This document describes an experiment to standardize a potassium permanganate solution using sodium oxalate and then determine the amount of calcium in limestone through redox titration. The experiment involves standardizing the potassium permanganate against sodium oxalate, precipitating calcium oxalate from limestone using ammonium oxalate, and titrating the calcium oxalate with the standardized potassium permanganate solution. The results show a calcium content of 22.57% in the limestone sample. Sources of error are discussed, including co-precipitation of other ions and incomplete precipitation or filtration of calcium oxalate.
This document describes an experiment to standardize a potassium permanganate solution using sodium oxalate and then determine the amount of calcium in limestone through redox titration. The experiment involves standardizing the potassium permanganate against sodium oxalate, precipitating calcium oxalate from limestone using ammonium oxalate, and titrating the calcium oxalate with the standardized potassium permanganate solution. The results show a calcium content of 22.57% in the limestone sample. Sources of error are discussed, including co-precipitation of other ions and incomplete precipitation or filtration of calcium oxalate.
This document describes an experiment to standardize a potassium permanganate solution using sodium oxalate and then determine the amount of calcium in limestone through redox titration. The experiment involves standardizing the potassium permanganate against sodium oxalate, precipitating calcium oxalate from limestone using ammonium oxalate, and titrating the calcium oxalate with the standardized potassium permanganate solution. The results show a calcium content of 22.57% in the limestone sample. Sources of error are discussed, including co-precipitation of other ions and incomplete precipitation or filtration of calcium oxalate.
* To standardize potassium permanganate solution using primary standard
sodium oxalate. * To determine the amount of calcium in limestone. Introduction: A redox titration is based on oxidation-reduction reaction between analyte (Na 2 C 2 O 4 ) and titrant (KMnO 4 ). Potassium permanganate is a powerful oxidizing agent and serves as a self indicator in the titration with reducing agent. Sodium oxalate is used for standardization of potassium permanganate as the following reaction show ) ( 2 ) ( 2 ) ( 2 ) ( 4 ) ( 4 2 2 2 8 10 2 5 aq l g aq aq Mn O H CO MnO O C + + + + 1 And this is the reaction which used in this experiment. Methods: 1- Standardization of Potassium Permanganate. Two samples of Na 2 C 2 O 4 were weighed and transferred to 250 ml conical flasks. Then 50 ml of H 2 SO 4 was added to each of the flasks and then heated to 80-90 0 C.After that titrated against KMnO 4 immediately when it is reached that temperature. 2- Analysis of the unknown Limestone. A sample of dry limestone were weighted and transferred to 250 ml beaker. 10ml of water was added and covered with watch glass. Then 10ml of concentrated HCl was added. After that 5 drops of saturated bromine was added followed by boiling in the hood for 5 minutes to remove the excess Br 2 . Then it was diluted to about 50 ml with water and heated to boiling. 100 ml of hot 6% ammonium oxalate solution were added in the hood 3 or 4 drops of methyl red indicator were added and precipitate CaC 2 O 4 by slowly adding 6M NH 3 and continue adding 1 drop every 3 to 4 second until the solution turn to yellow orange color. The solution was allowed to cool fro 30 minutes 2 then it was filtered. Then the precipitate was transferred to 250 ml conical flask. Finally titrated it against KMnO 4 . Apparatus: Two 250 ml conical flasks, 250 ml beaker, 100 ml graduated cylinder, burette, filter flask, funnel. Materials: KMnO 4 solution, Na 2 C 2 O 4 , Limestone, Bromine H 2 O, Concentration HCL, (NH 4 ) 2 C 2 O 4 solution, Methyl red indicator and dilute H 2 SO 4. Results: A sample 1 sample 2 m(NaC2O4) -(g) 0.233 0.0001 0.2345 0.0001 Vi(KMnO4) -(ml) 0.10 0.05 11.91 0.05 Vf(KMnO4) -(ml) 11.91 0.05 23.69 0.05 V(KMnO4) -a-(ml) 11.!1 0.0" 11."! 0.05 M(KMnO4) -(m#l$l ) 0.05!!9 0.0001 0.05916 0.0001 Table 1: Data taken from the experiment. % sample 1 sample 2 m-(g) 0.2590 0.0001 0.2593 0.0001 3 Vi(KMnO4) -(ml) 32.45 0.05 23.69 0.05 Vf(KMnO4) -(ml) 42.32 0.05 32.23 0.05 V(KMnO4) -a-(ml) 9.!" 0.05 !.45 0.05 & mass CaO 31.6 2".03 & mass Ca 22.5! 22.55 Table 2: Data taken from the experiment. Calculations: See the appendix. Discussion: We must get rid of other cations such as Fe 2+ & Ni 2+ to avoid forming of insoluble oxalates or co-precipitate of the unknown with calcium oxalate making it impure. Alternative methods to determine Ca 2+ is substitution titration in which the calcium oxalate titrated to get color changing from red to blue. The advantage in using my method is in the detection of color change from colorless to pink at the end point is easy, but in substitution method the color changes from red to blue and that difficult to detect. The advantage of using substitution method is the product solubility so it is easily to be filtered. The disadvantage of this method cannot be used to any sample except which contain magnesium or alkali metals. 4 Conclusions: Redox titration is important in determination of the mass of calcium in a sample and then determination of the percent of mass in limestone is by titrating it with KMnO 4 . The result is 22.57 % and it shows that there are many sources of errors in this experiment:
Co-precipitate of the other cations with the calcium oxalate and
incomplete precipitation of CaC 2 O 4 when adding NH 3 . Standardization process of KMnO 4 , impurities of the chemicals. Wrong determination of the end point. Errors in reading the burette. Errors in the analytical balance and the glassware used. Incomplete heating at a specific temperature and doing the titration when the media is cool. Loss of precipitate during filtration and loss of precipitate during transferring 5 Referances: Handout. D. C. Harris, Quantitative Chemical analysis, 6th ed, Freeman: New York, 1999. Index: Index Page no. Objectives 2 Introduction 2 Method 2 Apparatus 3 Materials 3 Results 4 Calculations In appendix Discussion 4 Conclusions 5 References 6 6
1991 International Conference on Coal Science Proceedings: Proceedings of the International Conference on Coal Science, 16–20 September 1991, University of Newcastle-Upon-Tyne, United Kingdom