This chapter transforms the conceptual knowledge of the previous chapter into rigorous practical and statistical technique. It opens with the three pillars of accurate volumetric work — purity of reagents, precision of glassware, and rigour of calculation — and gives a step-by-step protocol for preparing a primary standard solution. The chapter covers indicator selection theory with a full pH-range table, and prescribes the correct titration procedure: rough run (excluded from averages), followed by concordant accurate runs within plus or minus 0.10 cm3. The mean concordant titre (V1) is formally defined and calculated. Dixon's Q-test is introduced with critical values at 90% and 95% confidence for sample sizes 3–10, allowing statistical rejection of outliers. A comprehensive treatment of errors distinguishes systematic from random errors, explains the blank titration correction, and demonstrates error propagation. All common glassware tolerances are tabulated with worked percentage-error calculations. The mole-bridge stoichiometric pathway is illustrated with acid-base, non-1:1 redox, and back-titration worked examples. The chapter closes with a glossary of 20 key terms and a photocopiable student data template.