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EXPERIMENT 3 ACID-BASE TITRATION BETWEEN PHOSPHORIC(V) ACID AND SODIUM HYDROXIDE The aim of the experiment is to investigate the

reaction between phosphoric(V) acid, H3PO4, and sodium hydroxide, NaOH. It is possible that reaction produces NaH2PO4, Na2HPO4, or Na3PO4. Three chemicals are provided in this practical: Solution G is aqueous sodium hydroxide containing 4.40 g of NaOH in 1.00 dm3 of solution. Liquid H is a concentrated aqueous solution of phosphoric acid, H3PO4. Phenolpthalein solution. Procedure Record all your readings in the space provided. Place approximately 20 cm3 of deionised water into the volumetric flask provided. Weigh the flask and water. Next place about 1 cm3 of phosphoric acid, H, into your volumetric flask. Reweigh the flask with the phosphoric acid and water. Add deionised water and make up the solution to 250 cm3. Mix this solution thoroughly before using it for your titrations. Label this solution J. Fill the burette with aqueous NaOH, G. Using a pipette transfer 25 cm3 of solution J into a conical flask. Add about 3 drops of phenolphthalein indicator Titrate solution J with solution G from the burette. The end-point is when the indicator changes from colourless to pale pink. Repeat the titration and obtain two consistent values for the titre. In each case use 25.0 cm3 of solution J. Results Weighings Mass of volumetric flask + water + phosphoric acid / g Mass of volumetric flask + water /g Mass of phosphoric acid used / g 235.65 234.03 1.62

Mass of H used = ___1.62____ g Titration data (tabulated) 1 Final burette reading / cm3 Initial burette reading / cm3 Volume of NaOH(aq) used / cm3 2 3

32.50 28.35 26.55 7.70 2.55 0.65

24.80 25.80 25.90

Mean titre = 25.80 + 25.90 = 25.85 2

Summary 25.0 cm3 of solution J required a mean titre of .........25.85...... cm3 of solution G. Show the readings you used to obtain this value of the volume of G by putting a () under these readings. Skill Assessment Procedural safety State and explain what you would do if some phosphoric acid, H, splashed onto your hand ....... Wash thoroughly with water or with dilute sodium carbonate ......................................................................................................................................................... Skill Assessment Analysing (a) The phosphoric acid, H, used in this experiment was 85% pure by mass. Calculate the mass of pure H3PO4 you weighed out. 1.62 g 85 = 1.377 g 100 (b) Calculate the number of moles of H3PO4 in the 250 cm3 of solution you made up. 1.377 g = 0.0139 mols 99 g/mol

(c)

Calculate the number of moles of H3PO4 used in each titration. 0.0139 mol 25 cm3 = 0.00139 mol 250 cm3

(d)

Calculate the concentration of NaOH, in mol dm-3, in G. Concentration (mol dm-3) = 4.40 g dm-3 = 0.11 mol dm-3 -1 40 g mol

(e)

Calculate the number of moles of NaOH used in the mean titre. Number of mole = 0.11 mol dm-3 (25.85 10-3) dm3 = 2.844 10-3 mol

(f)

Use your answers to (c) and (e) to calculate how many moles of NaOH react with 1 mol H3PO4. Show your working and give your answers to the nearest whole numbers. 2.844 10-3 mol of NaOH reacted with 0.00139 mol of H3PO4 So, 1 mol of H3PO4 reacts with , 2.844 10-3 mol = 2 NaOH 0.00139

(g)

There are three possible reactions of NaOH with H3PO4, shown by the equations below. NaOH + H3PO4 NaH2PO4 + H2O 2NaOH + H3PO4 Na2HPO4 + 2H2O 3NaOH + H3PO4 Na3PO4 + 3H2O Put a tick () next to the equation which corresponds most closely to your answer to (f). Justify your answer

............End point is reached when the phosphoric acid completely reacts with NaOH. The mole ratio of J to G is 1:2. This means that 1 mole phosphoric acid reacts with 2 moles of NaOH ......................................................................................................................................................... .

Skill Assessment Evaluating (a) Why should the diluted solution of phosphoric acid in the volumetric flask be shaken

thoroughly before using it for the titration? ..... To mix the solution thoroughly and obtain a homogeneous solution ......................................................................................................................................................... . (b) State two advantages of doing a trial titration before carrying out the accurate ones.

....1 To check that the volume of titrants used are appropriate. ....2. To become familiar with colour change of indicator ....3. So that the subsequent accurate titrations can be carried out rapidly .....4. So that the final addition, near end point,can be done by dropwise addition ......................................................................................................................................................... ......................................................................................................................................................... .. (c) It is important that solutions of sodium hydroxide, such as G, are supplied in stoppered bottles. This is to prevent the reaction of sodium hydroxide with an acidic gas present in air. Suggest which gas in air would react with sodium hydroxide and give a balanced equation for the reaction.

.................Carbon dioxide ................. 2 NaOH + CO2 Na2CO3 + H2O or NaOH + CO2 NaHCO3 ......................................................................................................................................................... .. (d) Some 25.0 cm3 pipettes are calibrated to within 0.06 cm3. Calculate the possible percentage error when such a pipette is used 0.06 100 % = 0.24 % 25.0

(e)

Assume that the balance you used was accurate to within 0.01 g. The balance was used to determine the mass of phosphoric acid H,. Comment on the significance of the percentage errors with using the balance and the pipette in this experiment. .Mass error = (0.01 100% ) 2 = 1.25 % 1.65 The percentage error using the balance and pipette are relatively small. The percentage error due to weighing is higher than that due to the pipette since the mass weighed out was very small

(e)

Another student carried out a similar titration to obtain more evidence about the reaction taking place between phosphoric acid and sodium hydroxide. She used 0.0030 mol of NaOH to neutralise the phosphoric acid. The student calculated the mass of crystals that would be expected from each of the three possible reactions shown earlier. Below each equation write the masses of crystal expected according to the three equations in the boxes provided.

. NaOH + H3PO4 NaH2PO4 + H2O 0.36 2NaOH + H3PO4 Na2HPO4 + 2H2O 0.21 3NaOH + H3PO4 Na3PO4 + 3H2O 0.164 (f) After the titration, the student allowed the contents of the filtration flask to evaporate completely at room temperature for several days. At the end of that time, 0.54 g of colourless crystals were obtained at the bottom of the flask. Comment on the students result and suggest a possible reason for it. 0.54 g is much higher than expected. Mass expected should be between 0.36 and 0.164 g. The larger mass may be due to crystallisation of water with the product.