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PS57 Amendments to Recipe Cards

As a result of the publication of the new edition of Hazcards in September 2007, it has been necessary to make
changes to the majority of Recipe Cards. These changes include alterations to the hazard classification of some
chemicals together with updated references to specific Hazcard numbers and changes to the names of some
chemicals to match those on the 2007 edition of Hazcards. The cover, contents list, how to deal with unusual
recipes and Index cards have also been revised.
More-substantial changes have been made to Recipe Cards 28, 39, 45 and 59.
The only Recipe Cards that have not been altered are 1, 2, 4, 15, 29, 51, 55, 63 and 64.
It is recommended that all changed Recipe Cards are either downloaded from the members-only part of the
CLEAPSS web site: www.cleapss.org.uk or accessed from the 2008 CLEAPSS Science Publications CD-ROM
when it is issued. Recipe Cards dated 2007 include all changes made to cards since 1999 that have previously
been listed in this document, PS57. If the paper version of Recipe Cards is still consulted, all the changed cards
should be printed to replace existing cards. Check that the card below, changed in 2001, has been corrected.
Changes made in 2001 to cards that have not been revised in 2007 include the following.
Recipe Card 64. The recipe for alkaline pyrogallol solution was changed – please replace the original card.

PS57 JAT 09/07 © CLEAPSS®, The Gardiner Building, Brunel Science Park, Uxbridge UB8 3PQ
28 Gas solutions
Comment: Aqueous solutions of gases should be prepared and tested just before use. In storage, solutions become weaker.
Procedures
Solution Preparation of solution Risk assessment
3 3
Bromine water 1. Add 1 cm of bromine to 500 cm of water in a 1 litre beaker. Add a Bromine is very TOXIC and CORROSIVE. Use
(3 methods to stirrer bar and place on a magnetic stirrer to dissolve the bromine. This a fume cupboard. Wear goggles or a face
make a can take some time. Dilute to 1 litre with water. Alternatively, a small shield and chemical-resistant gloves.
3 3
0.02 M ampoule (1 cm ) can be crushed (under 500 cm of water) and made
solution) up to 1 litre. The solution must be decanted so that no glass is present.
3 3
2. Dissolve 4.76 g of potassium bromide in 76 cm of water, add 14 cm Sodium chlorate(I) is CORROSIVE. Use a
3
of 10% (available chlorine) sodium chlorate(I) solution and 10 cm of fume cupboard. Wear goggles or a face
-3
2 mol dm hydrochloric acid. Dilute to 1 litre with water. shield.
3. Add 1.12 g of potassium bromate(V), 12 g of potassium bromide and (See also Hazcards 15A & B and 89.)
3 -3
14 cm of 2 mol dm hydrochloric acid into a 1 litre jug or measuring
cylinder. Add water to 1 litre and pour into a bottle.
Label the bottle of bromine water HARMFUL.
3
Chlorine water 1. Chlorine gas is bubbled into 250 cm water in a fume cupboard until Chlorine is TOXIC. Use a fume cupboard.
the solution goes light green. Wear goggles or a face shield.
2. To prepare a 1% (v/v) solution, one volume of 10% (available chlor- Sodium chlorate(I) is CORROSIVE. Use a
ine) sodium chlorate(I) solution is diluted ten times with water and one fume cupboard. Wear goggles or a face
-3
volume of 2 mol dm hydrochloric acid is added. shield.
Label the bottle of chlorine water HARMFUL. Further dilution is possible (See also Hazcards 22A & B and 89.)
which lowers the level of hazard.
See Hazcard 22B for a recipe using sodium dichloroisocyanurate.
3
Sulfur dioxide 1. In a fume cupboard, SO2 is passed into 250 cm of water via an Sulfur dioxide is TOXIC. Use a fume
solution inverted funnel with the rim of the funnel just touching the water surface. cupboard. Wear goggles or a face shield.
2. In a fume cupboard, dissolve 9.5 g of sodium metabisulfite in Sodium metabisulfite is HARMFUL. Use a
3 3 -3
100 cm of water. Add 100 cm of 0.5 mol dm sulfuric(VI) acid and fume cupboard. Wear eye protection.
3
make up to 250 cm .
Label the bottle “TOXIC sulfur dioxide will be given off”. Further dilution is [See also Hazcards 92 & 97 and CLEAPSS
possible and recommended. Laboratory Handbook 13 (Gases).]
See Hazcard 92 for a recipe to simulate acid rain.

© CLEAPSS 2007
29 Gram stain – part 1
Comment: The Gram staining technique is used to distinguish between two types of bacteria: Gram-positive and Gram-
negative. The following procedure will provide you with a thin film of bacteria on a microscope slide, for
staining.
Preparation of a heat-fixed smear
♦ Using a clean microscope slide and, using a sterile inoculating loop, place a single drop of
water in the centre of the slide.
♦ Mix in a small amount of a sample from a single bacterial colony, until the suspension is
slightly turbid.
♦ Smear the suspension over the central area of the slide, to form a thin film. For liquid
cultures, use a single drop of culture fluid, spread in a similar manner.
♦ Allow to dry in the air at room temperature which may take a few minutes.
♦ Fix the air-dried film by passing the slide through a Bunsen burner flame. Using forceps to
hold the slide, pass it horizontally, film side up, rapidly through the hottest part of the flame
just above the blue cone. Repeat this twice more. (Excessive heating will ruin the
preparation. It is customary to check that the slide has not been overheated by touching it,
after each flaming, on the back of the hand. The slide will feel hot but should not be painful!
If it is, start again.)
♦ Allow to cool; the smear is now ready for staining.

© CLEAPSS 1999
38 Inorganic test reagents-2
Recipes for making 100 ml of solution
A. Magenta (basic fuchsin) for sulfite ions F. Sodium hexanitrocobaltate(III) (cobaltinitrite) (0.16 M) for
Dissolve 0.02 g in 100 ml of water. potassium ions
Dissolve 6.8 g of the solid in water and make up to 100 ml.
! Fuchsin is HARMFUL by inhalation, in contact with skin and if
swallowed. No hazard warning is required on the solution. ! This substance is TOXIC & OXIDISING. See Hazcard 95A. It is
B. Magneson(II) for magnesium ions an unstable solution with a maximum shelf-life of 3 weeks.
Dissolve 0.001 g in 100 ml of water. No hazard warning is required on the solution.
G. Sodium sulfide (0.2 M) for metal ions
! Magneson is HARMFUL if swallowed, if inhaled and by skin
Dissolve 5 g of the solid in water and make up to 100 ml.
contact. No hazard warning is required on the solution.
C. Potassium hexacyanoferrate(II) (0.1 M) for iron(III) ions ! The solid is CORROSIVE (see Hazcard 51). Prepare the solu-
Dissolve 4.22 g in 100 ml of water. tion in a fume cupboard, wearing gloves and eye protection.
The preparation produces hydrogen sulfide gas (see Haz-
! See Hazcard 79. No hazard warning is required on the card 51) which has an obnoxious smell. Label the solution
solution. IRRITANT.
D. Potassium hexacyanoferrate(III) (0.1 M) for iron(II) ions H. Thiourea for tin(II) ions
Dissolve 3.29 g in 100 ml of water. Dissolve 10 g in 100 ml of water.
! See Hazcard 79. No hazard warning is required on the ! Thiourea is a category 3 carcinogen (see section 7.8 of the
solution. CLEAPSS Laboratory Handbook) and HARMFUL if swallowed.
E. Potassium thiocyanate (0.1 M) for iron(III) ions I. Uranyl(VI), zinc(II) or magnesium ethanoate for sodium
Dissolve 1.0 g in 100 ml of water. ions
! Potassium thiocyanate is HARMFUL. See Hazcards 55C and Dissolve 10 g of uranyl(VI) ethanoate and either 30 g of
zinc(II) ethanoate or 33 g of magnesium ethanoate in 12 ml
95C. No hazard warning is required on the solution.
of 5 M ethanoic acid. Dilute to 100 ml, add 0.1 g of sodium
chloride, allow to stand for 24 hours, then filter.
! See Hazcard 105. Wear eye protection, gloves and a labor-
atory coat. Avoid raising dust. Label the solution VERY TOXIC
and RADIOACTIVE.

© CLEAPSS 2007
39 Iodine solution
Comment: Iodine is only sparingly soluble in water (0.3 g l-1) and it is usual to dissolve it in potassium iodide solution
(KI) or organic solvents such as ethanol. A 0.01 M solution is suitable as a starch test reagent.
Formula I2 Molar mass: 253.80 g mol-1
Hazards Iodine is HARMFUL by inhalation and in contact with the skin. See Hazcard 54. The organic solvents

! Control measures
used are also hazardous and the relevant Hazcard should be consulted.
Wear eye protection and gloves when weighing. The room should be well ventilated.
Mass of solids (g) to be used
Concentration Hazard warning Volume (ml) of solution required
required label 100 250 1000
0.01 M - Ten-fold dilution of the 0.1 M solution
0.05 M - 1.5 g of KI + 1.27 g of I2 5 g of KI + 3.17 g of I2 20 g of KI + 12.69 g of I2
0.1 M - 3.0 g of KI + 2.54 g of I2 10 g of KI + 6.35 g of I2 40 g of KI + 25.38 g of I2
Procedure
♦ Measure out the indicated quantity of potassium iodide (KI) into an appropriate beaker.
♦ Moisten the potassium iodide with a few drops of water.
♦ Measure out the indicated quantity of iodine and add it to the moistened potassium iodide.
♦ Add a small volume of water and stir. When no more iodine appears to dissolve, add some more
water and stir. Keep repeating this procedure until all the iodine has dissolved.
♦ Pour the solution into a measuring cylinder and dilute to the final volume. Make sure there are no
bits of iodine remaining. If there are, return the solution to the beaker and leave it on a magnetic
stirrer for several minutes.
♦ Add the solution to a labelled bottle and mix well.
‘Tincture of iodine’
♦ Dissolve 2.5 g potassium iodide and 2.5 g iodine in 100 ml of ethanol. Label this solution HIGHLY
FLAMMABLE & HARMFUL.
© CLEAPSS 2007
44 Nitric(V) acid
Comment: The strength of commercial concentrated solution is about 70% (w/v) and has a specific gravity of 1.42. Old
stock may be weaker in strength than freshly-bought solutions. It should be stored in dark bottles. When
exposed to light, the solution goes brown and TOXIC nitrogen dioxide gas is produced (see Hazcard 68).
Formula: HNO3 Molar mass: 63.01 g mol-1
Hazards Nitric(V) acid is CORROSIVE and OXIDISING. If in contact with the skin, this becomes yellow and layers of

! Control measures
skin peel off. See Hazcard 67.
Wear suitable eye protection (a face shield is preferable) and gloves. Use a fume cupboard if necess-
ary.

Volume of 70% (w/v) nitric(V) acid (ml) to be used


Concentration Hazard Volume (ml) of solution required
required warning label 500 1000 2500
0.01 M - Ten-fold dilution of the 0.1 M solution
0.1 M IRRITANT Ten-fold dilution of the 1 M solution 16
0.4 M IRRITANT 12 25 62
1M CORROSIVE 31 62 155
5M CORROSIVE 155 310 775

Procedure
♦ Measure out the indicated volume of concentrated nitric(V) acid in a measuring cylinder.
♦ Add the liquid to about two thirds of the final volume of water in a beaker.
♦ Stir the solution. (Heat will be given out and the solution will become warm.)
♦ Pour the solution into an appropriate measuring cylinder and dilute to the final volume.
♦ Pour the solution into a labelled bottle and mix well. Add a hazard warning if appropriate.
Comment: Also available from suppliers is 95-100% (fuming) nitric(V) acid, which is even more hazardous as it is unstable. If there
happens to be any old stock still present in the school, then it is better to dilute it as soon as possible.

© CLEAPSS 2007
45 Nylon rope experiment
Comment: Although used in the past, tetrachloromethane (carbon tetrachloride) (see Hazcard 100) and 1,1,1-trichloroethane
(see Hazcard 103), if available, should no longer be chosen as the solvent. An alternative solvent is cyclohexane.
Hexanedioyl chloride (adipoyl chloride) may be used but is more unstable in storage, so it is normally better to buy
decanedioyl (sebacoyl) chloride.

Hazards The acid chlorides and hexane-1,6-diamine are CORROSIVE (see Hazcards 3B & 41) and cyclohexane

! Control measures
is HIGHLY FLAMMABLE and HARMFUL (see Hazcard 45B).
Wear eye protection. Wear disposable nitrile gloves when pulling out the nylon thread. The room
should be well ventilated and there must be no sources of ignition.

Procedure using cyclohexane as the solvent


♦ Dissolve 2.2 g of hexane-1,6-diamine in 50 cm3 of distilled water in a beaker (label it ‘A’).
♦ Dissolve 1.5 g of decanedioyl chloride or hexanedioyl chloride in 50 cm3 of cyclohexane in
another beaker (label it ‘B’) and add HIGHLY FLAMMABLE & HARMFUL warning signs.
♦ Carefully pour the solution from beaker B onto solution A down a glass rod. The two liquid
phases do not mix; resist any attempt to stir the mixture at all.
♦ Use forceps to pull out the nylon formed at the interface of the two solutions.

© CLEAPSS 2007
59 Slime
Comment: The material formed is a gel. It is thought that borate ions react with hydroxyl groups in the polymer of vinyl alcohol to
form cross links with the elimination of water. These cross links probably involve hydrogen bonds which continually form
and break under flow. The ‘sliminess’ of the gel can be adjusted by altering the amount of sodium borate used. Viscosity
changes can be detected by timing the passage of a ball bearing through the ‘slime’ in a measuring cylinder. If acid is
added to the ‘slime’, the gel collapses to give a free-flowing solution. Although the slime can be stored in a labelled sealed
bag and placed in a refrigerator, it can develop mould if kept for long periods. Disposal: Add enough 1 M sulfuric(VI)
acid just to allow the solution to be free-flowing, dilute and pour down a foul-water drain.
Different sources of polyvinyl alcohol vary in their average molar mass; some are about 115 000 g mol-1, while others are
much less at around 17 000 g mol-1 (and less expensive). PVA wood glue is cheaper still and contains polyvinyl acetate
and alcohol but the formulations from suppliers vary considerably.
Hazards None of the reagents are particularly hazardous, although sodium tetraborate solutions are alkaline

! Control measures
and may irritate the skin. There is a lot of vigorous stirring of hot liquids.
Wear eye protection. Hot water from a kettle may be useful to start with.
Procedure
Using polyvinyl alcohol (PVA):
♦ Pour about 100 ml of water (no hotter than 90 °C) into a 400 ml beaker, add 4 g of high-mass (8 g of low-mass)
polyvinyl alcohol, stirring rapidly. Add food colouring and/or fluorescent dye, eg, fluorescein, for added
(disgusting) effect. (Solution A.)
♦ Heat to 90 °C (but do not boil) and keep stirring as required until the polymer dissolves. Allow the solution to
cool. All of this may take some time!
♦ If a high-mass PVA was used to make solution A, dissolve 0.80 g of sodium tetraborate-10-water (0.42 g of
anhydrous sodium tetraborate) in 20 ml of water. If a low-mass PVA was used, dissolve 1.6 g of sodium
tetraborate-10-water (0.84 g of anhydrous sodium tetraborate) in 20 ml of water. (Solution B.)
♦ Add solution B to A with vigorous stirring. Let the gel form before removing and washing it with water.
Using PVA glue:
♦ Dilute it to about 25%; there is no need to heat it but mix it well with water. Add sodium tetraborate as
prepared above for use with low-mass PVA. Change the concentration of PVA glue to alter the ‘slime’ quality.
© CLEAPSS 2007
60 Soap and bubble solutions
Comment: Soap solutions can be titrated against tap water in a stoppered bottle until a froth, stable for 15 seconds, is
obtained. The strength of the soap solution and/or volume of water involved in the titration will depend on the
hardness of the local tap water. Both solutions should be tested before being presented to a class so that minor
adjustments can be made.
Hazards Some of the solutions are made up in ethanol which is HIGHLY FLAMMABLE & HARMFUL (see Hazcard

! Control measures
40A). Propane-1,2,3-triol is LOW HAZARD (see Hazcard 37).
Do not heat soap solutions made up in ethanol with a naked flame. Use a hot plate or surround the
beaker with hot water.
Procedure to make a soap solution suitable for titration
♦ Dissolve 5 g of soap flakes (eg, Lux) in 500 ml of ethanol by stirring the suspension on a hot
plate. This may take some time.
♦ After cooling, pour the solution into a 1 litre volumetric flask and dilute to 1000 ml with
pure water. Mix the solution well.
♦ The titration with tap water to obtain a permanent froth should be rehearsed so that
adjustments to the volume of tap water or concentration of the soap solution can be made.
Bubble mixture1
♦ Mix together by volume, 10 parts liquid detergent, 85 parts pure water and 5 parts propane-
1,2,3-triol (glycerol).

1 From the Salters’ Chemistry Handbook. Contact The Salters’ Chemistry Club, Salters’ Hall, Fore St, London EC2Y 5DE.
Tel: 020 7628 5962; Fax: 020 7638 3679. © CLEAPSS 2007
63 Sodium chloride
Formula: NaCl Molar mass: 58.44 g mol-1

Mass (g) of solid to be used


Concentration Hazard Volume (ml) of solution required
required warning label 100 250 1000
0.01 M - Ten-fold dilution of 0.1 M solution
0.1 M - Ten-fold dilution of 1 M solution 5.84
1M - 5.84 14.61 58.44
Saturated (20°C) - >37 >93 >370
Procedure
♦ Measure out the indicated quantity of sodium chloride.
♦ Add the solid to about two thirds of the final volume of water in a beaker.
♦ Stir to dissolve. Warm it if necessary.
♦ Pour the solution into an appropriate measuring cylinder and dilute to the final volume.
♦ Pour the solution into an appropriate labelled bottle and mix well.

© CLEAPSS 1999
64 Sodium hydrogencarbonate
Formula: NaHCO3 Molar mass: 84.01 g mol-1
Mass (g) of solid to be used
Concentration Hazard Volume (ml) of solution required
required warning label 100 250 1000
0.01 M - Ten-fold dilution of the 0.1 M solution
0.1M - Ten-fold dilution of 1 M solution 8.40
1M - 8.40 21.00 84.01
Saturated (20°C) - 9.6 >24.0 >96
Procedure
♦ Measure out the indicated quantity of sodium hydrogencarbonate.
♦ Add the solid to about two thirds of the final volume of pure water.
♦ Stir to dissolve. Do not warm the solution.
♦ Pour the solution into an appropriate measuring cylinder and dilute to the final volume.
♦ Pour the solution into an appropriate labelled bottle and mix well.
Alkaline pyrogallol solution for absorbing / removing oxygen gas
Comment: Benzene–1,2,3-triol (pyrogallol) is HARMFUL (see Hazcard 12). Wear eye protection when preparing the solution. This
safer procedure replaces sodium hydroxide. However, the rate of absorption of oxygen by the alkaline solution produced
using sodium hydrogencarbonate may be too slow for some gas analysis activities in which air samples are exposed to the
benzene–1,2,3-triol for only a short time. In such circumstances, there is no alternative to the use of sodium hydroxide.
The procedure described below limits the absorption of oxygen from the air. For some activities, eg, the removal of oxygen
from the air around seeds in studies of germination, it is inappropriate. For such studies, first add the benzene–1,2,3-triol
crystals to the flask, tube etc and then the sodium hydrogencarbonate solution. Add the seeds and stopper the container.
♦ Prepare a saturated solution of sodium hydrogencarbonate using freshly-boiled pure water.
♦ Place a wide-bore glass tube into the water and then pour liquid paraffin on the water’s surface.
♦ Add a few crystals of benzene–1,2,3-triol (pyrogallol) down the glass tube and then slowly withdraw it. (1 g of
benzene-1,2,3-triol is capable of absorbing 190 cm3 of oxygen.)
© CLEAPSS 2001

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