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Titremetric analysis Dr. Mohammad Khanfar
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Titremetric analysis Dr. Mohammad Khanfar. Concept of Titremetric analysis In general, we utilize certain property of a substance to be analyzed in order.

Dec 22, 2015

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Page 1: Titremetric analysis Dr. Mohammad Khanfar. Concept of Titremetric analysis In general, we utilize certain property of a substance to be analyzed in order.

Titremetric analysis

Dr. Mohammad Khanfar

Page 2: Titremetric analysis Dr. Mohammad Khanfar. Concept of Titremetric analysis In general, we utilize certain property of a substance to be analyzed in order.

Concept of Titremetric analysis

• In general, we utilize certain property of a substance to be analyzed in order to be able to determine its amount or concentration in solution (quantitative) or to identify substance (qualitative). Titration is a procedure used in analytical chemistry to determine the amount or concentration of a substance. In a titration procedure, one reactant (titrant) is added to another (titrand or called analyte, whose concentration or amount to be determined) slowly from a special graduated glass tube called burette.

Page 3: Titremetric analysis Dr. Mohammad Khanfar. Concept of Titremetric analysis In general, we utilize certain property of a substance to be analyzed in order.

Concept of Titremetric analysis

• As the titrant is added to the titrand, the chemical reaction proceeds until no more of the titrand (analyte) is left, this point called equivalence point.

• We cannot determine the equivalence point of a titration experimentally.

• Instead, we can only estimate its position by observing some physical change associated with the condition of equivalence. This change is called the end point for the titration.

• We can determine this end point using other substance called indicator.

• Typical indicator changes include the appearance or disappearance of a color, a change in color, or the appearance or disappearance of turbidity.

Page 4: Titremetric analysis Dr. Mohammad Khanfar. Concept of Titremetric analysis In general, we utilize certain property of a substance to be analyzed in order.

Concept of Titremetric analysis

• The amount of the analyte based on the facts that we know:• 1) the concentration and the volume of titrant consumed in the reaction• 2) Volume of the analyte. • Therefore, if the reaction between the titrant and titrand occurs in 1:1

ratio, then the number of moles of titrant is equal the number of moles of analyte.

Page 5: Titremetric analysis Dr. Mohammad Khanfar. Concept of Titremetric analysis In general, we utilize certain property of a substance to be analyzed in order.

Concept of Titremetric analysis

• Example: The organic matter in a 3.776 g sample of a mercuric ointment is decomposed with HNO3, After dilution, the Hg2+ is titrated with 21.30 ml of a 0.1144 M solution of NH4SCN, Calculate the percent Hg (200.59 g/mol) in the ointment.

Hg2+ + 2SCN- Hg(SCN)2

Page 6: Titremetric analysis Dr. Mohammad Khanfar. Concept of Titremetric analysis In general, we utilize certain property of a substance to be analyzed in order.

Concept of Titremetric analysis

• In order to be suitable for titration, the reaction could be of an type as long as the following conditions are met:

1) The reaction must be complete i.e. any amount of the titrant should be able to convert equivalent amount (on molar bases) of the titrand to product.

2) the reaction must be spontaneous (fast). Sometime a catalyst may be used to increase the speed of the reaction.

3) There must be some means of detecting the end points.

• The most common types of chemical reactions that satisfy the above conditions are: 1) acid-base reactions 2) oxidations reduction reactions 3) complexation reactions 4) precipitation reactions

Page 7: Titremetric analysis Dr. Mohammad Khanfar. Concept of Titremetric analysis In general, we utilize certain property of a substance to be analyzed in order.
Page 8: Titremetric analysis Dr. Mohammad Khanfar. Concept of Titremetric analysis In general, we utilize certain property of a substance to be analyzed in order.

Concept of Titremetric analysis

• How do we know the concentration of the titrant?• In order to prepare a solution of with known concentration

(this is known as Standard solution) we need to take proper weight of the material (contains the required number of moles) and transfer it carefully to a proper volumetric flask, the volume is completed to the mark

Page 9: Titremetric analysis Dr. Mohammad Khanfar. Concept of Titremetric analysis In general, we utilize certain property of a substance to be analyzed in order.

Concept of Titremetric analysis

• The ideal standard solution for a titrimetric method will 1. Be sufficiently stable so that it is necessary to determine its

concentration only once2. React rapidly with the analyte so that the time required

between additions of reagent is minimized3. React more or less completely with the analyte so that

satisfactory end points are realized; 4. Undergo a selective reaction with the analyte that can be

described by a balanced equation

Page 10: Titremetric analysis Dr. Mohammad Khanfar. Concept of Titremetric analysis In general, we utilize certain property of a substance to be analyzed in order.

Concept of Titremetric analysis

• Primary standard are stable chemical compounds that are available in high purity and which can be used to standardize the standard solutions used in titrations.

• Titrant such as NaOH and HCl cannot be considered as primary standards since their purity is quite variable.

Page 11: Titremetric analysis Dr. Mohammad Khanfar. Concept of Titremetric analysis In general, we utilize certain property of a substance to be analyzed in order.

Concept of Titremetric analysis

• Important requirements for a primary standard are the following:

1. High purity. Established methods for confirming purity should be available.

2. Atmospheric stability. 3. Absence of hydrate water so that the composition of the solid

does not change with variations in humidity. 4. Modest cost. 5. Reasonable solubility in the titration medium. 6. Reasonably large molar mass so that the relative error

associated with weighing the standard is minimized.

Page 12: Titremetric analysis Dr. Mohammad Khanfar. Concept of Titremetric analysis In general, we utilize certain property of a substance to be analyzed in order.

Concept of Titremetric analysis

• Advantages of titremetric analysis• Capable of a higher degree of precision and accuracy• The method are generally robust• Analyses can be automated• Cheap to perform and do not require specialized apparatus• Not dependent on the calibration of an instrument

Page 13: Titremetric analysis Dr. Mohammad Khanfar. Concept of Titremetric analysis In general, we utilize certain property of a substance to be analyzed in order.

Concept of Titremetric analysis

• Limitations• Non-selective• Time consuming if not automated• Require large amount of sample and reagents• Reactions of standard solutions with the analyte should be

rapid and complete

Page 14: Titremetric analysis Dr. Mohammad Khanfar. Concept of Titremetric analysis In general, we utilize certain property of a substance to be analyzed in order.

Concept of Titremetric analysis

http://www.youtube.com/watch?v=8UiuE7Xx5l8&feature=related

Page 15: Titremetric analysis Dr. Mohammad Khanfar. Concept of Titremetric analysis In general, we utilize certain property of a substance to be analyzed in order.

Concept of Titremetric analysis

• Titration curve: are plots of a concentration-related variable as a function of reagent volume. In acid-base titration, it’s a plot between the pH of solution being titrated and the volume of the added titrant.

Potential end point

Page 16: Titremetric analysis Dr. Mohammad Khanfar. Concept of Titremetric analysis In general, we utilize certain property of a substance to be analyzed in order.

Titration curve for the titration of 50.00 mL of 0.1 000 M AgNO3 with 0.10 M KSCN.

Page 17: Titremetric analysis Dr. Mohammad Khanfar. Concept of Titremetric analysis In general, we utilize certain property of a substance to be analyzed in order.

Concept of Titremetric analysis

• Titration curve • End-point detection is based on large change in relative

concentration of the analyte (or the reagent) that occurs at and near the equivalence point for every type of titration.

• Titration curves for reactions involving complex formation, precipitation, and oxidation/reduction all exhibit the same sharp increase or decrease in p-function in the equivalence-point region.

Page 18: Titremetric analysis Dr. Mohammad Khanfar. Concept of Titremetric analysis In general, we utilize certain property of a substance to be analyzed in order.

Concept of Titremetric analysis

• Back titration• Addition of excess of standard solution (titrant) to a weighed

amount (or volume) of sample, and determination of excess (un-reacted) titrant using secondary titrant.

• In general this method is used for:• 1) Volatile substances, e.g. ammonia, some would be lost during

titration • 2) Insoluble substances, e.g. Calcium carbonate, which requires

excess volumetric solution• 3) Substances for which a quantitative reaction proceeds rapidly

only in presence of excess of the reagent, e.g. lactic acid• 4) Substances which require heating, e.g. formaldehyde solution

Page 19: Titremetric analysis Dr. Mohammad Khanfar. Concept of Titremetric analysis In general, we utilize certain property of a substance to be analyzed in order.

Concept of Titremetric analysis

• Example of back titration• The amount of phosphate in a sample can be determined by adding a

measured excess of standard silver nitrate to a solution of the sample, which leads to the formation of insoluble silver phosphate:

• The excess silver nitrate is then back-titrated with a standard solution of potassium thiocyanate:

• Here. the amount of silver nitrate is chemically equivalent to the amount of phosphate ion plus the amount of thiocyanate used for the back titration.