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Quantitative XRF Standardless Methods UniQuant Denver Conference 2002
Kurt Juchli Applied Research Laboratories Ecublens Switzerland Thermo ARL
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Topics Introduction to UniQuant Differences versus Scanning Programs
Analytical Conditions Calibration Analysis of Unknown Samples
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Topics Introduction to UniQuant Main Features Evolution
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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
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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)
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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.
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Topics Differences versus Scanning Programs Scanning - Peak Hopping
Impact on Counting Statistics Background Determination
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Differences versus Scanning Programs
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Differences versus Scanning Programs
Peak Hopping
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Differences versus Scanning Programs Counting Statistics (1/2)
th = SQR ( R * t ) R = counts/s t = counting time
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Differences versus Scanning Programs Counting Statistics (2/2)
th = SQR ( R * t ) R = counts/s t = counting time Simple rule: SQR (1’000’000) = 1000 % RSD
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Differences versus Scanning Programs Background Determination - Scanning Method
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Background Shape for Last Elements in Group
Differences versus Scanning Programs Background Determination - UniQuant 4 & 5 (1/2) Background Shape for Last Elements in Group ? ?
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Background Shape for First Elements in Group
Differences versus Scanning Programs Background Determination - UniQuant 4 & 5 (2/2) Background Shape for First Elements in Group
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Topics Analytical Conditions
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Analytical Conditions UniQuant 4 & 5
Special Crystals - Calibrated on request
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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)
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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 ?
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Universal Calibration Sensitivity of Sulfur in various Matrices
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Universal Calibration What are Kappas ? (1/2)
Conventional Sensitivity cps / % 40’000 cps / % S in Steel 300’000 cps / % S in Oil
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Universal Calibration What are Kappas ? (2/2)
Conventional Sensitivity cps / % 40’000 cps / % S in Steel 300’000 cps / % S in Oil Intrinsic Sensitivity = Instrumental Sensitivity = Kappa cps / atom cps / 0.1mg (very Thin Layer, Absorption negligible)
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Universal Calibration Intrinsic and Overlap Kappas table
Intrinsic Kappas cps / 0.1 mg Overlap Kappas ppm / %
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Universal Calibration Graphical Presentation of Intrinsic Kappas
La Lb Kb
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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)
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Calibration Background Shape and Impurities (Teflon)
Spectral Background determined with a Teflon Sample Spectral Impurities Mass Absorption Coefficients Background Shape expressed in cps / 0.1 mg
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Calibration Tables for Background Shapes and Impurities
Impurity Factors Background Shape
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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)
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Calibration The Wedge Effect (1/3)
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Calibration The Wedge Effect (2/3)
Liquid Sample Cup Oil Supporting Film
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Calibration The Wedge Effect (3/3)
Liquid Sample Cup Oil Wedge Supporting Film Direction of Incident Radiation Direction of detected Radiation
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Calibration Wedge Height
Wedge Height (mm)
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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)
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Calibration Absorption Factors for 6µ Polypropylene Film
Film Factor = Intensity without Film / Intensity with Film
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Calibration Table for Helium / Film Factors
Film Impurities (cps) Helium Factor Film Factor 1 Film Factor 2
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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)
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Calibration Determination of Tau Factors (Measurement)
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Calibration Determination of Tau Factors (Calculation)
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Calibration Tau Values
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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
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Calibration Setup of Drift Correction
Day 0 Today Drift
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Topics Analysis of Unknown Samples Basic Features Advanced Features
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Topics Analysis of Unknown Samples Basic Features Advanced Features
Import Intensities Select Job Specify General Data Calculate Concentrations Display Result Check Result Advanced Features
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Analysis of Unknown Samples Import Intensities (1/5)
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Analysis of Unknown Samples Import Intensities (2/5)
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Analysis of Unknown Samples Import Intensities (3/5)
Drift Range Indication
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Analysis of Unknown Samples Import Intensities (4/5)
Select Results File
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Analysis of Unknown Samples Import Intensities (5/5)
Each Result is stored in an individual file with the extension 000 to 999
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Topics Analysis of Unknown Samples Basic Features Advanced Features
Import Intensities Select Job Specify General Data Calculate Concentrations Display Result Check Result Advanced Features
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Analysis of Unknown Samples Select Job
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Topics Analysis of Unknown Samples Basic Features Advanced Features
Import Intensities Select Job Specify General Data Calculate Concentrations Display Result Check Result Advanced Features
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Analysis of Unknown Samples Specify General Data (1/12)
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Analysis of Unknown Samples Specify General Data (2/12)
Specify Chemistry
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Analysis of Unknown Samples Specify General Data (3/12)
Select Helium or Vacuum
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Analysis of Unknown Samples Specify General Data (4/12)
Specify Film
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Analysis of Unknown Samples Specify General Data (5/12)
Enter Sample Diameter
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Analysis of Unknown Samples Specify General Data (6/12)
Calculated for Effective Diameter Compensation for Non-Infinite Sample Thickness Effective Mass Enter Sample Weight
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Analysis of Unknown Samples Specify General Data (7/12)
Enter Sample Thickness to compensate for Wegde Effect
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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)
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Analysis of Unknown Samples Specify General Data (9/12)
Enter Concentration of Known Non-Analysed Compound Select Compound / Material
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Analysis of Unknown Samples Specify General Data - Materials (10/12)
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Analysis of Unknown Samples Specify General Data (11/12)
Specify your own, if necessary Enter Dilution Ratio Diluent / Sample Select Compound / Material
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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
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Topics Analysis of Unknown Samples Basic Features Advanced Features
Import Intensities Select Job Specify General Data Calculate Concentrations Display Result Check Result Advanced Features
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Analysis of Unknown Samples Calculate Concentrations (1/2)
! Only in Version 5 !
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Analysis of Unknown Samples Calculate Concentrations (2/2)
Result Display Options
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Topics Analysis of Unknown Samples Basic Features Advanced Features
Import Intensities Select Job Specify General Data Calculate Concentrations Display Result Check Result Advanced Features
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Analysis of Unknown Samples Display Result (1/7)
Result Display Options
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Analysis of Unknown Samples Display Result (2/7)
< 18 ppm
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Analysis of Unknown Samples Display Result (3/7)
< 18 ppm
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Analysis of Unknown Samples Display Result (4/7)
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Analysis of Unknown Samples Display Result (5/7)
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Analysis of Unknown Samples Display Result (6/7)
Result Display Options
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Analysis of Unknown Samples Display Result (7/7)
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Topics Analysis of Unknown Samples Basic Features Advanced 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
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Analysis of Unknown Samples Check Result - Sum before Normalisation (1/2)
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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
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Topics Analysis of Unknown Samples Basic Features Advanced 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
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Analysis of Unknown Samples Check Result - Intensity Table (1/4)
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Analysis of Unknown Samples Check Result - Intensity Table (2/4)
For all these lines the L lines are also measured
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Analysis of Unknown Samples Check Result - Intensity Table (3/4)
11.48 Ka Lines 0.202
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Source: Retsch - The Sample (International Edition Number 5)
Layer Thickness (in µm), where 90% of the Fluorescence Radiation originates from (4/4) L Lines K Lines Source: Retsch - The Sample (International Edition Number 5)
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Topics Analysis of Unknown Samples Basic Features Advanced 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
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Analysis of Unknown Samples Check Result - Wrong Sample Weight (1/3)
Specification of Wrong Sample Weight ! Recalculate !
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Analysis of Unknown Samples Check Result - Wrong Sample Weight (2/3)
11.48 0.202 Correct SampleWeight
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Analysis of Unknown Samples Check Result - Wrong Sample Weight (3/3)
11.48 60.64 0.202 Since Version 5.04 99.6
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Topics Analysis of Unknown Samples Basic Features Advanced 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
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Enter * / Space to select / deselect Alternative Lines
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 !
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Analysis of Unknown Samples Check Result - Select Alternative Lines (2/2)
11.48 60.64 0.202 99.6
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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
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Analysis of Unknown Samples Background Shapes - Select Shape (1/8)
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Analysis of Unknown Samples Background Shapes - Selection Criteria (2/8)
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0 = Automatic Shape Selection 1 = Teflon Shape (recommended)
Analysis of Unknown Samples Background Shapes - Define Default Shape (3/8) 0 = Automatic Shape Selection 1 = Teflon Shape (recommended) Since Version 5
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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
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Analysis of Unknown Samples Background Shapes - Table of Shapes (4/8)
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Analysis of Unknown Samples Background Shapes - Shapes and Impurity Factors (5/8)
Not Set up Not Set up Impurity Factors Background Shapes
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Analysis of Unknown Samples Background Shapes - Make New Shape (6/8)
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Analysis of Unknown Samples Background Shapes - Select Sample (7/8)
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Analysis of Unknown Samples Background Shapes - Check / Refine Shape (8/8)
Fe Absorption Edge Smoothed Shape
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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
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Analysis of Unknown Samples - Oil Sample Conostan S-21 / 50ppm (1/5)
Last Element in first group Problem of Shape Neighbours in second group Overlapped by Rh Ka Lines Wrong Impurity Factors
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Wrong Impurity Factors for Oil Matrix
Analysis of Unknown Samples - Oil Sample Inappropriate Background Shape (2/5) Background too low Wrong Impurity Factors for Oil Matrix
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Analysis of Unknown Samples - Oil Sample Shape and Impurity Factors for Oil Matrix (3/5)
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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
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Analysis of Unknown Samples - Oil Sample Conostan S-21 / 50ppm with Oil Background (5/5)
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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
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Analysis of Unknown Samples Special Case - Chemplex 55 Elements Standard Look ahead in Background Calculation
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Analysis of Unknown Samples Special Case - Chemplex 55 Elements Standard Look ahead of 8 Lines (Default Setting)
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Analysis of Unknown Samples Special Case - Chemplex 55 Elements Standard (1/2) Look ahead of 20 Lines (Special Setting)
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Analysis of Unknown Samples Special Case - Chemplex 55 Elements Standard (2/2) Look ahead of 20 Lines (Special Setting)
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Topics Analysis of Unknown Samples Basic Features Advanced Features
Background Shapes Shadow Loss Special Cases Subset Programs Kappa Lists Small Samples
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Analysis of Unknown Samples Compensation for Grain Size Effects (1/2)
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Analysis of Unknown Samples Compensation for Grain Size Effects (2/2)
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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
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Analysis of Unknown Samples Special Cases - Unknown Area (1/2)
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Analysis of Unknown Samples Special Cases - Unknown Area (2/2)
Case 1: Unknown Area Same Result ! Case 0: Everything is known
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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
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Analysis of Unknown Samples Unknown Rest % (1/2)
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Analysis of Unknown Samples Unknown Rest % (2/2)
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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
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Analysis of Unknown Samples Unknown Dilution (1/2)
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Analysis of Unknown Samples Unknown Dilution (2/2)
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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
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Analysis of Unknown Samples Unknown g/cm2 (Monolayer) (1/6)
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Analysis of Unknown Samples Unknown g/cm2 (Monolayer) (2/6)
“Schmauchspuren” Residues of unburnt powder after a gun shot
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Analysis of Unknown Samples Unknown g/cm2 (Monolayer) (3/6)
La Lb Case 0 (Bulk Sample)
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Analysis of Unknown Samples Unknown g/cm2 (Monolayer) (4/6)
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Analysis of Unknown Samples Unknown g/cm2 (Monolayer) (5/6)
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Analysis of Unknown Samples Unknown g/cm2 (Monolayer) (6/6)
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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
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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)
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Analysis of Unknown Samples Unknown Masses/Area (Multilayer) (2/7)
Select Case 5 Calculate Background
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Analysis of Unknown Samples Unknown Masses/Area (Multilayer) (3/7)
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Analysis of Unknown Samples Unknown Masses/Area (Multilayer) (4/7)
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Analysis of Unknown Samples Unknown Masses/Area (Multilayer) (5/7)
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Analysis of Unknown Samples Unknown Masses/Area (Multilayer) (6/7)
Check !
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Analysis of Unknown Samples Unknown Masses/Area (Multilayer) (7/7)
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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
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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 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
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Subset Programs How to create a Subset
Counting Time = 0 will not be measured
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Subset Programs Example - PetroQuant (1/4)
Additives in Oil Ca, Zn, P, Mg, Mo ( ppm) Cl, S ( %) Si (few ppm) Following elements are sometimes present Na, K, Ba ( ppm) Cu, Fe ( ppm) Abrasion Elements ( ppm) Al, Ti, V, Cr, Mn, Fe, Ni, Cu, Ag, Sn, Sb, Pb Total Measuring Time : 11 minutes
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Subset Programs Example - PetroQuant (2/4)
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Subset Programs Example - PetroQuant (3/4)
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Subset Programs Example - PetroQuant (4/4)
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Topics Analysis of Unknown Samples Basic Features Advanced Features
Background Shapes Shadow Loss Special Cases Subset Programs Kappa Lists Principle Practical Example Small Samples
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Kappa Lists Principle - New Calibration derived from a Parent (1/3)
AnySample Parent Beads Daughter Alloys Parent Pressed Powder Steel Daughter © 2000 Omega Data Systems BV All Rights Reserved Denver conference W.K. de Jongh (ODS), Kurt Juchli (ARL)
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Kappa Lists Principle - New Calibration derived from a Parent (2/3)
Homogeneous Samples Beads Copy Kappa List Daughter Mineralogical Effects One or more Standards to firm up calibration of Major Elements Pressed Powder © 2000 Omega Data Systems BV All Rights Reserved Denver conference W.K. de Jongh (ODS), Kurt Juchli (ARL)
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Kappa Lists Principle - Create New Kappa List (3/3)
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Kappa Lists Practical Example (1/4)
Difference in Sensitivity Reduction between High and Low Crystal Angles versus Sample Surface Size (Opening of Sample Holder) 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 Angles High 2 Theta Angles Pd = Ir = 56.68 Rh = Pt = 54.91
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Kappa Lists Practical Example (2/4)
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Kappa Lists Practical Example (3/4)
15 mm 29 mm
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Kappa Lists Practical Example (4/4)
Adjusted Kappas
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Kappa Lists Practical Example - Explanation (1/2)
Normal Sample Collimator Mask Collimator Mask Crystal at higher angles Crystal at lower angles
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Kappa Lists Practical Example - Explanation (2/2)
Small Sample Small Sample Collimator Mask Collimator Mask Crystal at higher angles Crystal at lower angles
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Topics Analysis of Unknown Samples Basic Features Advanced Features
Background Shapes Shadow Loss Special Cases Subset Programs Kappa Lists Small Samples
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Small Samples Irregular Shaped Small Sample
Polypropylene Insert to keep sample in place
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Small Samples Stainless Steel Drillings
Lowest Angle Element Drill. 90 Drill.180 Drill.360 Pressed Mn % 1.34 1.37 1.38 Si % 0.36 0.30 0.37 0.41 Cr % 18.12 18.37 18.26 18.18 Ni % 10.58 10.61 10.60 10.79 Mo % 1.91 1.47 1.80 1.59 Cu % 0.06 0.08 Ti % 0.021 0.012 0.011 0.014 Fe % 66.4 67.3 67.0 Nb % 0.009 Drill.90, Drill.180 and Drill.360 were analysed under helium environment with a film support (6µ PP) The pressed sample was analysed under vacuum
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Thank you very much for your Attention
Kurt Juchli Applied Research Laboratories Ecublens Switzerland Thermo ARL
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Crystal at higher angles Crystal at lower angles
Analysed Surface Collimator Mask Collimator Mask Crystal at higher angles Crystal at lower angles
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