Shou-Ze Wang

Analysis of Geting Bituminous Coal by Electrospray Ionization and Direct Analysis in Real Time Mass Spectrometry

Understanding the structure and composition of coals is important for effective, clean, and value-added utilization. In addition to gas chromatography/mass spectrometry which is commonly used to analyze coal, mass spectrometry (MS) may be used with other ion sources such as electrospray ionization (ESI) and direct analysis in real time (DART) for characterization. In this work, Geting bituminous coal was extracted sequentially and exhaustively with petroleum ether, carbon disulfide, methanol, acetone, an isometric acetone/carbon disulfide mixture, tetrahydrofuran, and an isometric tetrahydrofuran/carbon disulfide mixture. Raw coal, extracts, and the extraction residue were analyzed using MS equipped with ESI or DART. Organic heteroatomic species in the extracts were determined by liquid chromatography-mass spectrometry equipped with ESI. Molecular weight distributions of organic species in raw coal, extracts, and extraction residue were characterized by ESI-MS and DART-MS. Associated molecules and homologous compounds in coal extracts were identified.

Characterization of humic acids extracted from a lignite and interpretation for the mass spectra

Humic acids obtained from a Chinese lignite via alkali treatment were analyzed using Fourier transform infrared spectroscopy and Orbitrap mass spectrometry coupled with an electrospray ion source (ESI-Orbitrap-MS). Raw coal and the corresponding residue were characterized via scanning electron microscopy and energy dispersive spectrometry. Over 4700 heteroatom-containing compounds with wide distributions of molecular mass and unsaturation degree were detected via the ESI-Orbitrap-MS, and around 60 percent of the detected species were found to be oxygen-containing compounds. In addition, van Krevelen diagram and double-bond equivalent (DBE) plot were introduced to provide more structural details of the compounds. For the species only containing C, H, and O (HACHO), condensed aromatic compounds with a DBE value over 20 only contained 1 or 2 oxygen atoms. Carboxyl- and hydroxyl-containing aliphatic compounds (CHCACs) were predominant in HACHO with 5 or 6 oxygen atoms. Both the CHCACs and aromatic carboxylic acids or phenols were grouped into clusters in the van Krevelen diagram to be recognized. The introduction of a nitrogen atom to the HACHO species was based on the structures of the HACHO species, which is also indicated by the van Krevelen diagram.

Evaluation of the Oxidation of Rice Husks with Sodium Hypochlorite Using Gas Chromatography-Mass Spectrometry and Direct Analysis in Real Time-Mass Spectrometry

Rice husk powder was oxidized in aqueous sodium hypochlorite solution under mild conditions with different reaction times. Fourier transform infrared spectroscopy, gas chromatography-mass spectrometry (GC-MS), and direct analysis in real time-mass spectrometry (DART-MS) were used to analyze the oxidation products. Results showed that oxidation was a feasible way to depolymerize the macromolecules in the biomass and convert hydroxyl groups to carboxyl groups. In total, 113 organic compounds in oxidation products with molecular mass less than 500 Da were identified using GC-MS. As an ambient ionization technique, DART-MS was applied to the determination of biomass derivatives and revealed mass distribution and molecular structure information for the rice husk oxidation products.

Analysis of the Products from the Oxidation of Geting Bituminous Coal by Atmospheric Pressure Photoionization–Mass Spectrometry

Geting bituminous coal was directly oxidized in aqueous sodium hypochlorite. The reaction mixture was sequentially extracted with ethyl ether and ethyl acetate. Both extracts were esterified with diazomethane to obtain methyl esterified products, which were analyzed using high performance liquid chromatography–mass spectrometry with electrospray ionization or atmospheric pressure photoionization. A large number of low- and nonpolar products with relatively high molecular masses were determined using atmospheric pressure photoionization mass spectrometry. Toluene and a toluene/anisole mixture (vol/vol = 95:5) were added to the atmospheric pressure photoionization system as dopants. Toluene induced better ionization than the toluene/anisole mixture in both ion signal intensity and number of detected species. Most of the molecular associated compounds contained heteroatoms.

Characterization of Oxygenates, Nitrogenates, and Sulfonates in Shengli Lignite Extracts by Orbitrap Mass Spectrometry

ABSTRACT A series of carbon disulfide/acetone mixtures were used to extract organic species from Shengli lignite, a Chinese coal. Orbitrap mass spectrometry coupled with electrospray ionization was used to characterize the molecules in the extracts. Heteroatomic species, including oxygenates, nitrogenates, and sulfonates, were determined. Pure carbon disulfide or acetone had the lowest extraction for oxygenates while the mixtures increased the relative abundance of oxygenates. From the value of the double bond equivalence, the compounds with 1 oxygen contained the highest concentrations of aromatics and aliphatics, but compounds with 6 were aliphatic with a double bond equivalence of 3. For compounds containing 2 oxygens, aromatics with one ring were present at the highest concentrations in the 1:1 carbon disulfide:acetone extract. For compounds containing 3, 4, and 5 oxygens, most aromatic species were identified with double bond equivalence values between 4 and 6, showing the presence of an aromatic ring. The results indicated that the solvent mixtures enhanced the extraction of oxygenates from Shengli lignite.

The compositional features of thermally soluble fractions from two Chinese coals in cyclohexane

Shengli lignite (SL) and Shenmu-Fugu subbituminous coal (SFSBC) were subjected to thermal dissolution in cyclohexane at 300°C for 1 h under hydrogen. The reaction mixtures were extracted with petroleum ether (PE) and the PE-extractable fractions (PEEFs) were analyzed with a gas chromatography/mass spectrometer. The results show that the PEEFs from thermally dissolved SL (TDSL) and thermally dissolved SFSBC (TDSFSBC) mainly consist of alkanes, alkenes, arenes, and oxygen-containing organic compounds (OCOCs); the yields of alkanes and alkenes in the PEEF from TDSFSBC are appreciably higher than those from TDSL, while the yields of arenes and oxygen-containing organic compounds in the petroleum ether-extractable fraction from thermally dissolved Shenmu-Fugu subbituminous coal are significantly lower than those from thermally dissolved Shengli lignite; arenols are dominant OCOCs in the PEEF from TDSL, while main OCOCs in the PEEFs from TDSFSBC are arenols and esters.

Evaluation of an Upgraded Bio-oil from the Pyrolysis of Rice Husk by Acidic Resin-catalyzed Esterification

A raw bio-oil (RBO) from pyrolysis of rice husk was upgraded by catalytic esterification with methanol over an acidic resin. Both RBO and the upgraded bio-oil (UBO) were analyzed with a Fourier transform infrared spectrometer, pH meter, and an elemental analyzer. They were extracted sequentially with n-hexane, CCl4, CS2, benzene, and CH2Cl2. All of the extracts were analyzed with gas chromatography/mass spectrometer. The results showed that the carboxylic acids (CA) in the RBO were converted to their corresponding methyl esters (MEs), leading to a significant increase in pH value from 2.8 (RBO) to 5.3 (UBO). The total extract yield of UBO is much higher than that of RBO. In total, 20 CAs and 19 MEs were identified. The CAs include two alkenoic acids, a cycloalkanecarboxylic acid, a hydroxyalkanoic acid, a hydroxyalkenoic acid, an oxyalkanoic acid, a methoxyoxyalkanoic acid, an alkanedioic acid, an oxyalkanedioic acid, an aminoalkanoic acid, two furoic acids, three substituted benzoic acids, and five substituted phenylalkanoic acids.

Investigation on Infrared Laser Desorption of Solid Matrix Using Scanning Electron Microscope and Fast Photography

Infrared light from a pulsed optical parametric oscillator laser system was used to irradiate succinic acid (SA), a usual solid matrix used in matrix‐assisted laser desorption ionization, under vacuum. Ablated SA particles were trapped using a silica plate mounted 3.0 mm above and parallel to the sample surface. The morphology and particle size of ablated particles at different laser fluences were investigated using a scanning electron microscope (SEM). The dynamics of plume propagation for SA desorption process was studied with fast photography at atmospheric pressure. Plume expanding at 1.12 J/cm2 laser fluence was recorded using a high‐speed CMOS camera and corresponding propagation distance was measured. The solid matrix desorption was driven by phase explosion according to plume model fitting, which was consistent with the results of SEM. Microsc. Res. Tech. 76:744–750, 2013.