This chapter is designed to hel ed 10 help withthe internal ass It will also be useful in cis lend ee ear ty Util in answering question in Use Sen Practical work — for Cxample, enthaloy expemener tee Tests Tests for gases The fests used (0 identity the common laboratory gases have to be learnt. te is also important to be able to draw conclusions fom the identification of these gases. For example, if dilute sulfuric acid is added to a solidand a gare produced that turns limewater milky, the conclusions are tha = the gas is carbon dioxide = the unknown solid is a carbonate or a hydrogencarbonare Hydrogen Test: ignite the gas Observation: burns with a squeaky pop rogen is produced by = the reaction between an acid the reaction between an alcohol and sodium een water and either a group 1 metal, or calcium, strontium and a reactive metal m the reaction betw or barium Oxygen Test: place a glowing wooden splint in the gas Observation: splint catches fire Oxygen is produced by: = heating a group 1 nitrate (apart from LiNO3) = heating other nitrates, but NO, is also present = the catalytic decomposition of hydrogen peroxide, H,0, Carbon dioxide Test: Observation: pass gas into limewater limewater goes cloudy/milky Carbon dioxide is produced by: = the reaction between an acid and a carbonate or hydrogencarbonate ™ heating a carbonate (apart from sodium, potassium or barium carbonates) = heating a group 1 hydrogencarbonate Chapter 17: Laboratory chemistey 31S a aa aadplace damp red fitmus paper in the 3s vation: litmus paper goes blue ests, _ Obser t ctuced by: ania Micous sodiuin hyctroxide with an ammonium selt adding aqueous sodium hydroxide and aluminium powder to a nitrate Nitrogen dioxide. Tests ‘observe colour Observation: gas is brown “Nitrogen dioxide is produced by m heating a group 2 nitrate or lithium nitrate Chlorine Test: place damp litmus paper in the gas Observation: _titmus is rapidly bleached Chlorine is produced by: ‘electrolysis of a solution of a chloride adding dilute hydrochloric acid to a solution containing chlorate(t) ions Hydrogen chloride “Test: place damp blue litmus paper in the gas Observation: steamy fumes that turn damp litmus paper red place the stopper from a bottle of concentrated ammonia in the gas tvation: white smoke (ammonium chloride) is formed drogen chloride is produced by: hs reaction becween concentrated sulfuric acid and a chloride the reaction | Petween phosphorus pentachloride and either an alcohol orFlame tests ‘Fo carry out a flame test, a clean platinum or nichrome test wire is dipped into soncentrated hydrochloric acid, then into the solid to be tested and finally into howest part of a Bunsen flame. centrated hydrochloric acid converts some of the unknown solid into a ride. Chlorides are more volatile than other salts, so some of the unknown _gpes into the gas phase when heated in the hot flame. Aa electron is promoted energy level by the heat. It then falls back to the ground state and ‘of colour specific to the metal present in the compound. The colours in flame tests are given in Table 17:1. Flame colour Jonpresentin solid Table 17.1 Taine ee amecous. Yelow New ae & Yelowred Ge Red se Pelegreen Batt Or fiers tests connot be used on mires containing vo of thes ions because the colour produced by one of the ions will mask the colour produced by the other metal Fiame test is the only test fora group 1 metalin a compound. Precipitation reactions ici important to know which ionic compounds are soluble in water and which are insoluble. ‘Soluble ionic compounds incude: m= all group 1 selis 4 ail ammonium salts mall nitrates 4 ell chlorides. apart from silver chloride and lead(u) chloride, (The solubility ‘Cf bromides and iodides is similar to thar of chlorides.) *™ cll sulfates, apart from barium sulfate, strontium sulfate and lead(u) sulface. ‘alc sulfare and silver sulfate are slightly soluble,Solutions containing these ons are mixed ase Bat’ and SO. solutions of group 1% sulfate or from sulfuric acid) Batt and S03" (culate tons could be from sulfates, ammonium age and CC (silver ions are noemaly from 2 solution of silver nitrate) Ag’ and Br ‘Ag? and Io COs and any cation, other than a group 1 metal or ammonium (carbonate ions could be from solutions of group 1 carbonates or ammonium carbonate) ‘The ionic equations for these precipitation reactions will always be of the form: Result > white precipitate of barium sulfate ‘5 On adding dilute hydrachloricacié, the a precipitate remains ‘e White precipitate of barium sulfite = On adding dilute hydrochloric acid, the precipitate dissolves with no fizzing ‘s Chalky-white precipitate of silver chloride ‘o Precipitate dissolves in dilute aqueous ammonia «« Cream precipitate of silver bromide « Precipitate is insoluble in dilute ammonia, but soluble in concentrated ammonia «Pale yellow precipitate of silver iodide © Precipitate is insoluble in both dilute and concentrated ammonia ‘© White precipitate of the insoluble metal carbonate ‘e Onadding acid, the precipitate fizzes as it gives off carbon dioxide and disappears cation(aq) + anion(aq) — formula of precipitate(s) Ror a ‘ e example, the ionic equation for the formation of barium sulfate by mixing solutions of barium chloride and potassium sulfate is: Ba**(aq) + S0,2-(aq) ~ BaSO,(s) Tests for anions n of t the suspected sulfate, add dilute hydrochloric acid followed Sulfite: ‘To the suspected su dioxide gas will bs This test can be carei unknown. by aqueous bari ium chloride. A white hydrochloric acid is added, proves the ee tate, which remains when exces: nce of sulfate ions.Jy, heat the solid, Carbonates, other than sodium, potassium and natively, heat the s ona nonate, give off carbon dioxide, Q seth hese tess workwith hydrogencarbonates aswel so the initia conclusion Sata be that carbonate or hydrogencarbonate is present, However, the only sydrogencarbonates that exist as solids are group 1 compounds. Ifthe unknown ‘2 gioup 1 compound, the test for hydrogencarbonate must be carried cuits negative, the original compound isa carbonate. ponate rbonate vish between a group 1 carbonate and a hydrogencarbonate: add some of the unknown solid to almost boiling water. Hydrogencarbonates ;pose with the production of carbon dioxide — fizzing occurs. Carbon dioxide can be tested for by passing it into limewater, which goes milky. .d a solution of the unknown to a solution of calcium chloride. Hydrogen- carbonates do not give a precipitate because calcium hydrogencarbonate is soluble; carbonates give a white’ precipitate of calcium carbonate. 2 solution with pH paper. Carbonates have a high (alkaline) pH whereas irogencarbonates are almost neutral. On warming, if the solution is a hydrogencarbonate, the pH rises rapidly as the hydrogencarbonate umber ofmoles of in equation Step 3: calculate the concentration of the second solution. Make sure that you give your answer to the correct number of significant Figures. Ifindoubt, give it to 3s.f- Worked example A sample of 2.65 g of pure sodium carbonate, Na;CO;, was weighed out, jolved in water and made up to 250m? in a standard flask. Some of this solution was placed in a burette and used to titrate 25,0 cm? portions of a solution of hydrochloric acid. The titres obtained are shown in the table, ‘The equation for the reaction 2HCL+Na,CO, > 2NaCl + H.0 + CO; Experiment 7 2 3 4 ‘a Calculate the concentration of the sodium carbonare solution, b Calculate the mean titre. : € Calculate the amount (in moles) of sodium carbonate solution in the mean titre, ‘d Calculate the amount (in moles) of hydrochloric acid that reacted. e Calculate the concentration of the hydrochloric acid solution. e Answer By ‘a molar mass of sodium carbonate =(2%23.0)+ 12.0 (3x 16.0) = 105.0gmol* : i “ mass 2.659 cae Armount of sodium carbonate macs = agg pgimott = C0250 MOL see 2 mal 0,0250 mot aeb The titre for experiment 3 is at least 0.5 cm? less than any other titre, and so is not used in the calculation. 22.35 + 22.40 +22: mean titre = “225+ 2240+ 22.50 9) o> emt 3 {¢ amount of sodium carbonate = concentration x volume 22.42 dm? amount = 0.100 mol dm-? x aa = 0.00224 mol ratio HCLNa,C0, = 2:1 amount of HL= 2 x 0.00226 mol = 0.00448 mol concentration of hydrochloric acid = T2t 4 ote that attvotumes volume were converted from. 0.00448 mol cm} to dm? by =0.179 mol dm-? Gg (0/1000 dm dividing by 1000, Evaluation of error There is always a built-in error when using apparatus such as balances, thermometers, burettes and pipettes. The pipette may be stamped with the volume 25.0cm®, or the balance may read 1.23 g, but these quantities are all subject to some error. For example, the manufacturer of a balance may state that the mass of an object is accurate to +£0.01 g. Therefore, a reading of 1.23 g may mean a mass anywhere between 1.22 and 1.24g. Ifa container is weighed empty and then reweighed containing some solid, each weighing would be subject to a possible error of + 0.01 g and so the mass of the solid could have an error of + 0.02g. Worked example 1 An empty crucible was weighed, using a balance with a possible error of £0.01g, It was reweighed containing some solid metal carbonate, NCOs, and was then heated to constant weight. On heating, the mecal carbonate decomposes according to the equation: MCO, > MO+CO, 2 ‘The readings were as follows: ™ Mass of empty crucible = 14.23 g Mass of crucible + carbonate = 16.46 g Be i 1 3 Mass of crucible + contents after heating to constant weight = 15.61 g @ Calculate the mass of carbon dioxide given off. b Hence, calculate the amount in moles of carbon dioxide produced © Calculate the mass of metal carbonate taken. Using your answers to b and ¢ calculate the molar mass of the metal carbonate and hence the molar mass of the metal, M:,@ Assuming all the measurements of mass had an uncertainty of £0.01 g, calculate the uncertainty in the value of the molar mass of M. Answer : amass of carbon dioxide = 16.46 - 15.61=0.85 mass = mts 2 = 0.0193 mol b amounts volar mass 44.09 mol © mass of MCO; = 16.46 ~ 14.23 = 2.23 g amount (moles) of MCO; = amount (moles) of CO. mass 2.239 molar mass 0.0193 mol molar mass of M= 116 ~ [12.0 + (3x 16.0)] = 56.0 g mol mass of CO, =0.85 + 0.02 g The amount (moles) of C0, lies between 0.83/44.0 0.87/44.0 = 0.0198 mol. Since the ratio of MCO, to CO, is 1:1, the amount (moles) of MCO, also lies between 0.0189 and 0.0198 mol. mass of MCO; = 2.23 + 0.02 g .0193 mol molar mass of MCO, .0189 mol and bi 2.25 maximum molar mass of MCo, = igsest mass. _ 19 g mol smallest moles 0.0189 Therefore, ‘maximum molar mass of M = 119 ~ 60.0=59 g mol“? Oheetement, M, Iminimum molar mass of MCO;= FF motes * O.Giae 7 112 9 mol” could be Cr, Mn, Fe, aan Coor Ni, as their roe molar masses le in minimum molar mass of M = 112 ~ 60.0 = 52 ¢ mo terre este The uncertainty of the molar mass of iis that itis between 52 and 59 g mol 59g molt, Worked example 2 A thermometer is labelled as having an accuracy of + 0.2°C. In an enthalpy of neutralisation reaction, the temperature before the reaction was 17.4°G and after the reaction was 24,5°C, The mass of liquid used was 100 g. The specific heat capacity of the liquid is 4.18 J ¢1°C-!, Calculate the percentage error caused by the thermometer and hence the error in the evaluation of the heat produced, Answer temperature rise = (24.5 - 17,4) + 0. 7140.4 percentage error caused by the thermometer heat produced = 100 qx 4.18.3 9"! *C-1x 71°C = 2068), error in value of heat produced = +5.63% of 2968 © 330 Unit 5: Chemistry laboratory skills