17
Interferences: Pathological and Otherwise John Donovan Micro Analytical Facilit CAMCO (Center for Advanced Materials Characterization in ORegon University of Orego Eugene, O (541)-346-4632 [email protected] www.epmalab.uoregon.edu

Interferences: Pathological and Otherwise John Donovan Micro Analytical Facility CAMCOR (Center for Advanced Materials Characterization in ORegon) University

Embed Size (px)

Citation preview

Page 1: Interferences: Pathological and Otherwise John Donovan Micro Analytical Facility CAMCOR (Center for Advanced Materials Characterization in ORegon) University

Interferences: Pathological and Otherwise

John Donovan Micro Analytical Facility

CAMCOR

(Center for Advanced Materials

Characterization in ORegon)

University of OregonEugene, OR

(541)[email protected]

www.epmalab.uoregon.edu

Page 2: Interferences: Pathological and Otherwise John Donovan Micro Analytical Facility CAMCOR (Center for Advanced Materials Characterization in ORegon) University

Matrix Correction

stdistd

i

unkiunk

i CI

IC

Ciunk

Iiunk

Iistd

ZAFiunk

ZAFistd Ci

std

from Fournelle

Page 3: Interferences: Pathological and Otherwise John Donovan Micro Analytical Facility CAMCOR (Center for Advanced Materials Characterization in ORegon) University

Matrix Iteration...

Test for ZAF or -

z convergenc

e of the compositio

n

Correct x-ray intensities for deadtime, off-peak

background, beam drift and standard drift.

Calculate first approximation of composition based on raw k-

ratios

Calculate ZAF or -z correction factors based on

estimated composition

Output results

Sub TestMatrixCalculateMatrix(mLastElm As Long, mLastChan As Long, mElements() As Long, mXrays() As Long, mCations() As Double, mOxygens() As Double, mAtomicWts() As Double, mAlpha1() As Double, mAlpha2() As Double, mAlpha3() As Double, mUnkcts() As Double, mStdPercents() As Double, mStdcts() As Double, mStdBetas() As Double, mCalculationFlags() As Long, mCalculationPercents() As Double, mUnkBetas() As Double, mUnkPercents() As Double, mOldPercents() As Double, mTotal As Double)' Calculate matrix correction using a Bence-Albee iteration' mLastElm& = number of emitting elements (measured intensities)' mLastChan& = number of absorbing elements (not measured, only specified or calculated weight percents)' mElements&() = element atomic numbers (1 to mLastChan&)' mXrays&() = xray lines (1=Ka, 2=Kb, 3=La, 4=Lb, 5=Ma, 6=Mb, 7=absorber only) (1 to mLastChan&)' mCations#() = number of stoichiometric cations (1 to mLastChan&)' mOxygens#() = number of stoichiometric oxygens (1 to mLastChan&)' mAtomicWts#() = atomic weights (1 to mLastChan&)' mAlpha1#(), mAlpha2#(), mAlpha3#() = matrix of alpha factor parameters' mUnkcts#() = measured unknown intensities (1 to mLastElm&)' mStdcts#() = standard intensities (from call to MatrixGetMatrix, SETUP.MDB database) (1 to mLastElm&)' mStdPercents#() = standard percents (from call to MatrixGetMatrix, SETUP.MDB database) (1 to mLastElm&)' mStdbetas#() = standard beta factors (from call to MatrixGetMatrix) (1 to mLastElm&)' mCalculationFlags&() = absorbing element calculation flags (0 = specified concentration, 1 = by difference, 2 = by stoichiometry)' mCalculationPercents&() = absorbing element specified weight percents (1 to mLastChan&)'' Returned parameters and arrays' mUnkBetas#() = returned unknown beta factors (1 to mLastElm&) (must be initialized to 1.0)' mUnkPercents#() = corrected weight percents (matrix corrected) (1 to mLastChan&)' mOldPercents#() = original weight percents (1 to mLastChan&)' mTotal# = weight percent total

ierror = FalseOn Error GoTo TestMatrixCalculateMatrixError

Const MAXMATRIXITER& = 30Const MATRIXMINTOLER# = 0.005 ' in weight percentConst MATRIXMINTOTAL# = 0.001 ' in weight percent

Dim bDifferenceElement As Boolean, bStoichiometricElement As BooleanDim nDifferenceElement As Long, nStoichiometricElement As LongDim chan As LongDim MatrixIter As Long

Dim maxdiff As Double, diff As DoubleDim stoichiometricoxygen As Double

ReDim p(1 To mLastChan&) As Double ' stoichiometric ratio variable

' Determine if there is an element by diference and/or an element by stoichiometryFor chan& = mLastElm& + 1 To mLastChan&If mCalculationFlags&(chan&) = 1 Then ' element by differencebDifferenceElement = TruenDifferenceElement& = chan&End If

If mCalculationFlags&(chan&) = 2 Then ' element by stoichiometrybStoichiometricElement = TruenStoichiometricElement& = chan&End IfNext chan&

' Bence-Albee iteration begins hereMatrixIter& = 1#Do Until MatrixIter& >= MAXMATRIXITER&

' Calculate weight percents for analyzed elementsFor chan& = 1 To mLastElm&If mUnkBetas#(chan&) <= 0# Then GoTo TestMatrixCalculateMatrixBadUnkBetasIf mStdPercents#(chan&) <= 0# Then GoTo TestMatrixCalculateMatrixBadStdPercentsIf mStdcts#(chan&) <= 0# Then GoTo TestMatrixCalculateMatrixBadStdCountsIf mStdBetas#(chan&) <= 0# Then GoTo TestMatrixCalculateMatrixBadStdBetas

mUnkPercents#(chan&) = (mUnkcts#(chan&) * mStdPercents#(chan&) * mUnkBetas#(chan&)) / (mStdcts#(chan&) * mStdBetas#(chan&))Next chan&

' Load specified concentrations (could be zero wt% by default)For chan& = mLastElm& + 1 To mLastChan&mUnkPercents#(chan&) = 0#If mCalculationFlags&(chan&) = 0 ThenmUnkPercents#(chan&) = mCalculationPercents#(chan&)End IfNext chan&

' Sum stoichiometric oxygen (do not include oxygen from element by difference)If bStoichiometricElement Thenstoichiometricoxygen# = 0#For chan& = 1 To mLastChan&If chan& <> nStoichiometricElement& Thenp#(chan&) = mOxygens#(chan&) / mCations#(chan&) * mAtomicWts#(nStoichiometricElement&) / mAtomicWts#(chan&)stoichiometricoxygen# = stoichiometricoxygen# + mUnkPercents#(chan&) * p#(chan&)End IfNext chan&mUnkPercents#(nStoichiometricElement&) = stoichiometricoxygen#End If

' Total all weight percents for difference element calculationmTotal# = 0#For chan& = 1 To mLastChan&mTotal# = mTotal# + mUnkPercents#(chan&)Next chan&

' Calculate element by difference based on current weight percentsIf bDifferenceElement ThenIf mTotal# < 100# ThenmUnkPercents#(nDifferenceElement&) = 100# - mTotal#If bStoichiometricElement Thenp#(nDifferenceElement&) = mOxygens#(nDifferenceElement&) / mCations#(nDifferenceElement&) * mAtomicWts#(nStoichiometricElement&) / mAtomicWts#(nDifferenceElement&)mUnkPercents#(nDifferenceElement&) = mUnkPercents#(nDifferenceElement&) / p#(nDifferenceElement&)stoichiometricoxygen# = stoichiometricoxygen# + mUnkPercents#(nDifferenceElement&) * p#(nDifferenceElement&)mUnkPercents#(nStoichiometricElement&) = stoichiometricoxygen#End IfEnd IfmTotal# = 100#End If

' Check for decent totalIf mTotal# <= MATRIXMINTOTAL# Then GoTo TestMatrixCalculateMatrixBadTotal

' Compute change in weight percents since last iterationmaxdiff = 0#For chan& = 1 To mLastChan&diff# = Abs(mUnkPercents#(chan&) - mOldPercents#(chan&))If diff# > maxdiff# Then maxdiff# = diff#mOldPercents#(chan&) = mUnkPercents#(chan&)Next chan&

' Check for convergenceIf maxdiff# <= MATRIXMINTOLER# Then GoTo 6000

' Compute sum of alpha factors for each element (beta factors)Call TestMatrixCalculateBetaFactors(mLastElm&, mLastChan&, mAlpha1#(), mAlpha2#(), mAlpha3#(), mUnkPercents#(), mUnkBetas#(), mTotal#)If ierror Then Exit Sub

' Not converged, try againMatrixIter& = MatrixIter& + 1Loop

' If we get here, convergence failedMsgBox "WARNING in TestMatrixCalculateMatrix- Convergence failed", vbOKOnly + vbExclamation, "TestMatrixCalculateMatrix"

' Converged, calculate total6000:mTotal# = 0#For chan& = 1 To mLastChan&mTotal# = mTotal# + mUnkPercents#(chan&)Next chan&

Exit Sub

' ErrorsTestMatrixCalculateMatrixError:MsgBox Error$, vbOKOnly + vbCritical, "TestMatrixCalculateMatrix"ierror = TrueExit Sub

TestMatrixCalculateMatrixBadUnkBetas:msg$ = "WARNING in TestMatrixCalculateMatrix- Bad unknown beta factor for element" & Str$(mElements&(chan&)) & " " & Str$(mXrays&(chan&))MsgBox msg$, vbOKOnly + vbExclamation, "TestMatrixCalculateMatrix"ierror = TrueExit Sub

TestMatrixCalculateMatrixBadTotal:msg$ = "WARNING in TestMatrixCalculateMatrix- Insufficient total"MsgBox msg$, vbOKOnly + vbExclamation, "TestMatrixCalculateMatrix"ierror = TrueExit Sub

TestMatrixCalculateMatrixBadStdPercents:msg$ = "Insufficient standard percents for element" & Str$(mElements&(chan&)) & " " & Str$(mXrays&(chan&))MsgBox msg$, vbOKOnly + vbExclamation, "TestMatrixCalculateMatrix"ierror = TrueExit Sub

TestMatrixCalculateMatrixBadStdCounts:msg$ = "Insufficient standard counts for element" & Str$(mElements&(chan&)) & " " & Str$(mXrays&(chan&))MsgBox msg$, vbOKOnly + vbExclamation, "TestMatrixCalculateMatrix"ierror = TrueExit Sub

TestMatrixCalculateMatrixBadStdBetas:msg$ = "Bad standard beta factor for element" & Str$(mElements&(chan&)) & " " & Str$(mXrays&(chan&))MsgBox msg$, vbOKOnly + vbExclamation, "TestMatrixCalculateMatrix"ierror = TrueExit Sub

End Sub

Yes

No

Sub TestMatrixCalculateBetaFactors(mLastElm As Long, mLastChan As Long, mAlpha1() As Double, mAlpha2() As Double, mAlpha3() As Double, mUnkPercents() As Double, mUnkBetas() As Double, mTotal As Double)' This routine accepts an array of weight percents and alpha factors and returns an array of beta factors

ierror = FalseOn Error GoTo TestMatrixCalculateBetaFactorsError

Dim i As LongDim emitter As Long, absorber As LongDim betafraction As Double

ReDim wtfractions(1 To mLastChan&) As Double

' Convert to weight fractionsIf mTotal# = 0# Then GoTo TestMatrixCalculateBetaFactorsBadTotalFor i& = 1 To mLastChan&wtfractions#(i&) = mUnkPercents#(i&) / mTotal#Next i&

' Calculate beta factors for "mLastElm" emitters and "mLastChan" absorbersFor emitter& = 1 To mLastElm&mUnkBetas#(emitter&) = 0#

For absorber& = 1 To mLastChan&betafraction# = (mAlpha1#(emitter&, absorber&) + wtfractions#(absorber&) * mAlpha2#(emitter&, absorber&) + wtfractions#(absorber&) ^ 2 * mAlpha3#(emitter&, absorber&)) * wtfractions#(absorber&)

' Sum beta factors fractionsmUnkBetas#(emitter&) = mUnkBetas#(emitter&) + betafraction#

Next absorber&Next emitter&

Exit Sub

' ErrorsTestMatrixCalculateBetaFactorsError:MsgBox Error$, vbOKOnly + vbCritical, "TestMatrixCalculateBetaFactors"ierror = TrueExit Sub

TestMatrixCalculateBetaFactorsBadTotal:msg$ = "Total percent equals zero, cannot calculate beta factors"MsgBox msg$, vbOKOnly + vbExclamation, "TestMatrixCalculateBetaFactors"ierror = TrueExit Sub

End Sub

Page 4: Interferences: Pathological and Otherwise John Donovan Micro Analytical Facility CAMCOR (Center for Advanced Materials Characterization in ORegon) University

Other Compositionally Dependent Corrections

•Quantitative Spectral Interference Calculations

•Mean Atomic Number (MAN) Based Backgrounds

•Volatile Intensity Corrections

•Water by Difference (specified element effects)

•Compound Area-Peak Factor (APF) Calculations

•Blank (Zero) Value Corrections for Trace Elements

Page 5: Interferences: Pathological and Otherwise John Donovan Micro Analytical Facility CAMCOR (Center for Advanced Materials Characterization in ORegon) University

Spectral Interferences

W avelength

Inte

nsity

Elem ent A (Interfered)

E lem ent B (Interfering)

E lem ent A + E lem ent B

Page 6: Interferences: Pathological and Otherwise John Donovan Micro Analytical Facility CAMCOR (Center for Advanced Materials Characterization in ORegon) University

Matrix IterationF low D iagram of the Q uantita tive Iterated Interference C orrection

C orrect the x-ray in tensities for deadtim e,off-peak background, beam drift and

standard drift.

C alculate firs t approxim ation ofcom position based on raw k -ratios from

the x-ray in tensities.

C alculate ZAF or z m atrix correctionfactors based on com position and correct

the concentrations.

C alculate quantita tive in terferencecorrection based on com position and

correct the x-ray in tensities.

T est for ZAF or zconvergence of the

concentrations.

Yes

N o

T est for quantita tiveinterference convergence

of the x-ray in tensities.

Yes

N o

O utput results to user.

sB

BsB

BuB

sB

AsB

AuB C

I

I

C

II

)(

)()()(

Gilfrich, et al., 1978

)(

)(][

][)(

][][ A

sA

AsBu

uB

sB

s

Au

us

sAu

A I

IZAF

CC

ZAFI

ZAFZAF

CC A

A

A

A

Eq. 1

Eq. 2

)(][

][)( A

sBu

uB

sB

s

AUB I

ZAF

C

C

ZAFI

A

A

Donovan, Rivers and Snyder, 1993

Page 7: Interferences: Pathological and Otherwise John Donovan Micro Analytical Facility CAMCOR (Center for Advanced Materials Characterization in ORegon) University

Differences Between Eq. 1 and Eq. 2Self-Interfering Analyses

3 Benitoite (BaTiSi3O9) is assumed stoichiometric : Si 20.38, Ba 33.15, Ti 11.69, O 34.8964 Shultenite (HAsPbO4) is assumed stoichiometric : Pb 59.69, As 21.58, O 18.44. The oxygen concentration was measured at 19.8 wt. % and included in the matrix correction calculations.

wt. % (nominal) wt. %(uncorrected)

wt. % (Eq. 1) wt. % (Eq. 2)

Ni K Fe KFe K Co K

Co 0.022 1

0.089 0.008 0.010 0.022 0.008

Ti K V V K Cr K

Cr 0.025 2

0.268 0.01 -0.020 0.021 0.010

Cascade Interference Analyses

1 SRM 1159 includes : Ni 48.2, Fe 51.0, C 0.007, Mn 0.30, P 0.003, S 0.003, Si 0.32, Cu 0.038, Cr 0.06, Mo 0.012 SRM 654b includes : Ti 88.974, Al 6.34, V 4.31, Fe 0.23, Si 0.045, Ni 0.028, Sn 0.023, Cu 0.004, Mo 0.013, Zr 0.008

wt. % (nominal) wt. %(uncorrected)

wt. % (Eq. 1) wt. % (Eq. 2)

Ba L Ti K(PET)

Ba 33.15 3

Ti 11.6933.26 .1811.71 .08

33.0811.59

33.08 .1811.59 .08

Pb L As K Pb 59.69 4

As 21.58106.20 .33 41.38 .27

19.64 6.60

61.25 1.9722.15 1.04

Pb L (cps) As K (cps) S K (cps)PbS 1473.3 1213.0 1453.3

GaAs 1624.7 1771.7 2.5

FeS 14.0 13.9 4986.9

Page 8: Interferences: Pathological and Otherwise John Donovan Micro Analytical Facility CAMCOR (Center for Advanced Materials Characterization in ORegon) University

Pathological InterferencesUn 10 Zn-ReSCN gr2TakeOff = 40 KiloVolts = 20 Beam Current = 20 Beam Size = 0

Results in Elemental Weight PercentsSPEC: O N C HTYPE: SPEC SPEC SPEC SPEC

AVER: 1.900 5.000 4.200 .200SDEV: .000 .000 .000 .000 ELEM: Cs Fe Zn Re S Se SUM 53 .000 .000 19.463 74.142 17.309 .000 122.214 55 .000 .007 20.459 74.986 16.357 .000 123.108 56 .000 .019 19.578 75.195 17.997 .000 124.089

AVER: .000 .009 19.833 74.774 17.221 .000 123.137SDEV: .000 .010 .545 .558 .824 .000SERR: .000 .006 .314 .322 .476 .000%RSD: .1 113.3 2.7 .7 4.8 .1STDS: 834 730 660 575 730 660

Results Based on 6 Atoms of reSPEC: O N C HTYPE: SPEC SPEC SPEC SPEC

AVER: 1.774 5.334 5.225 2.965SDEV: .013 .040 .039 .022

ELEM: Cs Fe Zn Re S Se SUM 53 .000 .000 4.486 6.000 8.134 .000 34.048 55 .000 .002 4.663 6.000 7.600 .000 33.518 56 .000 .005 4.450 6.000 8.339 .000 34.005

AVER: .000 .002 4.533 6.000 8.025 .000 33.857SDEV: .000 .003 .114 .000 .382 .000SERR: .000 .001 .066 .000 .220 .000%RSD: .8 113.2 2.5 .0 4.8 .8

Re la 1.43298Zn ka 1.43652

“Self-Interferring”

Page 9: Interferences: Pathological and Otherwise John Donovan Micro Analytical Facility CAMCOR (Center for Advanced Materials Characterization in ORegon) University

With Iterated Interference CorrectionUn 10 Zn-ReSCN gr2TakeOff = 40 KiloVolts = 20 Beam Current = 20 Beam Size = 0

Results in Elemental Weight PercentsSPEC: O N C HTYPE: SPEC SPEC SPEC SPEC

AVER: 1.900 5.000 4.200 .200SDEV: .000 .000 .000 .000 ELEM: Cs Fe Zn Re S Se SUM 53 .000 .000 6.325 65.726 17.333 .000 100.683 55 .000 .007 7.471 65.113 16.343 .000 100.233 56 .000 .019 6.188 66.949 18.029 .000 102.486

AVER: .000 .009 6.661 65.929 17.235 .000 101.134SDEV: .000 .010 .704 .935 .848 .000SERR: .000 .006 .407 .540 .489 .000%RSD: .1 113.3 10.6 1.4 4.9 .0STDS: 834 730 660 575 730 660

Results Based on 6 Atoms of reSPEC: O N C HTYPE: SPEC SPEC SPEC SPEC

AVER: 2.013 6.050 5.926 3.363SDEV: .028 .085 .084 .047

ELEM: Cs Fe Zn Re S Se SUM 53 .000 .000 1.645 6.000 9.189 .000 34.236 55 .000 .002 1.961 6.000 8.745 .000 34.274 56 .000 .006 1.580 6.000 9.383 .000 34.053

AVER: .000 .003 1.728 6.000 9.106 .000 34.188SDEV: .000 .003 .204 .000 .327 .000SERR: .000 .002 .118 .000 .189 .000%RSD: 1.3 112.3 11.8 .0 3.6 1.4

6 rhenium to 9 sulfur

Page 10: Interferences: Pathological and Otherwise John Donovan Micro Analytical Facility CAMCOR (Center for Advanced Materials Characterization in ORegon) University

Large magnitude “Self-Interferences”

Interfering Pair Wavelength Region (Å) Approximate Overlap (% @ 50/50)Ba L Ti K 2.7 0.8 - 0.2Pb L As K 1.17 150 - 65

Hg L Ge K 1.25 120 - 15Ir L Ga K 1.34 70 - 30Re L Zn K 1.43 140 - 60Er L Co K 1.78 110 - 50Eu L Mn K 2.1 15 - 5In L K K 3.74 50 - 20Th M Ag L 4.13 30 - 60Bi M Tc L 5.1 50 - 70Mo L S K 5.4 30 - 15

Page 11: Interferences: Pathological and Otherwise John Donovan Micro Analytical Facility CAMCOR (Center for Advanced Materials Characterization in ORegon) University

Typical (nasty) Interference, but first...

~600 PPM Sr

Labradorite (Lake Co.)

LP

ET

cp

s (

20

se

c p

er

po

int)

Sr (2) Spectrometer

0.0

123.8

75867.1 76399.7 76932.4 77465.0 77997.7 78530.3 79063.0 79595.6 80128.3 80660.9 81193.5

4943. -4517.

Ca SKA4 II Ca SKA3` II Ca SKA3 II Ca SKA3`` II Ca SKA` II Ca SKA`` II

Ca KA1 II

Ba SLG1` III

Ca KA2 II

Ba LG1 III

Si SKB^5 Si SKBX Si SKBN

Si KB1

Si KB3

Rb LB3

Sr SLA7 K SKB^4 II

Sr SLA6 Si SKB`

Rb LB4

Sr SLA5 Sr SLA4 Sr SLA3

Sr LA1

Sr LA2

K SKB`` II K SKB^5 II

K KB1 II

K KB3 II

K SKB` II Fe SKB IV

K SKBN II Fe SKB`` IV

Si SKA6 Si SKA7

Fe KB3 IV

Fe KB1 IV

Si SKA5 Rb SLB1``

Fe SKB` IV

Si SKA4

Si SKA3`

Rb LB1

Si SKA3

Labradorite (Lake Co.)

LP

ET

cp

s (

20

se

c p

er

po

int)

Sr (2) Spectrometer

0.0

1919.4

75939.5 76428.3 76917.1 77405.9 77894.7 78383.5 78872.3 79361.1 79849.9 80338.8 80827.6

4943. -4517.

Ca SKB`` II Ca SKB^5 II

Ca KB1 II Ca KB3 II

Ca SKB` II Ca SKBN II Ba Ll II Sr LB3

Sr LB4 Ba LG3 III Ba SLG10 III Sr SLB1``

Sr LB1

Si SKB^4 Ca SKA4 II Ca SKA3` II Ca SKA3 II Ca SKA3`` II Ca SKA` II Ca SKA`` II

Ca KA1 II

Ba SLG1` III

Ca KA2 II

Ba LG1 III Si SKB^5 Si SKBX Si SKBN

Si KB1 Si KB3 Rb LB3

Sr SLA7 K SKB^4 II Sr SLA6 Si SKB` Rb LB4 Sr SLA5 Sr SLA4 Sr SLA3

Sr LA1

Sr LA2

K SKB`` II K SKB^5 II

K KB1 II K KB3 II

K SKB` II Fe SKB IV K SKBN II Fe SKB`` IV Si SKA6 Si SKA7 Fe KB3 IV Fe KB1 IV

Si SKA5 Rb SLB1`` Fe SKB` IV

Si SKA4

Si SKA3`

Rb LB1

Si SKA3

Si SKA` Si SKA``

Si KA1

Si KA2

Ba SLB2^1 III Fe SKBN IV Ba SLB2^2 III Ba SLB2^A III Ba SLB2^B III

Ba LB2 III

Rb SLA7 Rb SLA6 Rb SLA5 Rb SLA4 Rb SLA3

Rb LA1

Rb LA2

20 keV100 nAPET

Page 12: Interferences: Pathological and Otherwise John Donovan Micro Analytical Facility CAMCOR (Center for Advanced Materials Characterization in ORegon) University

Are we measuring background yet?Labradorite (Lake Co.)

LP

ET

cp

s (2

0 se

c p

er p

oin

t)

Sr (2) Spectrometer

0.00

3173.02

75892.5 76659.7 77426.9 78194.1 78961.4 79728.6 80495.8 81263.0 82030.3 82797.5 83564.7

4945. -4515.

Ca SKB`` II Ca SKB^5 II

Ca KB1 II

Ca KB3 II

Ca SKB` II Ca SKBN II

Ba Ll II

Sr LB3

Sr LB4

Ba LG3 III

Ba SLG10 III

Sr SLB1``

Sr LB1

Si SKB^4 Ca SKA4 II Ca SKA3` II Ca SKA3 II Ca SKA3`` II Ca SKA` II Ca SKA`` II

Ca KA1 II

Ba SLG1` III

Ca KA2 II

Ba LG1 III

Si SKB^5 Si SKBX Si SKBN

Si KB1

Si KB3

Rb LB3

Sr SLA7 K SKB^4 II Sr SLA6 Si SKB`

Rb LB4

Sr SLA5 Sr SLA4 Sr SLA3

Sr LA1

Sr LA2

K SKB`` II K SKB^5 II

K KB1 II

K KB3 II

K SKB` II Fe SKB IV

K SKBN II Fe SKB`` IV

Si SKA6 Si SKA7

Fe KB3 IV

Fe KB1 IV

Si SKA5 Rb SLB1``

Fe SKB` IV

Si SKA4

Si SKA3`

Rb LB1

Si SKA3

Si SKA` Si SKA``

Si KA1

Si KA2

Ba SLB2^1 III Fe SKBN IV Ba SLB2^2 III Ba SLB2^A III Ba SLB2^B III

Ba LB2 III

Rb SLA7 Rb SLA6 Rb SLA5 Rb SLA4 Rb SLA3

Rb LA1

Rb LA2

Labradorite (Lake Co.)

LP

ET

cp

s (

20

se

c p

er

po

int)

Sr (2) Spectrometer

0.0

55.8

75767.8 76557.5 77347.3 78137.0 78926.7 79716.5 80506.2 81296.0 82085.7 82875.4 83665.2

4945. -4515.

Page 13: Interferences: Pathological and Otherwise John Donovan Micro Analytical Facility CAMCOR (Center for Advanced Materials Characterization in ORegon) University

How about now?Labradorite (Lake Co.)

LP

ET

cp

s (

20

se

c p

er

po

int)

Sr (2) Spectrometer

0.0

1155.8

72115.3 73274.0 74432.7 75591.4 76750.1 77908.8 79067.5 80226.2 81384.9 82543.6 83702.3

4945. -4515.

Labradorite (Lake Co.)

LP

ET

cp

s (

20

se

c p

er

po

int)

Sr (2) Spectrometer

0.0

189.2

72172.3 73338.2 74504.0 75669.8 76835.6 78001.5 79167.3 80333.1 81499.0 82664.8 83830.6

4945. -4515.

Page 14: Interferences: Pathological and Otherwise John Donovan Micro Analytical Facility CAMCOR (Center for Advanced Materials Characterization in ORegon) University

Polygonization...

Page 15: Interferences: Pathological and Otherwise John Donovan Micro Analytical Facility CAMCOR (Center for Advanced Materials Characterization in ORegon) University

Labradorite (Lake Co.)

TAP

cps

(20

sec

per p

oint

)

Sr (1) Spectrometer

15.3

351.6

22485.60 23745.85 25006.10 26266.34 27526.59 28786.84 30047.09 31307.34 32567.59 33827.84 35088.09

7649. -1590.

Can we measure “true” background between Al and Si ka peaks?

Page 16: Interferences: Pathological and Otherwise John Donovan Micro Analytical Facility CAMCOR (Center for Advanced Materials Characterization in ORegon) University

Results

SiO2, WITH Interference Correction:

Sr (la) Sr (la) Sr (la) Sr (la)TAP LPET LPET TAP

Average: 0.003 0.002 0.000 -0.001Std Dev: 0.012 0.001 0.004 0.003

SiO2, WITHOUT Interference Correction:

Sr (la) Sr (la) Sr (la) Sr (la)TAP LPET LPET TAP

Average: 0.505 0.071 0.070 0.399Std Dev: 0.010 0.001 0.003 0.004

Page 17: Interferences: Pathological and Otherwise John Donovan Micro Analytical Facility CAMCOR (Center for Advanced Materials Characterization in ORegon) University

Conclusions

•Quantitative interference corrections require accurate background measurements

•Even “pathological” cascade and self-interfering interference correction are routine using iterative

correction methods