DF直读光谱仪操作规程

DocumentNo.文件编号:DFDocumentNo.文件编号:DF直读光谱仪操作规程作业指导书EffectiveDate生效日期:DFDirect-readingSpectrometerOperationProcedureTheinformationContainedinthisEdition版次TheinformationContainedinthisEdition版次A/0页数:10of15documentshallnotbecopiedordisclosedwithoutauthorizedpermission.目的和适用范围PurposeandApplicationScope本文件制订了DF直读光谱仪的操作规程，旨在准确地对钢铁材料进展化学成分定性定量分析。ThisdocumentspecifiesDFdirectreadingspectrometeroperatingprocedures,intendtoaccuratelyandquantitativelyanalyzethechemicalcompositionofsteelmaterial.技术要求Technologicalrequirements运输与移动Transportation&Setting-upDF系列光谱仪用木制标准包装箱，安装现场可用叉车〔承载力气为400kg〕来移动仪器。假设要把仪器移动到高于或低于地面的位置，则要用叉车或万能升降车或吊车。DFseriesspectrometerisdeliveredwithstandardwoodenpackage.Forklift(carryingcapacitymorethan400kg)canbeusedtomovethisinstrumentwheninstallation.Iftheinstrumentshouldbemovedhigherorlowerthanthelocationoftheground,thenforklifttrucksorageneralelevatororcraneshouldbeused.〔距离墙壁至少0.81.42×1.30m×0.92m10ｍ2，与仪器相接的全部接口都位于仪器后面。Forrepairandmaintenanceconveniently,thereshouldbeacertainspaceonallsides(atleast0.8mfromthewalls).Thesizeofinstrumentis1.38m×1.26m×0.88m.Inaddition,spaceshouldbeleftforprinter,computerandargongascylinder,soitneedsatleast10m2,andallinterfacesareontherearoftheinstrument.注：仪器必需确定避开一面受热〔比方：阳光直射，靠近加热装置等。Note:Theinstrumentmustbeavoidedheatedwithoneside(suchasdirectsunlight,neartheheatingdevice,etc.).环境要求EnvironmentalRequirement仪器内部有恒温系统，因此仪器工作环境温度在10℃~30℃之间，建议安装空调，以避开内部恒温连续工作或失去作用〔内部恒温在3℃。仪器工作现场的相对湿度应小于80高湿度可能会造成光学系统、高压系统或其它电子系统消灭不行推想的故障Thereisathermostatsystemintheinstrument,soworkingenvironmenttemperatureshouldbein10℃~30℃andairconditioningisproposedtoinstalltoavoidinternalheaterworkscontinuouslyorloseitsrole(internaltemperatureat30℃±1).Relativehumidityoftheworkingspaceshouldbelessthan80percent.Otherwise,itcanarouseunpredictablefaultinopticalsystem,high-voltagecircuitandotherelectronicsystemsduetolowtemperatureorhigh-humidity.电气连接ElectricalConnectionsDF系列光谱仪对电源的要求是：220V±10%，50Hz，16A慢熔保险丝。建议配电系统应有断电保护〔加装沟通接触器及复位开关〕和过压保护〔配备3~5KVA的稳压电源。主电源、计算机串口等在仪器后面。ThepowerrequirementofDFseriesspectrometeris:220V±10%,50Hz,16Adelayedsafetyfuse.Installationofpowerinterruptprotectssystem(powerrelayandresetswitchshouldbeinstalled)andover-voltageprotection(with3~5KVAofpowervoltageregulator)isrecommended.Themainpower,computerserialportandotherinterfacesareallintherearoftheinstrument.氩气要求ArgonGasRequirement依靠于分析材料，DF系列光谱仪使用光谱仪专用氩气，纯度为99.996%以上。安装仪器时，氩气瓶上应配备氩气表〔或氧气表代替，及与表连接的铜管，供给应仪器的氩气压力为0.3Mp0.4MP。Dependingonanalyzedmaterials,DFseriesspectrometerrequiresargongasofabove99.996percentpurity.Wheninstallingtheinstrument,argongascylindershouldbeequippedwithargongasgauge(oroxygengasgaugeassubstitute),withthecopperpipeconnectedtoit.Besides,thepressureoftheprovidedargongasis0.3Mpa~0.4Mpa.试样制备Samplepreparation用光谱仪分析试样时，试样制备极其重要。制备方法取决于分析材料，钢及其它硬质材料通常用托盘40-60目的氧化铁砂纸。Samplepreparationisextremelyimportantwhenanalyzingsampleswithaspectrometer.Preparationmethoddependsonanalysismaterials.Forsteelandotherhardmaterialsagrinderusing40~60grit(aluminumoxide)paper.操作规程PurposeandApplicationScope开机和关机：Turnon/off:开机:Turnon:总开关→检测→光源Masterswitch→Testing→Source翻开计算机→进入“东方”程序→仪器→检测真空电路Turnonthecomputer→enter“theoriental“program→Instrument→DetectionofVacuumCircuit.电脑屏幕左下方显示“高压已加”之后，再翻开高压按钮〔再开高压按钮，同时将实时检测真空电路前面的“√”去掉。Afterdisplaying“highvoltagehasbeenadded”atthelowerleftofthecomputerscreen,thenopenthehighvoltagebutton(ifthecomputerscreendisplays“highvoltagedoesnotadd“,youshouldpressthehighvoltagebuttonwhenthescreendisplays“highvoltagehasbeenadded”,atthesametimeputthe“√“outwhichisinfrontofthevacuumvalvecircuit).关机：高压→光源→检测→总开关Turnoff:highvoltage→testing→source→masterswitch3.13留意事项Notes假设知道要停电先将仪器关掉，关掉仪器后再开机需要先稳定4-6小时，再使用，必需重描迹。如果长时间关闭必要在使用的前一天开机。仪器需要恒定温度30度，留意后面温控仪的数值，保持在29-31操作。Ifyouknowtopoweroutage,mustpowerofftheinstrument,whenturnedonagainafterturningofftheinstrumentneedtobestablefor4to6hoursandre-profile.Ifpoweroffforalongtime,needtoturnonitthedaybeforeuse.Theinstrumentneedsconstanttemperature30centigrade,payattentiontothevalueoftemperaturecontrollerbehind,itwouldbebesttokeepthetemperaturebetween29and31centigrade.Ifthetemperatureistoohighortoolowmustinformtheinstrumentcompany.InstrumentoperationmustbeinstrictaccordancewiththeTurnon/offsequenceintheoperationsequence.氩气Argongas好坏推断：能激发起点了则好，假设打白点或激发不起来则不好，需要换另外一瓶。Whetherthepuritymeetthestandard:Thepuritymeetthestandardwheninstrumentcaninspireagoodpoint.Iftheinstrumentcannotinspirepointorinspirewhitepoint, youshouldreplaceanotherbottleoftheargongas.2-3瓶氩气，防止不纯或没有氩气时更换.Generallyneedtopreparetwoorthreebottlesofargon,replacetheargongaswhenabottleisimpurityorrunout.工作原理和试样制备Theworkingprincipleandsamplepreparation工作原理：Theworkingprinciple：原子放射光谱分析所承受的原理是用电弧〔或火花〕的高温使样品中各元素从固态直接气化并被激发过出射狭缝，射入各自的光电倍增管，光信号变成电信号，经仪器的把握测量系统将电信号积分并进展模/数转换，然后由计算机处理，并打印出各元素的百分含量。Hightemperatureproducedbyarcsorsparks makethesamplegasification,theelementsof thesampleisinspiredandlaunchcharacteristicspectralline.Aftersplittingthroughopticalgrating,characteristicspectrallineisbecomespectrumaccordingtowavelength.Thecharacteristicspectrallinesoftheseelementsinjectintotherespectivephotomultipliertubesthroughtheexitslit.Thelightsignalstransformintoelectricalsignals.Itismeasuredbytheinstrumentcontrolsystemandprocessedbycomputer.Theprinterprintoutthepercentagecontentofeachelement.试样的制备：取样要有代表性，没有气孔、裂纹、砂眼和夹渣。Samplepreparation:Thesampleshouldberepresentative,withoutpores,cracks,trachoma,andslag.样品的磨制：要平坦、有纹理、磨完不能用手摸，不能沾上水或油。Samplesgrinding:Thesampleshouldbesmooth,textured,cannotbetouchedandstainedwithwateroroilaftergrinding.1/21/2处〔不能在同一部位激发多点。Inspiredparts:Theinspiredpositionmustbecorrect,forcylindricalsamplesitisinthepositionof1/2ofradiusneartheoutside(Inspiremultiplepointsinthesameplaceisnotpermitted).光谱仪预热好坏的推断：Judgmenttothepreheatofthespectrometer：看点子：中间有银白色金属熔融物，外圈有黑色或褐色的放电物〔铸铁可能没有黑圈。Lookatdot:Thereissomesilver-whitemetalmeltinthemiddleofthedot,blackorbrowndischargematerial attheouterring(theremaybenoblackcircleinthecastironsample).连续激发几次看屏幕上元素浓度数据的接近程度。Seetheproximityoftheconcentrationdataoftheelementaftercontinuouslyinspiringseveraltimes.看“显示选择”→原始强度FeR的值是否到达确定数值且变化很小，上下相差不超过15%。See“Showoptions“→WhetherthevalueoftheoriginalstrengthofFeRreachesacertainvalueandhavelittlechanges,rangeabilityisnomorethan15%.描迹Profile点“系统维护”里面的“PMT自动描迹”。Click“PMTAuto-profile”inthe“Systemmaintenance”.点“参数设置“读电机位置”再点“确定A设置起始位置和终止位置，起始位置为A-100，终止位置为A+100。Click“conditionsset“,firstlyclick“readthemotorposition“ →OK,setthestartpositionandendpositionaccordingto themotorposition,startingpositionfortheA-100,theterminationoflocationA+100.点“复位”，再点“确认”Click“Reset”,then“Confirm”.放好样品后点“开头”Click“Start”afterputtingawaythesample.基体元素Fe和铁基中含量比较高的另一个元素〔废样假设是铸铁选C通道〕ClickFechannelandanotherironbaseelementofrelativelyhighcontent(Forcastironscrapsample,chooseCchannel).点“描迹位置”，读出位置点“确定”Click“Profileposition”andreadoutthepeakpositionthenclick“Confirm”.点“自动定位”，等自动定位完毕，点OKClick“Auto-positioning”andwhenitcompleted,clickOK.(8)关闭Close留意事项：以下状况需要描迹：Note:Thefollowingneedprofile：长期停电和突然断电.Long-termpoweroutagesandemergencypowerfailure.温控消灭故障Temperaturecontrolfaultoccurs擦完透镜Aftercleaningupthelens每一月做一次或按使用状况设定。Onceamonthoraccordingtotheservicecondition.标准化〔对光谱仪工作曲线的校准〕Standardization〔Calibrationcurve〕目的：Objective:把发生漂移曲线〔Ⅱ〕校正成正常曲线(Ⅰ)。[(Ⅰ)曲线是最正确工作曲线]Correctthedriftingcurve(Ⅱ)intothenormalcurve(Ⅰ).[Curve(Ⅰ)isthebestworkcurve]作法Process点“标准化”或F7进入。Click“standardization“orF7toenter.依据“品名规格”显示的样品名称找到此样品，放到火花台处激发2-3点，点“平均+偏差”看RSD333把较大的去掉，合格后点击下一个。Findthesampleaccordingwiththenameofthesampleshowedby“thesamplespecification“,theninspirethesample2-3points,click“average+deviation”, click“next”whentheRSDlessthan3.IftheRSDnotlessthan3,youshouldinspirethesampleagain,deletethepointwhosedeviationisgreater.数。Inspirethesampleaccordingtotheorderuntilthescreendisplay“routinestandardizedend”.标准化系数范围要求0.5-2.5，在范围内点“承受Thescopeofrequiredstandardizedcoefficientis0.5-2.5,inthescopeofrequiredclickOK→Accept留意事项：每激发一次刷一下电极，标准化样品不能放错，标准化系数不能为负数。Note:Theelectrodeshouldbebrushedafterinspiring,cannotplacethewrongsamples,standardizedcoefficientscannotbenegative.类型标准化Typestandardization适合材质、构造组织一样的样品，并且成分值和样品标准值接近。ThismethodisSuitforthesamplewhosematerial,structuralorganizationissame,andthecomponentvalueandsamplestandardvalueisclose.能一次校正全局部析元素。Cancorrectalltheanalyticalelementsonce.〔只有第一次要输入值，以后可以直接调用〕Inputmethod:(shouldinputvaluesonlythefirsttime,thefuturecanbedirectlyinvoked)程序→修改程序参数Programs→modifytheprogramparameters点“类型标准化样品Click“Typestandardizationsample“,click“Add”.输入样品名称“如31〔不能输入一样的名字〕Enterthesamplename“,suchas316“(cannotenterthesamename)点“确定”Click“Confirm“tosaveClick“Typestandardizedparameters“,enter“Elementname“andthe“Realconcentration.“点添加来增加行，直到输完全部元素为止〔屏幕上能分析的元素输进去，样品上有的元素但屏幕上没有的元素不要输进去，否则会出错误。全部输入完毕，点击“确定Usethekeyboard“↓“keytoincreasethelineuntilenteralltheelements(entertheelementcanbeanalyzedonthescreen,theelementsofthesamplebutnotonthescreencannotbeinputted,otherwiseerroroccurs〕.Alltheinputiscompleted,thenexit.类型标准化作法Theprocessoftypestandardization点击“类型标准化F”按键进入Click“typestandardization(F8)”toenter.查看“品名规格”显示的样品名称，找到相应的样品激发2-3次。Findthesampleaccordingwiththenameofthesampleshowedby“thesamplespecification“,theninspirethesample2-3points.看全部数据是否接近，假设接近，点“下一个F点“下一个F”Toseewhetherallthedataareclose.Ifclose,thenclick“thenext(F3)“,Ifthedataisnotclose,youshouldinspireonceagain,deletethepointwhosedeviationislarger.显示“类型标准化完毕Show“Typestandardizedend”,click“Confirm”.Click“Accept”,typeofstandardizationiscomplete.再打同一个试样，看是否全部值和标准值接近，接近就可以分析炉内样品了。Re-analyzeasample.Ifallvaluesclosetostandardvalues,youcananalyzethesampleofthefurnaceinside.类型标准化之间的转换Conversionbetweenthetypestandardization.前提：有各种材质并且都作完了类型标准化。Premise:Therearevarioustypesofmaterials,andallhavebeenfinishedtypestandardization.A的产品，就从“测量”→装入类型标准化→选择AA的产品。下炉不做A的产品而要做B的产品，就从“测量”→去除类型标准化→再装入类型标准化→选择B→确定，测量B的产品。AssumethatthisfurnaceisA,fromthe“measurement“→loadtypestandardization→SelectthetypeA-OK, measure A. Next do notProduce Abut B, from the “measurement“→Clear typestandardization→re-loadtypestandardization→selectB→OK,measureB.光谱仪校准的三种方法：描迹、标准化、类型标准化。Threemethodofcalibratingthespectrometer:profile,standardization,typestandardization.材质的输入方法〔便利对检测产品质量的推断〕Themethodofentermaterial(tofacilitatethedetectionofproductqualityjudgments).程序→质量治理文件Programs→QualityManagementdocuments点击“添加”输入材质名称Click“Add”toentermaterialsnames点“保存”Click“Save”.点“具体数据”Click“detaileddata“输入“元素〔具体依据工艺要求保存，假设出错点编辑来修改。Entertheupperlimitandlowerlimit(Accordingtothetechnicalrequirements),alsotoincreasethelinethroughthekeyboard“↓“,allinputiscompleted→save.Ifmakemistakes,clickedittomodify.当测量完样品后，点击平均，再点击程序→质量治理文件→选择你所输入的材质Whencompletelymeasuringthesample,clickthe“Average”,andthenclick“Program”→“Qualitymanagementfiles”andchoosethematerialwhichyouinput.看出是否合格Toseewhetherresultsqualified正常合格显示的是黑色字样Normalqualifyingshowstheblackwords高于上限显示的是红色字样Abovetheupperlimitisshowninredthewords低于下限显示的是蓝色字样Belowthelowerlimitisshowninbluewords表头的输入方法Theentermethodofthetablehead方法(1)：从“编辑”→修改样品参数来转变对话框相应的内容→确定Method(1)From“Edit“→modifythesampleparameterstochangethecorrespondingcontentsofthedialogboxOK方法(2)：双击屏幕上方的蓝色区域来转变对话框相应的内容→确定Methods(2):Double-clickthebluetopofthescreenareatochangethecorrespondingcontentsofthedialogboxOK〔这两种方法的好处：屏幕上的数据还照旧存在〕(Thebenefitsofbothmethods:on-screendataalsostillexist)方法(3：点“下一个F”→来转变对话框相应的内容→确)Methods(3):Click“thenext(F3)“ →tochangethecorrespondingcontentsofthedialogbox→OK(Thedatawilldisappearandbecomeablankscreeninthisway)〔注：材质的选取是通过对话框中材质项对应的下拉菜单项选择的〕(Note:selectthecorrespondingitemsthroughdialogMaterialpull-downmenu)数据的存储和查询方法Themethodofdatastorageandquery平均值存储方法：Storageoftheaveragevalue:在屏幕上激发出数据Inspirethedataonthescreen点击“平均”Clickthe“Average“(3)“文件”→“存储”“File“→“Storage“查询：点击“系统维护”里面的“分析结果查询”会消灭相应的对话框，可依据表头所记录材质名、品名规格等进展查询，也可多条件组合查询。Query:Click“theinquiriesofanalysisresults“inside“SystemMaintenance“,thenthecorrespondingdialogboxwillappear.Youcanqueryaccordingtothematerialnameandspecificationrecordedintheheader,alsobecombinedmulti-condition.全部数据存储方法：Alldatastoragemethods:点击“保存到文件”Click“Savetofile”.选择所要保存的位置Selectalocationtosave.清理火花台和废氩管CleaningSparkStandandargontube作法Process关闭光源按钮Turnoffthelightsourcebutton拿掉火花台罩，放在椅子上Removethecoverofthesparkstandonachair拔掉通废氩气的蓝色胶管Unpinthebluetubepassingwasteargon.用3mm的内六角扳手把火花台板卸掉〔先松开对角的螺丝，擦干净火花台板。Relieveandcleanthesparkstandplatewiththe3mmhexagonalwrench.(Loosenthescrewdiagonalfirst).用吸尘器将台板下面空腔里的灰尘吸干净Cleanthedustinthecavitybelowthetablewithavacuumcleaner把火花台板放回原位Putthesparkstandback.把极距规长端放在火花台板中心孔处，套住电极，用内六角扳手把螺丝拧上PuttheFar-gaugeinthecenterofthesparkstandplate,entangletheelectrodes,thentightenthescrewswithhexagonwrench.用极距规短端把电极压下去(确定要压到底)，看看极距规是否与火花台板接触良好，假设不好，先将前端的螺丝卸开，再用T型扳手卸开顶丝,调整好位置，在上好顶丝，最终拧上前端螺丝。Usingtheshortendofthegaugetopresstheelectrodedown(mustbepressedtotheend),toseewhetherthegaugeiswellcontactwiththesparkstandplate.Ifbad,releasethefrontscrewfirst,thenreleasethefasteningscrewbyaT-typewrench.Tightenthefasteningscrewafteradjustedtotheappropriatelocationandtwistthefrontscrewfinally.盖上火花台罩。并用试样把激发口盖住。Coverthesparksplatform,andtheinspireholeshouldbecoveredbyaspecimen.(10)到“东方程序”中→“仪器”→点“氩气冲洗”“Orientalprogram“→“Instrument“Aronflush“翻开仪器下面板，把废氩管拧下来，用手指堵住蓝管，猛松，把灰吹出，反复几次，并保证瓶内水在1/2-2/3处。Opentheinstrumentunderneathpanel,repeatedseveraltimes,andtoensurethatthewaterbottleat1/2-2/3.再到“东方程序”中→仪器→把“氩气冲洗”前面的“√”去掉。“Orientalprocedures“→Instruments→removed“√“infrontofthe“argonflush“把下面板装好。Installthecoverofthesparkstandandtheunderneathpanel.(14)把光源按钮翻开Turnonthelightsourcebutton.(15)激发废旧试样直至数据稳定Inspirethewastesamplesuntilthedataisstable.留意事项Notes按时清理火花台，每周一次；Cleanupthesparkstandontime,onceaweek.清理火花台时必需关闭光源，防止意外启动造成损害。取下台罩后且必需先拔下废氩管，防止清理内腔时，将液体吸入火花台和污染透镜，造成仪器损坏和影响测量；The“Source”mustbeturnoffwhencleaningthesparkstandtopreventtheinjurycausedbyaccidentalactivation.Unpinthebluetubepassingwasteargonfirstaftertakingdownthestandcover,topreventtheliquidabsorptionintothesparkstandandpollutelenswhencleaningtheinnerchamber,resultinginequipmentdamageandaffectthemeasurement;清理火花台时，台板及其四周如有激发痕迹，应用细砂纸磨平，防止放电产生；Whencleaningthesparkstand,ifthereareinspiremarksonthestandplateandthesurrounding,shouldbesandpaperedsmoothtopreventdischarge.电极磨损应准时更换，或许每半年换一次，可依据使用频率自行设定更换时间。Electrodewearshouldchangeintime,probablyinonceeverysixmonths.Alsocansetthereplacementtimeinaccordancewiththeoperatingfrequency.电极安装必需用极距规固定好，保证中心矩和深度；Electrodesmustbefixedwellbythegaugetoensurethecentralmomentanddepth.清理完火花台之后要对仪器进展校准，即：标准化、类型标准化，然后分析试样。Youshouldrecorrecttheinstrumentaftercleaningthesparkstand,profile,standardization,typestandardization,andanalyzethesample.擦透镜Cleanthelens具体步骤:Concretesteps:关闭“高压”开关。Closethehighvoltageswitch.拆掉上盖螺丝，掀开仪器上盖Removethecoverscrew,lifttheinstrumentonthecover.〔留意透镜抽板上的定位螺丝不要动，否则后果很严峻〕Holdupthelensboard(Notethatthepositioningscrewonthelenscannotbemoved,otherwisetheconsequenceisveryserious).用透镜纸〔或脱脂棉〕由中心向四周轻轻擦拭，将透镜外表的污迹擦干净。Usealenspaper(orcottonwool)towipethelensgentlyfromthecentertoaround,cleanthestainsonthesurfaceofthelens.用吸耳橡胶球将透镜外表的毛屑或纸屑吹干净。Usearubberpipettebulbtoblowoffthetoflockorscraponthesurfaceofthelens.轻轻压下透镜抽板，听到和下面接触的响声，盖上仪器上盖。Gentlypressdownthelensboarduntilhearthesoundofcontactwiththeunderside,coveronthecoveroftheinstrument.Turnontheorientalprogram→Instrument→Dete