The recoupled dipolar dephasing experiment combined with multiCP ¹³C ssNMR is implemented through the following continuous sequence: First, the multiCP (multi cross-polarization) sequence is applied using multiple short contact pulses (typically 0.1-0.5 ms duration) repeated 5-20 times with matched RF fields (γB₁(¹H) ≈ 50-100 kHz and γB₁(¹³C) ≈ 40-80 kHz) to efficiently transfer polarization from protons to carbons while maintaining broad bandwidth excitation. Following multiCP, high-power ¹H decoupling (SPINAL-64 or TPPM at 80-100 kHz) is immediately applied during the evolution period to initially average out ¹H-¹³C dipolar couplings.

The critical recoupled dipolar dephasing period (τ = 20-200 μs) is then introduced, during which the ¹H-¹³C dipolar interactions are deliberately recoupled using either rotor-synchronized π-pulses applied to ¹³C at half the rotor period (τ_R/2) for fast MAS conditions (>20 kHz) or continuous-wave ¹H irradiation at low power. This recoupling causes rapid dephasing of signals from protonated carbons (CH, CH₂ groups) due to their strong heteronuclear dipolar couplings, while non-protonated carbons (quaternary carbons, carbonyls) maintain coherence as their signals decay much more slowly.

After the dephasing period, high-power ¹H decoupling is resumed during signal acquisition to obtain high-resolution ¹³C spectra where the relative intensities reflect the degree of protonation and molecular mobility. The experiment must be carefully calibrated using model compounds (e.g., glycine) to optimize the dephasing time τ and validate the suppression of CHₓ signals versus retention of Cq signals. For quantitative analysis, a control experiment without dipolar recoupling should be acquired for comparison, and the signal decay can be fitted to extract dipolar coupling constants and mobility information.

Key experimental considerations include maintaining precise rotor synchronization for π-pulses at fast MAS rates, ensuring homogeneous RF fields, and implementing proper phase cycling to suppress artifacts. This technique is particularly valuable for characterizing heterogeneous materials like polymers, pharmaceuticals, and carbonaceous materials where distinguishing rigid versus mobile domains or protonated versus non-protonated sites is crucial for understanding molecular structure and dynamics.