Abandoned mines present considerable environmental risks through the release of toxic metals, particularly into adjacent water bodies. The implementation of reliable geotechnical cut-off walls containing bentonite stands as a crucial strategy in mitigating environmental groundwater contamination. This study evaluates the viability of employing the methylene blue titration method to quantify bentonite content in till samples, with the objective of verifying the assumed bentonite content (3.5%) and exploring the impact of sample preparation on bentonite content determined through titrations. Bentonite, known for its swelling properties and high cation exchange capacity, was introduced into till samples both in laboratory settings and on-site. The methylene blue titration method was utilized to measure bentonite content in these samples. Laboratory results indicated significant variations in bentonite content depending on the sample preparation method, with methods employing soil homogenization proving more effective in quantifying bentonite accurately. The study's findings support the hypothesis that the methylene blue method can reliably quantify bentonite in till soil samples with the correct preparation in a laboratory environment. On-site analysis exhibited larger variations and deviations in bentonite content quantifications compared to laboratory-based incorporations. Additionally, on-site incorporated samples demonstrated a statistically significant difference in bentonite content compared to laboratory-incorporated samples, highlighting the method's sensitivity and need for future research. This research contributes valuable insights into leveraging methylene blue titration for quantifying bentonite in till soils, crucial for establishing geotechnical barriers to control toxic metal output from mines.