<p>Accurate and reproducible determination of sodium chloride (NaCl) in processed meats is critical for product quality, safety, and regulatory compliance. This study compared the classical Mohr titration method with the Dicromat-II conductivity-based analyser for quantifying NaCl in dry-fermented sausages. Validation was performed across three matrices: aqueous NaCl standards, “added salt” pepperoni homogenates, and commercial pepperoni products. Both methods exhibited excellent linearity (<i>R</i>² &gt; 0.99) in standard and “added salt” matrices. However, the Dicromat-II demonstrated consistently higher precision (%RSD) and superior matrix tolerance, maintaining robust accuracy across all validation tiers. In commercial products, Mohr titration showed substantial variability, with weak correlation and poor agreement in most samples. The Dicromat-II, by contrast, offered reliable performance, reduced chemical handling, and strong repeatability, supporting its use in industrial meat analysis. This study represents the first direct validation-based comparison of these two methods in fermented meat matrices, highlighting the Dicromat-II as a practical and scalable alternative to traditional titration.</p>