聚间苯二胺空心纳米球银颗粒负载poly(m-phenylenediamine) hollow spheres.pdf

Electrochimica Acta 98 2013 104 108 Contents lists available at SciVerse ScienceDirect Electrochimica Acta jou rn al h om epa ge Synthesis of Ag nanoparticles decorated poly m phenylenediamine hollow spheres and the application for hydrogen peroxide detection Zhiping Wua Siwei Yanga Zhi Chenb Tingting Zhanga Tingting Guoa Zhoufeng Wanga Fang Liaoa aChemical Synthesis and Pollution Control Key Laboratory of Sichuan Province College of Chemistry and Chemical Engineering China West Normal University Nanchong 637002 China bSchool of Chemistry and Engineering Chongqing University of Technology Chongqing 400050 China a r t i c l e i n f o Article history Received 22 January 2013 Received in revised form 7 March 2013 Accepted 7 March 2013 Available online xxx Keywords Hollow spheres PmPD Silver nanoparticle Hydrogen peroxide detection a b s t r a c t Poly m phenylenediamine PmPD hollow spheres were synthesized for the fi rst time via chemical polymerization of m phenylenediamine mPD monomers by using ammonium persulfate APS as the oxidizing agent in 10 C Ag nanoparticles AgNP was reduced on the hollow spheres PmPD by an AgNO3 aqueous solution in the presence of NaBH4 The Ag nanoparticle decorated poly m phenylenediamine colloids AgNP PmPD exhibit remarkable catalytic performance toward H2O2reduction The correspond ing line arrange and detection limit are estimated to be from 0 1 mM to 10 mM r 0 999 and 0 88 M at a signal to noise ratio of 3 2013 Elsevier Ltd All rights reserved 1 Introduction Hydrogen peroxide takes part in a wide range of enzymatic reac tions playing an important role in the fi elds of chemistry biology clinical control and environmental protection Therefore it is very important for rapid accurate reliable and reagentless determina tion of hydrogen peroxide 1 3 Many detection techniques have been well developed 4 9 such as titrimetry photometry chemi luminescence and electrochemistry Among them electrochemical technique has been proven to be a cheap and effective way due to its intrinsic simplicity well sensitivity and good selectivity Most of this subject with the participation of the enzyme can speed up the electron transfer between the electrodes and H2O2 10 11 But its application is limited because the enzyme is expensive and easy to denature The problem was solved later by using nanostructures such as carbon nanotubes noble metal nanoparticles as catalysts to calatyze the oxidation or reduction of H2O2 12 15 Chemical reduction of metal ions is the most common methods But metal colloids are susceptible to irreversible aggregation because of their small size An effective way is to protect colloids with protective agents such as surfactants thiols polyelectrolytes and polymers 16 25 Among them conducting polymer have been paid close attention by researchers because of their potential applications in Corresponding author Tel 86 817 2568067 fax 86 817 2568067 E mail address liaozhang2003 F Liao optical and microelectronic devices chemical sensors drug deliv ery catalyses and energy storage systems 26 30 Among the conducting polymers polyaniline and its derivatives have been widely researched due to their controllable electrical conductivity high environmental stability unique interesting redox properties controlled by its different oxidation 31 32 In this paper we report a moderate and template free method to synthesis PmPD hollow spheres for the fi rst time Then AgNP PmPD was prepared by adding AgNO3and NaBH4aqueous solution on the suspension of PmPD It is found that such AgNP PmPD exhibit remarkable catalytic performance toward the reduction of H2O2 The corresponding linear range and detection limit was estimated to be from 0 1 mM to 10 mM r 0 999 and 0 88 M 2 Experimental 2 1 Materials Ultra pure water was used and its resistivity was 18 M cm AgNO3 KH2PO4 Na2HPO4 NH4 2S2O8 NaBH4 H2O2 30 and mPD were purchased from Chengdu KeLong All chemicals were of analytical grade and used without further purifi cation 2 2 Synthesis of PmPD hollow spheres Typical synthetic processes of PmPD hollow spheres were as follows 1 5 g mPD was added to 10 mL deionized water and 0013 4686 see front matter 2013 Elsevier Ltd All rights reserved http dx doi org 10 1016 j electacta 2013 03 038 Z Wu et al Electrochimica Acta 98 2013 104 108105 ultrasounded to all dissolved After that the mixture was main tained at ice water bath for 0 5 h before oxidative polymerization Then 6 mL 1 67 M of APS aqueous solution was added to the above mixture The resulting solution was stirred for another 0 5 min to ensure complete mixing and then the reaction was allowed to pro ceed without agitation for 12 h at 10 C Finally the product was centrifuged and washed with deionized water and alcohol till the fi ltrate became colorless and then dried in a vacuum at 60 C for 24 h 2 3 Loading AgNP onto PmPD colloids 20 mg PmPD colloids were dispersed in 5 mL of deionized water Then 5 mL 0 01 M AgNO3aqueous solution and 5 mL 0 01 M NaBH4 aqueous solution were added to the aforementioned PmPD col loids under magnetic stirring for 1 h at room temperature Finally the product was centrifuged and washed with deionized water and alcohol and then dried in a vacuum at 60 C for 24 h 2 4 Electrode preparation and electrochemical measurements All measurements were conducted on a conventional three electrode cell which included a SCE saturated KCl electrode as reference electrode a platinum wire as counter electrode and a bare or modifi ed GC electrode 3 mm in diameter as working elec trode Cyclic voltammetry CV was performed on with a LK2005A electrochemical analyzer LK Chemistry b the corresponding plot of current versus the square root of scan rate 108Z Wu et al Electrochimica Acta 98 2013 104 108 Table 1 A comparison of this work with literature works regarding the performance of the H2O2assays Type of electrodeDetection limit M Linear range mM Ref AgNP PQ11 graphene GCE 28 0 1 40 15 Ag microspheres GCE1 2 0 25 2 35 PQ11 AgNPs GCE 33 7 0 1 180 36 CS GNP HRP PtNP PANI Au 2 8 0 007 14 37 AgNP GO ssDNA AuE 1 9 0 1 20 38 Porous Au nPts electrode100 01 3 39 AuP GCE40 1 50 40 This work0 88 0 1 10 preparation of nanomaterials and feasible construction of sensor and exhibited relatively low detection limit 4 Conclusions In summary a facile and template free approach has been found to fabricate PmPD hollow spheres for the fi rst time by using APS as reductant at low temperature Then the as adsorbed AgNPs are suc cessfully adsorbed on the PmPD hollow spheres in the presence of NaBH4 It was found that AgNP PmPD exhibit good catalytic activity toward H2O2reduction The corresponding linearrange and detec tion limit are estimated to be from 0 1 mM to 10 mM r 0 999 and 0 88 M It is the fi rst demonstration of using AgNP PmPD for enzymeless H2O2detection This provides a promising approach to prepare polymer based nanoelectrocatalysts with high perfor mance for H2O2 Acknowledgement The work was supported by open project fund 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