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Accurate characterization of contaminant mass in zones of low hydraulic conductivity (low k) is essential for site management because this difficult-to-treat mass can be a long-term secondary source. This study developed a protocol for the membrane interface probe (MIP) as a low-cost, rapid data-acquisition tool for qualitatively evaluating the location and relative distribution of mass in low-k zones. MIP operating parameters were varied systematically at high and low concentration locations at a contaminated site to evaluate the impact of the parameters on data quality relative to a detailed adjacent profile of soil concentrations. Evaluation of the relative location of maximum concentrations and the shape of the MIP vs. soil profiles led to a standard operating procedure (SOP) for the MIP to delineate contamination in low-k zones. This includes recommendations for: (1) preferred detector (ECD for low concentration zones, PID or ECD for higher concentration zones); (2) combining downlogged and uplogged data to reduce carryover; and (3) higher carrier gas flow rate in high concentration zones. Linear regression indicated scatter in all MIP-to-soil comparisons, including R(2) values using the SOP of 0.32 in the low concentration boring and 0.49 in the high concentration boring. In contrast, a control dataset with soil-to-soil correlations from borings 1-m apart exhibited an R(2) of ≥ 0.88, highlighting the uncertainty in predicting soil concentrations using MIP data. This study demonstrates that the MIP provides lower-precision contaminant distribution and heterogeneity data compared to more intensive high-resolution characterization methods. This is consistent with its use as a complementary screening tool.