A Trifluoroacetylation-Fluorine-19 Nuclear Magnetic Resonance Technique for Characterization of Hydroxyl Groups in Poly(Propylene Oxides).

Manatt, Stanley L.; Lawson, D. D.; Ingham, J. D.; Rapp, Neville S.; Hardy, Judith P.

doi:10.1021/ac60240a028

Cited by 26 publications

(7 citation statements)

References 13 publications

(7 reference statements)

Supporting

Mentioning

Contrasting

Order By: Relevance

“…Recently, Manatt has reported the characterization of alcohols as their trifluoroacetates (TFA) by the fluorine magnetic resonance (2,3). This method has certain obvious advantages; first, the chemical shifts of fluorine are in general larger than those of protons by about one order of magnitude.…”

Section: Discussionmentioning

confidence: 99%

Spectrophotometric determination of cysteine

Bydalek¹,

Poldoski²

1968

Anal. Chem.

View full text Add to dashboard Cite

show abstract

Section: Discussionmentioning

confidence: 99%

Spectrophotometric determination of cysteine

Bydalek¹,

Poldoski²

1968

Anal. Chem.

View full text Add to dashboard Cite

show abstract

“…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

View full text Add to dashboard Cite

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.

show abstract

“…Later, other studies extended the trifluoroacetic anhydride approach to other organic functional groups including phenols (3), steroids (4), and hydroxy groups in polypropylene oxides) (5).…”

mentioning

confidence: 99%

Trifluoroacetyl chloride for characterization of organic functional groups by fluorine-19 nuclear magnetic resonance spectrometry

Sleevi¹,

Glass²,

Dorn³

1979

Anal. Chem.

View full text Add to dashboard Cite

The potential utility of trifluoroacetyl chloride as an analytical 19F NMR reagent to characterize alcohols, phenols, thiols, and primary and secondary amines is reported. The 19F chemical shift and yield data for trifluoroacetyl derivatives of approximately 50 model compounds are presented. The importance of an added organic base (2,6-lutidine) in derivative preparation for phenols and primary and secondary amines is discussed.During the past decade several NMR approaches have been suggested to characterize organic functionality (e.g., phenols, alcohols, carboxylic acids, etc.) present in organic compounds and/or mixtures. Nearly all of these approaches rely on the chemical shift parameter to distinguish molecular environment differences for an NMR probe nuclide either present in the functional moiety of interest or by tagging via an appropriate derivative.

show abstract

A Trifluoroacetylation-Fluorine-19 Nuclear Magnetic Resonance Technique for Characterization of Hydroxyl Groups in Poly(Propylene Oxides).

Cited by 26 publications

References 13 publications

Spectrophotometric determination of cysteine

Spectrophotometric determination of cysteine

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

Trifluoroacetyl chloride for characterization of organic functional groups by fluorine-19 nuclear magnetic resonance spectrometry

Contact Info

Product

Resources

About