To prepare a 100 mg/ml solution of glacial acetic acid in methanol, the process begins with weighing 100 mg of liquid acetic acid using a scale and then diluting it to 1 ml in a volumetric flask. For larger volumes, such as 10 ml, the amount of acetic acid needed can be multiplied accordingly. If the desired concentration is too small to weigh accurately, the volume of acetic acid can be calculated using its density. This involves determining the volume needed for the desired final solution based on the density of glacial acetic acid, which is 1.05 g/cm^3. It is recommended to prepare larger volumes to avoid precision issues in weighing small amounts. Additionally, for accuracy, volumetric measurements should be approached with caution since density can vary with temperature, which may affect the concentration of the solution.