First High-Resolution <sup>11</sup>B Nuclear Magnetic Resonance (NMR) Spectra of Coal Fly Ash by Satellite-Transition Magic Angle Spinning (STMAS) NMR

Takahashi, Takafumi; Kashiwakura, Shunsuke; Kanehashi, Koji; Nagasaka, Tetsuya

doi:10.1021/ef800886n

Cited by 8 publications

(29 citation statements)

References 20 publications

(34 reference statements)

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“…Furthermore, there are strong spinning side bands in the 11 B MAS spectra of N-CFA. As described elsewhere (Takahashi et al, 2009b), this observation implies that the boron and iron atoms in N-CFA are positioned at close range. The sidebands appear for the trigonal BO 3 , but not for tetrahedral BO 4 .…”

Section: Resultssupporting

confidence: 74%

“…in a sea-island structure, and boron is strongly concentrated in the CaO phase, and not in the MgO phase. Furthermore, the FIB-TOF-SIMS analysis has proved our estimation (Takahashi et al, 2009b) that boron and iron in N-CFA are positioned at close range.…”

Section: Resultssupporting

confidence: 63%

“…11 B MAS and STMAS NMR spectra were acquired using a 16.4 T narrow bore magnet (JEOL-ECA700) equipped with a home-built STMAS probe. The detailed experimental conditions were described elsewhere (Takahashi et al, 2009a;Takahashi et al, 2009b A TOF-SIMS instrument was also originally designed and developed. The details have been described elsewhere by one of the authors .…”

Section: Methodsmentioning

confidence: 99%

“…Few 11 B NMR spectra for CFA have been reported, although 29 Si and 23 Na NMR spectra have been often acquired to characterize activated CFA (Skavaraa et al, 2007;Criado et al, 2008). Most recently, some authors have succeeded in obtaining high-resolution B satellite transition magic angle spinning (STMAS) NMR spectra from two types of CFA samples (Takahashi et al, 2009a;Takahashi et al, 2009b). It has been proven by STMAS NMR that boron in the two CFA samples certainly differed in its chemical state.…”

Section: Introductionmentioning

confidence: 99%

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Chemical state of boron in coal fly ash investigated by focused-ion-beam time-of-flight secondary ion mass spectrometry (FIB-TOF-SIMS) and satellite-transition magic angle spinning nuclear magnetic resonance (STMAS NMR)

et al. 2010

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The chemical states of boron in coal fly ash, which may control its leaching into the environment, were investigated by focused-ion-beam time-of-flight secondary ion mass spectrometry (FIB-TOF-SIMS) and satellite-transition magic angle spinning nuclear magnetic resonance (STMAS NMR) spectroscopy. The distribution of boron on the surface and in the interior of micron-sized fly ash particles was directly observed by FIB-TOF-SIMS. Coordination numbers of boron and its bonding with different atoms from particles of bulk samples were investigated by STMAS NMR. Boron in coal fly ash with relatively poor leaching characteristics appears as trigonal BO(3) and coexists with Ca and Fe at the outer layer of every particle and inside CaO-MgO particles. In contrast, boron in coal fly ash with better leaching characteristics appears as CaO- or MgO-trigonal BO(3) and tetragonal BO(4), and it is distributed only on the outer surface of each ash particle without showing any correlation with a particular element.

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Section: Resultssupporting

confidence: 74%

Section: Resultssupporting

confidence: 63%

Section: Methodsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

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Chemical state of boron in coal fly ash investigated by focused-ion-beam time-of-flight secondary ion mass spectrometry (FIB-TOF-SIMS) and satellite-transition magic angle spinning nuclear magnetic resonance (STMAS NMR)

et al. 2010

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“…Boron is universally found in crust and ocean on the earth although scarcely in cosmic space (1). Stable isotope composition of boron ( 10 B, 11 B) is one of the most useful geological indicators for tracing the origin of fluids (2,3). Consumption of boron by organisms is essential for cell wall architecture, membrane function, and metabolic activities (4).…”

Section: Introductionmentioning

confidence: 99%

Analysis of Atomic Scale Chemical Environments of Boron in Coal by ¹¹B Solid State NMR

Takahashi

Kashiwakura

Kanehashi

et al. 2010

Environ. Sci. Technol.

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Atomic scale chemical environments of boron in coal has been studied by solid state NMR spectroscopy including magic angle spinning (MAS), satellite transition magic angle spinning (STMAS), and cross-polarization magic angle spinning (CPMAS). The (11)B NMR spectra can be briefly classified according to the degree of coalification. On the (11)B NMR spectra of lignite, bituminous, and sub-bituminous coals (carbon content of 70-90mass%), three sites assigned to four-coordinate boron ([4])B with small quadrupolar coupling constants (≤0.9 MHz) are observed. Two of the ([4])B sites in downfield are considered organoboron complexes with aromatic ligands, while the other in the most upper field is considered inorganic tetragonal boron (BO(4)). By contrast, on the (11)B NMR spectra of blind coal (carbon content >90mass%), the ([4])B which substitutes tetrahedral silicon of Illite is observed as a representative species. It has been considered that the organoboron is decomposed and released from the parent phase with the advance of coal maturation, and then the released boron reacts with the inorganic phase to substitute an element of inorganic minerals. Otherwise boron contained originally in inorganic minerals might remain preserved even under the high temperature condition that is generated during coalification.

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MAS, STMAS and DQMAS NMR Studies of the Thermal Transformation of Kaolinite

et al. 2013

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First High-Resolution ¹¹B Nuclear Magnetic Resonance (NMR) Spectra of Coal Fly Ash by Satellite-Transition Magic Angle Spinning (STMAS) NMR

Cited by 8 publications

References 20 publications

Chemical state of boron in coal fly ash investigated by focused-ion-beam time-of-flight secondary ion mass spectrometry (FIB-TOF-SIMS) and satellite-transition magic angle spinning nuclear magnetic resonance (STMAS NMR)

Chemical state of boron in coal fly ash investigated by focused-ion-beam time-of-flight secondary ion mass spectrometry (FIB-TOF-SIMS) and satellite-transition magic angle spinning nuclear magnetic resonance (STMAS NMR)

Analysis of Atomic Scale Chemical Environments of Boron in Coal by ¹¹B Solid State NMR

MAS, STMAS and DQMAS NMR Studies of the Thermal Transformation of Kaolinite

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First High-Resolution 11B Nuclear Magnetic Resonance (NMR) Spectra of Coal Fly Ash by Satellite-Transition Magic Angle Spinning (STMAS) NMR

Cited by 8 publications

References 20 publications

Chemical state of boron in coal fly ash investigated by focused-ion-beam time-of-flight secondary ion mass spectrometry (FIB-TOF-SIMS) and satellite-transition magic angle spinning nuclear magnetic resonance (STMAS NMR)

Chemical state of boron in coal fly ash investigated by focused-ion-beam time-of-flight secondary ion mass spectrometry (FIB-TOF-SIMS) and satellite-transition magic angle spinning nuclear magnetic resonance (STMAS NMR)

Analysis of Atomic Scale Chemical Environments of Boron in Coal by 11B Solid State NMR

MAS, STMAS and DQMAS NMR Studies of the Thermal Transformation of Kaolinite

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First High-Resolution ¹¹B Nuclear Magnetic Resonance (NMR) Spectra of Coal Fly Ash by Satellite-Transition Magic Angle Spinning (STMAS) NMR

Analysis of Atomic Scale Chemical Environments of Boron in Coal by ¹¹B Solid State NMR