End Group Analysis of Polyether Polyols by Nuclear Magnetic Resonance (NMR) Spectroscopy

Groom, T.; Babiec, John S.; Leuwen, Bruce G. Van

doi:10.1177/0021955x7401000105

Cited by 12 publications

(5 citation statements)

References 2 publications

(1 reference statement)

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“…Several 1 H‐NMR and 19 F‐NMR methods were developed for the determination of the polyol properties mentioned above . These methods, although very fast and accurate, rely on the addition of several reagents and hence require lengthy multistep sample preparation before the final measurement can be performed.…”

Section: Introductionmentioning

confidence: 99%

Quantitative adiabatic‐refocused INEPT (QA‐RINEPT) as a tool for fast and reliable characterization of polyols

Sabatino

Gao

Hou

2018

Magnetic Reson in Chemistry

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C nuclear magnetic resonance (NMR) is a powerful tool for the detailed characterization and structure elucidation of polymeric samples. The low natural abundance and sensitivity of the C isotope, however, lead to very long acquisition time, therefore limiting the use of such technique. We report here the implementation of a quantitative method, quantitative adiabatic-refocused insensitive nuclei enhanced by polarization transfer (QA-RINEPT), for the characterization of polyol samples. The method, based on the well-known insensitive nuclei enhanced by polarization transfer sequence, allows the boost in sensitivity of the carbon resonances without sacrificing the quantitative aspects of the analysis. This is achieved controlling the polarization transfer mechanism and introducing a response factor to calculate precisely the sensitivity gain of the different carbon signals. Compared with the standard single pulse quantitative experiment, the QA-RINEPT method produces up to 4.7× signals enhancement per unit of time. An in-depth statistical analysis was conducted to confirm the reliability of the QA-RINEPT method. We show that there is excellent agreement between the new and old C-NMR methods for the quantitative determination of several important polyol properties such as the comonomer and initiator content as well as the ratio of primary and secondary hydroxyl groups.

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Section: Introductionmentioning

confidence: 99%

Quantitative adiabatic‐refocused INEPT (QA‐RINEPT) as a tool for fast and reliable characterization of polyols

Sabatino

Gao

Hou

2018

Magnetic Reson in Chemistry

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“…The method was used to differentiate HG in the investigation of PPG [145], oxyethylated PPG [89], their mixtures [219], polybutadiene [201], and the product of interaction of phenylglycidic ether with phenol [220]. The method was used to differentiate HG in the investigation of PPG [145], oxyethylated PPG [89], their mixtures [219], polybutadiene [201], and the product of interaction of phenylglycidic ether with phenol [220].…”

Section: Ho/\-mentioning

confidence: 99%

Determination of hydroxyl groups in polymers. Review

Boiko¹,

Grischenko²

1985

Acta Polymerica

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The analysis of hydroxyl groups in polymers is reviewed. Recent achievements of chemical, physico-chemical and physical methods for the determination of hydroxyl groups and their differentiation by reactivity have been examined. Particularly, infrared spectroscopy and nuclear magnetic resonance used for this determination are considered. Die Bestimmung yon Hydroxylgruppen in Polymeren. FortschrittsberichtIn dem Bericht werden neuere Entwicklungen chemischer, physikalisch-chemischer und physikalischer Methoden zur Bestimmung von Hydroxylgruppen und ihrer Differenzierung hinsichtlich der Reaktivitat dargestellt. Insbesondere wird die Anwendung der Infrarotspektroskopie und der magnetischen Kernresonanz behandelt. Onpeaenenue zur3powuJabnwx zpynn 8 nom.wepax. O630p 0 6 3 0~ IIOCBfiQeH aHaJIH8y rHAPOKCHnbHhIX rpynn B IIOJIEiMepaX. PaCCMOTpeHbI IlOCJIeAHlle AOCTEiXeHllfi XHMH9eCKHX, @H3HHO-XHMH9eCHHX Ei @H3H4eCKHX MeTOAOB KOJIEi9eCTBeHHOrO OIIpeAeneHElH I' HApOKCHJIbHbIX I'pyIIII H HX AH@-@epeHqEi~EiEinOpeaKqHOHHOltCnOCO6HOCTH. ~C O 6 O~B H l l M~H H~~~~j I~H O H H @~~K~~C H O~C I I~K T~O C MarHHTHOMY pe30HaHCy. Chemical methods of analysisChemical methods a r e simple a n d accessible, t h e y do not require special equipment a n d expensive instruments. At t h e same t i m e t h e y a r e rather time-consuming a n d require considerable amounts of t h e substance t o be analyzed. These methods can mainly give quantitative information. If t h e differentiation of HG is necessary, they become much more time-consuming. Recently t h e effective methods of chemical analysis have appeared which enable HG t o b e determined rapidly a n d exactly enough. Acylation of HG is most widely used, its application for polymers is detailed in t h e handbooks o n polymer analysis. The classical acylation procedure [27, 281 uses acetic (AA) or phthalic anhydride (PA) in pyridine solution, t h e latter being t h e solvent and catalyst of t h e reaction. T h e use of propionic [29], succinic [30--321, nitrobenzoic [33], osulfobenzoic [34], nitrophthalic [35]anhydrides for t h e same purpose is described. As a rule, primary a n d secondary HG a r e fully acylated within 1 t o 2 h a t 100 t o 115°C. Pyromellitic dianhydride (PMDA) [36-381 is more effective. It has as high activity as AA a n d does not interact with aldehyde groups a n d phenolic HG which is characteristic of PA. Dimethylsulfoxide (DMSO) is especially recommended as a solvent [37].T o acylate HG, more active acyl chlorides can b e used. BOIKO and GRISHCHENKO:Deterinination of liydroryl groups in polymers. Review Acta Polymcrica 36 (1985) Nr. 9

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“…(4,5) Typically, there is a separation of 0.3-0.4 ppm between the signals, the lower field signal, a singlet, belonging to the primary trifluoroacetyl esters, and the upper field signal, a doublet of spacing 0.05 ppm, belonging to the secondary esters. Manatt et.…”

Section: Introductionmentioning

confidence: 99%