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HKDSE Chemistry A Modern View (Second Edition)

Laboratory Handbook

© 2009, 2014 Aristo Educational Press Ltd.


12–14/F Lok’s Industrial Building,
204 Tsat Tsz Mui Road,
North Point,
Hong Kong.
Tel.: 2811 2908
Fax: 2565 6626
Website: http://www.aristo.com.hk

All rights reserved. No part of this publication may be stored


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reproduction of this publication (or any part thereof), please
contact Aristo Educational Press Ltd. at the above
address.

This publication shall not be distributed in any other binding


or cover. All persons acquiring this publication shall observe
and be bound by the above conditions.

First published July, 2009


Second Edition August, 2014

ISBN 978-988-8243-30-3
Contents

A. Laboratory safety and experimental chemistry

A-1 Laboratory safety p.2


A-2 Hazardous chemicals p.2
A-3 Storage of chemicals p.5
A-4 Common laboratory apparatus p.6
A-5 Laboratory techniques p.11
 • Handling of chemicals p.11
 • Heating techniques p.13
 • Collecting gases p.14
 • Drying substances p.16
 • Smelling gases p.17
 • Testing gases p.17
 • Gas poisoning p.18
 • Using pipette and burette p.18

B. Uncertainty in measurements

B-1 Measured data p.22


B-2 Uncertainty and significant figures p.22
 • Use of significant figure to indicate uncertainty p.22
 • Number of significant figures p.23
B-3 Uncertainty in results calculated from measured data p.24
 • Addition and subtraction p.24
 • Multiplication and division p.25
Laboratory Handbook

A-1 Laboratory safety


In studying chemistry, you often have to do experiments in the
laboratory. While doing experiments, you should pay attention to the
points mentioned in Chapter 1, Section 1.4. At the same time, you
must also pay special attention to laboratory safety. Actually most
laboratory accidents result from carelessness or ignorance (Figure A-1).
Thus, you have to follow strictly all the laboratory safety rules.
Remember: Safety first! (Refer to Chapter 1, Section 1.4 for details).

Accidents in school laboratories


A report from the Education Bureau shows that there were 348
school laboratory accidents in the academic year 2011/12. The
majority of the accidents (97.0%) were due to carelessness of
students. Altogether 324 students and 4 teachers suffered
injuries. Heat burns or scalds and cuts were the most common
laboratory accidents and accounted for about 77% of the cases
reported.
16/5/2013

Figure A-1 A newspaper cutting about laboratory accidents.

A-2 Hazardous chemicals


We have briefly talked about hazardous chemicals in Chapter 1, Section
1.4 already. Hazard warning labels should be displayed on reagent
bottles containing hazardous chemicals. Table A-1 shows some
examples of hazardous chemicals and safety precautions are listed as
well.

hazard warning label 危險警告標籤 laboratory safety 實驗室安全


hazardous 危險的 safety precaution 安全措施
2
A. Laboratory safety and experimental chemistry

Hazard warning
Hazardous nature Examples Safety precautions
label
Explosive: • old stocks of potassium and • keep away from heat and
It is a substance sodium which have turned naked flames
which may yellow (due to formation of • handle with extreme care
explode if ignited superoxides), ammonium — avoid shock or friction
or
in air or exposed dichromate • make sure the container is
to heat. A shock or • 2,4-dinitrophenylhydrazine properly stoppered
friction may also
start an explosion.

Oxidizing: • concentrated sulphuric acid, • make sure the container is


It is a substance concentrated nitric acid properly stoppered
which may start a • nitrates, potassium • keep away from heat and
highly exothermic permanganate, potassium naked flames
reaction when in or dichromate, potassium • keep away from metals,
contact with easily chlorate, potassium iodate, combustible materials and
oxidizable potassium nitrite flammable chemicals
materials. It can • avoid contact with the eyes
create a fire risk. and skin; if any concentrated
acid is accidentally spilt into
the eyes or onto the skin,
wash the affected area with
running water for at least 3
minutes and go for medical
check-up

Flammable: • hydrogen, carbon monoxide, • in case of solids or liquids,


It is a gas, liquid or methane, LPG, town gas make sure the container is
solid that may • methanol, ethanol, ether, properly stoppered
easily catch fire ethyl ethanoate, carbon • in case of gases, make sure
under ordinary or disulphide, propanone, there is no leakage into the
conditions. benzene laboratory
• yellow phosphorus, sulphur, • keep away from heat and
potassium, sodium, fine naked flames
powders of aluminium,
magnesium and zinc

Carcinogenic: • known carcinogens: • must wear a laboratory coat,


It is a substance asbestos, benzene safety spectacles and gloves
which would cause • suspected carcinogens: • perform the experiment in
cancer or be nitrobenzene, fume cupboard
suspected to cause tetrachloromethane, • make sure the container is
cancer on trichloromethane properly stoppered
prolonged contact. • avoid breathing in their
vapours/particles
• should avoid using
carcinogens at schools

Table A-1 Classification of hazardous chemicals.

carcinogenic 致癌的 hazardous nature 危險性質


3 explosive 爆炸性 oxidizing 氧化性
flammable 易燃的
Laboratory Handbook

Hazard warning
Hazardous nature Examples Safety precautions
label
Toxic: • chlorine, hydrogen sulphide, • perform the experiment in
It is a substance, carbon monoxide, nitrogen fume cupboard
which if breathed dioxide, sulphur dioxide • in case of solids or liquids,
in, or swallowed, • bromine, carbon disulphide, make sure the container is
or methanol, properly stoppered
or absorbed
through the skin, tetrachloromethane, • avoid breathing in their
may involve methanal solution (37%) gases/vapours/particles
serious health risk • cyanides, lead compounds, • wear gloves (if gloves are not
or even death. mercury and most of its used, wash hands
compounds, potassium thoroughly after handling
chromate chemicals)
• yellow phosphorus
• 2,4-dinitrophenylhydrazine

Harmful: • trichloromethane, • avoid breathing in their


It is a substance, 1,1,1-trichloroethane vapours/particles
which if breathed • iodine, barium compounds • avoid contact with the eyes
in, or swallowed, (except barium sulphate), and skin; if accidentally spilt
or oxalic acid, oxalates, iron(II) into the eyes or onto the
or absorbed
through the skin, sulphate skin, wash the affected area
may involve with a lot of water
limited health risk. • the laboratory should be well
ventilated

Corrosive: • hydrogen chloride • wear a laboratory coat, safety


It is a substance • bromine, concentrated spectacles and gloves
which would mineral acids, concentrated • perform the experiment in
destroy living ethanoic acid, concentrated fume cupboard
or aqueous ammonia, • handle them with care,
tissues upon
contact. concentrated hydrogen especially when they are hot
peroxide solution, sodium or being heated
hypochlorite solution • avoid contact with the eyes
• potassium, sodium, sodium and skin; when accidentally
hydroxide, potassium spilt into the eyes or onto
hydroxide, silver nitrate, the skin, wash the affected
anhydrous aluminium area with running water for
chloride at least 3 minutes and go for
medical check-up

Irritant: • bench dilute mineral acids, • avoid contact with the eyes
It is a non- aqueous ammonia and skin; when accidentally
corrosive • anhydrous iron(III) chloride, spilt into the eyes or onto
substance but can ammonium dichromate, the skin, wash the affected
or
cause reddening potassium dichromate area with a lot of water
or inflammation of
the skin.

corrosive 腐蝕性 toxic 有毒的


harmful 有害的 well ventilated 空氣流通
4
irritant 刺激性
A. Laboratory safety and experimental chemistry

H20 Example A-1


Understanding hazard warning labels
What hazard warning label(s) should be put on bottles containing
(a) 0.2 M sodium hydroxide solution (b) 2 M sodium hydroxide solution
(c) trichloromethane (d) tetrachloromethane
(e) concentrated nitric acid (f) barium chloride
(g) potassium permanganate (h) mercury
(i) methanol (j) benzene?

Solution
If a substance is associated with different hazards of similar nature, then only the highest hazard
should be shown. The orders of increasing hazard are:
(A) ‘Flammable’ < ‘oxidizing’ < ‘explosive’
(B) ‘Harmful’ < ‘toxic’ < ‘carcinogenic’
(C) ‘Irritant’ < ‘corrosive’
For example, if a substance is both ‘flammable’ and ‘explosive’, only the ‘explosive’ warning label
should be shown. If a chemical is both ‘irritant’ and ‘harmful’, only the ‘harmful’ warning label is
shown.
(a) Irritant (b) Corrosive
(c) Carcinogenic (d) Toxic
(e) Oxidizing, corrosive (f) Harmful
(g) Oxidizing (h) Toxic
(i) Flammable, toxic (j) Flammable, carcinogenic

A-3 Storage of chemicals


Some chemicals require special storage methods. A few examples are:
(1) To prevent contact and reaction with air, potassium or sodium is
kept under paraffin oil (Figure A-2). Yellow phosphorus is kept
under water (Figure A-3).

water

Figure A-2 (left) Sodium is stored


under paraffin oil. phosphorus

Figure A-3 (right) Yellow phosphorus


is stored under water.

benzene 苯 similar nature 相似性 yellow phosphorus 黃磷


5 methanol 甲醇 storage 貯存
paraffin oil 石蠟油 trichloromethane 三氯甲烷
Laboratory Handbook

(2) Flammable or volatile liquids have to be stored in a cool place,


away from direct sunlight and heat sources. Their containers
should never be completely filled.

(3) Chemicals which readily absorb moisture are kept in well-sealed


containers, e.g. anhydrous aluminium chloride.

(4) Some chemicals will decompose much more quickly in the


Figure A-4 Concentrated nitric
presence of light. Examples are concentrated nitric acid, silver
acid is stored in a brown bottle. nitrate solution, hydrogen peroxide solution, chlorine water and
bromine water. They are kept in brown bottles (Figure A-4).

A-4 Common laboratory apparatus


24 mm
A chemistry laboratory contains many different pieces of apparatus
18 mm
designed for various purposes. Let us look at them briefly.

Test tubes Test tubes are the most common tools in a chemistry
150 mm laboratory. They are placed in a test tube rack when not in use. The
150 mm
usual size is 150 × 18 mm (Figure A-5a). Large test tubes (e.g. 150 × 24
mm) are also called boiling tubes (Figure A-5b). They are used to boil
a larger amount of liquid.

(a) (b) You can conveniently hold a test tube near its mouth using a test
Figure A-5 Two common tube holder. See Figure A-6.
types of test tubes.
(a) A 150 × 18 mm test tube.
(A depth of 1 cm roughly
mouth of
corresponds to a volume test tube holder
3
test tube
of 2 cm ).
(b) A 150 × 24 mm test tube
(also called boiling tube).

heat-resistant mat

Bunsen burner

Figure A-6 Holding a test tube for heating.

anhydrous 無水的 decompose 分解 volatile 揮發的


apparatus 儀器 test tube holder 試管夾 well-sealed 密封的
6
boiling tube 大試管 test tube rack 試管架
A. Laboratory safety and experimental chemistry

3 3
Beakers Different sizes are available (e.g. 100 cm , 250 cm , etc.)
(Figure A-7). Beakers can be used for holding and heating a large
volume of liquid.

Figure A-7 A beaker. Flasks Flat-bottomed flasks can stand on the bench without
support. Round-bottomed flasks are stronger but need support.
Conical flasks and volumetric flasks are used in volumetric analysis
(Figure A-8).

Evaporating basins Evaporating basins (dishes) are used to


evaporate solutions (Figure A-9).

solution
evaporating
basin
graduation
mark wire
gauze

tripod
heat

flat-bottomed round-bottomed conical flask volumetric flask


flask flask

Figure A-8 Different types of flasks. Figure A-9 Evaporating a solution


in an evaporating basin.

Crucibles Crucibles are made of porcelain (Figure A-10a). They


are used to hold substances for very strong heating. A pipeclay
triangle is used to support a crucible on a tripod for heating (Figure
Figure A-10 A-10b). A hot crucible can be handled with crucible tongs (Figure
(a) A crucible (with lid).
A-10c).
(b) Heating a crucible.
(c) Crucible tongs.
crucible lid

crucible

pipeclay
triangle

heat
tripod
lid crucible

(a) (b) (c)

beaker 燒杯 crucible tongs 坩堝鉗 lid 蓋 tripod 三腳架


7 conical flask 錐形瓶 evaporating basin 蒸發皿 pipeclay triangle 管土三角 volumetric flask 容量瓶
crucible 坩堝 flat-bottomed flask 平底燒瓶 round-bottomed flask 圓底燒瓶 wire gauze 鐵絲網
Laboratory Handbook

Bottles Some common types of bottles are shown in Figure


A-11.

Watch glass and Petri dish These are used for temporary storage
of solids and sometimes liquids (in small amounts). See Figure A-12.

rubber teat

watch glass
dropper

plastic wash bottle reagent bottle dropping bottle Petri dish

Figure A-11 Different types of bottles. Figure A-12 A watch glass and a Petri dish.

Gas syringe A gas syringe is used to collect a gas or to measure


the volume of a gas (Figure A-13).

plunger
short rubber tubing
plunger moves
out as the gas
gas 0 10 20 30 40 50 60 70 80 90 100
enters the
syringe
Figure A-13 A gas syringe. collected gas

Spatulas They are used to pick up small amounts of solids,


especially powders (Figure A-14).

Figure A-14 Spatulas.

Mortar and pestle The mortar pestle


and pestle are used to grind a solid
into a fine powder (Figure A-15).

mortar
Figure A-15 A mortar and a pestle.

dropping bottle 滴瓶 mortar 研缽 plastic wash bottle 塑膠洗滌瓶 watch glass 錶面玻璃
gas syringe 氣筒 pestle 研棒 reagent bottle 試劑瓶
8
grind 研磨 Petri dish 培養皿 spatula 刮勺
A. Laboratory safety and experimental chemistry

Droppers and teat pipettes These are used to add drop


quantities of a liquid (Figure A-16).

Glass rod A glass rod is used for stirring (Figure A-17).

Thermometer A thermometer is used to measure temperature


(Figure A-18).

rubber teat

Figure A-16 (left)


A dropper and a teat pipette.
Figure A-17 (middle)
A glass rod.
Figure A-18 (right)
A thermometer. dropper teat pipette glass rod thermometer

Bunsen burner A Bunsen burner is the main heating source in


the laboratory (Figure A-19).

barrel

gas tap
collar rubber tubing

jet air hole

Figure A-19 A lighted base

Bunsen burner. town gas

You can adjust a Bunsen flame in two different ways:

(1) The gas tap controls the supply of gaseous fuel, hence the size
of the flame.

(2) The air hole controls the air supply, hence the luminosity and
temperature of the flame.

air hole 氣孔 collar 空氣調節環 jet 噴嘴 teat pipette 長滴管


9 barrel 燈管 dropper 滴管 luminosity 發光度 thermometer 温度計
base 座 gas tap 煤氣掣 rubber teat 橡皮頭
Bunsen burner 本生燈 glass rod 玻璃棒 rubber tubing 橡膠管
Laboratory Handbook

When the air hole is open, a lot of air mixes with the gaseous fuel,
thus burning is more complete. The flame is non-luminous and blue,
with a high temperature (up to 1200°C). See Figure A-20a and Figure
A-20b. On the other hand, when the air hole is closed, very little air is
mixed with the gaseous fuel. Burning is incomplete, resulting in a
flame which is luminous and yellow, with a lower temperature (Figure
A-20c).

Figure A-20 The size of the (a) Roaring non-luminous (b) Non-luminous flame (c) Luminous flame (with
air hole controls the luminosity flame (with air hole (with air hole half air hole closed)
of a Bunsen flame. fully open) open)

Funnels Four common types of funnels are shown in Figure


A-21.
stopper
Figure A-21 Different types of
funnels.

tap

stopcock

sample filter funnel thistle funnel tap funnel separating funnel


lid
(for filtration and (for addition of (for controlled addition of (for separation of two
addition of liquid) liquid during gas liquid during gas preparation; immiscible liquids)
preparation) escape of gas through the
drying watch funnel can be prevented by
agent (e.g. glass closing the tap)
anhydrous gauze
calcium
chloride) Desiccator You can often keep solids or liquids out of contact
Figure A-22 A desiccator is with the moisture from the air by placing them in a desiccator. A
used to keep a solid (or a
desiccator contains a drying agent such as anhydrous calcium chloride
liquid) out of contact with
the moisture from the air. or silica gel (Figure A-22).

desiccator 乾燥器 luminous flame 黃焰 silica gel 硅膠


drying agent 乾燥劑 roaring non-luminous flame 發出「隆隆」聲的藍焰 tap funnel 活栓漏斗
10
filter funnel 過濾漏斗 separating funnel 分液漏斗 thistle funnel 長頸漏斗
A. Laboratory safety and experimental chemistry

Balances For accurate weighing, you should use an electronic


balance. Analytical balances (Figure A-23a) and ordinary top-loading
balances (Figure A-23b) are commonly used electronic balances.

Figure A-23
(a) An analytical balance.
(b) An ordinary top-loading balance. (b)

(a)

You should place chemicals to be weighed on a filter paper or in a


weighing bottle, not directly on the balance pan.

Burette, pipette, volumetric flask They are used to make


accurate measurements of liquid volumes in volumetric analysis. See
p.20, Figure A-48 (burette), p.18, Figure A-44 (pipette) and p.7, Figure
A-7 (volumetric flask).

Measuring cylinder You can use measuring cylinders to make


rough measurements of liquid volumes. The usual capacities are
3 3 3 3
10 cm , 25 cm , 50 cm and 100 cm .

A-5 Laboratory techniques


To perform experiments efficiently and safely, you need some basic
laboratory techniques as discussed below.

Handling of chemicals
You must handle chemicals carefully. Spillage of chemicals may cause
stains or burns on hands, clothes or bench tops.

accurate 準確的 capacity 容量 pipette 移液管 technique 技巧


11 balance pan 天平秤盤 electronic balance 電子天平 rough measurement 粗略的量度 volumetric analysis 容量分析
burette 滴定管 handling 處理 spillage 傾瀉
Laboratory Handbook

spatula Transferring solids


You can transfer a solid chemical into a test tube, using a clean dry
spatula (Figure A-24). Never put any chemicals back to the reagent
bottle.

Transferring liquids
Figure A-24 Transferring a You can transfer a liquid from a reagent bottle to a test tube as
solid into a test tube, with a
shown in Figure A-25. Before transferring, check the label of the bottle
spatula.
to make sure it is the correct reagent. After transferring, replace the
stopper immediately and return the bottle to its original place.

To pour a liquid from a beaker, hold a glass rod against the lip of
the beaker. Then pour the liquid slowly down into the receiving vessel
(Figure A-26).

glass rod
reagent bottle

Figure A-25 (left) The proper


way to transfer a liquid from a
reagent bottle to a test tube. label lip of
Figure A-26 (right) Transferring beaker
a liquid from a beaker. stopper

Mixing substances in test tubes


Very often you have to dissolve a solid in a liquid, or to mix two
liquids in a test tube. There would be five different ways in doing this.
See Figure A-27.

Shake the test Stir with a glass rod. Tap the bottom of the test Pour the contents to Stopper the test tube
tube gently. tube with the index finger. and fro between two and shake (useful
test tubes. when vigorous
Figure A-27 Five different ways of mixing substances in test tubes. shaking is required).

pour ... to and fro 來回傾倒 tap 輕敲


stir 攪拌 vigorous shaking 劇烈的搖動
12
A. Laboratory safety and experimental chemistry

Heating techniques
Lighting a Bunsen burner
lighted To light a Bunsen burner, close the air hole first. Put a lighted match
match near the top of the barrel (Figure A-28). Then turn on the gas tap.
barrel of
Bunsen burner
Open the air hole slowly, until the flame changes from luminous to
air hole non-luminous.
closed

Figure A-28 Lighting a Heating a solid


Bunsen burner.
(1) For a solid which does not give off water during heating, hold
the test tube horizontally, with the solid forming a shallow layer
along the tube.

(2) For a solid which gives off water during heating, hold the test
tube slightly sloping downwards (Figure A-29). This prevents the
condensed water (at the mouth of the tube) from running back and
cracking the hot glass.

(3) To heat a solid very strongly, heat it in a crucible.

hydrated compound test tube holder


test tube holder

heat
condensed water

Figure A-29 The tube should be held Figure A-30 Holding a test tube near
slightly sloping downwards when a the top with a test tube holder.
hydrated compound is being heated.

Heating a liquid
(1) Heating a non-flammable liquid
If you heat a non-flammable liquid in a test tube, pay attention to
the following points:
• Wear safety spectacles.
• Do not fill a tube with a liquid to more than one-third of its
capacity.
• Hold the test tube near the top with a test tube holder (Figure
A-30).
condensed water 凝結的水
13
Laboratory Handbook

• Use a small non-luminous flame for heating.


• Never point the test tube to anyone during heating.
liquid • Swirl the tube continuously during heating, so that the heating
is uniform (Figure A-31).

Alternatively, heat the liquid (especially with a large quantity) in a


beaker on a tripod and wire gauze (Figure A-32).

Figure A-31 Swirling a test (2) Heating a volatile or flammable liquid


tube continuously during
heating.
Use a water-bath to heat a volatile (low-boiling) or flammable
liquid. See Figure A-33. Use an oil-bath if a higher temperature
(up to 250°C) is required.

(3) Evaporating a solution


Use a steam-bath to evaporate a solution quickly (e.g. in
concentrating a solution to allow crystallization). See Figure A-34.

solution
evaporating basin
beaker steam
low-boiling (or
liquid
flammable water water
liquid)
wire gauze

heat heat heat


tripod

Figure A-32 Heating a liquid Figure A-33 Heating a liquid Figure A-34 Evaporating a solution
in a beaker on a tripod and with a water-bath. using a steam-bath.
wire gauze.

Collecting gases
collected gas Gases may be bought in cylinders or prepared in a laboratory by a
gas in test tube chemical reaction. The following methods may be used to collect gases
from either source.

delivery (1) Displacement of water


tube
trough See Figure A-35. This method is suitable for collecting gases which
water
are insoluble in water (e.g. hydrogen). This method is easy but the
gas collected is wet. So this method cannot be used when the
Figure A-35 Collecting a gas
by displacement of water. collected gases are required dry.

crystallization 結晶法 low-boiling 低沸點的 swirl 旋轉


delivery tube 導管 oil-bath 油浴 water-bath 水浴
14
displacement of water 排水法 steam-bath 蒸汽浴
A. Laboratory safety and experimental chemistry

(Note: If the gas being collected comes from a heated vessel, the
delivery tube must be removed from water before heating is
stopped. This is because once heating is stopped, water vapour
condenses and the gas inside the vessel contracts due to a drop of
temperature. A partial vacuum is thus created in the vessel. If the
end of delivery tube had not been removed from under water,
water would be sucked back via the delivery tube into the hot vessel.
This ‘sucking back’ of water might crack the hot glass vessel.)

(2) Downward displacement of air


Gases much lighter than air (e.g. hydrogen, ammonia) can be
collected by downward displacement of air. See Figure A-36.
This method is also known as upward delivery.

(3) Upward displacement of air


Gases much denser than air (e.g. chlorine, sulphur dioxide, carbon
dioxide) can be collected by upward displacement of air. See
Figure A-37. This method is also known as downward delivery.

Downward displacement of air Upward displacement of air


(for gases much lighter than air) (for gases much heavier than air)

gas in
air displaced out

air displaced out


gas in

Figure A-36 Collecting gases by Figure A-37 Collecting gases by


downward displacement of air. upward displacement of air.

(4) Using gas syringe


Gases can also be collected by a gas syringe. See Figure A-13 on p.8
again.

This method can be used for any gas, no matter it is soluble or


insoluble in water, heavier or lighter than air, coloured or
colourless.

downward delivery 向下導氣法 upward delivery 向上導氣法


15 downward displacement of air 向下排空氣法 upward displacement of air 向上排空氣法
Laboratory Handbook

H20 Example A-2


Determining the methods used for collecting gases
In finding whether a gas is lighter or heavier than air, its vapour density has to be calculated (by
dividing the relative molecular mass of the gas by 2). The vapour density is then compared with
the vapour density of air (approximately 14.4). Collecting gases by displacement of air would be
useful only if the difference in vapour densities is large enough.
Suggest a suitable method to collect (a) sulphur dioxide (b) carbon monoxide (c) dry nitrogen
in the laboratory. Give your reasoning.

Solution
Vapour density of air ≈ 14.4.

Method of collection
Gas Vapour density Using gas
Displacement of air Displacement of water
syringe
Yes (upward displacement
(a) Sulphur 32.1 + 16.0 × 2 No, as the gas is very
= 32.1 of air), as the gas is much Yes
dioxide 2 soluble in water
heavier than air

(b) Carbon 12.0 + 16.0 No, as the gas is about as Yes, as the gas is
= 14.0 Yes
monoxide 2 dense as air insoluble in water

No. Although the gas is


(c) Dry 14.0 × 2 No, as the gas is about as
= 14.0 insoluble in water, dry Yes
nitrogen 2 dense as air
gas is required here.

Drying substances
Drying solids
You can use an oven to dry solids. (Note: To dry hydrated salts, the
temperature of the oven should be set below 105°C. Otherwise, the
water of crystallization would be removed.)

Drying gases
You can dry a gas by passing it through a U-tube (packed with calcium
oxide), or a wash bottle (containing concentrated sulphuric acid). See
Figure A-38.

vapour density 蒸氣密度


16
A. Laboratory safety and experimental chemistry

wet gas dried gas

wet gas dried gas

Figure A-38 Drying a gas concentrated


sulphuric acid
using anhydrous
(a) a U-tube calcium
(b) a wash bottle. oxide U-tube wash bottle

Smelling gases
In doing experiments, smell gases only if necessary. Also, do it with
great caution. (Many gases are toxic!)

Do not smell a gas by breathing in directly above the test tube. You
should hold the tube about 15 cm away from the nose; then ‘fan’ a little
of the gas towards your nose. See Figure A-39.

Figure A-39 The proper


way to smell a gas.
Testing gases
There are three common ways of testing a gas.

(1) Using a delivery tube

reaction delivery Bubble the gas evolved through a testing solution (Figure A-40).
mixture tube
(Note: If the reaction mixture is being heated, always take out the
delivery tube from the testing solution before removing the flame.
This is to prevent sucking back of the solution.)
heat
(if necessary)
testing (2) Using a testing paper
solution
Test a gas by holding a moist testing paper (e.g. litmus paper) in
Figure A-40 Testing a gas by the mouth of the reaction vessel (Figure A-41).
bubbling it through a testing
solution.
glass rod
moist testing
paper drop of testing
solution

Figure A-41 (left) Testing a gas


reaction reaction
by using a moist testing paper.
mixture mixture
Figure A-42 (right) Testing a gas
by using a glass rod with a small heat heat
drop of testing solution. (if necessary) (if necessary)

fainted 昏倒 reaction vessel 反應容器


17 fan 搧動 sucking back 倒吸
litmus paper 石蕊試紙
Laboratory Handbook

(3) Using a glass rod


Hold the rod (with 1 drop of testing solution) in the mouth of the
reaction vessel (Figure A-42). Observe carefully the drop of testing
solution and look for any fumes produced.

Gas poisoning
Many gases (e.g. chlorine, nitrogen dioxide, carbon monoxide, sulphur
dioxide) and vapours (e.g. bromine, mercury, tetrachloromethane,
iodine) are very poisonous (Figure A-43). A person who has suffered
from gas poisoning must be removed from the laboratory at once, to
open areas. Smelling salt may be applied if he has fainted. After
Figure A-43 Sulphur dioxide
is a poisonous gas.
receiving first aid, he should be sent to the hospital by ambulance.

Using pipette and burette


Using pipette
A pipette (Figure A-44) is used to deliver a specific volume (e.g.
3
graduation 25.0 cm ) of a solution accurately in volumetric analysis. Before use,
mark
wash the pipette with distilled water, then with the solution it is going
to deliver.
bulb
(1) Washing a pipette
1. Dip the lower stem of a pipette well below the surface of the
distilled water as shown in Figure A-45a. Using a pipette filler,
suck sufficient amount of distilled water into the pipette to fill
part of the bulb.
tip
2. Close the top end of the pipette with an index finger. Then,
Figure A-44 A pipette.
hold the pipette horizontally. Rotate it slowly so that the
distilled water washes the inner wall, up to the graduation mark
completely (Figure A-45b).

pipette filler

pipette

(b)

Figure A-45 How to wash a


pipette with distilled water. distilled (a)
water
first aid 急救 specific 特定的
fumes 煙霧 stem 柄
18
gas poisoning 氣體中毒 suck 吸
index finger 食指
A. Laboratory safety and experimental chemistry

3. Allow the distilled water to run out into the sink.

4. Wipe dry the outside of the pipette tip with tissue paper.

5. Repeat steps 1 to 4, but using the solution it is going to deliver.

(2) Preparing a pipette of solution


1. Using a pipette filler, suck the solution into the pipette until
3
the solution level is about 2 cm above the graduation mark.

2. Close the top end of the pipette quickly with an index finger
(Figure A-46a). Then, hold the pipette vertically. Turn the
pipette slowly to allow the solution to run out slowly, until the
bottom of the meniscus just reaches the graduation mark
(Figure A-46b).

(3) Transferring the solution to a conical flask


1. Tilt the conical flask and keep holding the pipette vertically.
Allow the solution to run along the inner wall of the flask
(Figure A-47).

2. When all the solution has seemed to run out, touch the inner
wall of the flask with the tip of pipette two or three times.
(Note: After doing this, there will be some residual solution in
the pipette, but you must not blow it out.)

meniscus

pipette
solution

conical flask
solution
solution
(a) (b)

Figure A-46 (a) Close the top end of the pipette with an index finger. Figure A-47 Transferring a solution
Figure A-46 (b) The bottom of the meniscus of the solution just reaches from a pipette to a conical flask.
the graduation mark.

meniscus 彎液面 wipe 抹


19 tilt 傾斜
Laboratory Handbook

Using burette
A burette (Figure A-48) is used to deliver a variable volume (ranging
3
from 0.05 to 50.00 cm ) of a solution accurately in volumetric analysis.
Before use, wash the burette with distilled water, then with the solution
(i.e. the titrant) it is going to deliver.

(1) Washing a burette


stopcock 3
1. Using a filter funnel, add about 20 cm of distilled water to a
tip burette.
Figure A-48 A burette. 2. Hold the burette horizontally. Rotate it slowly so that the
distilled water washes its inner wall.
3. Open the stopcock to run out all the distilled water into the
sink.
4. Repeat steps 1 to 3, but using the solution it is going to
deliver.

(2) Preparing a burette of solution


1. Using a filter funnel, fill the burette with the titrant. (Note:
remember to remove the funnel immediately after use.)
2. Clamp the burette vertically in a stand. Place a beaker under
the burette. Then, open the stopcock to release a small amount
of the titrant. This is to make the burette tip also filled with the
titrant (Figure A-49). When the burette tip is filled with titrant,
close the stopcock. (Note: make sure that there is no air bubbles
inside the jet.)

stand solution

clamp

burette

Figure A-49 Open the stopcock to release a small amount of titrant.

titrant 滴定劑
variable 不同的
20
Laboratory Handbook

B-1 Measured data


We often use instruments to make measurements. For example, we
use a ruler to measure length, a balance to measure mass and a
thermometer to measure temperature. The values we get are called
22 measured data.
thermometer

21
mercury Suppose we have to take the temperature reading from the
thread
20 thermometer shown in Figure B-1. Which of the following data would
(reading in °C) be the most reasonable?

Figure B-1 What would be (1) 21°C


the thermometer reading? (2) 21.3°C
(The reading corresponds to
the top of the meniscus.) (3) 21.31°C
(4) 21.302°C

B-2 Uncertainty and significant figures


Use of significant figure to indicate uncertainty
The reasonable temperature reading as shown in Figure B-1 should be
21.3°C. Since the smallest graduation is ‘1’ for this thermometer, we are
uncertain about the value of the first decimal place i.e. 3. We have to
make an estimation about this. Obviously, the ‘21’ is certain; the
uncertainty lies in the first decimal place. The value recorded must
reflect this.

We can indicate the uncertainty in a datum by the number of


figures recorded. This is known as the ‘significant figure method’. In
this method, we put down

(a) all ‘certain’ digit(s); and

(b) one additional digit which is uncertain.

In other words, the uncertainty always lies in the last digit of the
recorded datum. In the example here, the value 21.3°C has three
significant figures. They are ‘2’, ‘1’ and ‘3’. The ‘2’ and ‘1’ are certain
while the ‘3’ is uncertain.

instruments 儀器 uncertainty 不確定性


measured data 量度數據 significant figure method 有效數字法
22
B. Uncertainty in measurements

Number of significant figures


We can easily find out the number of significant figures in most
measured data. For example:

31. 7 °C (3 significant figures)


3
26.8 5 cm (4 significant figures)

0.020 8 g (3 significant figures)

these zeros are not significant figures;


they just mark the position of the decimal place

2. 0 kg (2 significant figures)
this zero is a significant figure

(The digit of uncertainty is shaded in grey colour.)

(Note: For 25 930, the zero may only mark the position of the
decimal place or it may be the digit of uncertainty. Thus, it is better
4 4
to write as 2.593 × 10 (for 4 significant figures) or 2.5930 × 10 (for
5 significant figures).

H20 Example B-1


Understanding measured data
Two measured data are given:
3
First datum: 25 cm
3
Second datum: 25.0 cm
(a) What is the difference between them?
(b) Which datum is more accurate?

Solution
3 3
(a) The first datum implies that the actual volume lies between 24.5 cm and 25.5 cm . The
3 3
second datum implies that the actual volume lies between 24.9 cm and 25.1 cm .
(b) The second datum.

23
Laboratory Handbook

B-3 Uncertainty in results calculated


from measured data
We often do calculations involving measured data. It is important that
the calculated value should only include the correct number of
significant figures (not more, not less).

Addition and subtraction


In calculations using the ‘significant figure method’, the answer should
include all ‘certain’ digits and one ‘uncertain’ digit.

Consider the following example. Add up the following masses:

22 . 0 g (uncertainty in the first decimal place)


+ 1 . 31 3 g (uncertainty in the third decimal place)
23 . 313 g

round off

23.3 g (uncertainty in the first decimal place)

Consider another example:

24 3 cm (uncertainty in the units digit)


– 21. 7 2 cm (uncertainty in the second decimal place)
221. 28 cm

round off

221 cm (uncertainty in the units digit)

Class practice B-1


Calculate
(a) 18.45 + 103
(b) (15.4693 – 0.225) g

24
B. Uncertainty in measurements

Multiplication and division


In calculations using the ‘significant figure method’, the answer should
include the least number of significant figures among the data involved
in the calculation.

Consider the following examples:

(a) 2.1 × 1.212 = 2.5452


(answer should be rounded off to 2.5)

Number of
significant figures 2 4 2

(b) 13.22 ÷ 5.11 = 2.587 084 1


(answer should be rounded off to 2.59)

Number of
significant figures 4 3 3

(Note: The above rule does not apply to numbers with no uncertainty.
Thus, doubling 3.01 cm (3.01 × 2) gives 6.02 cm (not 6 cm), as ‘2’ is
an exact number here, not a measured datum.)

Class practice B-2


Find the total area of 2 rectangles each with a length of 18.5 cm and a
breadth of 2.6 cm.

25
Laboratory Handbook

Answers
Class Practice B-1:
(a) 121
(b) 15.244 g

Class Practice B-2:


2
96 cm

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