ST.

HILDAS SECONDARY SCHOOL

SC(CHEMISTRY) 5116/5118 PAPER 5 PRACTICAL MANUAL

NAME: ________________________ CLASS: ________________ DATE: January November 2012

SCHEME OF ASSESSMENT 2012 Candidates are required to enter for Paper 1, Paper 5 and two of Papers 2, 3 and 4.

Science (Physics, Chemistry), Syllabus 5116 Paper 1 will be based on the Physics and Chemistry sections of the syllabus. Paper 2 will be based on the Physics section of the syllabus. Paper 3 will be based on the Chemistry section of the syllabus. Paper 5 will be based on the Physics and Chemistry sections of the syllabus. Science (Chemistry, Biology), Syllabus 5118 Paper 1 will be based on the Chemistry and Biology sections of the syllabus. Paper 3 will be based on the Chemistry section of the syllabus. Paper 4 will be based on the Biology section of the syllabus. Paper 5 will be based on the Chemistry and Biology sections of the syllabus. Practical Assessment (Paper 5) Paper 5 is designed to test appropriate skills in C, Experimental Skills and Investigations. In one or more of the questions in Paper 5, candidates will be expected to suggest a modification or an extension, which does not need to be executed. Depending on the context in which the modification/extension element is set, the number of marks associated with this element will be in the range of 10% to 20% of the total marks available for the practical test.

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What is Qualitative Analysis?

Qualitative Analysis is an experimental method used to find out information about on one or more unknown samples after carrying out some basic tests on them. These samples may be pure substances or mixtures of substances. There are usually two things that you usually do when you do qualitative analysis (a) Determine the identity of an unknown sample (b) Determine the nature of a sample (a) In the determination of the identity of an unknown sample, you are expected to do the following things: Determine the name of the sample Determine the ions present in the sample (b) In the determination of the nature of an unknown sample, you are expected to do the following things: Determine if the sample is acidic, basic, amphoteric or neutral Determine if the sample is oxidizing or reducing Determine if the sample is organic or inorganic Determine if the sample is saturated or non-saturated Some basic tests that you are required to perform include: Test Appearance Solubility Heating Test for gases Test for cations Test for Anions Flame Test Descriptions colour and texture of substance whether they can dissolve in hot water, cold water or other solvents heating the solid or liquid and use chemical test for the gases evolved use chemical test for the gases evolved to make inference on the identity of unknown sample use chemical test to identify the positive ion (cation) present in a substance. Eg in NaCl, Na+ is the cation. use chemical test to identify the negative ion (anion) present in a substance. Eg in NaCl, Cl- is the anion. use flame colours to make inference on the identity of some cations Reference Table 1 Table 2 Table 3 & 3.1 Table 4 Table 5 Table 6 Table 7 Table 8 Table 9

Test for reducing use oxidising and reducing agents to agents determine the nature of the substance in a Test for oxidising redox reaction agents 1. Appearance of Unknown Substance
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When you are required to describe a sample, you must describe the following: (a) state (solid or solution) (b) colour of sample Table 1 Colour of Unknown Substance Black Blue Green Grey Inference oxides of copper(II), iron(II) or manganese(IV) or iodine crystals or charcoal copper(II) salts eg CuSO4 or Cu(NO3)2 copper(II) or iron(II) salts eg CuCO3 or FeSO4 powdered metals eg iron, aluminium, lead or zinc Note: shiny grey aluminium or zinc granules dark grey iron filings dull grey lead Orange Purple White Yellow or Brown Colourless solution K2Cr2O7 ( potassium dichromate(VI) ) KMnO4 ( potassium manganate(VII) ) salts of potassium, sodium, ammonium, zinc, aluminium or calcium iron(III) salts eg FeCl3 dilute acids or alkalis or H2O2 ( hydrogen peroxide)

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2. Solubility of Salts The following table describes the solubility of some common substances in water. Note that precipitate is produced when one of the products of a reaction is insoluble in water. Type of salts sodium, potassium and ammonium compounds (ie. SPA compounds) nitrate Table 2 Soluble in water All SPA compounds are soluble in water Insoluble in water None

All nitrates are soluble in water All chlorides are soluble in water except those listed on the right All iodides are soluble in water except those listed on the right All sulphates are soluble in water except those listed on the right sodium carbonate potassium carbonate ammonium carbonate All hydrogencarbonates are soluble in water sodium hydroxide potassium hydroxide ammonium hydroxide (ammonia solution)

None

chloride

silver chloride lead chloride (soluble only in hot water) silver iodide lead iodide (soluble only in hot water) lead sulphate barium sulphate calcium sulphate (slightly soluble only) All carbonates are insoluble in water except those listed on the left None

iodide

sulphate

carbonate

hydrogencarbonate

hydroxide

All hydroxides are insoluble in water except those listed on the left

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3. Action of Heat Background When heat is applied to a solid, thermal decomposition takes place. A gas may be released from anions such as carbonates, nitrates, hydroxides or water vapour from hydrated crystal. Heat however, will only melt the compounds if they are from Group I metals like sodium or potassium as their anions are held strongly by the Group I metal ions. Tests must be conducted for the gases released upon heating and any colour changes must be observed and recorded down. Residue left behind later heating may be used for further testing such as adding acids or dissolving it with water. Some notes on heating the unknown substance Normally when we heat an unknown, we have to test for the gas. Follow the instructions given in the question paper. There are the four common gases: (i) (ii) (iii) (iv) carbon dioxide ammonia oxygen hydrogen

Based on the gas given off, we can determine what are present in the unknown (i) if carbon dioxide is given off, that means that a carbonate (CO32-) is present and the unknown may be a metal carbonate (ii) If ammonia is given off, the unknown may be an ammonium salt. However, if you have added aqueous ammonia before heating, the ammonia gas may come form the aqueous ammonia itself. So be careful If ammonia is produce when we add sodium hydroxide (NaOH) and aluminium powder, then a metal nitrate is present If hydrogen gas is given off when an acid is added to the unknown, then unknown substance is a metal

(iii) (iv)

You can refer to table 3 and 3.1 for more details.

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Table 3 Gas Evolved substance sublimes oxygen evolved (relights glowing splint) carbon dioxide gas evolved (forms white ppt in limewater) Inference ammonium salts such as NH4Cl, I2 some oxides or nitrates carbonates or hydrogencarbonates such as CaCO3, Al2(CO3)3, except sodium carbonate and potassium carbonates *Note: Group I metal carbonates are normally not affected by heat. These carbonates will just melt when heated, with no gases evolved. ammonia gas evolved (pungent gas that turns damp red litmus paper blue) water vapour evolved (water droplets formed on the upper part of test-tube) nitrogen dioxide gas evolved (brown gas with irritating smell) ammonium salts

hydrated salts such as CuSO4.5H2O, some hydroxides such as Cu(OH)2, NaOH, or hydrogencarbonates some nitrates such as Cu(NO3)2, NaNO3 *Note: nitrate of potassium and sodium will only yield one gas (oxygen) while all of the other metals from Group II onwards will yield two gases (oxygen and nitrogen dioxide)

sulphur dioxide gas evolved (choking gas which turns acidified potassium dichromate (VI) solution green) Colour of residue/Sublimate after heating white residue yellow residue when hot, white when cold reddish brown residue black residue when hot, reddish brown when cold black residue violet fumes, black sublimate white sublimate yellow sublimate 4. Tests for Gases

sulphate(IV) except K2SO3 and Na2SO3

Table 3.1 Inference Na+, K+, Ca2+, Zn2+, Al3+ Zn2+ Fe3+ Fe2+ Cu2+ INH4+ Pb2+

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One of the skills you need to acquire is to know when to test for gases. You must be able to anticipate the production of a gas in certain experiments. Some common experiments where the production of gases is likely are listed below: (a) When a substance, especially a solid is heated (b) When an acid is added to a substance. If acid is added to a carbonate, then you would expect carbon dioxide gas to be produced. If acid is added to a metal, then you would expect hydrogen gas to be produced. (c) When an alkali is being added to a substance. If alkali is added to a substance that has NH4+, then you would expect ammonia gas to be produced. Table 4 Odour pungent odourless

Gas ammonia gas (NH3) carbon dioxide gas (CO2) chlorine gas (Cl2)

Colour colourless colourless

Litmus Test red to blue blue to red

Confirmatory Test forms white ppt in limewater

yellowish green

irritating

blue to red to white (bleached) neutral

extinguished a lighted splint with a pop sound relights a glowing splint turns acidified potassium dichromate(VI) from orange to green water droplets on the upper parts of the test tube

hydrogen gas (H2)

colourless

odourless

oxygen gas (O2)

colourless

odourless

neutral

sulphur dioxide gas (SO2)

colourless

choking

blue to red

water vapour

colourless

odourless

neutral

5. Test for Cations

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Background Ionic substance consists of a positive ion and negative ion. We therefore have to find out the identity of these two types of ions in our experiments. To determine the identity of the cation present in a substance, a solution containing the cation is required. For substances that dissolve in water, the solution is easily prepared. For substances that do not dissolve in water, an acid is usually used to produce a solution containing the cation. An alkali (sodium hydroxide and ammonia solution) is added to the solution containing the cation to precipitate out the metal in the form of insoluble hydroxide. This hydroxide that is precipitated will be able to provide clues to allow you to identify the cation present in the substance. The precipitates formed are insoluble metal hydroxides form from the combination of the cation in the solution and the hydroxide ions (OH-) from sodium hydroxide and aqueous ammonia (ammonium hydroxide) Eg. ZnSO4(aq) + 2NaOH Zn(OH)2(s) + Na2SO4(aq) (unknown) White ppt Procedure Add sodium hydroxide or aqueous ammonia drop by drop slowly (about 3 5 drops) into the test-tube. See if there is any ppt and observe the colour of the ppt. Add sodium hydroxide or aqueous ammonia in excess. (Add in excess means adding excess sodium hydroxide or aqueous ammonia to the same test-tube to about full). Then observe if the ppt dissolves in this excess amount of reagents. (may need to use a stirrer to stir the mixture)

The colour of the ppt when a few drops of NaOH/NH3 is added in, together with solubility of ppt in excess of these alkalis will help you determine the cation present in the sample. Refer to Table 5.

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Table 5 Cation ammonium (NH4+) calcium (Ca2+) copper (Cu2+) iron(II) (Fe2+) iron (III) (Fe3+) lead(II) (Pb2+) zinc (Zn2+) aluminum (Al3+) Effect of aqueous sodium hydroxide No ppt, ammonia gas produced White ppt, insoluble in excess Light blue ppt, insoluble in excess Green ppt, insoluble in excess Red-brown ppt, insoluble in excess White ppt, soluble in excess, giving a colourless solution White ppt, soluble in excess giving a colourless solution White ppt, soluble in excess, giving a colourless solution No ppt or very slight white ppt Light blue ppt, soluble in excess to produce a dark blue solution Green ppt, insoluble in excess Red-brown ppt, insoluble in excess White ppt, insoluble in excess White ppt, soluble in excess giving a colourless solution White ppt, insoluble in excess Effect of aqueous ammonia (ammonium hydroxide)

*[Lead(II) ions can be distinguished from aluminium ions by the insolubility of lead(II) chloride.]

*Note: About Al3+ and Pb2+ ions Both Al3+ and Pb2+ ions give the same results when testing using both sodium hydroxide and aqueous ammonia. This is because both Al(OH)3 and Pb(OH)2 that were formed are both soluble in excess sodium hydroxide and aqueous ammonia because they are both amphoteric in nature. One way to distinguish these two cations is to use dilute hydrochloric acid. The test-tube containing Pb2+ ions will produce a white ppt of PbCl2, an insoluble salt while the test-tube containing Al3+ will produce a soluble AlCl3.

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The flow chart below shows how to identify a cation from its reaction with aqueous sodium hydroxide.

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The flow chart below shows how to identify a cation from its reaction with aqueous ammonia.

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6. Test for Anions Background Two types of experiments can be used to identify anions: (a) Adding chemical reagent to form a precipitate. The colour of precipitate will help you to identify the anion. (b) Chemical reagent(s) are added to produce a gas. The identity of gas will help you to identify the anion.

*Note: For the identification of chloride, iodide and sulphate ions, a chemical is added to form a precipitate. For the identification of carbonate, nitrate and hydroxide ions, chemicals are added in to produce a gas. Carbonates This is the only anion in the syllabus that can be tested in the solid state or in solution form. An acid, usually nitric acid is added to the unknown (either in solid state or solution form). Effervescence (bubbles) will be observed. The identity of this gas can be confirmed by using limewater where a white ppt will be produced in limewater. This white ppt is calcium hydroxide. Chlorides, Iodides, Nitrates and Sulphates For all these 4 anions in the syllabus, solutions of the sample that contain these anions must be used for testing. If you are given sample in the solid state, you must first obtain a solution by dissolving with distilled water. If the sample is insoluble in water, you will have to use acid to obtain a salt solution. For chloride ions, you must first acidify the solution with dilute nitric acid first, to remove other anions. This is then followed by the addition of silver nitrate solution. The presence of a white ppt confirms the presence of the chloride ions. Ag+ (aq) + Cl- (aq) AgCl (s) White ppt For iodide ions, you must first acidify the solution with dilute nitric acid first, to remove other anions. This is then followed by the addition of lead(II) nitrate solution. The presence of a yellow ppt confirms the presence of the iodide ions. Pb2+ (aq) + I- (aq) PbI2 (s) Yellow ppt For sulphate ions, you must first acidify the solution with dilute nitric acid first, to remove other anions. This is then followed by the addition of barium nitrate solution. The presence of a white ppt confirms the presence of the sulphate ions. Ba2+ (aq) + SO42- (aq) BaSO4 (s)

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White ppt

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 For nitrate ions, aqueous sodium hydroxide is first added, followed by a few pieces of aluminium foil (also known as Devardas alloy). The mixture is then warmed. The gas produced is tested with a piece of damp red litmus paper. If the red litmus paper turns blue and a pungent smell of ammonia gas is produced, then nitrate ions are confirmed to be present. *Note: For chloride, iodide and sulphate ions test, if acid is to be added in after the other chemical reagent, do observe if the precipitate formed dissolves when the acid is added in. If the ppt dissolves, most likely the anion present is carbonate ions, and not the rest. Confirmatory test for this is to test for carbon dioxide gas.

Table 6 Anion carbonate (CO32-) chloride (Cl-) [in solution) iodide (I-) [in solution] nitrate (NO3-) [in solution] sulphate (SO42-) [in solution) Test add dilute acid (eg hydrochloric acid) acidify with dilute nitric acid, then add aqueous silver nitrate acidify with dilute nitric acid, then add aqueous lead(II) nitrate add aqueous sodium hydroxide and aluminium foil, warm carefully acidify with dilute hydrochloric acid or nitric acid, then add barium chloride/nitrate Test result Effervescence produed, Carbon dioxide produced White ppt Yellow ppt Ammonia produced

White ppt

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7. Flame Tests Background Some metallic chlorides are volatile. When these metallic chlorides are heated in a bunsen flame, they give characteristic coloured flames. Table 7 Flame Colour blue-green brick-red whitish blue lilac orange-yellow Inference copper(II) ions calcium ions lead(II) ions potassium ions sodium ions

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8. Tests for Oxidising and Reducing Agents Background An oxidising agent: Gives oxygen to another substance Takes away hydrogen from another substance Increases oxidation state of another substance Removes negative electrons from another substance In the process of oxidising another substance, the oxidising agent is reduced. A reducing agent: Takes away oxygen to another substance Gives hydrogen from another substance Reduces oxidation state of another substance Gives negative electrons from another substance In the process of reducing another substance, the reducing agent is reduced. Oxidation and reduction takes place simultaneously and such reactions are called redox reactions. These reactions usually involve changes in colour which will allow you to interpret the nature of the substance. Table 8 (To test if substance is reducing in nature) Oxidising Agent Colour of Final colour of oxidising Oxidising agent after oxidising Agent another substance (itself being reduced) acidified potassium purple colourless solution due to manganate(VII) solution solution Mn2+ (KMnO4) acidified potassium dichromate(VI) solution (K2Cr2O7) fresh iron(III) solution (Fe3+ solution) orange solution yellow solution green solution due to Cr3+

Reason for colour change Mn7+ in MnO4reduced to Mn2+ Cr6+ reduced to Cr3+ Fe3+ reduced to Fe2+ I2 reduced to ICl2 reduced to ClMn4+ reduced to Mn2+

green solution due to Fe2+ colourless solution due to Icolourless solution due to Clcolourless solution due to Mn2+

iodine solution (I2 solution) brown solution chlorine water (Clorox, Cl2 light yellow water) solution solid manganese(IV) oxide (MnO2) black powder

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Table 9 (To test if substance is oxidising in nature) Reducing Agent Colour of Final colour of reducing Reducing agent after reducing Agent another substance (itself being oxidised) acidified iron(II) sulphate green solution yellow solution due to Fe3+ solution (Fe2+ solution) acidified potassium iodide solution (I- solution) colourless solution brown solution due to I2 Note: Iodine formed is confirmed by adding starch which turn dark blue solid iron filings (Fe) dark grey powder iron filings used up, producing yellow solution due to Fe3+ Note: Fe3+ ion formed is confirmed by adding NaOH which forms a reddish-brown ppt Cr3+ salt concentrated hydrochloric acid (HCl) green solid/solution colourless solution orange solution due to Cr2O72colourless solution remained, chlorine gas produced Note: Chlorine gas is confirmed by moist blue litmus paper which is bleached

Reason for colour change Fe2+ oxidised to Fe3+ I- oxidised to I2

Fe oxidised to Fe3+

Cr3+ oxidised to Cr6+ in Cr2O72Cl- oxidised to Cl2 (gas)

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The following shows the data sheet you will be referring to during the practical exam.

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