Hg Cap for Natural Gas, 10ID August 2011
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Notes
When grinding samples 34363-87A and 34363-87B for Cu ex situ EXAFS on tape, there was an occasional white pill (unsulfided) that was ground and mixed in with the sulfided pills.
Cu References
# |
filename |
description |
Temp |
Gas |
EXAFS/XANES |
Done |
PIC |
Cu Foil, |
Foil from box |
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step 1 |
11Aug_Cu1.001-2 |
As Received at RT in Air |
RT |
Air |
2 EXAFS |
done |
|
34185-38, CuS alfa aesar Lot K04U021 |
2 layers on tape |
||||||
step 1 |
11Aug_Cu2.001-2 |
As Received at RT in Air |
RT |
Air |
2 EXAFS |
done |
|
34363-76C, Cu2S Ref |
4 layers on tape |
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step 1 |
11Aug_Cu3.003-4 |
As Received at RT in Air |
RT |
Air |
2 EXAFS |
done |
|
34363-76D, Cu2S Ref |
4 layers on tape |
||||||
step 1 |
11Aug_Cu4.003-4 |
As Received at RT in Air |
RT |
Air |
2 EXAFS |
done |
|
Hg References
# |
filename |
description |
Temp |
Gas |
EXAFS/XANES |
Done |
PIC |
Hg Foil, meta Cinnabar HgS Standard |
Foil from box |
||||||
step 1 |
11Aug_Hg1.002-3 |
As Received at RT in Air |
RT |
Air |
2 EXAFS |
done |
|
Cu Ex Situ
# |
filename |
description |
Temp |
Gas |
EXAFS/XANES |
Done |
PIC |
34363-83A1, Spent Hg guard with ~1-2 wt% Hg produced from sulfidation of Old bridge malachite |
12 layers on tape |
||||||
step 1 |
11Aug_Cu5.003-6 |
As Received at RT in Air |
RT |
Air |
4 EXAFS |
done |
|
34363-83B1, Spent Hg guard with ~1 wt% Hg produced from sulfidation of Old Bridge CuO |
16 layers on tape |
||||||
step 1 |
11Aug_Cu6.001-4 |
As Received at RT in Air |
RT |
Air |
4 EXAFS |
done |
|
34363-87A, Sulfided copper carbonate adsorbent ~20 wt%S, CuS by XRD |
8 layers on tape |
||||||
step 1 |
11Aug_Cu9.001-004 |
As Received at RT in Air |
RT |
Air |
4 EXAFS |
done |
|
34363-87B, Sulfided copper oxide adsorbent ~12 wt%S |
8 layers on tape |
||||||
step 1 |
11Aug_Cu10.002-5 |
As Received at RT in Air |
RT |
Air |
4 EXAFS |
done |
|
Hg Ex Situ
# |
filename |
description |
Temp |
Gas |
EXAFS/XANES |
Done |
PIC |
34363-83A1, Spent Hg guard with ~1-2 wt% Hg produced from sulfidation of Old bridge malachite |
149.8mg in 12.5mm Quartz holder |
||||||
step 1 |
11Aug_Hg2.001-4 |
As Received |
RT |
Air |
2 EXAFS data quality poor maybe fluor mode would work? |
-- |
|
34363-83B1, Spent Hg guard with ~1 wt% Hg produced from sulfidation of Old Bridge CuO |
150.9mg in 12.5mm Quartz holder |
||||||
step 1 |
11Aug_Hg3.001 |
As Received |
RT |
Air |
2 EXAFS data quality poor maybe fluor mode would work? |
-- |
|
Cu/Hg in situ Sulfiding
# |
filename |
description |
Temp |
Gas |
EXAFS/XANES |
Done |
PIC |
34363-69E, Old Bridge, spot 1 |
13mg Sample/12mg BN, 1:1 BN, 10.5mg packed |
use 4 barrel |
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34363-69D, Philotech, spot 2 |
13 mg Sample/12 mg BN, 1:1 BN 10mg packed |
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step 1 |
run @Cuedge.mx change reference foil to Cu |
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step 1 |
11Aug_Cu7.001 |
As Received at RT in He, spot 1 |
RT |
100% He |
1 XANES |
done |
|
step 1 |
11Aug_Cu8.001 |
As Received at RT in He, spot 2 |
RT |
100% He |
1 XANES |
done |
|
step 2 |
ramp to 150C at 3deg/min and dwell 145 min in 1000 ppm H2S/He (dwell ended no further changes in data) |
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step 2 |
purge with 1000ppm H2S/He at 100cc/min wait 5 min then start data collection and ramp |
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step 2 |
11Aug_Cu7.002-016 |
Sulfidation, spot1 |
RT to 150C |
1000ppm H2S/He |
xanes |
done |
|
step 2 |
11Aug_Cu8.002-016 |
Sulfidation, spot2 |
RT to 150C |
1000ppm H2S/He |
xanes |
done |
|
step 3 |
Cool to RT in 1000 ppm H2S/He |
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step 3 |
11Aug_Cu7.018-019 |
after sulfidation at RT in H2S/He, spot1 |
RT |
1000ppm H2S/He |
2 exafs |
done |
|
step 3 |
11Aug_Cu8.017-018 |
after sulfidation at RT in H2S/He, spot2 |
RT |
1000ppm H2S/He |
2 exafs |
done |
|