分析化学
分析化學
분석화학
CHINESE JOURNAL OF ANALYTICAL CHEMISTRY
2015年
9期
1395-1401
,共7页
卢圆圆%陈梦妮%高屹立%杨健茂%马小玉%刘建允
盧圓圓%陳夢妮%高屹立%楊健茂%馬小玉%劉建允
로원원%진몽니%고흘립%양건무%마소옥%류건윤
静电纺丝技术%氧化锌%石墨烯%修饰电极%铅%方波溶出伏安
靜電紡絲技術%氧化鋅%石墨烯%脩飾電極%鉛%方波溶齣伏安
정전방사기술%양화자%석묵희%수식전겁%연%방파용출복안
Electrospining technique%Zinc oxide%Graphene%Modified electrode%Lead%Square wave stripping voltammetry
以聚乙烯吡咯烷酮(PVP)、聚丙烯腈(PAN)和醋酸锌(Zn(Ac)2)为纺丝前驱液,利用静电纺丝技术制备Zn( Ac)2-PAN-PVP复合纳米纤维原丝,经高温煅烧得到ZnO纳米纤维。 X-射线衍射证明ZnO呈纤锌矿结构。扫描电子显微镜( SEM)显示,ZnO纳米纤维呈中空圆管状。将该ZnO纳米管与石墨烯( RGO)按一定比例混合,采用滴涂法制备ZnO-RGO/GC电极,并用于水体中重金属Pb2+的检测。方波溶出伏安分析表明,此修饰电极对重金属Pb2+有灵敏的响应,响应电位约为-0.4 V。在0.1 mol/L HAc-NaAc (pH=4.6)缓冲溶液中,-1.0 V电位下富集10 min, ZnO-RGO/GC电极对Pb2+检测的线性范围为2.4×10-9~4.8×10-7 mol/L,检出限达到4.8×10-10 mol/L(S/N>3)。此电极容易制作,稳定性好,在用于检测实际水体中Pb2+时,其结果与电感耦合等离子体-质谱法( ICP-MS)测试值一致。
以聚乙烯吡咯烷酮(PVP)、聚丙烯腈(PAN)和醋痠鋅(Zn(Ac)2)為紡絲前驅液,利用靜電紡絲技術製備Zn( Ac)2-PAN-PVP複閤納米纖維原絲,經高溫煅燒得到ZnO納米纖維。 X-射線衍射證明ZnO呈纖鋅礦結構。掃描電子顯微鏡( SEM)顯示,ZnO納米纖維呈中空圓管狀。將該ZnO納米管與石墨烯( RGO)按一定比例混閤,採用滴塗法製備ZnO-RGO/GC電極,併用于水體中重金屬Pb2+的檢測。方波溶齣伏安分析錶明,此脩飾電極對重金屬Pb2+有靈敏的響應,響應電位約為-0.4 V。在0.1 mol/L HAc-NaAc (pH=4.6)緩遲溶液中,-1.0 V電位下富集10 min, ZnO-RGO/GC電極對Pb2+檢測的線性範圍為2.4×10-9~4.8×10-7 mol/L,檢齣限達到4.8×10-10 mol/L(S/N>3)。此電極容易製作,穩定性好,在用于檢測實際水體中Pb2+時,其結果與電感耦閤等離子體-質譜法( ICP-MS)測試值一緻。
이취을희필각완동(PVP)、취병희정(PAN)화작산자(Zn(Ac)2)위방사전구액,이용정전방사기술제비Zn( Ac)2-PAN-PVP복합납미섬유원사,경고온단소득도ZnO납미섬유。 X-사선연사증명ZnO정섬자광결구。소묘전자현미경( SEM)현시,ZnO납미섬유정중공원관상。장해ZnO납미관여석묵희( RGO)안일정비례혼합,채용적도법제비ZnO-RGO/GC전겁,병용우수체중중금속Pb2+적검측。방파용출복안분석표명,차수식전겁대중금속Pb2+유령민적향응,향응전위약위-0.4 V。재0.1 mol/L HAc-NaAc (pH=4.6)완충용액중,-1.0 V전위하부집10 min, ZnO-RGO/GC전겁대Pb2+검측적선성범위위2.4×10-9~4.8×10-7 mol/L,검출한체도4.8×10-10 mol/L(S/N>3)。차전겁용역제작,은정성호,재용우검측실제수체중Pb2+시,기결과여전감우합등리자체-질보법( ICP-MS)측시치일치。
ZnO nanotubes were prepared via electrospinning the Zn ( AC ) 2-polyacrylonitrile-polyvinylpyrrolidone ( PAN-PVP) precursor, followed by thermal decomposition of the above polymers from the precursor fibers. SEM and XRD characterization confirmed that the as-prepared ZnO nanofibers presented the hollow nanotube form, which was composed of ZnO nanoparticles with the size of about 40 nm in wurtzite crystal structure. By mixing with graphene, the obtained ZnO-graphene composite modified glassy carbon electrode ( ZnO-RGO/GCE ) was successfully constructed by dip-coating, which was used for the determination of Pb2+in water. With the sensitive response of the ZnO-RGO/GC electrode to Pb2+in solution was demonstrated by square wave stripping voltammetry, the response pctential was at -0. 4V. Under the optimized conditions, a good linear relationship between peak current and Pb2+ concentration was obtained in the range of 2. 4×10-9-4. 8×10-7 mol/L (R=0. 9970) by 10 min preconcentration at -1. 0 V in 0. 1 mol/L HAc-NaAc buffer solution (pH=4. 6). The detection limit was 4. 8×10-10 mol/L (S/N>3). The ZnO-RGO/GC electrode had good stability. The practical analytical application of the ZnO-RGO modified electrode was assessed by the measurement of the actual water sample and the result was consistent with that obtained by ICP-MS.