BHOS LABORATORY PLANNING
The following contains a list of general items and a list specifically for each experiment that supports
Chemistry and Process Industries A/B in the 1st year of chemical engineering. The document is
divided into the following sections:
1.General Equipment – this is a list of general items that should be available in the laboratory areas.
It is not a complete list but serves to illustrate the type of facilities that should be in place. For
example, students should as a routine record the environmental conditions (temperature and
pressure) each time they do a laboratory experiment – so a weather station or general pressure and
temperature, and possibly humidity should be provided for).
2. Suppliers – these are suppliers we use in the UK for chemicals and equipment. They may not be
the most cost effective – many of the materials can be sourced from alternative sources.
3. Shopping List – this is a collection of items which should be available in the laboratory area. It
includes, safety gloves, glasses, clamp stands. Other items specific to each experiment are listed in
the next section.
4. Experiment List – This section lists each of the experiments together with a list of chemicals where
they are needed and equipment. Note that some experiments are duplicated so that several groups
of students can work on this at once. The equipment lists will therefore need to be multiplied by 2 or
3 as appropriate. The procedures mentioned in this section relate to the procedure the students will
go through and not the procedure needed to set up the experiment. For the chemicals, some of
these are made up from standard solutions or prepared from concentrated solutions – details of this
have not been included but staff preparing for these experiments must have access to balances,
volumetric measurement systems as appropriate.
1. General Equipment
This section lists the general infrastructure needed in the laboratory areas.
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Water for hand washing, glass wear washing and drainage
o Cold water supply
o Hot water supply
Lockers for storing PPE
Ice making machine – or a supply of ice. Several experiments use ice as a source of cold or to
provide freezing 0 deg C solutions.
Storage cabinets for solvents, acids and alkali’s
Analytical Balances – Suggest at least two balances one covering a low weight range the
other a larger range (experiment list suggests 0-120g, 0-2kg)
Atmospheric Temperature & Pressure – need to have the ambient conditions in the lab
recorded. Suggest a pressure and temperature measurement:
o pressure measurement – e.g Omega instruments HHP360
o temperature measurements – e.g Omega RH520 Series
Microscopes – at least 2 microscopes will be needed for 2nd year experiments.
Natural gas burners / natural gas source – Would be useful to have a gas supply and busen
type burners. Not many experiments use this so the area with gas taps can be kept to a
minimum.
Plastic tubing – a supply of small bore 2mm, 5mm, 8mm diameter flexible plastic tubing is
useful to have in the lab – for connection to water taps and to pipe water from beakers to
drain.
Stop clocks – have suggested at least 3 or at least 2 per lab area be available.
Clamp stands – need a variety of clamp stands to hold beakers, test tubes, immersion
heaters.
Thermometers (-10 to 110 deg C range) – suggest about 10 to have in case needed. Use the
non-mercury filled ones as breakages can be common place.
General glass ware : beakers, measuring cylinder, pipettes, burettes
pH Meter & Electrodes – at least 1 meter per lab, with buffer solutions.
Conductivity Meter – probably have 1 available.
Distilled water unit – need something to supply clean water free from salts. De-ionised water
would be better but this is more expensive to run.
2. Potential Suppliers
We would recommend using a number of suppliers to make sure the best price is offered for
equipment. Fischer Scientific is our main supplier but be aware that these sell their own branded
equipment and that from other manufacturers.
For equipment of the same type (e.g analytical balances, water baths), we’d recommend keeping to
one manufacturer – it will help for spare parts.
Supplier
Fischer Scientific
Web Site
http://www.fisher.co.uk
Omega
Instruments
PHYWE
http://www.omega.co.uk
3B Scientific
http://www.3bscientific.co.uk
Carl Roth GmbH +
Co. KG
CAMLAB
http://www.carlroth.com
Edwards Vacuum
www.edwardsvacuum.com
Maplin Electronics
www.maplin.co.uk
http://www.phywe-systeme.com/
http://www.camlab.co.uk
Supplier for
General chemicals, lab equipment,
glassware
Pressure gauges, thermocouples
Specific heat capacity of water P1043900
or PN1349160 experimental kit
Dedicated experimental; kit and
equipment supporting these:
 Critical Point Apparatus :
U104001
 Boyle’s Law U17210
 Vacuum Pump U14501-230
General chemicals, lab equipment,
glassware
General chemicals, lab equipment,
glassware
Vacuum pump for boiling point elevation
experiment
General electrical items
3. SHOPPING LIST
A. Essential Lab Equipment
Item
Supplier
Suggested
Quantity
10 pks
Code
Cost (each)
Gloves EP disposable
examination medium M
Gloves EP disposable
examination large L
Gloves EP disposable
examination extra large XL
*Safety glasses Slam modern
design.
*Safety glasses temple
overglasses hingeless
*Monospec 2 safety
spectacles
Fisher
Scientific
Fisher
Scientific
Fisher
Scientific
Fisher
Scientific
Fisher
Scientific
Camlab
10000822 -
10 pks
10769824
2 pks
10580043
100
12659200
£19.85 pk of
50
£19.85 pk of
50
£19.85 pk of
50
£6.89 each
50 OR
12900585
£9.57 each
50 of these
£7.16 each
3
1137798
SA-8CLR-MB
LSE.505
11739825
10
11517283
£5.38 each
2
10484245
2
12452340
£134 pk of 24
boxes
£109 pk of 12
Mild Steel retort stands
500x13mm
10
Base Plates 200x125mm
5
Stronghold T Connector
10
Stronghold Closed Connector
10
Stronghold Stainless Lattice
Rods
10
Stronghold Burette Clamps
5
Stronghold medium clamp
10
1137405
L010/03
LHW.0006
1137403
L007/02
LHW.0002
1131974
53-2032-W
HD/53-2032-W
1131972
53-2012-W
HD/53-2012-W
1131987
53-2522-R
HD/53-2522-R
1131981
53-2170-W
HD/53-2170-W
1131978
53-2106-W
HD/53-2106-W
Stopwatch
Fisher
Scientific
Thermometer general purpose Fisher
-10°C to 110°C x 1°C
Scientific
Tissue wipes KIMTECH
Fisher
SCIENCE 2-ply
Scientific
Paper wipe Wypall L20 1-ply
Fisher
sheet size 510mm x 380mm
Scientific
Retort Stand Systems
CAMLAB
£48 each
£4.41 each
£14.92 each
£5.69 each
£5.56 each
£11.25 each
£33.38
£20.91
Item
Supplier
Strong Hold V shape Base
Plates
Suggested
Quantity
5
Code
1131984
53-2342-W
HD/53-2342-W
*NB: Safety Spectacles – better to decide on a common version for the building –
Cost (each)
£24.22
B. PPE For Students
Minimum would be Laboratory Coat, safety glasses. The general laboratory store should have
sufficient supplies in case students don’t bring theirs. At Riccarton we ask students to buy their own
PPE Kit consisting of Lab Coat, Glasses and a set of gloves.
C. General list of useful lab equipment
List of additional items that may be needed – note that syringes, stoppers are listed with each
experiment.
Item
Supplier
Code
Cost (each)
Fisher Scientific
Fisher Scientific
Suggested
Quantity
20
20
Solid rubber stoppers 13mm
Solid rubber stoppers 9mm
11532922
11502922
£9.65
£9.28
Solid rubber stoppers 3mm
10ml Disposable Syringes
20mL Disposable syringe nonsterile
50mL Disposable syringe nonsterile
Fisher Scientific
Fischer Scientific
Fisher Scientific
20
1
2 pks
11542922
Fisher Scientific
2 pks
11901563
£12.35
£26.20/ pk100
£44.40 pk of
100
£48.80 pk of
30
10178894
10785126
D. Laboratory Hardware
List of major items of hardware that you should also consider. As these are major items, recommend
that these be provided for centrally and all lab areas use them.
Item
Supplier
Code
Cost (each)
Comments
Ice making machine
Hubbard Ice Systems AF80
Microscope
Carl Zeiss Axio Vert.A1
Microscope
Carl Zeiss Primo Star
Compound
Ultrapure water system
NANOpure Diamond D11931
Spectrophotometer
Fisher
Scientific
Fisher
Scientific
Fisher
Scientific
10049789
£3500
70 kg/24hrs
12828065
£8820
1.25x 100x objective lens
10227942
£1560
compound, binocular LED.
10630632
£7270
10708535
£3830
pH Meter & Electrode
Fisher
Scientific
Fisher
Scientific
Fisher
10755384
£372
Edwards vacuum pump – 1
pump for 3 or 4 rigs
Edwards
Vacuum
Grant Recirculating
refrigerated Water Bath
model TX150-R2
Fisher
240V 50/60Hz life science
(UV/ultrafiltration)
Evolution 60S UV-Vis PC
control with VISIONlite
I would have at least 2 in the
lab – and keep the units of the
same type to avoid different
electrodes being used.
We don’t know the capacity
of our pump. The vacuum will
depend on the boilup rate
from the heating mantle. I’ve
based the sums on a 250W
heating mantle, running for
30 minutes, removing 0.4
litres/hr of steam.
General circulating bath. Will
be needed for 3rd year labs,
but possible add more in time
as research projects grow.
Note that better to go for R3
or R4 types – higher cooling
capacity.
£1890
12767829
£2930
4. EXPERIMENT DETAILS
1
Aim
Gases: Determination of the Molar Mass of a Gas
To determine the molar mass (M) of a gas by measuring the volume occupied by a
known amount of gas at a known temperature and pressure.
Chemicals
Name
Supplier
Chloroform
Fisher - 10071970 - Chloroform 99+%
1.4919g/mL stabilised with ca 0.75%
ethanol £16.70 for 1 litre
Fisher 10169182 - Ethyl acetate 99+%
Acros Organics £36 for 5 litres
Fisher 10172520 - 1,2-Dichloroethane
99.8+% (GC) £13.10 for 1 litre
Fisher 10233962 - Ethanol 99+% (GLC)
absolute duty free SpeciFied £541 for 25
litres
Ethyl Acetate
1,2 Dichloroethane
Ethanol (Absolute Alcohol)
Equipment Item
5-10 cm3 Gas Syringe (code number has
100ml)
Self sealing (bobby) caps
2 cm3 hypodermic syringe with needle
Small cork
Analytical balance
500ml Iso heating mantle
Safety
Issues
Procedure
Supplier
Fisher 12359249 - Syringe 100mL gas precision
ground outlet tube 6.5mm diameter x 1mL £
42.99 each
Fisher 11522942 - Stopper solid BS 2775
57mm bottom diameter
Sigma Z181633-1EA
Fisher 12306457 Stopper tapered cork 6mm
bottom diameter £4.71 each/pack of 20
Fisher 12703215 - Balance EL104 120g
analytical x 0.1mg
£1600
Fisher 11522674 - Heating mantle EM0500/CE
controlled 500mL flask capacity
Paper tissues (2 boxes)
500ml round bottom flask (boiling flask)
Z414514 SIGMA-ALDRICH
The liquids employed may be flammable. No open flames are
allowed during the experiment.
Dispose of any excess liquid in the flammable liquid residue bottle
provided in the fume cupboard.
1. Check that the boiling flask is half-full of water; if not, replenish with hot tap water. Switch on
the heating mantle. (You start the experimental measurements when the water is at boiling
temperature).
2. Rinse the inside of the hypodermic syringe with your unknown liquid sample, then draw into
it ~ 2 cm3 of the sample. Note the number of your unknown!
3. Dry the hypodermic needle, seal the needle with a small rubber or cork bung and weigh the
syringe, its contents and the bung using a 4-figure balance.
4. Remove the red self-sealing cap from the nozzle of the large gas syringe and set its volume to
~ 5 cm3 (of air).
5. Refit the cap over the nozzle of the syringe and allow the steam to pass through the jacket
surrounding the gas syringe until the temperature is constant (~100°C).
6. Record the temperature and the volume of the air in the gas syringe.
7. Remove the bung from the hypodermic syringe and insert its needle through the self sealing
cap on the gas syringe, making sure the needle tip is beyond the narrow nozzle.
8. Slowly inject the liquid into the gas syringe. The liquid will vaporize, pushing the syringe
barrel downwards. Inject sufficient to give a final volume of ~ 80 cm3.
9. Withdraw the hypodermic syringe and reseal it with the bung. Immediately record the
volume of air plus vapour in the gas syringe. The difference between this volume and that
in step 6 is the volume occupied by the vapour.
10. Reweigh the hypodermic syringe to obtain the mass of liquid injected.
11. Remove the self-sealing cap and reset the gas syringe to ~ 5 cm3.
12. Carry out steps 5 to 10 five times, reweighing the hypodermic syringe after each injection.
2
Aim
Chemicals
Equipment
Safety
Procedure
Solutions: Determination of the Molar Mass of a Solute from Freezing Point Depression
Measurements
The aim of this experiment is to determine the molar mass of a solute by measuring the
depression of the freezing temperature of a solution of the solute.
Name
Supplier
p-Dichlorobenzene
Napthalene
Fluorene Cyclohexane
(Possible 50 unknowns are made from
above solutes and placed in small bottles
Supply of Ice
Use ICE machine or buy in.
Item
Supplier
Cost
Glass outer cooling vessel with lid and
stirrer
Freezing tube containing test liquid, stirrer
and thermometer (-20 to +20 deg C range)
Low temperature -35 to +50 (-20 to +20
Cole Pamer OU-90300-51
£21.08
would be better)
Rubber pipette filter
Stop Clock
Fisher 11739825 - Stopwatch
£47.50 ech
Magnifying glass
CAMLAB 1138301 MB155-12
$4.63
20ml. Bulb pipette
Fisher 11843980 - Bulb pipette
£48.00pk of 2
BLAUBRAND ETERNA Class AS
conformity certified 20mL
50ml Beaker
Fisher 11507402 - Beaker squat £32.20 pk 10
form with graduations and
spout 50mL
Spatula
Fisher 10068061 - Spatula
£79.57 case of
150mm length micro tapered
50
end, v-shaped scoop antistatic,
non-pyrogenic, RNAse/Dnasefree
Filter paper, 11cm
Fisher 10027990 - Filter paper
£9.83 for 100
Grade No. 1 routine qualitative
sheets
110mm diameter
1. Cyclohexane is flammable. No open flames are allowed during the
Provide
experiment. 2. Never pipette by mouth, always use a rubber suction bulb. 3.
flammable
Dispose of all solutions in the flammable liquid residue bottle provided.
liquid waste
disposal
1. Fill the outer cooling vessel with ice-water to produce a freezing mixture. (Use the
minimum amount of water to produce a slurry.)
2. Make sure that the freezing tube is clean and dry.
3. Pipette exactly 20 cm3 of cyclohexane into the freezing tube. Close it immediately by
replacing the bung fitted with the thermometer and stirrer. (This cuts down any evaporation
loss).
4. Stir the cyclohexane gently but constantly. This is critical if good results are to be obtained.
5. Record the temperature every 15 s until the cyclohexane is frozen. Using a magnifying
glass, you should be able to read the temperature to a precision of about 0.05 °C.
6. Remove the freezing tube from the cooling vessel and allow the cyclohexane to melt and
return to room temperature.
7. Replace the freezing tube containing the cyclohexane and repeat steps 4 to 6.
3
Aim
Chemicals
Equipment
Safety
Procedure
Thermochemistry: Thermochemistry and Hess’s Law
The aim of this experiment is to determine the enthalpy change (ΔH) for each of three reactions
and to test Hess's Law.
Name
Supplier
2M Hydrochloric Acid Solution
Fisher 10020210 - Hydrochloric acid solution 2M
(2N)
2M Sodium Hydroxide Solution
Fisher 10070190 - Sodium hydroxide solution 2M
(2N) £19.75 for 1 litre
2M Ammonia
2M Ammonium Chloride
( I ) Make up 2.05M Solutions, as solution has to be at least 2.0M.
( II ) NH3: 1059mls – 8L 2.05M
Item
Supplier
Cost
o
o
Thermometer -5 – 50 C or -5 to 100 C
Fisher 11517283
2 nested polystyrene cups
Stop clock
Fisher 11739825 - £47.50 ech
Stopwatch
3x50ml measuring cylinders
Fisher 11303564 - £20.35 pk 2
Cylinder 50mL
measuring
spouted x 1mL
Magnifying glass
Graph paper
Ruler
The solutions of HCl, NaOH, and NH3 are toxic and corrosive. In
Use foul drain disposal route
particular, solutions of HCl and NH3 can cause chemical burns
, provided concentration of
and ruin your clothing.
acids/alkali is not high.
In the event of spillage wash the contaminated area thoroughly
with water and report the incident to the lecturer in charge.
Dispose of all solutions in the aqueous residue bottle provided
1. Put 50 cm3 of 2.0 M solution of HCl and 50 cm3 of 2.0 M solution of NaOH into two clean,
dry measuring cylinders. (In each case, this is 0.1 mole).
2. Measure the temperature of each solution using the same thermometer. However, rinse the
thermometer and dry it after the first measurement. The average temperature of the two
solutions is the initial temperature, Ti.
3. Add the HCl to the calorimeter, then add the NaOH and immediately place the top on the
calorimeter and gently mix for 30 s.
4. Record the temperature of the calorimeter contents to the nearest 0.05 °C after the 30 s and
every 30 s thereafter for 5 min.
5. Plot the temperature against the time. Use a ruler to extrapolate your results backwards, as
shown in Figure 1, to the time of mixing (t = 0). Record the extrapolated temperature, this
is Tf and it represents the highest temperature corresponding to the time at which the
solutions were mixed.
6. Repeat the above procedures using 2.0 M NH3 instead of NaOH.
7. Repeat again using 2.0 M NH4Cl and 2.0 M NaOH.
4
Aim
Chemicals
Equipment
Safety
Procedure
Chemical Kinetics: The Iodine Clock
The aim of this experiment is to determine a reaction rate expression using an initial rate
method.
Name
Supplier
0.1M Potassium Iodide
0.5M Sulphuric Acid
0.01M Sodium Thiosulphate
0.2% Starch Solution
2 Vol. Hydrogen peroxide
Item
Supplier
Cost
4x50ml burettes
Fisher 12184222 - Burette
£21.73 each
single bore class B 50mL
Stop Clock
Fisher 11739825 - Stopwatch
£47.50 ech
Thermometer (-10 to 110 deg C)
Fisher 11517283
£5.38 each
4xlarge boiling tubes
Fisher - 10253650 - Test tube
£96.39 pk of
heavy wall rimmed 16mm x
100
125mm
Boiling Tube Stand
?????
1ml Graduated Pipette
Fisher 10126494 - Pipette 1mL
£86.39 pk of
graduated class B x 0.1mL
12
5ml Graduated Pipette
Fisher 10719385 - Pipette 5mL
£107.52 pk of
graduated class B x 0.1mL
12
Rubber pipette filler
4x100ml glass beakers
Fisher 11517402 - Beaker squat £34.46 pk 10
form with graduations and
spout 100mL
4x small filter funnels
Fisher 12344016 - Filter funnel
£30.00 pk of 6
high speed 51mm
1. 0.5 M sulphuric acid is toxic and corrosive, and can cause chemical burns.
2. In the event of spillage, wash the contaminated area thoroughly with water and report the
incident to the lecturer in charge.
3. Never pipette by mouth, pipette the starch solutions using a rubber suction bulb.
4. Dispose of all solutions in the aqueous residue bottle provided.
1. Fill each of 4 burettes with the KI, H2SO4, Na2S2O3 solutions and water.
2. Clean and dry three boiling tubes. Prepare the following solutions in these clean tubes.
3. Pipette 1 cm3 of starch solution into each tube and shake well.
4. Measure out 2 cm3 of H2O2 in a graduate pipette as accurately as possible.
5. To the mixture for Experiment 1, quickly add the H2O2 and start the stop-clock. Quickly
insert a rubber bung in the boiling tube and shake vigorously for 5 seconds to ensure a
completely homogeneous solution.
6. Record the exact time at which the blue colour appears. Be alert - the colour appears
suddenly throughout the solution. (If it does not, you have not mixed the solution
thoroughly enough)
7. Record the temperature of the solution.
8. Repeat steps 5 to 7 for Experiment 2, this time using 4 cm3 of H2O2.
9. Repeat steps 5 to 7 for Experiment 3, this time again using 2 cm3 of H2O2.
10. Wash, rinse and dry the boiling tubes and rubber stoppers.
11. Repeat steps 2 to 9 to obtain concordant results (that is times for each experiment which do
not differ by more than 10 seconds).
Note that the total volume for each experiment is constant and equal to 50 cm3. This
ensures that doubling the volume of a reagent doubles its concentration.
5
Aim
Chemicals
Equipment
Safety
Procedure
Equilibrium Constant: Determination of an Equilibrium Constant
The aim of this experiment is to evaluate the equilibrium constant of a chemical reaction.
Name
Supplier
0.20M Fe(NO3)3 in 1M Nitric Acid
0.0020M Sodium Thiocyanate Solution
0.0020M Fe(NO3)3 in 1M Nitric Acid
Item
Supplier
Cost
6 x Big Test Tubes ( 150 x 16mm )
Fisher 10243310 - Test tube
£61.87 pk of
medium wall without rim
100
16mm x 150mm
Rubber Pipette Bulb
Fisher 12406180 - Pipette bulb
£17.90 pk of
dropper teats rubber 1mL
20
nominal capacity
2 x 25ml Burettes
Fisher 12358378 - Burette 25mL £70.09
double oblique bore class B
Schellbach x 0.1mL
Disposable Pipettes
Fisher 11307883 - Transfer
£55.58 pk of
pipette maxi sterile 6mL
400
Test Tube Rack
Fisher 11378633 - Test tube
£27.69 each
rack traditional 2 tier 10 places
for 18mm dia. tubes 250mm x
60 x 74mm
10ml Bulb Pipette
Fisher 11883950 - Bulb pipette
£38.00 pk of 6
BLAUBRAND ETERNA Class AS
conformity certified 10mL
3 x 100ml Beakers
Fisher 11517402 - Beaker squat £34.46 pk 10
form with graduations and
spout 100mL
3 x small Filter funnels
Fisher 11322194 - Filter funnel
£63.00 pk of 3
high speed 140mm
Glass Pasteur pipettes
Fisher 10026041 - Pipette
£62.68 pk of
Pasteur unplugged disposable
1000
150mm length
Ruler
1. 1 M nitric acid is toxic and corrosive, and can cause chemical burns. Never
Use foul drain
pipette by mouth, always use a rubber suction bulb
disposal route
2. In the event of spillage, wash the contaminated area thoroughly with water , provided
and report the incident to the lecturer in charge.
concentration
3. Dispose of all solutions in the aqueous residue bottle provided
of acids/alkali
is not high.
1. Pipette 10 cm3 of 0.20 M Fe(NO3)3 in 1 M HNO3 into a clean, dry test tube. Add exactly 2
cm3 of 0.0020 M NaSCN from a burette following by 8 cm3 of deionised water from a burette.
2. Mix this solution thoroughly with a clean Pasteur pipette. In this solution, the concentration
of Fe3+ is very much greater than that of SCN-. Consequently, formation of Fe(SCN)2+ is driven
to the right of reaction (3), essentially to completion (Remember Le Chatelier’s
principle). That means that you may assume that all the SCN- is converted to Fe(SCN)2+ and so
[Fe(SCN)2+] equals the initial molarity of SCN-.
Note, although you used SCN- = 2.0 x10-3 M, 2 cm3 of this was diluted to 20 cm3 so that actual
molarity of SCN- = [Fe(SCN)2+] = 2.0 x10-4 M. This is your standard solution.
1. Label five clean, dry test tubes 1 to 5.
2. Charge a burette with 0.0020 M Fe(NO3)3 in 1 M HNO3.
3. Add exactly 5.0 cm3 of the Fe(NO3)3 solution to each of the five test tubes.
4. Charge a second burette with 0.002 M NaSCN and add exactly 1.0, 2.0, 3.0, 4.0, and 5.0 cm3
of this solution to tubes 1 to 5.
5. Empty and thoroughly clean the burette containing the Fe(NO3)3 solution and then refill the
burette with deionised water.
6. Add 4.0 cm3 of water to tube 1; 3.0 cm3 to tube 2; 2.0 cm3 to tube 3; 1.0 cm3 to tube 4. No
water is added to tube 5.
7. Mix each solution thoroughly with a clean Pasteur pipette. The solution compositions are
summarized in the following table. In all cases the total volume is equal to 10 cm3.
8. Place test tube 5 next to the test tube containing the standard solution. Look down both
tubes towards a well illuminated piece of white paper as the background. Adjust the depth
of the standard solution by removing solution using a disposable pipette. Do not discard
any of the standard solution - you may need to return some solution if you overshoot in the
removal of solution. When the intensities of the colours in the two tubes match, measure
the depth of each solution with a ruler. This gives x, the concentration (in mol L-1) of
coloured complex in the equilibrium mixture x = 2.0x10-4 (depth of standard solution)/(depth of
unknown solution)
9 Repeat the procedure for matching of colour intensities of tubes 4, 3, 2 and 1 with the
standard solution.
6
Aim
Chemicals
Equipment
Safety
Procedure
Acids and Bases: Acid-Base Titration Curves
The aim of this experiment is to measure the concentrations of acids and bases using the widely
used laboratory analytical technique of pH titration.
Name
Supplier
pH 7 Buffer Solution
pH4 Buffer solution
Standardised 0.1M HCl Acid
Fisher 12900934 - Hydrochloric Acid Ready-to-use
standardised solution 0.1mol/L £15.10 for 1 L
Standardised 9.98M Acetic Acid
Standardised 0.12M NaOH Solution
Standardised 0.1M Ammonia Solution
Fisher 12900754 - Ammonia solution 0.1mol/L
concentrate dilute to 1000mL £21 for 100mL
Item
Supplier
Cost
pH Meter & Electrode
Fisher 10755384 - pH meter
£372
FiveEasy FE20-Kit 200mm x
175mm x 52mm bench with 9V
d.c. power adapter, electrode,
Wash Bottle (deionised water)
Fisher 10004704 - Wash bottle
19.95 pk of 5
narrow neck round 500mL
Pipette Bulb
Fisher 11987984 - Bulb pipette
£5.38 each
filler rubber 30mL
20ml Bulb Pipette
Fisher 11843980 - Bulb pipette
£48 pk of 2
BLAUBRAND ETERNA Class AS
conformity certified 20mL
50ml Burette
Fisher 12368378 - Burette 50mL £70.93 each
double oblique bore class B
Schellbach x 0.1mL
4x100ml Beakers
Fisher 11517402 - Beaker squat £34.46 pk 10
form with graduations and
spout 100mL
2xsmall filter funnels
Fisher 12344016 - Filter funnel
£30.00 pk of 6
high speed 51mm
Graph paper
1. Aqueous solutions of HCl, NaOH, and NH3 are toxic and corrosive. Aqueous
Use foul drain
CH3OH is corrosive. Never pipette by mouth, always use a rubber suction
disposal route
bulb.
, provided
2. In the event of spillage, wash the contaminated area thoroughly with water concentration
and report the incident to the lecturer in charge.
of acids/alkali
3. Dispose of all solutions in the aqueous residue bottle provided.
is not high.
1. Follow the instructions given in Appendix IV for setting up the pH meter. Rinse the pH
electrode thoroughly in deionised water.
2. Pipette 20 cm3 of the HCl solution provided (it is about 0.1 mol L-1, but record its exact
molarity) into a beaker, place the electrode in the solution, swirl the solution and record the pH.
Keep the electrode in the solution and set up the burette so that it can deliver directly into the
solution.
3. Begin the titration by adding successive portions of ~1 cm3 of the NaOH solution and record
the burette reading and, after swirling the solution, record the pH after each addition. There is
no need to wait more than a few seconds between additions.
4. The pH will increase only slowly to begin with. When the increase in pH (that is the difference
between two successive pH values) gets to be more than about 0.3 pH units, decrease the
portions that you add to ~ 0.2 cm3. Once the equivalence point (end-point) has been passed,
the pH change after each addition will decrease. When the change is again ~ 0.3 pH units,
return to ~1 cm3 portions. Continue the titration until you are ~ 15 cm3 beyond the end-point.
This completes titration (a).
5. Similarly obtain results for the titration of
(b) CH3CO2H (weak acid, pipette) against NaOH (strong base, burette)
(c) HC1 (strong acid, pipette) against NH3 (weak base, burette).
(d) CH3CO2H (pipette) against NH3 (burette).
Remember to rinse the glassware and pH electrode between titrations.
7
Aim
Chemicals
Equipment
Spectroscopic Analysis: Analysis of Heavy Metal Contaminant
The aim of this experiment is to verify the Beer-Lambert law and to use it to estimate the
concentration of Co2+ ions in a sample of water.
Name
Supplier
Cobalt Chloride (to make up solution)
Fisher 10020070 - Cobalt (II) chloride, anhydrous
Laboratory Reagent £104 for 100g
Item
2 x Helios B UV Spectrophotometers
2 x Shimadzu UV mini 1240
Paper Tissues
8x Test Tubes
1xsize 13 Rubber bungs (to fit test tubes)
Rubber pipette filler
Test tube rack
Safety
Procedure
Supplier
Cost
Fisher 10186164 - Test tube
medium wall without rim
10mm x 75mm
Fisher 11527093 - Stopper solid
neoprene 8mm bottom
diameter
£40.88 pk of
100
£11.04 pk of
20
Fisher 10785016 - Test tube
£112.91
rack 6029 20 x 17mm diameter
polycarbonate type B
Plastic cuvettes for UV System
Depends what
Spectrophotometer is bought
1x25ml Burette
Fisher 12358378 - Burette 25mL £70.09 each
double oblique bore class B
Schellbach x 0.1mL
2x5ml Graduated Pipettes
Fisher 11932178 - Pipette 5mL
£13.95 pk of 5
graduated type 2 class B x
0.05mL
2x100ml Beakers
Fisher 11517402 - Beaker squat £34.46 pk 10
form with graduations and
spout 100mL
2 small filter funnels
Fisher 12344016 - Filter funnel
£30.00 pk of 6
high speed 51mm
1. Aqueous solutions of cobalt chloride are toxic and an irritant.
Use foul drain
2. In the event of spillage, wash the contaminated area thoroughly with water disposal route
and report the
, provided
incident to the lecturer in charge.
concentration
3. Never pipette by mouth, always use a rubber suction bulb.
of acids/alkali
4. Dispose of all solutions in the aqueous residue bottle provided.
is not high.
1. Mark 7 dry test tubes with identification numbers from 1 to 7.
2. Using a pipette mix the following volumes of the CoCl2 solution provided (concentration
0.150 mol L-1) and water.
3. Thoroughly mix the contents of each test tube, but do not use your thumb as a stopper.
4. Fill a cell with solution 1 and measure its absorbance as a function of Wavelength using the
spectrophotometer. Determine both λmax (the wavelength of the maximum absorbance) and
Amax (the absorbance at λmax). Evaluate Amax for the remaining solutions.)
1. You have been given a solution containing an unknown concentration of CoC12. This solution
is too concentrated to be used directly and must be diluted. To establish the correct dilution,
first pipette 5 cm3 into a clean, dry test tube and dilute with water from a burette.
Record the volume of added water. Measure the absorbance of this solution at the
previously determined λmax. Continue diluting until the absorbance lies within the range of
your calibration data.
2. Your final result contains large experimental errors which have accrued during the several
dilutions. You must therefore prepare a new sample in one accurate dilution which is
equivalent to the overall dilution obtained in the previous set of trials. Establish what this is
and measure Amax of this diluted solution.
8
Aim
Chemicals
Equipment
Safety
Procedure
Effect of Pressure on Boiling Point/Boiling Point Elevation by Dissolved Salts
The aim of this experiment is to show how the boiling point of a liquid (water) changes with
applied total pressure. Pressure is varied from a moderate vacuum up to atmospheric pressure.
Results should be plotted in the form of an Antoine plot, and checked against standard data.
Name
Supplier
Tap or distilled water
NaCl (common salt)
Fisher 10092740 - Sodium chloride £10 per kg
Item
Supplier
Cost
Heating Mantle – for 1L flask
Fisher Scientific 11502674
£280
1L Round Bottom flask
11301935 - Flask 1L round
£39.22
bottom 2 necks 1 angled 24/29
centre 14/23 side socket
thermometer & quick fit adaptor
Fisher Scientific
£70
Vacuum Source (pump)
Edwards Vacuum
£1900
Suggest RV5 2 stage rotary
vane pump
0 to -1bar vacuum pressure gauge
RS 257-8381
£89.99
Wire gauze cage flask surround
??
pvc sheet for implosion guard
??
Glassware adapter 7mm cone ST52/13 for
Fisher 10821900
£44.95 pk of 2
vacuum connection
Glassware adapter 7mm cone ST51/13 for
Fisher 10187988
£44.95 pk of 2
thermometer
Hot surfaces – wear gloves when draining
the oiling flask
Vacuum pressure – wear safety glasses at
all times
1. Using 500 ml ordinary tap water measure the boiling point of the liquid at
various pressures (by applying vacuum to the vessel).
Notes: At a steady vacuum measure the boiling point temperature when the
mercury in the thermometer stops rising.
Start at a high vacuum and work towards atmospheric pressure - high
vacuum (low pressure) means low boiling point. It is easier gradually to heat
up the water as you decrease the vacuum.
2. Repeat the above experiment this time using a solution of a known
quantity of salt (NaCl) dissolved in 500ml. tap water. Use a minimum of 30gm
of salt.
Picture
Set up
Notes
The picture shows a red gas line coming from the top of the boiling flask. This is connected to the
vacuum pump. There is a pressure gauge (not shown) which records the pressure inside the
boiling flask, and several shut off valves which control the vacuum level inside the flask (these
are not shown on the photograph). The wire gauze and plastic shield are listed as items to
purchase, but these are for safety reasons only. There should be 1 pump used to draw vapour
from all boiling flasks.
Main pipeline to the Vacuum Pump
P-3
P-4
P-5
TO VACUUM PUMP
PRESSURE
I-2
P-1
P-2
V-1
TO VACUUM PUMP
V-2
THERMOMETER
THERMOMETER
500ml Glass
Flask with Side
port
HEATING MANTLE
500ml Glass
Flask with Side
port
HEATING MANTLE
Main pipeline to the Vacuum Pump
P-3
P-4
P-5
TO VACUUM PUMP
PRESSURE
I-2
P-1
P-2
V-1
THERMOMETER
THERMOMETER
500ml Glass
Flask with Side
port
HEATING MANTLE
9
Aim
Chemicals
Equipment
Safety
Procedure
TO VACUUM PUMP
V-2
500ml Glass
Flask with Side
port
HEATING MANTLE
Verification of Boyle’s Law and the determination of the molar volume of air at S.T.P.
To verify Boyle’s Law and determine the molar volume of air at stp (20 deg C, 760
mmHg)
Name
Supplier
none
Item
Supplier
Cost
Boyles Law Kit
3B Scientific or
£285
Fisher Scientific - 13172840
£259
Spare oil for Fisher unit
13102850
£30
The equipment used at Riccarton consists of a purpose built rig; a syringe, a pressure gauge, a
pad on top of the syringe and a set of weights. A known volume of air fills the syringe. Different
weights are placed on the pan and the resulting pressure is recorded. From knowing the mass
applied, the reading of the pressure gauge, the relationship between volume of air and pressure
can be determined.
The part number above is for a similar device which would achieve the learning outcomes of
this experiment, but with a different more modern item of kit.
Picture
10
Aim
Chemicals
Equipment
Safety
Procedure
Flash Point using the Pensky Martens Apparatus
To establish the flammability limits of given mixtures of a flammable and nonflammable component
Name
Supplier
n-heptane
Fischer 10215463 £32.60 for 1 litre
Liquid paraffin
Fischer 10407460 £59 for 2.5 litre
(use to make solutions of different concentrations of n-heptane in liquid paraffin –
0.5cc, 2.5cc in 100cc liquid paraffin)
Item
Supplier
Cost
Pensky-Martens Apparatus
Stanhope-seta
tbc
5 x100ml for samples
Fischer Scientific 11744329
£26/ pk 24
5 x 10ml disposable syringes
Fischer Scientific 10178894
£30/pk 100
2litre waste container (Winchester)
Adjustable pipette 100 micro litres to
Fisher 10234204 / 12487642 £194/£20.50
1000 microlitre tips
Matches or ignition source
1. Be Careful! You are using a naked flame in conjunction with flammable
liquids.
2. Hot oil and water is a dangerous mixture - Dispose of tested solutions into
the beaker provided; when cool, decant into the marked waste bottle. DO
NOT USE THE SINK.
3. Wear safety spectacles at all times.
4. Because of the use of hazardous chemicals, please read and comply with
the COSHH ‘risk assessment’ compiled for this experiment BEFORE starting
any experimental work.
5. On completion of the experiment, please leave the apparatus in a clean,
tidy and safe condition
Various mixtures of n-heptane / liquid paraffin are provided - concentrations varying from
0.5cc n-heptane to 2.5cc n-heptane in 100cc liquid paraffin. For calculation purposes,
liquid paraffin can be treated as C11H24.
2. Thoroughly clean and dry all parts of the cup and its accessories before starting the test.
Take care to remove all solvent used in this cleaning.
3. Fill the cup with the n-heptane / liquid paraffin mixture up to the level indicated by the
marked line.
4. Place the cup in the apparatus and fit the lid (ensuring correct location). Insert the
appropriate thermometer. TAKE CARE WITH THE THERMOMETER - THIS IS A
SPECIAL AND IS EXPENSIVE AND DIFFICULT TO REPLACE.
5. Light the test flame and adjust to the size of a bead 0.16ins. (4mm) in diameter - the size of
the steel ball on the apparatus.
6. Light the Bunsen and control the heating to such a rate that the temperature recorded by the
thermometer increases not less than 9° nor more than 11°F /minute (5 to 6°C/min.). Turn
the stirrer at a rate of 1-2 revs/sec while heating.
7. Apply the test-flame at each temperature reading which is a multiple of 2°F (1°C) up to
230°F (110°C). For the temperature range above 230°F apply the flame every 5°F (2°C).
Make the first application at a temperature at least 30°F (18°C) below the flash
temperature. The test-flame should be lowered in 0.5 sec., left in its lowered position for 1
sec. and quickly raised. Stirring should be discontinued during application of the testflame.
8. Read the flash point as the temperature shown on the thermometer at the time of the flame
application that first causes a distinct flash in the cup. Do not confuse the true flash point
with the bluish halo, which sometimes surrounds the test flame in the preceding
applications.
Current Lab
Picture
11
Aim
Chemicals
Equipment
Determination of the Thermal Properties of Water
Measure the specific heat capacity, the latent heat of fusion and the latent heat of
vaporisation of water at standard room conditions.
Name
Supplier
Source of Ice
Item
Analytical balance 0-2000g range
Ohaus scout pro
OR The Fisher version
Lab immersion heater 1000W
Single phase power meter
5A Variac power supply – Bench top
variac autotransformer 5A, 240V
1000ml Beaker (Tall one)
0-110 deg thermometer
Stirring rod
Safety
Procedure
Supplier
Scales&balances.co.uk
Cost
£185
Or Fisher 12724986 Balance ML4002/01 290mm
x 184mm x 83mm top pan
4200g x 0.01g
Carlroth
0.116.1 Small Model
Maplin
NK47KB Mains or Battery
Energy Monitor with built in
timer
RS 347-3697
£2150
Fischer Scientific 13137434 Beaker tall form with
graduations and spout 1L
Fisher 11517283 Thermometer general
purpose
11392514 - Stirring rod fused
ends glass 7mm O.D
£113.33 pk
10
40 EURO
£21
£167
£5.38 each
£13.20 pk 10
1. Hot surfaces – boiling water
2. Power supply
1. Fill the beaker provided with ice up to the 800 ml mark and note the mass of ice used.
2. Add a known weight of water to fill the voids. (note its temperature before adding)
3. Submerge the heater (take care not to burn it out! SEE SAFETY NOTE).
4. Switch on the heater and start the stop-clock.
5. Keeping the mixture stirred (as far as possible), measure the temperature at regular intervals,
and note when all the ice has melted.
6. Continue heating and note the temperature as a function of time, until room temperature is
reached. Switch off the heater.
Picture
Notes
The variac power supply controls the voltage to the heater – and will either be set at a low or
medium level so as not to heat the water in the beaker too fast. The analytical balance is used
to measure the changes in water volume especially once the water reaches boiling point and
starts to evaporate off. You will also need to monitor the electircal energy used by the heater
so suggest you monitor the energy or consuption using a mains plug in meter – the one
specified will measure both power (W) and energy (kWh – which is useful to watch students
reaise this is energy not power).
12
Aim
Chemicals
Equipment
Safety
Procedure
Specific Volume/Density Changes of Water as a Function of Temperature
To determine the density of liquids (water) and to see the effect of temperature on the
property.
Name
Supplier
Water
Item
Supplier
Cost
Hot plate stirrer
Fischer Scientific 10625435 - Magnetic £346.62
hotplate stirrer C-MAG HS 7 digital
glass ceramic top 100 to 1500rpm,
50°C to 500°C
50ml Density bottle
Fischer Scientific 12378965
£115.65 pk
of 5
Retort stand set
Use from general store.
1000ml Beaker
Fischer Scientific 12942161 - - Beaker
£91pk 10
squat form with graduations and
spout 1L
Stirring rod/stick
Fisher 11392514 - Stirring rod fused
£13.20 pk 10
ends glass 7mm O.D
Hydrometer
Fisher 12308657 - Hydrometer density £29 each
20°C shot loaded 190mm
100ml measuring cylinder
Fischer Scientific 11313564 - Cylinder
£39.75 pk of
100mL measuring spouted x 1mL
2
Small filter funnel
Fisher 12344016 - Filter funnel high
£30.00 pk of
speed 51mm
6
1. Prepare a water system (approx. 800 ml.) at a temperature as close to 20°C as possible by
using tap water and ice. Use the hot plate provided to melt the ice if necessary, but stir well
before noting the temperature. (see operational notes later)
2. Use the hydrometer and the density bottle to obtain the density of the water. (Notes on how
to use density bottles are available in Appendix VIII.) Throughout the experiment, heat losses
will vary so that in certain cases it will be necessary to measure the temperature before and
after the density determination so that an average value can be obtained.
3. Using the hot plate increase the temperature in steps of 5-10°C and determine the water
density by both means if possible as a function of temperature. Proceed as far as you can to the
limit of the instrument or until the water becomes too hot to handle (i.e. not any more than
60°C.).
4. Obtain a water system whose temperature is exactly 20°C and check that the hydrometer
calibration is correct.
Picture