Abstract: Resonance difference between ¹³C and ²⁷Al is 0.738 MHz on AC-80 nuclear magnetic resonance spectrometer, Since wide frequence band is required for the determination of ¹³C nuclear magnetic resonance spectrum, the determination of ²⁷Al nuclear magnetic resonance is possible with 10mm ¹³C probe or 5mm¹³C-¹H double prode if proper parameters are used.When Al³⁺=0.1mol/L, the sensitivity is 42 and the line width is 4.8Hz if 10mm ¹³C probe is used, the sensitivity is 24.8 and the line width is 3.2Hz if 5mm ¹³C-¹H double probe is used.