Table of Contents

1 Si K edge XAS measurements

1.1 Sample list

formula common name Source in stock? Beamline
Si powder1   Alfa-Aeser Stock #44384 Lot #J06T047 yes X15b
SiO2 silica unknown yes X15b
SiO2 quartz H-122838 yes X15b
SiO silicon monoxide Aldritch 262951-50G Batch #01422EJ yes2 X15b
Si3N2 silicon nitride Alfa-Aeser Stock #14704 Lot #H14T015 yes X15b
FeSi iron silicide Alfa-Aeser Stock #14019 Lot #A15T045 yes X15b
SiC silicon carbide Alfa-Aeser Stock #43332 Lot #D03T026 yes X15b
Mg2SiO4 Forsterite unknown yes X15b
Fe2SiO4 Fayalite Alfa-Aeser stock #44278 yes X15b
MgSiO3 enstatite Alfa-Aeser stock #42638 Lot #E15T035 yes X15b
MgSiO3 enstatite (colorless) H-132059 yes X15b
MgSiO3 enstatite Indarch meteorite3 yes X15b
(Mg,Fe)SiO3 enstatite (black) H-130424 yes X15b
See note 4 montmorillonite H-142599 yes X15b
See note 5 nontronite H-102634 yes X15b
(Mg,Fe)3Si2O5(OH)4 antigorite/serpentine H-126645 yes X15b
Mg3(Si2O5)(OH)4 chrysotile/white asbestos H-98898 yes X15b
(Mg,Fe)2SiO4 forsterite/olivine H-88333B yes X15b
Notes
  1. partially oxidized
  2. See this paper which doubts commercial SiO phase purity, J. Non-Crystalline Solids 204:2, (1996) 202-203
  3. See http://www.mindat.org/loc-20446.html and http://www.meteoritestudies.com/protected_INDARCH.HTM and this Nature article. Googling for indarch returns lots of hits.
  4. Nominal formula for montmorillonite: (Na,Ca)0.33(Al,Mg)2(Si4O10)(OH)2.nH2O
  5. Nominal formula for nontronite: Ca0.5(Si7Al0.8Fe0.2)(Fe3.5Al0.4Mg0.1)O20(OH)4
Other minerals
* Andalusite, kyanite, and sillimanite are naturally occurring aluminosilicate minerals that have the composition Al2SiO5.
  • Garnets are nesosilicates having the general formula X3Y2(SiO4)3. The X site is usually occupied by divalent cations (Ca2+, Mg2+, Fe2+) and the Y site by trivalent cations (Al3+, Fe3+, Cr3+) in an octahedral/tetrahedral framework with [SiO4]4− occupying the tetrahedra.

2 Lab Book Transcription for February 2009 experiment

PASS form
13330
SAF
9554

2.1 19 February 2009

Mount a glass slide to test the beamline configuration

  • testsio2.001 - .002 (get calibration)

Time: 1551

  • glass.001 (test calibration)

Sample holder:

+------------------+
|                  |
|      +--------+  |
|      |        |  |
|      | Nothing|  |
|      |        |  |
|      | Si3N4  |  |   from Alfa-Aeser
|      |        |  |
|      | FeSi   |  |   from Alfa-Aeser
|      |        |  |
|      | SiC    |  |   from Alfa-Aeser
|      |        |  |
|      | C Tape |  |   blank carbon tape to check for Si content
|      |        |  |
|      +--------+  |
|                  |
+------------------+

Time: 1820

  • si3n4.001
  • si3n4.002 aborted
  • si3n4.003 longer postedge

New scan parameters:

energy ranges
1790, 1830, 1850, 1900, 1980
step sizes
0.5, 0.25, 1, 2

After fill move to a new spot on Si3N4.

  • si3n4.004 - .007
  • sife.001 test edge
  • sife.002 +
  • sic,001 edge scan

Time: 2240

  • sic.002 forgot to increase the number of scans! D'oh!

2.2 20 February 2009

Time: 0800

  • sic.003 - .006
  • ctape.001
+--------------------+
|                    |
|      +----------+  |
|      |          |  |
|      | SiO2     |  |
|      |          |  |
|      | FeSi     |  |   from Alfa-Aeser
|      |          |  |
|      | MgSiO3   |  | 
|      |          |  |
|      | Mg2SiO4  |  |
|      |          |  |
|      | Fe2SiO4  |  |   from Alfa-Aeser
|      |          |  |
|      +----------+  |
|                    |
+--------------------+
  • simg2o4.001 - .003
  • simg2o4.004 aborted for Paul to optimize beamline

Paul realigned beamline, increasing flux by at least an order of magnitude.

There is a small energy shift in the data of -0.415 eV, found by comparing simg2o4.003 and .006

alert.png alert.png alert.png All data from simg2o4.006 to the end of the experiment is shifted by -0.415 volts relative to earlier data alert.png alert.png alert.png

Time: 1520

  • simg2o4.006 after realignment
  • simg2o4.007 aborted

Time: 1640

  • sio2.001 - .004 OK
  • sio2.005 - .008 during fill
  • sio2.009 - .010 OK
  • sio2.011 aborted

Time: 2100

  • sife.001 - .005

Time: 2345

  • sife2o4.001 - .010, .017

2.3 21 February, 2009

+--------------------+
|                    |
|      +----------+  |
|      |          |  |
|      | Enstatite|  |   from Alfa-Aeser (sienaa)
|      |          |  |
|      | Enstatite|  |   Fe-free 132059 (sienfef)
|      |          |  |
|      | Enstatite|  |   Chondrite (Indarch meteorite) (sienchon)
|      |          |  |
|      | Enstatite|  |   "Paulite" 130424 (sienplt)
|      |          |  |
|      | Quartz   |  |   Hot Springs AK, Garland 6
|      |          |  |
|      +----------+  |
|                    |
+--------------------+
  • sienaa.001 - 004 (.005 aborted)
  • sienfef.001 - .004 (.005, .006 aborted)
  • sienplt.001 - .005

Time: 1800

  • siquartz.001 - .010 (of these, only .001, .007, .008, .009 are good)

Time: 2200

  • sienchon.001 - .014 (.015 + during morning fill)

2.4 22 February 2009

+--------------------+
|                    |
|      +----------+  |
|      |          |  |
|      | Si       |  |   very fine powder
|      |          |  |
|      | Quartz   |  |   SiO (silicon monoxide)
|      |          |  |
|      +----------+  |
|                    |
+--------------------+

Time: 0925

  • si.001 - .004 (This is somewhat oxidized)

Time 1210

  • sio.001 - .004
+----------------------+
|                      |
|      +------------+  |
|      |            |  |
|      | Montmor.   |  |   Montmorillonite 142599 (simont)
|      |            |  |
|      | Nontron.   |  |   Nontronite 102634 (sinon)
|      |            |  |
|      | Antogorite |  |   126645 (sianti)
|      |            |  |
|      | Crysotile  |  |   98898 (sicrys)
|      |            |  |
|      | Forsterite |  |   olivine from Rice Gila Co. AZ
|      |            |  |
|      | Quartz     |  |   Hot Springs AK, Garland 6 (again, slightly finer powder)
|      |            |  |
|      +------------+  |
|                      |
+----------------------+

Time: 1525

  • simont.001 - .004
  • sinon.001
  • sinon.002 - .005 during fill
  • sinon.006 - .008

Time: 1050

  • sianti.001 - .004

2.5 23 February, 2009

  • sicsys.001 - .004 (note that "sicsys" is the crysotile sample)
  • sifoist.001 - .019 (note that "sifoist" is Forsterite)
  • siq2.001 - .004 (I tried to grind this sample more finely than the first one. I succeeded, but only a bit more so)

Author: Bruce Ravel

Created: 2015-11-06 Fri 09:21

Validate