Thermal degradation of aromatic-aliphatic polyethers. 2. Flash pyrolysis-gas chromatography-mass spectrometry

Montaudo, Giorgio; Puglisi, Concetto; Scamporrino, Emilio; Vitalini, Daniele

doi:10.1021/ma00157a068

Cited by 12 publications

(5 citation statements)

References 9 publications

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“…The remaining material at 600 °C could be a combination of nonvolatile organics including char from polymerization of chemical additives and isotropic coke, as previously discussed using microscopic analysis. The results of high-resolution mass spectroscopy and pyrolysis GC-MS regarding the presence of polyethers and nonylphenols and their thermal chemistry are consistent with what has been reported in the literature. − …”

Section: Resultssupporting

confidence: 88%

“…Integrated analytical instruments such as TGA/high-resolution mass and pyrolysis GC-MS have been applied to characterize high boiling points and heavy hydrocarbons, including asphaltenes. 25−31 Thermal degradation of aromatic−aliphatic polyethers has been studied using direct pyrolysis mass spectrometry 32 and by pyrolysis GC-MS. 33 Among the pyrolysis products detected were aldehydes, phenols, ethers, and aliphatic and aromatic hydrocarbons. It was shown in Py-GC-MS experiments that the pyrolysis products are separated and quantified, and from product distribution, the authors identified the original polymer.…”

Section: ■ Results and Discussionmentioning

confidence: 99%

“…However, in some cases, from identification of the pyrolysis products, it was not possible to recompose the original polymer. 33 Using the PY-GC-MS method outlined in the Experimental Section, the TI fraction of exchanger 3 previously extracted in the ASE unit with CH 2 Cl 2 /CH 3 OH (9:1) was subjected to analysis outlined in Figure 11. The results are summarized in Table 3.…”

Section: ■ Results and Discussionmentioning

confidence: 99%

“…It was shown in Py-GC-MS experiments that the pyrolysis products are separated and quantified, and from product distribution, the authors identified the original polymer. However, in some cases, from identification of the pyrolysis products, it was not possible to recompose the original polymer …”

Section: Resultsmentioning

confidence: 99%

“…Since the solvents used were unable to remove organics from the surface of the solids, it was thought that applying heat should desorb organics, which were subsequently analyzed using different analytical tools. Integrated analytical instruments such as TGA/high-resolution mass and pyrolysis GC-MS have been applied to characterize high boiling points and heavy hydrocarbons, including asphaltenes. − Thermal degradation of aromatic–aliphatic polyethers has been studied using direct pyrolysis mass spectrometry and by pyrolysis GC-MS . Among the pyrolysis products detected were aldehydes, phenols, ethers, and aliphatic and aromatic hydrocarbons.…”

Section: Resultsmentioning

confidence: 99%

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Investigation of the Chemical Composition of the Organic Material Associated with Inorganic Solids Found in Heat Exchanger Deposits: Possible Fouling Precursor in Refinery Operation

Hurt,

Ovalles,

Murray

et al. 2023

Energy Fuels

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In the oil sand literature, the deposits containing organics associated with solids and insoluble in toluene are often referred to as toluene-insoluble organic material (TIOM). In this work, we call these materials toluene insolubles (TI) and clarify what TIOM means. Our focus in this work is to determine the chemical composition of the organic portion of the TI obtained from the extraction of fouling deposits collected from a heat exchanger unit of a refinery. Analysis of TI using thermogravimetric analysis (TGA), optical microscopy, inductive coupling plasma (ICP), and X-ray diffraction (XRD) showed that these materials are composed of both organic and inorganic solids/clay minerals. Using an accelerated solvent extraction (ASE) unit, the TI fraction was sequentially solvent-extracted using methylene chloride/methanol (9:1, at 110 °C/1000 psi) and acetonitrile CH 3 CN (ACN, at 130 °C/1000 psi). The extracted fractions were then analyzed by using high-resolution mass spectrometry (HRMS) and Fourier transform infrared (FTIR). The results showed that the extracted materials were mainly organic polymers consisting of a variety of polyethers used as chemical additives in the oil industry. The analysis by atmospheric pressure photoionization (APPI) in positive ion mode and electrospray ionization (ESI) in positive and negative ion modes revealed that besides the predominant polyether polymer in the form of ethylene oxide (EO) and propylene oxide (PO), there are also condensed aromatics, pyridine, alkylpyridines, sulfonates, low-carbon low-double bond equivalent (DBE) species with one heteroatom, and acidic species. A subsequent analysis of the blank solvent obtained from the ASE unit by HRMS showed that no polyether polymers were present, indicating that these polymers are part of the foulant deposits. To obtain more structural information on the organic fraction, the TI sample was subjected to pyrolysis gas chromatography−mass spectrometry (GC-MS) between 300 and 600 °C. Compositional analysis revealed that the volatile organic fraction of the TI is composed mostly of polar components with oxygen and nitrogen functionality, including phenols, indoles, alkylpyrroles, aldehydes, and carboxylic acids. These products are most likely from the decomposition of polyethers as well as nonylphenols used as chemical additives. The presence of intact nonylphenol indicates the desorption of polar molecules from the surface of clays/minerals during pyrolysis. The results of this work have demonstrated that fouling deposits of a heat exchanger formed by organic molecules associated with inorganic solids are not only derived from the original oil but also derived from chemical additives that are used during oil production/processing.

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Section: Resultssupporting

confidence: 88%

Section: ■ Results and Discussionmentioning

confidence: 99%

Section: ■ Results and Discussionmentioning

confidence: 99%

Section: Resultsmentioning

confidence: 99%

Section: Resultsmentioning

confidence: 99%

See 3 more Smart Citations

Investigation of the Chemical Composition of the Organic Material Associated with Inorganic Solids Found in Heat Exchanger Deposits: Possible Fouling Precursor in Refinery Operation

Hurt,

Ovalles,

Murray

et al. 2023

Energy Fuels

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Thermal analyses of graft copolymers of poly (methyl methacrylate) main chain with poly (propylene oxide‐b‐ethylene oxide) graft chain

Lucas

Porter

1993

J of Applied Polymer Sci

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SYNOPSISPoly (methyl methacrylate-g-(propylene oxide-b-ethylene oxide) ) and poly (methyl methacrylate-g-(ethylene oxide-b-propylene oxide) ) , comprising chemically dissimilar sequences, exhibit intramolecular phase separation. These compositions have applications in coatings and as surface-tension modifiers. This paper presents the thermal behavior of these graft copolymers: separate samples of the homopolymer and of the grafts were also analyzed to provide comparisons. The phase behavior has been analyzed by differential scanning calorimetry and by dynamic-mechanical thermal measurements. Two glass transitions ( T,) are observed, caused by the partial incompatibility within the copolymers. The activation energy of the Tg relaxation process of the main chain is decreased by the graft chain. The influence of poly (propylene oxide-b-ethylene oxide) grafts on the thermal degradation of the poly( methyl methacrylate) (PMMA) main chain was studied by using thermogravimetric analysis. Prolysis of the graft copolymers occurs in three stages and begins on the graft chain and at a lower temperature than the pyrolysis of pure PMMA. Both the phase behavior and the thermal stability are found to depend sensitively on the composition of the copolymer. 0 1993 John Wiley & Sons, Inc. INTRODUCTIONPoly ( methyl methacrylate-g-(propylene oxide-bethylene oxide) ) and poly (methyl methacrylate-g-(ethylene oxide-b-propylene oxide) ) , having sequences that are chemically dissimilar, exhibit intramolecular phase separation. Their properties lead to a number of specific applications such as in coatings, surface modifiers, and as surface-tension agents. The thermal behavior of these graft copolymers were examined in separate samples of the homopolymer and in the grafts analyzed to provide comparisons. Concerning the main chain, poly-(methyl methacrylate) (PMMA) , prepared by the conventional free-radical method is known to be about 60% syndiotactic, and has a glass transition temperature, Tg, of about 100°C. The pure syndiotactic stereoregular form has a Tg of 115°C.

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Mechanism of thermal generation of poly(p-phenylene vinylene) from poly(p-xylene-α-dimethylsulphonium halides)

Montaudo

Vitalini

Lenz

1987

Polymer

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Thermal degradation of aromatic-aliphatic polyethers. 2. Flash pyrolysis-gas chromatography-mass spectrometry

Cited by 12 publications

References 9 publications

Investigation of the Chemical Composition of the Organic Material Associated with Inorganic Solids Found in Heat Exchanger Deposits: Possible Fouling Precursor in Refinery Operation

Investigation of the Chemical Composition of the Organic Material Associated with Inorganic Solids Found in Heat Exchanger Deposits: Possible Fouling Precursor in Refinery Operation

Thermal analyses of graft copolymers of poly (methyl methacrylate) main chain with poly (propylene oxide‐b‐ethylene oxide) graft chain

Mechanism of thermal generation of poly(p-phenylene vinylene) from poly(p-xylene-α-dimethylsulphonium halides)

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