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海泡石纳米材料催化化学发光与其分析应用.pdf

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准确测定过氧化氢含量的化学发光方法。该分析方法的线性范围为1.010’8~8.OxlO-6 mol·L。1,检出限S/N3为8.8xlO。9 mol‘L一。该方法成功应用于自来水和雨水样品中过氧化氢含量的测定,加标回收率在98~104%之问。3.基于海泡石催化鲁米诺.过氧化氢化学发光体系,设计并开发了一种新型的化学发光传感器,该传感器测定葡萄糖的线性范围为7.510石~2.0 xlO。3 mol·L。1,检出限S/N3为3.210石mol·L一。采用该传感器测定饮料中葡萄糖的浓度,得到了令人满意的分析结果。关键词海泡石,化学发光,鲁米诺,过氧化氢,葡萄糖II北京化工大学硕士学位论文CHEMILUMINESCENCE CATALYZED BY SEPIoLITENANOML盯ERIAL AND ITS ANALYTICAL APPLICATIoNABSTRACTBecause of the attracting features such as high sensitivity,simple andinexpensive instrumentation,rapid analysis and low background signals,chemiluminescenceCLis of particular interest in the recent decades.Giventhe slow reaction rate and weak luminescence,hunting for novel and effectivecatalysts to enhance the CL intensity has been an attractive topic of intensiveresearch.Sepiolite,which is environmentally行iendly has been widely used aseffective catalysts,absorbent and functional materials as a result of thespecificity of porosity and fibrous morphology.However,as far as we know,no article to date has yet reported the CL properties of sepiolite.In this work,we chose the luminolHE02 CL reaction as a model systemand explored the effects of commercially available natural sepiolite onluminol CL for the first time.It was found that sepiolite possessed excellentcatalytic activity on luminolH202 CL system.The possible CL enhancementmechanism Was proposed according to a variety of characterization s.Moreover,satisfactory results were obtained when the proposed wasapplied in the detection of H202 and glucose in environmental and foodIII北京化工大学硕士学位论文samples.In view of the advantages of abundant storage,low cost,andnon-toxicity etc.,sepiolite seems to be a promising catalyst for luminolbasedCL.Thi s work is not only of importance for expanding the application fieldsof sepiolite,but also for developing natural clay minerals as a new type ofcatalyzer for CL systems.The main contributions of this paper are as follows1.In this section,we found sepiolite could significantly enhance thelumnol-H202 CL system.Based on the scanning electron microscope imagesSEM,powder Xray diffractionXRDand CL spectra,a possible CLmechanism was proposed.2.Based on the enhancement of sepiolite on luminolH202 CL,sepiolitewas used for luminoldriven CL detection of H202.Under the optimumconditions,the CL intensity was proportional to the concentration of H202 inthe range from O.O 1 to 8 I,tmol·L~.The detection limitS/N3was 8.8nm01.L。1 and the relative standard deviationRSDfor twelve repeatedmeasurements of 1.0 I_tmol·L’1 H202 was 2.5%.This proposed hadbeen successfully applied to detect H202 in tap and rain water samples withrecoveries of 981 04%,which could be used as a sensitive detection tool forH202 analysis.3.A novel CL sensor for glucose was developed based on theenhancement of sepiolite on luminolH202 CL.It was found that the CLintensity was linear with glucose concentration in the range of 7.5 x 1 0’6 to2.0 xlO。3 m01.-L 1,and the detection limit for glucose剐Ⅳ.3is 3.2x10石IV北京化工大学硕士学位论文tool‘L~.This proposed has been successfully applied to detect glucosein beverage samples with good accuracy and precision.KEYWORDSsepiolite,chemiluminescence,luminol,H202,glucoseV北京化工大学硕士学位论文VI北京化工大学硕士学位论文目录第一章绪论11.1化学发光概述.11.2纳米材料参与的化学发光反应.21.2.1金属纳米粒子参与的化学发光反应21.2.2金属氧化物纳米粒子参与的化学发光反应..31.2.3量子点参与的化学发光反应..41.3海泡石材料的结构性能及其应用.51.3.1海泡石材料的结构性能一61.3.2海泡石材料的应用..61.4论文研究意义与研究内容.71.4.1研究意义..81.4.2研究内容..82.1引言112.2实验部分122.2.1实验试剂122.2.2实验仪器122.2.3改性海泡石的制备与改性条件的设计132.2.4海泡石样品的表征142.2.5海泡石.鲁米诺.过氧化氢化学发光体系的化学发光反应强度测定..152.2.6海泡石.鲁米诺.过氧化氢化学发光体系的化学发光光谱分析.1 52.3结果与讨论162.3.1海泡石对鲁米诺.过氧化氢化学发光体系的影响162.3.2海泡石的pH值对鲁米诺.过氧化氢体系化学发光强度的影响.172.3.3海泡石的反应温度对鲁米诺.过氧化氢体系化学发光强度的影响192.3.4海泡石的反应时间对鲁米诺.过氧化氢体系化学发光强度的影响202.3.5海泡石催化鲁米诺.过氧化氢化学发光体系的发光体222.3.6海泡石催化鲁米诺.过氧化氢化学发光体系的反应机理探讨232.4本章小结27VII北京化工大学硕士学位论文第三章基于海泡石催化鲁米诺一过氯化氢化学发光体系测定环境和食品样品中微量组分..293.1引言293.2实验部分303.2.1实验试剂303.2.2实验仪器3 13.2.3样品的采集和前处理323.2.4化学发光静态注射实验323.2.5海泡石催化鲁米诺一过氧化氢化学发光分析条件的设计333.2.6化学发光传感器的制备343.2.7化学发光法测定过氧化氢和葡萄糖含量343.2.8分光光度法测定过氧化氢含量363.2.9碘量法测定葡萄糖含量363.3结果与讨论373.3.1化学发光法测定雨水和自来水样品中的过氧化氢373.3.2化学发光传感器测定饮料中葡萄糖含量443.4本章小结47第四章结论49参考文献51致谢 ..59研究成果及发表的学术论文..61作者和导师简介..63VIII北京化工大学硕士学位论文ContentsChapter 1 Introduction.......11.1 CL introduction.11.2 Nanomaterials CI二reaction..21.2.1 Metal nanoparticles CL reaction21.2.2 Metal oxide nanoparticles CL reaction.....31.2.3 Quantum dots CL reaction...41.3 Properties and application of sepiolite materials..............51.3.1 Structure properties of sepiolite materials..................51.3.2 Applications of sepiolite materials.....61.4 Purpose and research content ofthis paper.71.4.1 Purpose ofthis paper.,......,。.,..............71.4.2 Research contents ofthis pape..8Chapter 2 Sepiolite catalyze luminoiH202 eL system1 12.1 Introduction.....................,.l l2.2 Experimental section1 22。2.1 Materials...................122.2.2 Apparatus.....。.。................122.2.3,nle preparation of modified sepiolite and the design of the modified conditions1 32.2.4 111e characterization of sepiolite samples..142.2.5 CL intensity of sepioliteluminol-Hz02 system..1 52.2.6 Luminophor ofsepioliteluminol-H202 CL system.152.3 Results and discussion.1 62.3.1 Effect of sepiolite on luminol-H202 CL system.1 62.3.2 Effect ofthe pH of sepiolite on luminolH202 CL system172.3.3 Effect ofthe reaction temperture ofsepiolite on luminol-H202 CL system.192.3.4 Effect of the reaction time of sepiolite on luminol-H202 CL system202.3.5 CL spectrum ofsepioliteluminolH202 system.222.3.6 Mechanism of sepiolite-luminol-H202 CL system232.4 Conclusions..27TX北京化工大学硕士学位论文Chapter 3 The application of sepioliteluminolH202 CL system inenvironment and food analysis.293.1 Introduction..293.2 Experimental section...303.2.1 Materials.303.2.2 Apparatus...3 13.2.3 Collection and pretreatment ofsamples.323.2.4 The static chemiluminescence experiment323.2.5 The designment of the analytical conditions for the determination of H202..333.2.6 Prepare of CL sensor...343.2.7 Determination ofhydrogen peroxide and glucose by CL.343.2.8 Determination ofhydrogen peroxide by spectrophotometry..363.2.9 Determination ofglucose by odometry..363.3 Results and discussion.373.3.1 CL Detection ofH202 in卸and rain water samples..373.3.2 CL biosensor for determination ofglucose in drinks..443.4 Conclusions..47Chapter 4 Conclusions.·49Reference...............................。........。............................................................51Acknowledgement.59Achievements in scientific research。....................................................61Brief introduction of author and supervisor63X北京化工大学硕士学位论文CLCl砸TAuNPsZENSAGOD溺IgGDNAFLXRDSEMFT-IRUv.VisEDXBETEDlAGODHRPPBSGAMODPN符号说明化学发光化学发光共振能量转移金纳米粒子玉米烯酮链霉亲和素氧化石墨烯鸡卵白蛋白免疫球蛋白G脱氧核糖核酸荧光光谱X射线粉末衍射扫描电子显微镜傅立叶红外光谱紫外可见光谱能量色散X射线光谱比表面积测试乙二胺四乙酸二钠葡萄糖氧化酶辣根过氧化物酶磷酸缓冲溶液戊二醛甲基橙二羟基二过碘酸合镍XI
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