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Pharmaceutical Analytical Chemistry / PHC 213

Pharmaceutical Analytical Chemistry / PHC 213. Course syllabus:. Acid _ base titration ( 2 labs ) Precipitimetric titration ( 1 lab) Complexmetric titration (1 lab) Redox(oxidation-reduction) titration ( 2 lab ). Analytical Chemistry.

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Pharmaceutical Analytical Chemistry / PHC 213

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  1. Pharmaceutical Analytical Chemistry / PHC 213

  2. Course syllabus: • Acid _ base titration ( 2 labs ) • Precipitimetrictitration ( 1 lab) • Complexmetrictitration (1 lab) • Redox(oxidation-reduction) titration ( 2 lab )

  3. Analytical Chemistry is the study of the separation, identification, and quantification of the chemical components of natural and artificial materials

  4. Analytical chemistry answer two important questions • What is it ?? (Qualitative analysis) gives an indication of the identity of the chemical species in the sample • How much is it ?? (quantitative analysis) determines the amount (concentration) of one or more of the components in the sample

  5. Classification of Analytical Methods : • Gravimetric method • Volumetric method • Instrumental methods

  6. Gravimetric method : Gravimetric methods of analysis are based on the measurement of mass.

  7. :(Volumetric method (Titration involves the addition of a reactant to a solution being analyzed until some equivalence point is reached

  8. Types of Titration: • Acid _ base titration • Precipitimetric titration • Complexmetric titration • Redox(oxidation-reduction) titration

  9. Instrumental methods : • Spectrophotometry

  10. Chromatography

  11. Application of Analytical Chemistry : Analytical chemistry play an important role in nearly all aspect of chemistry • Medicine • Industry • Environmental • Food and Agriculture • Quality control

  12. Application of Analytical Chemistry : • In medicine, analytical chemistry is the basis for clinical laboratory tests which help the physicians diagnose disease • In industry, analytical chemistry provides the means of testing the raw materials for assuring the quality of finished products whose chemical composition is critical (eg. Drugs )

  13. The nutritional value of food determined by chemical analysis for major component such as protein and carbohydrate and trace components such as vitamins and minirals

  14. Definition of some terms : • Sample: is a material that we wish to analyze • Analyte: is the substance or element in the sample whose presence or concentration we wish to determine • titrant: is a solution of known concentration which is added (titrated) to another solution to determine the concentration of second chemical species

  15. Titration: • is a process which is performed by slow addition of standard solution "titrant" from a burette to a solution of the analyte until the reaction between the two is complete.

  16. Standard Solution: - is a solution of known concentration - prepared by dissolving a known amount of the substance (primary standard substance)in a known volume of liquid - They provide a reference to determine unknown concentrations -Two types,, primary and secondary standard solution

  17. Standard solution Secondary standard Primary standard 1-Must be easily obtained in very high grade of purity and of known composition. 2-Very stable, and resists reactions with air ( non-hygroscopic ) 3- It is recommended to have high equivalent weight to minimize weighing error. 4- It must react with other substances in quantitative way according to balanced chemical equations (stoichiometry) 1-The concentration of which can’t be directly calculated from the weight of the solute and volume of the solution. 2- The exact concentration is determined by: - Titration against a primary standard solution Dr. Hadir Shalaby

  18. Standard solution Examples: Primary standard Secondary standard potassium acid phthalate, oxalic acid, benzoic acid, sulphamic acid. Borax, sodium carbonate. Potassium dichromate, potassium bromate and potassium iodate. Sodium oxalate, arsenious oxide, and potassium ferrocyanide. Hydrochloric acid, sulphuric acid. Sodium hydroxide, ammonia Potassium permanganate Acids Bases Oxidizing agents Reducing agents Dr. Hadir Shalaby

  19. Equivalence point: End point: The point in a titration when the amount of added standard reagent is exactly equal to ( is chemically equivalentto) the amount of the analyte. The point in a titration when a physical change occurs that is associated with the condition of chemical equivalence. Volume difference between the equivalence point and the end point should be small . This difference in volume is the titration error

  20. Detection of the end point • Indicator : a substance that indicate the presence, absence, or concentration of another substance ,,often used in a titration to indicate the point at which the reaction is complete by means of a characteristic change, especially in color such as: litmus paper in acid media in base media

  21. Methods of expressing concentration of standard solutions I-Molarity Molar solution: It is a solution of the substance containing one mole (gram molecular weight) of the substance perone literof solution. Molarity (M) : It is the number of moles (gram molecular weight )of solute per one liter of solution. Dr. HadirShalaby

  22. M=Molarity V=volume in liter Some useful algebraic relationships: M = no. moles solute V( L) No. of moles = M x V ( L ) No. of moles = wt.solute, g fwt Fwt= formula weight or molecular weight ( g) Dr. Hadir Shalaby

  23. Examples: Example 1: Calculate the molarity of 17g Na2CO3 in 500ml of solution (fwt=106) Example 2: ( HOME WORK) Calculate the weight in grams of Na2CO3 required to prepare 250ml of 0.15M solution. (fwt=106) Convert 500 ml to liter by ÷1000 = 0.5 L Dr. Hadir Shalaby

  24. II. Normal solution: II-Normality It is the solution that contains one gram equivalent weight of solute per liter of solution. Normality (N) : It is the number of equivalents (gram equivalent weight) per literof solution. If the equivalent weight = formula weight so, N = M Dr. Hadir Shalaby

  25. Normality (N) = Number of equivelant weight Volume(V) in (Liter) No.ofeq.wt = N x V(L) OR \ No.ofeq.wt = weight of solute (g) equivalent weight (Eq.wt) Eq.wt = Formula weight (F.wt ) n (no. of (H+) OR (OH-) ) N=Normality n = number of (H+) or (OH-) M= Molarity N=nM Dr. Hadir Shalaby

  26. Problem??? Calculate the eq.wt for each of the following: HCl , H2SO4 , H2CO3 , H3PO4 , Ba(OH)2 *In case of HCl or NaOH HCl 1 H+eqwt = fwt / 1 NaOH 1 OH- *In case of Ba(OH)2 Ba(OH)2 2 OH-eqwt = fwt / 2 *In case of H3PO4 H3PO4 H2PO4- + H+ eqwt = fwt / 1 H3PO4 HPO4-2 + 2 H+ eqwt = fwt / 2 Dr. Hadir Shalaby

  27. Examples: 1-How much primary standard potassium acid phthalate, KHC8H4O4, is required to prepare 499.5 ml of 0.10 N solution?(fwt = 204.23) Weight ( g) = ?? Convert 499.5 ml to Liter by ÷1000 = 0.4995 L Dr. Hadir Shalaby

  28. TYPES OF WATER USED: • Distilled water: is water that has many of its impurities removed through distillation • Deionized water : is water that has had all minerals removed from it,ascations like sodium, calcium, iron, and copper, and anions such as chloride and sulfate, using an ion exchange process

  29. Lab glassware and equipment

  30. burette

  31. Pipette: Graduated pipettes Volumetric pipettes

  32. beaker

  33. cylinder

  34. funnels

  35. Volumetric flask

  36. Conical flask: Glass stopper conical flask Conical flask

  37. Glass rod

  38. Mortar and pestle

  39. Hot plate

  40. electronic balance

  41. hood

  42. GENERAL GUIDELINES: 1- When first entering the lab , do not touch any equipment, chemicals, or other materials in the laboratory area until you are instructed to do so 2- Follow all written and verbal instructions carefully.  If you do not understand a direction or part of a procedure, ASK YOUR TEACHER BEFORE PROCEEDING WITH THE ACTIVITY 3- Never work alone in the laboratory,No student may work in the laboratory without the presence of the teacher

  43. 4- Do not eat food, drink beverages, or chew gum in the laboratory,Do not use laboratory glassware as containers for food or beverages 5- Observe good housekeeping practices , Work areas should be kept clean at all times 

  44. 7- Labels and equipment instructions must be read carefully before use 8- Keep hands away from face, eyes, mouth, and body while using chemicals , Wash your hands with soap and water after performing all experiments

  45. 9-you should Know the locations and operating procedures of all safety equipment

  46. CLOTHING: Dress properly during a laboratory activity.  Long hair must be tied back, Shoes must completely cover the foot

  47. HANDLING CHEMICALS: 1- All chemicals in the laboratory are to be considered dangerous. Avoid handling chemicals with fingers , Do not taste or smell any chemicals 2- Check the label on all chemical bottles twice before removing any of the contents 3- Never return unused chemicals to their original container, and Never remove chemicals or other materials from the laboratory area

  48. HANDLING GLASSWARE AND EQUIPMENT: 1- Never handle broken glass with your hands , Place broken glass in the sharps container 2- Examine glassware before each use 3- Never look into a container that is being heated 4- hood (how can we use it in the safe way )

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