Man versus off peak background measurements
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MAN versus Off-peak Background Measurements. What Is It Good For? Saving TIME!. How Much Time?. 186 seconds w/ Off-Peaks. 94 seconds w/ MAN. What Else is it Good For?. Avoiding Off-Peak Interferences Spectrometer Reproducibility Issues Sensitive Samples Quantitative Imaging

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MAN versus Off-peak Background Measurements

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Man versus off peak background measurements

MAN versus Off-peak Background Measurements

  • What Is It Good For?

    Saving TIME!


How much time

How Much Time?

186 seconds w/ Off-Peaks

94 seconds w/ MAN


What else is it good for

What Else is it Good For?

  • Avoiding Off-Peak Interferences

  • Spectrometer Reproducibility Issues

  • Sensitive Samples

  • Quantitative Imaging

  • Avoiding Wear and Tear on Spectrometers


Avoiding off peak interferences

Avoiding Off-Peak Interferences

By not measuring off-peak intensities in samples of unknown composition, one can eliminate even unforseen off-peak interferences.


Spectrometer reproducibility issues

Spectrometer Reproducibility Issues

  • Ultra High Precision Measurements

  • Handle spectrometer re-positioning problems

By reserving a spectrometer for a single MAN corrected element x-ray line (monochromator), one can obtain:


Sensitive samples

Sensitive Samples

Na/K Loss in glass (or Si/Al “grow-in”)

  • Everyone knows about sodium loss over time in some glasses and especially, hydrous phases- but did you know that sodium can also “grow-in”?


Man versus off peak background measurements

Sodium Calcium Silicate (cement “gel”)


Quantitative imaging

Quantitative Imaging

  • Eliminate acquisition time for off-peak intensity images and still obtain background corrected quantitative images

(512 x 2048 pixels @ .5 sec equals 6 days!)


How good is it

How Good Is It?

  • Major Elements

  • Minor Elements

  • Trace Elements

  • Comparison to Off-Peak Measurements

  • Matrix Issues (Low Z-bar vs High Z-bar)

  • Accuracy (reproducibility, drift, etc)


Comparison with off peak

Comparison with Off-peak

Off-Peak

20 kev, 20 nA, 5 um, 20 sec on, 20 sec off

St 305 Set 2 Labradorite (Lake Co.)

ELEM: Ca K Fe Ti Na Al Mn Ni O H Si SUM

AVER: 9.625 .102 .326 .023 2.841 16.529 .008 .003 46.823 .000 23.957 100.239

SDEV: .036 .008 .018 .014 .039 .032 .008 .005 .000 .000 .000

%RSD: .4 7.7 5.5 61.8 1.4 .2 89.4 165.7 .0 .0 .0

PUBL: 9.577 .100 .319 n.a. 2.841 16.359 .000 n.a. 46.823 n.a. 23.957 99.976

%VAR: .51 1.69 2.29 .00 .01 1.04 .00 .00 .00 .00 .00

DIFF: .048 .002 .007 .000 .000 .170 .000 .000 .000 .000 .000

STDS: 358 374 395 22 305 374 25 28 0 0 0

PKBG: 137.20 3.16 4.33 1.35 34.33 217.83 1.09 1.00 .00 .00 .00

MAN

St 305 Set 2 Labradorite (Lake Co.)

ELEM: Ca K Fe Ti Na Al Mn Ni O H Si SUM

AVER: 9.640 .100 .321 .023 2.864 16.543 .002 .004 46.823 .000 23.957 100.277

SDEV: .034 .007 .017 .012 .037 .033 .003 .005 .000 .000 .000

%RSD: .3 7.1 5.4 51.9 1.3 .2 140.3 126.3 .0 .0 .0

PUBL: 9.577 .100 .319 n.a. 2.841 16.359 .000 n.a. 46.823 n.a. 23.957 99.976

%VAR: .65 .23 .78 .00 .81 1.13 .00 .00 .00 .00 .00

DIFF: .063 .000 .002 .000 .023 .184 .000 .000 .000 .000 .000

STDS: 358 374 395 22 305 374 25 28 0 0 0

PKBG: 171.37 3.06 4.10 1.33 47.17 258.11 1.00 .99 .00 .00 .00


High z bar off peak comparison

High Z-bar Off Peak Comparison

Off-Peak

20 kev, 20 nA, 5 um, 20 sec on, 20 sec off

St 396 Set 2 Chromite (UC # 523-9)

ELEM: Ca K Fe Ti Na Al Mn Ni O H Cr SUM

AVER: .002 .004 20.392 .333 .006 8.004 .162 .087 33.042 .000 31.905 100.349

SDEV: .003 .005 .109 .021 .009 .036 .013 .014 .000 .000 .000 .000

%RSD: 114.0 129.1 .5 6.5 156.9 .5 8.0 15.9 .0 .0 .0 .0

PUBL: n.a. n.a. 20.692 .300 n.a. 7.690 .225 n.a. 33.042 n.a. 31.905 100.266

%VAR: .00 .00 -1.45 10.84 .00 4.09 -28.03 .00 .00 .00 .00 .00

DIFF: .000 .000 -.300 .033 .000 .314 -.063 .000 .000 .000 .000 .000

STDS: 358 374 395 22 305 374 25 28 0 0 0 0

PKBG: 1.00 1.04 101.90 4.90 1.01 73.21 2.07 1.44 .00 .00 .00 .00

MAN

St 396 Set 2 Chromite (UC # 523-9)

ELEM: Ca K Fe Ti Na Al Mn Ni O H Cr SUM

AVER: .001 .001 20.441 .346 .007 7.976 .155 .087 33.042 .000 31.905 100.372

SDEV: .002 .002 .109 .016 .009 .036 .014 .008 .000 .000 .000 .000

%RSD: 316.2 223.9 .5 4.5 118.4 .5 9.1 9.0 .0 .0 .0 .0

PUBL: n.a. n.a. 20.692 .300 n.a. 7.690 .225 n.a. 33.042 n.a. 31.905 100.266

%VAR: .00 .00 -1.21 15.40 .00 3.72 -31.27 .00 .00 .00 .00 .00

DIFF: .000 .000 -.251 .046 .000 .286 -.070 .000 .000 .000 .000 .000

STDS: 358 374 395 22 305 374 25 28 0 0 0 0

PKBG: .98 .98 133.63 5.76 1.04 57.37 1.97 1.44 .00 .00 .00 .00


Drift issues in man

Drift Issues in MAN

Drift array background intensities for standards:

ELMXRY: ca ka k ka fe ka ti ka na ka al ka mn ka ni ka

MOTCRS: 2 PET 2 PET 4 LIF 3 LIF 1 TAP 1 TAP 3 LIF 4 LIF

STDASS: 358 374 395 22 305 374 25 28

19.3 15.7 33.0 20.3 9.3 28.5 25.1 46.8

20.0 15.6 33.0 21.2 9.9 28.9 25.8 47.5

Drift array standard intensities (background corrected):

ELMXRY: ca ka k ka fe ka ti ka na ka al ka mn ka ni ka

MOTCRS: 2 PET 2 PET 4 LIF 3 LIF 1 TAP 1 TAP 3 LIF 4 LIF

STDASS: 358 374 395 22 305 374 25 28

4564.9 2741.4 6926.4 2341.0 325.7 3296.5 6976.5 8176.6

4583.7 2745.9 6884.5 2305.0 327.5 3272.7 6960.2 8192.3


Typical sequence of man fit

Typical Sequence of MAN Fit


Cr k b interference removed

Cr K-b interference removed


Trace ni contamination removed natural chromite 0 087 wt ni

Trace Ni “contamination” removed (natural chromite, 0.087 wt. % Ni)


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