Volumetric Analysis

Volumetric Analysis
Volumetric analysis is one of the most useful analytical techniques. It is fairly rapid and very good accuracy can be obtained.

Volumetric Analysis
Titration also known as titrimetry. a common laboratory method of quantitative chemical analysis that is used to determine the unknown concentration of an identified analyte. a lab procedure where a measured volume of one solution (burette) is added to a known volume (flask) of another solution until the reaction is complete.

Volumetric Analysis
Requirements of Titration: 1. The reaction should be stoichiometric. 2. The reaction should be rapid. 3. The reaction should be complete. 4. There should be no side reactions and the reaction should be specific. 5. There should be a marked change in some property of the solution when the reaction is complete.

Volumetric Analysis
Standard solution a solution of known concentration. are used to determine the concentrations of other substances, such as solutions in titrations. Titrant the solution which is added. Also known as titrator

Volumetric Analysis
Use of standard solution: A solution of acid can be standardized by titrating it against a solution of alkali of known concentration. Once this has been calculated, it can in turn be used as a standard solution to find the concentration of a solution of alkali.

Volumetric Analysis
Use of standard solution: Standard solutions are also commonly used to determine the concentration of an analyte species. *By comparing the absorbance of the sample solution at a
specific wavelength to a series of standard solutions at differing known concentrations of the analyte species, the concentration of the sample solution can be found via Beer's Law.

Volumetric Analysis
Standard solutions: A standard solution is prepared by dissolving an accurately weighed quantity of a highly pure material (primary standard) and diluting to an accurately known volume in a volumetric flask.

Volumetric Analysis
Standard solutions: If the material is not sufficiently pure, a solution is prepared to give approximately the desired concentration, and this is standardized by titrating a weighed quantity of a primary standard

Volumetric Analysis
Standard solutions: For example, sodium hydroxide is not sufficiently pure to prepare a standard solution directly, it is standardized by titrating a primary standard acid, such as potassium acid phthalate (KHP). Potassium acid phthalate is a solid that can be weighed accurately.

Volumetric Analysis
Requirements of a primary standard: 1. It should be 100.00% pure. (0.01 0.02% impurity is tolerable if accurately known). 2. It should be stable to drying temperatures and it should be stable indefinitely at room temperature. (The primary standard is always dried before weighing). 3. It should be readily available.

Volumetric Analysis
Requirements of a primary standard: 4. If it is to be used in a titration, it should possess the properties required for a titration. 5. It must dissolve easily in water. 6. It should have a fairly high relative molecular weight.

Non standard solutions

Sodium hydroxide absorbs carbon dioxide from atmosphere HCl can produce chlorine gas in reactions and liberate hydrogen when exposed to air Nitric acid can act as an oxidising agent interfering with reactions Sulphuric acid absorbs water form the air

Volumetric Analysis
Keeping analytical reagents pure Pour directly from the bottle to the flask or beaker. Never return reagents to the original container. Replace caps immediately. Store reagents in cool, dry, dark place.

Volumetric Analysis
Classification of Volumetric Methods
By Reaction: Acid-Base Precipitation Complexometric Reduction-Oxidation By Indicator: Spectrophotometric Electrochemical pH

Volumetric Analysis
Classification of Volumetric Methods: 1. Acid-Base many compounds can be titrated with a standard solution of a strong base or a strong acid. the end points of these titrations are easy to detect (either by means of an indicator or change in pH). depend on the neutralization between an acid and a base when mixed in solution.

Volumetric Analysis
Classification of Volumetric Methods: 2. Precipitation the titrant forms an insoluble product with the analyte. indicators can be used to detect the end point, or the potential of the solution can be monitored electrically.

Volumetric Analysis
Classification of Volumetric Methods: 3. Complexometric the titrant is a complexing agent and forms a water-soluble complex with the analyte - a metal ion. the titrant is often a chelating agent*.
*Chelating agent is a type of complexing agent that contains two or more groups capable of complexing with a metal ion. Ethylenediaminetetraecetic acid (EDTA) has six such groups.

Volumetric Analysis
Classification of Volumetric Methods: 4. Reduction-oxidation these redox titrations involve the titration of an oxidizing agent with a reducing agent, or vice versa. (an oxidizing agent gains electrons and a reducing agent loses electrons in a reaction between them)

Volumetric Analysis
Apparatus used: Burette Volumetric flask Beaker Pipette Funnel Indicator White tile

Volumetric Analysis
FAQs in Titration:
Why is a conical flask preferred over a beaker when performing titration? To allow easy mixing of the contents by swirling.

Volumetric Analysis
FAQs in Titration:
Why is the funnel removed from the burette after adding the titrant? So that drops of the solution will not fall into the buretter

Volumetric Analysis
FAQs in Titration:
In using the burette, why is it important to rinse it with a little of the solution it is going to contain? To remove any residual water so as to avoid dilution of the solution when it is poured into the burette.

Volumetric Analysis
FAQs in Titration:
In using the burette, why is it important to clamp it vertically? To enable the liquid level to be read correctly.

Volumetric Analysis
FAQs in Titration:
In using the burette, why is it important to have the part below the tap full? To ensure that the actual volume of liquid delivered into the flask is read accurately.

Volumetric Analysis
Titration calculation:

Ca = concentration of analyte Ct = concentration of the titrant Vt = volume of the titrant used Va = volume of the analyte used M = mole ratio of the analyte and reactant

Volumetric Analysis Titration calculation: For a general reaction: aA + tT P where: A = analyte T = titrant P = all product molesA = molesT x a/t (molesA/molesT) molesA = CT x VT x a/t (molesA/molesT)

Volumetric Analysis
For the concentration of a solution of T standardized by titrating a known number of moles of primary standard A can be calculated from: CT x VT = molesA x t/a (molesT/molesA) CT x VT = wtA/f.w.A x t/a (molesT/molesA)

Volumetric Analysis
Exercise: How many milliliters of 0.25M solution of HSO will react with 10 ml of a 0.25M solution of NaOH?