Cross-polarization magic-angle spinning 2026-11-05
Cross-polarization magic-angle spinning, abbreviated CPMAS, combines two operations in solid-state nuclear magnetic resonance. Cross-polarization (nuclear magnetic resonance) transfers nuclear spin polarization from a more strongly detected spin population, commonly protons, to a less sensitive one such as carbon-13. Magic angle spinning rotates the sample to average appropriate orientation-dependent interactions. Signal enhancement and spectral narrowing address different experimental obstacles.
The angle is fixed by a geometrical condition:This nulls the relevant second-rank angular factor under the averaging assumptions; it does not remove every interaction or every source of linewidth. Chemical shift anisotropy and sample motion must still be interpreted within the actual experiment.
In their 1976 paper, Jacob Schaefer and Edward O. Stejskal compared carbon-13 spectra of solids obtained with cross-polarization (nuclear magnetic resonance), with and without magic angle spinning, against solution spectra. The polysulfone example showed how the combined method could reveal much more resolved structural detail in a solid.[ref]
Carbon-13 nuclear magnetic resonance of polymers spinning at the magic angle by Jacob Schaefer and E. O. Stejskal. Page1031 and Figure1: CP/MAS, static CP and solution comparisons
For an original comparison, consider two carbon sites with equal populations but different efficiencies of polarization transfer. Their measured peak areas can differ even when their populations are equal. Changing contact time or relaxation conditions can change that weighting. NMR signal integration in a CPMAS spectrum therefore requires a justified acquisition model before peak areas are treated as direct composition measurements.
Jacob Schaefer 2026-11-05
Jacob Schaefer was a physical chemistry researcher who developed methods for studying complex solid materials using solid-state nuclear magnetic resonance. After his 1964 doctorate he worked at Monsanto, then joined Washington University in 1986. His contributions included cross-polarization magic-angle spinning with Edward O. Stejskal and rotational-echo double resonance with Terry Gullion.[ref]
Jacob Schaefer obituary by Washington University in St. Louis. Education, appointments and joint CPMAS/REDOR contributions
Jacob Schaefer, in the portrait accompanying Washington University's institutional memorial
. The materials in the 1976 cross-polarization magic-angle spinning demonstration made the method's reach tangible. They included polysulfone, ebony wood and a cylinder cut from an ivory billiard ball. Schaefer's father and grandfather were billiards champions; a familiar object became a specimen for measuring carbon-13 responses in a complex solid. Combining polarization transfer with magic angle spinning made weak and broadened solid-state responses much more accessible.[ref]
Jacob Schaefer, 1938-2022 by Lynette Cegelski and Terry Gullion. Tribute: family connection,1976 sample choices and high-sensitivity/high-resolution CPMAS demonstration
REDOR addresses another measurement problem. Magic angle spinning averages interactions that broaden spectra, but some of those interactions carry structural information. Appropriately timed radio frequency pulses restore sensitivity to NMR dipolar coupling between different nuclear species. Comparing a reference echo with a deliberately dephased echo then probes that coupling, with structural interpretation supplied by a suitable spin model.[ref]
Schaefer reproduced a laboratory record from 29 May 1987 in which Gullion measured carbon-13 spectra of nitrogen-15-labelled alanine. Carbon remained at natural isotopic abundance. The record compares full and dephased echoes at a carbon frequency of , using magic angle spinning at and 10 rotor periods of dipolar evolution. The corresponding duration isThe reproduced record does not give sample mass or number of accumulated scans. Later use of XY8 NMR phase cycling suppressed pulse-train amplitude and phase errors, enabling measurements of weaker couplings over longer pulse trains.[ref]
Development of REDOR rotational-echo double-resonance NMR by Jacob Schaefer (2011). p.422, Figure1 caption: sample, frequencies and missing acquisition quantities; following paragraphs: XY8 and weak-coupling measurements
Polyethersulfone 2026-11-05
Polyethersulfone, commonly abbreviated PESU, is an aromatic polymer with ether and sulfone linkages in its polymer backbone. It belongs to the sulfone-containing engineering thermoplastics. The complete repeat unit, rather than the presence of one sulfur-containing group, distinguishes its chemical identity from related polysulfone and polyphenylsulfone materials.[ref]
Ultrason E, S, P product information by BASF. Product range: PESU, PSU and PPSU families; corresponding family descriptions in brochure printed p.10.
BASF identifies its PESU family as an amorphous thermoplastic. These terms answer different questions: amorphous concerns the absence of long-range crystalline order, while thermoplastic concerns the material's ability to soften for reshaping. A glass transition is therefore a change in physical response, rather than necessarily a chemical cleavage of the polymer backbone.[ref]
Ultrason E, S, P product information by BASF. Product range: amorphous thermoplastic classification.
For an illuminating comparison, imagine testing the same polymer chemistry with two different chain-length distributions. The local ether and sulfone connections can remain the same while flow behavior and mechanical response differ. A useful measurement report must identify both the chemical family and the sample being tested; naming PESU alone does not specify every processing or mechanical property.
Polyphenylsulfone 2026-11-05
Polyphenylsulfone, commonly abbreviated PPSU, is an aromatic sulfone-containing thermoplastic. Its backbone contains aromatic, ether and sulfone structural features. Manufacturers identify PPSU separately from polysulfone and polyethersulfone; similar family names do not make their full repeat units interchangeable.[ref]
Ultrason E, S, P product information by BASF. Product range and brochure printed p.10: separate PPSU, PSU and PESU families and amorphous thermoplastic classification.
The structural label is useful when interpreting material tests, but it is not itself a measured strength or toughness. Two specimens can have the same initial slope on a stress-strain curve yet fail at different strains. The first observation concerns stiffness; the later part of the curve also affects the energy absorbed before failure. Thus comparing only the initial response would conceal another important mechanical difference.
An original identification example is to record three separate descriptors: the PPSU chemical family, a particular material grade and a measured response under stated conditions. The first establishes a broad chemical identity, the second narrows the formulation, and the third reports behavior. This separation prevents a property measured for one sample from being silently promoted into a universal property of every polyphenylsulfone material.
