The measurement of lignin content in ruminant diet and faecal samples is important for digestibility studies, but it is typically time consuming and costly. The work reported involved correlation of traditional wet chemistry data with that from three rapid instrumental techniques, Fourier Transform Infrared spectroscopy (FTIR), Conventional Thermogravimteric Analysis (TGA) and High Resolution TGA (MaxRes TGA) to predict lignin content of diets and faeces from digestibility trials. Calibration and performance data indicated that the FTIR model was acceptable for screening whilst the Conventional and MaxRes TGA predictions were of high accuracy for quantitative analysis. Cross validation and model performance data revealed that MaxRes TGA provided the best performing predictive model. This work showed that MaxRes TGA can accurately predict lignin content in ruminant diet and faecal samples with distinct advantages over traditional wet chemistry, namely the requirement for small sample size, ease of sample preparation, speed of analysis and high sample throughput at considerably lower cost.