substance, called a titrant with the analyte. The C. Preparation of Standard CaCO3 volume of the titrant is measured with a glassware known as buret. - Weigh 0.10-0.15g (0.1mg) CaCO3 in a 250mL beaker The amount of the titrant required to - Add concentrated HCl drop by drop until react with the analyte is then used to all the CaCO3 dissolves. determine the amount of the analyte - Cover the beaker with a watch glass present. and evaporate the HCl - implies that the reaction stoichiometry - Quantitatively transfer the residue to of the titrant and analyte & a 500mL volumetric flask and dilute to concentration of the titrant must be volume known. D. Standardization of EDTA (refer to p. 25 of manual for equations)
Standardization - Place 10mL of the Standard CaCO3 in a
(compared to a standard) convenient titration vessel (determining the exact conc. of the titrant) - Add 5mL of Ammonia buffer - to know the volume needed to - Add 5 drops of the EBT indicator completely react with 0.2xxx of KHP when Wine red coloration the reaction ratio for NaOH & KHP is 1:1 - titrate until light blue
Compleximetric Determination of Water E. Determination of Water Hardness
Hardness - direct titration because the titrant reacts - Use DILUTED EDTA TITRANT for the directly with the analyte titration - Follow procedure D but instead of using Modified Winkler Method for Dissolved Oxygen 10mL of the standard CaCO3 use 10mL of - indirect titration because a reagent is the sample added to the analyte - reaction results in a product that is proportional to the amount of the analyte. Determination of the pKa of a Weak Acid Determination of the pKa of a Weak Acid - chemical property of a weak acid is determined by titration When a solution of a weak acid is titrated completely with a strong base, the salt that is 3 Distinct Stages (Pre, Sta, Tit or PST) formed is the conjugate base of the weak acid. 1. Preparation of the Titrant If the reaction is only 50% complete, then we have a 2. Standardization of the Titrant situation wherein only half of the weak acid has been 3. Titration of the sample titrated while the other half remains untitrated. In other words, the concentration of the weak acid is Usual data in volumetric analysis include initial and the same as the concentration of its conjugate final volume of the buret, weight of the sample base. or standard. At this point, pH = pKA Compleximetric Determination of Water Hardness A. Preparation of the NAOH Titrant Water hardness - concentration of CaCO3 and MgCO3 in - Boil 250mL distilled water to remove water expressed as ppm CaCO3 the dissolved carbon dioxide - Add 1g of NaOH - cool and store A. Preparation of 5x10^-3 M EDTA Titrant
- Dissolve 0.47g of EDTA in 250mL B. Preparation of the pH meter
distilled water - Add pinch of MgCl2 * 6H20 (ca. 0.05 g) - Be sure to rinse the electrode tip with distilled water before and after soaking the B. Preparation of Diluted EDTA Titrant electrode in a solution
- Take a 10.00mL aliquot of the prepared C. Standardization of the NaOH Titrant
titrant - Place in a 100mL volumetric flask and D. Preparation of the sample dilute to volume E. Determination of pKa - Volume of NaoH (x-axis) - Adding NaOH in 0.5mL increments until - pH (y-axis) there is a sudden rise in pH - Determine the volume of NaOH at the - At this point, add the increments of 0.1mL inflection point on the curve until the pH shows a gradual rise in pH - Divide the volume by 2 - Determine the pH coordinate of the F. Treatment of Results quotient