Topic 01 · Experimental Chemistry

Experimental
Chemistry

1

Measuring Physical Quantities

1.1Quantities, units and apparatus

QuantitySI unitApparatusOther units
timesecond, sstopwatchminute (min), hour (h)
temperaturekelvin, Kthermometerdegree Celsius (°C)
lengthmetre, mmetre rule, measuring tapecm, dm, mm
masskilogram, kgelectronic balancegram (g), tonne (t)
volumecubic metre, m3burette, pipette, measuring cylinder, gas syringecm3, dm3
60153045stopwatchthermometer12.34 gelectronic balance
  • A digital stopwatch reads to ±0.01 s and an analogue stopwatch to ±0.1 s.
  • Laboratory thermometers are alcohol, mercury or digital. A temperature probe joined to a data logger collects readings automatically.
  • An electronic balance reads to about ±0.01 g.

1.2Converting units

Time1 min = 60 s   1 h = 60 min = 3600 s
Temperaturetemperature in K = temperature in °C + 273
Length1 m = 10 dm = 100 cm = 1000 mm
Mass1 kg = 1000 g   1 g = 1000 mg
Volume1 dm3 = 1000 cm3 = 1 litre
Volume1 m3 = 1000 dm3
Note1 m = 10 dm, but 1 m3 is not 10 dm3. A cube of side 10 dm has a volume of 10 × 10 × 10 = 1000 dm3.

Worked exampleConvert 250 cm3 to dm3.

1 dm3 = 1000 cm3250 ÷ 1000 = 0.250 dm3
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Measuring Physical Quantities (continued)

1.3Measuring volume

pipettevolumetric flaskmeasuring cylinderburettegas syringe
ApparatusWhat it measures
pipettean accurate fixed volume, e.g. 10.0 cm3 or 25.0 cm3
volumetric flaskan accurate fixed larger volume, e.g. 100 cm3 or 250 cm3
measuring cylindera range of volumes, to the nearest 0.5 cm3, e.g. 31.5 cm3
burettea range of volumes, to the nearest 0.05 cm3, e.g. 23.00 cm3
gas syringethe volume of a gas, up to 100 cm3
323130meniscusread here:31.0 cm³
  • Place your eye level with the meniscus to avoid parallax error.
  • For water, read the bottom of the meniscus.
2

Collecting and Drying Gases

2.1Methods of collecting gases

The method depends on how soluble the gas is in water and how dense it is compared with air.

gaswater
Water displacementinsoluble or slightly soluble gases
gasair out
Upward deliverygases less dense than air
gasair out
Downward deliverygases denser than air
MethodSolubility in waterDensityExamples
water displacementinsoluble or slightly solubleanyhydrogen, oxygen, carbon dioxide
upward deliverysoluble or insolubleless dense than airammonia
downward deliverysoluble or insolubledenser than airchlorine, hydrogen chloride, sulfur dioxide
NoteTo decide if a gas is denser than air, compare its Mr with the average Mr of air, about 29. A gas with Mr above 29 is denser than air (e.g. Cl2, 71). A gas with Mr below 29 is less dense (e.g. NH3, 17).
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Collecting and Drying Gases (continued)

2.2Drying agents for gases

wet gas indry gas outconcentratedsulfuric acidgas indry gascalcium oxide(quicklime)gas indry gasfused calcium chloride
Drying agentUse it forDo not use it for
concentrated sulfuric acidmost gases, e.g. chlorine and hydrogen chloridegases that react with it, e.g. ammonia
calcium oxide (quicklime)ammoniagases that react with it, e.g. carbon dioxide
fused calcium chloridemost gasesammonia
NoteCalcium oxide and calcium chloride absorb water from the air, so they must be freshly heated before use.
3

Separation and Purification

3.1Choosing a method

A mixture has two or more substances that are not chemically combined. Each is separated using a difference in a physical property: particle size, solubility, melting or boiling point, or magnetism.

What is in the mixture?solid + solidsolid + liquidliquid + liquidone solid is magneticmagnetdifferent particle sizessievingonly one solid dissolvesdissolve, filter, evaporateone solid sublimessublimationsolid does not dissolvefiltrationsolid dissolved, solid wantedevaporation to drynesscrystals wanted, or solid decomposescrystallisationthe liquid is wantedsimple distillationliquids do not mix (immiscible)separating funnelmiscible, boiling points differfractional distillationdissolved coloured substancespaper chromatography
NoteKey terms. A solute dissolves in a solvent to make a solution. Miscible liquids mix completely, while immiscible liquids form separate layers. The filtrate, residue, distillate and sublimate are what each method collects.
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Separation and Purification (continued)

3.2Solid and solid mixtures

Magnetic attraction

A magnet removes magnetic solids (iron, cobalt, nickel), e.g. iron filings from sulfur.

Sieving

Separates solids with different particle sizes.

A suitable solvent

If only one solid dissolves, add the solvent and filter. For sand and salt, the salt solution is the filtrate and the sand is the residue.

Sublimation

A solid that changes straight to a gas, e.g. iodine or naphthalene, is warmed and collected as the sublimate on a cold surface.

cotton woolcold funneliodine crystalsiodine and salt

3.3Solid and liquid mixtures

Filtration filter paperresiduefilter funnelfiltrate

Separates an insoluble solid from a liquid. The liquid that passes through is the filtrate. The solid left on the paper is the residue.

Evaporation to dryness steamsolutionevaporating dishtripod and gauzeheat

Separates a dissolved solid from its solvent by heating until all the solvent has boiled off.

Crystallisation

Used for a solid that decomposes on strong heating, or to obtain pure crystals of a salt.

  1. Heat the solution until it is saturated. Stop before all the solvent evaporates.
  2. Cool the solution so that crystals form.
  3. Filter, wash the crystals with a little cold distilled water, and dry them between filter papers.

Why crystals form: hot water holds more solute than cold. 100 g of water holds 55 g of copper(II) sulfate at 80 °C but only 21 g at 20 °C, so on cooling the other 34 g comes out as crystals.

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Separation and Purification (continued)

3.3Solid and liquid mixtures (continued)

Simple distillation
thermometerwater outwater incondensersalt waterboiling chipsheatdistillate
  • Separates a pure solvent from a solution, e.g. pure water from salt water. The solvent is collected as the distillate.
  • The thermometer bulb is level with the side arm, to measure the temperature of the vapour entering the condenser.
  • Cold water enters the condenser at the bottom, so the condenser stays full of water and cools the vapour efficiently.
  • Boiling chips give smooth boiling.

3.4Liquid and liquid mixtures

less dense liquiddenser liquidtap
Separating funnel

Separates immiscible liquids. The less dense liquid forms the upper layer.

  1. Run off the lower layer into a beaker.
  2. Close the tap just as the boundary reaches it.
  3. Run the upper layer into a second beaker.

Worked exampleA mixture contains W and X, two immiscible liquids with X denser, Y, a solid that dissolves in W but not in X, and Z, a solid that is insoluble in both liquids. Outline how to separate all four.

Remove the insoluble solid Z by filtration. Use a separating funnel to run off liquid X, the lower layer. Obtain solid Y from its solution in W by evaporation or crystallisation.
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Separation and Purification (continued)

3.4Liquid and liquid mixtures (continued)

ethanolthermometerglass beadsfractionatingcolumnwater outwater incondenserethanol and waterheat
Fractional distillation
  • Separates miscible liquids with different boiling points, e.g. ethanol (78 °C) and water (100 °C).
  • The glass beads give a large surface area for the vapour to condense and boil again.
  • The liquid with the lower boiling point distils first. When the temperature rises, change the receiver.
NoteFractional distillation separates crude oil into fractions and liquid air into nitrogen, oxygen and argon.

3.5Chromatography

Chromatography separates a mixture of substances that have different solubilities in a given solvent.
mixturedye Amixturedye Axysolvent frontstart line
  • Draw the start line in pencil, as graphite does not dissolve in the solvent.
  • The solvent level must be below the start line, so the spots do not dissolve into the solvent.
  • The more soluble a substance, the further it travels. A spot that matches a known pure substance is probably that substance.
  • Colourless substances are shown with a locating agent or ultraviolet light.
Rf = distance moved by the substancedistance moved by the solvent front  both from the start line
4

Purity

4.1Pure substances and mixtures

Pure substance

Melts and boils at one fixed temperature. Gives one spot on a chromatogram.

Mixture

Melts and boils over a range of temperatures. Impurities lower the melting point and raise the boiling point.

Purity matters in medicines and food: impurities in a medicine may cause harmful side effects.

Exam tipTo show a sample is pure, state that it has a sharp, fixed melting point that matches the known value.
Topic 01 · Experimental Chemistry7