EXPERIMENT 6 DETERMINATION OF MOLAR MASS OF A CARBOXYLIC ACID BY TITRATION WITH MANGANATE(VII) IONS Some organic acids can be identified

by determination of their relative molecular masses. In the case of carboxylic acids this can be done using a titration In this experiment, ou will determine the relative mass of a carboxylic acid whose formula can be represented as H2X. This acid is a reducing agent. You will carry out a redox titration using potassium manganate(VIII) FA1 is a solid sample of the carboxylic acid, H2X. FA2 is a 0.020 mol dm3 solution of potassium manganate(VII), KMnO4. Procedure: Do Not Use The Tare Function 1. Weigh the empty bottle provided. Add approximately between 1.50 and 1.60 g of FA1. Weigh the bottle + content accurately. Record the masses and all your other readings in the space provided Dissolve your solid H2X carefully in about 10 cm3 of deionised water. When all of the solid has dissolved, make the solution up to 250 cm3 in a volumetric flask using more deionised water. Label this solution as FA3. Fill the burette with FA2. Pipette 25.00 cm3 of FA3 into a conical flask, and add about 10 cm3 of dilute sulphuric acid. Put the conical flask and its contents on a tripod and gauze and heat them up to about 70 o C and then remove the Bunsen burner. Check the temperature of the mixture with a thermometer. Take out the thermometer before continuing with the next step. Titrate this solution with the manganate(VII) solution, FA2, until the first permanent pale pink colour remains in the solution. Add the solution FA2 slowly at first. Repeat the titration two more times. Record your results in space provided. Work out your mean titre by placing a tick under the readings used.

2.

3. 4.

5.

6.

Results

Summary 25.00 cm3 of FA3 reacted with __________ cm3 of FA2. Skil Assessment l: Analysis (a) Calculate how many moles of manganate(VII) ions were run into the conical flask. Mols of MnO4 = (16.90 10-3)dm3 0.02 mol dm3 = 3.384 10-4 mol

(b)

Calculate the concentration, in mol dm3, of the carboxylic acid, H2X, in the solution FA3. [In this reaction, 1 mole of manganate(VII) ions reacts with 2.5 moles of the H2X.] Mol of H2X used for titration = (3.384 10-4) mol 2.5 = 8.46 10-4 mol Concentration of H2Xin FA3 = 8.46 10-4 mol = 0.03384 mol dm-3 0.025 dm3

(c)

Calculate the amount, in moles, of H2X dissolved in 250 cm3 of solution in the volumetric flask. Mols of H2X = 0.0338 mol dm-3 0.250 dm3 = 8.46 10-3 mol

(d)

Hence calculate the relative molecular mass of H2X. 1.54 g 8.46 10-3 mol = 182.00 g mol-1

(e) The structural formula of H2X is (COOH)2.nH2O. Deduce the value of n, the number of moles of water of crystallization in one mole of H2X. Mass of nH2O = 182.00 90 = 92.00 g Mols of H2O = 92 g 18 g /mol = 5.11 5

n= 5

Skill Assessment Evaluating evidence and procedures Information The relative molecular mass of acid H2X was determined by a different method. H2X is a dibasic(diprotic) acid. A solution of H2X was made, using weighted quantities of the acid and water. This solution was allowed to react with excess sodium hydrogen carbonate, NaHCO 3, which was also weighed before use. HCO3- + H+ CO2 + H2O The reaction was carried out in a conical flask. As soon as the chemicals had been mixed, a close-fitting plug of cotton wool was put into the neck of the flask. Cotton wool plug

reagents When fizzing stopped, the flask and its contents were reweighed. Readings Mass of conical flask(empty) with cotton wool Mass of solid H2X used Mass of water used to dissolve H2X Mass of sodium hydrogen carbonate added Total mass of flask, cotton wool and all contents at the end of the reaction Questions (a) Use these data to: (i) calculate the amount, in moles, of CO2 released Mass of CO2 = (78.54 + 5.20 + 100 + 10.50) - 193.10 = 1.14 g CO2 Moles of CO2 = 1.14 g 44 g mol-1 = 0.026 mol = = = = 78.54 g 5.20 g 100.0 g 10.50 g

193.10 g

(ii)

deduce the amount, in moles, of H2X used 1 mol H2X releases 2 mol CO2 moles of H2X used in expt = 0.013 moles

(iii)

calculate the relative molecular mass of H2X. 5.20 g 0.013 moles = 400 g

(b) Why was the cotton wool plug used in the conical flask? 1 prevent loss of water / acid spray 2 3 Prevent dust from falling into the conical flask Allows gas to escape

(c) Discuss whether the result from this experiment would be more or less reliable if the chemicals were heated gently during the reaction. Explain your answer. 1 Heating would speed up rate of reaction, since the acid used a weak, dilute acid 2 It would ensure reaction is complete 3 Heating would reduce solubility of CO2 in solution and would cause all the gas to escape 4 Water may evaporate 5 NaHCO3 decomposes when heated. More CO2 would be formed. (d) This experiment gives a larger value for the relative molecular mass of H2X than the titration method you carried out. Identify three sources of inaccuracy for the experiment involving sodium hydrogen carbonate. 1 experiment not repeated for consistent value. 2 Some CO2 dissolves in the solution, so not all of it escapes 3 CO2 is trapped in the flask, making the final mass of flask heavier 4 In the experiment, weighing is done 5 times. there is significant cumulative error 5 reaction may be incomplete. The flask should have been weighed repeatedly until mass stays constant.

Less reliable

EXPERIMENT 7 DETERMINATION OF THE PERCENTAGE OF WATER OF CRYSTALLISATION IN HYDRATED MAGNESIUM SULPHATE

Many salts contain water of crystallization. These are called hydrated salts. One example is the hydrated salt MgSO4 .nH2O. 1 mole of MgSO4.nH2O contains n moles of H2O When many hydrated compounds are heated, they lose their water of crystallisation. The residue is an anhydrous compound, which contains no water. You are provided with a sample of hydrated magnesium sulphate. You are to determine the percentage by mass of water of crystallisation in the salt and the value of n. Procedure Note. Your balance may have a tare facility, but this facility should not be used in this experiment. 1. 2. 3. Weigh accurately an empty crucible and lid. Add between 2.00 g and 2.50 g of MgSO4.nH2O and weigh accurately the crucible and lid. Support the crucible on a tripod using a pipe-clay triangle. Heat the crucible gently, with the lid off, for about one minute Then heat it strongly for a further 4 minutes Put the lid on and leave the crucible to cool for at least 5 minutes. When the crucible is cool, weigh it with the contents and the lid Remove the lid. Heat the crucible and contents again for two minutes. Replace the lid. Cool, then weigh the crucible, lids and contents.

4. 5. 6.

Prepare two tables to record your weighings in the space provided below. Table 1. Weighings before heating.

Mass of crucible + lid + MgSO4.xH2O / g Mass of empty crucible + lid / g Mass of MgSO4xH2O used /g

36.56 34.18 2.38

Table 2. Weighings after heating.

1 Mass of crucible + lid + residue

35.89 35.56 35.38 35.38

(a) What is the mass of water of crystallisation lost during heating? Show clearly the figures you use to calculate your answer. Mass of water of crystallization = 36.56 35.38 = 1.18 g

(b)

Calculate the percentage, by mass, of water of crystallisation present in FA4. 1.18 100% = 49.58% 2.38

(c)

Deduce how many moles of water of crystallization were lost. 1.18 g = 0.0656 mol 18 g mol-1

(d)

Determine the moles of anhydrous magnesium sulphate produced (2.38 1.18)g = 9.97 10-3 mols 120.4 g mol-1

(e)

Estimate the value of n in the formula, MgSO4nH2O. [Ar: H, 1.0; O, 16.0; Mg, 24.3; S, 32.1.] n= Mol of water of crystallisation = 6.58 7 Mol of anhydrous magnesium sulphate

Skill Assessment: Evaluation (a) Why was the sample of hydrated magnesium sulphate heated gently?

.To prevent spluttering as the water evaporates/boils off. (b) Explain why the residue was heated for a further two minutes after the third weighing in your experiment.

To ensure that all the water has been evaporated ......................................................................................................................................................... ......................................................................................................................................................... .. (c) Suggest two reasons why the hot crucible was cooled with the lid on before weighing it.

1 .To prevent the moisture in the air from rehydrating the anhydrous MgSO 4 2. Hot surfaces cause eddies that can result in inaccurate weighing ......................................................................................................................................................... . Skills assessment : Analysing and Evaluating Introduction The water of crystallisation in calcium sulphate crystals can be removed as water vapour by heating as shown in the following equation. CaSO4.xH2O(s) CaSO4(s) + xH2O(g) hydrated calcium anhydrous calcium sulphate sulphate A student weighed a clean dry crucible. The student transferred 0.250g of hydrated calcium sulphate to the crucible. The crucible was then heated. When the crucible and its contents had reached constant mass, the mass was recorded. The experiment was repeated using different masses of hydrated calcium sulphate. For each experiment, the student recorded the original mass of hydrated calcium sulphate and the mass of anhydrous calcium sulphate left after heating. The students results are shown in the table opposite. Mass CaSO4.xH2O/g Mass of CaSO4/g of 0.25 0.15 0.65 0.50 0.81 0.70 1.05 0.85 1.43 1.15 1.45 1.20

Analysis 1. Using the data provided above plot a graph. 2. Draw a best fit straight line on the graph

1.20

1.00 Mass of CaSO4 / g 0.80 0.60 0.40

0.20

0 0 0.20 0.40 0.60 0.80 1.00 1.20 1.40 Mass of CaSO4.xH2O / g

. 3.

Use the graph to determine the mass of hydrated calcium sulphate which would have formed 1.000 g of anhydrous calcium sulphate. 1.21 g of hydrated calcium sulphate would have formed 1.00 g of anhydrous calcium sulphate

4.

Calculate the number of moles of CaSO4 present in 1.000 g of anhydrous calcium sulphate. 1.000 g = 7.342 10-3 mol -1 136.2 g mol

5.

Use your answers to part 3 and part 4 to calculate the Mr of hydrated calcium sulphate. 1.21 g = 164.8 g /mol 7.342 10-3 mol

6.

Use your answer to part 5 to calculate the value of x in CaSO4.xH2O Mass of xH2O in 1 mol CaSO4.xH2O = 164.8 136.2 = 28.6 x = 28.6 = 1.588 2 18

7.

Assume that the maximum error in weighing 0.250 g on a balance was 0.001g. Calculate the percentage error in using the balance. 0.001 100% = 0.4% 0.250

Evaluation 1. Consider your graph and comment on the results obtained by the student. Is your line of best fit good enough for you to use with confidence? Identify any anomalous results. 1 Yes a good straight line 2. anomalous results are at 0.25g and 0.65 g ......................................................................................................................................................... ......................................................................................................................................................... .

2.

Explain why it was necessary for the student to heat the crucible to constant mass. To ensure all the water had been evaporated.

3.

Pure hydrated calcium sulphate has the formula CaSO4.2H2O Calculate the difference between the Mr determined in part 5 of the Analysis section and the Mr of the literature value, 172.2 Express this as a percentage of the Mr of the literature value. If you could not complete part 5 of the Analysis section, you should assume that the Mr determined from the graph is 165.2; this is not the correct result. Difference : 7.4 g

Percentage :

7.4 172.2

100% = 4.29 %

4.

Suggest one reason in each case why (a) small amounts of hydrated calcium sulphate, such as 0.100 g, should not be used in this experiment, % error will increase when small mass such as 0.10 g is used (b) large amounts of hydrated calcium sulphate, such as 50g, should not be used in this experiment.

The compound may not be completely dried