简介:建立了一种电感耦合等离子体质谱(ICP-MS)法测定环境水样中Cu、Zn、Mn、Pb、Cd5种重金属元素含量的方法。经过仪器条件优化和干扰校正后,方法中5种元素的工作曲线的相关系数均大于0.999,检出限为0.014-0.22μg/L。对加入国家标准物质作为质控样15个批次的环境水样进行统计分析并绘制质控图。同时与原子吸收光谱法测定结果进行对比分析,测定值与标准值基本一致,质控样的测定值基本都在控制线范围之内。结果表明,方法精密度和准确度均能满足环境水样的分析,ICPMS法更适用于大批量、多样化环境水样的监测分析。
简介:建立了电感耦合等离子体原子发射光谱(ICP-AES)法测定锌锭中的Pb、Cd、Fe、Cu、Sn5种杂质元素的方法。样品用硝酸(1+1)溶解后,在稀硝酸介质中利用电感耦合等离子体原子发射光谱仪测定其中Pb、Cd、Fe、Cu、Sn的含量,测定的相对标准偏差(RSD,n=3)小于1.7%,对锌光谱标样BYG0505的测定结果与标准值基本一致。实现了对锌锭中多种杂质元素的简便、快速、准确的同时测定。
简介:Zn/ZSM-5(NZ2)andZn/Ni/ZSM-5(NZ3)asthecatalystsformethanoltoaromatics(MTA)weresynthesizedbyasimpleultrasonicimpregnation.ThetexturalandacidpropertiesofallcatalystswerecharacterizedusingXRD,HRTEM,NH3-TPD,Py-IR,XPS,XRFandTGtechniques.TheXRDandHRTEMresultsshowedthatthebasiczeolitestructureswerenotaffectedmuchwiththeincorporationofZnandNispecies.However,greatchangeshavetakenplaceinacidproperties.ThePy-IRandXPSresultsindicatedthattheZn-Lewisacidsites(ZnOH+species),whichhavestrongerinteractionwiththezeoliteframeworkcomparedwithZnOspecies,weregeneratedattheexpenseofBacidsiteswiththeincorporationofzincspecies.Moreover,theproductanalysisresultsshowedthattheincorporationofzincspeciespromotedtheprimaryaromatizationbyenhancingthedehydroaromatizationandsuppressingthecrackingandsubsequentH-transferreaction.Furthermore,theadditionofNispecieswellinhibitedthelossofzincspeciesbyconvertingpartialZnOspeciestoZnOH+species,andthusimprovedthearomatizationactivityandcatalyststability.ThecatalyticperformanceresultsshowedthattheNZ3possesshigherconversionofmethanolinalongertimeandloweraveragerateofcokeformationcomparedwithNZ2.Inaddition,theNZ3alsoexhibitedthehighestyieldofBTXasthereactionproceeds.
简介:CarbondepositionduringmethanoltohydrocarbonsleadstothequickdeactivationofZSM-5catalystanditisoneofthemajorproblemsforthistechnology.DecreasingthecrystalsizeorintroducingmesoporesintoZSM-5zeolitescanimproveitsdiffusionpropertyanddecreasethecokeformation.Inthispaper,nano-sizedZSM-5zeolitewithintercrystallinemesoporescombiningthemesoporousandnanosizedstructurewasfabricated.Forcomparison,themesoporousZSM-5andnano-sizedZSM-5werealsoprepared.ThesecatalystsampleswerecharacterizedbyXRD,BET,NH3-TPD,TEM,Py-IRandTGtechniquesandusedontheconversionofmethanoltogasolineinafixed-bedreactoratT=405°C,WHSV=4.74h-1andP=1.0MPa.Itwasfoundthattheexternalsurfaceareaofthenano-sizedZSM-5zeolitewithintercrystallinemesoporesreached104m2/g,largerthanthatofmesoporousZSM-5(66m2/g)andnanosizedZSM-5(76m2/g).Catalyticlifetimeofthenano-sizedZSM-5zeolitewithintercrystallinemesoporeswas93h,whichwasonlylongerthanthatofmesoporousZSM-5(86h),butshorterthanthatofnanosizedZSM-5(104h).Strongaciditypromotedthecokeformationandthusdecreasedthecatalyticlifetimeofthenano-sizedZSM-5zeolitewithintercrystallinemesoporesthoughitpresentedlargeexternalsurfacethatcouldimprovethediffusionproperty.Thespecialzeolitecatalystwasfurtherdealuminatedtodecreasethestrongacidity.Afterthis,itscokeformationratewasslowedandcatalyticlifetimewasprolongedto106hbecauseofthelargeexternalsurfaceareaanddecreasedweakacidity.Thisspecialstructuralzeoliteisapotentialcatalystformethanoltogasolinereaction.
简介:建立了微波消解-电感耦合等离子体质谱(ICP-MS)法测定4种纳米银抗菌产品中多种微量元素的分析方法。比较了湿法消解和微波消解这两种样品前处理方法对样品测定的影响,探讨了消除汞记忆效应的方法,并研究了待测元素的质谱干扰的消除。实验结果表明,采用Au(100μg/L)+HCl(2%)能较好地消除Hg的记忆效应。与湿法消解相比,微波消解可短时间消解样品并获得好的Hg回收率。在优化ICP-MS条件后,各元素线性相关系数均大于0.999。采用微波消解-ICP-MS法对样品进行加标回收,样品加标回收率在84.0%-109%,相对标准偏差在0.97%-13.2%。方法快速、简便,能够满足纳米银抗菌产品中微量元素的定量测定。
简介:Unlikeorganic–inorganichybridperovskites,all-inorganiccesiumleadhalideperovskitesholdgreatpromisefordevelopinghigh-performanceoptoelectronicdevices,owingtotheirimprovedstability.Herein,weinvestigatetheperovskite-relatedCsPb2Br5nanoplatelets(NPLs)withtunableemissionwavelengthsviachangingthereactiontemperaturesto100°C,120°C,and140°C.ReactiontemperatureplaysakeyroleindeterminingtheshapesandthicknessesoftheresultingCsPb2Br5NPLs.AhighertemperatureisinfavoroftheformationofsmallerandthickerNPLs.Todeveloptheirpotentialapplicationsinoptoelectronicdevices,greenlightemittingdiodes(LEDs)andphotodetectorsbasedonCsPb2Br5NPLsarefabricated.ThegreenLEDsbasedonCsPb2Br5NPLssynthesizedat140°Cexhibitanexcellentpuregreenemission(fullwidthathalf-maximumof<20nm)anddisplayaluminousefficiencyof34.49lm∕Wunderanoperationcurrentof10mA.Moreover,thephotodetectorbasedonCsPb2Br5NPLssynthesizedat100°Chasbetterperformancewitharisetimeof0.426s,adecaytimeof0.422s,andaratioofthecurrent(withandwithoutirradiation)of364%.
简介:Aserialofprotonatedandlayeredtransitionmetaloxides,includinglayeredHTaWO6,HNbMoO6aswellasHNbWO6,weresynthesizedbysolid-statereactionandion-exchange.ThelayeredHTaWO6hasbeensystematicallystudiedasasolidacidtorealizethedehydrationoffructoseto5-hydroxymethylfurfural(HMF).ThetransitionmetaloxidesampleswerecharacterizedwithICP-OES,EDS,XRD,XPS,SEM,TGA,FT-IR,N2adsorption–desorptionandNH3-TPD.Theinfluentialfactorssuchasreactiontemperature,reactiontime,solvent,catalystamountandsubstrateconcentrationweredeeplyinvestigated.Theoptimizedfructoseconversionrateof99%withHMFyieldof67%wereachievedafter30minat140°Cindimethylsulfoxide.
简介:研究翼型绕流的转捩预测方法,对于翼型流动细节的精确模拟和气动力的准确计算以及精细化设计均具有十分重要的意义.采用动模态分解(dynamicmodedecomposition,DMD)代替线性稳定性理论(linearstabilitytheory,LST)与e^N方法结合,不需要求解稳定性方程,成为一种数据驱动的翼型边界层转捩预测新方法,称为DMD/e^N方法.在原有方法的基础上,改进了DMD网格线生成方法和扰动放大N因子的积分策略,并将RANS求解器与改进的DMD/e^N方法进行耦合,实现了翼型定常绕流转捩预测自动化.采用该方法对LSC72613跨声速自然层流翼型以及NLF0416低速自然层流翼型在不同攻角下的绕流进行转捩预测,转捩点计算结果均与实验值和LST/e^N方法吻合良好.该方法计算得到的N值增长曲线与LST/e^N方法的包络线也较为吻合,进一步验证了积分策略的正确性.改进的DMD/e^N方法可作为自然层流翼型设计的新的有力工具.