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Practical Guide EDEXCEL

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Practical Guide EDEXCEL Practical Guide EDEXCEL This guide includes details about the core practicals for A-level chemistry. It also contains information about other experiments that often occur in A-level examinations. You may be asked to describe these experiments in details or be asked about reasons for doing individual steps. You may be asked about other unfamiliar experiments but these will be using the skills and techniques that are described in the following experiments. Safety and hazards Irritant - dilute acid and alkalis- wear googles Hazardous substances in low Corrosive- stronger acids and alkalis wear goggles concentrations or amounts will Flammable – keep away from naked flames not pose the same risks as the Toxic – wear gloves- avoid skin contact- wash hands after use pure substance. Oxidising- Keep away from flammable / easily oxidised materials Measuring gas volumes Make sure you don’t leave gaps in Using a gas syringe your diagram where gas could Gas syringes can be used for a variety of escape experiments where the volume of a gas is measured, possibly to work out moles of gas or to follow reaction rates. Potential errors in using a gas syringe •gas escapes before bung inserted If drawing a gas syringe make sure •syringe sticks you draw it with some • some gases like carbon dioxide or sulphur dioxide are measurement markings on the soluble in water so the true amount of gas is not barrel to show measurements can measured. be made. The volume of a gas depends on pressure Alternatively gas volumes can be and temperature so when recording volume measured ‘over water’ with an up-turned it is important to note down the measuring cylinder in a trough of water temperature and pressure of the room. Moles of gas can be calculated from gas volume (and temperature and pressure) using ideal gas equation PV = nRT or using the molar gas volume (1mol gas =24dm3 at room temperature and pressure N Goalby chemrevise.org 1 Core Practical 1: Measure the molar volume of a gas Detailed method 1. Measure 30 cm3 of 1 mol dm 3 ethanoic acid and transfer to a conical flask. 2. Attach conical flask to gas syringe⁻ or use collection over 3 water method (see previous page) in cmin 3. Measure the mass of a weighing bottle with approximately 2 0.05 g of calcium carbonate 4. Add the calcium carbonate to the conical flask- quickly resealing the bung so no gas escapes 5. Measure the final total volume of gas 6. Reweigh the empty weighing bottle test tube from step 3 CO of Volume 7. Repeat the experiment several more times, increasing the mass of calcium carbonate by about 0.05 g each time. Mass of CaCO3 in g Analysis From the graph read the volume of CO2 given off with 0.25 g CaCO3 -3 Work out the moles of CaCO3 in 0.25g = 0.25/100.1 = 2.5 x 10 Assume the moles of CO2 = moles of CaCO3 Work out molar volume of CO2 = volume of CO2/ moles of CO2 Method for using a gas syringe to calculate the Mr of propanone 1. Extract 0.20 cm3 of propanone into a hypodermic syringe and then measure the mass of this syringe 2. using hand protection, remove a gas syringe from the oven and note the volume of air already in the barrel – about 5 cm3. 3. inject the propanone through the self-seal cap into the barrel. The plunger will move straight away. 4. Put the gas syringe back into the oven. 5. Measure the mass of the empty hypodermic syringe immediately. 6. After a few minutes measure the volume of the gas in the gas syringe, record the temperature of the oven shelf and the pressure of the room. Example 1 : 0.150g of a volatile liquid was injected into a sealed gas syringe. The gas syringe was placed in an oven at 70oC at a pressure of 100kPa and a volume of 80cm3 was measured. Calculate the Mr of the volatile liquid (R = 8.31) moles = PV/RT 100 kPa = 100 000 Pa = 100 000 x 0.00008 / (8.31 x 343) 80 cm3 = 0.00008 m3 = 0.00281 mol Mr = mass/moles = 0.15 / 0.00281 = 53.4 g mol-1 N Goalby chemrevise.org 2 Heating in a crucible This method could be used for measuring mass loss in various thermal decomposition reactions and also for mass gain when reacting magnesium in oxygen. The water of crystallisation in calcium sulfate crystals can be The lid improves the accuracy of the removed as water vapour by heating as shown in the following experiment as it prevents loss of solid equation. from the crucible but should be loose CaSO4.xH2O(s) → CaSO4(s) + xH2O(g) fitting to allow gas to escape. Method. •Weigh an empty clean dry crucible and lid . •Add 2g of hydrated calcium sulphate to the crucible and weigh again •Heat strongly with a Bunsen for a couple of minutes •Allow to cool •Weigh the crucible and contents again •Heat crucible again and reweigh until you reach a constant mass ( do this to ensure reaction is complete). Large amounts of hydrated calcium sulfate, such as 50g, should not be used in this experiment as the decomposition is likely to be incomplete. Small amounts of the solid , such as 0.100 g, should not be used in this The crucible needs to be dry otherwise a wet crucible would experiment as the percentage give an inaccurate result. It would cause mass loss to be too uncertainties in weighing will be too large as the water would be lost when heating. high. Example 2. 3.51 g of hydrated zinc sulfate were heated and 1.97 g of anhydrous zinc sulfate were obtained. Use these data to calculate the value of the integer x in ZnSO4.xH2O Calculate the mass of H2O = 3.51 – 1.97 = 1.54g Calculate moles of 1.97 Calculate moles of = 1.54 = H O ZnSO4 161.5 2 18 = 0.0122 =0.085 Calculate ratio of mole of = 0.0122 = 0.085 ZnSO4 to H2O 0.0122 0.0122 =7 =1 X = 7 N Goalby chemrevise.org 3 Core practical 2. Make up a volumetric solution and carry out a simple acid–base titration Making a solution • Weigh the sample bottle containing the required mass of solid Alternatively the known mass of solid on a 2 dp balance in the weighing bottle could be • Transfer to beaker transferred to beaker, washed and • Reweigh empty sample bottle washings added to the beaker. • Record the difference in mass • Add 100cm3 of distilled water to the beaker. Use a glass rod to stir to help dissolve the solid. •Sometimes the substance may not dissolve well in cold water so the beaker and its contents could be heated gently until all the solid had dissolved. Remember to fill so the bottom of the • Pour solution into a 250cm3 graduated flask via a funnel. meniscus sits on the line on the neck of the • Rinse beaker and funnel and add washings from the beaker flask. With dark liquids like potassium and glass rod to the volumetric flask. manganate it can be difficult to see the • make up to the mark with distilled water using a dropping meniscus. pipette for last few drops. • Invert flask several times to ensure uniform solution. Shake the volumetric flask thoroughly to ensure a uniform concentration A graduated flask has one mark on the neck which the level to fill to get the accurate volume. Do not heat or put hot solutions in the volumetric flask because the heat would cause the flask to expand and the volume would then be incorrect. Measuring mass accurately: In many experiments the best method for measuring mass is 1. Measure mass on 2 or 3d.p. balance of a weighing bottle with the required quantity of solid in it 2. Empty mass into reaction vessel/flask 3. Reweigh the now empty weighing bottle 4. Subtract the mass of the empty weighing bottle from the Graduated/volumetric flask first reading to give exact of mass actually added. Dilutions Diluting a solution Using a volumetric pipette is more accurate than a measuring cylinder because it has a 3 3 •Pipette 25cm of original solution into a 250cm volumetric smaller uncertainty flask •make up to the mark with distilled water using a dropping Use a teat pipette to make up to the mark in pipette for last few drops. volumetric flask to ensure volume of solution • Invert flask several times to ensure uniform solution. accurately measured and one doesn’t go over the line N Goalby chemrevise.org 4 Titrations Core Practical 3: Make up a volumetric solution and carry out a simple acid–base titration General Method •rinse equipment (burette with acid, pipette with alkali, conical flask with distilled water) •pipette 25 cm3 of alkali into conical flask •touch surface of alkali with pipette ( to ensure correct amount is added) •adds acid solution from burette •make sure the jet space in the burette is filled with acid •add a few drops of indicator and refer to colour change at end point •phenolphthalein [pink (alkali) to colourless (acid): end point pink colour just disappears] [use if NaOH is used] •methyl orange [yellow (alkali) to red (acid): end point orange] [use if HCl is used] •use a white tile underneath the flask to help observe the colour change •add acid to alkali whilst swirling the mixture and add acid drop wise at end point •note burette reading before and after addition of acid •repeats titration until at least 2 concordant results are obtained- two readings within 0.1 of each other Titrations are done often to find out the concentration of one substance by reacting it with another substance of known concentration.
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