QUANTITATIVE ANALYSIS The term quantitative analysis refers to the analysis carried out by reacting a standard solution (a solution of accurately known concentration) with a solution whose concentration is to be determined. It’s usually called volumetric analysis. Standard solution. This is a solution whose concentration is accurately known. The concentration can be in moles per litre (Molarity) or grams in a given volume like 1 litre, 500cm3 etc Primary standard. This is a substance which is analytically pure and whose composition is accurately known and is used to prepare a standard solution. E.g Anhydrous sodium carbonate, borax, potassium iodate, oxalic acid e.t.c Properties of a good primary standard. It must be readily available in a state of high purity. It should be readily soluble in water. It should have a high molecular mass to reduce errors during weighing. It must be stable in air (have a constant composition) i.e should not be hygroscopic, deliquescent or efflorescent. The following substances cannot be used as primary standards; (a) Sodium hydroxide. This is because; It is deliquescent (absorbs water from the atmosphere and dissolves in it) It absorbs carbon dioxide from air forming a solution of sodium carbonate solution. 2NaOH(aq) + CO2(g) Na2CO3(aq) + H2O(l) This reduces the concentration of sodium hydroxide solution. When excess carbon dioxide comes into contact with sodium hydroxide solution, a white precipitate is formed. Na2CO3(aq) + H2O(l) + CO2(g) 2NaHCO3(s) (b) Concentrated Sulphuric acid. It is hygroscopic hence does not have a constant composition. (c) Ammonia solution. It is highly volatile. (d) Concentrated nitric acid. It is a strong oxidizing agent. (e) Sodium thiosulphate It is efflorescent (loses its water of crystallization to the atmosphere) When left exposed in air, it absorbs carbon dioxide from air forming carbonic acid. The carbonic acid decomposes the thiosulphate ions to form sulphur dioxide, sulphur and water. This reduces the concentration of sodium thiosulphate. H2O(l) + CO2(g) H2CO3(s) 2+ S2O3 (aq) + 2H (aq) S(s) + SO2(g) + H2O(l) Distinguish between S2O32- and SO32Reagent: Dilute Sulphuric acid or dilute hydrochloric acid. S2O32- - A yellow precipitate and bubbles of a colourless gas. SO32- - Bubbles of a colourless gas. 1 (f) Potassium mangante(VII) It is impure, contaminated with manganese(IV) oxide, thus its solution should be filtered first before use. In the neutral or alkaline medium, it is reduced to a dark brown solid of manganese(IV) oxide. MnO-4(aq) + 2H2O(l) + 3e MnO2(s) + 4OH-(aq) ACID BASE TITRATIONS. EXPERIMENT 1. You are provided with the following; FA1, which is a solution of hydrochloric acid Solid A, which is anhydrous sodium carbonate. You are required to standardize FA1 using sodium carbonate. Procedure. Weigh accurately about 2.7g of A and place it in a beaker. Add 100cm3 of water and carefully stir to dissolve. Transfer the contents of the beaker into a 250cm3 volumetric flask and add water to make up to the mark. Label the solution FA2. Pipette 20cm3 or 25cm3 of FA2 into a clean conical flask. Add 2-3 drops of methyl orange indicator and titrate with FA1 from the burette until the endpoint. Repeat the titration 2-3 times until you obtain consistent results. Enter your results in the table below. Results; Mass of empty bottle + A=……………………………………………..g Mass of empty bottle alone=………………………………………….g Mass of A alone=……………………………………………………………g Volume of pipette used=…………………………………………….cm3 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading (cm3) Volume of FA1 used (cm3) Titre values used to calculate average volume of FA1. ………………………………………………………………………………………………………cm3 Average volume of FA1 used …………………………………………………………..cm3 Questions; Calculate the; (i) Number of moles of sodium carbonate in FA2 that reacted with hydrochloric acid in FA1. 2 …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ……………………………………………………………………………………………………………………………. (ii) Molarity of hydrochloric acid in FA1. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ………………………………………………………………………………………………………………………… Experiment 2 You are provided with the following; Solid B, which is borax. FA1, which is a solution of hydrochloric acid You are required to standardize of FA1 using borax. Theory Borax(Na2B4O7.10H2O) is a salt of a strong base and a weak acid. Borax undergoes partial hydrolysis to form boric acid and sodium hydroxide. Na2B4O7(aq) + 7H2O(l) 2NaOH(aq) + 4H3BO3(aq) The sodium hydroxide imparts on the alkaline reaction to the solution. Hence borax reacts with hydrochloric acid according to the equation below Na2B4O7.10 H2O(aq) + 2HCl(aq) 2NaCl(aq) + 4H3BO3(aq) + 5H2O(l) Procedure. Weigh accurately about 4.8g of B and place it in a beaker. Add 100cm3 of water and carefully stir to dissolve. Transfer the contents of the beaker into a 250cm3 volumetric flask and add water to make up to the mark. Label the solution FA2. Pipette 20cm3 or 25cm3 of FA2 into a clean conical flask. Add 2-3 drops of methyl orange indicator and titrate with FA1 from the burette until the endpoint. Repeat the titration 2-3 times until you obtain consistent results. Enter your results in the table below. Results; Mass of empty bottle + B=……………………………………………..g Mass of empty bottle alone=………………………………………….g Mass of B alone=……………………………………………………………g 3 Volume of pipette used=…………………………………………….cm3 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading (cm3) Volume of FA1 used (cm3) Titre values used to calculate average volume of FA1. ………………………………………………………………………………………………………cm3 Average volume of FA1 used ………………………………………………………….. cm3 Questions; Calculate the concentration of; (i) Borax in FA2 in moles per litre. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ……………………………………………………………………………………………………………………………. (ii) Hydrochloric acid in FA1 in moles per litre. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ………………………………………………………………………………………………………………………… Experiment 3 You are provided with the following; FA1, which is approximately 0.1M solution of sodium hydroxide. FA2, which is 0.1M hydrochloric acid Solid C, which is an organic acid of formula, (COOH)2. xH2O 4 You are required to standardize FA1 and use it to determine the number of moles of water of crystallization, x of an organic acid, (COOH)2. xH2O Procedure I Pipette 20cm3 or 25cm3 of FA1 into a clean conical flask. Add 2-3 drops of phenolphthalein indicator and then titrate with FA2 from the burette until you reach the end point. Repeat the titration 2-3 times until you obtain consistent results. Enter your results in the table below. Results Volume of pipette used…………………………………..cm3 Table 1 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading(cm3) Volume of FA2 used(cm3) Titre values used for calculating average volume of FA2 used ………………………………………………………………………………………………………cm3 Average volume of FA2 used……………………………………………………………cm3 Questions; (a) Calculate the molar concentration of FA1. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… Procedure II Weigh accurately about 1.6g of C and place it in a beaker. Add 100cm3 of water and carefully stir to dissolve. Transfer the contents of the beaker into a 250cm3 volumetric flask and add water to make up to the mark. Label the solution FA3. Pipette 20cm3 or 25cm3 of FA1 into a clean conical flask. Add 2-3 drops of 5 phenolphthalein indicator and titrate with FA3 from the burette until the endpoint. Repeat the titration 2-3 times until you obtain consistent results. Enter your results in the table below. Results; Mass of empty bottle + C=……………………………………………..g Mass of empty bottle alone=………………………………………….g Mass of C alone=……………………………………………………………g Volume of pipette used=…………………………………………….cm3 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading (cm3) Volume of FA3 used (cm3) Titre values used to calculate average volume of FA3. ………………………………………………………………………………………………………cm3 Average volume of FA3 used …………………………………………………………..cm3 Questions; (b) Calculate the; (i) Number of moles of sodium hydroxide in FA1 that reacted with FA3. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ……………………………………………………………………………………………………………………………... (ii) Molecular mass of the organic acid (COOH)2.xH2O. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (c) Determine the value of x in the organic acid, (COOH)2.xH2O …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ……………………………………………………………………………………………………………………………... 6 Experiment 4 You are provided with the following; FA1, which is a solution of sodium hydroxide. FA2, which is 0.1M hydrochloric acid Solid D, which is an organic acid of formula, (CH2)n(COOH)2. You are required to standardize FA1 and use it to determine the value, n in the organic acid (CH2)n(COOH)2. Procedure I Pipette 20cm3 or 25cm3 of FA1 into a clean conical flask. Add 2-3 drops of phenolphthalein indicator and then titrate with FA2 from the burette until you reach the end point. Repeat the titration 2-3 times until you obtain consistent results. Enter your results in the table below. Results Volume of pipette used…………………………………..cm3 Table 1 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading(cm3) Volume of FA2 used(cm3) Titre values used for calculating average volume of FA2 used ………………………………………………………………………………………………………cm3. Average volume of FA2 used……………………………………………………………cm3 Questions; (a) Calculate the molar concentration of sodium hydroxide solution in FA1. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… 7 Procedure II Weigh accurately about 1.6g of D and place it in a beaker. Add 100cm3 of water and carefully stir to dissolve. Transfer the contents of the beaker into a 250cm3 volumetric flask and add water to make up to the mark. Label the solution FA3. Pipette 20cm3 or 25cm3 of FA1 into a clean conical flask. Add 2-3 drops of phenolphthalein indicator and titrate with FA3 from the burette until the endpoint. Repeat the titration 2-3 times until you obtain consistent results. Enter your results in the table below. Results; Mass of empty bottle + D=……………………………………………..g Mass of empty bottle alone=………………………………………….g Mass of D alone=……………………………………………………………g Volume of pipette used=…………………………………………….cm3 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading (cm3) Volume of FA3 used (cm3) Titre values used to calculate average volume of FA3. ………………………………………………………………………………………………………cm3 Average volume of FA3 used ………………………………………………… cm3 Questions; (b) Calculate the; (i) Number of moles of sodium hydroxide in FA1 that reacted with FA3. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (ii) Concentration of FA3 in moles per litre. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (iii) Determine the value of n in the organic acid, (CH2)n(COOH)2 …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… 8 …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………….. TRIAL QUESTIONS 1. 20cm3 of 0.15M sodium hydroxide solution required 20cm3 of a solution of an acid H2X for complete reaction which was made by dissolving 2.45g of the acid in 250cm3. Calculate the relative molecular mass of the acid. 2. 25cm3 of 0.04M sodium carbonate solution was neutralized by 6.67cm3 of 0.15M solution of an acid HX. Determine the mole ratio for the reaction that took place. 3. 20cm3 of 0.2M potassium hydroxide solution required 25cm3 of hydrochloric acid for complete reaction. Calculate the concentration of hydrochloric acid in grams per litre. 4. 2.0g of an impure acid H2X was dissolved in water and the solution made to 250cm3 with distilled water. 25cm3 of this solution required 25cm3 of 0.1M sodium hydroxide solution for complete reaction. Calculate the percentage purity of the acid. [X=124] 5. 4.0g of hydrated sodium carbonate, Na2CO3.XH2O was dissolved in water and the solution made to 250cm3 in a volumetric flask. 25cm3 of this solution required 21cm3 of 0.2M hydrochloric acid for complete reaction. Determine the value of X. 6. 5.0g of an acid YCO2H was dissolved in water and the solution made to 250cm3 with distilled water in a volumetric flask. 25cm3 of this solution required 20.5cm3 of 0.4M sodium hydroxide solution for complete reaction. Determine the value of Y in the acid. 7. 20cm3 of an acid HOOC(CH2)nCOOH made by dissolving 10g in a litre required 33.9cm3 of 0.1M sodium hydroxide solution for complete neutralization. Determine the value of n in the acid. 9 BACK TITRATION. Back titration is a technique of analyzing the composition of a substance by reacting it with an excess reagent of known concentration and then titrating the unreacted reagent with another standard solution. Theory An excess standard solution X is reacted with a substance Y whose concentration is to be determined. Y+X Product + Unreacted X The unreacted X is diluted to a given volume i.e 250cm3. A given volume of the diluted solution is then titrated against another standard solution Z. Unreacted X + Z Product By back calculation, the amount of Y that reacted with X can be determined. Procedure Calculate the number of moles of Z that reacted with unreacted X. Calculate the number of unreacted X using the mole ratios. Calculate the number of moles of unreacted X in the diluted volume i.e 250cm3 Calculate the original moles of X that was added. By subtraction, calculate the number of moles X that reacted with Y. Calculate the number of moles of Y that reacted with X using moles ratios. Worked examples 4.0g of impure calcium carbonate was added to 150cm3 of 0.48M hydrochloric acid and the mixture shaken until effervescence stopped. The resultant solution was made to a 250cm3 mark in a volumetric flask using distilled water. 25cm3 of this solution required 22.5cm3 of 0.2M sodium hydroxide solution for complete neutralization. Calculate the; (a) Number of moles hydrochloric acid that reacted with sodium hydroxide. (b) Number of moles of hydrochloric acid that reacted with calcium carbonate. (c) Number of moles of calcium carbonate that reacted with hydrochloric acid. (d) Percentage purity of calcium carbonate in the sample. Solution 3 (a) 1000cm of solution contains 0.2 moles of NaOH 22.5cm3 of solution contains 0.2×22.5 1000 moles of NaOH =0.0045 moles NaOH(aq) + HCl(aq) NaCl(aq) + H2O(l) Mole ratio NaOH: HCl = 1:1 Moles of HCl that reacted = 0.0045 moles (b) 25cm3 of solution contains 0.0045 moles of HCl 250cm3 of solution contains 0.0045×250 25 =0.045 moles Original moles of HCl 1000cm3 of solution contains 0.48 moles of HCl 10 150cm3 of solution contains 0.48×150 1000 moles of HCl =0.072 moles Moles of HCl that reacted with CaCO3 = 0.072- 0.045 = 0.027 moles (c) CaCO3(s) + 2HCl(aq) CaCl2(aq) + CO2(g) + H2O(l) Mole ratio CaCO3: HCl = 1:2 1 Moles of CaCO3 that reacted = 2 × 0.027 = 0.0135 moles (d) Rmm of CaCO3 = 40 + 12 + (3×16) = 100 1 mole of CaCO3 weighs 100g 0.0135 moles of CaCO3 weighs Percentage purity of CaCO3 = 0.0135×100 1 1.35×100 4.0 = 1.35g = 33.75% Experiment 5 You are provided with the following; FA1, which is 1M sodium hydroxide solution FA2, which is 1M hydrochloric acid Solid E, which is a metal carbonate, XCO3. You are required to determine the relative atomic mass of X in XCO3. Procedure Weigh accurately about 1.0g of E and place it in a beaker. Add 100cm3 of FA2 and carefully stir to dissolve. Transfer the contents of the beaker into a 250cm3 volumetric flask and add water to make up to the mark. Label the solution FA3. Pipette 20cm3 or 25cm3 of FA3 into a clean conical flask. Add 2-3 drops of phenolphthalein indicator and titrate with FA1 from the burette until the endpoint. Repeat the titration 2-3 times until you obtain consistent results. Enter your results in the table below. Results; Mass of empty bottle + E=……………………………………………..g Mass of empty bottle alone=………………………………………….g Mass of E alone=……………………………………………………………g Volume of pipette used=…………………………………………….cm3 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading (cm3) Volume of FA1 used (cm3) Titre values used to calculate average volume of FA1. ………………………………………………………………………………………………………cm3 Average volume of FA1 used …………………………………………………………cm3 11 Questions; (a) Calculate the number of moles of; (i) Excess hydrochloric acid that reacted with sodium hydroxide. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (ii) Hydrochloric acid that reacted with E. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ……………………………………………………………………………………………………………………………... (iii) E that reacted with hydrochloric acid. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (b) Determine the relative atomic mass of X in XCO3. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ………………………………………………………………………………………………………………………… 12 Experiment 6 You are provided with the following; FA1, which is 0.1M sodium hydroxide solution FA2, which is 2M hydrochloric acid Solid F, which is impure calcium carbonate. You are required to determine the percentage impurity of solid F. Procedure Weigh accurately about 1.5g of F and place it in a beaker. Add 20cm3 of FA2 and carefully stir to dissolve. Add 80cm3 of distilled water and label the solution FA3. Pipette 20cm3 or 25cm3 of FA1 into a clean conical flask. Add 2-3 drops of phenolphthalein indicator and titrate with FA3 from the burette until the endpoint. Repeat the titration 2-3 times until you obtain consistent results. Enter your results in the table below. Results; Mass of empty bottle + F=……………………………………………..g Mass of empty bottle alone=………………………………………….g Mass of F alone=……………………………………………………………g Volume of pipette used=…………………………………………….cm3 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading (cm3) Volume of FA3 used (cm3) Titre values used to calculate average volume of FA3. ………………………………………………………………………………………………………cm3 Average volume of FA3 used …………………………………………………………..cm3 Questions; (a) Calculate the number of moles of; (i) Hydrochloric acid in 100cm3 of FA3. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ……………………………………………………………………………………………………………………………... (ii) Hydrochloric acid that reacted with F. 13 …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (b) Determine the percentage impurity of solid F. (Ca=40, C=12, 0=16) …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… Experiment 7 You are provided with the following; FA1, which is 0.1M sodium hydroxide solution FA2, which is 0.05M sulphuric acid Solid G, which is an organic acid, (COOH)2.nH2O . You are required to determine the number of moles of water of crystallization, n in the organic acid. Procedure Weigh accurately about 1.0g of G and place it in a beaker. Add 200cm3 of FA1 and carefully and stir to dissolve. Transfer the contents of the beaker into a 250cm3 volumetric flask and add water to make up to the mark. Label the solution FA3. Pipette 20cm3 or 25cm3 of FA3 into a clean conical flask. Add 2-3 drops of phenolphthalein indicator and titrate with FA2 from the burette until the endpoint. Repeat the titration 2-3 times until you obtain consistent results. Enter your results in the table below. Results; Mass of empty bottle + G=……………………………………………..g Mass of empty bottle alone=………………………………………….g Mass of G alone=……………………………………………………………g Volume of pipette used=…………………………………………….cm3 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading (cm3) Volume of FA2 used (cm3) 14 Titre values used to calculate average volume of FA2. ………………………………………………………………………………………………………cm3 Average volume of FA2 used …………………………………………………………..cm3 Questions; (a) Calculate the number of moles of; (i) Excess sodium hydroxide that reacted with sulphuric acid. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (ii) Sodium hydroxide that reacted with G. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ……………………………………………………………………………………………………………………………... (iii) G that reacted with sodium hydroxide. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (c) Determine the value of n in (COOH)2. nH2O. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ………………………………………………………………………………………………………………………… 15 Experiment 8 You are provided with the following; FA1, which is 1M sodium hydroxide solution FA2, which is 0.2M hydrochloric acid Solid H, which is impure ammonium chloride. You are required to determine the percentage purity of solid H. Procedure Weigh accurately about 4.0g of H and transfer it into a conical flask and add 100cm3 of FA1 and carefully boil the mixture for about 10 minutes. Cool and transfer the contents into a 250cm3 volumetric flask and add water to make up to the mark. Label the solution FA3. Pipette 20cm3 or 25cm3 of FA3 into a clean conical flask. Add 2-3 drops of phenolphthalein indicator and titrate with FA2 from the burette until the endpoint. Repeat the titration 2-3 times until you obtain consistent results. Enter your results in the table below. Results; Mass of empty bottle + H=……………………………………………..g Mass of empty bottle alone=………………………………………….g Mass of H alone=……………………………………………………………g Volume of pipette used=…………………………………………….cm3 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading (cm3) Volume of FA2 used (cm3) Titre values used to calculate average volume of FA2. ………………………………………………………………………………………………………cm3 Average volume of FA2 used …………………………………………………………..cm3 Questions; (a) Calculate the number of moles of; (i) Excess sodium hydroxide that reacted with FA2. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (ii) Sodium hydroxide that reacted with H. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… 16 …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ……………………………………………………………………………………………………………………………... (iii) H that reacted with FA1. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (b) Determine the percentage purity in H. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ………………………………………………………………………………………………………………………… Experiment 9 You are provided with the following; FA1, which is a 1M hydrochloric acid FA2, which is sodium hydroxide solution FA3, which is 0.1M Sulphuric acid Solid I, which is an acid H3X You are required to standardize sodium hydroxide solution in FA2 and use to determine the value of X in H3X. Procedure I Pipette 20cm3 or 25cm3 of FA2 into a clean conical flask. Add 2-3 drops of phenolphthalein indicator and then titrate with FA1 from the burette until you reach the end point. Repeat the titration 2-3 times until you obtain consistent results. Enter your results in the table below. Results 17 Volume of pipette used…………………………………..cm3 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading(cm3) Volume of FA1 used(cm3) Titre values used for calculating average volume of FA1 used ………………………………………………………………………………………………………cm3. Average volume of FA1 used……………………………………………………………cm3 Questions; (a) Calculate the molar concentration of sodium hydroxide solution in FA2. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… Procedure II Weigh accurately about 3.4g of I and place it in a beaker. Add 100cm3 of FA2 and carefully stir to dissolve. Transfer the contents of the beaker into a 250cm3 volumetric flask and add water to make up to the mark. Label the solution FA4. Pipette 25cm3 of FA4 into a clean conical flask. Add 2-3 drops of phenolphthalein indicator and titrate with FA3 from the burette until the endpoint. Repeat the titration 2-3 times until you obtain consistent results. Enter your results in the table below. Results; Mass of empty bottle + I=……………………………………………..g Mass of empty bottle alone=………………………………………….g Mass of I alone=……………………………………………………………g Volume of pipette used=…………………………………………….cm3 18 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading (cm3) Volume of FA3 used (cm3) Titre values used to calculate average volume of FA3. ………………………………………………………………………………………………………cm3 Average volume of FA3 used …………………………………………………………..cm3 Questions; (b) Calculate the number of moles of; (i) Sulphuric acid in FA3 that reacted with sodium hydroxide in FA4. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (ii) Excess sodium hydroxide in 250cm3 of FA4. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ………………………………………………………………………………………………………………………… (iii) Sodium hydroxide that reacted with I. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ……………………………………………………………………………………………………………………………... (iv) I that reacted with sodium hydroxide. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… 19 …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ……………………………………………………………………………………………………………………………... (c) Determine the value of X in H3X. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ……………………………………………………………………………………………………………………………... TRIAL QUESTIONS 1. To 2.0g of impure calcium carbonate in a beaker was added 50cm3 of 1M hydrochloric acid. The resultant solution was made to 250cm3 with distilled water. 25cm3 of this solution required 20cm3 of 0.1M hydrochloric acid for complete reaction. Determine the percentage of pure calcium carbonate in the sample. 2. To 1.6g of ammonium sulphate was added 50cm3 of 1M sodium hydroxide solution and the mixture boiled until all the ammonia was expelled. The resultant solution was made to 250cm3 with distilled water. 25cm3 of this solution required 20cm3 of 0.1M hydrochloric acid for complete reaction. Determine the percentage of ammonia expelled. 3. 4.0g of ammonium chloride was added to 200cm3 of 0.17M sodium hydroxide solution. The mixture was boiled until all the ammonia was expelled and the resultant solution made to 250cm3 with distilled water. 25cm3 of this solution required 20cm3 0f 0.05M Sulphuric acid for complete neutralization using phenolphthalein indicator. Calculate the percentage of ammonia expelled. 4. 10g of ammonium chloride was added to 200cm3 of 1M sodium hydroxide solution. The mixture was boiled until ammonia ceased to be evolved. The resultant solution was titrated with 1M hydrochloric acid and 11.8cm3 of hydrochloric acid was required for complete reaction. Calculate the percentage of ammonia in the salt. 20 DOUBLE INDICATOR TITRATIONS. INTRODUCTION A double indicator titration is a technique used for analyzing the composition of a mixture of two different bases that react with an acid in the same reaction using two different indicators. In one type of analysis, the indicators are added separately i.e each indicator is used in separate titrations. [Separate titrations] In another type of titration, the indicators are added simultaneously i.e one indicator (usually phenolphthalein) is added to reach the first end point and the second indicator (usually methyl orange) is added to complete the reaction and reach the second end point. (Continuous titrations) The mixtures considered include; (a) Sodium carbonate and sodium hydrogencarbonate. (b) Sodium carbonate and sodium hydroxide (c) Sodium hydrogencarbonate and sodium hydroxide Sodium carbonate Vs phenolphthalein indicator Phenolphthalein indicator changes colour to pink under alkaline conditions i.e pH range of 8.2-10.0 Sodium carbonate solution is alkaline (pH=9.0) is able to turn the indicator pink. During the titration with an acid, the carbonate is converted to a hydrogencarbonate which is an acid salt (pH =3.7), the indicator turns colourless to mark the end point for half neutralization. If the volume of the acid needed is V1, therefore for complete reaction of the carbonate, the volume of the acid needed is twice V1 i.e 2V1 Sodium hydrogencarbonate Vs phenolphthalein indicator A solution of sodium hydrogencarbonate is acidic (pH =3.7). A drop of phenolphthalein indicator to this solution remains colourless and therefore cannot be used to mark the end point for the titration with an acid. Sodium carbonate Vs methyl orange indicator Methyl orange indicator turns yellow in a solution of sodium carbonate. During the titration with an acid, the carbonate reacts completely to form a salt, water and carbon dioxide. Sodium hydrogencarbonate also reacts completely. 21 ANALYSIS OF A MIXTURE OF SODIUM CARBONATE AND SODIUM HYDROGENCARBONATE. Method I (continuous titration) (a) The mixture is pipetted, phenolphthalein indicator added and titrated against a standard solution of hydrochloric acid until the end point. The volume of the acid, V1 used is recorded. Sodium carbonate undergoes half neutralization to form sodium hydrogencarbonate while the original sodium hydrogencarbonate does not react. Na2CO3(aq) + HCl(aq) V1 NaHCO3(aq) + NaCl(aq) Therefore for the complete neutralization of sodium carbonate alone, the volume of the acid would be 2V1. (b) To the resultant solution in (a) is added a few drops of methyl orange indicator and the titration continued until the end point. The volume of the acid, V2, used is recorded. Both the formed sodium hydrogencarbonatein (a) and the original sodium hydrogencarbonate react with the acid. NaHCO3(aq) + HCl(aq) V1 NaCl(aq) + CO2(g) + H2O(l) (Formed) V2 NaHCO3(aq) + HCl(aq) NaCl(aq) + CO2(g) + H2O(l) (Original) The volume of the acid that reacted with the NaHCO3 formed=V1 The volume of the acid that reacted with the original NaHCO3 =V2-V1 Method II (separate titration) (a) The mixture is pipetted, phenolphthalein indicator added and titrated against a standard solution of hydrochloric acid until the end point. The volume of the acid, V1 used is recorded. Sodium carbonate undergoes half neutralization to form sodium hydrogencarbonate while the original sodium hydrogencarbonate does not react. Na2CO3(aq) + HCl(aq) V1 NaHCO3(aq) + NaCl(aq) Therefore for the complete neutralization of Na2CO3 alone, the volume of the acid would be 2V1. (b) A fresh sample of the mixture is pipetted, a few drops of methyl orange indicator is added and then titrated with the acid until the end point. The volume of the acid, V2, used is recorded. Both the sodium carbonate and the sodium hydrogencarbonate react with the acid completely. Na2CO3(aq) + 2HCl(aq) 2V1 2NaCl(aq) + CO2(g) + H2O(l) V2 NaHCO3(aq) + HCl(aq) NaCl(aq) + CO2(g) + H2O(l) (original) 22 The volume of the acid that reacted completely with Na2CO3 alone = 2V1 The volume of the acid that reacted with the original NaHCO3 =V2-2V1 Worked example. 25cm3 of a mixture containing sodium carbonate and sodium hydrogencarbonate required 12cm3 of 0.1M hydrochloric acid using phenolphthalein indicator. When three drops of methyl orange indicator are added to the resultant mixture and the titration continued, 21.3cm3 of the acid was used. Determine the percentage composition of the mixture. Solution Sodium carbonate The volume of the acid that reacted with Na2CO3 alone = 2V1=2 × 12 = 24 cm3 1000cm3 of solution contains 0.1 moles of HCl 24cm3 of solution contains 0.1×24 1000 moles of HCl =0.0024 moles Na2CO3(aq) + 2HCl(aq) 2NaCl(aq) + CO2(g) + H2O(l) Mole ratio Na2CO3: HCl = 1:2 1 Moles of Na2CO3 that reacted = 2 × 0.0024 = 0.0012 moles 25cm3 of solution contains 0.0012 moles of Na2CO3 1000cm3 of solution contains 0.0012×1000 25 moles of Na2CO3 =0.048 moles Molarity of Na2CO3 is 0.048M RFM of Na2CO3= (2 × 23) + 12 + (3 × 16) = 106 1 mole of Na2CO3 weighs 106g 0.048 moles of Na2CO3 weighs (106 × 0.048) = 5.088𝑔 Concentration of Na2CO3 is 5.088gl-1 Sodium hydrogencarbonate The volume of the acid that reacted with NaHCO3 = V2-V1 =21.3 − 12 = 9.3 cm3 1000cm3 of solution contains 0.1 moles of HCl 9.3cm3 of solution contains 0.1×9.3 1000 moles of HCl =0.00093 moles NaHCO3(aq) + HCl(aq) NaCl(aq) + CO2(g) + H2O(l) Mole ratio NaHCO3: HCl = 1:1 Moles of NaHCO3 that reacted = = 0.00093 moles 25cm3 of solution contains 0.00093 moles of NaHCO3 1000cm3 of solution contains 0.00093×1000 25 moles of NaHCO3 =0.0372 moles Molarity of NaHCO3 is 0.0372M RFM of NaHCO3= 23 + 1 + 12 + (3 × 16) = 84 1 mole of NaHCO3 weighs 84g 0.0372 moles of NaHCO3 weighs (84 × 0.0372) = 3.1248𝑔 23 Concentration of NaHCO3 is 3.1248gl-1 Total concentration = 5.088+3.1248= 8.2128gl-1 Hence, percentage of Na2CO3 = Percentage of NaHCO3 = 5.088×100 8.2128 3.1248×100 8.2128 = 61.95% = 38.05% ANALYSIS OF A MIXTURE OF SODIUM CARBONATE AND SODIUM HYDROXIDE. Method I (continuous titration) (a) With phenolphthalein indicator, Na2CO3 undergoes half neutralization to form NaHCO3. The sodium hydroxide also reacts. The volume of the acid, V1 used is recorded. Na2CO3(aq) + HCl(aq) NaHCO3(aq) + NaCl(aq) V1 NaOH(aq) + HCl(aq) NaCl(aq) + H2O(l) (b) To the resultant solution in (a) is added a few drops of methyl orange indicator and the titration continued until the end point. The volume of the acid, V2, used is recorded. The formed NaHCO3 in (a) reacts with the acid. NaHCO3(aq) + HCl(aq) V2 NaCl(aq) + CO2(g) + H2O(l) (formed) The volume of the acid needed for the complete neutralization of Na2CO3 =2V2 The volume of the acid needed to react with NaOH alone =V1-V2 Method II (separate titration) (a) With phenolphthalein indicator, Na2CO3 undergoes half neutralization to form NaHCO3. The sodium hydroxide also reacts. The volume of the acid, V1 used is recorded. Na2CO3(aq) + HCl(aq) NaHCO3(aq) + NaCl(aq) V1 NaOH(aq) + HCl(aq) NaCl(aq) + H2O(l) (b) A fresh sample of the mixture is pipetted, a few drops of methyl orange indicator is added and then titrated with the acid until the end point. The volume of the acid, V2, used is recorded. Both the sodium carbonate and the sodium hydroxide react with the acid completely. Na2CO3(aq) + 2HCl(aq) 2NaCl(aq) + CO2(g) + H2O(l) V2 NaOH(aq) + HCl(aq) NaCl(aq) + H2O(l) The volume of the acid for half neutralization of Na2CO3 = V2 - V1 24 The volume of the acid for complete neutralization of Na2CO3 =2(V2 - V1) The volume of the acid that reacted with NaOH alone = V2 - 2(V2 - V1) = 2V1-V2 ANALYSIS OF A MIXTURE OF SODIUM HYDROGENCARBONATE AND SODIUM HYDROXIDE. Method I (continuous titration) (a) With phenolphthalein indicator, only NaOH reacts with the acid to reach the first end point. The volume of the acid, V1 used is recorded. NaOH(aq) + HCl(aq) V1 NaCl(aq) + H2O(l) (b) To the resultant solution in (a) is added a few drops of methyl orange indicator and the titration continued until the end point. The volume of the acid, V2, used is recorded. The NaHCO3 reacts with the acid. NaHCO3(aq) + HCl(aq) V2 NaCl(aq) + CO2(g) + H2O(l) (original) The volume of the acid needed for the complete neutralization of NaHCO3 =V2 The volume of the acid needed to react with NaOH alone =V1 Method II (separate titration) (a) With phenolphthalein indicator, only NaOH reacts with the acid to reach the first end point. The volume of the acid, V1 used is recorded. NaOH(aq) + HCl(aq) V1 NaCl(aq) + H2O(l) (b) A fresh sample of the mixture is pipetted, a few drops of methyl orange indicator is added and then titrated with the acid until the end point. The volume of the acid, V2, used is recorded. Both the sodium hydrogencarbonate and the sodium hydroxide react with the acid completely. NaHCO3(aq) + HCl(aq) NaCl(aq) + CO2(g) + H2O(l) V2 NaOH(aq) + HCl(aq) V1 NaCl(aq) + H2O(l) The volume of the acid needed to react with NaOH alone =V1 The volume of the acid for complete neutralization of NaHCO3 =V2 - V1 25 Experiment 10 You are provided with the following; FA1, which is 0.1M hydrochloric acid FA2, which is a solution containing sodium carbonate and sodium hydroxide. You are required to determine the molar concentration of sodium carbonate and sodium hydroxide. Procedure Pipette 20cm3 or 25cm3 of FA2 into a clean conical flask. Add 2-3 drops of phenolphthalein indicator and then titrate with FA1 from the burette until you reach the end point. Record your results in table I. Without pouring away the mixture, add 2-3 drops of methyl orange indicator and continue to titrate with FA1 from the burette until you reach the second end point. Record your results in table II. Repeat the titration 2-3 times until you obtain consistent results Note: The final reading with phenolphthalein indicator is the initial reading with methyl orange indicator. Results Volume of pipette used…………………………………..cm3 Table 1 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading(cm3) Volume of FA1 used(cm3) Titre values used for calculating average volume of FA1 used ………………………………………………………………………………………………………cm3. Average volume of FA1 used……………………………………………………………cm3 Table II Titration number 1 2 3 Final burette reading (cm3) Initial burette reading(cm3) Volume of FA1 used(cm3) Titre values used for calculating average volume of FA1 used ………………………………………………………………………………………………………cm3. 26 Average volume of FA1 used……………………………………………………………cm3 Questions; Calculate the molar concentration of; (a) Sodium carbonate solution in FA2. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (b) Sodium hydroxide solution in FA2. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… Experiment 11 You are provided with the following; FA1, which is a solution of hydrochloric acid. FA2, which is a solution containing sodium carbonate and sodium hydrogencarbonate. FA3, which is a solution containing 19.10g of borax, Na2B4O7.10H2O in 1dm3 of solution. You are required to standardize FA1 and use it to determine the composition of the mixture in FA2 Borax reacts with hydrochloric acid according to the equation: Na2B4O7.10 H2O(aq) + 2HCl(aq) 2NaCl(aq) + 4H3BO3(aq) + 5H2O(l) 27 Procedure I Pipette 20cm3 or 25cm3 of FA3 into a clean conical flask. Add 2-3 drops of methyl orange indicator and then titrate with FA1 from the burette until you reach the end point. Repeat the titration 2-3 times until you obtain consistent results. Record your results in the table I. Results Volume of pipette used=…………………………………..cm3 Table 1 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading(cm3) Volume of FA1 used(cm3) Titre values used for calculating average volume of FA2 used ………………………………………………………………………………………………………cm3. Average volume of FA2 used……………………………………………………………cm3 Questions; (a) Calculate the molar concentration of hydrochloric acid in FA1. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… Procedure II Pipette 20cm3 or 25cm3 of FA2 into a clean conical flask. Add 2-3 drops of phenolphthalein indicator and then titrate with FA1 from the burette until you reach the end point. Record your results in the appropriate section of table II (using phenolphthalein indicator). Without pouring away the mixture, add 2-3 drops of methyl orange indicator and titrate with FA1 from the burette until you reach the second end point. Record your results in the appropriate section table II (using methyl orange indicator). 28 Repeat the titration 2-3 times until you obtain consistent results Note: The final reading with phenolphthalein indicator is the initial reading with methyl orange indicator. Phenolphthalein indicator Methyl orange indicator Final burette reading (cm3) Initial burette reading (cm3) Volume of FA1 used (cm3) Titre values used to calculate average volume of FA1 using phenolphthalein indicator. …………………………………………………………………………………………………………………….. cm3 Average volume of FA1 used with phenolphthalein indicator ………………………… cm3 Titre values used to calculate average volume of FA1 using methyl orange indicator ……………………………………………………………………………………………………………………… cm3 Average volume of FA1 used with methyl orange indicator……………………………… cm3 Questions; (b) Calculate the concentration of; (i) Sodium carbonate solution in FA2 in grams per litre. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (ii) Sodium hydrogencarbonate solution in FA2 in grams per litre. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… 29 Experiment 12 You are provided with the following; FA1, which is 0.1M hydrochloric acid FA2, which is a solution containing sodium hydroxide and sodium hydrogencarbonate. You are required to determine the percentage composition of sodium hydroxide and sodium hydrogencarbonate. Procedure Pipette 20cm3 or 25cm3 of FA2 into a clean conical flask. Add 2-3 drops of phenolphthalein indicator and then titrate with FA1 from the burette until you reach the end point. Record your results in table I. Pipette another 20cm3 or 25cm3 of FA2 into a clean conical flask. Add 2-3 drops of methyl orange indicator and then titrate with FA1 from the burette until you reach the end point. Record your results in table II. Repeat the titration 2-3 times until you obtain consistent results Results Volume of pipette used…………………………………..cm3 Table 1 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading(cm3) Volume of FA1 used(cm3) Titre values used for calculating average volume of FA1 used ………………………………………………………………………………………………………cm3. Average volume of FA1 used …………………………………………………………………...cm3 Table II Titration number 1 2 3 Final burette reading (cm3) Initial burette reading(cm3) Volume of FA1 used(cm3) Titre values used for calculating average volume of FA1 used ………………………………………………………………………………………………………cm3 Average volume of FA1 used……………………………………………………………cm3 Questions; (a)Calculate the concentration of; 30 (i) Sodium hydroxide solution in FA2 in grams per litre. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (ii) Sodium hydrogencarbonate solution in FA2 in grams per litre. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (b) Calculate the percentage composition of sodium hydroxide and sodium hydrogencarbonate in the mixture. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… 31 Experiment 13 You are provided with the following; FA1, which is 0.1M sulphuric acid FA2, which is a solution containing sodium carbonate and sodium hydrogencarbonate. You are required to determine the composition of sodium carbonate and sodium hydrogencarbonate. Procedure Using a measuring cylinder, measure 100cm3 of FA2 into a 250cm3 volumetric flask and make it to the mark with more distilled water. Label the solution FA3 Pipette 20cm3 or 25cm3 of FA3 into a clean conical flask. Add 2-3 drops of phenolphthalein indicator and then titrate with FA1 from the burette until you reach the end point. Record your results in the appropriate section of table I (using phenolphthalein indicator). Pipette another 20cm3 or 25cm3 of FA3 into a clean beaker. Add 2-3 drops of methyl orange indicator and titrate with FA1 from the burette until you reach the second end point. Record your results in the appropriate section table I (using methyl orange indicator). Repeat the titration 2-3 times until you obtain consistent results Results Volume of pipette used…………………………………..cm3 Phenolphthalein indicator Methyl orange indicator (cm3) Final burette reading Initial burette reading (cm3) Volume of FA1 used (cm3) (i) Titre values used to calculate average volume of FA1 using phenolphthalein indicator. ………………………………………………………………………………………………………cm3 Average volume of FA1 used with phenolphthalein indicator ………………………… cm3 (ii) Titre values used to calculate average volume of FA1 using methyl orange indicator ………………………………………………………………………………………………………cm3 Average volume of FA1 used with methyl orange indicator……………………………… cm3 Questions; Calculate the concentration of; (i) Sodium carbonate solution in FA2 in grams per litre. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… 32 …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ……………………………………………………………………………………………………………………………... (ii) Sodium hydrogencarbonate solution in FA2 in grams per litre. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ……………………………………………………………………………………………………………………………... TRIAL QUESTIONS 1. 25cm3 of a solution containing a mixture of sodium carbonate and sodium hydrgencarbonate required 7.1cm3 of 0.1M hydrochloric acid using phenolphthalein indicator. Another 25cm3 of the solution needed 21.6cm3 of 0.1M hydrochloric acid using methyl orange indicator. Determine the percentage of each component in the mixture. 2. 25cm3 of a mixture containing sodium carbonate and sodium hydroxide required 27.1cm3 of 0.1M hydrochloric acid using phenolphthalein indicator. Without pouring away the solution, a further 8.3cm3 of 0.1M hydrochloric acid 33 was used using methyl orange indicator. Determine the concentration of each component in the mixture. 3. 25cm3 of a solution containing a mixture of sodium hydroxide and sodium hydrgencarbonate was diluted to 250cm3. 25cm3 of the diluted solution required 12.5cm3 of 0.1M hydrochloric acid using phenolphthalein indicator. Another 25cm3 of the diluted solution needed 32.4cm3 of 0.1M hydrochloric acid using methyl orange indicator. Determine the concentration of each component in the original undiluted solution. REDOX TITRATIONS. PERMANGANATE TITRATIONS. Experiment 15 You are provided with the following; FA1, which is a solution of potassium manganate(VII). 1M sulphuric acid Solid J, which is ammonium iron(II) sulphate-6-water, (NH4)2SO4FeSO4.6H2O You are required to determine the molar concentration of potassium managanate(VII) in FA1. Procedure. Weigh accurately about 4.9g of J and place it in a beaker. Add 100cm3 of water and carefully stir to dissolve. Transfer the contents of the beaker into a 250cm3 volumetric flask and add water to make up to the mark. Label the solution FA3. Pipette 20cm3 or 25cm3 of FA3 into a clean conical flask. Add an equal volume of 1M sulphuric acid and titrate with FA1 from the burette until the endpoint. Repeat the titration 2-3 times until you obtain consistent results. Enter your results in the table below. Results; Mass of empty bottle + J=……………………………………………..g Mass of empty bottle alone=………………………………………….g Mass of J alone=……………………………………………………………g Volume of pipette used=…………………………………………….cm3 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading (cm3) Volume of FA1 used (cm3) Titre values used to calculate average volume of FA1. ………………………………………………………………………………………………………cm3 Average volume of FA1 used …………………………………………………………..cm3 34 Questions; Calculate the molar concentration of FA1. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… Experiment 16 You are provided with the following; FA1, which is a solution of potassium manganate(VII). FA2, which is a solution containing 5.6g of sodium ethanedioate, Na2C2O4 per litre. 2M sulphuric acid Solid K, which is ammonium iron(II) sulphate-6-water, (NH4)2SO4FeSO4.nH2O You are required to standardize FA1 and use it to determine the value, n in (NH4)2SO4FeSO4.nH2O Procedure I Pipette 20cm3 or 25cm3 of FA2 into a clean conical flask. Add an equal volume of 2M sulphuric acid and heat the mixture to about 700C. Titrate the hot mixture with FA1 from the burette until you reach the end point. Repeat the titration 2-3 times until you obtain consistent results. Enter your results in the table below. Results Volume of pipette used…………………………………..cm3 Table 1 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading(cm3) Volume of FA1 used(cm3) 35 Titre values used for calculating average volume of FA1 used ……………………………………………………………………………………………………………...cm3 Average volume of FA1 used…………………………………………………………………...cm3 Questions; (a) Calculate the molar concentration of FA1. [Na=23, C=12, O=16] …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… Procedure I Weigh accurately about 4.4g of K and place it in a beaker. Add 100cm3 of water and carefully stir to dissolve. Transfer the contents of the beaker into a 250cm3 volumetric flask and add water to make up to the mark. Label the solution FA4. Pipette 20cm3 or 25cm3 of FA4 into a clean conical flask. Add an equal volume of 2M sulphuric acid and titrate with FA1 from the burette until the endpoint. Repeat the titration 2-3 times until you obtain consistent results. Enter your results in the table below. Results; Mass of empty bottle + K=……………………………………………..g Mass of empty bottle alone=………………………………………….g Mass of K alone=……………………………………………………………g Volume of pipette used=…………………………………………….cm3 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading (cm3) Volume of FA1 used (cm3) Titre values used to calculate average volume of FA1. ………………………………………………………………………………………………………cm3 Average volume of FA1 used …………………………………………………………..cm3 36 Questions; (b) Calculate the; (i) Molar concentration of iron(II) ions in FA4. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (ii) Molar mass of K and hence the value of n. [N=14, H=1, S=32, O=16, Fe=56] …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ………………………………………………………………………………………………………………………… Experiment 17 You are provided with the following; FA1, which is a solution of potassium manganate(VII). FA2, which is a 0.05M solution ammonium iron(II) sulphate-6water,(NH4)2SO4FeSO4.nH2O 2M sulphuric acid Solid L, which is an ethanedioate (oxalate) with the formula, CO2Y CO2Y You are required to standardize FA1 and use it to determine the relative atomic mass of Y. Procedure I Pipette 20cm3 or 25cm3 of FA2 into a clean conical flask. Add an equal volume of 2M sulphuric acid. Titrate the hot mixture with FA1 from the burette until you reach the end point. Repeat the titration 2-3 times until you obtain consistent results. Enter your results in the table below. Results Volume of pipette used…………………………………..cm3 37 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading(cm3) Volume of FA1 used(cm3) Titre values used for calculating average volume of FA1 used ………………………………………………………………………………………………………cm3 Average volume of FA1 used……………………………………………………………cm3 Questions; (a) Calculate the molar concentration of FA1. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… Procedure II Weigh accurately about 1.0g of L and place it in a beaker. Add 100cm3 of water and carefully stir to dissolve. Transfer the contents of the beaker into a 250cm3 volumetric flask and add water to make up to the mark. Label the solution FA4. Pipette 20cm3 or 25cm3 of FA4 into a clean conical flask. Add an equal volume of FA3 and heat the mixture to about 600C. Titrate the hot mixture with FA1 from the burette until the endpoint. Repeat the titration 2-3 times until you obtain consistent results. Enter your results in the table below. Results; Mass of empty bottle + L=……………………………………………..g Mass of empty bottle alone=………………………………………….g Mass of L alone=……………………………………………………………g Volume of pipette used=…………………………………………….cm3 38 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading (cm3) Volume of FA1 used (cm3) Titre values used to calculate average volume of FA1. ………………………………………………………………………………………………………cm3 Average volume of FA1 used …………………………………………………………..cm3 Questions; (b) Calculate the; (i) Number of moles oxalate ions in 250cm3 of FA4. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (ii) Molar mass of L. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (iii) Relative atomic mass of Y. [O=16, C=12] …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ……………………………………………………………………………………………………………………………. 39 Experiment 18 You are provided with the following; FA1, which is a 0.02M solution of potassium manganate(VII). FA2, which is a solution containing a mixture of sodium ethanedioate and ethanedioic acid. FA3, which is a 0.1M solution of sodium hydroxide. 2M sulphuric acid You are required to determine the percentage composition of sodium ethanedioate in FA2. Procedure I Pipette 20cm3 or 25cm3 of FA2 into a clean conical flask. Add 2-3 drops of phenolphthalein indicator and titrate with FA3 from the burette until you reach the end point. Repeat the titration 2-3 times until you obtain consistent results. Enter your results in the table below. Results Volume of pipette used…………………………………..cm3 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading(cm3) Volume of FA3 used(cm3) Titre values used for calculating average volume of FA3 used ………………………………………………………………………………………………………cm3. Average volume of FA3 used …………………………………………………………………...cm3 Procedure II Pipette 20cm3 or 25cm3 of FA2 into a clean conical flask. Add an equal volume of 2M sulphuric acid and heat the mixture to about 600C. Titrate the hot mixture with FA1 from the burette until the endpoint. Repeat the titration 2-3 times until you obtain consistent results. Enter your results in the table below. Volume of pipette used=…………………………………………….cm3 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading (cm3) Volume of FA1 used (cm3) Titre values used to calculate average volume of FA1. ………………………………………………………………………………………………………cm3 Average volume of FA1 used ………………………………………………… cm3 40 Questions; (a) Calculate the concentration of; (i) Ethanedioic acid in FA2 in grams per litre. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (ii) Sodium ethanedioate in FA2 in grams per litre. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (b) Calculate the percentage composition of sodium ethanedioate in FA2. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… 41 Experiment 19 You are provided with the following; FA1, which is a solution of potassium manganate(VII). FA2, which is a solution containing 2.8g of sodium oxalate, Na2C2O4 in 500cm3. FA3, which is a solution of ammonium iron(III) sulphate-24-water, (NH4)2SO4Fe2(SO4)3.24H2O 2M sulphuric acid. Zinc powder. You are required to standardize FA1 and use it to determine the percentage of iron in FA3. Procedure I Pipette 20cm3 or 25cm3 of FA2 into a clean conical flask. Add an equal volume of 2M sulphuric acid and heat the mixture to about 700C. Titrate the hot mixture with FA1 from the burette until you reach the end point. Repeat the titration 2-3 times until you obtain consistent results. Enter your results in the table below. Results Volume of pipette used…………………………………..cm3 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading(cm3) Volume of FA1 used(cm3) Titre values used for calculating average volume of FA1 used ………………………………………………………………………………………………………cm3. Average volume of FA1 used …………………………………………………………………...cm3 Questions; (a) Calculate the molar concentration of FA1. [Na=23, C=12, O=16] …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… 42 Procedure II Measure 100cm3 of FA3 using a measuring cylinder into a conical flask and add 3g of zinc powder followed by 5 cm3 of concentrated Sulphuric acid. Heat the mixture until a pale green solution is obtained and allow the mixture to cool. Label the solution FA5. Pipette 20cm3 or 25cm3 of FA5 into a clean conical flask. Add an equal volume of 2M sulphuric acid and titrate with FA1 from the burette until the endpoint. Repeat the titration 2-3 times until you obtain consistent results. Enter your results in the table below. Results; Volume of pipette used=…………………………………………….cm3 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading (cm3) Volume of FA1 used (cm3) Titre values used to calculate average volume of FA1. ………………………………………………………………………………………………………cm3 Average volume of FA1 used ………………………………………………… cm3 Questions; (b) Calculate the; (i) Concentration of iron(III) ions in FA3 in moles per litre. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (ii) Concentration of iron(III) ions in FA3 in grams per litre. .…………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… 43 …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ……………………………………………………………………………………………………………………………... (iii) The percentage of iron in FA3. [N=14, H=1, S=32, O=16, Fe=56] .…………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ……………………………………………………………………………………………………………………………... Experiment 20 You are provided with the following; FA1, which is a solution 2.41g of manganate(VII) ions per litre. FA2, which is a solution containing a mixture of ammonium iron(III) sulphate-24water, (NH4)2SO4Fe2(SO4)3.24H2O and ammonium iron(II) sulphate-6-water, (NH4)2SO4FeSO4.6H2O 2M sulphuric acid Zinc powder. You are required to determine the percentage of iron(III) in FA2. Procedure I Pipette 20cm3 or 25cm3 of FA2 into a clean conical flask. Add an equal volume of 2M sulphuric acid and titrate with FA1 from the burette until you reach the end point. Repeat the titration 2-3 times until you obtain consistent results. Enter your results in the table below. Volume of pipette used…………………………………..cm3 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading(cm3) Volume of FA1 used(cm3) Titre values used for calculating average volume of FA1 used ………………………………………………………………………………………………………cm3. Average volume of FA1 used…………………………………………………………...cm3 44 Procedure II Measure 100cm3 of FA2 using a measuring cylinder into a conical flask and add 3g of zinc powder followed by 5 cm3 of concentrated Sulphuric acid. Heat the mixture until a pale green solution is obtained and allow the mixture to cool. Label the solution FA4. Pipette 20cm3 or 25cm3 of FA4 into a clean conical flask. Add an equal volume of 2M sulphuric acid and titrate with FA1 from the burette until the endpoint. Repeat the titration 2-3 times until you obtain consistent results. Enter your results in the table below. Volume of pipette used=…………………………………………….cm3 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading (cm3) Volume of FA1 used (cm3) Titre values used to calculate average volume of FA1. ………………………………………………………………………………………………………cm3 Average volume of FA1 used ………………………………………………… cm3 Questions; (b)Calculate the; (i) Molar concentration of FA1. [Mn=55, O=16] …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (ii) Concentration of iron(II) ions in FA2 in moles per litre. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… 45 (iii) Concentration of iron(III) ions in FA2 in moles per litre. .…………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ……………………………………………………………………………………………………………………………... (iv) The percentage of iron(III) ions in FA2. [N=14, H=1, S=32, O=16, Fe=56] .…………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ……………………………………………………………………………………………………………………………... …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ……………………………………………………………………………………………………………………………... Experiment 21 You are provided with the following; FA1, which is 0.02M solution of potassium manganate(VII). FA2, which is a 0.08M solution of sodium hydroxide. 2M sulphuric acid Solid M, which is an oxalate with the formula, HX(C2O4)Y.nH2O You are required to determine the value of X, Y and n in compound M. Procedure I Weigh accurately about 1.6g of M and place it in a beaker. Add 100cm3 of water and carefully stir to dissolve. Transfer the contents of the beaker into a 250cm3 volumetric flask and add water to make up to the mark. Label the solution FA4. Pipette 20cm3 or 25cm3 of FA4 into a clean conical flask, add 2-3 drops of phenolphthalein indicator and titrate the hot mixture with FA2 from the burette until you reach the end point. Repeat the titration 2-3 times until you obtain consistent results. Enter your results in the table below. 46 Results; Mass of empty bottle + M=……………………………………………..g Mass of empty bottle alone=………………………………………….g Mass of M alone=……………………………………………………………g Volume of pipette used=…………………………………..cm3 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading(cm3) Volume of FA2 used(cm3) Titre values used for calculating average volume of FA2 used ………………………………………………………………………………………………………cm3 Average volume of FA2 used…………………………………………………………...cm3 Procedure I Pipette 20cm3 or 25cm3 of FA4 into a clean conical flask. Add an equal volume of 2M sulphuric acid and heat the mixture to about 600C. Titrate the hot mixture with FA1 from the burette until the endpoint. Repeat the titration 2-3 times until you obtain consistent results. Enter your results in the table below. Volume of pipette used=…………………………………………….cm3 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading (cm3) Volume of FA1 used (cm3) Titre values used to calculate average volume of FA1. ………………………………………………………………………………………………………cm3 Average volume of FA1 used …………………………………………………………..cm3 Questions; (a) Calculate the number of moles of; (i) Hydrogen ions per litre in FA4 that reacted with hydroxide ions in FA2. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… 47 …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (ii) Oxalate ions per litre in FA4 that reacted with manganate(VII) ions in FA1 …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (b) Determine the mole ratio of hydrogen ions to oxalate ions and hence the value of X and Y. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ……………………………………………………………………………………………………………………………... (c) Determine the molar mass of M and hence the value of n. [H=1, C=12, O=16] …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… 48 Experiment 22 You are provided with the following; FA1, which is a solution of potassium manganate(VII) of unkown concentration. FA2, which is a solution made by dissolving 2.016g of anhydrous sodium sulphite in 0.5dm3 of solution. FA3, which is a 0.3M ethanedioic acid solution. 2M sulphuric acid Solid N, which is a sample of pyrolusite. You are required to standardize FA1 and use it to determine the percentage of manganese(IV) oxide in pyrolusite. THEORY Pyrolusite is impure form of manganese(IV) oxide. When heated with excess ethanedioic acid, it reacts according to the following equation. MnO2(s) + H2C2O4(aq) + 2H+(aq) Mn2+(aq) + 2CO2(g) + 2H2O(l) Sulphite ions and oxalate ions react with manganate(VII) ions according to the equations; 2MnO4- (aq) + 5C2O42-(aq) + 16H+(aq) 2Mn2+(aq) + 10CO2(g) + 8H2O(l) 2MnO4- (aq) + 5SO32-(aq) + 6H+(aq) 2Mn2+(aq) + 5SO42- (aq) + 3H2O(l) Procedure I Pipette 20cm3 or 25cm3 of FA2 into a clean conical flask. Add an equal volume of 2M sulphuric acid and titrate with FA1 from the burette until you reach the end point. Repeat the titration 2-3 times until you obtain consistent results. Enter your results in the table below. Results Volume of pipette used…………………………………..cm3 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading(cm3) Volume of FA1 used(cm3) Titre values used for calculating average volume of FA1 used ………………………………………………………………………………………………………cm3 Average volume of FA1 used……………………………………………………………cm3 Questions; (a) Calculate the molar concentration of potassium manganate(VII) in FA1. (Na=23, S=32, O=16) 49 …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… Procedure II Weigh accurately about 0.2g of N and place it in a beaker. Add 100cm3 of FA3 and heat the mixture until it just dissolves. Cool the mixture and transfer the contents into a 250cm3 volumetric flask and add distilled water to make up to the mark. Label the solution FA4. Pipette 20cm3 or 25cm3 of FA4 into a clean conical flask. Add an equal volume of 2M Sulphuric acid and heat the mixture to about 700C. Titrate the hot mixture with FA1 from the burette until the endpoint. Repeat the titration 2-3 times until you obtain consistent results. Enter your results in the table below. Results; Mass of empty bottle + N=……………………………………………..g Mass of empty bottle alone=………………………………………….g Mass of N alone=……………………………………………………………g Volume of pipette used=…………………………………………….cm3 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading (cm3) Volume of FA1 used (cm3) Titre values used to calculate average volume of FA1. ………………………………………………………………………………………………………cm3 Average volume of FA1 used …………………………………………………………..cm3 Questions; (b) Calculate the Number of moles of; (i) Excess ethanedioic acid in FA4 that reacted with FA1. 50 …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (ii) Ethanedioic acid that reacted with the manganese(IV) oxide in the pyrolusite. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (iii) Percentage of manganese(IV) oxide in pyrolusite. [Mn=55, O=16] …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… Experiment 23 You are provided with the following; FA1, which is a solution of potassium manganate(VII). FA2, which is a solution of hydrogen peroxide Solid P, which is sodium ethanedioate. 2M Sulphuric acid You are required to standardize FA1 and use it to determine the volume strength of hydrogen peroxide in FA2. 51 Procedure I Weigh accurately about 1.3g of P. Add 100cm3 of water and carefully stir to dissolve. Transfer the contents into a 250cm3 volumetric flask and add water to make up to the mark. Label the solution FA3. Pipette 20cm3 or 25cm3 of FA3 into a clean conical flask. Add an equal volume of 2M Sulphuric acid and heat the mixture to about 600C. Titrate the hot mixture with FA1 from the burette until the endpoint. Repeat the titration 2-3 times until you obtain consistent results. Enter your results in the table below. Results; Mass of empty bottle + P=……………………………………………..g Mass of empty bottle alone=………………………………………….g Mass of P alone=……………………………………………………………g Volume of pipette used…………………………………..cm3 Table 1 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading(cm3) Volume of FA1 used(cm3) Titre values used for calculating average volume of FA1 used ………………………………………………………………………………………………………cm3 Average volume of FA1 used …………………………………………………………..cm3 Questions; (a) Calculate the molar concentration of FA1. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… 52 Procedure II Using a measuring cylinder, measure 10cm3 of FA2 into a 250cm3 volumetric flask and add distilled water to make up to the mark. Label the solution FA4. Pipette 10cm3 of FA4 into a clean conical flask. Add an equal volume of 2M Sulphuric acid and titrate with FA1 from the burette until the endpoint. Repeat the titration 2-3 times until you obtain consistent results. Enter your results in the table below. Volume of pipette used=…………………………………………….cm3 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading (cm3) Volume of FA1 used (cm3) Titre values used to calculate average volume of FA1. ………………………………………………………………………………………………………cm3 Average volume of FA1 used …………………………………………………………..cm3 Questions; (b) Calculate the; (i) Number of moles hydrogen peroxide in 250cm3 of FA4. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (ii) Concentration of hydrogen peroxide in moles per litre in FA2. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… 53 (iii) Volume strength of hydrogen peroxide in FA2. [1 mole of a gas occupies 22.4dm3 at s.t.p] …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… EXPERIMENT 24. You are provided with the following; FA1, which is a solution containing 3.16g of potassium manganate(VII) per litre of solution. FA2, which is a solution of diammonium iron(II) sulphate-6-water, (NH4)2SO4FeSO4.6H2O. Solid X, which is impure potassium chlorate(V), KClO3 2M Sulphuric acid. A thermometer. You are required to standardize FA2 and use it to determine the percentage purity of potassium chlorate(V) in solid X. THEORY. In acidic medium, chlorate(V) ions reacts with iron(II) ions according to the equation. ClO3-(aq) + 6H+(aq) + 6Fe2+(aq) 6Fe3+(aq) + Cl-(aq) + 3H2O(l) Procedure I Pipette 10cm3 of FA2 into a clean conical flask, add an equal volume of 2M Sulphuric acid and titrate the mixture with FA1 from the burette until the end point. Repeat the titration 2-3 times until you obtain consistent results. Enter your results in the table below. Results Volume of pipette used…………………………………..cm3 Table 1 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading(cm3) Volume of FA1 used(cm3) 54 Titre values used for calculating average volume of FA1 used ………………………………………………………………………………………………………cm3. Average volume of FA1 used …………………………………………………………………...cm3 Questions; (a) Calculate the molar concentration of diammonium iron(II) sulphate-6-water in FA2. (K=39, Mn=55, O=16) …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… Procedure II Weigh accurately about 0.5g of X and place it in a beaker. Add 100cm3 of water and carefully stir to dissolve. Transfer the contents of the beaker into a 250cm3 volumetric flask and make up the solution to the mark using distilled water. Label the solution FA3. Pipette 10cm3 of FA3 into a clean conical flask. Add 25cm3 of FA2 using a measuring cylinder followed by an equal volume of 2M Sulphuric acid. Heat the mixture to about 850C and then cool for about 3 minutes. Titrate the cold mixture with FA1 from the burette until the end point. Repeat the titration 2-3 times until you obtain consistent results. Enter your results in the table below. Results; Mass of empty bottle + X=……………………………………………..g Mass of empty bottle alone=………………………………………….g Mass of X alone=……………………………………………………………g Volume of pipette used=…………………………………………….cm3 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading (cm3) Volume of FA1 used (cm3) 55 Titre values used to calculate average volume of FA1. ………………………………………………………………………………………………………cm3 Average volume of FA1 used …………………………………………………………..cm3 Questions; (b) Calculate the number of moles of; (i) Excess iron(II) ions in FA1 that reacted with manganate(VII) ions. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ……………………………………………………………………………………………………………………………. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (ii) Iron(II) ions that reacted with 10cm3 of chlorate(V) ions in FA3. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ……………………………………………………………………………………………………………………………... …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (c) Determine the percentage purity of potassium chlorate(V) in solid X. (K=39, O=16, Cl=35.5) …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… 56 Experiment 25 You are provided with the following; FA1, which is approximately 0.02M potassium manganate(VII) solution. FA2, which is a solution of containing 5.2gdm-3 of a metal persuphate, molecular mass=270 Solid P, which is diammonium iron(II) sulphate-6-water, (NH4)2SO4FeSO4.6H2O 2M Sulphuric acid You are required to standardize FA1 and use it to determine the mole ratio for the reaction between aqueous iron(II) ions and the persulphate ions. Procedure I Weigh accurately about 6.0g of P. Dissolve it 150cm3 of 2M Sulphuric acid and transfer the contents into a 250cm3 volumetric flask and add water to make up to the mark. Label the solution FA3. Pipette 20cm3 or 25cm3 of FA3 into a clean conical flask and titrate with FA1 from the burette until the endpoint. Repeat the titration 2-3 times until you obtain consistent results. Enter your results in the table below. Results; Mass of empty bottle + P=……………………………………………..g Mass of empty bottle alone=………………………………………….g Mass of P alone=……………………………………………………………g Volume of pipette used…………………………………..cm3 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading(cm3) Volume of FA1 used(cm3) Titre values used for calculating average volume of FA1 used ……………………………………………………………………………………………………………….cm3 Average volume of FA1 used …………………………………………………………………...cm3 Questions; (a) Calculate the molar concentration of iron(II) ions in FA4. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… 57 (b) Determine the concentration of FA1 in moldm3. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… Procedure II Pipette 20cm3 or 25cm3 of FA3 into a clean conical flask followed by 10cm3 of 2M Sulphuric acid and titrate with FA1 from the burette until the endpoint. Repeat the titration 2-3 times until you obtain consistent results. Volume of pipette used=…………………………………………….cm3 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading (cm3) Volume of FA1 used (cm3) Titre values used to calculate average volume of FA1. ………………………………………………………………………………………………………cm3 Average volume of FA1 used ………………………………………………… cm3 Questions; (b) Calculate the number of moles of; (i) iron(II) ions that reacted with manganate(VII) ions in FA1. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (ii) iron(II) ions that reacted with persulphate ions. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… 58 (c) Determine the; (i) Number of moles of persulphate ions that reacted. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (ii) Reaction mole ratio between persulphate ions and iron(II) ions. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… EXPERIMENT 26. You are provided with the following; DA1 which Is 19.6g ammonium ferrous sulphate, (NH4)2SO4.FeSO4.6H2O in 500cm3 of solution. DA2 which is a solution of potassium manganate (VII) of unknown concentration Solid T which is an impure metal persulphate, YS2O8 (Y=24). 1M sulphuric acid solution You are required to determine; (i) The molar concentration of potassium manganate(VII) in DA2 (ii) The percentage of purity of YS2O8 in T. Procedure I Pipette 25cm3 (or 20cm3) of DA1 into a clean conical flask, then add 20cm3 of 1M sulphuric acid and titrate with solution DA2 from the burette until the end point. Repeat the titration 2-3 times until you obtain consistent results. Enter your results in the table below. Volume of pipette used = ……………………………………………………………….. cm3 Titration number 1 2 3 Final burette reading(cm3) Initial burette reading(cm3) Volume of DA2 used(cm3) 59 Titre values for calculating average volume of DA2. …………………………………………………………………………………………………………….. Average volume of DA2 …………………………………………………………………. Cm3 Questions (b) Calculate the molar concentration of manganate (VII) ions in DA2 (H = 1, N = 14, O = 16, S = 32, Fe = 56) …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………….. ……………………………………………………………………………………………..……………………………… ……………………………………………………………………………..……………………………………………… ……………………………………………………………..……………………………………………………………… ……………………………………………..……………………………………………………………………………… ……………………………..……………………………………………………………………………………………… ……………..…………………………………………………………………………………………………………….. ……………………………………………………………………………………………………………..……………… Procedure II Weigh accurately about 0.5g of solid T and place it in a beaker. Add to it about 50cm3 of water and stir to dissolve. Transfer the contents of a beaker into a 250cm3 volumetric flask. Add exactly 150cm3 of DA1 to the solution in a volumetric flask and top up with distilled water to the mark. Shake and allow to stand for 4-5 minutes. Label the resultant solution DA3. Pipette 25cm3 (or 20cm3) of DA3 into a clean conical flask followed by 10cm3 of 1M sulphuric acid and then titrate with DA2 from the burette until the end point. Repeat the titration 2-3 times to obtain consistent results. Enter your results in the table below. Mass of T + empty bottle = ……………………………………………. g Mass of empty bottle = ……………………………………………. g Mass of T alone = ……………………………………………. g Volume of pipette used = ………………………………………….. cm3 Titration number 1 2 3 Final burette reading(cm3) Initial burette reading(cm3) Volume of DA2 used(cm3) 60 Titre values for calculating average volume of DA2 ………………………………………………………………………………………………………….. cm3 Average volume of DA2 used ……………………………………………………………… cm3 Questions (b) Calculate the moles of; (i) Excess iron(II) ion that reacted with the MnO4- in DA2 …………………………………………………………………………………………………………….. …………………………………………………………………………………………………………….. …………………………………………………………………………………………………………….. …………………………………………………………………………………………………………….. …………………………………………………………………………………………………………….. …………………………………………………………………………………………………………….. …………………………………………………………………………………………………………….. …………………………………………………………………………………………………………….. (ii) Excess iron(II) ions contained in 250cm3 of DA3 …………………………………………………………………………………………………………….. …………………………………………………………………………………………………………….. …………………………………………………………………………………………………………….. …………………………………………………………………………………………………………….. …………………………………………………………………………………………………………….. …………………………………………………………………………………………………………….. (iii) Iron (II) ions that reacted with persulphate ions in T. …………………………………………………………………………………………………………….. …………………………………………………………………………………………………………….. …………………………………………………………………………………………………………….. …………………………………………………………………………………………………………….. …………………………………………………………………………………………………………….. 61 (c) Determine the percentage purity YS2O8 in T. …………………………………………………………………………………………………………….. …………………………………………………………………………………………………………….. …………………………………………………………………………………………………………….. …………………………………………………………………………………………………………….. …………………………………………………………………………………………………………….. …………………………………………………………………………………………………………….. …………………………………………………………………………………………………………….. …………………………………………………………………………………………………………….. THIOSULPHATE TITRATIONS. EXPERIMENT 27. You are provided with the following; FA1, which is a solution of iodine. Solid Q, which is sodium thiosulphate-5-water, Na2SO3.5H2O. You are required to standardize FA1 using sodium thiosulphate-5-water. Procedure Weigh accurately about 6.2g of Q and place it in a beaker. Add 100cm3 of water and carefully stir to dissolve. Transfer the contents of the beaker into a 250cm3 volumetric flask and add water to make up to the mark. Label the solution FA2. Pipette 20cm3 or 25cm3 of FA1 into a clean conical flask and titrate with FA2 from the burette until the solution just turns pale yellow. Add 2cm3 of starch indicator and continue titrating until the blue-black solution turns colourless. Repeat the titration 2-3 times until you obtain consistent results. Enter your results in the table below. Results; Mass of empty bottle + Q=……………………………………………..g Mass of empty bottle alone=………………………………………….g Mass of Q alone=……………………………………………………………g Volume of pipette used=…………………………………………….cm3 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading (cm3) Volume of FA2 used (cm3) 62 Titre values used to calculate average volume of FA2. ………………………………………………………………………………………………………cm3 Average volume of FA2 used ………………………………………………… cm3 Questions; Calculate the number of moles of; (i) Sodium thiosulphate in FA2 that reacted with FA1. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ……………………………………………………………………………………………………………………………. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (ii) Concentration of iodine in FA1 in grams per litre. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ………………………………………………………………………………………………………………………… EXPERIMENT 28. You are provided with the following; FA1, which is a solution of sodium thiosulphate. Solid T, which is potassium iodate, KIO3 2M Sulphuric acid. 10% potassium iodide. You are required to standardize FA1 using potassium iodate. Procedure. Weigh accurately about 0.9g of T and place it in a beaker. Add 100cm3 of water and carefully stir to dissolve. Transfer the contents of the beaker into a 250cm3 volumetric flask and add water to make up to the mark. Label the solution FA2. Pipette 20cm3 or 25cm3 of FA2 into a clean conical flask. Add an equal volume of 2M Sulphuric acid followed by 10cm3 of 10% potassium iodide solution and titrate the liberated iodine with FA1 from the burette until the solution just turns pale yellow. Add 2cm3 of starch indicator and continue titrating until the blue-black solution turns colourless. 63 Repeat the titration 2-3 times until you obtain consistent results. Enter your results in the table below. Results; Mass of empty bottle + T=……………………………………………..g Mass of empty bottle alone=………………………………………….g Mass of T alone=……………………………………………………………g Volume of pipette used=…………………………………………….cm3 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading (cm3) Volume of FA1 used (cm3) Titre values used to calculate average volume of FA1. ………………………………………………………………………………………………………cm3 Average volume of FA1 used …………………………………………………………..cm3 Questions; Calculate the concentration of; (i) Sodium thiosulphate in FA1 in moles per litre. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ……………………………………………………………………………………………………………………………. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ……………………………………………………………………………………………………………………………. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (ii) Sodium thiosulphate in FA1 in grams per litre. . …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ……………………………………………………………………………………………………………………………... 64 EXPERIMENT 29. You are provided with the following; FA1, which is a solution of sodium thiosulphate. FA2, which is a 0.02M solution of potassium manganate(VII). Solid U, which is copper(II) sulphate-5-water. 2M Sulphuric acid. 10% potassium iodide. You are required to standardize FA1 and use it to determine the percentage of copper in the sample U. Procedure I Pipette 20cm3 or 25cm3 of FA2 into a clean conical flask, add an equal volume of 2M Sulphuric acid followed by 10cm3 of 10% potassium iodide solution. Titrate the liberated iodine with FA1 from the burette until the solution just turns pale yellow. Add 2cm3 of starch indicator and continue titrating until the blue-black solution turns colourless. Repeat the titration 2-3 times until you obtain consistent results. Enter your results in the table below. Results Volume of pipette used…………………………………..cm3 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading(cm3) Volume of FA1 used(cm3) Titre values used for calculating average volume of FA1 used ………………………………………………………………………………………………………cm3. Average volume of FA1 used …………………………………………………………………...cm3 Questions; (a) Calculate the concentration of FA1 in moles per litre. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… 65 Procedure II Weigh accurately about 6.0g of U and place it in a beaker. Add 100cm3 of water and carefully stir to dissolve. Transfer the contents of the beaker into a 250cm3 volumetric flask. Add sodium carbonate solution drop-wise until a slight blue precipitate has formed and make up the solution to the mark using distilled water. Label the solution FA3. Pipette 20cm3 or 25cm3 of FA3 into a clean conical flask. Add 10cm3 of 10% potassium iodide solution and titrate the liberated iodine with FA1 from the burette until the solution just turns pale yellow. Add 2cm3 of starch indicator and continue titrating until the blue-black solution turns colourless. Repeat the titration 2-3 times until you obtain consistent results. Enter your results in the table below. Results; Mass of empty bottle + U=……………………………………………..g Mass of empty bottle alone=………………………………………….g Mass of U alone=……………………………………………………………g Volume of pipette used=…………………………………………….cm3 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading (cm3) Volume of FA1 used (cm3) Titre values used to calculate average volume of FA1. ………………………………………………………………………………………………………cm3 Average volume of FA1 used …………………………………………………………..cm3 Questions; (b) Calculate the number of moles of; (i) Iodine liberated by FA3. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ……………………………………………………………………………………………………………………………. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (ii) Copper(II) ions in FA3 in 250cm3. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… 66 …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ……………………………………………………………………………………………………………………………... (b) Determine the percentage of copper in U. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… EXPERIMENT 30. You are provided with the following; FA1, which is approximately a 0.1M solution of sodium thiosulphate. FA2, which is a solution containing 2.4gdm3 of potassium iodate. Solid V, which is a salt containing dichromate ions. 2M Sulphuric acid. 5% potassium iodide. Starch solution. You are required to standardize FA1 and use it to determine the percentage by mass of chromium in V. Procedure I Pipette 20cm3 or 25cm3 of FA2 into a clean conical flask, add an equal volume of 2M Sulphuric acid followed by 10cm3 of 5% potassium iodide solution. Titrate the liberated iodine with FA1 from the burette using starch indicator. Repeat the titration 2-3 times until you obtain consistent results. Enter your results in the table below. Results Volume of pipette used…………………………………..cm3 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading(cm3) Volume of FA1 used(cm3) Titre values used for calculating average volume of FA1 used ………………………………………………………………………………………………………cm3. Average volume of FA1 used …………………………………………………………………...cm3 67 Questions; (a) Calculate the number of moles of iodine liberated by FA2. (K=39, I=127, O=16) …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (b) Determine the concentration of FA1 in moles per dm3. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… Procedure II Weigh accurately about 1.2g of V and place it in a beaker. Add 100cm3 of water and carefully stir to dissolve. Transfer the contents of the beaker into a 250cm3 volumetric flask and make up the solution to the mark using distilled water. Label the solution FA3. Pipette 20cm3 or 25cm3 of FA3 into a clean conical flask, add an equal volume of 2M Sulphuric acid followed by 10cm3 of 5% potassium iodide solution. Titrate the liberated iodine with FA1 from the burette using starch indicator. Repeat the titration 2-3 times until you obtain consistent results. Enter your results in the table below. Results; Mass of empty bottle + V=……………………………………………..g Mass of empty bottle alone=………………………………………….g Mass of V alone=……………………………………………………………g Volume of pipette used=…………………………………………….cm3 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading (cm3) Volume of FA1 used (cm3) 68 Titre values used to calculate average volume of FA1. ………………………………………………………………………………………………………cm3 Average volume of FA1 used …………………………………………………………..cm3 Questions; (c) Calculate the number of moles of iodine liberated by FA3. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ……………………………………………………………………………………………………………………………. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (d) Determine the; (i) Concentration of FA3 in moles per dm3. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ……………………………………………………………………………………………………………………………... (ii) Mass of chromium in V and hence its percentage. (Cr = 52) …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… 69 EXPERIMENT 31. You are provided with the following; FA1, which is a solution of sodium thiosulphate. FA2, which is a solution containing 2.0g of potassium dichromate(V) in 500cm3 of solution. Solid W, which is potassium halate(V), KYO3. 2M Sulphuric acid. 10% potassium iodide. Starch solution. You are required to standardize FA1 and use it to determine the relative atomic mass of element Y in W. Procedure I Pipette 20cm3 or 25cm3 of FA2 into a clean conical flask, add an equal volume of 2M Sulphuric acid followed by 10cm3 of 10% potassium iodide solution. Titrate the liberated iodine with FA1 from the burette using starch indicator. Repeat the titration 2-3 times until you obtain consistent results. Enter your results in the table below. Results Volume of pipette used…………………………………..cm3 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading(cm3) Volume of FA1 used(cm3) Titre values used for calculating average volume of FA1 used ………………………………………………………………………………………………………cm3. Average volume of FA1 used …………………………………………………………………...cm3 Questions; (a) Calculate the concentration of FA1 in moles per litre. (K=39, Cr=52, O=16) …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… 70 Procedure II Weigh accurately about 1.0g of W and place it in a beaker. Add 100cm3 of water and carefully stir to dissolve. Transfer the contents of the beaker into a 250cm3 volumetric flask and make up the solution to the mark using distilled water. Label the solution FA3. Pipette 20cm3 or 25cm3 of FA3 into a clean conical flask, add an equal volume of 2M Sulphuric acid followed by 10cm3 of 10% potassium iodide solution. Titrate the liberated iodine with FA1 from the burette using starch indicator. Repeat the titration 2-3 times until you obtain consistent results. Enter your results in the table below. Results; Mass of empty bottle + W=……………………………………………..g Mass of empty bottle alone=………………………………………….g Mass of W alone=……………………………………………………………g Volume of pipette used=…………………………………………….cm3 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading (cm3) Volume of FA1 used (cm3) Titre values used to calculate average volume of FA1. ………………………………………………………………………………………………………cm3 Average volume of FA1 used ………………………………………………… cm3 Questions; (b) Calculate the number of moles of iodine liberated by FA3. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ……………………………………………………………………………………………………………………………. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (c) Determine the; (i) Concentration of FA3 in moles per dm3. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… 71 (ii) Relative molecular mass of V and hence the relative atomic mass of Y in KYO3. (K=39, O=16) …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… EXPERIMENT 32. You are provided with the following; FA1, which is approximately a 0.1M solution of sodium thiosulphate. FA2, which is a solution containing 2.41g of manganate(VII) ions per litre. FA3, which is a solution of hydrogen peroxide. 2M Sulphuric acid. 10% potassium iodide. You are required to standardize FA1 and use it to determine the concentration of hydrogen peroxide in FA3. Procedure I Pipette 20cm3 or 25cm3 of FA2 into a clean conical flask, add an equal volume of 2M Sulphuric acid followed by 10cm3 of 10% potassium iodide solution. Titrate the liberated iodine with FA1 from the burette until the solution just turns pale yellow. Add 2cm3 of starch indicator and continue titrating until the blue-black solution turns colourless. Repeat the titration 2-3 times until you obtain consistent results. Enter your results in the table below. Results Volume of pipette used…………………………………..cm3 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading(cm3) Volume of FA1 used(cm3) Titre values used for calculating average volume of FA1 used ………………………………………………………………………………………………………cm3. Average volume of FA1 used …………………………………………………………………...cm3 72 Questions; (a) Calculate the concentration of FA1 in moles per litre. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… Procedure II Using a measuring cylinder, measure 10cm3 of FA3 into a 250cm3 volumetric flask and add distilled water to make up to the mark. Label the solution FA4. Pipette 20cm3 or 25cm3 of FA4 into a clean conical flask. Add an equal volume of 2M Sulphuric acid followed by 10cm3 of 10% potassium iodide solution and titrate the liberated iodine with FA1 from the burette until the solution just turns pale yellow. Add 2cm3 of starch indicator and continue titrating until the blue-black solution turns colourless. Repeat the titration 2-3 times until you obtain consistent results. Enter your results in the table below. Results; Volume of pipette used=…………………………………………….cm3 Titration number 1 2 Final burette reading (cm3) Initial burette reading (cm3) Volume of FA1 used (cm3) Titre values used to calculate average volume of FA1. ………………………………………………………………………………………………………cm3 Average volume of FA1 used …………………………………………………………..cm3 Questions; (b) Calculate the; (i) Number of moles hydrogen peroxide in 250cm3 of FA4. 73 3 …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (ii) Concentration of hydrogen peroxide in moles per litre in FA3. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (iii) Volume strength of hydrogen peroxide in FA3. [1 mole of a gas occupies 22.4dm3 at s.t.p] …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… EXPERIMENT 33. You are provided with the following; FA1, which is approximately a 0.1M solution of sodium thiosulphate. FA2, which is a solution prepared by dissolving 1.0g of potassium iodate in 250cm3 of distilled water. Liquid X, which is a commercial bleaching agent containing sodium hypochlorite. FA3; which is 0.5M potassium iodide. 2M Sulphuric acid. You are required to standardize FA1 and use it to determine the percentage of chlorine in the commercial bleaching agent. 74 THEORY In acidic medium, iodate ions react with iodide ions according to the equation; IO3-(aq) + 6H+(aq) + 5I-(aq) 3I2(aq) + 5H2O(l) In acidic medium, hypochlorite ions produce chlorine according to the equation; Cl-(aq) + OCl-(aq) + 2H+(aq) H2O(l) + Cl2(g) The chlorine produced displaces iodine from potassium iodide according to the equation; Cl2(g) + 2I-(aq) I2(aq) + 2Cl-(aq) The iodine liberated in both cases reacts with thiosulphate ions according to the equation; I2(g) + 2S2O32-(aq) 2I-(aq) + S4O62-(aq) Procedure I Pipette 10cm3 of FA2 into a clean conical flask, add an equal volume of 2M Sulphuric acid followed by 10cm3 of FA3. Titrate the liberated iodine with FA1 from the burette until the solution just turns pale yellow. Add 2cm3 of starch indicator and continue titrating until the blue-black solution turns colourless. Repeat the titration 2-3 times until you obtain consistent results. Enter your results in the table below. Results Volume of pipette used…………………………………..cm3 Table 1 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading(cm3) Volume of FA1 used(cm3) Titre values used for calculating average volume of FA1 used ………………………………………………………………………………………………………cm3. Average volume of FA1 used …………………………………………………………………...cm3 Questions; (a) Calculate the concentration of FA1 in moles per litre. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… 75 Procedure II Using a measuring cylinder, measure 30cm3 of liquid X into a 250cm3 volumetric flask and add distilled water to make up to the mark. Label the solution FA5. Pipette 10cm3 of FA5 into a clean conical flask. Add an equal volume of 2M Sulphuric acid followed by 10cm3 of FA3 and titrate the liberated iodine with FA1 from the burette until the solution just turns pale yellow. Add 2cm3 of starch indicator and continue titrating until the blue-black solution turns colourless. Repeat the titration 2-3 times until you obtain consistent results. Enter your results in the table below. Results; Volume of pipette used=…………………………………………….cm3 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading (cm3) Volume of FA1 used (cm3) Titre values used to calculate average volume of FA1. ………………………………………………………………………………………………………cm3 Average volume of FA1 used ………………………………………………… cm3 Questions; (b) Calculate the; (i) Number of moles sodium thiosulphate in FA1 that reacted. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (ii) Number of moles of iodine liberated by 10cm3 of FA5. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (iii) Number of moles of chlorine in 30cm3 of X. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… 76 (iv)The mass of chlorine in 30cm3 of X. (Cl=35.5) …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (V) The percentage by mass of chlorine in X. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… EXPERIMENT 34. You are provided with the following; FA1, which is a solution of sodium thiosulphate. FA2, which is a solution containing 2.94g of dichromate(V) ions per litre. Solid Y, which is calcium hypochlorite (bleaching powder). 2M Sulphuric acid. 2M Ethanoic acid. 10% potassium iodide. Starch indicator. You are required to standardize FA1 and use it to determine the relative atomic mass of element Y in W. THEORY In acidic medium, dichromate(VI) ions react with iodide ions according to the equation; Cr2O72-(aq) + 14H+(aq) + 6I-(aq) 2Cr3+(aq) + 3I2(aq) + 7H2O(l) In acidic medium, hypochlorite ions produce chlorine according to the equation; Cl-(aq) + OCl-(aq) + 2H+(aq) H2O(l) + Cl2(g) The chlorine produced displaces iodine from potassium iodide according to the equation; Cl2(g) + 2I-(aq) I2(aq) + 2Cl-(aq) The iodine liberated in both cases reacts with thiosulphate ions according to the equation; I2(aq) + 2S2O32-(aq) 2I-(aq) + S4O62-(aq) Procedure I Pipette 20cm3 or 25cm3 of FA2 into a clean conical flask, add an equal volume of 2M Sulphuric acid followed by 10cm3 of 10% potassium iodide solution. Titrate the liberated iodine with FA1 from the burette using starch indicator. Repeat the titration 2-3 times until you obtain consistent results. Enter your results in the table below. 77 Results Volume of pipette used…………………………………..cm3 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading(cm3) Volume of FA1 used(cm3) Titre values used for calculating average volume of FA1 used ………………………………………………………………………………………………………cm3. Average volume of FA1 used …………………………………………………………………...cm3 Questions; (a) Calculate the concentration of FA1 in moles per litre. (Cr=52, O=16) …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… Procedure II Weigh accurately about 1.3g of Y and place it into a clean beaker, add little water and grind to form a thin paste. Add more little water and carefully pour the milky liquid into a 250cm3 volumetric flask and make up the solution to the mark using distilled water. Label the solution FA3. Pipette 20cm3 or 25cm3 of FA3 into a clean conical flask, add an equal volume of 2M ethanoic acid followed by 10cm3 of 10% potassium iodide solution. Titrate the liberated iodine with FA1 from the burette using starch indicator. Repeat the titration 2-3 times until you obtain consistent results. Enter your results in the table below. Results; Mass of empty bottle + Y=……………………………………………..g Mass of empty bottle alone=………………………………………….g Mass of Y alone=……………………………………………………………g 78 Volume of pipette used=…………………………………………….cm3 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading (cm3) Volume of FA1 used (cm3) Titre values used to calculate average volume of FA1. ………………………………………………………………………………………………………cm3 Average volume of FA1 used …………………………………………………………..cm3 Questions; (b) Calculate the (i) Number of moles of iodine liberated. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ……………………………………………………………………………………………………………………………. …………………………………………………………………………………………………………………………… (ii) Concentration of chlorine in FA3 in moles per dm3. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ……………………………………………………………………………………………………………………………... (iii) Mass of chlorine and hence the percentage of chlorine in Y. (Cl=35.5) …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… 79 EXPERIMENT 35. You are provided with the following; FA1, which is a solution of sodium thiosulphate. FA2, which is a solution containing 10.7g of a mixture of potassium iodate and potassium iodide per litre. Solid Y, which is potassium manganate(VII) crystals. 2M Sulphuric acid. O.5M potassium iodide solution. Starch indicator. You are required to standardize FA1 and use it to determine the percentage of potassium iodate in FA2. Procedure I Weigh accurately about 0.8g of Y and place it into a clean beaker, add little water to dissolve and transfer the contents into a 250cm3 volumetric flask and make up the solution to the mark using distilled water. Label the solution FA3. Pipette 20cm3 or 25cm3 of FA3 into a clean conical flask, add an equal volume of 2M Sulphuric acid followed by 10cm3 of 0.5M potassium iodide solution. Titrate the liberated iodine with FA1 from the burette using starch indicator. Repeat the titration 2-3 times until you obtain consistent results. Enter your results in the table below. Results Mass of empty bottle + Y=……………………………………………..g Mass of empty bottle alone=………………………………………….g Mass of Y alone=……………………………………………………………g Volume of pipette used…………………………………..cm3 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading(cm3) Volume of FA1 used(cm3) Titre values used for calculating average volume of FA1 used …………………………………………………………………………………………………………………..cm3 Average volume of FA1 used …………………………………………………………………...cm3 Questions; (a) Calculate the concentration of FA1 in moles per litre. (K=39, Mn=55, O=16) …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… 80 …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… Procedure II Pipette 20cm3 or 25cm3 of FA2 into a clean conical flask, add an equal volume of 2M ethanoic acid followed by 10cm3 of 0.5M potassium iodide solution. Titrate the liberated iodine with FA1 from the burette using starch indicator. Repeat the titration 2-3 times until you obtain consistent results. Enter your results in the table below. Results; Volume of pipette used=…………………………………………….cm3 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading (cm3) Volume of FA1 used (cm3) Titre values used to calculate average volume of FA1. ………………………………………………………………………………………………………cm3 Average volume of FA1 used …………………………………………………………..cm3 Questions; (b) Calculate the (i) Number of moles of iodine liberated. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ……………………………………………………………………………………………………………………………. …………………………………………………………………………………………………………………………… (ii) Concentration of potassium iodate in FA2 in moles per dm3. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… 81 …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ……………………………………………………………………………………………………………………………... (iii) Percentage of potassium iodate in FA2. (K=39, I=127, 0=16) …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… EXPERIMENT 36. You are provided with the following; FA1, which is a solution of iodine. FA2, which is a 0.1M solution of sodium thiosulphate. Solid R, which is a reducing agent of molecular mass 126. Solid S *NaHCO3 You are required to standardize FA1 and use it to determine the mole ratio for the reaction between iodine and R. Procedure I Pipette 10cm3 of FA1 into a clean conical flask and titrate with FA2 from the burette using starch indicator. Repeat the titration 2-3 times until you obtain consistent results. Enter your results in the table below. Results Volume of pipette used…………………………………..cm3 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading(cm3) Volume of FA2 used(cm3) Titre values used for calculating average volume of FA2 used ………………………………………………………………………………………………………………….cm3 Average volume of FA2 used …………………………………………………………………...cm3 82 Questions; (a) Calculate the concentration of iodine in moles per litre of FA1. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… Procedure II Weigh accurately about 1.6g of R and place it in a beaker. Add 100cm3 of distilled water and carefully stir to dissolve. Transfer the contents of the beaker into a 250cm3 volumetric flask and add water to make up to the mark. Label the solution FA3. Pipette 10cm3 of FA3 into a clean conical flask. Add 20cm3 of FA1 using a measuring cylinder followed by two spatula end-fuls of solid S and shake the mixture well. Titrate the excess iodine in the mixture with FA2 from the burette using starch indicator. Repeat the titration 2-3 times until you obtain consistent results. Enter your results in the table below. Results; Mass of empty bottle + R=……………………………………………..g Mass of empty bottle alone=………………………………………….g Mass of R alone=……………………………………………………………g Volume of pipette used=…………………………………………….cm3 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading (cm3) Volume of FA2 used (cm3) Titre values used to calculate average volume of FA2. ………………………………………………………………………………………………………cm3 Average volume of FA2 used …………………………………………………………..cm3 Questions; (b) Calculate the number of moles of; 83 (i) Excess iodine in FA1 that reacted with the thiosulphate ions in FA2. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ……………………………………………………………………………………………………………………………. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (ii) Iodine that reacted with X. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ……………………………………………………………………………………………………………………………... (c) Determine the; (i) The number of moles of X that reacted. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ……………………………………………………………………………………………………………………………. (ii) Reaction mole ratio of X and iodine. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… 84 PHYSICAL CHEMISTRY PRACTICALS COLLIGATIVE PROPERTIES Experiment 37 You are provided with the following; Naphthalene (C10H8) Camphor (C10H16O) A thermometer. You are required to determine the freezing point constant, Kf per kg of naphthalene. Procedure. (a) Pour 200cm3 of water into a 250cm3 beaker. Heat the water to boiling point on a tripod stand. Weigh separately and accurately about 5.0g of naphthalene and 1.0g of camphor. Record the results in the spaces provided below. Results. Mass of container + Naphthalene = ……………………………………………………..g Mass of empty container = ……………………………………………………..g Mass of naphthalene = ……………………………………………………..g Mass of container + Camphor = ……………………………………………………..g Mass of empty container = ……………………………………………………..g Mass of Camphor = ……………………………………………………..g (b) Transfer the whole of naphthalene into a clean dry boiling tube. Immerse the boiling tube containing naphthalene into the beaker of hot water and continue heating the water until the whole naphthalene melts. Insert a thermometer in the liquid formed and heat to about 890C. Remove the boiling tube from the hot water and start a stop clock when its temperature drops to 850C. Allow the liquid to cool while stirring with a thermometer and record its temperature after every half a minute for three minutes. Enter your results in the table below. (c) Transfer the whole of camphor into a boiling tube containing naphthalene. Immerse the boiling tube into the beaker of hot water and continue heating the water until the mixture melts. Continue heating until the temperature of the molten mixture is about 890C. Remove the boiling tube from the hot water and start a stop clock when its temperature of the mixture drops to 850C. Allow the mixture to cool while stirring with a thermometer and record its temperature after every half a minute for three minutes. Enter your results in the table below. Time (minutes) 0.0 0.5 1.0 1.5 2.0 2.5 3.0 Temperature of naphthalene(0C) Temperature of mixture of naphthalene and camphor (0C) Questions: (a) Plot on the same axes, a graph of temperature; 85 (i) Pure naphthalene against time. (ii) Mixture of naphthalene and camphor against time. (b) From the graphs, read off the temperature after 2.5 minutes of; (i) Pure naphthalene. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (ii) Mixture of naphthalene and camphor. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………...... (c) Use the temperatures you have obtained in (b) above to determine the depression in freezing point of naphthalene. …………………………………………………………………………………………………………………………… ……………………………………………………………………………………………………………………………... (d) Calculate the freezing point depression constant, Kf per kg of naphthalene. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ……………………………………………………………………………………………………………………………... 86 87 Experiment 38. You are provided with the following; Naphthalene Camphor A thermometer. You are required to determine the relative molecular mass of camphor using freezing point depression method. Procedure. Weigh accurately about 5.0g of naphthalene into a dry boiling tube, then insert a thermometer into the tube. Put the boiling tube and its contents in a beaker of boiling water. Stir continuously with a thermometer until the whole solid melts. Remove the beaker of boiling water from the heat source while keeping the boiling tube in the water and allow the melted solid to cool while stirring gently with a thermometer. Record the steady temperature, T10C when the crystals start to appear. Weigh accurately about 1.0g of camphor, carefully add it to naphthalene in the boiling tube. Put back the boiling tube into a beaker of boiling water. Stir continuously with a thermometer until the whole mixture melts. Remove the beaker of boiling water from the heat source while keeping the boiling tube in the water and allow the melted mixture to cool while stirring gently with a thermometer. Record the steady temperature, T20C when the crystals start to appear. Record your results in the spaces below. Results. Mass of naphthalene used = ………………………………………..g Mass of camphor used = ………………………………………..g Freezing point of naphthalene = ………………………………….g Freezing point of the mixture = …………………………………..g Questions: Calculate the; (a) Freezing point depression, T30C …………………………………………………………………………………………………………………………… ……………………………………………………………………………………………………………………………... (b) Relative molecular mass of camphor given that the freezing point constant of naphthalene is 6.90C/mol/kg …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… 88 89 THERMOCHEMISTRY Experiment 39 You are provided with the following: FA1, which is a solution of hydrochloric acid. Metal X Substance Y, which is an oxide of X, with a formula XO You are required to determine the enthalpy change for the reduction of the oxide of X and comment on your answer. PART I Procedure: Weigh accurately about 1.2g of X. Using a measuring cylinder, transfer 100cm3 of FA1 into a plastic beaker. Read and record its initial temperature, in the table I. Add at once the 1.2g of X into FA1 into the plastic beaker and at the same time start the stop clock or watch. Stir gently with the thermometer and record the temperature of the solution after every half-minute in table I, up to the four minute. Results Mass of the weighing container + X = …………………………… g Mass of the weighing container alone = …………………………… g Mass of X used = ……………………........... g Table I Time (minutes) 0 ½ 1 1½ 2 2½ 3 3½ 4 Temperature of solution (0C) PART II Procedure Weigh accurately about 2.0g of Y. Using a measuring cylinder, transfer 100cm3 of FA1 into a plastic beaker. Read and record its initial temperature, in the table II. Add at once the 2.0g of Y into FA1 into the plastic beaker and at the same time start the stop clock or watch. Stir gently with the thermometer and record the temperature of the solution after every half-minute in table II, up to the four minute. Results Mass of the weighing container + Y = …………………………… g Mass of the weighing container alone = …………………………… g Mass of Y used = ……………………........... g Table II Time (minutes) 0 ½ 1 1½ 2 2½ 3 3½ 4 Temperature of solution (0C) 90 (a) (i) Plot on the same axes, graphs of temperature against time for results obtained in both Part I and Part II. (ii) From your graphs, determine the maximum temperature change for the reaction. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (iii) Calculate the heat of reaction in Part I and Part II. [Specific heat capacity of the solution=4.2 Jg-1K-1 and its density=1gcm-3 in each case, equations of the reactions of X and Y are as follows] X(s) + 2HCl(aq) XCl2(aq) + H2(g) XO(s)+ 2HCl(aq) XCl2(aq) + H2O(l) Part I …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… Part II …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (iv) Calculate the molar heat of reactions in Part I and Part II. [X=24, O=16] …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… 91 …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ……………………………………………………………………………………………………………………………... (b) Determine the heat energy change for the reaction. XO(s) + H2 (g) X(s) + H2O(l) …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (c) Comment on your answer in (b). …………………………………………………………………………………………………………………………… ……………………………………………………………………………………………………………………………... 92 93 Experiment 40 You are provided with the following; FA1; which is 2M sodium hydroxide solution FA2; which is 2M solution of a strong acid You are required to determine the basicity and heat of neutralization of the acid in FA2 Procedure. Pour 50cm3 of FA2 into a plastic beaker using a measuring cylinder. Using the same measuring cylinder, add 10cm3 of water to the plastic beaker. Stir and record the temperature of the mixture, T10C in the table below. Using a clean measuring cylinder, measure 60cm3 of FA1 into another plastic beaker and record its temperature, T20C in the table below. Pour the 60cm3 of FA1 into the plastic beaker containing FA2 and stir gently with a thermometer. Record the maximum temperature of the mixture, T30C. Repeat the procedures above with different volumes of water, FA1 and FA2 given in the table below. Make sure the plastic beakers and the thermometer used between each experiment is rinsed. Record your results in the table below. Experiment number 1 2 3 4 5 6 7 8 Volume of FA2 (cm3) 50 40 35 30 25 20 15 10 Volume of water (cm3) 10 20 25 30 35 40 45 50 Volume of FA1 (cm3) 60 60 60 60 60 60 60 60 Temperature, T1 (0C) Temperature, T2 (0C) Average temperature, 𝑇1 + 𝑇2 0 ( C) 2 Maximum temperature, T3 (0C) Temperature rise, T3 - 𝑇1 + 𝑇2 2 (0C) Questions 94 (a) Plot a graph of temperature rise against volume of FA2 used. (b) From the graph, determine the; (i) Maximum temperature rise …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (ii) Volume of FA2 required to produce the maximum temperature rise. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (c) Calculate the number of moles of the; (i) Acid in FA2 that completely reacted with sodium hydroxide in FA1. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (ii) Sodium hydroxide in FA1 that completely reacted with the acid in FA2. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (d) Calculate the basicity of the acid. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (e) Calculate the heat of neutralization of the acid. (Specific heat capacity of solution is 4.2j/g/0C and the density of solution is 1gcm-3) 95 …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ………………………………………………………………………………………………..…………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ……………………………………………………………………………………………………………………………... 96 97 Experiment 41 You are provided with the following; FA1; which is 0.25M copper(II) sulphate solution. Solid X, which is zinc powder. You are required to determine the heat of displacement of copper(II) sulphate solution using zinc. Procedure Weigh roughly 1.3g of X. Place 50cm3 of FA1 into a plastic beaker and record the temperature of the solution every minute for four minutes. On exactly the fifth minute, add solid X to the solution and stir continuously with the thermometer. Record the temperature after every minute until 11 minutes. Record your results in the table below. Results Mass of the weighing container + X = …………………………… g Mass of the weighing container alone = …………………………… g Mass of X used = ……………………........... g Table Time (min) 0 1 2 3 4 5 6 7 8 9 10 11 Temperature (0C) (a) Plot a graph of temperature against time. (b) From the graph, determine the; (i) Experimental (observed) temperature rise. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (ii) Corrected (theoretical) temperature rise. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (c) Hence calculate the; (i) Experimental enthalpy of displacement of copper(II) sulphate solution. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ………………………………………………………………………………………………..…………………………… …………………………………………………………………………………………………………………………… 98 (ii) Heat of displacement of copper(II) sulphate solution using the corrected temperature rise. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ………………………………………………………………………………………………..…………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ………………………………………………………………………………………………........................................... 99 100 PARTITION COEFFICIENT Experiment 42 You are provided with the following; FA1, which is 1.5M aqueous ammonia. FA2, which is trichloromethane FA3, which is 0.5M hydrochloric acid. FA4, which is 0.05M hydrochloric acid. You are required to determine the partition coefficient of ammonia between water and trichloromethane. Procedure. Add 50cm3 of FA1 to 50cm3 of FA2 in a conical flask. Shake vigorously for about 5 minutes and allow to stand for about 10 minutes. Carefully decant the upper (aqueous) layer into a beaker. Transfer the lower (organic) layer into another beaker and cover. Read and record the room temperature. Pipette 10cm3 of the aqueous layer into a conical flask, add 2-3 drops of methyl orange indicator and titrate with FA3 from the burette. Repeat the titration 2-3 times to obtain consistent results. Record your results in table I below. Results Room temperature = …………………………………………………………………………..0C Volume of pipette used=……………………………………………………………………... cm3 Table I Titration number 1 2 3 Final burette reading (cm3) Initial burette reading(cm3) Volume of FA3 used(cm3) Titre values used for calculating average volume of FA3 used ………………………………………………………………………………………………………cm3 Average volume of FA3 used …………………………………………………………………...cm3 Pipette 10cm3 of the organic layer into a conical flask, add 2-3 drops of methyl orange indicator and titrate with FA4 from the burette. Repeat the titration 2-3 times to obtain consistent results. Record your results in table II below. Results Volume of pipette used=…………………………………………….cm3 Table II 101 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading(cm3) Volume of FA4 used(cm3) Titre values used for calculating average volume of FA4 used ………………………………………………………………………………………………………cm3 Average volume of FA4 used …………………………………………………………………...cm3 Questions (a) Calculate the; (i) Molar concentration of ammonia in the aqueous layer. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ………………………………………………………………………………………………..…………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………..………………………………………………………… …………………………………………………………………………………………………………………………… ………………………………………………………………………………………………………………….. (ii) Molar concentration of ammonia in the organic layer. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ………………………………………………………………………………………………..…………………………… …………………………………………………………………………………………………………………………… 102 …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………..………………………………………………………… …………………………………………………………………………………………………………………………… ……………………………………………………………………………………………………………………………. (b) Determine the value of the distribution coefficient of ammonia between water and trichloromethane at the temperature you have recorded. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ………………………………………………………………………………………………..…………………………… …………………………………………………………………………………………………………………………… ………………………………………………………………....................................................................................... Experiment 43 You are provided with the following; FA1, which is 0.5M sodium thiosulphate solution. FA2, which is 0.005M sodium thiosulphate solution. FA3, which is 0.1M potassium iodide solution. Solid D, which is iodine crystals. You are required to determine the partition coefficient of iodine between tretrachloromethane and water. Procedure Weigh accurately 1.0g of D and dissolve it in tetrachloromethane to make 50cm3 of solution. Transfer the solution into a separating funnel and add about 200cm3 of distilled water. Cork the funnel and shake the mixture vigorously for every half a minute for about 10-15 minutes and allow to stand for about 10 minutes. Carefully tap off the lower (organic) layer into a beaker. Pipette 10cm3 of the organic layer into a conical flask, add 20cm3 of FA3 and titrate with FA1 from the burette using starch indicator. Repeat the titration 2-3 times to obtain consistent results. Record your results in table I below. 103 Results Mass of empty bottle + D=……………………………………………..g Mass of empty bottle alone=………………………………………….g Mass of D alone=……………………………………………………………g Volume of pipette used=…………………………………………….cm3 Table 1 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading(cm3) Volume of FA1 used(cm3) Titre values used for calculating average volume of FA1 used ………………………………………………………………………………………………………cm3 Average volume of FA1 used…………………………………………………………………...cm3 Pipette 25cm3 of the aqueous layer into a conical flask and titrate with FA2 from the burette using starch indicator. Repeat the titration 2-3 times to obtain consistent results. Record your results in table II below. Results Volume of pipette used=…………………………………………….cm3 Table II Titration number 1 2 3 Final burette reading (cm3) Initial burette reading(cm3) Volume of FA2 used(cm3) Titre values used for calculating average volume of FA2 used ………………………………………………………………………………………………………cm3 Average volume of FA2 used …………………………………………………………………...cm3 Questions (a) Calculate the; (i) Molar concentration of ammonia in the organic layer. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… 104 …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ………………………………………………………………………………………………..…………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………..………………………………………………………… …………………………………………………………………………………………………………………………… ……………………………………………………………………………………………………………………………... (ii) Molar concentration of ammonia in the aqueous layer. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ………………………………………………………………………………………………..…………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………..………………………………………………………… …………………………………………………………………………………………………………………………… ……………………………………………………………………………………………………………………………... (b) Determine the value of the distribution coefficient of iodine between tetrachloromethane and water at room temperature. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ………………………………………………………………………………………………..…………………………… 105 SOLUBILITY Experiment 44 You are provided with the following; FA1, which is approximately a 0.1M solution of hydrochloric acid. FA2, which is a solution containing 19.10g of borax, Na2B4O7.10H2O in 1dm3 of solution. Solid W, which is calcium hydroxide You are required to standardize FA1 and use it to determine the solubility product of calcium hydroxide. Borax reacts with hydrochloric acid according to the equation: Na2B4O7.10 H2O(aq) + 2HCl(aq) 2NaCl(aq) + 4H3BO3(aq) + 5H2O(l) Procedure I Pipette 20cm3 or 25cm3 of FA3 into a clean conical flask. Add 2-3 drops of methyl orange indicator and then titrate with FA1 from the burette until you reach the end point. Repeat the titration 2-3 times until you obtain consistent results. Record your results in the table I. Results Volume of pipette used=…………………………………..cm3 Table 1 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading(cm3) Volume of FA1 used(cm3) Titre values used for calculating average volume of FA2 used ………………………………………………………………………………………………………cm3 Average volume of FA2 used …………………………………………………………………...cm3 Questions; (a) Calculate the molar concentration of hydrochloric acid in FA1. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… 106 Procedure Weigh accurately 2.0g of W and transfer the whole mass into a conical flask. Add 100cm3 of distilled water, cork the flask and shake the mixture vigorously for 15 minutes and filter. Label the solution FA3. Pipette 20cm3 or 25cm3 of FA3 into a conical flask, add 2-3 drops of phenolphthalein indicator and titrate with FA1 from the burette. Repeat the titration 2-3 times to obtain consistent results. Record your results in table I below. Results Mass of empty bottle + W=……………………………………………..g Mass of empty bottle alone=………………………………………….g Mass of W alone=……………………………………………………………g Volume of pipette used=…………………………………………….cm3 Table 1 Titration number 1 2 3 Final burette reading (cm3) Initial burette reading(cm3) Volume of FA1 used(cm3) Titre values used for calculating average volume of FA1 used ………………………………………………………………………………………………………………….cm3 Average volume of FA1 used …………………………………………………………………...cm3 Questions (b) Calculate the; (i) Number of moles of hydrochloric acid in FA1 that reacted with FA3. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ………………………………………………………………………………………………..…………………………… (ii) Molar concentration of hydroxide ions. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… 107 ………………………………………………………………………………………………..…………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (iii) Solubility product, Ksp of calcium hydroxide. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ……………………………………………………………………………………………………………………………... CHEMICAL KINETICS Experiment 45 You are provided with the following; FA1, which is a solution of iodine. FA2, which is a solution of propanone. FA3, which is a solution of sodium thiosulphate. 1M Sulphuric acid. Sodium hydrogencarbonate solution. You are required to determine the order of reaction with respect to iodine and the rate constant. (Assume that the acid and propanone are in large excess) Propanone reacts with iodine in the presence of an acid according to the following equation. CH3COCH3(aq) + I2(aq) H+(aq) CH3COCH2I(aq) + HI(aq) Procedure (a) Using a measuring cylinder, measure 25cm3 of FA2 into a beaker followed by 25cm3 of 1M Sulphuric acid. (b) Using a measuring cylinder, 50cm3 of FA1 is added into the beaker and at the same time the stop clock is started. The mixture is shaken well for about 1 minute. Label the resultant mixture FA4. 108 (c) After exactly five minutes, pipette 10cm3 of FA4 into a conical flask followed by an equal volume of sodium hydrogencarbonate solution and shake well until evolution of a gas stops. Titrate the mixture with FA3 from the burette using starch indicator. (d) Repeat procedure (c) at intervals of five minutes and enter your results in the table below. Table Time (minutes) 5 10 15 20 25 Final burette reading(cm3) Initial burette reading (cm3) Volume of FA3 used (cm3) Questions (a) Plot a graph of volume of FA3 against time. (b) From the graph, (i) Deduce the order of reaction with respect to iodine and give a reason for answer. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (ii) Determine the rate constant for the reaction. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ……………………………………………………………………………………………………………………………... (c) State the role of; (i) Sodium hydrogencarbonate solution. …………………………………………………………………………………………………………………………… ……………………………………………………………………………………………………………………………... (ii) Sulphuric acid. …………………………………………………………………………………………………………………………… 109 Experiment 46 You are provided with the following; FA1, which is a 0.02M solution of hydrogen peroxide. FA2, which is prepared by dissolving 3.2g of potassium manganate(VII) in water to make 1 litre of solution. 2M sodium hydroxide solution. 1M Sulphuric acid. 1M iron(III) chloride solution. The decomposition of hydrogen peroxide catalyzed by iron(III) ions under alkaline conditions proceeds according to the following equation. 2H2O2(aq) Fe3+(aq) 2H2O(l) + O2(g) The undecomposed hydrogen peroxide can then be titrated with potassium manganate(VII) solution. 2MnO4-(aq) + 6H+(aq) + 5H2O2(aq) 2Mn2+(aq) + 8H2O(l) + 5O2(g) The volume of the manganate(VII) used is directly proportional to the amount of hydrogen peroxide undecomposed. You are required to determine the order of reaction with respect to hydrogen peroxide and the rate constant for the reaction. Procedure. (a) Pipette 10cm3 of FA1 into a conical flask. Add 1cm3 of sodium hydroxide solution followed by 1cm3 of iron(III) chloride solution and the stop clock started at the same time. Shake the flask well and leave it to stand for 2 minutes. (b) After 2 minutes, add 20cm3 of 1M Sulphuric acid and titrate the mixture with FA2 from the burette until the end point. (c) Repeat procedure (a) and (b) but allow the hydrogen peroxide to decompose for 4, 6, 8 and 10 minutes before adding 1M Sulphuric acid. (d) Record the results in the table below. Time (minutes) 2 Volume of FA2 used, Vt (cm3) logVt 110 4 6 8 10 Questions (a) Plot a graph of logVt against time. (b) Use the graph to; (i) Deduce the order of reaction with respect to hydrogen peroxide and give a reason for your answer. …………………………………………………………………………………………………………………………… ……………………………………………………………………………………………………………………………... (ii) Determine the rate constant and state its units. Hence determine the half-life for the reaction. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… ………………………………………………………………………………………………..…………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (c) State the role of Sulphuric acid. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… Experiment 47 You are provided with the following; FA1, which is 0.12M sodium thiosulphate solution. FA2, which is 1.0M hydrochloric acid Distilled water. You are required to determine the rate constant and hence the half-life of the reaction. Theory Sodium thiosulphate reacts with hydrochloric acid according to the equation below; 111 Na2S2O3(aq) + 2HCl(aq) S(s) + 2NaCl(aq) + H2O(l) + SO2(g) Procedure (a) Make a small cross on a white paper using a pen. (b) Using a measuring cylinder, measure 50cm3 of FA1 into a conical flask. (c) Place the conical flask on the cross. (d) Using a clean measuring cylinder, add 10cm3 of FA2 to the flask and simultaneously start the stop clock. Shake the mixture to mix the solutions thoroughly. Look at the cross through the solution from above and stop the clock when the cross just becomes invisible. (e) Record the time taken in the table below. (f) Repeat the procedure (b) to (e) by measuring 40, 30, 20 and 10cm3 of FA1 into the conical flask. In each case make up the total volume of solution to 50cm3 by adding distilled water before adding 10cm3 of FA2. (g) Record your results in the table below. Volume of FA1, V Volume of distilled (cm3) water added (cm3) 50 0 40 10 30 20 20 30 10 40 Time (s) Log10V Questions (a) Plot a graph of Log10V against time. (b) Deduce the order of reaction with respect to sodium thiosulphate. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (c) Determine the; (i) Slope of the graph. 112 …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (ii) Rate constant, K for the reaction. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… (iii) Half-life for the reaction. …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… …………………………………………………………………………………………………………………………… 113 114 QUALITATIVE INORGANIC ANALYSIS This involves identifying cation(s) and anion(s) in the given substance or mixture of substances. The cations normally tested can be grouped according to their colour in solution as follows: 𝐍𝐇𝟒+ (aq) NON – COLOURED CATIONS IN SOLUTION 1. It forms no precipitate with sodium hydroxide solution. NB: Ammonium ions are confirmed by adding sodium hydroxide solution and warming the mixture. Observation A colourless gas with a chocking smell that turns damp red litmus paper blue and forms dense white fumes with concentrated hydrochloric acid. − NH4+ (aq) + OH(aq) NH3(g) + H2O(l) Note; When the ammonium salt is heated with sodium hydroxide , ammonia gas is given off . This is the confirmatory test for ammonium cation. 2. Ba 2+(aq), Ca2+(aq) and Mg2+(aq) (a) Addition of sodium hydroxide solution. These form a white precipitate insoluble in excess. Ba2+(aq) + 2OH-(aq) Ba(OH)2(s) Ca2+(aq) + 2OH-(aq) Ca(OH)2 (s) Mg2+(aq) + 2OH − (aq) Mg(OH)2 (s) (b) Addition of ammonia solution. (i) Ba 2+(aq) and Mg2+(aq) They form a white precipitate insoluble in excess. Ba2+(aq) + 2OH-(aq) Ba(OH)2(s) Mg2+(aq) + 2OH − (aq) Mg(OH)2 (s) (ii) Ca2+(aq) It gives no observable change. Note. Magnesium and barium ions can be distinguished from calcium ions by using ammonia solution. Magnesium ions are confirmed as follows. Test. Add solid ammonium chloride followed by disodium hydrogenphosphate solution followed by excess ammonia solution. Observation. A white precipitate insoluble in ammonia solution. Mg2+(aq) + Na2HPO4(aq) + NH4+(aq) MgNH4PO4(s) + 2Na+(aq) + H+(aq) Barium ions are confirmed by; 115 Adding potassium chromate(VI) solution followed by excess sodium hydroxide solution.. Observation. A yellow precipitate insoluble in excess sodium hydroxide solution. Ba2+(aq) + CrO42-(aq) BaCrO4(s) Adding ammonium oxalate solution followed by excess ethanoic acid. Observation A white precipitate soluble in ethanoic acid. Ba2+(aq) + C2O42-(aq) BaC2O4(s) BaC2O4(s) + 2CH3COOH(aq) (CH3COO)2Ba(aq) + H2C2O4(aq) Calcium ions are confirmed by; Test Adding ammonium oxalate solution followed by excess ethanoic acid. Observation A white precipitate insoluble in excess ethanoic acid. Ca2+(aq) + C2O42-(aq) CaC2O4(s) 3. Zn2+(aq) , Al3+(aq), Pb 2+(aq) and Sn2+(aq) (a) Addition of sodium hydroxide solution These form a white precipitate soluble in excess to form a colourless solution. i.e They form amphoteric hydroxides. Zn2+(aq) + 2OH-(aq) Zn(OH)2(s) Zn(OH)2(s)+ 2OH (aq) Zn(OH)42-(aq) Al3+(aq) + 3OH-(aq) Al(OH)3(aq) + OH-(aq) Al (OH)3(s) Al(OH)4-(aq) Pb2+ + 2OH-(aq) Pb(OH)2(s) + 2OH-(aq) Pb(OH)2(s) Pb(OH)42-(aq) Sn2+(aq) + 2OH-(aq) Sn(OH)2(s) Sn(OH)2(s) + 2OH-(aq) Sn(OH)42-(aq) (b) Addition of ammonia solution (i) Zn2+(aq) It forms a white precipitate soluble in excess to form a colourless solution. Zn2+(aq) + 2OH-(aq) Zn(OH)2(s) Zn(OH)2(s)+ 4NH3(aq) Zn(NH3)42+(aq) + 2OH-(aq) (ii) Al3+(aq), Pb 2+(aq) and Sn2+(aq) They form a white precipitate insoluble in excess. Al3+(aq) + 3OH-(aq) Al(OH)3(s) Pb2+ + 2OH-(aq) Pb(OH)2(s) 2+ Sn (aq) + 2OH (aq) Sn(OH)2(s) Note. Zn2+(aq) are distinguished from Al3+(aq) Pb2+(aq) and Sn2+(aq) by using ammonia solution. 116 Zn2+(aq) are confirmed by adding solid ammonium chloride followed by disodium hydrogenphosphate solution and excess ammonia solution. Observation. A white precipitate soluble in excess ammonia solution is observed. Pb2+ (aq) ions can be confirmed by; Adding potassium iodide solution. Observation A yellow precipitate. Pb2+(aq) + 2I-(aq) PbI2 (s) Adding potassium chromate(VI) solution followed by excess sodium hydroxide solution. Observation A yellow precipitate soluble in excess sodium hydroxide solution. Pb2+(aq) + CrO42-(aq) PbCrO4(s) PbCrO4(s) + 4OH (aq) Pb(OH)42-(aq) + CrO42-(aq) Adding dilute hydrochloric acid Observation A white precipitate Pb2+(aq) + 2Cl- (aq) PbCl2(S) Lead(II) chloride is soluble on heating and recrystallizes on cooling. Adding dilute Sulphuric acid/ sodium sulphate solution. Observation A white precipitate Pb2+(aq) + SO42-(aq) PbSO4(s) With Al3+(aq) and Sn2+(aq) there is no observable change. Aluminum ions can be confirmed by; Adding litmus solution followed by excess ammonia solution. Observation A blue “lake” is formed. Adding a few drops of Alizarin solution followed by ammonia solution. Observation A pink precipitate in a colourless solution. Sn2+(aq) ions can be distinguished from Al3+ (aq) ions by using an oxidizing agent such as; Acidified potassium manganate(VII) solution which will oxidize it to tin(IV) ions and itself reduced to manganese(II) ions Observation. The purple solution turns colourless. Sn2+(aq) + 2MnO-4(aq) + 16H+(aq) 5Sn4+(aq) + 2Mn2+(aq) + 8H2O(aq) Mercury(II) chloride solution. Observation A white precipitate is formed and it slowly turns grey. Sn2+(aq) + 2HgCl2 (aq) Sn4+(aq) + Hg2Cl2 (s) + 2Cl- (aq) 117 COLOURED CATIONS IN SOLUTION. GREEN IONS IN SOLUTION. These include; Fe2+(aq), Cr 3+(aq) , Ni2+(aq) and Cu2+(aq) 1. Cu2+(aq) (a) With sodium hydroxide solution. Observation It forms a blue precipitate insoluble in excess. Cu2+(aq) + 2OH-(aq) Cu(OH)2(S) (b) With ammonia solution. Observation A blue precipitate soluble in excess to form a deep blue solution. Cu2+(aq) + 2OH-(aq) Cu(OH)2(S) Cu(OH)2(s) + 4NH3(aq) Cu(NH3) 42+(aq) + 2OH-(aq) NB: Copper(II) ions are confirmed by; Adding potassium iodide solution. Observation A white precipitate in a brown solution. 2Cu2+(aq) + 4 I-(aq) Cu2I2(s) + I2(aq) Adding potassium hexacyanoferrate(II) solution. Observation A brown precipitate. 2Cu2+(aq) + [Fe(CN)6]4-(aq) Cu2Fe(CN)6(S) 2+ 2. Ni (aq) (a) With sodium hydroxide solution Observation A green precipitate insoluble in excess. Equation Ni2+(aq) + 2OH-(aq) Ni (OH)2(s) (b) With ammonia solution Observation A green precipitate soluble in excess to form a blue solution. Ni2+(aq) + 2OH-(aq) Ni (OH)2(s) Ni (OH)2 (s) + 6NH3(aq) Ni(NH3)62+(aq) + 2OH-(aq) NB: Ni2+(aq) ions are confirmed by Adding ammonia solution and then 2-3 drops of dimethylglyoxime. Observation. A red precipitate. 2+ 3. Fe (aq) (a) With sodium hydroxide solution Observation A green precipitate insoluble in excess that turns brown on standing. Fe2+(aq) + 2OH-(aq) Fe (OH)2 (S) 4Fe(OH)2(s) + O2(g) 2Fe2O3 . 2H2O(s) or 4Fe(OH)2(s) + O2(g) + 2H2O(l) 4 Fe(OH)3(s) 118 (b) With ammonia solution Observation A green precipitate insoluble in excess that turns brown on standing. Fe2+(aq) + 2OH-(aq) Fe(OH)2 (S) 4Fe(OH)2(s) + O2(g) 2Fe2O3 . 2H2O(s) or 4Fe(OH)2(s) + O2(g) + 2H2O(l) 4 Fe(OH)3(s) NB: Fe2+ ions are confirmed by; Adding potassium hexacyanoferrate(III) solution Observation A dark- blue precipitate. Fe2+(aq) + K+(aq) + Fe(CN)63- (aq) KFe[Fe(CN)6](s) 3+ 4. Cr (aq) (a) With sodium hydroxide solution Observation A green precipitate soluble in excess to form a green solution. Equations Cr3+(aq) + 3OH-(aq) Cr(OH)3 (s) Cr(OH)3(s) + OH-(aq) Cr(OH)4-(aq) Tetrahydroxochromate(III) ions (b) With dilute ammonia solution Observation A green precipitate insoluble in excess. Cr3+(aq) + 3OH-(aq) Cr(OH)3 (s) NB: If concentrated ammonia solution is used, then a green precipitate soluble in excess to form a pink solution is observed. Cr3+(aq) + 3OH-(aq) Cr(OH)3 (s) Cr(OH)3(s) + 6NH3(aq) Cr(NH3)63+(aq) + 3OH-(aq) Hexaamminechromium(III) ions Chromium(III) ions can be confirmed by; Adding excess sodium hydroxide solution followed by hydrogen peroxide solution and boiling the resultant mixture for a few minutes. Observation A green precipitate soluble in excess to form a green solution which turns yellow on addition of hydrogen peroxide solution. ̅ H(aq) Cr3+(aq) + 3O Cr(OH) 3 (s) ̅ Cr(OH)3 (s)+ OH(aq) Cr(OH) (aq) ̅ H(aq)+3H202(aq) 2Cr(OH) (aq)+2O 2CrO (aq)+8H20(l) When lead(II) acetate solution is added to the resultant solution (yellow solution), a yellow precipitate is formed. Pb2+(aq) + 2Cr0 (aq) PbCr04 (s) 119 PINK IONS IN SOLUTION 1. Mn2+(aq) These include Mn2+(aq) and Co2+(aq) (a) With sodium hydroxide solution Observation A white precipitate insoluble in excess that turns brown on standing. Mn2+(aq) + 2OH-aq) Mn(OH)2(S) Or 4Mn(OH)2(s) + O2(g) 2Mn2O3.2H2O(s) (b) With ammonia solution Observation A white precipitate insoluble in excess that turns brown on standing. Mn2+(aq) + 2OH-aq) Mn(OH)2(S) Or 4Mn(OH)2(s) + O2(g) 2Mn2O3.2H2O(s) NB: Mn2+ ions can be confirmed by; Adding concentrated nitric acid followed by either solid lead(IV) oxide or sodium bismuthate solution and the mixture boiled. Observation A purple solution is formed. 2Mn2+(aq) + 5BiO3- (aq) + 14H+(aq) 2MnO-4(aq) + 5Bi3+(aq) + 7H2O(l) 2Mn2+(aq) + 5 PbO2(s) + 4 H+(aq) 2MnO-4(aq) + 5 Pb2+(aq) + 2H2O(l) 2+ 2. Co (aq) (a) With sodium hydroxide solution Observation A blue precipitate insoluble in excess that turns brown on standing. Co2+(aq) + 2OH-aq) Co(OH)2(S) 4Co(OH)2(s) + O2(g) 2Co2O3 .2H2O(s) (b) With ammonia solution Observation A blue precipitate soluble in excess to form a brown solution that turns reddish brown on standing. Co2+(aq) + 2OH-(aq) Co(OH)2(S) Co(OH)2(s) + 6NH3(aq) Co(NH3)62+(aq) + 2OH-(aq) 4Co(NH3)62+(aq) + O2(g) + 2H2O(l) 4Co(NH3)63+(aq) + 4OH-(aq) NB: Co2+ ions can be confirmed by; Adding potassium thiocyanate solution. Observation A blue solution is formed. Co2+(aq) + 2SCN-(aq) Co(SCN)2(aq) Adding concentrated hydrochloric acid Observation The pink solution turns blue. 120 CO(H2O)62+(aq) + 4 Cl-(aq) CoCl42-(aq) + 6 H2O (l) However, when excess water is added to the resultant solution, the blue solution turns pink CoCl42-(aq) + 6 H2O (l) CO(H2O)62+(aq) + 4 Cl-(aq) YELLOW IONS IN SOLUTION. This only includes Fe3+(aq) (a) With sodium hydroxide solution Observation A brown precipitate insoluble in excess. Fe3+(aq) + 3OH-(aq) Fe(OH)3 (S) (b) With ammonia solution Observation A brown precipitate insoluble in excess. Fe3+(aq) + 3OH-(aq) Fe(OH)3 (S) NB: Fe3+ ions are confirmed by; Adding potassium hexacyanoferrate(II) solution Observation A dark- blue precipitate. Fe3+(aq) + K+(aq) + Fe(CN)64- (aq) KFe[Fe(CN)6](s) Adding potassium thiocyanate solution(KSCN), Observation A blood red colouration. Fe3+(aq) + SCN-(aq) [FeSCN]2+(aq) ANIONS The anions include; CO32-(aq), HCO3-(aq), C2O42-(aq), CH3 COO-, SO42-, SO32-, Cl-(aq), Br-(aq), I-(aq), NO3-(aq), NO2-(aq) and PO43- ions 1. C2O42-(aq) (a) Effect of heat on the solid substance. All oxalates decompose to form oxides, carbon dioxide and carbon monoxide except those of group(I) which form carbonates and carbon monoxide. XC2O4(s) XO(s) + CO2(g) + CO(g) Observation. A colourless gas that turns damp blue litmus paper red and lime water milky. (The gas evolved is carbon dioxide hence C2O42-(aq) should be suspected.) (b) Addition of lead(II) nitrate solution. Observation. A white precipitate is formed. (The precipitate is soluble in dilute nitric acid) Pb2+(aq) + C2O42-(aq) PbC2O4(s) 121 (c) Addition silver nitrate solution. Observation. A white precipitate is formed. (The precipitate is soluble in dilute nitric acid and ammonia solution) 2Ag+(aq) + C2O42-(aq) Ag2C2O4(s) (d) Addition of barium nitrate solution. Observation. A white precipitate is formed. (The precipitate is soluble in dilute nitric acid) Ba2+(aq) + C2O42-(aq) BaC2O4(s) NB: C2O42-(aq) are confirmed by; Adding acidified potassium manganate(VII) solution and warm. Observation. The purple solution turns colourless. 2MnO4-(aq) + 16H+(aq) + 5C2O42-(aq) 2Mn2+(aq) + 8H2O(l) + 10CO2(g) 2. CO32-(aq) and HCO3-(aq) (a) Effect of heat on the solid substance. Observation. A colourless gas that turns damp blue litmus paper red and lime water milky. (The gas evolved is carbon dioxide hence CO32-(aq) and HCO3-(aq) should be suspected.) XCO3(s) XO(s) + CO2(g) X(HCO3)2(s) XCO3(s) + CO2(g) + H2O(l) (b) Addition of dilute acid on the solid substance. Observation. Bubbles of a colourless gas that turns damp blue litmus paper red and lime water milky. (The gas evolved is carbon dioxide hence CO32-(aq) and HCO3-(aq) should be suspected.) XCO3(s) + 2H+(aq) X2+(aq) + CO2(g) + H2O(l) X(HCO3)2(s) + 2H+(aq) X2+(aq) + CO2(g) + 2H2O(l) NB: CO32-(aq) and HCO3-(aq) can be distinguished from C2O42- by using a dilute acid, both carbonates and hydrogen carbonates liberate carbon dioxide gas on addition of dilute acid. Oxalates do not liberate carbon dioxide gas. C2O42-(aq) can be distinguished from CO32-(aq) using silver nitrate solution or lead(II) nitrate solution or barium nitrate solution followed by dilute nitric acid. C2O42-(aq), a white precipitate soluble in the acid is observed. CO32-(aq), a white precipitate soluble in the acid with bubbles of a colourless gas. 2 A CO3 (aq) is distinguished from HCO-3(aq) using magnesium sulphate solution With a CO32-(aq) - A white precipitate is observed. Mg2+(aq) + CO32-(aq) MgCO3(s) With a HCO3 (aq) - No observable change. But a white precipitate is observed on heating. Mg(HCO3)2(aq) MgCO3(s) + CO2(g) + H2O(l) 122 When a dilute acid is added to a residue obtained after filtering and there is bubbles of a colourless gas that turns damp blue litmus paper red and lime water milky, a CO32-(aq) should be confirmed since all HCO3-(aq) are soluble. 3. SO32(a) Addition of lead(II) nitrate solution. Observation. A white precipitate is formed. (The precipitate is soluble in dilute nitric acid) Pb2+(aq) + SO32-(aq) PbSO3(s) (b) Addition of barium nitrate solution. Observation. A white precipitate is formed. (The precipitate is soluble in dilute nitric acid) Ba2+(aq) + SO32-(aq) BaSO3(s) NB: SO32-(aq) are confirmed by; Adding acidified potassium manganate(VII) solution. Observation. The purple solution turns colourless. 2MnO4-(aq) + 6H+(aq) + 5SO32-(aq) 2Mn2+(aq) + 3H2O(l) + 5SO42-(aq) Adding iodine solution or bromine solution. Observation. The brown solution turns colourless. I2(aq) + H2O(l) + SO32-(aq) 2I-(aq) + 2H+(aq) + SO42-(aq) 2Br2(aq) + H2O(l) + SO3 (aq) 2Br-(aq) + 2H+(aq) + SO42-(aq) 4. SO42-(aq) (a) Addition of lead(II) nitrate solution. Observation. A white precipitate is formed. (The precipitate is insoluble in dilute nitric acid and on heating) Pb2+(aq) + SO42-(aq) PbSO4(s) NB: SO42-(aq) are confirmed by; Adding barium nitrate solution followed by dilute nitric acid. Observation. A white precipitate is formed insoluble in the acid. Ba2+(aq) + SO42-(aq) BaSO4(s) 35. PO4 (a) Addition of lead(II) nitrate solution. Observation. A white precipitate is formed. (The precipitate is soluble in dilute nitric acid) 3Pb2+(aq) + 2PO43-(aq) Pb3(PO4)2( (s) (b) Addition of barium nitrate solution. Observation. A white precipitate is formed. (The precipitate is soluble in dilute nitric acid) 3Ba2+(aq) + 2PO43-(aq) Ba3(PO4)2( (s) 123 (c) Addition silver nitrate solution. Observation. A yellow precipitate is formed. (The precipitate is soluble in dilute nitric acid and ammonia solution) 3Ag+(aq) + PO43-(aq) Ag3PO4( (s) (d) Addition iron(II) chloride solution. Observation. A brown precipitate is formed. 3Fe2+(aq) + 2PO43-(aq) Fe3(PO4)2(s) NB: PO43-(aq) are confirmed by; Adding dilute nitric acid followed by ammonium molybdate solution. Observation. A yellow precipitate is formed. (The precipitate is soluble in ammonia solution) 6. Cl-(aq), Br-(aq), I-(aq) (a) Effect of heat on the solid sample. (i) Cl-(aq) Observation. White fumes which turn damp blue litmus red and form dense white fumes with concentrated ammonia solution or form a white precipitate with silver nitrate solution. (HCl gas is evolved hence a Cl- should be highly suspected). (ii) Br-(aq) Observation. Brown fumes. (Br2 gas evolved, hence Br- should be highly suspected) (iii) I-(aq) Observation. Purple fumes. (I2 gas evolved, hence I- should be highly suspected) (b) Addition of concentrated Sulphuric acid to a solid sample and heat. (i) Cl-(aq) Observation. White fumes which form dense white fumes with concentrated ammonia solution. (HCl gas is evolved hence a Cl- present). (ii) Br-(aq) Observation. Brown fumes. (Br- oxidized to Br2) (iii) I-(aq) Observation. Purple fumes which form a black sublimate. (I- oxidized to I2) (c) Addition of lead(II) nitrate solution. (i) Cl-(aq) Observation. A white precipitate. (The precipitate is insoluble in dilute nitric acid) Pb2+(aq) + 2Cl-(aq) PbCl2(s) The white precipitate is soluble on heating and recrystallizes on cooling. 124 (ii) Br-(aq) Observation. A white precipitate. Pb2+(aq) + 2Br-(aq) PbBr2(s) (iii) I-(aq) Observation. A yellow precipitate. Pb2+(aq) + 2I-(aq) PbI2(s) (d) Addition of silver nitrate solution [Confirmatory test] (i) Cl-(aq) Observation. A white precipitate. (The precipitate is insoluble in dilute nitric acid) Ag+(aq) + Cl-(aq) AgCl(s) The white precipitate is soluble in ammonia solution. AgCl(s) + 2NH3(aq) Ag(NH3)2+(aq) + Cl-(aq) (ii) Br (aq) Observation. A pale yellow precipitate. (The precipitate is insoluble in dilute nitric acid) Ag+(aq) + Br-(aq) AgBr(s) (iii) I-(aq) Observation. A yellow precipitate. (The precipitate is insoluble in dilute nitric acid) Ag+(aq) + I-(aq) AgI(s) The yellow precipitate is insoluble in ammonia solution. NB: Br-(aq) and I-(aq) can also be confirmed by adding bleaching powder/jik followed by concentrated nitric acid followed by carbon tetrachloride. Observation With Br-(aq), a reddish-brown colouration in the organic layer. With I-(aq), a purple colouration in the organic layer. 7. CH3COO-(aq) (a) Effect of heat on the solid. Metal oxalates decompose on heating to form acetone (propanone) which burns on application of heat, carbon dioxide and a metal oxide. O (CH3COO)2X(s) CH3CCH3(g) + CO2(g) + XO(s) Observation White fumes with a sweet odour that form a yellow precipitate with Brady’s reagent. NB: Carbon dioxide is also produced and should therefore be tested for. [ A colourless gas that turns damp blue litmus paper red and lime water milky] 125 (b) Addition of concentrated Sulphuric acid to a solid sample and heat. Observation White fumes with a vinegar smell (smell of acetic acid) which turns damp blue litmus paper red. CH3COO-(aq) + H+(aq) CH3COOH(aq) NB: Ethanoate ions are confirmed by; Adding an alcohol (ethanol) followed by 2-3 drops of concentrated Sulphuric acid and the mixture warmed. Observation A sweet fruity smell. [An ester formed] CH3COOH(aq) + CH3CH3OH(l) CH3COOCH2CH3 (aq) + H2O(l) Adding iron(III) chloride solution and the mixture warmed. Observation A reddish-brown precipitate 3CH3COO-(aq) + Fe3+(aq) (CH3COO)3Fe(s) 8. NO3 (aq) (a) Effect of heat on the solid. Most nitrates when heated produce nitrogen dioxide except those of sodium and potassium. Observation Brown fumes. [Nitrogen dioxide evolved] (b) Addition of concentrated Sulphuric acid to a solid sample and heat. Observation Brown fumes. [Nitrogen dioxide evolved] NB: Nitrate ions can be confirmed by; Adding Devarda’s alloy (A mixture of Al, Cu and Zn) or Zinc or Aluminium powder followed by sodium hydroxide solution and warm. [Ammonia gas is evolved] Observation A colourless gas with a chocking smell that turns damp red litmus paper blue and forms dense white fumes with concentrated hydrochloric acid. Adding copper turnings followed by 2-3 drops of concentrated Sulphuric acid and heat. Observation Brown fumes Adding freshly prepared iron(II) sulphate solution followed by concentrated Sulphuric acid down the sides of the test tube carefully. Observation A brown ring is formed at the junction of the two layers. 9. NO2 (aq) (a) Addition of concentrated/dilute Sulphuric acid to a solid sample. Observation Brown fumes. [Nitrogen dioxide evolved] Nitrate ions do not react with dilute Sulphuric acid. 126 NB: Nitrite ions can be confirmed by; Adding Devarda’s alloy (A mixture of Al, Cu and Zn) or Zinc or Aluminium powder followed by sodium hydroxide solution and warm. [Ammonia gas is evolved] Observation A colourless gas with a chocking smell that turns damp red litmus paper blue and forms dense white fumes with concentrated hydrochloric acid. Adding freshly prepared iron(II) sulphate solution followed by concentrated Sulphuric acid down the sides of the test tube carefully. Observation A brown ring is formed at the junction of the two layers. Adding acidified potassium manganate(VII) solution. Observation. The purple solution turns colourless. 2MnO4-(aq) + 6H+(aq) + 5NO2-(aq) 2Mn2+(aq) + 3H2O(l) + 5NO3-(aq) Experiment 48 You are provided with substance A, which contains two cations and two anions. You are required to carry out the following tests on A and identify the cations and anions in A. Identify any gas(es) evolved. Record your observations and deductions in the table below. Tests Observations (a) Heat two spatula endfuls of A strongly in a dry test tube until there is no further change. (b) To about 6cm3 of water, add two spatula end-fuls of A and shake well. Filter the mixture and keep both the filtrate and residue. Divide the filtrate into six portions. 127 Deductions (i) To the first portion of the filtrate, add dilute sodium hydroxide dropwise until in excess. (ii) To the second portion of the filtrate, add dilute ammonia solution dropwise until in excess. (iii) To the third portion of filtrate, add 3-4 drops of dilute Sulphuric acid. (iv) To the fourth portion of the filtrate, add 3-4 drops of potassium chromate(VI) solution followed by excess sodium hydroxide solution. (v) To the fifth portion of filtrate, add lead (II) nitrate solution and heat. (v) Use the sixth portion of the filtrate to carry out a test of your own to confirm one of the first anion in A. (c) Wash the residue and then add dilute nitric acid until no further change. Divide the resultant solution into four portions. (i) To the first portion, add dilute sodium hydroxide solution drop-wise until in excess. (ii) To the second portion, add dilute ammonia solution drop-wise until in excess. 128 (iii) To the third portion, add 3-4 drops of dilute Sulphuric acid. (iv) Use the fourth portion to carry out a test of your own to confirm the second cation in A. (d) Identify the; (i) Cations in A …………………………………… and …………………………………………………………. (ii) Anions in A …………………………………… and …………………………………………………………. Experiment 49 You are provided with substance B, which contains two cations and two anions. You are required to carry out the following tests on B and identify the cations and anions in B. Identify any gas(es) evolved. Record your observations and deductions in the table below. Tests Observations (a) Heat two spatula endfuls of B strongly in a dry test tube until there is no further change. (b) To a spatula end-full of B, add 3-4 drops of concentrated Sulphuric acid and heat. (c) To about 6cm3 of water, add two spatula end-fuls of B and shake well. Filter the 129 Deductions mixture and keep both the filtrate and residue. Divide the filtrate into five portions. (i) To the first portion of the filtrate, add dilute sodium hydroxide dropwise until in excess. (ii) To the second portion of the filtrate, add dilute ammonia solution dropwise until in excess. (iii) Use the third portion of filtrate to carry out a test of your own choice to confirm the first cation in B. (iv) To the fourth portion of filtrate, add 3 drops of neutral iron(III) chloride solution and heat. (v) To the fifth portion of the filtrate, add 1cm3 of ethanol followed 3 drops of concentrated Sulphuric acid and heat. Pour the hot mixture in beaker of cold water. (d) Wash the residue and then add dilute nitric acid until no further change. Divide the resultant solution into four portions. (i) To the first portion, add dilute sodium hydroxide solution drop-wise until in excess. 130 (ii) To the second portion, add dilute ammonia solution drop-wise until in excess. (iii) To the third portion, add 3-4 drops of dilute Sulphuric acid. (iv) Use the fourth portion to carry out a test of your own to confirm the second cation in B. (e) Identify the; (i) Cations in B …………………………………… and ………………………………………. (ii) Anions in B …………………………………… and ………………………………………. Experiment 50 You are provided with substance C, which contains two cations and two anions. You are required to carry out the following tests on C and identify the cations and anions in C. Identify any gas(es) evolved. Record your observations and deductions in the table below. Tests Observations (a) Heat two spatula endfuls of C strongly in a dry test tube until there is no further change. (b) To about 6cm3 of water, add two spatula end-fuls of C and shake well. Filter the 131 Deductions mixture and keep both the filtrate and residue. Divide the filtrate into six portions. (i) To the first portion of the filtrate, add dilute sodium hydroxide dropwise until in excess. (ii) To the second portion of the filtrate, add dilute ammonia solution dropwise until in excess. (iii) To the third portion of filtrate, add 3-4 drops of dilute Sulphuric acid. (iv) To the fourth portion of the filtrate, add litmus solution followed by dilute ammonia solution. (v) To the fifth portion of filtrate, add lead (II) nitrate solution. (v) Use the sixth portion of the filtrate to carry out a test of your own to confirm one of the first anion in C. (c) Wash the residue and then add dilute nitric acid until there is no further change. Divide the resultant solution into four portions. (i) To the first portion, add dilute sodium hydroxide solution drop-wise until in excess. 132 (ii) To the second portion, add dilute ammonia solution drop-wise until in excess. (iii) Use the third portion to carry out a test of your own to confirm the second cation in C. (d) Identify the; (i) Cations in C …………………………………… and ………………………………………. (ii) Anions in C …………………………………… and ………………………………………. Experiment 51 You are provided with substance D, which contains two cations and two anions. You are required to carry out the following tests on D and identify the cations and anions in D. Identify any gas(es) evolved. Record your observations and deductions in the table below. Tests Observations (a) Heat two spatula endfuls of D strongly in a dry test tube until there is no further change. (b) To about 6cm3 of water, add two spatula end-fuls of D and shake well. Filter the mixture and keep both the filtrate and residue. Divide the filtrate into four portions. 133 Deductions (i) To the first portion of the filtrate, add dilute sodium hydroxide solution and warm. (ii) To the second portion of the filtrate, add 3-4 drops of lead(II) nitrate solution followed by dilute nitric acid. (iii) To the third portion of filtrate, add 3-4 drops of silver nitrate solution followed by dilute nitric acid. (iv) To the fourth portion of the filtrate, add acidified potassium manganate(VII) solution and heat. (c) Wash the residue and then add dilute hydrochloric acid until there is no further change. Divide the resultant solution into three portions. (i) To the first portion, add dilute sodium hydroxide solution drop-wise until in excess. (ii) To the second portion, add dilute ammonia solution drop-wise until in excess. (iii) Use the third portion to carry out a test of your own to confirm the second cation in D. 134 (d) Identify the; (i) Cations in D …………………………………… and ………………………………………. (ii) Anions in D …………………………………… and ………………………………………. Experiment 52 You are provided with substance E, which contains two cations and two anions. You are required to carry out the following tests on E and identify the cations and anions in E. Identify any gas(es) evolved. Record your observations and deductions in the table below. Tests Observations (a) Heat two spatula endfuls of E strongly in a dry test tube until there is no further change. (b) To a spatula end-full of E, add 3-4 drops of concentrated Sulphuric acid and heat. (c) To about 6cm3 of water, add two spatula end-fuls of E and shake well. Filter the mixture and keep both the filtrate and residue. Divide the filtrate into five portions. (i) To the first portion of the filtrate, add dilute sodium hydroxide dropwise until in excess. (ii) To the second portion of the filtrate, add dilute 135 Deductions ammonia solution dropwise until in excess. (iii) To the third portion of the filtrate, add 3-4 drops of sodium sulphate solution. (iv) Use the fourth portion of filtrate to carry out a test of your own choice to confirm the first cation in E. (v) To the fifth portion of filtrate, add a few copper turnings followed by 3 drops of concentrated Sulphuric acid and heat. (d) Wash the residue and then add dilute nitric acid until no further change. Divide the resultant solution into four portions. (i) To the first portion, add dilute sodium hydroxide solution drop-wise until in excess. (ii) To the second portion, add dilute ammonia solution drop-wise until in excess. (iii) Use the third portion to carry out a test of your own to confirm the second cation in E. 136 (e) Identify the; (i) Cations in E …………………………………… and ………………………………………. (ii) Anions in E …………………………………… and ………………………………………. Experiment 53 You are provided with substance F, which contains two cations and two anions. You are required to carry out the following tests on F and identify the cations and anions in F. Identify any gas(es) evolved. Record your observations and deductions in the table below. Tests Observations (a) Heat two spatula endfuls of F strongly in a dry test tube until there is no further change. (b) To a spatula end-full of F, add 3-4 drops of concentrated Sulphuric acid and warm. (b) To two spatula end-fuls of F, add dilute nitric acid drop-wise until there is no further change. (c) To the resultant solution in (b), add dilute sodium hydroxide solution drop-wise until in excess and then filter. Keep both the filtrate and residue. 137 Deductions (d) To the filtrate from (c), add dilute nitric acid dropwise until the solution is just acidic. Divide the acidic solution into five portions. (i) To the first portion of the acidic solution, add dilute sodium hydroxide solution drop-wise until in excess. (ii) To the second portion of the acidic solution, add dilute ammonia solution drop-wise until in excess. (iii) Use the third portion of acidic solution to carry out a test of your own to confirm one of the cations in F. (iv) To the fourth portion of acidic solution, add lead (II) nitrate solution and heat. (v) Use the fifth portion of the acidic solution to carry out a test of your own choice to confirm one of the anions in F. 138 (e) Wash the residue and then add dilute nitric acid solution until there is no further change. Divide the resultant solution into four parts. (i) To the first part, add dilute sodium hydroxide solution drop-wise until in excess. (ii) To the second part, add aqueous ammonia dropwise until in excess. (iii) To the third part, add 3-4 drops of dilute Sulphuric acid. (iv) Use the fourth part to carry out a test of your own to confirm the second cation in F. (f) Identify the; (i) Cations in F …………………………………… and ………………………………………. (ii) Anions in F …………………………………… and ………………………………………. 139 Experiment 54 You are provided with substance G, which contains three cations and one anion. You are required to carry out the following tests on G and identify the cations and anion in G. Identify any gas(es) evolved. Record your observations and deductions in the table below. Tests Observations (a) Heat two spatula endfuls of G strongly in a dry test tube until there is no further change. (b) To about 6cm3 of water, add two spatula end-fuls of G and shake well. To the resultant solution, add dilute sodium hydroxide solution dropwise until there is no further change, warm and filter. Keep both the filtrate and residue. (c) To the filtrate in (b) above, add dilute nitric acid drop-wise until the solution is just acidic. Divide the acidic solution into five portions. (i) To the first portion of the acidic solution, add dilute sodium hydroxide 140 Deductions solution drop-wise until in excess. (ii) To the second portion of the acidic solution, add dilute ammonia solution drop-wise until in excess. (iii) Use the third portion of acidic solution to carry out a test of your own choice to confirm the one of the cations in G. (iv) To the fourth portion, add lead(II) nitrate solution. (v) Use the fifth portion to carry out a test of your own choice to confirm the anion in G. (d) Wash the residue and then add dilute hydrochloric acid until there is no further change. Divide the resultant solution into three portions. (i) To the first portion, add dilute sodium hydroxide solution drop-wise until in excess. 141 (ii) To the second portion, add dilute ammonia solution drop-wise until in excess. (iii) To the third portion, add little solid ammonium chloride followed by disodium hydrogenphosphate solution followed by excess ammonia solution. (d) Identify the; (i) Cations in G ………………………, ……………………… and …………………………………….. (ii) Anion in G …………………………………… Experiment 55 You are provided with substance H, which contains two cations and two anions. You are required to carry out the following tests on H and identify the cations and anions in H. Identify any gas(es) evolved. Record your observations and deductions in the table below. Tests Observations (a) Heat two spatula endfuls of H strongly in a dry test tube until there is no further change. 142 Deductions (b) To a spatula end-full of H, add 3-4 drops of concentrated Sulphuric acid and heat. (c) To about 6cm3 of water, add two spatula end-fuls of H and shake vigorously. (d) To the resultant solution in (b) above, add dilute sodium hydroxide solution drop-wise until in excess and filter. Keep both the filtrate and residue. (e) To the filtrate, add dilute nitric acid dropwise until the solution is just acidic. Divide the acidic filtrate into eight portions. (i) To the first portion of the acidic filtrate, add dilute sodium hydroxide solution drop-wise until in excess. (ii) To the second portion of the acidic filtrate, add dilute ammonia solution drop-wise until in excess. (iii) Use the third portion of acidic filtrate to carry out a test of your own choice to confirm one of the cations in H. 143 (iv) To the fourth portion of the acidic filtrate, add 45 drops of silver nitrate solution. (v) To the fifth portion of the acidic filtrate, add 3-4 drops of lead(II) nitrate solution. (vi) Use the sixth portion of the acidic filtrate to carry out a test of your own choice to confirm one of the anions in H. (vii) To the seventh portion of the acidic filtrate, add 3 drops of neutral iron(III) chloride solution and heat. (viii) To the eighth portion of the acidic filtrate, add 1cm3 of ethanol followed 3 drops of concentrated Sulphuric acid and heat. Pour the hot mixture in beaker of cold water. (f) Wash the residue and then add dilute hydrochloric acid until no further change. Divide the resultant solution into three portions. (i) To the first portion, add dilute sodium hydroxide solution drop-wise until in excess. (ii) To the second portion, add dilute ammonia 144 solution drop-wise until in excess. (iii) Use the third portion to carry out a test of your own to confirm the second cation in H. (e) Identify the; (i) Cations in H …………………………………… and ………………………………………. (ii) Anions in H …………………………………… and ………………………………………. Experiment 56 You are provided with substance I, which contains two cations and two anions. You are required to carry out the following tests on I and identify the cations and anions in I. Identify any gas(es) evolved. Record your observations and deductions in the table below. Tests Observations (a) Heat two spatula endfuls of I strongly in a dry test tube until there is no further change. (b) To about 6cm3 of water, add two spatula end-fuls of I, shake vigorously and filter. Keep both the filtrate and the residue. Divide the filtrate into three portions. 145 Deductions (i) To the first portion of the filtrate, add lead(II) nitrate solution. (ii) To the second portion of the filtrate, add barium nitrate solution followed by dilute nitric acid. (iii) Use the third portion of filtrate to carry out a test of your own choice to confirm one of the anions in I. (c) Dissolve the residue in (b) in minimum dilute nitric acid. To the resultant solution, add dilute sodium hydroxide solution dropwise until in excess and filter. Keep both the filtrate and residue. (d) To the filtrate in (c) above, add dilute nitric acid drop-wise until the solution is just acidic. Divide the acidic filtrate into five portions (i) To the first portion of the acidic filtrate, add dilute sodium hydroxide 146 solution drop-wise until in excess. (ii) To the second portion of the acidic filtrate, add 34 drops of dilute Sulphuric acid. (iii) To the third portion of the acidic filtrate, add dilute ammonia solution drop-wise until in excess. (iv) Use the fourth portion of the acidic filtrate to carry out a test of your own choice to confirm one of the cations in I. (e) Wash the residue with dilute sodium hydroxide solution and dissolve it in dilute nitric acid. Divide the resultant solution into three portions. (i) To the first portion, add dilute sodium hydroxide solution drop-wise until in excess. (ii) To the second portion, add dilute ammonia solution drop-wise until in excess. 147 (iii) To the third portion, add 3-4 drops of dilute Sulphuric acid. (iv) Use the fourth portion to carry out a test of your own to confirm the second cation in I. (f) Identify the; (i) Cations in I …………………………………… and ………………………………………. (ii) Anions in I …………………………………… and ………………………………………. Experiment 57 You are provided with substance J, which contains two cations and two anions. You are required to carry out the following tests on J and identify the cations and anions in J. Identify any gas(es) evolved. Record your observations and deductions in the table below. Tests Observations (a) Heat two spatula endfuls of J strongly in a dry test tube until there is no further change. 148 Deductions (b) To a spatula end-full of J, add half a spatula endfull of manganese(IV) oxide followed by 4-5 drops of concentrated Sulphuric acid and heat gently. (c) To three spatula endfuls of J, add dilute nitric acid drop-wise until there is no further change. Warm gently. (d) To the resultant solution in (c) above, add dilute ammonia solution drop-wise until in excess and filter. Keep both the filtrate and the residue. (e) To the filtrate in (d) above, add dilute nitric acid drop-wise until the solution is just acidic. Divide the acidic filtrate into five portions. (i) To the first portion of the acidic filtrate, add dilute sodium hydroxide solution drop-wise until in excess. (ii) To the second portion of the acidic filtrate, add dilute ammonia solution drop-wise until in excess. 149 (iii) Use the third portion of acidic filtrate to carry out a test of your own choice to confirm one of the cations in J. (f) Wash the residue and dissolve it in dilute Sulphuric acid. Divide the resultant solution into three portions. (i) To the first portion, add dilute sodium hydroxide solution drop-wise until in excess. (ii) To the second portion, add dilute ammonia solution drop-wise until in excess. (iii) Use the third portion to carry out a test of your own choice to confirm the second cation in J. (g) To two spatula endfuls of J, add 4cm3 of water, shake vigorously and filter. Divide the filtrate into three portions. (i) To the first portion, add 3-4 drops of silver nitrate solution followed by ammonia solution dropwise until in excess. 150 (ii) To the second portion, add 1-2 drops of concentrated nitric acid followed by sodium thiosulphate solution drop-wise until in excess. (iii) To the third portion, add 3-4 drops of lead(II) nitrate solution. (f) Identify the; (i) Cations in J …………………………………… and ………………………………………. (ii) Anions in J …………………………………… and ………………………………………. Experiment 58 You are provided with substance K, which contains three cations and one anion. You are required to carry out the following tests on K and identify the cations and anion in K. Identify any gas(es) evolved. Record your observations and deductions in the table below. Tests Observations (a) Heat two spatula endfuls of K strongly in a dry test tube until there is no further change. (b) To about 6cm3 of water, add two spatula end-fuls of K and shake thoroughly. To the resultant solution, add dilute sodium hydroxide solution dropwise until there is no further change, warm and filter. Keep both the filtrate and residue. 151 Deductions (c) To the filtrate in (b) above, add dilute nitric acid drop-wise until the solution is just acidic. Divide the acidic solution into six portions. (i) To the first portion of the acidic solution, add dilute sodium hydroxide solution drop-wise until in excess. (ii) To the second portion of the acidic solution, add dilute ammonia solution drop-wise until in excess. (iii) To the third portion of the acidic solution, add 2-3 drops of potassium iodide solution. (iv) Use the fourth portion of acidic solution, add 2-3 drops of litmus solution followed by dilute ammonia solution dropwise until in excess. (v) To the fifth portion of the acidic solution, add 2-3 drops of lead(II) nitrate solution and heat. (vi) Use the sixth portion of the acidic solution to carry out a test of your own choice to confirm the anion in K. (d) Wash the residue and dissolve it in dilute hydrochloric acid. Divide the resultant solution into three portions. 152 (i) To the first portion, add dilute sodium hydroxide solution drop-wise until in excess. (ii) To the second portion, add dilute ammonia solution drop-wise until in excess. (iii) To the third portion, add 3-4 drops of potassium thiocyanate solution. (e) Identify the; (i) Cations in K ………………………, ……………………… and …………………………………….. (ii) Anion in K …………………………………… Experiment 59 You are provided with substance L, which contains two cations and two anions. You are required to carry out the following tests on L and identify the cations and anions in L. Identify any gas(es) evolved. Record your observations and deductions in the table below. Tests Observations (a) Heat two spatula endfuls of L strongly in a dry test tube until there is no further change. (b) To about 6cm3 of water, add two spatula end-fuls of L and shake vigorously. Filter and keep both the filtrate and residue. Divide the filtrate into five portions. 153 Deductions (i) To the first portion of the filtrate, add 2-3 drops of lead(II) nitrate solution. (ii) To the second portion of the filtrate, add silver nitrate solution followed by dilute nitric acid. (iii) To the third portion of filtrate, add 2-3 drops of iron(II) chloride solution. (iv) To the fourth portion of the filtrate, add concentrated nitric acid followed by ammonium molybdate solution followed by excess dilute ammonia solution. (c) To the residue from (b) above, add dilute nitric acid until there is no further change. To the resultant solution, add dilute sodium hydroxide solution dropwise until in excess and filter. Keep both the filtrate and residue. (d) To the filtrate in (c) above, add dilute nitric acid drop-wise until the solution is just acidic. Divide the acidic filtrate into three portions. (i) To the first portion of the acidic filtrate, add dilute sodium hydroxide solution drop-wise until in excess. 154 (ii) To the second portion of the acidic filtrate, add dilute ammonia solution drop-wise until in excess. (iii) Use the third portion of the acidic filtrate to carry out a test of your own choice to confirm one of the cations in L. (e) Wash the residue from (c) above and dissolve it in minimum amount of dilute nitric acid. Divide the resultant solution into three portions. (i) To the first portion, add dilute sodium hydroxide solution drop-wise until in excess. (ii) To the second portion, add dilute ammonia solution drop-wise until in excess. (iii) Use the third portion to carry out a test of your own to confirm the second cation in L. (f) Identify the; (i) Cations in L …………………………………… and ………………………………………. (ii) Anions in L …………………………………… and ………………………………………. 155 Experiment 60 You are provided with substance M, which contains two cations and two anions. You are required to carry out the following tests on M and identify the cations and anions in M. Identify any gas(es) evolved. Record your observations and deductions in the table below. Tests Observations (a) Heat two spatula endfuls of M strongly in a dry test tube until there is no further change. (b) To a spatula end-full of M, add 4-5 drops of concentrated Sulphuric acid and heat. (c) To two spatula end-fuls of M in a test tube, add 5cm3 of water, shake well and filter. Keep both the filtrate and residue. Divide the filtrate into three portions. (i) To the first portion, add 3-4 drops lead(II) nitrate solution. (ii) To the second portion, add silver nitrate solution followed by excess ammonia solution. 156 Deductions (iii) To the third portion, add bleaching powder followed by concentrated nitric acid followed by 3cm3 of carbon tetrachloride. (d) Dissolve the residue in (c) above in minimum amount of dilute nitric acid. To the resultant solution, add dilute sodium hydroxide solution dropwise until in excess and filter. Keep both the filtrate and the residue. (e) To the filtrate in (d) above, add dilute nitric acid drop-wise until the solution is just acidic. Divide the acidic filtrate into five portions. (i) To the first portion of the acidic filtrate, add dilute ammonia solution drop-wise until in excess. (ii) To the second portion of the acidic filtrate, add 34 drops of dilute hydrochloric acid. (iii) To the third portion of the acidic filtrate, add dilute sodium hydroxide solution drop-wise until in excess. 157 (iv) Use the fourth portion of acidic filtrate to carry out a test of your own choice to confirm one of the cations in M. (f) Wash the residue and dissolve it in dilute nitric acid. Divide the resultant solution into three portions. (i) To the first portion, add dilute sodium hydroxide solution drop-wise until in excess. (ii) To the second portion, add dilute ammonia solution drop-wise until in excess. (iii) Use the third portion to carry out a test of your own choice to confirm the second cation in M. (g) Identify the; (i) Cations in M …………………………………… and ………………………………………. (ii) Anions in M …………………………………… and ………………………………………. Experiment 61 You are provided with substance N, which contains two cations and two anions. You are required to carry out the following tests on N and identify the cations and anions in N. Identify any gas(es) evolved. Record your observations and deductions in the table below. 158 Tests Observations (a) Heat two spatula endfuls of N strongly in a dry test tube until there is no further change. (b) To a spatula end-full of N, add 4-5 drops of concentrated Sulphuric acid and warm. (c) To two spatula end-fuls of N in a test tube, add 5cm3 of water, shake well and filter. Keep both the filtrate and residue. Divide the filtrate into four portions. (i) To the first portion, add 3-4 drops concentrated nitric acid followed by sodium thiosulphate solution. (ii) To the second portion, add silver nitrate solution followed by excess ammonia solution. (iii) To the third portion, add copper(II) sulphate solution followed by 4 drops of starch indicator. 159 Deductions (iv) To the third portion, add 2cm3 of jik followed by concentrated nitric acid followed by 3cm3 of carbon tetrachloride. (d) Wash the residue in (c) and dissolve it in minimum amount of dilute nitric acid. (Do not divide the resultant solution) (i) To 1cm3 of the resultant solution, add dilute sodium hydroxide solution drop-wise until in excess. (ii) To 1cm3 of the resultant solution, add 3-4 drops of potassium iodide solution. (iii) To 1cm3 of the resultant solution, add dilute ammonia solution drop-wise until in excess. (e) To the remaining solution in (d) above, add dilute ammonia solution drop-wise until in excess. Filter and keep the filtrate. (f) To the filtrate in (e) above, add dilute nitric acid drop-wise until the solution is just acidic. Divide the resultant solution into three portions. 160 (i) To the first portion, add dilute sodium hydroxide solution drop-wise until in excess. (ii) To the second portion, add dilute ammonia solution drop-wise until in excess. (iii) Use the third portion to carry out a test of your own choice to confirm the second cation in N. (g) Identify the; (i) Cations in N …………………………………… and ………………………………………. (ii) Anions in N …………………………………… and ………………………………………. 161 ORGANIC QUALITATIVE ANALYSIS Organic qualitative analysis involves identifying the nature of the functional group of a given organic compound. The nature of the organic compound can be obtained when the organic compound is burnt i.e when an organic compound burns with a non – sooty flame, the organic compound is aliphatic and when it burns with a sooty flame, the organic compound is aromatic. Functional groups are identified using different reagents after dissolving the organic compound in water and testing the resultant solution with a litmus paper. When the resultant solution is acidic (turns blue litmus paper red), then a carboxylic acid, an acid chloride and acid anhydride, should be suspected. When the resultant solution is neutral (has no effect on litmus paper), then an alcohol, carbonyl compound and ester should be suspected. When the resultant solution is alkaline (turns red litmus paper blue), then an amine should be suspected. The following are tests for some common functional groups. 1. Test for carboxyl group (-COOH) To the suspected organic compound, Add sodium carbonate solution or sodium hydrogencarbonate solution or magnesium metal. When effervescence of a colourless gas occurs, then a carboxylic acid is confirmed. 2CH3COOH(l) + Na2CO3(aq) 2CH3COONa(aq) + CO2(g) + H2O(l) CH3COOH(l) + NaHCO3(aq) CH3COONa(aq) + CO2(g) + H2O(l) 2CH3COOH(l) + Mg(s) (CH3COO)2Mg(aq) + H2(g) Add an alcohol (ethanol) followed by a few drops of concentrated Sulphuric acid and heat the mixture. When a sweet fruity smell is observed (an ester) then a carboxylic acid is confirmed. CH3COOH(aq) + CH3CH3OH(l) CH3COOCH2CH3 (aq) + H2O(l) Add phosphorous(V) chloride . When white fumes of the Hydrogen chloride gas is produced. Then a carboxylic acid is highly suspected. CH3COOH(l) + PCl5(g) CH3 COCl(l) + POCl3(s) + HCl(g) Using sulphur dichloride oxide (thionyl chloride) When white fumes of the Hydrogen chloride gas is produced. Then a carboxylic acid is highly suspected. CH3COOH + SOCl2 (s) CH3COCl + SO2 + HCl 162 2. Test for carbonyl group. To the suspected organic compound, add Brady’s reagent (2,4dinitrophenylhydrazine solution) When a yellow precipitate is formed, then an aldehyde or ketone should be suspected. Differentiating between aldehydes and ketones Aldehydes are easily oxidized to corresponding carboxylic acids while ketones are resistant to oxidation. (cannot be oxidized) Therefore aldehydes are differentiated from ketones by using strong and mild oxidizing agents such as (a) Acidified potassium dichromate(VI) solution and the mixture warmed. With an aldehyde, the orange solution turns green. With a ketone, there is no observable change. (b) Acidified potassium manganate(VII) solution and the mixture warmed. With an aldehyde, the purple solution turns colourless. With a ketone, there is no observable change. (c) Tollen’s reagent (Ammoniacal silver nitrate solution) With aldehydes, a silver mirror is observed on heating. With ketones, there is no observable change. CH3CHO(l) Ag(NH3)2+(aq) Ag(s) + CH3COO-(aq) (d) Fehling’s solution (Ammoniacal copper(II) sulphate solution) With aldehydes, a reddish-brown precipitate is observed on heating. With ketones, there is no observable change. CH3CHO(l) Fehling’s solution Cu2O(s) + CH3COO-(aq) Note Carbonyl compounds with a methyl group attached to carbonyl carbon form a yellow precipitate with Iodine solution in presence of sodium hydroxide solution. CH3CHO(l) I2(aq)/NaOH(aq) CHI3(s) + HCOONa(aq) 3. Test for hydroxyl (-OH) group. The following reagents can be used to confirm whether the organic compound is an alcohol. (a) Using sodium metal Effervescence of a colourless gas is observed. CH3CH2OH(l) + Na(s) CH3CH2ONa(aq) + ½ H2 (g) (b) Using phosphorous(V) chloride . White fumes of the hydrogen chloride gas is produced. CH3CH2OH(l) + PCl5 CH 3CH2Cl(l) + POCl3(s) + HCl(g) (c) Using sulphur dichloride oxide (thionyl chloride) White fumes of the hydrogen chloride gas is produced. CH3CH2OH + SOCl2 CH3CH2Cl + SO2 + HCl (d) Using a carboxylic acid (ethanoic acid) followed by a few drops of concentrated Sulphuric acid and the mixture heated. A sweet fruity smell is observed (an ester is formed). CH3COOH(l) + CH3CH3OH(l) CH3COOCH2CH3 (l) + H2O(l) 163 Distinguishing between classes of alcohols. Primary, secondary and tertiary alcohols can be distinguished using; 1. Anhydrous zinc chloride and concentrated hydrochloric acid. (Lucas reagent) With a primary alcohol, there is no observable change at room temperature. With a secondary alcohol, a cloudy solution forms between 5-10 minutes. With a tertiary alcohol, a cloudy solution forms immediately. 2. Using an oxidizing agent such as acidified potassium dichromate(VI) solution. With tertiary alcohols there is no observable change. [They are resistant to oxidation] With primary and secondary alcohols, the orange solution turns green. However, on addition of Brady’s reagent to the resultant solution, a yellow precipitate is formed for the case of secondary alcohols and no observable change for primary alcohols. Note: Secondary and primary alcohols with a methyl group attached to the carbon atom carrying the hydroxyl group form a yellow precipitate with iodine solution in sodium hydroxide solution. CH3CH2OH(l) I2(aq)/NaOH(aq) CHI3(s) + HCOONa(aq) 4. Test for an amine group. Amines are identified using a mixture of sodium nitrite and concentrated hydrochloric acid (Nitrous acid) below 50C. With a primary aromatic amine, there is no observable change, but effervescence of a colourless gas occurs on warming. With a primary aliphatic amine, effervescence of a colourless gas occurs below 5°C. With a secondary amine, a yellow oily liquid is observed. With a tertiary amine, there is no observable change. SUMMARY TESTS ON ORGANIC SAMPLES. 1. Burning /combustion. Observation Deduction. Burns with yellow non-sooty Saturated aliphatic compound of low C:H ratio flame Burns with yellow sooty flame Aromatic compound 2. Solubility in water Observation Miscible/soluble in water. Deduction Polar compound of low molecular mass. 164 Sparingly miscible/soluble in water. Polar compound of high molecular mass. 3. Solubility in NaOH solution. (If compound was immiscible with water) Observation Deduction Soluble Acidic compound, phenol or carboxylic acid present. Insoluble Basic compound, amine present. 4. Testing the solution with litmus Observation Solution has no effect on litmus paper. Solution turns blue litmus paper red. Solution turns red litmus paper to blue. Deduction Neutral compound, alcohol or carbonyl compound present Acidic compound, carboxylic acid or phenol present Basic compound, amine or salt of carboxylic acid. 5. Action of sodium hydrogencarbonate or sodium carbonate (solid or solution) or magnesium ribbon. Observation Deduction Bubbles of a colourless gas. Carboxylic acid present No observable change. Carboxylic acid absent 6. Alcohol with conc. H2SO4 (esterification) Observation Deduction Sweet fruity smell Ester formed. Therefore, carboxylic acid present. No observable change Carboxylic acid absent. 7. Action of acidified potassium dichromate(VI) solution Observation Deduction Orange solution turns Reducing agent present, primary alcohol, secondary green. alcohol, aldehyde or methanoic acid present. No observable change Reducing agent absent, primary alcohol, secondary alcohol, aldehyde or methanoic acid absent. 8. Action of sodium metal. Observation Deduction Bubbles of a colourless Alcohol present. gas. 9. Brady’s reagent. (2,4–dinitrophenylhydrazine solution) Observation Deduction Yellow precipitate Carbonyl compound present No observable change Carbonyl compound absent 165 10. Sodium hydrogensulphite solution. Observation White precipitate No observable change Deduction Carbonyl compound present Carbonyl compound absent 11. Lucas reagent (Anhydrous zinc chloride and concentrated hydrochloric acid) Observation Deduction Cloudy solution formed immediately. Tertiary alcohol Cloudy solution formed between 5-10 Secondary alcohol minutes No observable change Primary alcohol 12. Tollen’s Reagent (Ammoniacal silver nitrate solution) Observation Deduction Silver mirror Aldehyde present (if carboxylic acid, then methanoic acid) No observable Aldehyde absent. change 13. Fehling’s solution Observation Deduction A reddish-brown precipitate. Aldehyde present. (If carboxylic acid, then methanoic acid) No observable change. Aldehyde absent. 14. Iodine solution and sodium hydroxide solution. (Iodoform) Observation Deduction Yellow CH3CH2OH, CH3CH(OH)R, CH3CHO or CH3COR precipitate Note: Ethanol is the only primary alcohol and ethanal is the only aldehyde that gives positive iodoform test. 15. Neutral iron(III) chloride solution. Observation Violet/purple colouration. No observable change. Brown precipitate. 16. Bromine water Observation White precipitate. Deduction Phenol present Phenol absent Benzoic acid present Deduction Phenol (also aromatic amine, in case solution was alkaline) 166 Commenting Aliphatic (or aromatic) Low C:H ratio ie saturated (or high C:H ratio i.e unsaturated) Functional group alcohol, aldehyde, ketone, carboxylic acid or phenol Primary or secondary or tertiary (where applicable) CH3CH2OH, CH3CH(OH)R, CH3CHO or CH3COR (where applicable) Experiment 62 You are provided with an organic compound A. You are required to carry out tests below on A and describe the nature of A. Record your observations and deductions in the table below. TESTS OBSERVATIONS DEDUCTIONS (a) Burn a small amount of A on a spatula end. (b) To about 0.5cm3 of A, add 1 cm3 water, shake and test the mixture with litmus paper. (c) To about 1cm3 of A, add 2-3 drops of neutral iron(III) chloride solution. (d) To about 1cm3 of A, add 3- 4 drops of Brady’s reagent. (e) To about 1cm3 of A, add 4-5 drops of acidified potassium dichromate(VI) solution and heat. (f) To about 1cm3 of A, add 4 cm3 of iodine solution followed by sodium hydroxide solution drop-wise until the solution is paleyellow. Warm and allow to cool. (g) Describe the nature of A. ………………………………………………………………………………………………………………………… ………………………………………………………………………………………………………………………… 167 Experiment 63 You are provided with an organic compound B. You are required to carry out tests below on B and describe the nature of B. Record your observations and deductions in the table below. TESTS OBSERVATIONS DEDUCTIONS (a) Burn a small amount of B on a spatula end (b) To about 0.5cm3 of B, add 1 cm3 water, shake and test the mixture with litmus paper. (c) To about 1cm3 of B, add 2-3 drops of neutral iron(III) chloride solution. (d) To about 1cm3 of B, add 3- 4 drops of Brady’s reagent. (e) To about 1cm3 of B, add 4-5 drops of acidified potassium dichromate(VI) solution and heat. Allow to cool and use it in part (f). (f) To the mixture from (e), add 3-4 drops of Brady’s reagent. (g) To about 1cm3 of B, add 2cm3 of Lucas reagent. (h) Describe the nature of B. ………………………………………………………………………………………………………………………… ………………………………………………………………………………………………………………………… ………………………………………………………………………………………………………………………… 168 Experiment 64 You are provided with an organic compound C. You are required to carry out tests below on C and describe the nature of C. Record your observations and deductions in the table below. TESTS OBSERVATIONS DEDUCTIONS (a) Burn a small amount of C on a spatula end (b) To about one spatula end-full of C, add 1cm3 water, shake and test the mixture with litmus paper. Divide the resultant solution into five portions. (i) To the first portion, add 2-3 drops of neutral iron(III) chloride solution. (ii) To the second portion, add half a spatula end-full of sodium carbonate. (iii) To the third portion, add 3- 4 drops of 2,4dinitrophenylhydrazine solution. (iv) To the fourth portion, add 4-5 drops of acidified potassium dichromate(VI) solution and heat. (v) To the fifth portion, add an equal volume of ethanol followed by 2-3 drops of concentrated Sulphuric acid and heat the mixture. (c) Describe the nature of C. ………………………………………………………………………………………………………………………… ………………………………………………………………………………………………………………………… ………………………………………………………………………………………………………………………… 169 Experiment 65 You are provided with an organic compound D. You are required to carry out tests below on D and describe the nature of D. Record your observations and deductions in the table below. TESTS OBSERVATIONS DEDUCTIONS (a) Burn a small amount of D on a spatula end. (b) To about 1cm3 of D, add 2 cm3 water, shake and test the mixture with litmus paper. Divide the resultant solution into four portions. (i) To first portion, add 3- 4 drops of 2,4dinitrophenylhydrazine solution. (ii) To the second portion, add half a spatula end-full of sodium hydrogencarbonate. (iii) To the third portion, add 2-3 drops of neutral iron(III) chloride solution. (iv) To the fourth portion, add 4-5 drops of acidified potassium dichromate(VI) solution and heat. (c) To 1cm3 of D, add an equal volume of ethanoic acid followed by 2-3 drops of concentrated Sulphuric acid and heat the mixture. Pour it in a beaker of cold water and allow to stand. (d) To 1cm3 of D, add 2-3 drops of concentrated Sulphuric acid and heat. Pass the vapour evolving into a test tube containing acidified potassium manganate(VII) solution. 170 (e) To 1cm3 of D, add 2cm3 of Luca’s reagent. (f) Describe the nature of D. ………………………………………………………………………………………………………………………… ………………………………………………………………………………………………………………………… ………………………………………………………………………………………………………………………… Experiment 66 You are provided with an organic compound E. You are required to carry out tests below on E and describe the nature of E. Record your observations and deductions in the table below. TESTS OBSERVATIONS DEDUCTIONS (a) Burn a small amount of E on a spatula end (b) To half a spatula endfull of E in a test tube, add sodium hydroxide solution and shake vigorously. (c) To about one spatula end-full of E in a boiling tube, add about 5cm3 of water, shake. Heat and test the resultant solution with litmus paper. Divide the resultant solution into three portions. (i) To the first portion of the hot solution, add 2-3 drops of neutral iron(III) chloride solution. (ii) To the second portion of the hot solution, add half a spatula end-full of sodium carbonate. (iii) To the third portion of the hot solution, add 3- 4 drops of Brady’s reagent. 171 (d) To half a spatula endfull of E in a test tube, add about 2cm3 of methanol. Shake to dissolve and then add 2-3 drops of concentrated Sulphuric acid and heat the mixture. Pour the contents into a beaker of cold water. (e) Describe the nature of E. ………………………………………………………………………………………………………………………… ………………………………………………………………………………………………………………………… ………………………………………………………………………………………………………………………… Experiment 67 You are provided with an organic compound F. You are required to carry out tests below on F and describe the nature of F. Record your observations and deductions in the table below. TESTS OBSERVATIONS DEDUCTIONS (a) Burn a small amount of F on a spatula end (b) To about 1cm3 of F, add 1 cm3 water, shake and test the mixture with litmus. (c) To about 1 cm3 of F, add 2-3 drops of neutral iron(III) chloride solution. (d) To about 1 cm3 of F, add 3- 4 drops of Brady’s reagent. (e) To about 1cm3 of F, add 2-3 drops of sodium carbonate solution. 172 (f) To about 1 cm3 of F, add 4-5 drops of acidified potassium dichromate(VI) solution and heat. Then add 1cm3 of ethanol followed by 23 drops of concentrated Sulphuric acid and heat. Pour the mixture into a small beaker of cold water. (g) To about 1cm3 of F, add 4 cm3 of iodine solution followed by sodium hydroxide solution drop-wise until the solution is paleyellow. Warm and allow to cool. (h) To about 1cm3 of F, add about 1cm3 of Tollen’s reagent and heat gently. (i) Describe the nature of F. ………………………………………………………………………………………………………………………… ………………………………………………………………………………………………………………………… ………………………………………………………………………………………………………………………… Experiment 68 You are provided with an organic compound G. You are required to carry out tests below on G and describe the nature of G. Record your observations and deductions in the table below. TESTS OBSERVATIONS DEDUCTIONS (a) Burn a small amount of G on a spatula end (b) To about 1cm3 of G, add 1 cm3 water, shake and test the mixture with litmus paper. 173 (c) To about 1 cm3 of G, add 2-3 drops of neutral iron(III) chloride solution. (d) To about 1 cm3 of G, add 3- 4 drops of Brady’s reagent. (e) To about 1cm3 of G, add half a spatula endfull of magnesium powder. (f) To about 2cm3 of G, add 2cm3 of sodium hydroxide solution, shake well and boil the mixture. Cool for 1 minute and add 2cm3 of dilute nitric acid followed by 3 drops of silver nitrate solution and filter. (g) To the filtrate in (f), add an equal volume of ethanol followed by 2-3 drops of concentrated Sulphuric acid and heat. Pour the mixture into a small beaker of cold water. (h) Describe the nature of G. ………………………………………………………………………………………………………………………… ………………………………………………………………………………………………………………………… ………………………………………………………………………………………………………………………… Experiment 69 You are provided with an organic compound H. You are required to carry out tests below on H and describe the nature of H. Record your observations and deductions in the table below. TESTS OBSERVATIONS DEDUCTIONS (a) Burn a small amount of H on a spatula end 174 (b) To about 2cm3 of H, add 4 cm3 water, shake and test the resultant solution with litmus paper. Divide the resultant solution into five portions. (i) The first portion, add 34 drops of sodium carbonate solution. (ii) To the second portion, add 3-4 drops of acidified potassium dichromate(VI) solution and heat. (iii) To the third portion, add 2-3 drops of 2,4dinitrophenylhydrazine solution. (iv) To fourth portion, add ammoniacal silver nitrate solution and heat. (v) To the fifth portion, add an equal volume of ethanol followed by 2-3 drops of concentrated Sulphuric acid and heat the mixture. Pour it in a beaker of cold water. (f) Describe the nature of H. ………………………………………………………………………………………………………………………… ………………………………………………………………………………………………………………………… ………………………………………………………………………………………………………………………… 175 Experiment 70 You are provided with an organic compound I. You are required to carry out tests below on I and describe the nature of I. Record your observations and deductions in the table below. TESTS OBSERVATIONS DEDUCTIONS (a) Burn a small amount of I on a spatula end (b) To about 1cm3 of I, add 1 cm3 water, shake and test the mixture with litmus paper. Divide the mixture into two portions. (i) To the first portion, add 2-3 drops of neutral iron(III) chloride solution. (ii) To second portion, add 3- 4 drops of Brady’s reagent. (c) To about 1cm3 of I, add 2-3 drops of concentrated Sulphuric acid. Heat the mixture and pass the gas through acidified potassium manganate(VII) solution. (d) To about 1 cm3 of I, add 4-5 drops of acidified potassium dichromate(VI) solution and heat. Divide the resultant solution into two portions. (i) To the first portion, add 3- 4 drops of Brady’s reagent. (ii) To the second portion, add about 1cm3 of Fehling’s solution and heat. 176 (e) To about 1cm3 of I, add 4 cm3 of iodine solution followed by sodium hydroxide solution drop-wise until the solution is paleyellow. Warm and allow to cool. (f) To about 1cm3 of I, add 1cm3 of Lucas reagent. (i) Describe the nature of I. ………………………………………………………………………………………………………………………… ………………………………………………………………………………………………………………………… ………………………………………………………………………………………………………………………… Experiment 71 You are provided with an organic compound J. You are required to carry out tests below on J and describe the nature of J. Record your observations and deductions in the table below. TESTS OBSERVATIONS DEDUCTIONS (a) Burn a small amount of J on a spatula end (b) To about 2cm3 of J, add 2 cm3 water, shake and allow to stand. Test the mixture with litmus paper. Divide the mixture into two portions. (i) To the first portion, add 2-3 drops of neutral iron(III) chloride solution. (ii) To second portion, add a spatula end-full of sodium carbonate. 177 (c) To about 1 cm3 of J, add 4-5 drops of acidified potassium dichromate(VI) solution and heat (d) To about 1 cm3 of J, add 3- 4 drops of Brady’s reagent. (e) To about 1cm3 of J, add Tollen’s reagent and heat. (f) To about 1cm3 of J, add 4 cm3 of iodine solution followed by sodium hydroxide solution drop-wise until the solution is paleyellow. Warm and allow to cool. (g) Describe the nature of J. ………………………………………………………………………………………………………………………… ………………………………………………………………………………………………………………………… ………………………………………………………………………………………………………………………… Experiment 72 You are provided with an organic compound K. You are required to carry out tests below on K and describe the nature of K. Record your observations and deductions in the table below. TESTS OBSERVATIONS DEDUCTIONS (a) Burn a small amount of K on a spatula end (b) To about 2cm3 of K, add 2 cm3 water, shake and test the mixture with litmus paper. Divide the mixture into three portions. (i) To the first portion, add 2-3 drops of neutral iron(III) chloride solution. 178 (ii) To second portion, add 2-3 drops of Brady’s reagent. (c) To the third portion of the mixture from (b), add 4-5 drops of acidified potassium manganate(VII) solution and heat gently. Allow to cool and divide the resultant solution into three portions. (i) To the first portion, add 3- 4 drops of Brady’s reagent. (ii) To the second portion, add 2-3 drops of acidified potassium dichromate(VI) solution and heat. (iii) To the third portion, add 4-5 drops of Fehling’s solution and heat. (d) To about 1cm3 of K, add 1cm3 of Lucas reagent. (e) To about 1cm3 of K, add 4 cm3 of iodine solution followed by sodium hydroxide solution drop-wise until the solution is paleyellow. Warm and allow to cool. (f) Describe the nature of K. ………………………………………………………………………………………………………………………… ………………………………………………………………………………………………………………………… ………………………………………………………………………………………………………………………… 179 Experiment 73 You are provided with an organic compound L. You are required to carry out tests below on L and describe the nature of L. Record your observations and deductions in the table below. TESTS OBSERVATIONS DEDUCTIONS (a) Burn a small amount of L on a spatula end (b) To one spatula endfull of Z in a test tube, add about 2cm3 of sodium hydroxide solution and shake. (c) Shake one spatula end-full of L with about 4cm3 of water and test the mixture with litmus paper. Divide the mixture into five portions. (i) To the first portion, add 2-3 drops of neutral iron(III) chloride solution. (ii) To second portion, add 2-3 drops of Brady’s reagent. (iii) To the second portion, add 1cm3 of sodium carbonate solution. (iv) To the fourth portion, add soda lime and heat. (d) To the fifth portion of the solution from (c), add 4-5 drops of acidified potassium manganate(VII) solution and heat. Divide the resultant solution into two portions. 180 (i) To the first portion, 1cm3 of Brady’s reagent. Shake and allow to stand for about 2 minutes. (ii) To the second portion, add Tollen’s reagent and heat. (e) Dissolve a spatula end-full of L in water and add Lucas reagent. (f) Describe the nature of L. ………………………………………………………………………………………………………………………… ………………………………………………………………………………………………………………………… ………………………………………………………………………………………………………………………… Experiment 74 You are provided with an organic compound M. You are required to carry out tests below on M and describe the nature of M. Record your observations and deductions in the table below. TESTS OBSERVATIONS DEDUCTIONS (a) Burn a small amount of M on a spatula end (b) To about 0.5 cm3 of M, add 1 cm3 water, shake and test the mixture with litmus paper. (c) To about 1 cm3 of M, add 2-3 drops of neutral iron(III) chloride solution. (d) To about 1cm3 of M, add sodium carbonate solution. (e) To about 1 cm3 of M, add 4-5 drops of acidified potassium dichromate(VI) solution and heat. 181 (f) To about 1 cm3 of M, add ammoniacal silver nitrate solution and heat. (h) Describe the nature of M. ………………………………………………………………………………………………………………………… ………………………………………………………………………………………………………………………… ………………………………………………………………………………………………………………………… Experiment 75 You are provided with an organic compound N. You are required to carry out tests below on N and describe the nature of N. Record your observations and deductions in the table below. TESTS OBSERVATIONS DEDUCTIONS (a) Burn a small amount of N on a spatula end. (b) Shake one spatula end-full of N with about 6cm3 of water and test the mixture with litmus paper. Divide the mixture into five portions. (i) To the first portion, add sodium hydroxide solution. (ii) To the second portion, add a spatula end-full of sodium carbonate. (iii) To third portion, add 4-5 drops of acidified potassium manganate(VII) solution and heat. 182 (iv) To the fourth portion, add 2-3 drops of Brady’s reagent. (v) To the fifth portion, add 2-3 drops of neutral iron(III) chloride solution.. (f) Describe the nature of N. ………………………………………………………………………………………………………………………… ………………………………………………………………………………………………………………………… ………………………………………………………………………………………………………………………… 183