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EPMA Sample Preparation / Re: EPMA Sample Preparation Discussion Board
« Last post by Probeman on Today at 07:30:33 AM »
You might want to watch these videos of Tim Teague (master technical petrologist) discussing his methods:

https://probesoftware.com/smf/index.php?topic=1163.0

He used Petropoxy for almost everything and could obtain a mirror polish on lead metal!

With respect to your question I think he would heat the sample slightly until the Petropoxy "gelled", and then removed all the tape and only then cured it fully with more heat.

He was able to get very amazing grain mounts of anything using this method:

https://probesoftware.com/smf/index.php?topic=172.msg12595#msg12595

https://probesoftware.com/smf/index.php?topic=172.msg8991#msg8991
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Any thoughts on resin/hardener brands? The current mixture we are using results in epoxy mounts that contain sulphur which is a pain when measuring apatite.

My favorite epoxy is "Petropoxy" which is sold here:

https://www.burnhampetrographics.com/petropoxy/ppp.php

It's stay liquid until heated so give one a long working time which is useful for complicated mounts like this:

https://probesoftware.com/smf/index.php?topic=172.msg12595#msg12595

When using sticky tape or vaseline to mount grains, heating up the petropoxy will get rid of the tape and vaseline. Grains will more or start floating around. Any alternative to this problem?
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Very nice Ben.

Note that one can also quickly obtain both detection limits (in wt%) and analytical sensitivity (in one sigma relative percent units) for quant x-ray maps in CalcImage by just checking the boxes in the Project | Specify Quantitative Parameters menu dialog:

https://probesoftware.com/smf/index.php?topic=393.msg9220#msg9220

https://probesoftware.com/smf/index.php?topic=1452.0
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Hi, in case of interest/use

A long bit of code for R calculating detection limits and errors for a map, it's interesting when you consider situations where the error on peak (number of pixels of peak map averaged) can become smaller than the error on the background (a series of quant points - if a few points are taken)

The code reads
1. background quant points - reading count intensities.
2. background quant points - reading kraw, count times, analytical conditions, std assign
3. map setup file - for map analytical condtions

Code attached
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I actually had bad long-term results with Petropoxy where, after two years, the epoxy had shrunk enough to create gaps between my standard grains and the epoxy. Maybe I did something wrong when curing the Petropoxy but I am a big believer in cold-setting, slow-curing epoxies for epoxy mounts that are supposed to last a long time (like standard mounts).

We use Stuers Epofix.
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Cameca Camebax, purchased by WSU in 1981. I had the "pleasure" of using this puppy early in my graduate career, when it was a little over 20 years old. By that time, it had been upgraded to have motorized stages! You still had to navigate with hand cranks, looking through a binocular scope with an FOV that felt like it was 10 microns, but at least it could do automated analyses through Probe For Windows!

This probe was a real work horse, and served WSU for 27 years under the masterful hand of Scott Cornelius, until it was replaced by our current JEOL 8500F in about 2008.



Back in 1981, this beauty could be yours for under $200,000...$199,999.99 after tax. That's just shy of $700K in today's money.



Anyway, thought some might enjoy a little history snapshot.
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EPMA Standard Materials / Re: Geophysical Lab Probe Standards
« Last post by Probeman on July 18, 2024, 07:32:35 AM »
Several people responded but Andrew gave a very informative reply:

Hello,
The attached paper of MacGregor (1974) mentions EnAl-5, EnAl-10, and EnAl-15 in his Table 1, and mentions them again as glasses in the Starting Material section of his Appendix. The Acknowledgments mention a fellowship ath the Geophysical Lab and also thank Dr. F.R. Boyd.

Marinenko (1982) in Table 3 of NBS Special Publication 260-74 describes “ENAL 10 – from Geophysical Laboratories)”, “a synthetic glass”, with the same composition, but presented as elements rather than oxides.

P-140 is apparently olivine from the Balsalm Gap dunite in North Carolina.

A typewritten letter, headed Finland, April 20, 1971 from H.B. Wiik (Hugo Birger Wiik of Finland) to F.R. Boyd gives the composition of the olivine (which includes 0.13 Al2O3).  In my photocopy, this letter is annotated with a handwritten note: “Zies give 7.28 Fe as FeO”.   The exact same analysis of Wiik is reproduced in Table J on page 17 of the PhD thesis P.J. Lawless (Cape Town, 1978).

My researches on P-140 in 2016 yielded:

The material may have been collected by Hess, and a hand-specimen is described in detail in the appendix of:

Davis, G.L. and Hess, H.H., 1949. Radium content of ultramafic igneous rocks; II, Geological and chemical implications. American Journal of Science, 247(12), pp.856-882.

The wet-chemical analysis was performed by E.G. Zies of the Geophysical Laboratory, according to a footnote to Table 2 of:
Boone, G.M. and Fernandez, L.A., 1971. Phenocrystic olivines from the eastern Azores. Mineralogical Magazine, 38, pp.165-78.

This olivine analysis was apparently reported by F.R. Boyd of the Geophysical Laboratory, according to the supplementary Table A1 in the appendix (p. 13) of:
Hofmeister, A.M., Xu, J., Mao, H.K., Bell, P.M. and Hoering, T.C., 1989. Thermodynamics of Fe-Mg olivines at mantle pressures: Mid-and far-infrared spectroscopy at high pressure. American Mineralogist, 74, pp. 281-306.

http://www.minsocam.org/msa/ammin/Supplemental_Data/Vol%2074%20p0281%20AM-89-400.pdf

Finally, a partial analysis of this same olivine is found in Table 2 of:
Jarosewich, E., Parkes, A.S. and Wiggins, L.B., 1979. Microprobe analyses of four natural glasses and one mineral: an interlaboratory study of precision and accuracy. Smithsonian contributions to the earth sciences, 22, pp.53-67.

Based on the literature references that I have found, it appears that the P-140 Balsam Gap olivine (forsterite) was used as an electron microprobe standard at the following, in addition to the Geophysical Laboratory:

-              Chicago (Mason et al., 1982);
-              MIT (Jarosewich et al., 1979);
-              Yale (Boone and Fernandez, 1971).

In addition to the notes about sample P-140 in Davis and Hess (1949), I did note that in the Carnegie Institution of Washington Year Book No. 46 (published 1947) it was reported (p. 38) that about 1000 pounds of the Balsam Gap dunite were collected.

I corresponded with Shaun Hardy at Carnegie, who inspected Dr. Zies’ notebooks and research files, and Dr. Boyd’s correspondence and research files, but no luck with regard to Balsam Gap olivine.  Shaun put me in touch with the Smithsonian (Leslie Hale), but no documentation was available.

Finally, my own analyses of the P-140 olivine in the University of Alberta lab do not show the same high Al contents. I suspect that the analysis of Wiik was by wet chemistry, and perhaps contaminated with some amount of clinochlore or some such.

I hope that this information proves useful to you.

Best regards,
Andrew

Andrew Locock, PhD
EPMA Lab Manager

Dept. of Earth and Atmospheric Sciences
Room 1-26 Earth Sciences Building
11223 Saskatchewan Drive NW
University of Alberta
Edmonton, Alberta, Canada T6G 2E3

Tel: 780-492-3191
Fax: 780-492-2030
www.eas.ualberta.ca/eml/
www.microprobe.ca
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EPMA Standard Materials / Geophysical Lab Probe Standards
« Last post by Probeman on July 18, 2024, 07:30:30 AM »
John Fournelle and Anette asked the following on the Cameca listserver:

Quote
This is a history-of-microbeam-standards quiz question for the _really_ old timers out there (you know who you are). Anette found these both in the Smithsonian’s back room files as well as at the University of Minnesota.

The Carnegie Probe Lab (at the Carnegie Geophysical Lab in DC) provided series of EPMA starndards to several labs, probably in the 1970s and on a bit. We are looking for someone to provide some more details. Who developed and send out these materials? Was it Joe Boyd? They include both natural and synthetic (including WEF14, DJ35, ENAL series, doped Diopside glasses). This is a poorly recorded/reported part of our history.

John and Anette






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Discussion of General EPMA Issues / Re: Using fityk to determine flank positions
« Last post by Probeman on July 17, 2024, 07:07:13 AM »
For others interested in the Flank method, please search for "flank" in this user forum to see more on this method. For example:

https://probesoftware.com/smf/index.php?topic=1605.msg12395#msg12395
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EPMA Sample Preparation / Re: EPMA Sample Preparation Discussion Board
« Last post by Probeman on July 17, 2024, 06:57:12 AM »
Any thoughts on resin/hardener brands? The current mixture we are using results in epoxy mounts that contain sulphur which is a pain when measuring apatite.

My favorite epoxy is "Petropoxy" which is sold here:

https://www.burnhampetrographics.com/petropoxy/ppp.php

It's stay liquid until heated so give one a long working time which is useful for complicated mounts like this:

https://probesoftware.com/smf/index.php?topic=172.msg12595#msg12595
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