RS-FP基本参数法教程.docx

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1、XRSFP Fundamental Parameters Tutorial XRS-FP根本参数教程The following withassociated files (spectra, *.mca and application,*.tfr) guidesa new user of CrossRoads Scientific XRF Fundamental Parameters Application softwarethrough the setup and implementation ofananalysis.Thisincludes:以下相关文件光谱，*。MCA 和应用程序，*。T

2、FR引导一个的用户十字路口科学 X 射线荧光光谱根本参数，通过设置中的应用软件和实施分析。这包括：1. Qualitative inspection of the sample1。样品的定性检验2. Spectrum processing3. Calibration2。频谱处理3。校准4. Analysis4。分析It ismost convenientto copythe suppliedTutorial Folder toyourhard drive. 这是最便利供给的教程文件夹复制到硬盘驱动器。It is assumed that the x ray spectrometer has b

3、een energy calibrated see section 5.1, XRF Spectrometer Calibration and Monitoring of the XRSFP Software Guide.And that spectrometer excitation parameters have been selected, i.e., incident beam collimation (if required), tube accelerating voltage, tube current, primary beam filter.The setup of thes

4、e parameters will be spectrometer / application specific and are not within the scope of this tutorial other than to emphasize that in order to obtain accurate XRF analysis these must be defined and maintained in the XRS Application, tfr file.据推想，X 射线光谱仪已能量校准 - 见 5.1 节，X 射线荧光光谱仪的校准和XRS 型 FP 软件指南监测。和

5、光谱激发参数已被选中，即入射光束准直如需要，管，加速电压，管电流，主梁的过滤器。这些参数的设置，将光谱仪/特定应用，并没有比强调，为了获得准确的 X 射线荧光分析这些必需定义和XRS 型应用，TFR 文件保持本教程的范围内。Application:Bronzealloy (CuSn alloy) 3 approaches are demonstrated here:Standardless analysis, Calibration using purebulkmaterials and Calibration using a single “type standard”.A typestan

6、dardis a standardofsimilar composition tothatofthe unknowns.应用：铜合金铜锡合金 - 这里呈现的是 3 种方法：标样分析，校准，使用纯粹的大宗物资和校准用一个单一的“标准型”。 A 型标准是一个未知数组成类似的标准。Procedure: 步骤1. Launch XRSFP Click anywhere onthe splash screen toremoveitfrom the display1. 推出XRS型，FP - 飞溅屏幕上的任何地方，从显示屏中删除2. From the AutoModeFP Analysiswindow,

7、click Expert Mode 2。从自动模式的FP分析“窗口中，单击”专家模式“Figure1图1ThiswillrecalltheMaster.tfrfile(seesection4.1,Loadingthe SoftwareoftheXRSFPSoftware Guide).这将召回Master.tfr文件见4.1节，载入软件XRS型FP软件指南。3. From the XRSFP Analyzer interface:Click FileOpen (file typeXRF report, *.tfr)Bronze BulkAnalysis Tutorial.tfr(this is

8、the completed tfr / application)3. 从XRS型-FP接口：点击文件翻开文件类型的X射线荧光光谱报告，* TFR青铜散，分析Tutorial.tfr这是完成的TFR/应用3.1 To start afresh, from the XRSFP Analyzerinterface click:FileNew this willclear all oftheapplication information, i.e., Component Table, Elements Table and Thickness information.TheMeasurement inf

9、ormation (spectrometer configuration)isretained.Thereisnowa“cleansheet” for set up ofanapplication.As noted above,itis not withinthe scope of this tutorialtogointo the details of setting upspecificspectrometer configurations.However, wewillbriefly reviewthe excitation conditions usedfor the example

10、presented here.Referring tothe Measurement Conditions of the New XRSFP Analyzer viewonyourdisplay and presented below, Figure 2.The spectrom eter is configuredwith a tungsten(W) target tube.A primary filter is usedtoremoveth e W L emissions fromacquired spectra thatwould otherwise interfere with app

11、lication analyteemissions, Cufromthe Bronze.Anaccelerating potential isselectedthat issufficientto fluoresce the desired xray emissions ofthe analytes.Inthiscase, dictated bythe Sn emissions K critical potential is29.190keV, so, 47kVtubepotential was selected(1.5 2 X) the critical potential, ifpossi

12、ble.This is alsosufficientenergy tofluoresce the Cu analyte line.A 240 Atubecurrent was selected toprovide count rates thatwould provide efficient analysis.Thiscan bejudged by%DT (dead time) typically 45% 10%.开头从重XRS型-FP分析界面点击：文件建 - 这将去除全部的应用程序的信息，即，成分表，元素表和厚度信息。测量信息光谱仪配置将被保存。现在有“丢球”应用程序的设立。如上所述，它是不

13、属于本教程的范围，进入设立特定的光谱仪配置的细节。然而，我们将简要地回忆这里介绍的例子使用的鼓舞条件。指XRS型，打算生育分析认为您的显示器上的测量条件，并提出如以以下图2。与钨W目标管光谱仪的配置。一个主要的过滤器是用来删除从获得的光谱轮候册的排放，否则将影响应用分析物的排放，从青铜铜。选择一个加速的潜力是足够的荧光X射线分析物所需的排放量。在这种状况下，出于锡排放的 - 关键潜力为29.190 keV的，所以，47千伏管潜力被选中1.5-2 X的潜力的关键，假设可能的话。这也是足够的能量，荧光铜待测线。一个240A，管电流被选中来供给计数率，将供给有效的分析。这可以推断DT死区时间 - 通

14、常为4510。Figure 2图24. Specimen / Application Components:Add the application components(see section 5.2,XRF Elemental FPCalibration orStandardization of the XRS FPSoftwareGuide).Componentscan be elementsorcompounds.Inthisapplication we are working with alloying metals, e lemental metals.In line 1 ofthe

15、 Components table enter Cu.To add another component, use the downar row of your computer keyboard.Enter Snand on line 2,# 2 component.Sample Components4。标本/应用程序组件：添加应用程序组件参见5.2节，X射线荧光元素FP校准或标准化XRS型FP软件指南。组件可以是元素或化合物。在此应用中，我们正在与金属合金，金属元素。在成分表的第1行，进入铜。要添加其他组件，请使用您的电脑键盘上的向下箭头。进入锡和2号线，2组件。样品组分Figure 3 图

16、35. Element Table: As components are defined, the Element Table is filled in defaulting to wh at would nominally be the most intense analyte line available. In this case, the Cu K a nd Sn K. These are appropriate selections for this application.5. Element表：由于组件的定义，元素表中默认会名义上是最猛烈的待测线填补。在这种状况下，Cu靶和Sn的

17、K。这些都是为这个应用程序的适当的选择。6. Thickness Table:Accurate XRF analysisrequires definitionofthe thickness ofthe sample material.Inthe case of thistutorial, the bronze isinfinitelythick, which means thati t has greater thickness than the escapedepth of the highest energy line, the SnK.Thi s isdefined asbulkand

18、isthe default Type setting inthe Thickness Table.The defaultthickness for bulk analysis is zero (0). XRSFP facilitates the analysis of less than in finitely thick samples by calculating the thickness; the Type field is set using the pull do wn to and selecting Calculate. Thickness of less than infin

19、itely thick samples can also beFixed (thickness and units mustthenbedefined inthe fieldsprovided), orcalculatedby absorption (Absn)fromthe absorptionofanemission from materialbelow the layer being anal yzed. Density and Unitfields onlyapply toless thaninfinitelythick samples.6.Thickness 表：准确的X 射线荧光分

20、析要求的样品材料厚度的定义。在本教程的状况下，青铜是无限厚，这意味着它具有更大的比能量最高的线，锡的 K逃命深度厚度。这被定义为散装和厚度表的默认类型设置。默认厚度为散装分析是零0。XRS 型-FP 便于计算厚度小于无限厚的样品分析;使用下拉选择计算类型“字段设置。厚度小于无限厚的样品，也可以被修正厚度和单位，然后必需在供给的字段定义，或通过吸取，从吸取从下面所分析的层物质的排放Absn计算。密度和单位字段只适用于无限小于厚的样品。6.1.The Normalize field ofthe thickness table refers tocomponent concentration.Int

21、hinfilm work layer concentration needs tobenormalizedto 100%.Normalizing to 100% isnot require d for bulk analysis, but isoften employed.If not already done, this is a verygoodpoi nt tosave the tfr that you are creatingbyclicking FileSave As (file type, XRF repor t, *.tfr) Enter the File NameBronzeB

22、ulkAnalysis.tfr.Atthispoint the application isd efined.The nextsteps are toextract analyte intensities fromthe standard spectrumacquire d under the excitationconditions defined inthe Measurement and Processing ConditionsTable a nd derive Calibration coefficients (sensitivities for each analyte emiss

23、ion).6.1.厚度表的标准化领域是指组分浓度。工作在薄膜层浓度必需归到100。散装分析正常化，以100，但常常被雇用。假设不这样做，这是一个格外好的点，以节约您正在创立的总和生育率，通过点击文件另存为 - 文件类型，XRF报告，* TFR。输入文件名，铜奖散装Analysis.tfr。在这一点上，应用程序定义。接下来的步骤是提取自定义的测量和加工条件表中得到校正系数每个分析物排放的灵敏度的激发条件下获得的标准频谱分析物的强度。7.Spectrum Processing/ Extracting Net Intensities (see Section 14.3, Process Spectr

24、umofthe XR S Software Guide):Spectra suppliedfor thistutorial havebeenenergyadjusted (seesection12.11,Setup SpectrumAdjustoftheXRSSoftwareGuide).Toavoiddoingadoubleadjust,fromthe XRSFPInterface SetupProcess and makecertain that the AutoAdjustSpectrum Gain& Offseton Load is unchecked,Figure 4,followi

25、ng.7.频谱处理/已提取的净强度见14.3节，工艺频谱XRS型软件指南：本教程供给的光谱能量调整见第12.11节，设置频谱调整XRS型软件指南。为了避开从XRS型-FP做双重调整。接口 - 安装过程，使某些自动调整负荷频谱增益和偏移是不加制止，图4。Figure 4图47.1.Recall the Bronzespectrum:Fromthe XRSFP Analyzer interface FileOpen (theTutorialF ile type isAmptekSpectrum (*.mca),BronzeSpectrum_Adjusted.mca Figure 5.7.1 。记得

26、铜牌频谱：从XRS型FP接口 - 文件翻开教程文件类型谱Amptek公司MCA，青铜Spectrum_Adjusted.mca- 图5。Figure 5图5It isalways a goodidea toqualitatively inspect the spectrumprior processing.The spectr um, Bronze Spectrum_Adjusted thathas beenrecalled below (Figure 6)ispresented inLog mode, which can beveryuseful for qualitative inspec

27、tion.Cuand Snanalyte peaks are identif ied, as wellas, the processed escapepeaks (black dottedlinespectrum), trace ofPb(not uncommon tobronzes)and a small Zrsystempeak(coming fromthe spectrometer, not the sampl e).The Pband Zrare verysmall peaks and will notinterfere with the application calibration

28、 setup or analysis.定性检查前处理的频谱，它始终是一个好方法。频谱，青铜Spectrum_Adjusted已被召回图6在日志模式，它可以是格外有用的定性检查。 Cu和Sn待测峰确实定，以及处理逃逸峰黑色虚线谱，微量的铅并不少见青铜器和一个小的锆系统峰值来自谱仪，而不是样品。铅和锆是格外小的山峰，并不会干扰应用程序校准设置或分析。Figure 6 图67.2.Spectrum Smooth, Escape PeakRemoval Background Removal and Deconvolute:Click the Proc essing Radio Buttonabove

29、the Measurement & Processing Conditions Table to obtainthe viewof the XRSFP Analyzerinterface below Figure7, resection 3.1 and 3.2, SpectrumProcessi ng ofthe XRSFP Software Guide.Wehavechosen toapply one smoothfunction, removeescape peaks, and apply the Auto Background removal. Background low pass f

30、ilter width parameter is set in SetupProcessing see Figure 4 above. To apply these three functions and extract intensities from the XRSFP Analyzer Interface Click: ProcessSpectrumAll (SmoothEscape Peak RemovalBackground RemovalDeconvolution).There are several peak intensity extraction options. By cl

31、icking on the Intensity Method fie lds for the analyte lines of the Element Table these are displayed Intensity, Gaussian an d Reference. The tutorial uses the Gaussian fit of which there a 2, linear and nonlinear.Nonlinear is used here and is set as a processing parameter SetupProcessing (see Figur

32、e4 above). Each Processing Function can also be applied manually (individually). Manual sele ction is very useful when selecting functions and associated parameters. Net peak intensitiesare extracted, integrated and displayed in the Intensity field of the Element Table of the XRSFP Analyzer Interfac

33、e. Intensities are expressed as count rates counts/second see Figure 8 below. Note that the intensities that you obtain may be slightly different from those displayed in Figure 8.7.2 。频谱平滑，逃逸峰去除背景去除和Deconvolute：点击上述测量及加工条件表处理单项选择按钮来获得XRS型FP接口 - 图7，重3.1节和3.2，频谱处理XRS型-FP软件指南。我们选择申请一个光滑函数，删除逃逸峰，并适用于自动背

34、景去除。背景低通滤波器的宽度参数设置中设置处理 - 见上面的图4。申请这三个函数和XRS型FP接口点击提取强度：过程 频谱光面逃逸峰去除背景去除反卷积。有几个峰值强度的提取选项。通过点击元素表待测线路上强法领域，这些都显示 - 强度，高斯和参考。本教程使用高斯拟合，其中有2，线性和非线性。非线性这里使用和设置加工工艺参数的设置见上面的图4。每个处理功能也可用于手动个别。选择功能和相关参数时，手动选择是格外有用的。净峰强度，提取，集成和XRS型FP接口的元素表的强度领域中显示。强度表示为计数率 - 计数/秒 - 看到下面的图8。请留意，您获得的强度可能会略有不同，从图8中显示这些。Figure

35、7图7Figure 8图88.Calibrate unique case: Most instrumental analysis requires calibration to a standard mater ial. XRF is somewhat unique. Because Xray physics are very well defined there are analy sis circumstances where analysis can be performed without standards truly standardless analy sis. Standard

36、less analysis requires Xray fundamental parameters algorithms be employed XR SFP is a fundamental parameters analysis program, that all the components in the sample mat erial be defined either by the XRF analysis or input by the user and that the sample mater ial be infinitely thick. The tutorial ap

37、plication meets these criteria.8.校准 - 独特的状况下，多数仪器分析需要校准标准物质。 XRF是有点独特。由于X射线物理学是格外明确的，有没有标准执行状况的分析可以分析 - 真正的无标分析。标样分析需要雇用X射线根本参数算法 - XRS型，打算生育是一项根本参数分析程序，样品材料中的全部组件的定义，由X射线荧光分析或输入用户和样品材料是无限厚。本教程的应用程序符合这些标准。8.1.So, having defined the elements inthe bronzeand extracted the net intensities a Standardles

38、 s analysis can bemade.Click ProcessAnalyze and results ofthe standardless analysisoft he bronze are displayed Wt% (Conc.inthe Component Table)and Mole% (see Figure9).N ote that standardlessresults are alwaysnormalized to100% the total sample matrixmust be defined.8.1。因此，定义在青铜元素和提取的净强度1标样分析，可以作出。点击流

39、程分析和铜牌的无标分析的结果显示 - WTConc.在成分表和鼹鼠见图9。请留意，标样的结果总是归到100 - 总样本矩阵必需定义。Figure 9 StandardlessAnalysis图9标样分析9.Calibration withPureElemental orCompoundStandards:StandardlessAnalysis isconvenientand provides a goodsemiquantitative analysis.Another quantitative approach isusing pureele mental bulk materials o

40、rcompounds toestablish Calibration Coefficients.The tutorialapplica tion provides a goodexample for thisapproach pure bulkSnand pure bulkCuare easilyobtained. To implement this approach create a new tfr from the Bronze Bulk Analysis.tfr.9。校准纯元素或化合物的标准：标样分析的便利，供给了一个良好的半定量分析。另一种定量方法是使用纯元素的散装材料或化合物，建立校

41、准系数。本教程的应用程序为这种做法供给了一个很好的例子 - 纯散装锡和纯散装铜很简洁获得。为了实现这种方法创立的从青铜散装Analysis.tfr的总和生育率。9.1.FileOpen (file typetfr) BronzeBulkAnalysisthat was created instep6.1 above.Thenpe rform a FileNewcommand and enter Cuinthe component table (Cu K)is the default.A pure bulk Cuspectrumwas acquiredunder the same excitat

42、ion conditionsthat weredefined fortheBronzeapplication.Recallthisfilefromthetutorialdisk/folder OpenFile(filetypeMCAspectra, *.mca) Cu Bulk_adjusted. Process this spectrum as described previously ProcessSpe ctrumAll9.1 。文件翻开文件类型TFR，在上述步骤6.1创立的青铜散装分析。然后执行文件建“命令，进入组件表中的铜Cu靶是默认的。一个纯粹的散装铜频谱收购青铜应用程序定义的条件

43、下，一样的鼓舞。记得这个文件，从本教程的磁盘/文件夹 - 翻开“”文件文件类型马华谱，* MCA。铜Bulk_adjusted的。处理如前所述谱 - 工艺频谱9.1.1. Now Setup Quantification to determine the Calibration Coefficient (TCC) for Cu K for these excitation conditions input the Concentration of the Cu in the Component Table to 100% and click SetupQuant Fundamental Par

44、ameters Calibration Method and click on the Multiple Standard radio button (we will be using 2 pure metals standards) and OK Figure 109.1.1。现在已经安装量化，以确定这些鼓舞条件为Cu靶校准系数TCC - 输入组件表中的铜浓度为100，并单击“设置” QUANT根本参数标定方法上的多重标准单项选择按钮并单击我们将使用2个纯金属标准，并确定 - 图10Figure 10图109.2. Generate the CuCalibration CoefficientCalibrateFPa TCC calibration coefficient for Cuis generated Figure 119.2 。生成铜的校准系数 - FP TCC校准系数为铜生成校准 - 图11Figure