The dehydration process in the zeolite laumontite: a real-time synchrotron X-ray powder diffraction study
Abstract The dehydration process of the natural zeolite laumontite $ Ca_{4} $$ Si_{16} $$ Al_{8} $$ O_{48} $ · 18 $ H_{2} $O has been studied in situ by means of powder diffraction and X-ray synchrotron radiation. Powder diffraction profiles suitable for Rietveld refinements were accumulated in time...
Ausführliche Beschreibung
Gespeichert in:
| Autor*in: |
Ståhl, K. [verfasserIn] |
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| Format: |
Artikel |
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| Sprache: |
Englisch |
| Erschienen: |
1996 |
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| Schlagwörter: |
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| Anmerkung: |
© Springer-Verlag 1996 |
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| Übergeordnetes Werk: |
Enthalten in: Physics and chemistry of minerals - Springer-Verlag, 1977, 23(1996), 6 vom: Aug., Seite 328-336 |
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| Übergeordnetes Werk: |
volume:23 ; year:1996 ; number:6 ; month:08 ; pages:328-336 |
| Links: |
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| DOI / URN: |
10.1007/BF00199498 |
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| Katalog-ID: |
OLC2072359392 |
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|---|---|---|---|
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| 245 | 1 | 0 | |a The dehydration process in the zeolite laumontite: a real-time synchrotron X-ray powder diffraction study |
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| 520 | |a Abstract The dehydration process of the natural zeolite laumontite $ Ca_{4} $$ Si_{16} $$ Al_{8} $$ O_{48} $ · 18 $ H_{2} $O has been studied in situ by means of powder diffraction and X-ray synchrotron radiation. Powder diffraction profiles suitable for Rietveld refinements were accumulated in time intervals of 5 minutes using a position sensitive detector (CPS-120 by INEL), while the temperature increased in steps of about 5 K. The synchronization of accumulation time and temperature plateau allowed collection of 62 temperature-resolved powder patterns in the range 310–584 K, whose analysis produced a dynamic picture of the laumontite structure response to dehydration. The first zeolitic water molecules diffusing out of the channels are those not bonded to the Ca cations and located in the W(1) site, whose occupancy drops smoothly to 10% during heating to 349 K, while the sample in the capillary is still submerged in water. The remaining W(1) and 60% of W(5) water molecules are expelled rather sharply at about 370 K. At this temperature all remaining water submerging the powder crystallites is lost, the structure contains about 13 water molecules/cell, and the crystal structure is that of leonhardite. On continued heating 80% of the water molecules from the W(2) site are lost between 420 and 480 K, while a small amount of the diffusing water is reinserted in the W(5) site. The occupancy factor of the W(8) site decreases starting at 480 K, and reaches a maximum loss of 20% at 584 K. The combined occupancy of the Ca-coordinated W (2) and W (8) water sites never falls much below two, so that the Ca cations in the channels, which are bonded to four framework oxygen atoms, are nearly six-coordinated in the explored temperature range. The water loss is accompanied by large changes in the unit cell dimensions. Except at 367 K, where the excess surrounding water is leaving, all changes in cell dimensions are gradual. The loss of the hydrogen bonded W(1) and W(5) water molecules is related to most of the unit cell volume reduction below 370 K, as shown by the contraction of the a-, b- and c-axes and the increase in the monoclinic angle. Loss of the Ca-coordinated W(2) and W(8) water molecules has a small effect on the unit cell volume as the continued contraction of the a- and c-axes is counter-balanced by a large expansion in the b-axis and a decrease in the monoclinic β angle. | ||
| 650 | 4 | |a Unit Cell Volume | |
| 650 | 4 | |a Rietveld Refinement | |
| 650 | 4 | |a Dehydration Process | |
| 650 | 4 | |a Natural Zeolite | |
| 650 | 4 | |a Position Sensitive Detector | |
| 700 | 1 | |a Artioli, G. |4 aut | |
| 700 | 1 | |a Hanson, J. C. |4 aut | |
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10.1007/BF00199498 doi (DE-627)OLC2072359392 (DE-He213)BF00199498-p DE-627 ger DE-627 rakwb eng 550 540 530 VZ BIODIV DE-30 fid Ståhl, K. verfasserin aut The dehydration process in the zeolite laumontite: a real-time synchrotron X-ray powder diffraction study 1996 Text txt rdacontent ohne Hilfsmittel zu benutzen n rdamedia Band nc rdacarrier © Springer-Verlag 1996 Abstract The dehydration process of the natural zeolite laumontite $ Ca_{4} $$ Si_{16} $$ Al_{8} $$ O_{48} $ · 18 $ H_{2} $O has been studied in situ by means of powder diffraction and X-ray synchrotron radiation. Powder diffraction profiles suitable for Rietveld refinements were accumulated in time intervals of 5 minutes using a position sensitive detector (CPS-120 by INEL), while the temperature increased in steps of about 5 K. The synchronization of accumulation time and temperature plateau allowed collection of 62 temperature-resolved powder patterns in the range 310–584 K, whose analysis produced a dynamic picture of the laumontite structure response to dehydration. The first zeolitic water molecules diffusing out of the channels are those not bonded to the Ca cations and located in the W(1) site, whose occupancy drops smoothly to 10% during heating to 349 K, while the sample in the capillary is still submerged in water. The remaining W(1) and 60% of W(5) water molecules are expelled rather sharply at about 370 K. At this temperature all remaining water submerging the powder crystallites is lost, the structure contains about 13 water molecules/cell, and the crystal structure is that of leonhardite. On continued heating 80% of the water molecules from the W(2) site are lost between 420 and 480 K, while a small amount of the diffusing water is reinserted in the W(5) site. The occupancy factor of the W(8) site decreases starting at 480 K, and reaches a maximum loss of 20% at 584 K. The combined occupancy of the Ca-coordinated W (2) and W (8) water sites never falls much below two, so that the Ca cations in the channels, which are bonded to four framework oxygen atoms, are nearly six-coordinated in the explored temperature range. The water loss is accompanied by large changes in the unit cell dimensions. Except at 367 K, where the excess surrounding water is leaving, all changes in cell dimensions are gradual. The loss of the hydrogen bonded W(1) and W(5) water molecules is related to most of the unit cell volume reduction below 370 K, as shown by the contraction of the a-, b- and c-axes and the increase in the monoclinic angle. Loss of the Ca-coordinated W(2) and W(8) water molecules has a small effect on the unit cell volume as the continued contraction of the a- and c-axes is counter-balanced by a large expansion in the b-axis and a decrease in the monoclinic β angle. Unit Cell Volume Rietveld Refinement Dehydration Process Natural Zeolite Position Sensitive Detector Artioli, G. aut Hanson, J. C. aut Enthalten in Physics and chemistry of minerals Springer-Verlag, 1977 23(1996), 6 vom: Aug., Seite 328-336 (DE-627)129323039 (DE-600)131393-9 (DE-576)014557398 0342-1791 nnns volume:23 year:1996 number:6 month:08 pages:328-336 https://doi.org/10.1007/BF00199498 lizenzpflichtig Volltext GBV_USEFLAG_A SYSFLAG_A GBV_OLC FID-BIODIV SSG-OLC-PHY SSG-OLC-CHE SSG-OLC-GEO SSG-OLC-PHA SSG-OLC-DE-84 SSG-OPC-GGO GBV_ILN_11 GBV_ILN_32 GBV_ILN_40 GBV_ILN_70 GBV_ILN_130 GBV_ILN_2010 GBV_ILN_2018 GBV_ILN_2027 GBV_ILN_2279 GBV_ILN_4012 GBV_ILN_4046 GBV_ILN_4103 GBV_ILN_4112 GBV_ILN_4277 GBV_ILN_4306 GBV_ILN_4313 GBV_ILN_4319 GBV_ILN_4323 AR 23 1996 6 08 328-336 |
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10.1007/BF00199498 doi (DE-627)OLC2072359392 (DE-He213)BF00199498-p DE-627 ger DE-627 rakwb eng 550 540 530 VZ BIODIV DE-30 fid Ståhl, K. verfasserin aut The dehydration process in the zeolite laumontite: a real-time synchrotron X-ray powder diffraction study 1996 Text txt rdacontent ohne Hilfsmittel zu benutzen n rdamedia Band nc rdacarrier © Springer-Verlag 1996 Abstract The dehydration process of the natural zeolite laumontite $ Ca_{4} $$ Si_{16} $$ Al_{8} $$ O_{48} $ · 18 $ H_{2} $O has been studied in situ by means of powder diffraction and X-ray synchrotron radiation. Powder diffraction profiles suitable for Rietveld refinements were accumulated in time intervals of 5 minutes using a position sensitive detector (CPS-120 by INEL), while the temperature increased in steps of about 5 K. The synchronization of accumulation time and temperature plateau allowed collection of 62 temperature-resolved powder patterns in the range 310–584 K, whose analysis produced a dynamic picture of the laumontite structure response to dehydration. The first zeolitic water molecules diffusing out of the channels are those not bonded to the Ca cations and located in the W(1) site, whose occupancy drops smoothly to 10% during heating to 349 K, while the sample in the capillary is still submerged in water. The remaining W(1) and 60% of W(5) water molecules are expelled rather sharply at about 370 K. At this temperature all remaining water submerging the powder crystallites is lost, the structure contains about 13 water molecules/cell, and the crystal structure is that of leonhardite. On continued heating 80% of the water molecules from the W(2) site are lost between 420 and 480 K, while a small amount of the diffusing water is reinserted in the W(5) site. The occupancy factor of the W(8) site decreases starting at 480 K, and reaches a maximum loss of 20% at 584 K. The combined occupancy of the Ca-coordinated W (2) and W (8) water sites never falls much below two, so that the Ca cations in the channels, which are bonded to four framework oxygen atoms, are nearly six-coordinated in the explored temperature range. The water loss is accompanied by large changes in the unit cell dimensions. Except at 367 K, where the excess surrounding water is leaving, all changes in cell dimensions are gradual. The loss of the hydrogen bonded W(1) and W(5) water molecules is related to most of the unit cell volume reduction below 370 K, as shown by the contraction of the a-, b- and c-axes and the increase in the monoclinic angle. Loss of the Ca-coordinated W(2) and W(8) water molecules has a small effect on the unit cell volume as the continued contraction of the a- and c-axes is counter-balanced by a large expansion in the b-axis and a decrease in the monoclinic β angle. Unit Cell Volume Rietveld Refinement Dehydration Process Natural Zeolite Position Sensitive Detector Artioli, G. aut Hanson, J. C. aut Enthalten in Physics and chemistry of minerals Springer-Verlag, 1977 23(1996), 6 vom: Aug., Seite 328-336 (DE-627)129323039 (DE-600)131393-9 (DE-576)014557398 0342-1791 nnns volume:23 year:1996 number:6 month:08 pages:328-336 https://doi.org/10.1007/BF00199498 lizenzpflichtig Volltext GBV_USEFLAG_A SYSFLAG_A GBV_OLC FID-BIODIV SSG-OLC-PHY SSG-OLC-CHE SSG-OLC-GEO SSG-OLC-PHA SSG-OLC-DE-84 SSG-OPC-GGO GBV_ILN_11 GBV_ILN_32 GBV_ILN_40 GBV_ILN_70 GBV_ILN_130 GBV_ILN_2010 GBV_ILN_2018 GBV_ILN_2027 GBV_ILN_2279 GBV_ILN_4012 GBV_ILN_4046 GBV_ILN_4103 GBV_ILN_4112 GBV_ILN_4277 GBV_ILN_4306 GBV_ILN_4313 GBV_ILN_4319 GBV_ILN_4323 AR 23 1996 6 08 328-336 |
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10.1007/BF00199498 doi (DE-627)OLC2072359392 (DE-He213)BF00199498-p DE-627 ger DE-627 rakwb eng 550 540 530 VZ BIODIV DE-30 fid Ståhl, K. verfasserin aut The dehydration process in the zeolite laumontite: a real-time synchrotron X-ray powder diffraction study 1996 Text txt rdacontent ohne Hilfsmittel zu benutzen n rdamedia Band nc rdacarrier © Springer-Verlag 1996 Abstract The dehydration process of the natural zeolite laumontite $ Ca_{4} $$ Si_{16} $$ Al_{8} $$ O_{48} $ · 18 $ H_{2} $O has been studied in situ by means of powder diffraction and X-ray synchrotron radiation. Powder diffraction profiles suitable for Rietveld refinements were accumulated in time intervals of 5 minutes using a position sensitive detector (CPS-120 by INEL), while the temperature increased in steps of about 5 K. The synchronization of accumulation time and temperature plateau allowed collection of 62 temperature-resolved powder patterns in the range 310–584 K, whose analysis produced a dynamic picture of the laumontite structure response to dehydration. The first zeolitic water molecules diffusing out of the channels are those not bonded to the Ca cations and located in the W(1) site, whose occupancy drops smoothly to 10% during heating to 349 K, while the sample in the capillary is still submerged in water. The remaining W(1) and 60% of W(5) water molecules are expelled rather sharply at about 370 K. At this temperature all remaining water submerging the powder crystallites is lost, the structure contains about 13 water molecules/cell, and the crystal structure is that of leonhardite. On continued heating 80% of the water molecules from the W(2) site are lost between 420 and 480 K, while a small amount of the diffusing water is reinserted in the W(5) site. The occupancy factor of the W(8) site decreases starting at 480 K, and reaches a maximum loss of 20% at 584 K. The combined occupancy of the Ca-coordinated W (2) and W (8) water sites never falls much below two, so that the Ca cations in the channels, which are bonded to four framework oxygen atoms, are nearly six-coordinated in the explored temperature range. The water loss is accompanied by large changes in the unit cell dimensions. Except at 367 K, where the excess surrounding water is leaving, all changes in cell dimensions are gradual. The loss of the hydrogen bonded W(1) and W(5) water molecules is related to most of the unit cell volume reduction below 370 K, as shown by the contraction of the a-, b- and c-axes and the increase in the monoclinic angle. Loss of the Ca-coordinated W(2) and W(8) water molecules has a small effect on the unit cell volume as the continued contraction of the a- and c-axes is counter-balanced by a large expansion in the b-axis and a decrease in the monoclinic β angle. Unit Cell Volume Rietveld Refinement Dehydration Process Natural Zeolite Position Sensitive Detector Artioli, G. aut Hanson, J. C. aut Enthalten in Physics and chemistry of minerals Springer-Verlag, 1977 23(1996), 6 vom: Aug., Seite 328-336 (DE-627)129323039 (DE-600)131393-9 (DE-576)014557398 0342-1791 nnns volume:23 year:1996 number:6 month:08 pages:328-336 https://doi.org/10.1007/BF00199498 lizenzpflichtig Volltext GBV_USEFLAG_A SYSFLAG_A GBV_OLC FID-BIODIV SSG-OLC-PHY SSG-OLC-CHE SSG-OLC-GEO SSG-OLC-PHA SSG-OLC-DE-84 SSG-OPC-GGO GBV_ILN_11 GBV_ILN_32 GBV_ILN_40 GBV_ILN_70 GBV_ILN_130 GBV_ILN_2010 GBV_ILN_2018 GBV_ILN_2027 GBV_ILN_2279 GBV_ILN_4012 GBV_ILN_4046 GBV_ILN_4103 GBV_ILN_4112 GBV_ILN_4277 GBV_ILN_4306 GBV_ILN_4313 GBV_ILN_4319 GBV_ILN_4323 AR 23 1996 6 08 328-336 |
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10.1007/BF00199498 doi (DE-627)OLC2072359392 (DE-He213)BF00199498-p DE-627 ger DE-627 rakwb eng 550 540 530 VZ BIODIV DE-30 fid Ståhl, K. verfasserin aut The dehydration process in the zeolite laumontite: a real-time synchrotron X-ray powder diffraction study 1996 Text txt rdacontent ohne Hilfsmittel zu benutzen n rdamedia Band nc rdacarrier © Springer-Verlag 1996 Abstract The dehydration process of the natural zeolite laumontite $ Ca_{4} $$ Si_{16} $$ Al_{8} $$ O_{48} $ · 18 $ H_{2} $O has been studied in situ by means of powder diffraction and X-ray synchrotron radiation. Powder diffraction profiles suitable for Rietveld refinements were accumulated in time intervals of 5 minutes using a position sensitive detector (CPS-120 by INEL), while the temperature increased in steps of about 5 K. The synchronization of accumulation time and temperature plateau allowed collection of 62 temperature-resolved powder patterns in the range 310–584 K, whose analysis produced a dynamic picture of the laumontite structure response to dehydration. The first zeolitic water molecules diffusing out of the channels are those not bonded to the Ca cations and located in the W(1) site, whose occupancy drops smoothly to 10% during heating to 349 K, while the sample in the capillary is still submerged in water. The remaining W(1) and 60% of W(5) water molecules are expelled rather sharply at about 370 K. At this temperature all remaining water submerging the powder crystallites is lost, the structure contains about 13 water molecules/cell, and the crystal structure is that of leonhardite. On continued heating 80% of the water molecules from the W(2) site are lost between 420 and 480 K, while a small amount of the diffusing water is reinserted in the W(5) site. The occupancy factor of the W(8) site decreases starting at 480 K, and reaches a maximum loss of 20% at 584 K. The combined occupancy of the Ca-coordinated W (2) and W (8) water sites never falls much below two, so that the Ca cations in the channels, which are bonded to four framework oxygen atoms, are nearly six-coordinated in the explored temperature range. The water loss is accompanied by large changes in the unit cell dimensions. Except at 367 K, where the excess surrounding water is leaving, all changes in cell dimensions are gradual. The loss of the hydrogen bonded W(1) and W(5) water molecules is related to most of the unit cell volume reduction below 370 K, as shown by the contraction of the a-, b- and c-axes and the increase in the monoclinic angle. Loss of the Ca-coordinated W(2) and W(8) water molecules has a small effect on the unit cell volume as the continued contraction of the a- and c-axes is counter-balanced by a large expansion in the b-axis and a decrease in the monoclinic β angle. Unit Cell Volume Rietveld Refinement Dehydration Process Natural Zeolite Position Sensitive Detector Artioli, G. aut Hanson, J. C. aut Enthalten in Physics and chemistry of minerals Springer-Verlag, 1977 23(1996), 6 vom: Aug., Seite 328-336 (DE-627)129323039 (DE-600)131393-9 (DE-576)014557398 0342-1791 nnns volume:23 year:1996 number:6 month:08 pages:328-336 https://doi.org/10.1007/BF00199498 lizenzpflichtig Volltext GBV_USEFLAG_A SYSFLAG_A GBV_OLC FID-BIODIV SSG-OLC-PHY SSG-OLC-CHE SSG-OLC-GEO SSG-OLC-PHA SSG-OLC-DE-84 SSG-OPC-GGO GBV_ILN_11 GBV_ILN_32 GBV_ILN_40 GBV_ILN_70 GBV_ILN_130 GBV_ILN_2010 GBV_ILN_2018 GBV_ILN_2027 GBV_ILN_2279 GBV_ILN_4012 GBV_ILN_4046 GBV_ILN_4103 GBV_ILN_4112 GBV_ILN_4277 GBV_ILN_4306 GBV_ILN_4313 GBV_ILN_4319 GBV_ILN_4323 AR 23 1996 6 08 328-336 |
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10.1007/BF00199498 doi (DE-627)OLC2072359392 (DE-He213)BF00199498-p DE-627 ger DE-627 rakwb eng 550 540 530 VZ BIODIV DE-30 fid Ståhl, K. verfasserin aut The dehydration process in the zeolite laumontite: a real-time synchrotron X-ray powder diffraction study 1996 Text txt rdacontent ohne Hilfsmittel zu benutzen n rdamedia Band nc rdacarrier © Springer-Verlag 1996 Abstract The dehydration process of the natural zeolite laumontite $ Ca_{4} $$ Si_{16} $$ Al_{8} $$ O_{48} $ · 18 $ H_{2} $O has been studied in situ by means of powder diffraction and X-ray synchrotron radiation. Powder diffraction profiles suitable for Rietveld refinements were accumulated in time intervals of 5 minutes using a position sensitive detector (CPS-120 by INEL), while the temperature increased in steps of about 5 K. The synchronization of accumulation time and temperature plateau allowed collection of 62 temperature-resolved powder patterns in the range 310–584 K, whose analysis produced a dynamic picture of the laumontite structure response to dehydration. The first zeolitic water molecules diffusing out of the channels are those not bonded to the Ca cations and located in the W(1) site, whose occupancy drops smoothly to 10% during heating to 349 K, while the sample in the capillary is still submerged in water. The remaining W(1) and 60% of W(5) water molecules are expelled rather sharply at about 370 K. At this temperature all remaining water submerging the powder crystallites is lost, the structure contains about 13 water molecules/cell, and the crystal structure is that of leonhardite. On continued heating 80% of the water molecules from the W(2) site are lost between 420 and 480 K, while a small amount of the diffusing water is reinserted in the W(5) site. The occupancy factor of the W(8) site decreases starting at 480 K, and reaches a maximum loss of 20% at 584 K. The combined occupancy of the Ca-coordinated W (2) and W (8) water sites never falls much below two, so that the Ca cations in the channels, which are bonded to four framework oxygen atoms, are nearly six-coordinated in the explored temperature range. The water loss is accompanied by large changes in the unit cell dimensions. Except at 367 K, where the excess surrounding water is leaving, all changes in cell dimensions are gradual. The loss of the hydrogen bonded W(1) and W(5) water molecules is related to most of the unit cell volume reduction below 370 K, as shown by the contraction of the a-, b- and c-axes and the increase in the monoclinic angle. Loss of the Ca-coordinated W(2) and W(8) water molecules has a small effect on the unit cell volume as the continued contraction of the a- and c-axes is counter-balanced by a large expansion in the b-axis and a decrease in the monoclinic β angle. Unit Cell Volume Rietveld Refinement Dehydration Process Natural Zeolite Position Sensitive Detector Artioli, G. aut Hanson, J. C. aut Enthalten in Physics and chemistry of minerals Springer-Verlag, 1977 23(1996), 6 vom: Aug., Seite 328-336 (DE-627)129323039 (DE-600)131393-9 (DE-576)014557398 0342-1791 nnns volume:23 year:1996 number:6 month:08 pages:328-336 https://doi.org/10.1007/BF00199498 lizenzpflichtig Volltext GBV_USEFLAG_A SYSFLAG_A GBV_OLC FID-BIODIV SSG-OLC-PHY SSG-OLC-CHE SSG-OLC-GEO SSG-OLC-PHA SSG-OLC-DE-84 SSG-OPC-GGO GBV_ILN_11 GBV_ILN_32 GBV_ILN_40 GBV_ILN_70 GBV_ILN_130 GBV_ILN_2010 GBV_ILN_2018 GBV_ILN_2027 GBV_ILN_2279 GBV_ILN_4012 GBV_ILN_4046 GBV_ILN_4103 GBV_ILN_4112 GBV_ILN_4277 GBV_ILN_4306 GBV_ILN_4313 GBV_ILN_4319 GBV_ILN_4323 AR 23 1996 6 08 328-336 |
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Enthalten in Physics and chemistry of minerals 23(1996), 6 vom: Aug., Seite 328-336 volume:23 year:1996 number:6 month:08 pages:328-336 |
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the dehydration process in the zeolite laumontite: a real-time synchrotron x-ray powder diffraction study |
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The dehydration process in the zeolite laumontite: a real-time synchrotron X-ray powder diffraction study |
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Abstract The dehydration process of the natural zeolite laumontite $ Ca_{4} $$ Si_{16} $$ Al_{8} $$ O_{48} $ · 18 $ H_{2} $O has been studied in situ by means of powder diffraction and X-ray synchrotron radiation. Powder diffraction profiles suitable for Rietveld refinements were accumulated in time intervals of 5 minutes using a position sensitive detector (CPS-120 by INEL), while the temperature increased in steps of about 5 K. The synchronization of accumulation time and temperature plateau allowed collection of 62 temperature-resolved powder patterns in the range 310–584 K, whose analysis produced a dynamic picture of the laumontite structure response to dehydration. The first zeolitic water molecules diffusing out of the channels are those not bonded to the Ca cations and located in the W(1) site, whose occupancy drops smoothly to 10% during heating to 349 K, while the sample in the capillary is still submerged in water. The remaining W(1) and 60% of W(5) water molecules are expelled rather sharply at about 370 K. At this temperature all remaining water submerging the powder crystallites is lost, the structure contains about 13 water molecules/cell, and the crystal structure is that of leonhardite. On continued heating 80% of the water molecules from the W(2) site are lost between 420 and 480 K, while a small amount of the diffusing water is reinserted in the W(5) site. The occupancy factor of the W(8) site decreases starting at 480 K, and reaches a maximum loss of 20% at 584 K. The combined occupancy of the Ca-coordinated W (2) and W (8) water sites never falls much below two, so that the Ca cations in the channels, which are bonded to four framework oxygen atoms, are nearly six-coordinated in the explored temperature range. The water loss is accompanied by large changes in the unit cell dimensions. Except at 367 K, where the excess surrounding water is leaving, all changes in cell dimensions are gradual. The loss of the hydrogen bonded W(1) and W(5) water molecules is related to most of the unit cell volume reduction below 370 K, as shown by the contraction of the a-, b- and c-axes and the increase in the monoclinic angle. Loss of the Ca-coordinated W(2) and W(8) water molecules has a small effect on the unit cell volume as the continued contraction of the a- and c-axes is counter-balanced by a large expansion in the b-axis and a decrease in the monoclinic β angle. © Springer-Verlag 1996 |
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Abstract The dehydration process of the natural zeolite laumontite $ Ca_{4} $$ Si_{16} $$ Al_{8} $$ O_{48} $ · 18 $ H_{2} $O has been studied in situ by means of powder diffraction and X-ray synchrotron radiation. Powder diffraction profiles suitable for Rietveld refinements were accumulated in time intervals of 5 minutes using a position sensitive detector (CPS-120 by INEL), while the temperature increased in steps of about 5 K. The synchronization of accumulation time and temperature plateau allowed collection of 62 temperature-resolved powder patterns in the range 310–584 K, whose analysis produced a dynamic picture of the laumontite structure response to dehydration. The first zeolitic water molecules diffusing out of the channels are those not bonded to the Ca cations and located in the W(1) site, whose occupancy drops smoothly to 10% during heating to 349 K, while the sample in the capillary is still submerged in water. The remaining W(1) and 60% of W(5) water molecules are expelled rather sharply at about 370 K. At this temperature all remaining water submerging the powder crystallites is lost, the structure contains about 13 water molecules/cell, and the crystal structure is that of leonhardite. On continued heating 80% of the water molecules from the W(2) site are lost between 420 and 480 K, while a small amount of the diffusing water is reinserted in the W(5) site. The occupancy factor of the W(8) site decreases starting at 480 K, and reaches a maximum loss of 20% at 584 K. The combined occupancy of the Ca-coordinated W (2) and W (8) water sites never falls much below two, so that the Ca cations in the channels, which are bonded to four framework oxygen atoms, are nearly six-coordinated in the explored temperature range. The water loss is accompanied by large changes in the unit cell dimensions. Except at 367 K, where the excess surrounding water is leaving, all changes in cell dimensions are gradual. The loss of the hydrogen bonded W(1) and W(5) water molecules is related to most of the unit cell volume reduction below 370 K, as shown by the contraction of the a-, b- and c-axes and the increase in the monoclinic angle. Loss of the Ca-coordinated W(2) and W(8) water molecules has a small effect on the unit cell volume as the continued contraction of the a- and c-axes is counter-balanced by a large expansion in the b-axis and a decrease in the monoclinic β angle. © Springer-Verlag 1996 |
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Abstract The dehydration process of the natural zeolite laumontite $ Ca_{4} $$ Si_{16} $$ Al_{8} $$ O_{48} $ · 18 $ H_{2} $O has been studied in situ by means of powder diffraction and X-ray synchrotron radiation. Powder diffraction profiles suitable for Rietveld refinements were accumulated in time intervals of 5 minutes using a position sensitive detector (CPS-120 by INEL), while the temperature increased in steps of about 5 K. The synchronization of accumulation time and temperature plateau allowed collection of 62 temperature-resolved powder patterns in the range 310–584 K, whose analysis produced a dynamic picture of the laumontite structure response to dehydration. The first zeolitic water molecules diffusing out of the channels are those not bonded to the Ca cations and located in the W(1) site, whose occupancy drops smoothly to 10% during heating to 349 K, while the sample in the capillary is still submerged in water. The remaining W(1) and 60% of W(5) water molecules are expelled rather sharply at about 370 K. At this temperature all remaining water submerging the powder crystallites is lost, the structure contains about 13 water molecules/cell, and the crystal structure is that of leonhardite. On continued heating 80% of the water molecules from the W(2) site are lost between 420 and 480 K, while a small amount of the diffusing water is reinserted in the W(5) site. The occupancy factor of the W(8) site decreases starting at 480 K, and reaches a maximum loss of 20% at 584 K. The combined occupancy of the Ca-coordinated W (2) and W (8) water sites never falls much below two, so that the Ca cations in the channels, which are bonded to four framework oxygen atoms, are nearly six-coordinated in the explored temperature range. The water loss is accompanied by large changes in the unit cell dimensions. Except at 367 K, where the excess surrounding water is leaving, all changes in cell dimensions are gradual. The loss of the hydrogen bonded W(1) and W(5) water molecules is related to most of the unit cell volume reduction below 370 K, as shown by the contraction of the a-, b- and c-axes and the increase in the monoclinic angle. Loss of the Ca-coordinated W(2) and W(8) water molecules has a small effect on the unit cell volume as the continued contraction of the a- and c-axes is counter-balanced by a large expansion in the b-axis and a decrease in the monoclinic β angle. © Springer-Verlag 1996 |
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The loss of the hydrogen bonded W(1) and W(5) water molecules is related to most of the unit cell volume reduction below 370 K, as shown by the contraction of the a-, b- and c-axes and the increase in the monoclinic angle. 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