The magnitudes of vectors \( \mathbf{a} \) and \( \mathbf{b} \) are calculated first. The formula for the magnitude of a vector \( \mathbf{v} = v_x \hat{i} + v_y \hat{j} + v_z \hat{k} \) is \(|\mathbf{v}| = \sqrt{v_x^2 + v_y^2 + v_z^2}\).
For vector \( \mathbf{a} = 3 \hat{i} + 2 \hat{j} - \hat{k} \), its magnitude is \(|\mathbf{a}| = \sqrt{3^2 + 2^2 + (-1)^2} = \sqrt{9 + 4 + 1} = \sqrt{14}\).
For vector \( \mathbf{b} = \hat{i} - \hat{j} + \hat{k} \), its magnitude is \(|\mathbf{b}| = \sqrt{1^2 + (-1)^2 + 1^2} = \sqrt{1 + 1 + 1} = \sqrt{3}\).
Comparing the magnitudes, \(|\mathbf{a}| = \sqrt{14}\) and \(|\mathbf{b}| = \sqrt{3}\). Since \( \sqrt{14}>\sqrt{3} \), it follows that \( |\mathbf{a}|>|\mathbf{b}| \).
Consequently, the correct option is (C).