Synchrotron X-ray studies of metal-organic framework M2(2,5-dihydroxyterephthalate), M = (Mn, Co, Ni, Zn) (MOF74)

2012 ◽  
Vol 27 (4) ◽  
pp. 256-262 ◽  
Author(s):  
W. Wong-Ng ◽  
J. A. Kaduk ◽  
H. Wu ◽  
M. Suchomel
Keyword(s):  
Powder Diffraction ◽  
Metal Organic Framework ◽  
National Laboratory ◽  
Argonne National Laboratory ◽  
Lattice Parameter ◽  
X Ray ◽  
Metal Organic ◽  
Sorbent Materials ◽  
Diffraction Patterns ◽  
Unsaturated Metal Sites

M2(dhtp)·nH2O (M = Mn, Co, Ni, Zn; dhtp = 2,5-dihydroxyterephthalate), known as MOF74, is a family of excellent sorbent materials for CO2 that contains coordinatively unsaturated metal sites and a honeycomb-like structure featuring a broad one-dimensional channel. This paper describes the structural feature and provides reference X-ray powder diffraction patterns of these four isostructural compounds. The structures were determined using synchrotron diffraction data obtained at beam line 11-BM at the Advanced Photon Source (APS) in the Argonne National Laboratory. The samples were confirmed to be hexagonal R 3 (No. 148). From M = Mn, Co, Ni, to Zn, the lattice parameter a of MOF74 ranges from 26.131 73(4) Å to 26.5738(2) Å, c from 6.651 97(5) to 6.808 83(8) Å, and V ranges from 3948.08 Å3 to 4163.99 Å3, respectively. The four reference X-ray powder diffraction patterns have been submitted for inclusion in the Powder Diffraction File (PDF).

scholarly journals Reference diffraction patterns, microstructure, and pore-size distribution for the copper (II) benzene-1,3,5-tricarboxylate metal organic framework (Cu-BTC) compounds

2014 ◽  
Vol 30 (1) ◽  
pp. 2-13 ◽  
Author(s):  
W. Wong-Ng ◽  
J.A. Kaduk ◽  
D.L. Siderius ◽  
A.L. Allen ◽  
L. Espinal ◽  
...  
Keyword(s):  
Pore Size Distribution ◽  
Pore Size ◽  
Size Distribution ◽  
Powder Diffraction ◽  
Small Angle ◽  
Metal Organic Framework ◽  
X Ray ◽  
Metal Organic ◽  
Diffraction Patterns ◽  
Organic Framework

Cu-paddle-wheel-based Cu3(BTC)2 (nicknamed Cu-BTC, where BTC ≡ benzene 1,3,5-tricarboxylate) is a metal organic framework (MOF) compound that adopts a zeolite-like topology. We have determined the pore-size distribution using the Gelb and Gubbins technique, the microstructure using small-angle neutron scattering and (ultra) small-angle X-ray scattering (USAXS\SAXS) techniques, and X-ray powder diffraction reference patterns for both dehydrated d-Cu-BTC [Cu3(C9H3O6)2] and hydrated h-Cu-BTC [Cu3(C9H3O6)2(H2O)6.96] using the Rietveld refinement technique. Both samples were confirmed to be cubic Fm$\bar 3$m (no. 225), with lattice parameters of a = 26.279 19(3) Å, V = 18 148.31(6) Å3 for d-Cu-BTC, and a = 26.3103(11) Å, and V = 18 213(2) Å3 for h-Cu-BTC. The structure of d-Cu-BTC contains three main pores of which the diameters are approximately, in decreasing order, 12.6, 10.6, and 5.0 Å. The free volume for d-Cu-BTC is approximately (71.85 ± 0.05)% of the total volume and is reduced to approximately (61.33 ± 0.03)% for the h-Cu-BTC structure. The d-Cu-BTC phase undergoes microstructural changes when exposed to moisture in air. The reference X-ray powder patterns for these two materials have been determined for inclusion in the Powder Diffraction File.

Powder X-ray structural studies and reference diffraction patterns for three forms of porous aluminum terephthalate, MIL-53(A1)

2019 ◽  
Vol 34 (3) ◽  
pp. 216-226 ◽  
Author(s):  
W. Wong-Ng ◽  
H. G. Nguyen ◽  
L. Espinal ◽  
D. W. Siderius ◽  
J. A. Kaduk
Keyword(s):  
High Temperature ◽  
Metal Organic Framework ◽  
Space Group ◽  
X Ray ◽  
Porous Aluminum ◽  
Refinement Method ◽  
Three Samples ◽  
Metal Organic ◽  
A Cell ◽  
Diffraction Patterns

Powder X-ray diffraction patterns for three forms of MIL-53(Al), a metal organic framework (MOF) compound with breathing characteristics, were investigated using the Rietveld refinement method. These three samples are referred to as the MIL-53(Al)as-syn (the as synthesized sample), orthorhombic, Pnma, a = 17.064(2) Å, b = 6.6069(9) Å, c = 12.1636(13) Å, V = 1371.3(2) Å3, Z = 4), MIL-53(Al)LT-H (low-temperature hydrated phase, monoclinic P21/c, a = 19.4993(8) Å, b = 15.2347(6) Å, c = 6.5687(3) Å, β = 104.219(4) °, V = 1891.55(10) Å3, Z = 8), and MIL-53(Al)HT-D (high-temperature dehydrated phase, Imma, a = 6.6324(5) Å, b = 16.736(2) Å, c = 12.840(2), V = 1425.2(2) Å3, Z = 4). The crystal structures of the “as-syn” sample and the HT-D sample are confirmed to be the commonly adopted ones. However, the structure of the MIL-53(Al)LT-H phase is confirmed to be monoclinic with a space group of P21/c instead of the commonly accepted space group Cc, resulting in a cell volume double in size. The structure has two slightly different types of channel. The pore volumes and pore surface area were estimated to be 0.11766 (8) cm3/g and 1461.3(10) m2/g for MIL-53(Al)HT-D (high-temperature dehydrated phase), and 0.08628 (5) cm3/g and 1401.6 (10) m2/g for MIL-53(Al)as-syn phases, respectively. The powder patterns for the MIL-53(Al)as-syn and MIL-53(Al)HT-D phases are reported in this paper.

scholarly journals High pressure effects on hydrate Cu-BTC investigated by vibrational spectroscopy and synchrotron X-ray diffraction

RSC Advances ◽  
2017 ◽  
Vol 7 (87) ◽  
pp. 55504-55512 ◽  
Author(s):  
Zhaohui Dong ◽  
Zhongying Mi ◽  
Weiguang Shi ◽  
Hui Jiang ◽  
Yi Zheng ◽  
...  
Keyword(s):  
High Pressure ◽  
Vibrational Spectroscopy ◽  
Powder Diffraction ◽  
Metal Organic Framework ◽  
Pressure Effects ◽  
X Ray Diffraction ◽  
X Ray ◽  
Metal Organic ◽  
High Pressure Effects

The high pressure behaviors of hydrate Cu-BTC metal–organic framework (MOF) in terms of phase stability, compressibility and reversibility were investigated in situ by synchrotron X-ray powder diffraction as well as vibrational spectroscopy.

The Far Infrared Spectra and X-Ray Powder Diffraction Patterns of the Structure I Hydrates of Cyclopropane and Ethylene Oxide at 100 °K

1975 ◽  
Vol 53 (1) ◽  
pp. 71-75 ◽  
Author(s):  
John E. Bertie ◽  
Frances E. Bates ◽  
David K. Hendricksen
Keyword(s):  
Infrared Spectrum ◽  
Ethylene Oxide ◽  
Diffraction Pattern ◽  
Powder Diffraction ◽  
Low Frequency ◽  
Far Infrared ◽  
Lattice Parameter ◽  
X Ray ◽  
Oxide Hydrate ◽  
Diffraction Patterns

This paper presents the far-infrared spectrum and X-ray powder diffraction pattern of the structure I hydrate of cyclopropane at 100 °K, and the powder diffraction pattern of the isostructural ethylene oxide hydrate at 100 °K. Between 360 and 100 cm−1 the absorption by cyclopropane hydrate is essentially identical to that by ethylene oxide hydrate, but is shifted to low frequency by about 2%. This shift is undoubtedly related to the hydrogen bonds being slightly longer in cyclopropane hydrate, whose cubic lattice parameter is 11.98 ± 0.02 Å compared to 11.89 ± 0.02 Å for ethylene oxide hydrate, both at 110 ± 20 °K. The absorption by cyclopropane hydrate below 100 cm−1 decreases rapidly with decreasing frequency; this confirms that the absorption plateau observed for ethylene oxide hydrate between 100 and about 50 cm−1 is due to primarily rotational vibrations of ethylene oxide. A recent statement, that the orientational disorder of the water molecules need not be invoked to explain the far infrared spectrum of ice 1 h, is disputed.

Pyromorphite formation and stability after quick lime neutralisation in the presence of soil and clay sorbents

2007 ◽  
Vol 4 (2) ◽  
pp. 109 ◽  
Author(s):  
Mark A. Chappell ◽  
Kirk G. Scheckel
Keyword(s):  
Phosphoric Acid ◽  
Contaminated Soils ◽  
National Laboratory ◽  
Argonne National Laboratory ◽  
Natural Soil ◽  
X Ray Diffraction ◽  
Quick Lime ◽  
X Ray ◽  
Soil Systems ◽  
Diffraction Patterns

Environmental context. Questions remain regarding the potential risk of human Pb exposure from metal-contaminated soils. Studies show that the risk of human exposure is more accurately linked to the toxicity of the Pb species in soil than the total quantity of Pb. This work explores the practicality of converting Pb to a less toxic, less bioavailable species called pyromorphite in the presence of soil. Abstract. Soluble Pb is immobilised in pure systems as pyromorphite by adding sources of P, but doubts remain about the effectiveness of this approach in natural soil systems, particularly given the ability of soil humic substances to interfere with Pb-mineral formation. In addition, recent thermodynamic modelling predicts that pyromorphite formed by the addition of phosphoric acid to Pb-contaminated soils, followed by neutralisation with quick lime (Ca(OH)2) will destabilise the mineral, reverting the Pb back to more soluble species such as cerussite or anglesite. In this paper, we describe experiments to form pyromorphite in the presence of two different sorbents: a reference smectite called Panther Creek Bentonite, and a commercially available, organically rich potting mixture. We present X-ray diffraction (XRD) evidence suggestive of pyromorphite formation, yet, like similar studies, the evidence is less than conclusive. Linear combination fits of Pb X-ray absorption fine-structure spectroscopy (XAFS) data collected at the Advanced Photon Source at Argonne National Laboratory show that pyromorphite is the major Pb species formed after the addition of phosphoric acid. Furthermore, XAFS data shows that neutralising with quick lime enhances (as opposed to reducing) pyromorphite content in these systems. These results call into question relying solely on XRD data to confirm or deny the existence of minerals like pyromorphite, whose complex morphology give less intense and more complicated diffraction patterns than some of the simpler Pb minerals.

scholarly journals Equation of state of hydrous Fo90 ringwoodite to 45 GPa by synchrotron powder diffraction

2005 ◽  
Vol 69 (3) ◽  
pp. 317-323 ◽  
Author(s):  
M. H. Manghnani ◽  
G. Amulele ◽  
J. R. Smyth ◽  
C. M. Holl ◽  
G. Chen ◽  
...  
Keyword(s):  
Equation Of State ◽  
Powder Diffraction ◽  
National Laboratory ◽  
Argonne National Laboratory ◽  
X Ray Diffraction ◽  
Third Order ◽  
X Ray ◽  
Synchrotron Powder Diffraction ◽  
Murnaghan Equation ◽  
Photon Source

AbstractThe equation of state of Fo90 hydrous ringwoodite has been measured using X-ray powder diffraction to 45 GPa at the GSECARS beam line at the Advanced Photon Source synchrotron at Argonne National Laboratory. The sample was synthesized at 1400°C and 20 GPa in the 5000 ton multi anvil press at Bayerisches Geoinstitut in Bayreuth. The sample has the formula Mg1.70Fe0.192+ Fe0.023+H0.13- Si1.00O4 as determined by electron microprobe, Fourier transform infrared and Mössbauer spectroscopies, and contains ~0.79% H2O by weight. Compression of the sample had been been measured previously to 11 GPa by single crystal X-ray diffraction. A third-order Birch-Murnaghan equation of state fit to all of the data gives V0 = 530.49±0.07 Å3, K0 = 174.6±2.7 GPa and K' = 6.2±0.6. The effect of 1% H incorporation in the structure on the bulk modulus is large and roughly equivalent to an increase in the temperature of ∼600°C at low pressure. The large value of K' indicates significant stiffening of the sample with pressure so that the effect of hydration decreases with pressure.

scholarly journals Powder X-ray diffraction of fluorometholone, C22H29FO4

2020 ◽  
Vol 35 (1) ◽  
pp. 71-72
Author(s):  
Diana Gonzalez ◽  
Joseph T. Golab ◽  
James A. Kaduk ◽  
Amy M. Gindhart ◽  
Thomas N. Blanton
Keyword(s):  
Hydrogen Bonds ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Density Functional ◽  
National Laboratory ◽  
Argonne National Laboratory ◽  
The United States ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
X Ray

Commercial fluorometholone, CAS #426-13-1, crystallizes in the monoclinic space group P21 (#4) with a = 6.40648(2), b = 13.43260(5), c = 11.00060(8) Å, β = 92.8203(5)°, V = 945.517(5) Å3, and Z = 2. A reduced cell search in the Cambridge Structural Database yielded one previous structure determination, using single-crystal data at 292 K. In this work, the sample was ordered from the United States Pharmacopeial Convention (Lot # R032K0) and analyzed as-received. The room temperature (295 K) crystal structure was refined using synchrotron (λ = 0.412826 Å) powder diffraction data and optimized using density functional theory (DFT) techniques. Hydrogen positions were included as a part of the structure and were re-calculated during the refinement. The diffraction data were collected on beamline 11-BM at the Advanced Photon Source, Argonne National Laboratory, and the powder X-ray diffraction pattern of the compound has been submitted to ICDD® for inclusion in the Powder Diffraction File™. The agreement of the Rietveld-refined and DFT-optimized structures is excellent; the root-mean-square Cartesian displacement is 0.060 Å. In addition to the O–H⋯O hydrogen bonds observed by Park et al. (Park, Y. J., Lee, M. Y., and Cho, S. I. (1992). “Fluorometholone,” J. Korean Chem. Soc. 36, 812–817), C–H⋯O hydrogen bonds contribute to the crystal energy.

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