钴镍前驱体纳米材料电化学检测过氧化氢

刘梅¹，孙晓红¹，杨池²，程旺兴^*1

（1.安徽中医药大学 药学院，安徽 合肥  230012；2.南京信息工程大学 应用气象学，江苏 南京  210044）

摘要：通过一种简便、绿色的无模板的沉淀法合成钴镍微纳米复合结构，并对该材料进行场发射扫描电子显微镜(FESEM)，透射电子显微镜(TEM)和能量色谱X射线分析(EDX)表征，结果表明该材料为中空结构，并具有呈针状的纳米线和多孔的特征；同时该材料有较高的比表面积71.95 m²/g。将该钴镍微纳米复合结构前驱体材料用于溶液中过氧化氢的电化学检测，结果显示电流峰值和过氧化氢浓度(c)之间呈良好线性关系(系数R = 0.998)，检测限为3.2 μmol/L(信噪比=3)，实验结果表明所合成的钴镍微纳米复合结构前驱体材料具有优良的电化学性能，对过氧化氢的检测具有高灵敏性，可应用于过氧化氢的检测。

关键词：钴镍; 前驱体; 电化学; 过氧化氢; 中空结构; 材料

中图分类号：Z6      文献标识码：A      文章编号：0258-3283（2020）--

Electrochemical Detection of Hydrogen Peroxide by Cobalt-Nickel Precursor Nanomaterials LIU Mei¹, SUN Xiao-hong¹, YANG Chi², CHENG Wang-xing^*1 (1.School of Pharmacy, Anhui University of  Chinese Medicine, Hefei 230012, China; 2.Applied Meteorology, Nanjing University of Information Science and Technology, Nanjing 210044, China), Huaxue Shiji, 2020, 42(5), ～

Abstract: The cobalt-nickel micro-nano composite precursor material was synthesized by a simple，green template-free precipitation method，and the material was conformed by field emission scanning electron microscopy(FESEM)，transmission electron microscopy (TEM) and energy chromatography X-ray analysis (EDX). The material has a hollow structure and nanowires and porous features with a sharp tip shape; It has a high specific surface area of 71.95 m²·g^-1. The cobalt-nickel micro-nano composite precursor material was used for the electrochemical detection of hydrogen peroxide. The good linear relationship between the current peak and the hydrogen peroxide concentration (C) (coefficient R=0.998)，detection limit: 3.2 μmol/L (S/N= 3). The synthesized cobalt-nickel micro-nano composite precursor material has excellent electrochemical performance and high sensitivity to the detection of hydrogen peroxide，which can be applied to the detection of hydrogen peroxide.

Key words: cobalt nickel; precursor; electrochemistry; hydrogen peroxide; hollow structure; materia

引用本文：刘梅, 孙晓红, 杨池, 等. 钴镍前驱体纳米材料电化学检测过氧化氢[J]. 化学试剂, 2020, 42(5): 473-477.

原子转移自由基聚合法合成7-乙酰氧基-4-甲基香豆素分子印迹聚合物及吸附性能研究

宋立新¹，黄志鹏²，许铭华，芮超凡²，何娟^*2

（1. 河南水利与环境职业学院 环境工程系，河南 郑州450001；2. 河南工业大学 化学化工学院，河南 郑州450001）

摘要：以黄曲霉毒素结构类似物7-乙酰氧基-4-甲基香豆素为替代模板，甲基丙烯酸缩水甘油酯为单体，氯化苄为引发剂，氯化亚铜为过渡金属卤化物，2，2-联吡啶为配体，利用原子转移自由基聚合法合成分子印迹聚合物，通过一系列实验对其合成条件进行优化；对聚合物进行表征，并对其吸附黄曲霉毒素的能力进行研究。通过单因素实验和正交实验，得到最佳的合成条件：模板与功能单体的物质的量比为1：80，引发剂的量为1.5%（单体的质量百分比），反应温度为60℃，过渡金属卤化物与配体的物质的量比为1：3。在最优的合成条件合成分子印迹聚合物，并将其作为填充材料制作固相萃取柱，用于选择性分离样品中的黄曲霉毒素，并与商品柱对比。

关键词：分子印迹聚合物；原子转移自由基聚合；7-乙酰氧基-4-甲基香豆素；黄曲霉毒素；自制固相萃取柱；

中图分类号：O652.62  文献标识码：A     文章编号：0258-3283（2020）--

Synthesis and Adsorption Properties of 7-Acetoxy-4-methylcoumarin Molecularly Imprinted Polymers by Atomic Transfer Radical Polymerization SONG Li-xin¹, HUANG Zhi-peng², RUI Chao-fan², HE Juan^*2(1. Henan Vocational College of Water Conservancy and Environment,Department of Environmental Engineering, Zhengzhou 450001,China;2. Henan University of Technology,School of Chemistry and Chemical Engineering, Zhengzhou 450001,China), Huaxue Shiji, 2020, 42(5), ～

Abstract：With aflatoxin structure analogues 7 - acetoxyl group - 4 - methyl coumarin as alternative templates, methyl glycidyl ester of acrylic acid monomer and benzyl chloride as the initiator, cuprous chloride as a transition metal halide, 2, 2 - pyridine as ligand, using atom transfer radical polymerization to synthesize molecularly imprinted polymers, through a series of experiments to optimize the synthesis conditions. The polymer was characterized and its ability to adsorb aflatoxin was investigated. Based on single factor experiment and orthogonal experiment, the best synthesis conditions were obtained: template: molar ratio of functional monomer was 1:80, the amount of initiator was 1.5% (monomer mass percentage), reaction temperature was 60℃, transition metal halide: ligand was 1:3.Molecularly imprinted polymers were synthesized under optimal conditions and used as fillers to prepare solid phase extraction columns for selective separation of aflatoxin from samples and comparison with commercial columns.

Keywords: molecular imprinting technique; atom transfer radical polymerization; 7-acetoxy-4-methylcoumarin; aflatoxins; self-made SPE cartridge

引用本文：宋立新, 黄志鹏, 许铭华, 等. 原子转移自由基聚合法合成7-乙酰氧基-4-甲基香豆素分子印迹聚合物及吸附性能研究[J]. 化学试剂, 2020, 42(5):478-482.

5-苯基-2-邻甲苯-2H-1, 2, 3-三氮唑-4-羧酸乙酯的结构性质及其罗丹明衍生物检测汞离子

何文英^*a，廖元淏^a，丁国华^b,李建玲^a，刘炜^a，刘艳萍^a，冯华杰^a

（海南师范大学 a.热带药用植物化学教育部重点实验室，b. 生命科学学院, 海南 海口  571158）

摘要：应用计算化学的方法研究了5-苯基-2-邻甲苯-2H-1, 2, 3-三氮唑-4-羧酸乙酯（EPTC）的结构及理论光谱，并与实验测定结果相比较；再将EPTC与罗丹明B合成了新化合物REPTC，采用紫外吸收和荧光光谱法测定了REPTC与15种金属离子的相互作用。实验结果表明：在pH 7.4的DMF（N，N-二甲基甲酰胺）-水溶液中，REPTC在2.33×10^-5 ～ 4.00×10^-5 mol/L 的浓度范围内，它仅对Hg²⁺有高选择性的响应，表现为在577 nm 出现一个新的发射峰且强度显著增大，同时肉眼可观察到明显的颜色变化。结合电喷雾质谱及理论计算表明Hg²⁺的存在使得REPTC分子中罗丹明的螺环结构从闭环转为开环，可与Hg²⁺可形成物质的量比为1: 2 的新配合物。荧光成像实验表明：REPTC可成功标记HeLa细胞中的Hg²⁺，进而可开发用于生物体系中Hg²⁺的测定。

关键词：5-苯基-2-邻甲苯-2H-1, 2, 3-三氮唑-4-羧酸乙酯；结构性质；合成；Hg²⁺离子；细胞成像

中图分类号：O657      文献标识码：A         文章编号：0258-3283（2020）--

Structural Properties of Ethyl 5-Phenyl-2-(o-tolyl)-2H-1, 2, 3-triazole-4-carboxylate and its Appended Rhodamine for Detection of Hg²⁺ HE Wen-ying^*a, LIAO Yuan-hao^a, DING Guo-hua^b, LI Jian-ling^a, LIU Wei^a, LIU Yan-ping^a, FENG Hua-jie^a (a. Key Laboratory of Tropical Medicinal Plant Chemistry of Ministry of Education; b. College of Life and Sciences, Hainan Normal University, Haikou 571158, Hainan, China), Huaxue Shiji, 2020, 42(5), ～

Abstract：A newly synthesized compound，ethyl 5-phenyl-2-(o-tolyl)-2H-1,2,3- triazole-4-carboxylate (EPTC) has  been used to investigate its structural properties and theoretical spectrum which is consistent with the experimental spectrum. Then EPTC was successfully designed and synthesized to a new rhodamine B derivative REPTC confirmed by ¹HNMR, ¹³CNMR, and HRMS. The spectral sensing behaviors of REPTC toward 15 kinds of metal ions were determined by fluorescence spectra and UV absorption spectra. The probe REPTC shows high selectivity toward Hg²⁺ ions in DMF-H₂O between a range of REPTC concentration 2.33×10^-5 ～4.00×10^-5mol/L under physiological conditions (pH 7.4). A new emission peak appeared at 577 nm and enhanced significantly along with naked-eye sensitive color changes, which spirolactamring moiety of rhodamine was converted to the open-ring form in the presence of Hg²⁺ and formed the new complex as 1: 2 molar ratio. The fluorescence imaging results of Hg²⁺ in HeLa cell demonstrated that the probe was successfully labeled and it could be further exploited and used in biological systems.

Key words: ethyl 5-phenyl -2-(o-tolyl)-2H-1,2,3-triazole-4-carboxylate, structural properties, synthesis, Hg²⁺, cell imaging.

引用本文：何文英，廖元淏，丁国华，等. 5-苯基-2-邻甲苯-2H-1, 2, 3-三氮唑-4-羧酸乙酯的结构性质及其罗丹明衍生物检测汞离子[J]. 化学试剂，2020，42（5）：483-492.

邻氨基苯甲酰胺衍生物的合成及其鲍曼不动杆菌生物膜抑制活性测试

薛维娜^{1a, 2}，杨果^1b，程铖^1b，李应贤^1b，杨元勇^*1b

（1. 贵州医科大学 a. 医药卫生管理学院，b. 药学院，贵州 贵阳  550025；

2. 中国海洋大学 医药学院，山东 青岛  266100）

摘要：研究显示，鲍曼不动杆菌的院内持续传播与反复发作与生物膜形成密切相关。生物膜的形成受群体行为模式调控，研究发现通过添加自诱导剂类似物，可以竞争性抑制细菌自诱导体的作用从而抑制生物膜的生成。本文以邻氨基苯甲酰胺为母体结构，合成出20个化合物，并测试其对鲍曼不动杆菌生物膜的抑制活性。研究发现在50 μm的抑制浓度下，大部分化合物均显示出对鲍曼不动杆菌一定的生物膜抑制活性，其中化合物N，N-二苄基-2-苄基氨基苯甲酰胺、2-苄基氨基-N-氨基甲酰胺、2-苄基氨基-N-（4-羟基苯基）苯甲酰胺在50 μm条件下生物膜抑制率超过30%，通过细菌MIC试验，证明了化合物对细菌并无杀灭作用而是抑制了细菌生物膜。

关键词：鲍曼不动杆菌；生物膜抑制剂；群体感应；邻氨基苯甲酰胺

中图分类号：O625.53      文献标识码：A      文章编号：0258-3283（2020）--

Synthesis and Biofilm Inhibition Activity Test of o-Aminobenzamide Derivatives against Acinetobacter Baumannii XUE Wei-na^{1a, 2}, YANG Guo^1b, CHENG Cheng^1b, LI Ying-xian^1b, YANG Yuan-yong^*1b (1a. School of Medicine and Health Management; 1b. School of pharmacy, Guizhou Medical University, Guiyang 550025; 2. School of Medicine and Pharmacy, Ocean University of China, Qingdao 266100, China), Huaxue Shiji, 2020, 42(5), ～

Abstract: The work has shown that the persistent transmission and recurrence of Acinetobacter baumannii infection in hospital is closely related to biofilm formation. The formation of biofilm is controlled by quorum sensing. The formation of biofilm can be inhibited by adding auto-inducer analogues, which can competitively inhibit the effect auto-inducer. 26 Compounds were synthesized using o-aminobenzamide as the parent structure, and their inhibitory activities on Acinetobacter baumannii biofilm were tested. The most of the compounds exhibited certain biofilm inhibitory activity at the inhibitory concentration of 50 μm. Among them, compounds N, N-dibenzyl-2-(benzylamino) benzamide, 2-(benzylamino)-N- (diaminomethylene)benzamide and 2-(benzylamino)-N- (4-hydroxyphenyl) benzamide exhibited more than 30% biofilm inhibitory activity at the inhibitory concentration of 50 μm. The inhibitory effect of the synthetic compounds on biofilm was further illustrated by the MIC test, and the results shows that the compounds inhibit the biofilm formation instead of kill the bacteria.

Key words：Acinetobacter Baumannii; biofilm inhibitors; quorum sensing; o-aminobenzamide

引用本文：薛维娜, 杨果, 程铖, 等. 邻氨基苯甲酰胺衍生物的合成及其鲍曼不动杆菌生物膜抑制活性测试[J]. 化学试剂, 2020, 42(5): 493-499.

4-烯丙氧基萘酰亚胺的合成与光学性质研究

卜明^a，王海君^*a，马玉坤^b，王静^a，李爽^a，陈颂^a，刘磊^a，孙靖文^a

（齐齐哈尔医学院 a.药学院，b.医药科学研究院，黑龙江 齐齐哈尔  161006）

摘要：以4-溴-1,8-萘二甲酸酐为原料，与正丁胺反应生成4-溴萘酰亚胺，再与甲醇钠在硫酸铜的作用下反应，生成4-甲氧基萘酰亚胺，经HI作用，脱去保护得到4-羟基萘酰亚胺，最后与3-溴丙烯反应合成了4-烯丙氧基萘酰亚胺。结构经¹HNMR、¹³CNMR、MS等加以表征，并对其吸收与荧光性质进行测定。结果表明，4-烯丙氧基萘酰亚胺收率为78%，紫外吸收波长为370 nm，荧光发射峰波长为450 nm。对HepG2细胞进行染色，激发后细胞呈现出强烈的蓝色荧光，成功实现细胞内荧光成像，具有良好的生物应用前景。

关键词：合成；1,8-萘酰亚胺；烯丙氧基；结构表征；荧光；细胞成像

中图分类号：O626.2      文献标识码：A      文章编号：0258-3283（2020）--

Synthesis and Spectral Properties of 4-Allyloxy Naphthalimide BU Ming^a, WANG Hai-jun^*a, MA Yu-kun^b, WANG Jing^a, LI Shuang^a, CHEN Song^a, LIU-Lei^a, SUN Jing-wen^a (a. College of Pharmacy, b. Research Institute of Medicine & Pharmacy, Qiqihar Medical University, Qiqihar 161006, China), Huaxue Shiji, 2020, 42(5), ～

Abstract：4-Bromo-naphthalimide was obtained by condensation of 4-bromo-1, 8-naphthalene dimethyl anhydride and n-butylamine, and then reacted with sodium methoxide in the presence of copper sulfate to generate 4-methoxyl naphthalimide. 4-Hydroxyl naphthalimide was obtained by the removal of protective group by hydroiodate. Finally, 4-hydroxyl naphthalimide was synthesized by reaction of 4-hydroxynaphthalimide and with 3-bromo-propylene. The structures were confirmed by ¹HNMR, ¹³CNMR and MS, the absorption and fluorescence properties were determined. The yield of 4-aloxy naphthalimide was 78%, the absorption wavelength was 370 nm, and the fluorescence emission peak wavelength was 450 nm. HepG2 cells were stained and stimulated to show a strong blue fluorescence. The compound successfully realized the fluorescence imaging in cells, which has a good biological application prospect.

Key words：synthesis; 1,8-naphthalimide; allyloxy; structural characteristics; fluorescence; cell imaging

引用本文：卜明，王海君，马玉坤，等. 4-烯丙氧基萘酰亚胺的合成与光学性质研究[J].化学试剂，2020，42（5）：500-504.

电化学整流研究及应用进展

常凤霞¹，朱志伟^*2

（1. 西南民族大学 化学与环境保护工程学院，四川 成都 610041；

2. 北京大学 化学与分子工程学院，北京100871）

摘要：细胞膜上的离子通道是细胞与周围环境进行物质交换的重要途径，而对离子通道的“掌控”起决定性作用的正是电化学整流。电化学整流的研究对于深入理解细胞膜离子通道的作用机理，以及仿生纳米器件的构筑具有非常重要的科学意义和应用价值。从体系构建到机理推导直至应用这几个方面对国内外课题组有关电化学整流的研究进行了综述，并展望了其未来的发展方向。

关键词：电化学整流；离子电流整流；纳米孔；微米通道；综述

Progress and Application of Ionic Current Rectification CHANG Feng-xia¹, ZHU Zhi-wei^*2 (1. College of Chemistry and Environmental Protection Engineering, Southwest Minzu University, Chengdu 610041, China; 2. College of Chemistry and Molecular Engineering, Peking University, Beijing 100871, China), HuaxueShiji, 2020, 42(6)

Abstract: Ion channel on the cell membrane is a key path through which cell exchange materials with the surrounding environment, and it is ionic current rectification (ICR) that plays a decisive role in the precise control of ion channel. The study on ICR has very important scientific significance and application value for both understanding of the mechanism of membrane ion channel and the fabrication of bionic nano-devices. The research on ionic current rectification at home and abroad is reviewed from the aspects of system construction, mechanism derivation and application, and its future development direction is prospected.

Key word:electrochemicalrectification;ionic current rectification; nanopore; micro channel; review

引用本文：常凤霞, 朱志伟. 电化学整流研究及应用进展[J]. 化学试剂, 2020, 42(5): 505-513.

铝合金气瓶表面处理方法概述

赵鑫蕊，毕哲^*，贡鸣，韩笑

(中国计量科学研究院，北京  100013)

摘要：气体标准物质是一种带特性量值的气态物质，是气体物质分析、量值传递的标准。气体标准物质通常用与目标气体组分不发生反应的气瓶存储，合适的气瓶内壁钝化处理方式对保持气体标准物质量值稳定意义重大。近年来高吸附和易反应气体标准物质的需求对气瓶的惰性处理提出了较高的要求。铝合金气瓶是目前应用最广泛的标准气体盛装气瓶之一，目标气体组分在铝合金气瓶内壁的吸附、反应、凝结等物理化学过程有待深入研究，这些过程对标准物质量值稳定性的影响亟需深入考察。目前文献报道了包括化学转化、阳极氧化、硅烷化处理等多种表面处理方式，结合这些研究成果，探索既满足标准气体使用要求，又普遍适用、低能耗、环境友好的铝合金气瓶内壁处理工艺，成为接下来研究的重点。

关键词：气体标准物质；铝合金；吸附；阳极氧化；硅烷化

中图分类号：TB9      文献标识码：A      文章编号：0258-3283（2020）--    

Overview of Aluminium Alloy Gas Cylinders Surface Treatment Methods ZHAO Xin Rui, BI Zhe^*, GONG Ming, HAN Xiao (National Institute of Metrology, Beijing 100013, China), Huaxue Shiji, 2020, 42(5), ～

Abstract： Gas standard materials are gaseous substances with characteristic values, which are considered as the standard for gas analysis and calibration. They are usually kept in gas cylinders that don’t react with the target gas components. It is of great significance to explore appropriate inner surface treatment methods in order to maintain the stability of the magnitudes of gas standard materials. In recent years, the demand for gas standard materials which are reactive with high adsorption capacity puts forward higher requirements for the inert treatment of gas cylinders. Aluminum alloy gas cylinders are one of the most widely used types of gas cylinders to package standard gases. However, adsorption, reaction and condensation of these target components may occur on the inner surface of cylinders. The mechanism of these processes and the impact on the stability of reference value are urgently needed to be further understood. A variety of surface treatment methods have been reported, such as chemical conversion, anodization, salinization and so on. The ideal treatment process should meet the inert requirements, less energy consuming, widely applicable and environment friendly. How to make use of existing research results to make the ideal process become a reality is the focus of the future study.

Key words：gas standard material; aluminium alloy; adsorption; anodizing; silanization

引用本文：赵鑫蕊，毕哲，贡鸣，等. 铝合金气瓶表面处理方法概述[J].化学试剂，2020，42（5）：514-521.

聚吡咯氨气传感器快速检测变形杆菌

张玲玲，孙芬芳，周霞，王建化^*

（青岛农业大学 海都学院，山东莱阳265200）

摘要：首次提出了一种快速检测变形杆菌的聚吡咯氨气传感器。传感器采用聚吡咯作为导电电极，代替金属电极，克服了检测系统的背景电导率限制。即使在二氧化碳气体存在下，它也能响应氨浓度的变化，可用于定量检测代谢过程中释放氨的变形杆菌。采用该方法检测普通变形杆菌，普通变形杆菌初始浓度的对数在0.9～8.5的范围内与频率检测时间呈线性关系。与串联压电石英晶体（SPQC）传感器相比，系统具有更高的灵敏度，降低了对培养基的要求。

关键词：聚吡咯；氨气传感器；检测系统；变形杆菌；背景电导率

中图分类号：O657.1      文献标识码：A      文章编号：0258-3283（2020）--

PolypyrroleAmmonia Sensor for the Detection of Bacterium VulgareZHANG Ling-ling, SUN Fen-fang, ZHOU Xia, WANG Jian-hu^* (Haidu College, Qingdao Agricultural University ,Laiyang 265200, China), Huaxue Shiji, 2020, 42(5), ～

Abstract: A new polypyrrole system was proposed to detect bacterium vulgare. In new system, polypyrrolewas used as conduct electrode instead of metal electrode, it overcame the background conductivity limit of detection system. Polypyrrole ammonia sensor can response the concentration changes of ammonia even in the presence of carbon dioxide. Based on this response, it can be used to detect bacterium vulgare which would release ammonia during its metabolism process. Proteus vulgaris was detected using polypyrrole ammoniasensor. The Frequency detection time and the logarithm of the initial concentration of Proteus vulgarishad a linear relationship in the range of 0.9～8.5. Compared with series piezoelectric quartz crystal (SPQC) sensor, polypyrrole ammonia sensor was more sensitive and able to reduce the requirement of culture medium.

Key words:polypyrrole; ammonia sensor; detection system; Bacterium vulgare; background conductivity

引用本文：张玲玲, 孙芳芳, 周霞, 等. 聚吡咯氨气传感器快速检测变形杆菌[J]. 化学试剂, 2020, 42(5): 522-526.

模拟汽油中痕量磷元素的ICP-OES和ICP-MS方法测定

任丹华^{1, 2}，张艾蕊¹，范冰奇^{1, 2}，王梅玲¹，韩艳祥^{1, 2}，张鑫²，王海^*1

（1.   中国计量科学研究院，北京  1000291；2.中国石油大学（北京） 化学工程与环境学院，北京  102249）

摘要：采用浓硝酸结合过氧化氢的酸消解体系对模拟汽油样品进行了微波消解前处理，建立了电感耦合等离子体发射光谱（ICP-OES）和电感耦合等离子体质谱（ICP-MS）准确测量模拟汽油中痕量磷元素的分析方法，整个过程安全、高效、无污染。结果表明，ICP-OES和ICP-MS测量痕量磷元素（30～400 μg/kg）具有良好的线性，相关系数优于0.9999，方法检出限为2～3 μg/kg；ICP-OES和ICP-MS测得模拟汽油中痕量磷元素的含量分别为0.4507、0.444 mg/kg、加标回收率为98%～107%，两种方法测量结果具有良好的一致性。以ICP-MS测定方法为例，评定了模拟汽油中痕量磷元素的测量结果不确定度（2.6%，k=2），测量重复性和工作标准溶液配制是测量结果不确定度的两个主要来源。所建立的模拟汽油中痕量磷含量准确测量方法为进一步的汽油中痕量磷元素标准物质研制积累了良好的技术基础。

关键词：痕量磷；模拟汽油；ICP-OES；ICP-MS；不确定度；微波消解

中图分类号：TE622.1      文献标识码：A     文章编号：0258-3283（2020）--

Determination of Trace Phosphorous in Simulated Gasoline Using ICP-OES and ICP-MS Methods REN Dan-hua^{1, 2}, ZHANG Ai-rui¹, Fan Bing-qi^1,2, WANG Mei-ling¹, Han Yan-xiang^1,2, ZHANG Xin², WANG Hai^*1 (1. National Institute of Metrology, Beijing 100029; 2. China University of Petroleum(Beijing), College of Chemical Engineering and Environment, Beijing 102249) Huaxue Shiji, 2020, 42(5), ～

Abstract: The simulated gasoline sample was pre-treated with concentrated nitric acid and hydrogen peroxide by microwave digestion and the trace phosphorous element contained in the digested solutions was then analyzed by inductively coupled plasma optical emission spectrometry (ICP-OES) and inductively coupled plasma mass spectrometry (ICP-MS) methods. The whole process was safe and efficient without any contaminations. The analytical results showed that the content of phosphorus had a good linear relationship (the correlation coefficient better than 0.9999) in the range of 30 to 400 μg/kg for ICP-OES and ICP-MS measurement with the limit of detection (LOD) between 2 μg/kg and 3 μg/kg. The analytical results of ICP-OES and ICP-MS were 0.451 mg/kg and 0.444 mg/kg, respectively and the recovery of standard addition was in the range of 98-107%. The measured contents of phosphorus in simulated gasoline sample showed a good consistency between ICP-OES and ICP-MS techniques. The expanded uncertainty (2.6%, k=2) of phosphorus content in simulated gasoline was evaluated when ICP-MS method was exampled and its uncertainty contributions were mainly from the measurement repeatability and the working standard solutions. This work has established a good technical foundation for the development of certified reference materials for trace phosphorus in gasoline in the future.

Key words: trace phosphorus; simulated gasoline; ICP-OES; ICP-MS; uncertainty; microwave digestion

引用本文：任丹华, 张艾蕊, 范冰奇, 等. 模拟汽油中痕量磷元素的ICP-OES和ICP-MS方法测定[J]. 化学试剂, 2020, 42(5): 527-532.

超高效液相色谱-串联质谱法测定泡泡液玩具中异噻唑啉酮类杀菌防腐剂

刘萍^1*，臧珊珊²

(1. 台州科技职业学院 农业与生物工程学院，浙江 台州 318020；2. 中国科学院生物物理研究所，北京 100101）

摘要：建立了超高效液相色谱-串联质谱（UPLC-MS/MS）法同时测定泡泡液中2-甲基-4-异噻唑啉-3-酮（MI）、5-氯-2-甲基-4-异噻唑啉-3-酮（CMI）和1,2-苯并异噻唑啉-3-酮（BIT）的含量。考察了不同提取溶剂和提取时间对MI、CMI和BIT的提取，以及不同流动相和不同色谱柱对MI、CMI和BIT的色谱分离效果。泡泡液样品经20%甲醇水溶液超声提取10 min，过滤膜后进样。以5 mmol/L乙酸铵水和5 mmol/L乙酸铵甲醇为流动相梯度洗脱，MI、CMI和BIT在C₈柱上4.5 min内到达到基线分离。MI、CMI和BIT分别在1～20、3～60和5～100 μg/L范围内，相关系数r²≥0.9992；信噪比法获得的MI、CMI和BIT定量限范围为0.06～0.1 mg/kg；MI、CMI和BIT在泡泡液阳性样品中3水平加标平均回收率范围为86.4%～108%，相对标准偏差范围为1.2%～4.5%。方法快速、简便、灵敏度高、重复性好，准确度高，定量限也满足欧盟指令中MI、CMI和BIT的限量要求，具有较好的实用性，并已用于实际样品的检测。

关键词：UPLC-MS/MS；泡泡液；异噻唑啉酮；杀菌；防腐剂

中图分类号：O658      文献标识码：A      文章编号：0258-3283（2020）--

Determination of Isothiazolinone Bactericides and Preservatives in Bubble Liquid Products by Ultra High Performance Liquid Chromatography-tandem Mass Spectrometry LIU Ping*¹, ZANG Shan-shan²(1. College of Agriculture and Biotechnology, Taizhou Vocational College of Science & Technology, Taizhou 318020, China; 2. Institute of Biophysics, Chinese Academy of Sciences, Beijing 100101, China), Huaxue Shiji, 2020, 42(5), ～

Abstract：An ultra high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was established to determine the contents of 2-methyl-4-isothiazolin-3-one (MI), 5-chloro-2-methyl-4- isothiazolin-3-one (CMI) and 1,2-benzisothiazol 3-one (BIT) in bubble liquid products. The effects of different extraction solvents and extraction time were investigated, and different mobile phase components and chromatographic columns were also compared. The optimized sample pretreatment procedure was that the bubble liquid samples were extracted with 20% ethanol aqueous solution by sonification for 10 min, and then filtered with needle filters before injection. With 5 mmol/L ammonium acetate aqueous solution and 5 mmol/L ammonium acetate methanol solution as mobile phase and gradient elution, the base separations of MI、CMI and BIT could be achieved within 4.5 min on a C₈ column. The correlation coefficient r² was greater than or equal 0.9992 in the range of 1～20, 3～60, 5～100 μg/L. The limits of quantification (LOQs) were between 0.06～0.1 µg/kg. The average recoveries for MI, CMI and BIT were between 86.4%～108% with the relative standard deviation (RSD) between 1.2%～4.5% in the MI and CMI positive bubble liquid sample. The method is apt to operate and shows good accuracies and repeatabilities. The LOQs of MI、CMI and BIT are also met the requirements of relevant regulations. The method has been applied to analyze bubble liquid samples.

Key words：UPLC-MS/MS; Bubble liquid; Isothiazolinone; Bactericides; Preservatives

引用本文：刘萍, 臧珊珊.超高效液相色谱-串联质谱法测定泡泡液玩具中异噻唑啉酮类杀菌防腐剂[J]. 化学试剂, 2020, 42(5):533-537.

全自动固相萃取-高效液相色谱-电感耦合等离子体质谱法测定太湖三白中氯化乙基汞

孟元华^1,2，龚燕^*1，徐志飞¹，刘文卫¹，薛静³

（1.无锡市疾病预防控制中心，江苏 无锡  214023；2.江南大学 公共卫生研究中心，江苏 无锡  214122；

3.南京医科大学 公共卫生学院，江苏 南京  211166）

摘要：建立太湖三白中氯化乙基汞的全自动固相萃取-高效液相色谱-电感耦合等离子体质谱的检测方法。将样品用0.15% L-半胱氨酸+5%甲醇，超声浸提20 min，经全自动固相萃取仪MCX柱富集，5 mL甲苯淋洗，氮气吹干后流动相定容至1 mL。用ZORBAX SB-C18（4.6 mm×150 mm，5 μm）色谱柱分离，电感耦合等离子体质谱进行定量测定。样品中氯化乙基汞在0.2～10.0 μg/kg的范围内线性关系良好，相关系数r > 0.999。该方法的检出限（LOD）为0.06 μg/kg，定量限(LOQ)为0.2 μg/kg。氯化乙基汞的回收率在88.8%～101.5%之间，相对标准偏差为3.6%～6.8%（n = 7）。本方法准确、简单、自动化程度高，可用于太湖三白样品中氯化乙基汞的监测。

关键词：氯化乙基汞；液相色谱；电感耦合等离子体质谱；全自动固相萃取；太湖三白

中图分类号：O657.6       文献标识码：A         文章编号：0258-3283（2020）

Determination of Ethylmercuric Chloride in Taihu Lake Three Whites by HPLC-ICP-MS with Automatic Solid Phase Extraction MENG Yuan-hua^1,2, GONG Yan^*1, XU Zhi-fei¹, LIU Wen-wei¹, XUE Jing³ (1. Wuxi Center for Disease Control and Prevention, Wuxi 214023,China; 2. Public Health Research Center, Jiangnan University, Wuxi 214122, China; 3. School of Public Health, Nanjing Medical University, Nanjing 211166,China), Huaxue Shiji, 2020, 42(5), ～

Abstract: To establish a method for the determination of ethylmercuric chloride in Taihu Lake Three Whites by high performance liquid chromatography-inductively coupled plasma mass spectrometry (HPLC-ICP-MS) with automatic solid phase extraction. Samples were extracted with extractant containing 0.15% L-cysteine+5% methanol, and then purified with automatic solid phase extraction. The analysis was absorbed by MCX solid phase extraction column and eluted with 5 mL methylbenzene, dried by N₂ and dissolved in the mobile phase. The sample was separated on a ZORBAX SB-C18 column (4.6 mm×150 mm, 5 μm), and the identification and quantification were performed by ICP-MS. Ethylmercuric chloride can be separated effectively and have good linear relationship within the range of 0.2～10.0 μg/kg with correlation coefficients above 0.999. The LOD of the method was 0.06 μg/kg, the LOQ was 0.2 μg/kg, the precision was 6.34%～9.43%, the recovery rate of ethylmercuric chloride was between 88.8% and 101.5%, and the relative standard deviation were between 3.6%～6.8%(n = 7). The method was accurate, simple, automatic, and can be applied to the determination of ethylmercuric chloride in Taihu Lake Three Whites.

Key words：ethylmercuric chloride; liquid chromatography; inductively coupled plasma-mass spectrometry; automatic solid phase extraction; Taihu Lake Three Whites

引用本文：孟元华, 龚燕, 徐志飞, 等. 全自动固相萃取-高效液相色谱-电感耦合等离子体质谱法测定太湖三白中氯化乙基汞[J]. 化学试剂, 2020, 42(5): 538-541 .

热解析-气相色谱-质谱法测定塑胶跑道中35种挥发性有机化合物（VOCs）释放量的研究

郭亚丽^*，王文枝，宋小莉，胡会清，孟妍

（中国检验检疫科学研究院综合检测中心，北京100123）

摘要：建立了塑胶跑道中35种挥发性有机化合物（VOCs）的热解析-气相色谱-质谱法的检测方法。样品预平衡后，经环境舱释放并采集气体，用热解析-气相色谱-质谱法测定，标准曲线定量。35种挥发性有机化合物（VOCs）在0.01～1.0mg/m³浓度范围内线性良好，相关系数＞0.99。当采样体积为5L时，检出限为0.00001～0.0004mg/m³。在0.02、0.1和0.6mg/m³ 3个浓度下，相对标准偏差（n=6）为1.6%～9.7%。该方法可用于塑胶跑道中挥发性有机化合物（VOCs）的定性和定量检测，为研究其对人体可能产生的危害提供重要依据。

关键词：热解析；气相色谱；质谱；挥发性有机物化合物；塑胶跑道

中图分类号：O657.63，TQ317      文献标识码：A      文章编号：0258-3283（2020）--

Release of 35 Organic Compounds (VOCs) in Plastic Track by Thermal Desorption-Gas Chromatography-Mass Spectrometry GUO Ya-li^*, WANG Wen-zhi, SONG Xiao-li, HU Hui-qing, MENG Yan (Chinese Academy of Inspection and Quarantine Comprehensive Test Center, Beijing 100123, China), Huaxue Shiji, 2020, 42(5),～

Abstract: A method for the determination of 35 volatile organic compounds (VOCs) in plastic track by thermal desorption-gas chromatography-mass spectrometry was established. After pre-equilibrium, the gas was released and collected in the environment chamber. The gas was determined by thermal desorption-gas chromatography-mass spectrometry, and was quantified by the standard curve. 35 Volatile organic compounds (VOCs) showed good linearity in the concentration range of 0.01～1.0 mg/m³, with correlation coefficient > 0.99. When the sampling volume was 5L, the detection limit was 0.00001～0.0004mg/m³. The relative standard deviation (n=6) was 1.6%～9.7% at 0.02, 0.1 and 0.6 mg/m³. This method can be used for the qualitative and quantitative detection of volatile organic compounds (VOCs) in plastic track, and provides an important basis for the study of its possible hazards to human body.

Keywords:thermal desorption; gas chromatography; mass spectrometry; volatile organic compounds (VOCs); plastic track

引用本文：郭亚丽，王文枝，宋小莉，等. 热解析-气相色谱-质谱法测定塑胶跑道中35种挥发性有机化合物（VOCs）释放量的研究[J].化学试剂，2020，42（5）：542-545.

食品添加剂面碱溶液与重碱溶液的检测

李大塘^*1,2a,2b，刘秋华^{2a, 2b}，汤璐¹

（1.   广州工商学院 物流系，广东 佛山  528138；2. 湖南科技大学 a.化学化工学院，b. 理论有机化学与功能分子教育部重点实验室 湖南 湘潭  411201）

摘要:为免混用并很方便的区分两种不同用途的添加剂面碱溶液与重碱溶液，采用分别向两种无色溶液中滴加镍盐溶液的措施，建立了检测和鉴别食品添加剂面碱溶液和重碱溶液的有效方法。实验结果表明，面碱溶液呈清晰的白色或灰绿色浑浊或沉淀，而重碱溶液则没有发生明显变化。该方法现象明显、安全可靠、重现性好、成功率高、适用性强、应用面广，可应用于食品、药品检测，食品质量与安全，医药健康，化学化工等技术领域。

关键词：镍盐；面碱；重碱；多重性；组分含量

中图分类号：TS201.2      文献标识码：A    文章编号：0258-3283（2020）--  

Detection and identification of food additive sodium carbonate and sodium bicarbonate solution LI Da-Tang^1,2a,2b, LIU Qiu-Hua^2a,2b, TANG Lu¹ (1. Department of Logistics, Guangzhou Business College, Foshan 528138, China; 2a. College of Chemistry ＆ Chemical Engineering, 2b. Key Laboratory of Theoretical Organic Chemistry and Functional Molecules, Hunan University of Science and Technology, Xiangtan 411201, China), Huaxue Shiji, 2020, 42(5), ～

Abstracts: In order to avoid mixing and easily distinguish two kinds of additives sodium carbonate and sodium bicarbonate solution, a method was successfully established to fast, convently and effectively identify additive sodium carbonate and sodium bicarbonate solution by dropping nickel salt solution into two kinds of colorless solutions respectively. The results showed that the sodium carbonate solution showed clear white or greenish turbidity or precipitation, while the sodium bicarbonate solution did not change significantly. This method possesses the following advantages: obvious experimental phenomenon, safety and reliability, good reproducibility, high success rate, strong applicability, wide application. It can be applied in food and drug testing, food quality and safety, medical health, chemical industry and other technical fields.

Key words: Nickel salt; sodium carbonate; sodium bicarbonate;multiplicity;set of components

引用本文：李大塘，刘秋华，汤璐. 食品添加剂面碱溶液与重碱溶液的检测[J].化学试剂， 2020，42（5）: 546-551.

不同风格类型卷烟中性香味成分差异化研究

陈晨¹，郭春生^*1，何山²，李力群¹，叶亚军¹，田数¹，张涵²，邹严颉²

（1.    内蒙古昆明卷烟有限责任公司，内蒙古呼和浩特010020；2. 郑州轻工业大学食品与生物工程学院，河南郑州450001）

摘要：为研究不同风格类型卷烟中性香味成分的差异性，采用同时蒸馏萃取法和气相色谱质谱联用技术对9种不同风格类型卷烟中性香味成分进行测定，并通过方差分析、主成分分析和聚类分析对4类型香味成分进行分析。结果表明：由方差分析结果可知，针对类胡萝卜素降解产物、棕色化反应产物、芳香族氨基酸裂解产物的总量在I风格卷烟之间没有显著性差异，并且I风格卷烟棕色化反应产物与其他品类卷烟均存在显著性差异；由主成分分析可知，4大类中性香味成分简化为5个主成分，通过计算中性香味成分在5个主成分上的权重，得出不同风格类型卷烟之间差异主要体现在氧化异佛尔酮、6-甲基-5-庚烯-2-醇、β-大马酮和苯乙醛的含量变化；由聚类分析可知，可将不同风格卷烟分为9类，相同风格卷烟能够被分为一类，不同风格卷烟分类效果良好，表明中性香味成分能够用来区分不同风格的卷烟，该方法可以为中式卷烟品类构建以及风格特征剖析提供依据。

关键词：卷烟；中性香味成分；方差分析；主成分分析；聚类分析

中图分类号：TS41      文献标识码：A       文章编号：0258-3283（2020）--

Difference of Neutral Aroma Components in Different Style Types of Cigarettes CHEN Chen¹, GUO Chun-sheng^*1, HE Shan ², LI Li-qun ¹, YEYa-jun¹, TIANShu¹, ZHANG Han ², ZOU Yan-yu²(1. Inner Mongolia Kunming Cigarette Co., Ltd., Huhhot 010020, China; 2. School of Food and Bioengineering, Zhengzhou University of Light Industry, Zhengzhou 450001, China), HuaxueShiji, 2020, 42(5), ～

Abstract:In order to understand the differences of neutral aroma components in different styles of cigarettes, the simultaneous distillation extraction and gas chromatography-mass spectrometry were used to determine the neutral flavor components in 9 different styles of cigarettes, and the four types of flavor components were analyzed by variance analysis, principal component analysis and cluster analysis.The results of analysis of variance showed that there was no significant difference between the total amount of carotenoid degradation products, browning reaction products and aromatic amino acid cleavage products in I-style cigarettes, and the browning reaction products of I-style cigarettes were significantly different from those of other categories of cigarettes; based on the principal component analysis, the four major categories of neutral aroma components were simplified into five principal components. By calculating the weight of neutral flavor components on the five principal components, it was concluded that the difference between different styles of cigarettes was mainly reflected in the content changes of isophorone, 6-methyl-5-hepten-2-ol, β-damascone and phenylacetaldehyde. Cluster analysis shows that different styles of cigarettes can be divided into 9 categories, and the same style of cigarettes can be divided into one category. The classification effect of different styles of cigarettes is good, which shows that neutral aroma components can be used to distinguish different styles of cigarettes. The method can provide a basis for the construction of Chinese cigarette categories and the analysis of style characteristics.

Key words: cigarette; neutral aroma components; analysis of variance; principal component analysis; cluster analysis

引用本文：陈晨, 郭春生, 何山, 等. 不同风格类型卷烟中性香味成分差异化研究[J]. 化学试剂, 2020, 42(5): 552-556.

环境空气监测用氮气中多组分醛酮气体标准物质的研制

聂巍，周鑫^*，郑力文，董了瑜，王滨

（中国测试技术研究院，四川成都 610021）

摘要：介绍了氮气中13组分醛酮气体标准物质的制备方法。气体标准物质的组分为甲醛、乙醛、丙烯醛、正丁醛、戊醛、2-丁酮、丙酮、丁烯醛、甲基丙烯醛、丙醛、己醛、间甲基苯甲醛和苯甲醛，标准值为1μmol/mol。根据组分的不同性质，经研究采用三步称量法来制备13组分醛酮标准气体，建立了气相色谱-质谱连用及选择扫描离子模式的分析方法，对研制的气体标准物质在气瓶中的均匀性和长期稳定性进行了考察。将研制的气体标准物质分别送至中国计量科学研究院（NIM）和中国环监总站（CNEMC）进行了对比测试，取得了良好的对比结果。结果表明，1μmol/mol氮气中13组分醛酮气体标准物质具有较好的均匀性和稳定性，其有效期为12个月，取得了国家二级标物证书，标物号GBW（E）083618。

关键词：醛酮；气体标准物质；称量法；环境空气监测；不确定度

中图分类号：0657.71      文献标识码：A      文章编号：0258-3283（2020）--

Preparation ofReference Material for Multi-Component Aldehydes and Ketones in Nitrogen Gas for Environmental Air Monitoring NIE Wei, ZHOU Xin*, ZHENG Li-wen, DONG Liao-yu, WANG Bin (National Institute of Measurement and Testing Technology, Chengdu, Sichuan, 610021, China) , Huaxue Shiji, 2020, 42(5), ～

Abstract: The development of multi-component aldehydes and ketones in nitrogen gas reference material, containing formaldehyde, acetaldehyde, acrolein, butyraldehyde, pentanal, 2-butanone, acetone, crotonaldehyde, methacrylaldehyde, propionaldehyde, hexaldehyde, m-tolualdehyde and benzaldehyde, at the concentration of 1 μmol/mol level is described. The work adopts three-step weighting method to prepare the standard gas of thirteen aldehydes and ketones based on the different properties of the components. The stability and homogeneity of target analytes in cylinder was checked using GC coupled with aquadruple mass selective detector. The validation result between NIM and NIMTT showed a satisfied consistency, and a reliable accuracy between CNEMC and NIMTT. The results indicated that have been better homogeneity and stability with one year shelf life havebeen achieved, This gas reference material has acquired the certificate of national secondary gas reference material GBW(E) 083618.

Key words: aldehydes and ketones; gas reference material; gravimetric method; Environmental Air Monitoringuncertainty

引用本文：聂巍，周鑫，郑力文，等. 环境空气监测用氮气中多组分醛酮气体标准物质的研制[J]. 化学试剂，2020，42(5):557-562.

基于双8-羟基喹啉半花菁铜离子复合物的S^2-置换型荧光探针的制备及应用研究

吕荫妮，李宏达^*

（中国刑事警察学院 法化学系，辽宁 沈阳  110035）

摘要: 设计合成了基于双8-羟基喹啉半花菁染料铜离子复合物识别硫离子的荧光探针，并通过质谱对其进行了结构表征。通过紫外-可见光谱和荧光光谱研究了探针对硫化物的传感性能，结果表明，荧光探针对硫离子具有非常高的选择性和抗干扰能力，不受其他分析物的干扰，荧光滴定光谱中随着加入不同浓度的硫离子，谱图呈现均匀的变化，探针溶液的荧光强度变化与S^2- （0～5 µmol/L）的浓度呈现良好的线性关系（R² = 0.9984），其检测限低至0.12 μmol/L，反应动力学显示探针识别硫离子仅仅需要30 s，其准一级动力学常数k为（1.13±0.12）s⁻¹，可以实现快速检测的目的，差谱图像呈现明显的颜色变化，可以实现可视化半定量分析环境样品中硫离子的含量。

关键词：荧光探针；硫离子检测；定量分析；可视化分析；差谱图像技术

中图分类号：D918.93      文献标识码：A      文章编号：0258-3283（2020）--

Preparation and Application of S^2- Replacement Fluorescent Probe Based on Bis8-hydroxyquinoline-hemicyanine Cuprine Ion Complex LV Yin-ni, LI Hong-da^* (Department of Forensic Chemistry, Criminal Investigation Police University of China, Shenyang 110035, China), Huaxue Shiji, 2020, 42(5), ～

Abstract: A fluorescence probe which is based on the copper ion complex of the quinolin-8-ol cyanine dye to recognize sulfur ions was designed and synthesized, and its structure was confirmed by mass spectrometry. The sensor performance of the probe to sulfide was investigated via the ultraviolet-visible spectra and fluorescence spectra. The fluorescence probe had very high selectivity and anti-interference ability for sulfur ions, and without the interference of other analytes, the spectrum in the fluorescence titration uniformly changed with adding different concentrations of sulphur ions, and there was a good linear relationship between the fluorescence intensity of the probe solution and the concentration of S^{2 -}(0～5 µmol/L)and R² = 0.9984, the detection limit of which was as low as 0.12 mol / L. The reaction kinetics showed it only takes 30s for the probe to recognize Sulfur Ions and the quasi-first-order kinetic constant k is 1.13± 0.12s ⁻¹, which can realize the purpose of rapid detection. The difference spectrum image presents obvious color changes, which can realize the visual semi-quantitative analysis of the content of Sulfur Ions in the environmental samples.

Key words: fluorescent probe; sulfur ion detection; quantitative analysis; visual analysis; differential spectral imaging technique

引用本文：吕荫妮, 李宏达. 基于双8-羟基喹啉半花菁铜离子复合物的S2-置换型荧光探针的制备及应用研究[J]. 化学试剂, 2020, 42(5):563-567.

一种Rhodol型氟离子荧光探针的合成及性能研究

司乐乐，陈卫星^*，金洗郎，王婷

（西安工业大学材料与化工学院，陕西西安  710021）

摘要：氟离子作为一种特殊的氢键受体，对硅、硼有很强的亲和力，被认为是最重要的阴离子之一。以Rhodol类衍生物和叔丁基二苯基氯硅烷为原料，合成了一种可用于检测氟离子的新型荧光探针。通过红外光谱、元素分析、飞行质谱、热重分析、核磁共振氢谱和核磁共振碳谱对该探针的结构进行表征。通过荧光和紫外-可见光谱法研究探针对氟离子的检测能力。实验结果表明，氟离子浓度范围为0～10μmol/L时，荧光强度与氟离子浓度的关系曲线为y=138.01x+3859.8；紫外吸光度与氟离子浓度的关系曲线为y=0.0133x+0.3296；说明探针可用于溶液中氟离子的定量检测。

关键词：氟离子；荧光探针；Rhodol类衍生物；叔丁基二苯基氯硅烷；Si-O键；定量检测

中图分类号：O657.3文献标识码：A文章编号: 0258-3283（2020）--

Synthesis and Performance of Rhodol Fluoroion Fluorescent Probe SI Le-le, CHEN Wei-xing^*, JIN Xi-lang, WANG Ting (School of Materials and Chemical Engineering, Xi' an Technological University, Xi'an 710021,China) Huaxue Shiji, 42(5), ～

Abstract:As a special hydrogen bond receptor, fluorine ion has a strong affinity for silicon and boron and is considered to be one of the most important anions. Using Rhodol derivatives and tert-butyldiphenylchlorosilane as raw materials, a new fluorescent probe for the detection of fluorine ions was synthesized. The structure of the probe was confirmed by IR, elemental analysis, MS, TGA, ¹HNMR and ¹³CNMR. The detection ability of the probe for fluorine ions was investigated by fluorescence and UV-vis spectroscopy. The results show that the concentration range of fluorine ion is 0 ～ 10 μ mol/L, the relation curve between fluorescence intensity and fluorine ion concentration is y = 138.01x + 3859.8, the relation curve between ultraviolet absorbance and fluorine ion concentration is y = 0.0133x + 0.3296, and it shows that the probe can be used for quantitative detection of fluorine ion in solution.

Key words: fluoride ion; fluorescent probe; rhodol derivatives; tert-butyldiphenylchlorosilane; Si-O bond;quantitative detection

引用本文：司乐乐, 陈卫星, 金洗郎, 等. 一种Rhodol型氟离子荧光探针的合成及性能研究[J]. 化学试剂, 2020, 42(5): 568-571.

对金属离子具有荧光选择识别作用的4-甲醛肟基苯甲酸乙酯的合成

于孟，万芳，王勇^*

（荆楚理工学院 药物合成与优化湖北省重点实验室，湖北 荆门  448000）

摘要：以4-溴苯甲酸为原料，将其与二氯亚砜在乙醇溶液中回流反应制得4-溴苯甲酸乙酯。将4-溴苯甲酸乙酯与氰化亚铜反应制得4-氰基苯甲酸甲酯，将4-氰基苯甲酸甲酯与盐酸羟胺在碱性条件下反应得到白色固体目标化合物。对化合物进行IR、¹HNMR和¹³CNMR等结构表征确证。该合成路线具有操作简单、反应条件温和、生产成本低、产率高等优点。金属离子对目标化合物的荧光响应研究表明，其对Cu(Ⅱ)、 Fe(Ⅲ)和Pb(II)有很好的选择型。随着金属离子Cu(Ⅱ)、Fe(Ⅲ)和Pb(II)的加入，目标化合物的荧光强度逐渐降低至基本消失。对于Mn(Ⅱ)、Fe(II)、Cd(Ⅱ)、Ni(Ⅱ)、Zn(Ⅱ)和Cr(III)等离子，随着金属离子的加入，目标化合物的荧光强度改变甚微或不改变。

关键词：荧光光谱；肟；Cu(Ⅱ)离子；合成；结构表征

中图分类号：O621.3      文献标识码：A      文章编号：0258-3283（2020）--

The synthesis of 4-(hydroxyimino-methyl) benzoic acid ethyl ester and its fluorescence selection recognition with selected metal ions YU Meng, FANG Wan, WANG Yong^* (Hubei Key Laboratory of Drug Synthesis and Optimization, Jingchu University of Technology, Jingmen, Hubei, 444800, China) , Huaxue Shiji, 2020, 42(5), ～

Abstract：4-Bromobenzoic acid was used as a raw material, and it was refluxed with thionyl chloride in ethanol solution to obtain 4-bromo benzoic acid ethyl ester. Reaction of 4-bromo benzoic acid ethyl ester with cuprous cyanide afforded 4-cyano benzoic acid ethyl ester. The target compound, a white solid, was obtained by reaction of 4-cyano benzoic acid ethyl ester with hydroxylamine hydrochloride under basic condition. The compounds was structurally confirmed by IR, ¹HNMR and ¹³CNMR. The synthetic route has the advantages of simple operation, mild reaction conditions, low production cost and high yield. The fluorescence spectroscopy indicates that the target compound has a good selectivity for Cu(II), Fe(III) and Pb(II) ions. With the addition of the metal ions Cu(II), Fe(III) and Pb(II), the fluorescence intensity of the target compound gradually decreased to substantially disappear. For the Mn(II), Fe(II), Cd(II), Ni(II), Zn(II) and Cr(III) ions, the fluorescence intensity of the compound changes little or no change with the addition of metal ions.

Keywords：Fluorescence spectroscopy; Oxime group; Cu(II) ion; Synthesis; Structurally characterized

引用本文：于孟，万芳，王勇. 对金属离子具有荧光选择识别作用的4-甲醛肟基苯甲酸乙酯的合成[J].化学试剂，2020，42（5）：572-577.

印制电路板企业显影去膜有机废水电催化预处理研究

廖泽远^1,2，任大军¹，陶敏^*2，杨芳显³，奚益翔³，梁剑成³，肖文胜²

(1. 武汉科技大学 资源与环境工程学院，湖北 武汉430081；2. 湖北理工学院 环境科学与工程学院，湖北 黄石435003；3. 桂润环境科技股份有限公司，广西 南宁530221)

摘要：印制电路板企业显影去膜有机废水具有有机物浓度高、可生化性差、水质波动大等特点，一直是该行业废水处理的难点问题之一。为此，研究了显影去膜有机废水的电催化处理效果，通过正交试验探讨了废水流量、电流密度、电极材料、电极是否反转4个因素对COD、NH₄⁺-N、SS去除率的影响。结果表明，4个因素的影响大小依次为：电极材料>流量大小>电极是否反转>电流密度；电催化最优运行参数为流量0.048m³/h、电流密度19.11 A/m²、电极材料（酸碱改性活性炭45%，Al₂O₃-TiC复合电极30%，载Mn/Sn/Sb的γ- Al₂O₃半导体电极25%）、电极不反转，此时显影去膜废水中COD、NH₄⁺-N去除率分别达到67.08%、85.63%，然而电催化装置出水中SS浓度明显增加；另外，SS去除率与COD去除率之间呈显著相关，COD去除率随SS去除率先减小后增大，这表明SS浓度的增加显著强化了电絮凝效果，提高了COD去除效率。

关键词：印制电路板企业；显影去膜废水；电催化；正交试验；电絮凝

中图分类号：X703.1      文献标识码：A      文章编号：0258-3283（2020）--

Electro-catalytic Pretreatment of Developingand Stripping Film Organic Wastewater from PCB Factory LIAO Ze-yuan^1,2, Ren Da-jun¹, TAO Min^2*, YANG Fang-xian³, XI Yi-xiang³, LIANG Jian-cheng³, XIAO Wen-sheng² (1. School of Resources and Environmental Engineering, Wuhan University of Science and Technology, Wuhan 430081, China; 2. School of Environmental Science and Engineering, Hubei Polytechnic University, Huangshi 435003, China; 3. Green Environmental Technology Company Limited, Nanning 530221, China), Huaxue Shiji, 2020, 42(5), ～

Abstract: The developing and stripping film organic wastewater from printed circuit board factoryischaracterizedby high concentration of organic pollutants, poor biodegradability and large fluctuation of water quality, which has been one of the difficult problems in wastewater treatment in printed circuit board industry. Therefore, the electro-catalysispretreatment effect of developing and stripping film organic wastewaterwas investigated, and the effects of four factors including wastewater flow size, current density, electrode material and electrode reversal on the removal rate of COD, NH₄⁺-N and SS were studied by orthogonal test. The influence of the four factors was in order: electrode material> flow size> electrode reversal> current density. While the flow rate was 0.048m³/h, current density was 19.11 A/m², electrode material was (acid-base modified activated carbon 45%, Al₂O₃-TiC composite electrode 30%, Mn/Sn/Sb γ-Al₂O₃ semiconductor electrode 25%) and the electrode didn’t reverse, the electro-catalysis effect of developing and stripping film organic wastewater was the best, and the removal rate of COD, NH₄⁺-N were 67.08% and 85.63%, respectively. However, the concentration of SS in the effluent increased significantly. In addition, there was a significant correlation between the removal rate of SS and the removal rate of COD. The removal rate of CODfirst decreased and then increasedwith the removal rate of SS, which indicated that the increase ofSS concentrationsignificantly enhanced the electro-coagulation effect and improved the COD removal efficiency.

Key words: printed circuit board factory; developingorganic wastewater; electro-catalysis; orthogonal test; electric flocculation

引用本文：廖泽远，任大军，陶敏，等. 印制电路板企业显影去膜有机废水电催化预处理研究[J]. 化学试剂, 2020, 42(5): 578-583.

星宿菜总黄酮提取工艺及抗氧化性活性

郭蒙^*1，韦启道¹，刘韬¹，田琴¹，杨再波^{1, 2}

（1．黔南民族师范学院 化学化工学院，贵州 都匀 558000；2．贵州省普通高校民族药用植物资源开发工程研究中心，贵州 都匀 558000）

摘要：为了最大限度获取星宿菜中的总黄酮，以星宿菜为原料，通过单因素试验和正交试验优化出提取星宿菜总黄酮含量的最佳工艺条件：35倍星宿菜的45%乙醇浓度溶解，45 ℃时超声提取55 min，此条件下总黄酮含量平均值为120.31 mg/g。同时测得星宿菜中黄酮的总抗氧化活性为2.266 mmol/L（FeSO₄当量值）。当星宿菜中总黄酮浓度为2.75 mg/mL时，DPPH自由基清除率为85.0%。方法操作简单、快捷、灵敏度高、成本低，仪器价格及日常维护费用不高。

关键词：总黄酮；正交设计；星宿菜；超声提取；抗氧化活性

中图分类号：R284   文献标识码：A   文章编号：0258-3283（2020）--

Extraction Technology and Antioxidant Activity of Total Flavonoids from Lysimachia Fortune Maxim GUO Meng^*1, WEI Qi-dao¹, LIU Tao¹, TIAN Qin¹, YANG Zai-bo^{1, 2} (1. School of Chemistry and Chemical Engineering, Qiannan Normal College for Nationalities, Duyun 558000, China; 2. Engineering Research Center for Development of Ethnic Medicinal Plant Resources in Colleges and Universities of Guizhou Province, Duyun 558000, China), Huaxue Shiji, 2020, 42(5), ～

Abstract: In order to obtain maximum limit content of total flavonoids from the Lysimachia fortune Maxim., single factor and orthogonal design experiments were optimized. The optimizing conditions were obtained, which were 45 % of ethanol concentration, 1:35 of feed liquid ratio (W:V), 55 min of ultrasonic time and 45 °C of ultrasonic temperature. The average content value of total flavonoids was 120.31 mg/g. Meanwhile, the total antioxidant activity of total flavonoids in the Lysimachia fortune Maxim. was 2.266 mmol/L (FeSO₄ equivalent value). The free radical scavenging rate of DPPH was 85.0%, when the concentration of total flavonoids in the Lysimachia fortune Maxim. was 2.75 mg/mL. The method was simple, rapid, high sensitivity and low-cost. In addition, the instrument price and maintenance cost were not high.

Key words: total flavonoids; orthogonal design; Lysimachia fortune maxim; ultrasonic extraction; antioxidant activity

引用本文：郭蒙, 韦启道, 刘韬, 等.星宿菜总黄酮提取工艺及抗氧化性活性 [J]. 化学试剂, 2020, 42(5): 584-588.

磺酸功能化黄原胶催化四氢苯并[b]吡喃的绿色合成

王英磊^*，李文欢，叶红勇，杜朝军，谢英男

(南阳理工学院 生物与化学工程学院，河南 南阳  473004)

摘要：黄原胶是一种由微生物发酵而生产的多糖，具有稳定性好、安全环保等特性。由于其分子中含有羟基等活性基团，可通过简单的结构修饰来制备环境友好型催化剂。采用黄原胶与氯磺酸的磺化反应，制备了磺酸功能化黄原胶固体酸催化剂，在无溶剂条件下催化芳香醛、丙二腈和双甲酮（或1,3-环己二酮）的三组分缩合反应，以85%～97%的产率合成了一系列四氢苯并[b]吡喃衍生物。该催化剂具有安全无毒、可生物降解且可重复利用等优点，符合绿色和可持续发展化学的理念。

关键词：磺酸功能化黄原胶；四氢苯并[b]吡喃；三组分反应；循环使用

中图分类号：TQ612.6       文献标识码：A      文章编号：0258-3283（2020）--

Green Synthesis of Tetrahydrobenzo[b]pyrans Catalyzed by Sulfonic Acid Functionalized Xanthan WANG Ying-lei^*, LI Wen-huan, YE Hong-yong, DU Chao-jun, XIE Ying-nan(School of Biological and Chemical Engineering, Nanyang Institute of Technology, Nanyang 473004, China), Huaxue Shiji, 2020, 42(5), ～

Abstract: Xanthan is a polysaccharide produced by microbial fermentation, which has the characteristics of excellent stability, safety and environment. Xanthan is easy to prepare environmentally and friendly catalyst by simple structural modification, because of active sites of hydroxyl groups. The solid acid of sulfonic acid functionalized xanthan was prepared by the sulfonation reaction of xanthan and chloro sulfonic acid, which was used as an efficient catalyst for the synthesis of a series of tetrahydrobenzo[b]pyran derivatives via the three-component condensation reaction of aromatic aldehyde, malonitrile and dimedone (or 1,3-cyclohexanedione) under solvent-free conditions, in yields of 85% ~ 97%. The main advantages of this catalyst are safe, non-toxic, biodegradable and reusable, which accords with the concept of green and sustainable development chemistry.

Key words: sulfonic acid functionalized xanthan; tetrahydrobenzo[b]pyran; three-component reaction; recycling

引用本文：王英磊, 李文欢, 叶红勇, 等. 磺酸功能化黄原胶催化四氢苯并[b]吡喃的绿色合成[J]. 化学试剂, 2020, 42(5):589-594.

固体超强酸SO₄^2-/M_xO_y催化合成PESA、MA/SAS及MA/SSS聚合物阻垢剂的工艺研究

姚元勇^*，吴兰艳，唐帮成，付蓉

  （铜仁学院 材料与化学工程学院，贵州 铜仁  554300）

摘要：为了进一步地揭示固体超强酸SO₄^2-/M_xO_y“一锅法”催化合成马来酸酐类共聚物阻垢剂的作用机理。采用“分步合成法”，探讨了以固体超强酸SO₄^2-/ZnO或 SO₄^2- /TiO₂-SiO₂为催化剂，马来酸酐（MA）为催化底物，再分别与马来酸酐（MA）、烯丙基磺酸钠（SAS）、苯乙烯基磺酸钠（SSS）发生共聚作用，合成共聚物阻垢剂PESA、MA/SAS及MA/SSS，并对其碳酸钙垢的阻垢效率进行评价。结果表明，采用“分步合成法”制备的共聚物阻垢剂对碳酸钙垢的阻垢效率分别为95.8%（MA/SAS）、90%（PESA）及93%（MA/SSS），与“一锅法”的阻垢效率基本一致。同时，实验采用固体酸SO₄^2-/ZnO或 SO₄^2- /TiO₂-SiO₂分别对马来酸酐（MA）、烯丙基磺酸钠（SAS）及苯乙烯基磺酸钠（SSS）的环氧化反应进行评价。结果表明，固体超强对马来酸酐（MA）环氧化作用时，可成功地分离出马来酸酐的环氧化物--环氧马来酸，相比催化底物烯丙基磺酸钠（SAS）和苯乙烯基磺酸钠（SSS）而言，实验并未分离出相应的环氧化物。另外，以环氧琥珀酸的生成率为超强固体酸的催化活性指标，在较优的催化条件下，实验成功地评价了不同类型固体超强酸SO₄^2-/M_xO_y催化环氧化反应的催化活性。结果表明，在相同条件下，超强固体酸SO₄^2-/ZnO、SO₄^2-/Al₂O₃、SO₄^2-/Fe₂O₃、SO₄^2-/ZrO₂、SO₄^2-/TiO₂-SiO₂、SO₄^2-/SiO₂-Al₂O₃及SO₄^2-/ZrO₂-TiO₂对马来酸酐的环氧化作用，环氧琥珀酸的生成率分别为20%、12%、8%、10.2%、8.9%、7.1%及9.8%，其对应的催化剂催化活性为SO₄^2-/ZnO> SO₄^2-/Al₂O₃> SO₄^2-/ZrO₂> SO₄^2-/ZrO₂-TiO₂> SO₄^2-/TiO₂-SiO₂> SO₄^2-/Fe₂O₃> SO₄^2-/SiO₂-Al₂O₃。

关键词: 固体超强酸；共聚物阻垢剂；马来酸酐；环氧琥珀酸；阻垢性能

中图分类号：O69      文献标识码：A      文章编号： 0258-3283（2020）--

Synthesis of PESA, MA/SAS, MA/SSS Co-polymer Scale Inhibitors Catalyzed by Solid Super Acids SO₄^2-/M_xO_y YAO Yuan-yong^*, WU Lan-yan, TANG Bang-cheng, FU Rong (School of material and chemical engineering, Tongren university, Tongren 554300, China), Huaxue Shiji, 2020, 42(5), ～

Abstract: To explore further the pathway of co-polymers of maleic anhydride as scale inhibitor promoted by solid super acid SO₄^2-/MxOy in “one-pot” way. The experiments applied an approach of “step by step reaction” to explore co-polymerization made of maleic anhydride（MA）with maleic anhydride（MA）, sodium allysulfonate（SAS）and Sodium styrene sulfonate(SSS), respectively, for condensation of PESA, MA/SAS and MA/SSS co-polymer scale inhibitors. And they were made an evaluation on efficiency of scaling inhibition of CaCO₃. The efficiency of co-polymer scale inhibitors PESA, MA/SAS and MA/SSS, which were made by means of “step by setp reaction”, on scaling inhibition of CaCO₃, are 95.8%（MA/SAS), 90%（PESA）and 93%（MA/SSS), respectively. They are almost agreeable with co-polymer scale inhibitors made by “one-pot” way in scale-inhibiting efficiency. Simultaneously, epoxidations of maleic anhydride(MA), sodium allysulfonate(SAS) and sodium styrene sulfonate(SSS) were respectively promoted by solid super acid SO₄^2-/ZnO or SO₄^2- /TiO₂-SiO₂ as a catalyst. It obviously showed that epoxide of maleic anhydride is successfully made and isolated to confirmed to be cis-epoxysuccinic acid by ¹H-NMR,¹³C-NMR and ESI-Ms, in contrast to that of sodium allysulfonate(SAS) and sodium styrene sulfonate(SSS). In addition, the trials had estimated catalytic activities of various solid super acids SO₄^2-/M_xO_y in epoxidation, under the optimal conditions. The results demonstrated that under the same conditions, the catalytic activities of solid super acids SO₄^2-/M_xO_y perform to be SO₄^2-/ZnO> SO₄^2-/Al₂O₃> SO₄^2-/ZrO₂> SO₄^2-/ZrO₂-TiO₂> SO₄^2-/TiO₂-SiO₂> SO₄^2-/Fe₂O₃>  SO₄^2-/SiO₂-Al₂O_3, by yields of cis-epoxysuccinic acid of 20%, 12%, 8%, 10.2%, 8.9%, 7.1% and 9.8%.

Key words: solid super acid; co-polymer scale inhibitor; maleic anhydride; cis-epoxysuccinic acid; scaling inhibition

引用本文：姚元勇, 吴兰艳, 唐帮成, 等。固体超强酸SO₄^2-/M_xO_y催化合成PESA、MA/SAS及MA/SSS聚合物阻垢剂的工艺研究[J]. 化学试剂, 2020, 42(5): 595-600.

基于高选择性碳正离子串联环化反应的Drimane环系合成

冯翔宇^{1, 2}，杨刚^{1, 2}，韩丛丛^{1, 2}，康亮亮^{1, 2}，曹盼盼^{1, 2}，彭碧^{1, 2}，何述钟^{*1, 2}

（1. 贵州大学 药学院，贵州 贵阳  550025；2. 贵州省合成药物工程实验室，贵州 贵阳  550025）

摘要：Drimane型混源倍半萜是一类具有多种生物活性的重要天然产物。分别以(2E, 6E)-金合欢醇和(2Z, 6E)-金合欢醇为原料，经酯化、环氧化、碳正离子串联环化3步反应高选择性地构建出8-hydroxydrimane骨架和具环内双键的drimane骨架，并经区域选择性消除后得到具环外双键的drimane骨架，其结构经¹HNMR、¹³CNMR、COSY、NOESY和MS确证。为具有drimane骨架的天然产物全合成提供了一种高选择性的合成方法。

关键词：Drimane骨架；碳正离子串联环化；高立体选择性；高区域选择性

中图分类号：O626.13    文献标识码：A     文章编号：0258-3283(2020)--

Rapid Synthesis of Drimane Skeleton via Selective Cationic Polyene Cyclization FENG Xiang-yu^{1, 2}, YANG Gang^{1, 2}, HAN Cong-cong^{1, 2}, KANG Liang-liang^{1, 2}, CAO Pan-pan^{1, 2}, PENG Bi^{1, 2}, HE Shu-zhong^{*1, 2} (1.School of Pharmaceutical Sciences, Guizhou University, Guiyang 550025, China; 2. Guizhou Engineering Laboratory for Synthetic Drugs, Guiyang 550025, China), Huaxue Shiji, 2020, 42(5), ～

Abstract：A highly regioselective and diastereoselective cationic polyene cyclization cascade was developed for the synthesis of drimane-type sesquiterpenoids, which represented an array of important natural products with diverse biological activities such as anticancer, anti-HIV, and antifungal. The reaction sequence features a unique cyclization precursor using 3-oxobutanoyl as the protection group which can lead to diastereoselective cyclization and regioselective elimination. This work achieved highly selective synthesis of 8-hydroxydrimane skeleton and endo/exo double-bond drimane skeletons. The products of the above reaction sequence were unambiguously confirmed by ¹HNMR, ¹³CNMR, COSY, NOESY and MS.

Key words: Drimane skeleton; cationic polyene cyclization; diastereoselectivity; regioselectivity

引用本文：冯翔宇, 杨刚, 韩丛丛, 等. 基于高选择性碳正离子串联环化反应的Drimane环系合成[J]. 化学试剂, 2020, 42(5):601-607.

7-溴吡咯-并[2,1-f][1,2,4]三嗪-4-胺的合成

郑军，曹国锐^*

(青岛科技大学 化工学院，山东 青岛 266042)

摘要：吡咯并[2,1-f][1,2,4]三嗪类化合物作为抗肿瘤药的关键母核，其应用越来越广。以水合肼和二碳酸二叔丁酯为原料经酰化、Clauson Kaas吡咯合成、取代、脱保护、环化、溴化6步反应合成了标题化合物。本路线6步反应总收率达到了36%，化合物结构经¹HNMR和MS确定。该合成方法具有反应条件温和、易于操作、后处理方便和产率较高等优点。

关键词：7-溴吡咯并[2,1-f][1,2,4]三嗪-4-胺；小分子抗癌药；关键母核；三嗪；医药中间体；合成

中图分类号：O626.13      文献标识码：A      文章编号：0258-3283（2020）--

Synthesis of 7-Bromopyrrolo[2,1-f][1,2,4]triazin-4-amine ZHENG Jun, CAO Guo-rui^* (College of Chemical Engineering, Qingdao University of Science and Technology, Qingdao 266042, China), Huaxue Shiji, 2020, 42(5), ～

Abstract：Pyrrolo[2,1-f][1,2,4]triazines are widely used as key nucleus for antitumor drugs.The title compound was synthesized from hydrazine hydrate and di-tert-butyl dicarbonate by acylation, Clauson Kaas,substitution, deprotection, cyclization and bromination.The total yield of the 6-step reaction of this route reached 36% and the structure of the target molecules was confirmed by ¹HNMR and MS.The synthesis method has the advantages of mild reaction conditions, easy operation, convenient post-treatment and high yield.

Key words:7-bromopyrrolo[2,1-f][1,2,4]triazin-4-amine;small molecule anticancer drug; key nucleus; triazin; pharmaceutical intermediate; synthesis

引用本文：郑军，曹国锐.7-溴吡咯-并[2,1-f][1,2,4]三嗪-4-胺的合成[J]. 化学试剂, 2020, 42(5): 608-611.

一种环保型发动机油污清洗剂的配制研究

陈红，朱宝伟，古龙

（营口理工学院 化学与环境工程系，辽宁 营口  115014）

摘要：研发了一种环保型发动机油污清洗剂，采用正交试验的方法优化了该清洗剂的配方。考察了复配表面活性剂用量、二乙二醇乙醚的用量、加料顺序、乳化温度及乳化时间对目标产品去污能力的影响，确定了最佳配方组成。其中月桂醇聚氧乙烯(10)醚添加的质量分数为8%、椰子油脂肪酸二乙醇酰胺（6501）为8%、十六醇聚氧乙烯(10)醚8%、溶剂二乙二醇乙醚为2%、缓蚀剂苯并三氮唑的质量分数为0.2%、柠檬酸钠为1%，余量为水。配制得到的清洗剂在高、低温下均有良好的稳定性，对被清洗物的腐蚀性较小并且安全环保，可以代替传统的发动机油污清洗剂。

关键词：发动机油污；清洗剂；复配；安全环保；正交试验

中图分类号：U472.2，TQ649     文献标识码：A      文章编号：0258-3283（2020）

Preparation of Environmental-friendly Engine Grease Cleaner CHEN Hong, ZHU Bao-wei, GU Long (Department of Chemical and Environmental Engineering, Yingkou Institute of Technology, Yingkou 115014,China ), Huaxue Shiji, 2020, 42(5), ～

Abstract: An environmental-friendly engine grease cleaner was developed. The formulation of environmental-friendly engine grease cleaner was optimized by orthogonal experiment. The effects of dosage of surfactant, dosage of diethylene glycol ether, charging sequence, emulsification temperature and emulsification time on the deconditioning ability were investigated. The optimum formula composition was determined. The mass fraction of lauryl alcohol polyoxyethylene (10) ether was 8%, coconutt diethanol amide (6501) was 8%, cetyl alcohol polyoxyethylene (10) ether was 8%, solvent diethylene glycol diethyl ether was 2%, corrosion inhibitor benzotriazole was 0.2%, sodium citrate was 1%, and the remainder was water. There was good stability under high and low temperature for environmental-friendly engine grease cleaner. Cleaning agent is less corrosive to the cleaned material and safety. It can replace the traditional engine oil cleaning agent.

Key words: engine grease; cleaning agent; mixed; safety and environmental protection; orthogonal test

引用本文：陈红, 朱宝伟, 古龙. 一种环保型发动机油污清洗剂的配制研究[J]. 化学试剂, 2020, 42(5):612-615.