jingfeng;HU Fang;LIU Qinghai(Jiaozuo Coal Industry Kaiyuan Chemical Limited Liability Company,Jiaozuo 454191,China;Henan Billions Advanced Material Co.,Ltd.,Jiaozuo 454191,China)

机构地区：[1]焦作煤业(集团)开元化工有限责任公司,河南焦作454191 [2]河南佰利联新材料有限公司,河南焦作454191

出　　处：《化学与粘合》2024年第2期206-210,共5页Chemistry and Adhesion

基　　金：龙佰集团工程项目:20万吨/年双氧水项目(编号:010001)。

摘　　要：根据蒽醌法生产过氧化氢中控质量控制的需求,建立了一种高效液相色谱法检测蒽醌法生产过氧化氢工作液中有效蒽醌的方法。采用Acclaim TM 120 C18 (150 mm×4.6 mm,5μm)液相色谱柱,40℃恒定柱温,流动相为75%色谱甲醇水溶液,流动相流速为1 m L/min,紫外检测器,检测波长254 nm,进样量20μL的检测条件,先根据2-乙基蒽醌(EAQ)、2-乙基四氢蒽醌(THEAQ)单标的保留时间进行定性分析,再采用标准曲线法对工作液中EAQ和THEAQ进行定量分析。结果表明:高效液相色谱法可准确测定蒽醌法生产过氧化氢工作液中2种有效蒽醌的质量浓度,EAQ和THEAQ的保留时间分别为8.275 min和11.080 min,经检测,分析2022年5月28日新配制工作液中EAQ、THEAQ分别为143.64和0.86 g/L,10月21日循环工作液中EAQ、THEAQ分别为123.94和27.74 g/L,该方法操作简单、相对标准偏差在0.02%~0.18%之间、加标回收率在98.59%~1 01.05%之间,可作为蒽醌法生产过氧化氢中间过程质量控制。A method for the determination of the effective anthraquinones in hydrogen peroxide working fluid produced by anthraquinone process with high performance liquid chromatography(HPLC) has been developed according to demand of the central control QC.The detecting conditions are showed as follows:the AcclaimTM 120 C18(150 mm ×4.6 mm,5 μm)liquid chromatographic column is adopted at 40 ℃ constant temperature,the75% chromatographic methanol aqueous solution is used as the mobile phase and its flow rate is 1 mL/min,the ultraviolet detector with a detection wavelength of 254 nm is used and the injection volume is 20 μL.Firstly,the qualitative analysis is carried according to the retention time of 2-ethylanthraquinone(EAQ) and 2-ethyltetrahydroanthraquinone(THEAQ),and then the standard curve method is applied to the quantitative analysis of the EAQ and THEAQ in working fluid.The results show that the mass concentration of two kinds of effective anthraquinones in the hydrogen peroxide working fluid produced by anthraquinone process can be accurately determined by HPLC,the retention time of EAQ and THEAQ is 8.275 min and11.080 min respectively;after testing,the mass concentration of EAQ and THEAQ is 143.64 and 0.86 g/L in the new prepared working fluid sample on May 28,2022,and the mass concentration of EAQ and THEAQ is 123.94 and 27.74 g/L in the circulated working fluid sample on October 21,2022 from some company.The relative standard deviation and recovery rate of this method is in the range of 0.02%-0.18% and 98.59%-101.05%respectively,and this method is simple operation which can be used for monitoring the intermediate process quality of hydrogen peroxide produced by anthraquinone process.

关 键 词：高效液相色谱法 紫外检测器 保留时间 定量分析 2-乙基蒽醌 2-乙基四氢蒽醌 

分 类 号：O657.7[理学—分析化学]