Gravimetric analysis
Transcript of Gravimetric analysis
1G R A V I M E T R I C A N A L Y S I S
MATER IALS
Invest igat ion
(per student or group)- 100 g wet beach sand or soil from high salinity area- filter funnel- filter paper- glass rod- 250 mL beaker- large evaporating basin- drying oven or electric hot plate- Bunsen burner and heatproof mat- tripod and gauze- balance (accurate to 0.01 g)- 100 mL measuring cylinder- retort stand with ring clamp
MATER IALS
1Invest igat ion
Gravimetric analysis
� SyllabusIdentify data sources, plan, choose equipmentand perform a first-hand investigation toseparate the components of a naturallyoccurring or appropriate mixture such as sand,salt and water, and gather first-hand informationby carrying out a gravimetric analysis of themixture to estimate its percentage composition.
Introduction
In this investigation you will plan your own investigation in order todetermine the percentage of water and the percentage of soluble salts ina sample of sand or soil.
On completion of this investigation, you will be able to:● select and assemble appropriate equipment● perform an investigation safely according to your plan● recognise the practical applications of gravimetric analysis● identify various procedures for the separation of mixtures ● report your findings in an acceptable, scientific way.
Procedure
1 Search the literature using the library or the Internet to find outabout gravimetric analysis.
2 Plan an investigation to separate water and soluble salts from yoursample of sand or soil. Assess all the possible risks associated with yourchosen procedure.
3 Choose and set up your equipment.4 Perform the gravimetric analysis and collect all the data necessary to
calculate the percentage of water and soluble salts present in yoursample.
5 Record your data and observations.6 Write a report of your investigation. Your report must include the
following headings:● Purpose—brief outline of what your investigation aims to achieve.● Procedure—step-by-step outline and diagrams of the equipment
used to collect your data; also include references to any sourcesused.
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2 G R A V I M E T R I C A N A L Y S I S
� Disposal of wasteAll solids should bedisposed of by wrappingin paper and placing inthe garbage bin. Allliquids can be washeddown the sink. Avoidspilling sand or soil in the sink.
Discussion
1 What was the basis of separation of the soluble salt from the insolublecomponent in your sample?
2 Is the salt you have isolated a pure substance or a mixture? Explainyour answer.
3 Describe two situations where gravimetric analysis can supply usefuldata for chemists and other scientists (such as geologists).
4 Give one practical application from industry where the followingseparation techniques are applied:a sievingb sedimentationc evaporationd distillatione fractional distillation.
● Results—table of data collected and observations made, as shownin the examples in Tables 1 and 2.
● Calculations—percentage composition of your sample.● Conclusion—this must answer the purpose.● Discussion—answer the questions below.
R E S U LT S
TABLE 2
TABLE 1
Material Observations
sample of sand
sand without water
soluble salts
Item Mass (to nearest 0.01 g)
empty beaker
beaker and wet sand
beaker and dry sand
empty evaporating basin
mass of basin and salt
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3G R A V I M E T R I C A N A L Y S I S
The iron ore that is richest in iron is magnetite (Fe3O4).
a Calculate the percentage of iron in this ore.
b How many kilograms of pure iron could you theoretically obtain from 1 tonne of magnetite?
FOLLOW- UP
5 A team of geologists has found a possible iron ore source, whichhappens to be magnetic. They have analysed a 1 kg sample of ore as follows:
The sample was crushed and passed over a magnetic belt toseparate magnetite from the non-magnetic residue. An amount of345 g magnetic ore was obtained. The non-magnetic residue wasplaced in a tank and underwent froth flotation. The lighter, copper-containing material floated while the heavier, silicon-containingmaterial sank. 152 g copper ore was extracted.
Calculate the percentage composition of the original sample, withrespect to iron ore and copper ore.
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4 I N V E S T I G A T I O N O F P H Y S I C A L P R O P E R T I E S O F A R A N G E O F E L E M E N T S
Invest igat ion
Please indicate by signing that you have understood the information in the safety table.
Name (print):
I understand the safety information (signature):
Stations 1 & 2(for teacher demonstration)- 1 L liquid nitrogen in Dewar flask- banana- soft wooden board- nail- leaves, flowers- rubber tubing- sodium- scalpel and forceps- 250 mL beaker with watch-glass cover- phenolphthalein- filter paper
Stations 3 & 4(per student or group)- DC source- 3 electrical leads, 2 with crocodile clips at one end- ammeter or multimeter- petri dish- 3 strips each of aluminium, zinc, tin, lead, magnesium- 3 pieces of copper wire- 2 graphite rods- powdered carbon- amorphous sulfur (2 petri dishes with 1 g chunk in each)- iodine (2 covered petri dishes with 0.5 g in each)- small hammer and anvil- red phosphorus- 4 iron nails
MATER IALS
2Invest igat ion
Investigation of physical properties of a range of elements
Material used Hazard Control
lead metal Lead salts are highly toxic Wash hands with soap and water after polishing metal
iodine Toxic by all routes of exposure, Wear safety glasses and gloves stains skin and clothing, vapour highly irritating to lungs
red phosphorus Toxic if ingested Wear safety glasses and gloves
Pre-lab safety information
INVESTIGATION 2: Investigation of physical properties of a range of elements
� SyllabusPlan and perform an investigation to examinesome physical properties, including malleability,hardness and electrical conductivity, and someuses of a range of common elements to presentinformation about the classification of elementsas metals, non-metals or semi-metals.
Introduction
Very few elements found in nature are pure. Most pure elements areinvisible gases. Solid elements are mainly extracted from theircompounds.
You will investigate a range of common elements and use theirphysical properties to classify them as metals or non-metals.
On completion of this investigation, you will be able to:● list physical properties that are common to all metals● distinguish the physical properties of non-metals● recognise the uses of a range of common elements● position metals in the appropriate section of the Periodic Table.
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5I N V E S T I G A T I O N O F P H Y S I C A L P R O P E R T I E S O F A R A N G E O F E L E M E N T S
� Disposal of wasteAll solids can be wrappedin paper and disposed ofin the garbage bin. Keepany elements that couldbe reused.
TABLE 1R E S U LT S
Test Observation before cooling Observation after cooling
test-tube with air
banana
leaves
flowers
rubber tubing
Station 1: LIQUID NITROGEN (TEACHER DEMONSTRATION)
1 Your teacher will immerse in the liquid nitrogen a test-tube (containingair) suspended from the retort stand.
2 Your teacher will immerse a banana in the liquid nitrogen. The bananacan then be used to hammer a nail into the wooden board.
3 Your teacher will immerse leaves and flowers in the liquid nitrogen.4 Your teacher will demonstrate the effect of cooling on the flexibility
of rubber tubing.
Discussion
1 At what temperature does nitrogen liquefy?2 What is the main source of nitrogen on Earth? What percentage of
this nitrogen is found as a gas?3 a What effects does liquid nitrogen have on plants such as bananas,
flowers and leaves?b How could these effects be used in an industrial application?
4 a What was the result of cooling the test-tube, containing air, inliquid nitrogen?
b Give one industrial application of this observation.
Station 2: SODIUM METAL (TEACHER DEMONSTRATION)
1 Your teacher will take a piece of sodium out of paraffin oil, wipe itwith filter paper and test the sample for electrical conductivity.
2 Your teacher will cut a small piece of sodium (about 3 mm3), drop itinto a half-filled 250 mL beaker of water and cover the beaker with awatch-glass.
3 When the reaction stops, your teacher will add a few drops ofphenolphthalein.
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6 I N V E S T I G A T I O N O F P H Y S I C A L P R O P E R T I E S O F A R A N G E O F E L E M E N T S
TABLE 2R E S U LT S
Test Observation
sodium in oil
sodium (cut)
conductivity test
reaction with water
phenolphthalein added
Discussion
1 Does sodium look like a typical metal?2 Why is sodium kept under oil?3 Name two physical properties that would indicate that sodium is a metal.4 List at least five different observations you made when sodium reacted
with water.5 Write a word equation that is consistent with your observation of
sodium reacting with water.6 Explain why the indicator changed colour during the reaction of
sodium with water.7 On Earth, where would you find sources from which sodium could
be extracted?8 Name one chemical that contains sodium. What is its use?
Station 3: LUSTRE, DUCTILITY, MALLEABILITY AND HARDNESSOF SOLID ELEMENTS
1 Plan an investigation to rank given metals for their: a lustre (reflection of light, shininess, dullness, silver or gold colour)b ductility (if metal can be drawn out into a wire)c malleability (if metal is able to be hammered into sheets)d hardness (soft or hard, brittle or flexible)
2 Record your observations in Table 3.
TABLE 3R E S U LT S
Element Lustre and shape Hardness Malleable Ductileyes/no yes/no
aluminium
zinc
iron
copper
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7I N V E S T I G A T I O N O F P H Y S I C A L P R O P E R T I E S O F A R A N G E O F E L E M E N T S
Discussion
1 Rank the above elements according to:a descending order of lustreb increasing order of hardnessc increasing order of malleability.
2 Name the most ductile element and its industrial use.3 Name an industrial use for:
a aluminiumb iron.
FIGURE 1 Conductivity tester
DC ammeter
petri dishelement to be tested
crocodile clips
Station 4: CONDUCTIVITY OF ELEMENTS
1 Set up the conductivity tester, as in Figure 1.2 Set up a DC source to deliver 2 V. Place a piece of the element to be
tested on a watch-glass or petri dish. Touch the ends of the elementwith the crocodile clips (attached to leads). Observe the movement ofthe ammeter needle.
3 Repeat the test with each element, both lumps and powders.4 Record your observations in Table 4.
tin
lead
magnesium
graphite rod (carbon)
sulfur
iodine Do not test Do not test
red phosphorus Do not test Do not test
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FOLLOW- UP
8 I N V E S T I G A T I O N O F P H Y S I C A L P R O P E R T I E S O F A R A N G E O F E L E M E N T S
Identify the five most abundant (by weight) elements in the biosphere, the lithosphere, thehydrosphere and the atmosphere. Describe the most common physical and chemical forms in whichthey are found. Tabulate your answers.
TABLE 4R E S U LT S
Element Current (amps)
aluminium
zinc
iron
copper
tin
lead
magnesium
graphite rod (carbon)
powdered carbon
sulfur
iodine
red phosphorus
Discussion
1 List the common properties of the elements that conducted electricity.2 Is there an element that conducted electricity, but has other
properties that are different from the other conductors?3 List the common properties of those elements that did not conduct
electricity.4 Classify all the elements in this investigation into two distinct classes,
leaving those that cannot be clearly classified as ‘undecided’.5 In what general area of the Periodic Table will you find:
a metals c semi-metalsb non-metals d gaseous elements?
6 Name the liquid elements.
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9
MATER IALS
Invest igat ion
Please indicate by signing that you have understood the information in the safety table.
Name (print):
I understand the safety information (signature):
(per student or group)- 1 g calcium carbonate (powdered)- 1 g sodium carbonate (anhydrous)- 1 g copper(II) carbonate- 1 g nickel carbonate- 40 mL limewater- 9 test-tubes- 4 delivery tubes with stoppers- 4 spatulas or teaspoons- Bunsen burner and heatproof mat- test-tube holders
MATER IALS
3Invest igat ion
Decomposition of carbonates
Material used Hazard Control
sodium carbonate Slightly toxic if ingested Wear safety glasses
copper carbonate Slightly toxic if ingested Wear safety glassesand by skin contact Wash hands after use
nickel carbonate Toxic if ingested Wear safety glasses May cause allergic reaction, Wash hands after use teratogen (pregnant females to avoid)
limewater Slightly toxic if ingested Wash hands after use
Pre-lab safety information
INVESTIGATION 3: Decomposition of carbonates
� SyllabusPlan and safely perform a first-handinvestigation to show the decompositionof a carbonate by heat, using appropriatetests to identify carbon dioxide and theoxide as the products of the reactions.
Introduction
Decomposition of compounds by heat is common practice in manyindustries. In this investigation, you will decompose a variety ofcarbonates to compare the strength of the bonds in these compounds.
On completion of this investigation, you will be able to:● recognise that heat energy can cause a chemical change● identify the products of decomposition ● demonstrate the difference between physical and chemical change● relate decomposition to the strength of bonds between atoms.
D E C O M P O S I T I O N O F C A R B O N A T E S
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10 D E C O M P O S I T I O N O F C A R B O N A T E S
Procedure
1 Add about 0.5 g (one spatula-full or half a teaspoon) of the first car-bonate to a clean, dry test-tube. Insert a stopper with delivery tube.
2 To another test-tube add about 10 mL clear limewater.3 Set up the apparatus as shown in Figure 1.
test-tube holder
glass tube
rubber tubing
limewater
carbonate
Bunsen burner
FIGURE 1 Experimental set-up
� Disposal of wasteAll solids can bedisposed of in thegarbage bin, and liquidswashed down the sink.
4 Gradually warm the test-tube containing the carbonate. Then heatthe test-tube strongly over the clear Bunsen flame and observe thechanges in the limewater.
5 Stop heating as soon as you observe changes. If changes are notobserved after 5 minutes, stop heating.
6 Record your observations in the results table below.7 Repeat with the other carbonates. When you are finished, leave the
test-tubes to cool in the rack.8 Plan and safely perform an investigation of solubility of these four
carbonates in water. (Hint: take only a small amount of each solid, thesize of a rice grain.)
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FOLLOW- UP
11D E C O M P O S I T I O N O F C A R B O N A T E S
TABLE 1R E S U LT S
Carbonate Effect of heat on solid Effect on limewater Solubility in water
calcium carbonate
sodium carbonate
copper carbonate
nickel carbonate
Discussion
1 Was heat energy absorbed or released during each decomposition?2 On a molecular level, explain what happened to the carbonate when
heated.3 Write balanced equations for the decomposition reactions you
observed, and indicate whether energy was released or absorbed byplacing E on the appropriate side of the equation.
4 Explain why some carbonates easily decomposed and others did not.5 Give evidence from your investigation that carbon dioxide gas was
produced, and that an oxide was formed.6 Write a balanced equation for the observation with limewater
(Ca(OH)2(aq)).7 On a molecular level, explain what process is involved when a carbonate
dissolves.8 Why did some carbonates easily dissolve on heating, but did not
decompose?
Decomposition of carbonates is common in many industries. Find out:
a What is the natural raw material for the cement industry?
b What processes are involved in the manufacture of cement?
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12 E F F E C T O F L I G H T A N D E L E C T R I C I T Y O N A C O M P O U N D
Invest igat ion
Please indicate by signing that you have understood the information in the safety table.
Name (print):
I understand the safety information (signature):
(per student or group)- 0.5 g silver carbonate- 0.5 g silver nitrate- 0.5 g silver sulfate- 0.5 g silver chloride- 100 mL 0.1 M sulfuric acid- 4 petri dishes- sunlight, spotlight, overheadprojector or similar light source- voltameter or similar apparatus- 12 V DC source- 2 test-tubes- taper and splint- molecular model kit
MATER IALS
4Invest igat ion
Effect of light and electricity on a compound
Material used Hazard Control
silver carbonate Toxic if ingested, stains skin black Wear eye and skin protection
silver nitrate Toxic if ingested, corrosive to skin and eyes, Do not touch, wear eye and stains skin black skin protection
silver sulfate Harmful by inhalation and if swallowed Wear eye and skin protection Irritating to the eyes and skin
Pre-lab safety information
INVESTIGATION 4: Effect of light and electricity on a compound
� SyllabusGather information using first-hand sources toobserve the effect of light on silver salts andidentify an application of the use of thisreaction. Observe the electrolysis of water,analyse the information provided as evidencethat water is a compound and identify anapplication of the use of this reaction.
Introduction
Conversion of energy to other forms of energy is an everyday occurrence.In this investigation you will investigate the effect of light energy on silversalts, and the conversion of electrical energy to chemical energy.
On completion of this investigation, you will be able to:● recognise the effect of light energy on compounds● identify an application of decomposition of silver salts● use models to explain what is happening when water boils● trace movements of atoms and ions during electrolysis of water.
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13E F F E C T O F L I G H T A N D E L E C T R I C I T Y O N A C O M P O U N D
� Disposal of wasteDo not dispose ofanything. Cover allpetri dishes and returnthem to your teacher.
TABLE 1R E S U LT S
Salt Immediate observation Effect of light
silver nitrate
silver chloride
silver carbonate
silver sulfate
Procedure A: EFFECT OF LIGHT ON SILVER SALTS
1 Position the petri dishes containing 0.5 g silver salts under the lightsource.
2 Remove the cover and leave them exposed until a change of colour isobserved.
3 Record your observations in Table 1.4 When all observations are completed and recorded in the table, see if
any further colour change has occurred. If so, note this further change.
Discussion
1 From your observations, what energy conversion has taken place?2 On a molecular level, what is happening to the silver salt when it is
exposed to light?3 Account for the colour change of silver chloride and silver carbonate
and write the balanced equation for their decomposition.4 Are the above reactions exothermic or endothermic?5 What are the practical applications of the above reactions?6 Give formulae for the other two silver salts tested.
Procedure B: ELECTROLYSIS OF WATER(TEACHER DEMONSTRATION)
1 Set up a voltameter or equivalent apparatus, as shown in Figure 1. Fill itwith sulfuric acid. Connect electrodes to a 4 V DC supply and continueelectrolysis until one of the tubes above the electrode is full of gas.
2 Measure the length of gas collected above each electrode and recordthe polarity of each electrode. Record the results in Table 2.
3 Collect the gas from the voltameter by placing a clean, dry test-tubeover one of its taps. Close the tap.
4 Test the gas at the negative electrode with a lighted taper. Test theother gas with a glowing splint.
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