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Quantitative XRF Standardless Methods UniQuant Denver Conference 2002 Kurt Juchli Applied Research Laboratories Ecublens Switzerland Thermo ARL Slide 2 Topics Introduction to UniQuant Differences versus Scanning Programs Analytical Conditions Calibration Analysis of Unknown Samples Slide 3 Topics Introduction to UniQuant Main Features Evolution Slide 4 Introduction to UniQuant Main Features 74 elements (F to Am) determined in 15 minutes (4 to 12 seconds / spectral line) Peak to Peak Hopping + some Background Positions Be, B, C, N and O if appropriate crystals are present Samples: Solids, Liquids, Loose Powders, Filter Papers, etc. Sample Shape: Flat or uneven, odd shaped, small quantities or small pieces, etc. Determination of Multilayers (Thickness and Mass) Balance of unanalysed Elements or Compounds present in the sample, e.g. Organic Rest or Ultra-light Elements Slide 5 Introduction to UniQuant Evolution (1/2) Version 1 (1989): Calibration required special knowledge Background Determination influenced by strong Absorption Edges Version 2 (1992): Improved Calibration Improved Background Determination Program split into 2 parts (due to lack of conventional memory) Version 3 (1995): Improved Alpha and Kappa Coefficients Better results on Major Elements Improved Handling (only 1 Program) Slide 6 Introduction to UniQuant Evolution (2/2) Version 4 (1997): Improved Background Determination with Manual or Automatic Selection among up to 32 Background Shapes Easy Calibration through Graphical Displays Graphical Presentations to check Plausibility of Results More Elements and alternative Lines Version 5 (2001): Parent - daughter principle to derive specific calibrations Setup of user specific calibrations Thin layer on a substrate: may also employ attenuation of intensity from a substrate element Analysis of predefined compounds for any compound that contains at least one XRF feasible element. Slide 7 Topics Differences versus Scanning Programs Scanning - Peak Hopping Impact on Counting Statistics Background Determination Slide 8 Differences versus Scanning Programs Scanning Slide 9 Differences versus Scanning Programs Peak Hopping Slide 10 Differences versus Scanning Programs Counting Statistics (1/2) th = SQR ( R * t ) R = counts/s t = counting time Slide 11 Differences versus Scanning Programs Counting Statistics (2/2) th = SQR ( R * t ) R = counts/s t = counting time Simple rule: SQR (1000000) = 1000 0.1% RSD Slide 12 Differences versus Scanning Programs Background Determination - Scanning Method Slide 13 Differences versus Scanning Programs Background Determination - UniQuant 4 & 5 (1/2) ? ? Background Shape for Last Elements in Group Slide 14 Differences versus Scanning Programs Background Determination - UniQuant 4 & 5 (2/2) Background Shape for First Elements in Group Slide 15 Topics Analytical Conditions Slide 16 Analytical Conditions UniQuant 4 & 5 Special Crystals - Calibrated on request Slide 17 Topics Calibration Measurement of 64 Specimens Determination of Background Shapes and Spectral Impurities Determination of Wedge Effect (Geometry of Instrument) Determination of Helium and Film Factors Determination of Tau values (Fine Tuning of Dead Time Correction) Setup of Drift Correction (5 Setting-up Samples) Slide 18 Calibration Measurement of 64 Specimens Provides over 100 Spectrometer Channel Sensitivities (Kappas) Establishes over 1500 Line Overlap Coefficients Mostly single Compounds, e.g. Elements in the form of pure Metal foils, Oxides, Quartz, Cryolithe, etc. Universal Calibration ? Slide 19 Universal Calibration Sensitivity of Sulfur in various Matrices Slide 20 Universal Calibration What are Kappas ? (1/2) Conventional Sensitivity cps / % 40000 cps / % S in Steel 300000 cps / % S in Oil Slide 21 Universal Calibration What are Kappas ? (2/2) Conventional Sensitivity cps / % 40000 cps / % S in Steel 300000 cps / % S in Oil Intrinsic Sensitivity = Instrumental Sensitivity = Kappa cps / atom cps / 0.1mg (very Thin Layer, Absorption negligible) Slide 22 Universal Calibration Intrinsic and Overlap Kappas table Intrinsic Kappas cps / 0.1 mg Overlap Kappas ppm / % Slide 23 Universal Calibration Graphical Presentation of Intrinsic Kappas Ka La Lb Kb Slide 24 Topics Calibration Measurement of 64 Specimens Determination of Background Shapes and Spectral Impurities Determination of Wedge Effect (Geometry of Instrument) Determination of Helium and Film Factors Determination of Tau values (Fine Tuning of Dead Time Correction) Setup of Drift Correction (5 Setting-up Samples) Slide 25 Calibration Background Shape and Impurities (Teflon) Spectral Background determined with a Teflon Sample Spectral ImpuritiesMass Absorption Coefficients Background Shape expressed in cps / 0.1 mg Slide 26 Calibration Tables for Background Shapes and Impurities Background Shape Impurity Factors Slide 27 Topics Calibration Measurement of 64 Specimens Determination of Background Shapes and Spectral Impurities Determination of Wedge Effect (Geometry of Instrument) Determination of Helium and Film Factors Determination of Tau values (Fine Tuning of Dead Time Correction) Setup of Drift Correction (5 Setting-up Samples) Slide 28 Calibration The Wedge Effect (1/3) Slide 29 Calibration The Wedge Effect (2/3) Liquid Sample Cup Supporting Film Oil Slide 30 Calibration The Wedge Effect (3/3) Liquid Sample Cup Supporting Film Oil Direction of Incident Radiation Direction of detected Radiation Wedge Slide 31 Calibration Wedge Height Wedge Height (mm) Slide 32 Topics Calibration Measurement of 64 Specimens Determination of Background Shapes and Spectral Impurities Determination of Wedge Effect (Geometry of Instrument) Determination of Helium and Film Factors Determination of Tau values (Fine Tuning of Dead Time Correction) Setup of Drift Correction (5 Setting-up Samples) Slide 33 Calibration Absorption Factors for 6 Polypropylene Film Film Factor = Intensity without Film / Intensity with Film Slide 34 Calibration Table for Helium / Film Factors Helium Factor Film Factor 1 Film Factor 2 Film Impurities (cps) Slide 35 Topics Calibration Measurement of 64 Specimens Determination of Background Shapes and Spectral Impurities Determination of Wedge Effect (Geometry of Instrument) Determination of Helium and Film Factors Determination of Tau values (Fine Tuning of Dead Time Correction) Setup of Drift Correction (5 Setting-up Samples) Slide 36 Calibration Determination of Tau Factors (Measurement) Slide 37 Calibration Determination of Tau Factors (Calculation) Slide 38 Calibration Tau Values Slide 39 Topics Calibration Measurement of 64 Specimens Determination of Background Shapes and Spectral Impurities Determination of Wedge Effect (Geometry of Instrument) Determination of Helium and Film Factors Determination of Tau values (Fine Tuning of Dead Time Correction) Setup of Drift Correction (5 Setting-up Samples) Samples 223, 246, 295, 298, 299 Slide 40 Calibration Setup of Drift Correction Day 0Today Drift Slide 41 Topics Analysis of Unknown Samples Basic Features Advanced Features Slide 42 Topics Analysis of Unknown Samples Basic Features Import Intensities Select Job Specify General Data Calculate Concentrations Display Result Check Result Advanced Features Slide 43 Analysis of Unknown Samples Import Intensities (1/5) Slide 44 Analysis of Unknown Samples Import Intensities (2/5) Slide 45 Analysis of Unknown Samples Import Intensities (3/5) Drift Range Indication Slide 46 Analysis of Unknown Samples Import Intensities (4/5) Select Results File Slide 47 Analysis of Unknown Samples Import Intensities (5/5) Each Result is stored in an individual file with the extension 000 to 999 Slide 48 Topics Analysis of Unknown Samples Basic Features Import Intensities Select Job Specify General Data Calculate Concentrations Display Result Check Result Advanced Features Slide 49 Analysis of Unknown Samples Select Job Slide 50 Topics Analysis of Unknown Samples Basic Features Import Intensities Select Job Specify General Data Calculate Concentrations Display Result Check Result Advanced Features Slide 51 Analysis of Unknown Samples Specify General Data (1/12) Slide 52 Analysis of Unknown Samples Specify General Data (2/12) Specify Chemistry Slide 53 Analysis of Unknown Samples Specify General Data (3/12) Select Helium or Vacuum Slide 54 Analysis of Unknown Samples Specify General Data (4/12) Specify Film Slide 55 Analysis of Unknown Samples Specify General Data (5/12) Enter Sample Diameter Slide 56 Analysis of Unknown Samples Specify General Data (6/12) Effective Mass Calculated for Effective Diameter Compensation for Non-Infinite Sample Thickness Enter Sample Weight Slide 57 Analysis of Unknown Samples Specify General Data (7/12) Enter Sample Thickness to compensate for Wegde Effect Slide 58 Analysis of Unknown Samples Specify General Data (8/12) Density is only used to calculate the XRF measuring Depth and to check Weight and Height (esp. for Liquids) Slide 59 Analysis of Unknown Samples Specify General Data (9/12) Enter Concentration of Known Non-Analysed Compound Select Compound / Material Slide 60 Analysis of Unknown Samples Specify General Data - Materials (10/12) Slide 61 Analysis of Unknown Samples Specify General Data (11/12) Enter Dilution Ratio Diluent / Sample Select Compound / Material Specify your own, if necessary Slide 62 Analysis of Unknown Samples General Data - Summary (12/12) Specify everything you know about the Sample Choice of Chemistry Weight (Effective Mass) to compensate for Non-Infinite Thickness Height (Thickness) to compensate for Wedge Effect Known unmeasured Compounds Dilution Specify everything you know about the Analysis Helium or Vacuum Film Slide 63 Topics Analysis of Unknown Samples Basic Features Import Intensities Select Job Specify General Data Calculate Concentrations Display Result Check Result Advanced Features Slide 64 Analysis of Unknown Samples Calculate Concentrations (1/2) ! Only in Version 5 ! Slide 65 Analysis of Unknown Samples Calculate Concentrations (2/2) Result Display Options Slide 66 Topics Analysis of Unknown Samples Basic Features Import Intensities Select Job Specify General Data Calculate Concentrations Display Result Check Result Advanced Features Slide 67 Analysis of Unknown Samples Display Result (1/7) Result Display Options Slide 68 Analysis of Unknown Samples Display Result (2/7) < 18 ppm Slide 69 Analysis of Unknown Samples Display Result (3/7) < 18 ppm Slide 70 Analysis of Unknown Samples Display Result (4/7) Slide 71 Analysis of Unknown Samples Display Result (5/7) Slide 72 Analysis of Unknown Samples Display Result (6/7) Result Display Options Slide 73 Analysis of Unknown Samples Display Result (7/7) Slide 74 Topics Analysis of Unknown Samples Basic Features Import Intensities Select Job Specify General Data Calculate Concentrations Display Result Check Result Sum before Normalisation Information contained in the Intensity Table Influence of Wrong Sample Weight Alternative Lines Advanced Features Slide 75 Analysis of Unknown Samples Check Result - Sum before Normalisation (1/2) Slide 76 Analysis of Unknown Samples Check Result - Sum before Normalisation (2/2) Reasons for Bad Sum before Normalisation Wrong Chemistry Dilution not specified (Binder - Fused Bead) Helium not selected Film not specified Wrong Effective Sample Diameter Known or Unknown Rest not specified (Not analysable Elements) Grain Size Effects Slide 77 Topics Analysis of Unknown Samples Basic Features Import Intensities Select Job Specify General Data Calculate Concentrations Display Result Check Result Sum before Normalisation Information contained in the Intensity Table Influence of Wrong Sample Weight Alternative Lines Advanced Features Slide 78 Analysis of Unknown Samples Check Result - Intensity Table (1/4) Slide 79 Analysis of Unknown Samples Check Result - Intensity Table (2/4) For all these lines the L lines are also measured Slide 80 Analysis of Unknown Samples Check Result - Intensity Table (3/4) 11.48 0.202 Ka Lines Slide 81 Layer Thickness (in m), where 90% of the Fluorescence Radiation originates from (4/4) Source: Retsch - The Sample (International Edition Number 5) L Lines K Lines Slide 82 Topics Analysis of Unknown Samples Basic Features Import Intensities Select Job Specify General Data Calculate Concentrations Display Result Check Result Sum before Normalisation Information contained in the Intensity Table Influence of Wrong Sample Weight Alternative Lines Advanced Features Slide 83 Analysis of Unknown Samples Check Result - Wrong Sample Weight (1/3) Specification of Wrong Sample Weight ! Recalculate ! Slide 84 Analysis of Unknown Samples Check Result - Wrong Sample Weight (2/3) 11.48 0.202 Correct Sample Weight Slide 85 Analysis of Unknown Samples Check Result - Wrong Sample Weight (3/3) 11.48 0.202 60.64 99.6 Since Version 5.04 Slide 86 Topics Analysis of Unknown Samples Basic Features Import Intensities Select Job Specify General Data Calculate Concentrations Display Result Check Result Sum before Normalisation Information contained in the Intensity Table Influence of Wrong Sample Weight Alternative Lines Advanced Features Slide 87 Analysis of Unknown Samples Check Result - Select Alternative Lines (1/2) Move Cursor here or Click here Enter * / Space to select / deselect Alternative Lines ! Recalculate ! Slide 88 Analysis of Unknown Samples Check Result - Select Alternative Lines (2/2) 11.48 0.202 60.64 99.6 Slide 89 Topics Analysis of Unknown Samples Basic Features Advanced Features Background Shapes General Information How to make a New Shape Example Oil Standard Conostan S-21 / 50 ppm Example Chemplex 55 Elements Standard Shadow Loss Special Cases Subset Programs Kappa Lists Small Samples Slide 90 Analysis of Unknown Samples Background Shapes - Select Shape (1/8) Slide 91 Analysis of Unknown Samples Background Shapes - Selection Criteria (2/8) Slide 92 Analysis of Unknown Samples Background Shapes - Define Default Shape (3/8) Since Version 5 0 = Automatic Shape Selection 1 = Teflon Shape (recommended) Slide 93 Topics Analysis of Unknown Samples Basic Features Advanced Features Background Shapes General Information How to make a New Shape Example Oil Standard Conostan S-21 / 50 ppm Example Chemplex 55 Elements Standard Shadow Loss Special Cases Subset Programs Kappa Lists Small Samples Slide 94 Analysis of Unknown Samples Background Shapes - Table of Shapes (4/8) Slide 95 Analysis of Unknown Samples Background Shapes - Shapes and Impurity Factors (5/8) Background Shapes Impurity Factors N o t S e t u p N o t S e t u p Slide 96 Analysis of Unknown Samples Background Shapes - Make New Shape (6/8) Slide 97 Analysis of Unknown Samples Background Shapes - Select Sample (7/8) Slide 98 Analysis of Unknown Samples Background Shapes - Check / Refine Shape (8/8) Fe Absorption EdgeSmoothed Shape Slide 99 Topics Analysis of Unknown Samples Basic Features Advanced Features Background Shapes General Information How to make a New Shape Example Oil Standard Conostan S-21 / 50 ppm Example Chemplex 55 Elements Standard Shadow Loss Special Cases Subset Programs Kappa Lists Small Samples Slide 100 Analysis of Unknown Samples - Oil Sample Conostan S-21 / 50ppm (1/5) Neighbours in second group Overlapped by Rh Ka Lines Wrong Impurity Factors Last Element in first group Problem of Shape Slide 101 Analysis of Unknown Samples - Oil Sample Inappropriate Background Shape (2/5) Wrong Impurity Factors for Oil Matrix Background too low Slide 102 Analysis of Unknown Samples - Oil Sample Shape and Impurity Factors for Oil Matrix (3/5) Slide 103 Analysis of Unknown Samples - Oil Sample Appropriate Background Calculation (4/5) Background Shape and Impurity Factors calculated with Base Oil Sample Background calculated for Unknown Oil Sample Slide 104 Analysis of Unknown Samples - Oil Sample Conostan S-21 / 50ppm with Oil Background (5/5) Slide 105 Topics Analysis of Unknown Samples Basic Features Advanced Features Background Shapes General Information How to make a New Shape Example Oil Standard Conostan S-21 / 50 ppm Example Chemplex 55 Elements Standard Shadow Loss Special Cases Subset Programs Kappa Lists Small Samples Slide 106 Analysis of Unknown Samples Special Case - Chemplex 55 Elements Standard Look ahead in Background Calculation Slide 107 Analysis of Unknown Samples Special Case - Chemplex 55 Elements Standard Look ahead of 8 Lines (Default Setting) Slide 108 Analysis of Unknown Samples Special Case - Chemplex 55 Elements Standard (1/2) Look ahead of 20 Lines (Special Setting) Slide 109 Analysis of Unknown Samples Special Case - Chemplex 55 Elements Standard (2/2) Look ahead of 20 Lines (Special Setting) Slide 110 Topics Analysis of Unknown Samples Basic Features Advanced Features Background Shapes Shadow Loss Special Cases Subset Programs Kappa Lists Small Samples Slide 111 Analysis of Unknown Samples Compensation for Grain Size Effects (1/2) Slide 112 Analysis of Unknown Samples Compensation for Grain Size Effects (2/2) Slide 113 Topics Analysis of Unknown Samples Basic Features Advanced Features Background Shapes Shadow Loss Special Cases Case 1 Unknown Area Case 2 Unknown % Rest Case 3 Unknown Dilution Case 4 Unknown g/cm2 (Monolayer) Case 5 Unknown Masses/Area (Multilayer) Subset Programs Kappa Lists Small Samples Slide 114 Analysis of Unknown Samples Special Cases - Unknown Area (1/2) Slide 115 Analysis of Unknown Samples Special Cases - Unknown Area (2/2) Case 0: Everything is known Case 1: Unknown Area Same Result ! Slide 116 Topics Analysis of Unknown Samples Basic Features Advanced Features Background Shapes Shadow Loss Special Cases Case 1 Unknown Area Case 2 Unknown % Rest Case 3 Unknown Dilution Case 4 Unknown g/cm2 (Monolayer) Case 5 Unknown Masses/Area (Multilayer) Subset Programs Kappa Lists Small Samples Slide 117 Analysis of Unknown Samples Unknown Rest % (1/2) Slide 118 Analysis of Unknown Samples Unknown Rest % (2/2) Slide 119 Topics Analysis of Unknown Samples Basic Features Advanced Features Background Shapes Shadow Loss Special Cases Case 1 Unknown Area Case 2 Unknown % Rest Case 3 Unknown Dilution Case 4 Unknown g/cm2 (Monolayer) Case 5 Unknown Masses/Area (Multilayer) Subset Programs Kappa Lists Small Samples Slide 120 Analysis of Unknown Samples Unknown Dilution (1/2) Slide 121 Analysis of Unknown Samples Unknown Dilution (2/2) Slide 122 Topics Analysis of Unknown Samples Basic Features Advanced Features Background Shapes Shadow Loss Special Cases Case 1 Unknown Area Case 2 Unknown % Rest Case 3 Unknown Dilution Case 4 Unknown g/cm2 (Monolayer) Case 5 Unknown Masses/Area (Multilayer) Subset Programs Kappa Lists Small Samples Slide 123 Analysis of Unknown Samples Unknown g/cm2 (Monolayer) (1/6) Slide 124 Analysis of Unknown Samples Unknown g/cm2 (Monolayer) (2/6) Schmauchspuren Residues of unburnt powder after a gun shot Slide 125 Analysis of Unknown Samples Unknown g/cm2 (Monolayer) (3/6) La Lb Case 0 (Bulk Sample) Slide 126 Analysis of Unknown Samples Unknown g/cm2 (Monolayer) (4/6) Slide 127 Analysis of Unknown Samples Unknown g/cm2 (Monolayer) (5/6) Slide 128 Analysis of Unknown Samples Unknown g/cm2 (Monolayer) (6/6) Slide 129 Topics Analysis of Unknown Samples Basic Features Advanced Features Background Shapes Shadow Loss Special Cases Case 1 Unknown Area Case 2 Unknown % Rest Case 3 Unknown Dilution Case 4 Unknown g/cm2 (Monolayer) Case 5 Unknown Masses/Area (Multilayer) Subset Programs Kappa Lists Small Samples Slide 130 Analysis of Unknown Samples Unknown Masses/Area (Multilayer) (1/7) Up to 9 unknown (Masses) and 6 fixed layers can be specified Layers can be specified by an Element, Oxide or Compound (Material) Each Layer must have at least one Element of which the Intensity can be measured The order of the layers must be specified (Substrate = 0) Slide 131 Analysis of Unknown Samples Unknown Masses/Area (Multilayer) (2/7) Select Case 5 Calculate Background Slide 132 Analysis of Unknown Samples Unknown Masses/Area (Multilayer) (3/7) Slide 133 Analysis of Unknown Samples Unknown Masses/Area (Multilayer) (4/7) Slide 134 Analysis of Unknown Samples Unknown Masses/Area (Multilayer) (5/7) Slide 135 Analysis of Unknown Samples Unknown Masses/Area (Multilayer) (6/7) Check ! Slide 136 Analysis of Unknown Samples Unknown Masses/Area (Multilayer) (7/7) Slide 137 Topics Analysis of Unknown Samples Basic Features Advanced Features Background Shapes Shadow Loss Special Cases Subset Programs Reasons How to create a Subset Example Kappa Lists Small Samples Slide 138 Subset Programs Reasons To speed up the Analysis measure only Elements present in the Samples measure only Elements that can be measured (e.g. eliminate F to Be in He and/or with Foil) To optimise the Analysis measure only Elements present in the Samples increase Counting Times for important Traces decrease Counting Times for Majors The analysis of oils or polymers does not require to measure lanthanides and precious metals. The total exposure time to X-Rays for Samples using a thin Foil is limited (15 to 20 minutes) - Risk of Damage Slide 139 Subset Programs How to create a Subset Counting Time = 0 will not be measured Slide 140 Subset Programs Example - PetroQuant (1/4) Additives in Oil Ca, Zn, P, Mg, Mo (0 - 5000 ppm) Cl, S (0 - 2.5 %) Si (few ppm) Following elements are sometimes present Na, K, Ba (0 - 5000 ppm) Cu, Fe (0 - 1000 ppm) Abrasion Elements (0 - 500 ppm) Al, Ti, V, Cr, Mn, Fe, Ni, Cu, Ag, Sn, Sb, Pb Total Measuring Time : 11 minutes Slide 141 Subset Programs Example - PetroQuant (2/4) Slide 142 Subset Programs Example - PetroQuant (3/4) Slide 143 Subset Programs Example - PetroQuant (4/4) Slide 144 Topics Analysis of Unknown Samples Basic Features Advanced Features Background Shapes Shadow Loss Special Cases Subset Programs Kappa Lists Principle Practical Example Small Samples Slide 145 AnySample Pressed Powder BeadsAlloys Steel Parent Daughter Parent Daughter 2000 Omega Data Systems BV All Rights Reserved Denver conference 2000 W.K. de Jongh (ODS), Kurt Juchli (ARL) Kappa Lists Principle - New Calibration derived from a Parent (1/3) Slide 146 Pressed Powder Beads Copy Kappa List One or more Standards to firm up calibration of Major Elements Parent Homogeneous Samples Daughter Mineralogical Effects Kappa Lists Principle - New Calibration derived from a Parent (2/3) 2000 Omega Data Systems BV All Rights Reserved Denver conference 2000 W.K. de Jongh (ODS), Kurt Juchli (ARL) Slide 147 Kappa Lists Principle - Create New Kappa List (3/3) Slide 148 Difference in Sensitivity Reduction between High and Low Crystal Angles versus Sample Surface Size (Opening of Sample Holder) Kappa Lists Practical Example (1/4) Sample with 90% Pt / 10% Rh (CAL 278) analysed with 29 and 15 mm Sample Holder Openings Sample with 10% Ir / 90% Pd (CAL 246) measured to adjust Kappas for 15 mm Sample Holder Opening Sample with 90% Pt / 10% Rh (CAL 278) recalculated with new Kappa list Low 2 Theta AnglesHigh 2 Theta Angles Pd = 16.76Ir = 56.68 Rh = 17.54Pt = 54.91 Slide 149 Kappa Lists Practical Example (2/4) Slide 150 Kappa Lists Practical Example (3/4) 29 mm 15 mm Slide 151 Kappa Lists Practical Example (4/4) Adjusted Kappas Slide 152 Collimator Mask Crystal at higher angles Crystal at lower angles Normal Sample Collimator Mask Kappa Lists Practical Example - Explanation (1/2) Slide 153 Crystal at higher angles Small Sample Collimator Mask Crystal at lower angles Kappa Lists Practical Example - Explanation (2/2) Slide 154 Topics Analysis of Unknown Samples Basic Features Advanced Features Background Shapes Shadow Loss Special Cases Subset Programs Kappa Lists Small Samples Slide 155 Polypropylene Insert to keep sample in place Small Samples Irregular Shaped Small Sample Slide 156 Element Drill. 90 Drill.180Drill.360PressedMn%1.341.371.371.38Si%0.360.300.370.41Cr%18.1218.3718.2618.18Ni%10.5810.6110.6010.79Mo%1.911.471.801.59Cu%0.060.080.08Ti%0.0210.0120.0110.014Fe%66.467.366.467.0Nb%0.0090.009 Drill.90, Drill.180 and Drill.360 were analysed under helium environment with a film support (6 PP) The pressed sample was analysed under vacuum Small Samples Stainless Steel Drillings Lowest Angle Slide 157 Thank you very much for your Attention Kurt Juchli Applied Research Laboratories Ecublens Switzerland Thermo ARL Slide 158 Collimator Mask Crystal at higher angles Crystal at lower angles Analysed Surface Collimator Mask