The NMR tube was connected to the hyperpolarization system, repressurized under 4 bars of H2, and inserted into an NMR spectrometer. Hyperpolarization was facilitated by bubbling pH2 through the sample under pulse program control. 1D and 2D pH2 nh-PHIP spectra were recorded at 25 °C sample temperature on an 800 MHz Bruker Avance III spectrometer with or without cryoprobe. Spectral widths were 8012 and 2000 Hz in f2 and f1 dimensions, respectively. Data sets consisted of 8192 (complex) × 512 (real) points. pH2 was bubbled through the sample for 2.5 s between scans. A 90° shifted square sine window function was applied in both dimensions and f1 dimension was zero-filled to 1024 points before Fourier transformation.