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There didn't appear to be boron in the light element scans. As for
Li, I've been assured it is unlikely because there isn't a probable
source in their experiments. Also, because Li is so light, the
analyses for oxygen would've picked up half of the mass for Li2O -- I
don't that he's seeing that when he analyzing for oxygen. The same
for boron... But I'll suggest that he double-checks this.
I think he's also considered trivalent iron, but I'll suggest that he
double-checks this possibility too.
On Jun 11, 2008, at 10:14 AM, Andersen, Jens wrote:
> Have you tested for the valency of Iron? Trivalent Fe would give low
> totals, right? Any boron, lithium???
> Jens C. Andersen
> Senior lecturer
> Camborne School of Mines
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> -----Original Message-----
> From: JEOL-Focused Probe Users List
> [mailto:[log in to unmask]] On
> Behalf Of Ellery Frahm
> Sent: 11 June 2008 16:02
> To: [log in to unmask]
> Subject: [PROBE-USERS] Hydrous melt analysis boggle
> JEOL Probe Users Listserver
> Moderator: Ellery Frahm, [log in to unmask], Electron Microprobe Lab,
> University of Minnesota
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> Probe folks,
> A researcher in our lab (an experimental petrologist) is trying to
> analyze a few of his samples (experimental andesitic melts/glasses
> containing between 3% and 6% water), and he is trying to (1) get good
> totals and (2) correlate measurements of the water content using FTIR
> and oxygen analysis in the microprobe. He is getting a linear fit
> between water contents from the FTIR and microprobe, but his totals
> low on the probe when we analyzes his samples as both oxides and
> He is an experienced user, and we've gone through all of the usual
> procedures for testing the causes of low totals -- nothing.
> The FTIR measured total water contents ranging of 3.37, 4.12, 4.54,
> 5.25, 5.45, and 5.88 to 5.9 wt%. When we analyze the glasses with the
> electron microprobe, assuming a deficit from a 100% total is
> to H2O, the calculated water contents are 5.29, 6.45, 7.12, 7.75,
> and 9.21 wt. %, respectively. So his totals are about 5% low,
> occasionally more, causing overestimation of water.
> Here is what he has tried (based on the notes he's given me):
> 1) Periodically aligned beam and checked for astigmatism on
> 2) Beam conditions: 10 nA current, 30 micron spot size.
> 3) Always analyzed Na first (monitored counts rates, found Na counts
> did not drop for at least 30 seconds).
> 4) Analyzed for oxygen using three different standards: enstatite,
> pyrope, and almandine -- all yielded similar results.
> 5) Counted the area under the peak for oxygen.
> 6) Adjusted the detector settings for oxygen: PHA Gain: 32, High V:
> 1708, Base L. (V) 0.70, Window: 2.5, Mode: Diff. Set up this way to
> filter out high-order Al and Na peaks. WDS scans indicated these
> were eliminated by this filtering method but had little effect on
> improving the water contents of the glasses when compared to an
> "unfiltered" method.
> 7) Set oxygen backgrounds based on WDS scans and software overlap
> database: Back +: 12.000 mm, Back -: 6.500 mm.
> 8) Total counting time on oxygen: ~44 seconds. Other elements: 10
> seconds for peak, 5 seconds for background.
> 9) Elements present in samples (and analyzed for): Si, Ti, Al, Cr,
> Mn, Mg, Ca, Na, K, O, H (known from FTIR)
> 10) Full WDS scans (including light elements) revealed no missed
> elements that could have led to low totals.
> 11) Used basaltic glass to standardize MgO, CaO, FeO. Rhyolitic
> (basaltic glass) for Al2O3. SiO2 Glass (Quartz, basaltic glass,
> rhyolitic glass) for SiO2. Benitoite for TiO2. Chromite for Cr2O3.
> Mn-Hortonolite for MnO. Omphacite (albite) for Na2O. K-Spar for K2O.
> Standards in brackets were also tries, and produced worse results.
> Standardized as oxides, and then measured the unknowns as a metal.
> Oxygen was standardized as a metal on the enstatite standard, and
> analyzed as a metal on the unknowns.
> 12) Sample thicknesses were 100 microns or greater.
> 13) Two carbon coat thicknesses tried: about 50 and 200 angstroms --
> produced similar results, so charging isn't a problem.
> 14) Glasses were free of quench crystals, so the interaction volume
> should be homogeneous.
> 15) Moving elements to different spectrometers had no effect on
> improving the results.
> 16) Using these conditions, analyses on two different basaltic glass
> standards yielded matching elemental concentrations. These glasses
> relatively dry (a few tenths of a wt.% H2O) compared to the
> specimens in
> 17) This technique was also performed on hydrous rhyolitic glasses
> 1.3, 3.3, 4, 5, and 6 wt. % H2O (determined by FTIR) and produced the
> similar water contents (1.06, 3.11, 4.74, 5.65, and 7.24,
> respectively) and overall chemistry.
> The only real issue I see above is the benitoite as a Ti standard
> because it has CL, but the TiO2 content of these glass samples isn't
> high enough to account for the difference. Because these glasses are
> amorphous (presumably), even most of my usual "exotic" explanations
> low totals are ruled out, like X-ray polarization between the crystals
> in the sample and the dispersing crystal. I'd like to have a better
> explanation for these low totals other than "well, something is
> the electrons and/or X-rays to be more strongly absorbed or behave
> in an
> unexpected way" -- that's not very satisfying.
> So I need to get some fresh ideas or find out if others have had
> problems with hydrous andesitic melts. Anyone have an ideas about
> to try next or what the problem might be (even if we can't fix it)?
> Ellery E. Frahm
> Research Fellow & Manager
> Electron Microprobe Laboratory
> University of Minnesota - Twin Cities
> Department of Geology & Geophysics
> Lab Website: http://probelab.geo.umn.edu Personal Website: