All Questions are to be attempted 1- Redox Titration (35 Marks)
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1 SOHAG UNIVERSITY FACULTY OF PHARMACY PHARM. ANAL. CHEM. DEPT. Pharm. Anal. Chem-2 Second Year Students May, 31, 2016 TIME ALLOWED: TWO HOURS Total marks: 90 All Questions are to be attempted 1- Redox Titration (35 Marks) Question 1: A- Write the balanced equation of the reaction between potassium permanganate and ferrous sulfate in acid medium. (2 Marks) B- Calculate the equilibrium constant (K eq ) of the above reaction (E 0 Fe +3 /Fe +2 = 0.77 V, E 0 MnO4- /Mn +2 = 1.52 V) (2 Marks) B- If chloride ions present in the above solution, what is the Problem? Mention How it can be overcome? (2 Marks) 1
2 Question 2: Mark ( ) for the correct statement and ( X ) for the wrong one and correct the wrong (Each item one Mark) 1- Starch is the specific indicator in all titrations involving iodine. ( ) 2- M 0 /M n+ system of positive potential can oxidize and displace those of negative potential. ( ) 3- Titrations with ceric sulfate can be applied in alkaline medium. ( ) 4- The sign of the standard electrode potential is similar to charge on the electrode. ( ) 5- Diphenylamine is a redox indicator (E 0 =0.76, n=2), accordingly, its E 0 range from ( ) 6- The lower the ph, the weaker the oxidation potential of AsO /AsO 3 system. ( ) 7- H 2 O 2 behaves as oxidant and reductant. ( ) 8- Standard bromine solution can be prepared by dissolving bromine in water. ( ) 9- K 2 Cr 2 O 7 has more than equivalent weight at different ph. ( ) 10- Equivalent weight of Na 2 S 2 O 3 equals its half molecular weight. ( ) 11- When titrating 100 ml 0.1 N ferrous solution (E 0 Fe +3 /Fe +2 = 0.77 V) 2
3 with 100 ml 0.1N ceric solution (E 0 Ce 4+ /Ce 3+ = 1.44 V) in dil. H 2 SO 4, the potential at equivalence point equals 1.33 V. ( ) Iodimetric determination of SO 3 is possible under anhydrous condition. ( ) 13- KMnO 4 can oxidize Cl -, Br - and I - at ph 5. ( ) 14- Metallic iron can displace Cu 2+ in its salts. ( ) 15- Methyl red is used as redox indicator when titrating AsO 3 3- BrO 3 - in acid medium. ( ) with 16- The oxidation product of thiosulfate, by reaction with oxidants stronger than iodine, is tetrathionate. ( ) 17- In weakly alkaline medium glycerol is oxidized by KMnO 4 into oxalate and CO 2. ( ) 18- Chloroform is the specific indicator in Andrew's method. ( ) 19- Isonicotinic acid hydrazide can be determined bromometrically and its reaction product is the bromoderivative. ( ) 20- In determination of copper salts by treatment with excess of KI thiocyanate must be added at the beginning of titration to prevent adsorption of I 2 on Cu 2 I 2. ( ) 3
4 Question 3: Explain, by equations only, How you can analyze the following: a) Iodine solution. (3 Marks) b) Mixture of acetic and formic acids. (4 Marks) c) Vitamin C (ascorbic acid). (2 Marks) 4
5 II-Compleximetry (20 marks) 1-Mention in one word or two words the scientific name or expression for the following : (7x1 points) a-a compound whose color changes when it binds to metal ion. ( ) b-chelating agent, non toxic, serves as an effective antidote for the treatment of lead poisoning. ( ) c-complex species containing two metal ions or more than two metal ions. ( ) d-the value which give the ratio of the total uncombined EDTA (in all forms ) to the fully ionized form. e-a substance added in complexation titration that prevents the formation of insoluble metal hydroxide but does not prevent the reaction of metal with EDTA. ( ) f-a type of EDTA titration in which the librated hydrogen ions are neutralized with standard alkali. ( ) g-substance refers to the release of a metal ions from a complex. ( ) 2-Explain (only be equations) how can you analyze the following: (2x2points) a-determination of iodide by mercuric chloride. b- Determination of copper by cyanometric method. 5
6 3-Write the most suitable indicator for each of the following titrations: a-lead ions with EDTA at ph 10 b-calcium ions with EDTA at ph 12. c-bismuth ions with thiosulphate at ph 1-3. d-mercuric ions with thiocyanate. e-halide ions with mercuric nitrate. f-zinc ion with EDTA at ph 10. (6x0.5 points) 4-Mark the following with right ( ) or wrong ( x) and correct the wrong one. (6x1 points) a-magnesium ions form stable complex with cyanide ions. ( ) b-aluminium ions block Erio T indicator. ( ) c-silver ions can be analyzed by direct titration with EDTA. ( ) d-the stability of EDTA complexes is affected only by ph. ( ) e-direct titration of calcium ions with EDTA, Eriochrome Black T gives a poor end point. ( ) f-ca-chelate is too weak to be titrated in acid solution, while mercury-chelate is strong enough to be titrated in that medium. ( ) 6
7 III. STATISTICS (15 marks) Ques. I (6 marks) In a titrimetric method, the following volumes were obtained: 10.0, 9.9, 9.0, 9.9 & 9.7 ml. -Should we reject or retain the outlier? -Calculate the standard deviation, the coefficient of variation, and the standard error of the mean for the five measurements. Rejection quotient, Q n Confidence level Q 90 Q 95 Q Ques. II Mention the validation parameters (performance criteria) for an analytical method (3 marks) 7
8 Ques. III (3 marks) Group A: Suggested methods for minimization of determinable errors: 1- Blank experiments. 2- Standard addition method. 3- Internal standard method. 4- Running a control determination. 5- Calibration of apparatus. 6- Use of independent method of analysis. Group B: Some examples of determinable errors: - Interference from excipients or additives of pharmaceutical formulations. - Errors due to variation in analytical techniques. - Impurities from some reagents or samples. - Errors due to experimental procedures or steps like boiling and cooling. - Errors due to equipments. - Variations in experimental chromatographic conditions (e.g. in HPLC). Put the proper number from group A into each of the items of group B. Ques. IV Differentiate by definitions between (a) & (b): (a) Accuracy: Precision: (3 marks) (b) Ruggedness: Robustness: Limit of detection: Limit of quantitation: WITH BEST WISHES 8
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