Omnian PANalytical Day 2009 Final

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    Omnian

    The benchmark

    Standardless analysis

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    Content

    Analytical strategies Introduction standardless analysis Omnian advantages Omnian features

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    Analytical strategies

    Highest precision

    Highest accuracy

    Highest measurement efficiency

    Full traceability

    Full flexibility

    Good accuracy without in-type standards Good comparative data/trend analysis

    / Ideal screening tool

    Conventional calibration or Standardless analysis?

    PK?

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    Introduction Standardless analysis

    Complete composition of most types of unknownmaterials can be quantified with a single calibrationprogram Calibration set up with a selected range of reference

    materials to calibrate the instrument response

    Covers all common elements that can be measured by XRF:by default O-U O-UXRF

    Makes use of (a form of) Fundamental Parameter (FP)

    calculations to correct for all sample-matrix specificproperties

    Handles most types of samples, including solids, pressedpowders, fused beads, loose powders and liquids

    ,

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    Introduction Standardless analysis

    How is a quantitative result obtained?

    Two steps: 1.

    Determine which elements are present in the

    sample

    2.

    Calculate the concentration of each element that is

    present. This gives the total sample composition

    NOTE: A conventional analysis only has to deal withstep 2, because the elements of interest are alreadyknown.

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    Omnian advantages

    The right result every time Easy to use Problem solving power foryour analytical challenges

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    The right result every time The basis of a good result is toobtain accurate net intensities

    Having advanced algorithms forthe determination of background,peak search & match and line-

    overlaps

    Using a scan-based measurementprogram, for a comprehensivepicture of the sample

    but can be combined with peakmeasurements for higher precision andlower detection limits for key elements

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    The right result every time By using scans a comprehensive picture of thesample is given:

    Allowing both qualitative and quantitative

    analysis

    Quick visual screening or full quantification

    Providing an accurate background profile

    Superior to the estimations obtained from fixedbackground positions

    Providing a view of all peaks and backgrounds across theperiodic table

    Reduces the chance of incorrect element identification

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    Easy to use Handles almost all sample types with one calibrationprogram

    Solids, pressed powders, fused beads, loose powders andliquids

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    Easy to use

    Scaleable from routine to advanced usage

    Easy operation procedure for daily routine usage Advanced functions for experienced users to fine tune analytical

    parameters

    Results can be viewed inthe SuperQ results viewerSuperQ

    Easy comparison of data Print or transfer to LIMS

    system LIMS

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    Easy to use daily operation process 1.

    Place your sample on the

    Axios

    changer

    1.

    Simply assign the Omnian

    application to the chosensample location Omnian

    2.

    Fill in sample preparation

    details if applicable

    1.

    Measure!

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    Easy to use daily operation process After measurement completionthe result is displayed

    automatically

    For further results evaluation,

    the SuperQ results viewer is used uperQ

    For comparison of different

    analyses For applying statistics For editing of results

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    Problem solving power R&D analysis tool

    For analyses of all types of samples For detailed investigation of results

    Failure analysis

    To identify steps in a process where things might gowrong, e.g by analyzing:

    A particular bolt or screw A powder that was found in an instrument; itmight come from components wear

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    Problem solving power Comparative analysis For comparison of different samples

    To distinguish samples on matrix differences (e.g. stainless vs.low-alloy steel or PE vs. PVC polymer) PE PVC

    Helps to monitor and steer your process by comparingsamples from different batches

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    Omnian features Advanced technology Boosting the accuracy with ASC

    FastScan

    analysis

    Easy data retrieval

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    Advanced technology Finite thickness characteristics High-energy lines will have a larger

    penetration

    depth in the sample than low

    energy lines

    The penetration depth in light matrices is

    larger than in heavy matrices

    FP corrects in case the sample is not infinite

    thick for all measured energies

    Steel

    Irradiated and detected

    (Penetration depth)

    Not irradiated and detected

    OilOmnians advanced FP algorithms dealwith:

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    Irradiated and detected

    Not irradiated and detected

    Advanced technology Fluorescence Volume Geometry (FVG)

    The irradiated area of a light-matrixsample is not only determined by thepenetration depth

    It is also determined by the geometry ofthe optical path

    FP corrects for the FVG effect

    It takes into account the real geometry ofthe irradiated area, which is far morecomplex than the wedge-shape as drawnin the picture

    Omnians advanced FP algorithmsdeal with:

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    Example FVG and Finite Thickness effect

    Polymer CRM: BCR681k

    2 mm

    FT

    (16 mm)Cd-Ka (

    )

    FVG/ FT

    Cd-Ka in thick PE sample

    0

    20

    40

    60

    80

    100

    120

    140

    160

    With FVG and FT No FVG, with FT No FVG, No FT

    Concentration(ppm)

    Certified

    Measured

    BCR 681k Certified 1 disc

    1 disc, no

    FTElement Conc. (ppm) Conc. (ppm) Conc. (ppm)

    S 630 589 581

    Cl 800 927 914

    Cr 100 102 98

    As 29.1 38 18Br 770 809 300

    Cd 137 148 19

    Sb (La) 99 77 75

    Hg 23.7 20 10

    Pb 98 108 36

    FVG

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    Example FVG and Finite Thickness effect The scans show the bigdifferences in intensity

    between the 1 and 8

    disc measurements

    This all needs to be

    corrected for! 1 8

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    Advanced technology

    FP calculates the Dark Matrix compounds from the measuredCompton-scattered tube intensity

    This Compton intensity is reversely proportional to the density of thesample

    A heavy

    matrix (e.g. Copper) will have low Compton scatter whereas a light

    matrix (e.g. B4

    C) will have a high Compton scatter:B4

    C

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    Example Calculation of Dark Matrix compound

    Example: B in glass

    This clearly indicates that using the

    Compton intensity gives a far moreaccurate result

    Example: LOI in Limestone

    There is not much difference between

    calculating LOI as balance or from theCompton line, but: this comparisongives a clear indication of thecorrectness of the results!

    ,NBS 1411, glass

    Certified

    (wt%

    Measured

    (wt%

    Measured

    (wt%B2O3 10.94 Compton 10.1 Balance 20.2

    F ~0.5 0 0

    Na2O 10.14 11.1 10.3

    MgO 0.33 0.32 0.29

    Al2O3 5.68 6.04 5.43

    SiO2 58.04 57.9 51.6

    K2O 2.97 2.7 2.33

    CaO 2.18 2.2 1.89

    Fe2O3 0.05 0.059 0.049

    ZnO 3.85 4.04 3.36

    SrO 0.09 0.092 0.076

    BaO 5 5.33 4.35

    TiO2 0.02 0 0

    GBW07215a, Limestone fused beadCertified

    (wt%)

    Measured

    (wt%)

    Measured

    (wt%

    Na2O 0.072 0.072

    MgO 2.29 2.266 2.262

    Al2O3 0.77 0.812 0.811

    SiO2 1.8 1.951 1.947SO3 0.755 0.716 0.714

    K2O 0.168 0.134 0.133

    CaO 51.2 51.31 51.041

    Fe2O3 0.446 0.571 0.562

    SrO 0.041 0.039

    L.O.I.: Compton 40.549 Balance42.42

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    Example Using ASC

    Use ASC for calibration lines ofAl, Si and Ca All results clearly improve!

    ASCAlSi a

    Use of ASC increases theaccuracy Especially for Si

    Rawmix pressed pellet

    ASC Default

    Certified

    (wt%

    Measured

    (wt%

    Measured

    (wt%Na2O 0.202 0.206 0.205

    MgO 1.504 1.267 1.252

    Al2O3 3.194 3.358 2.591

    SiO2 12.726 13.331 10.547

    P2O5 0.118 0.082 0.077

    SO3 0.631 0.595 0.56K2O 0.608 0.529 0.494

    CaO 44.06 44.778 39.85

    TiO2 0.314 0.307 0.278

    MnO 0.054 0.043 0.038

    Fe2O3 2.035 2.063 1.673

    SrO 0.074 0.07 0.063

    CO2 34.48 33.159 42.177

    CKD 238 Al alloy

    ASC Default

    Certified

    (wt%

    Measured

    (wt%

    Measured

    (wt%)Mg 0.32 0.296 0.301

    Si 11.78 12.083 13.949

    Ti 0.16 0.163 0.14

    Cr 0.004 0.004

    Mn 0.145 0.138 0.133

    Fe 0.56 0.584 0.579Ni 0.03 0.021 0.025

    Cu 0.37 0.395 0.474

    Zn 0.32 0.236 0.307

    Ga 0.008 0.008

    Zr 0.001 0.001

    Pb 0.007 0.007

    Al (bal) 86.064 84.071

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    FastScan analysis

    FastScan

    analysis is a unique feature of Omnian

    coupled with

    an Axios

    spectrometer OmnianAxios

    For a quick determination of all majors and minors

    For samples that are likely to be damaged by X-rays

    X

    With a measurement time of about 1 minute the scan program

    covers the complete periodic table 1

    Combining FastScan

    with selected peak

    measurements, the accuracy for critical or low-

    concentration elements canbe

    increased

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    Easy data retrieval Omnian is built into the proven SuperQ

    analysis software platformOmnian

    SuperQ Results fully integrate into SuperQ

    results viewers

    SuperQ

    Easy comparison of data

    Print or transfer to files or LIMSLIMS Default measurement program can be easily extended with

    extra scans or peak measurements

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    Omnian the benchmark With Omnian: Omnian You get the right results every time with an easy to use package

    with problem solving power for your analytical challenges!

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    Omnian

    Application examples

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    Application example Aluminum alloys

    Default calibration is used

    CKD 236 Al alloy CKD 240 Al alloy CKD 242 Al alloy CKD 245 Al alloyDefault Default Default Default

    Certified

    (wt%)

    Measured

    (wt%)

    Certified

    (wt%)

    Measured

    (wt%

    Certified

    (wt%)

    Measured

    (wt%)

    Certified

    (wt%)

    Measured

    (wt%

    Mg 0.21 0.212 0.66 0.669 7.50 7.533 4.39 4.491

    Si 7.46 7.849 10.13 11.468 0.33 0.376 1.80 1.932

    Ti 0.025 0.027 0.07 0.058 0.10 0.087

    Mn 0.095 0.088 0.27 0.27 0.01 0.005 0.52 0.498

    Fe 0.23 0.227 0.45 0.452 0.05 0.051 0.74 0.727

    Ni 0.36 0.361 0.91 1.069 0.209

    Cu0.21 0.237 0.7 0.831 0.005 0.008 0.19 0.225

    Zn 0.05 0.041 0.06 0.059 0.01 0.019 0.14 0.198

    Ga 0.007 0.006 0.006 0.008

    Zr 0.001 0.002 0.001 0.023

    Al (bal) 90.945 85.1 92.001 91.588

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    Application example failure analysis

    Metal drillings

    Pressed in boric acid

    Default calibration is used

    The results are obtained by

    normalizing to 100 %00%

    Certified Measured

    Element (%) (%)

    Si 0.42 0.889

    P 0.016 0.01

    S 0.016 0.058

    V 0.029

    Cr 15.2 16.008

    Mn 0.78 0.789

    Fe 74.701

    Co 0.04 0.034

    Ni 6.26 7.003

    Cu 0.175As 0.023

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