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HSC Chemistry Practicals

Production of Materials

 PRACTICAL – Identify data, plan and perform a first-hand investigation to compare the reactivities of
appropriate alkenes with the corresponding alkanes in bromine water:
– In this experiment, 10ml of an alkene (cyclohexene) and 10ml of its corresponding alkane
(cyclohexane), were placed in two separate test tubes, each containing 10ml of a solution of yellow
bromine water.
– RESULT: It was observed that cyclohexene turned the bromine water colourless, whereas the
cyclohexane solution remained yellow.
– Thus ONLY cyclohexene reacted with the bromine water, and thus the alkene was said to be more
reactive than its corresponding alkane; this is due to the double bond of the alkene.
– Reaction:

– JUSTIFY the method:


 Cyclohexene and cyclohexane were used, instead of ethylene or propene because C1 to C4 are
gases at room temperature, and would be hard to manage; cyclohexene is liquid at room
temperature.
 Also cyclohexene/ane was used instead of hexene/ane because cyclic hydrocarbons are more
stable than their linear counterparts.
– LIMITATIONS of the method:
 The alkane reacted slightly, as UV radiation caused slow substitution reactions.
– SAFETY precautions:
 Bromine water is highly toxic if ingested, and is slightly corrosive.
 Cyclohexene and cyclohexane are both poisonous if ingested, and both give off fumes, as they
are highly volatile and highly flammable.
 PRACTICAL – Analyse information from secondary sources such as computer simulations, molecular
model kits or multimedia resources to model the polymerisation process:
– In this experiment, molecular modelling kits were used to show how polyethylene is produced
through the polymerisation of ethylene.
– The class was divided into groups, and each group was provided with a kit.
– 3 ethylene monomers were created by each group, with black balls representing carbons and smaller,
white balls representing hydrogen.
– Then the monomers were ‘polymerised’: each group combined their monomers with every other
group until a large chain was created – a section of polyethylene.
– JUSTIFY the method:
 The models created a 3D representation of the chemical process, which led to greater
understanding of polymerisation.
 The use of ball-and-stick models, depicting the double-bond with flexible rubber rods, greater
increased understanding of the process.
– LIMITATIONS of the method:
 The model only provided a very limited section of a polyethylene molecule, as there were limited
numbers of kits.
 The use of catalysts (such as Zeigler-Natta catalysts) was not shown in the process, and thus it
was not completely accurate.
 PRACTICAL – Process information from secondary sources such as molecular model kits, digital
technologies or computer simulations to model the addition of water to ethylene and the dehydration of
ethanol:
– Molecular modelling kits were used to model:
 the addition of water to ethylene (hydration)
 the removal of water from ethanol (dehydration)
– “Ball-and-stick” kits were used, where black balls represented carbons, smaller, white balls
representing hydrogen, and red balls represented oxygen.
– Firstly, and ethylene molecule was created, and a water molecule created:
 Then, the water molecule was split into a H+ ion and an OH- ion
 The double-bond of ethylene was opened, and the ions were attached where there were free
bonding sites; the resultant molecule was ethanol
– Secondly, a separate ethanol molecule was created:
 The hydroxide group (OH-) and a hydrogen was removed from the ends
 They were combines, and water was formed; the two open bonding sites of the ethanol were
joined, and ethylene was formed.
– JUSTIFY the method:
 The models created a 3D representation of the chemical process, which led to greater
understanding of dehydration and hydration processes.
 The use of ball-and-stick models, depicting the double-bond with flexible rubber rods, greater
increased understanding of chemical reactions.
– LIMITATIONS of the method:
 Both were severely simplified representations of chemical processes, which had many multiple
steps and consisted of a series of aqueous (dilute sulfuric acid) or solid catalysts.
 PRACTICAL – Solve problems, plan and perform a first-hand investigation to carry out the
fermentation of glucose and monitor mass changes:
– In this experiment, sucrose solution was fermented to form
ethanol and carbon dioxide. The yeast cells first split sucrose
into two glucose molecules using the invertase enzyme .
– A 250 mL side-arm conical flask with a rubber stopper was
used. A plastic hose was connected to the side arm, and the end
of the hose was placed in another conical flask in a solution of
limewater. No gas was allowed to escape the apparatus:
– 100 ml of 0.15 M sucrose solution was placed in the conical
flask. ONE gram of active yeast was placed into the sucrose, along with a pinch of sodium
biphosphate (Na2HPO4) as a yeast nutrient. This was mixed thoroughly.
– The stopper firmly put on, and the flask was WEIGHED with an electronic scale.
– The apparatus was then set up as shown, with the yeast beaker in a water bath at a constant
temperature (37°C).
– Both flasks were weighed daily for 5 days.
– RESULTS:
 The yeast flask turned foamy and smelt clearly of alcohol, while the limewater turned cloudy;
this proved that CO2 and ethanol were produced, and that fermentation occurred.
 The mass of the yeast flask also steadily decreased by about half a gram each day; this is due to
the carbon dioxide escape; the limewater flask also gained approximately the same mass.

– JUSTIFY the method:


 A “closed” system (where no gas was allowed to escape) was used to ensure an accurate
experiment.
 Limewater was employed to prove CO2 was produced.
 The water bath ensured that the most optimal fermentation occurred.
– LIMITATIONS of method:
 The combined masses of both flasks steadily decreased as well; this was due to inevitable
leakages of gas.
 The atmosphere in the flasks was not anaerobic (oxygen-free) and this could have hampered the
fermentation process.

 PRACTICAL – Identify data sources, choose resources and perform a first-hand investigation to
determine and compare heats of combustion of at least three liquid alkanols per gram and per mole:
– The 3 alkanols used were: methanol,
ethanol, and 1-propanol
– Each alkanol was placed in a spirit burner;
the original mass recorded, and then was used
to heat 200 mL of water (at 25°C) in a tin
can.
– A thermometer was used to stir the water as
well as measure the temperature
– Once the temperature rose by 10 degrees
(Kelvin or Celsius, it doesn’t matter; they
both use the same scale) the spirit burner was
capped and immediately reweighed.
– RESULTS:
 The ΔH (change in heat) was calculated for each alkanol by using the formula ΔH = -mCΔT.
This was then calculated per gram, and then per mole, to give the heat of combustion per gram,
as well as the molar heat of combustion.
 Methanol has the lowest value, followed by ethanol, and then 1-propanol.
 NOTE: This is not because of the extra bonds in longer hydrocarbon chains, but rather more
bonds need to be created in the products (H2O and CO2); recall that:
 creating bonds releases energy.
 breaking bonds absorbs energy.
– JUSTIFY the method:
 A tin can was used as it is a better thermal conductor than a glass beaker
 Methanol, ethanol and 1-propanol were used as they are the shortest alkanols and thus are the
most likely to undergo complete combustion
– LIMITATIONS of method:
 Molar heat of combustion refers ONLY to complete combustion; the yellow flames and soot
formed indicated that the combustion was incomplete. Thus the experimental data gathered is
inaccurate.
 Also, much heat was lost to the air, as there was not 100% efficiency of heat transfer from flame
to tin can.
– Heat was also radiated from the can to the air; insulation would reduce this.

 PRACTICAL – Perform a first-hand investigation to identify the conditions under which a galvanic cell
is produced:

– A galvanic cell was produced in the lab


in the same set-up as on the right; that
is, in the form of a DANIELL CELL
– A 2 cm strip of zinc and copper were
cut from metal strips. Using wire leads
and crocodile clips, the zinc strip was
connected to the NEGATIVE terminal
of a voltmeter, and the copper strip
connected to the POSITIVE terminal
– The zinc was then placed in 50 mL of
1M solution of zinc sulfate, and the copper in 50 mL of 1M solution of copper sulfate.
– A strip of filter paper was soaked in potassium nitrate; the two cells were then connected using this
‘salt bridge’
– RESULTS: The voltmeter showed a reading of 0.4 volts. When more electrolyte was added, the
voltage stayed at 0.4 volts; thus the voltage is determined ONLY by the metals used, and has nothing
to do with the amount of copper or zinc.
– JUSTIFY the method:
 Copper and zinc were used as they are readily available, non-toxic metals
 1M solution was used as the ratio of moles of the salts was 1:1
 A potassium nitrate salt bridge was used as potassium and nitrate ions do not react with zinc,
copper of sulfate ions.
 PRACTICAL – Perform a first-hand investigation and gather first-hand information to measure the
difference in potential of different combinations of metals in an electrolyte solution:
– The same experiment above was performed again, except a range of difference electrode electrolyte
couples were used
– RESULTS:
 [ Zn | Zn2+ || Cu2+ | Cu ]: TOTAL voltage = 0.4 V
 [ Mg | Mg2+ || Cu2+ | Cu ]: TOTAL voltage = 0.95 V
 [ Al | Al3+ || Cu2+ | Cu ]: TOTAL voltage = 0.2 V
 [ Fe | Fe2+ || Cu2+ | Cu ]: TOTAL voltage = 0.5 V
The Acidic environment

 PRACTICAL – Perform a first-hand investigation to prepare and test a natural indicator:


– Most indicators are derived from natural plant sources.
– In this experiment, an indicator was made from beetroot.
– One large beetroot was peel and chopped; it was then blended thoroughly using a food processor
with 100 mL of distilled water.
– The mixture was strained into a beaker; this is the indicator.
– In 4 separate test-tubes, 3 mL of distilled water, sodium chloride (NaCl) solution, hydrochloric acid
(HCl) and sodium hydroxide (NaOH) solution was placed.
– Then using a dropper, 3 drops of beetroot indicator was added to the test-tubes.
– RESULTS:
 In the distilled water, it was DARK PURPLE.
 In the NaCl solution, it was DARK RED.
 In the HCl solution, it was PINK.
 In the NaOH solution, it turned YELLOW.
– JUSTIFY the method:
 Beetroot was used as it is a very vividly coloured plant; and its pigmentation is very easily
extracted.
 A fresh beetroot was used instead of canned beetroot as the canned version may contain
preservatives (many of which are weak acids) that may affect the results.
 HCl and NaOH was used as they are on opposite ends of the pH scale; this was to show the range
of colours the indicator could produce.
– LIMITATIONS of the method:
 Beetroot come in many sizes; this was not controlled.
 The exact pH at which the transition of colours occurred was not determined.
 This could be performed through the use of pH meters or data loggers.
 PRACTICAL – Identify data, plan and perform a first-hand investigation to decarbonate soft
drink and gather data to measure the mass changes involved and calculate the volume of
gas released at 25˚C and 100kPa.
– A 300mL bottle of soft drink was decarbonated by vigorous shaking, and then releasing the gas by
opening the cap; no drink was allowed to spill.
– The bottle was weighed at the beginning, and the end.
– It was assumed that any mass loss was due to carbon dioxide loss.
– RESULTS:
 2.4 g of CO2 was released. To calculate the volume of gas released at 25˚C:
n = m/M (mass/molar mass)
= 2.4/44; molar mass of CO2 = 44
= 0.0545 mol
V = n × MV (moles × molar volume)
= 0.0545 × 24.79
= 1.35L
– JUSTIFY the method:
 The shaking affected the CO2/H2CO3 equilibrium, and this forced the gas out.
 No liquid was allowed to spill to try to keep a high level of accuracy.
 Electronic scales were also used for accuracy.
– LIMITATIONS of the method:
 The accuracy of this method is limited, as there may be loss of water as gas, or there may still be
CO2 dissolved.
 PRACTICAL – Solve problems and perform a first-hand investigation to use pH
meters/probes and indicators to distinguish between acidic, basic and neutral chemicals:
– Part A - Testing Substances With Methyl Orange:
 10 test-tubes were set up with 5 mL of acidified solution (0.1 M HCl).
 2 drops of methyl orange were placed in each test-tube.
 A range of substances was dropped in each test-tube, from various carbonates, metal oxides,
sulfates, and common household substances.
 Any change, such as indicator colour change or bubbles, was recorded.
– RESULTS:
 It is known that methyl orange is red in strongly acidic solutions, and yellow in slightly acidic to
highly alkaline solutions.
 Any substance that caused the acidified solution to turn yellow was classified as a base. This
included:
 Carbonates: Calcium carbonate and sodium hydrogen carbonate caused the solution to turn
yellow and formed bubbles.
 Metal Oxides: Calcium oxide and zinc(II) oxide turned the solution yellow, without any
bubbles.
 Hydroxides: Magnesium hydroxide rapidly turned the solution yellow.
 The other substances caused no change in the solution; these were labelled acidic or neutral.
These included sucrose, salt (NaCl), lemon juice, vinegar and magnesium sulfate.
– Part B – Testing Common Substances Using a pH Meter:
 5g of the substance was dissolved in 20 mL of water and the pH tested.
 They were then classified as acids, bases or neutral.
 Neutral: Both table salt and milk were neutral.
 Bases: Washing powder, the antacid tablet and toothpaste.
 Acids: Soil, vitamin C tablet and aspirin.
– JUSTIFY the method:
 Methyl orange is only red in strongly acidic solutions, so even a very weak base would have been
able to elicit a colour change.
 A wide range of substances was used to portray the wide range of possible bases. This showed
that bases are not only limited to metal hydroxides.
 A pH meter gave instantaneous accurate results.
 Equal amounts of each substance, dissolved in 20 mL of water made for a fair test of the
substance’s pH.
– LIMITATIONS of the method:
 The methyl orange test was not able to distinguish acidic and neutral substances, as both caused
no colour change from the red.
 PRACTICAL – Plan and perform a first-hand investigation to measure the pH of identical
concentrations of strong and weak acids:
– 20 mL of 0.1 M solutions of ethanoic, citric, hydrochloric and sulfuric acid were placed in four
separate beakers.
– A pH meter was used to measure the pH’s of the solutions.
– RESULTS:
 Sulfuric acid; pH = 0.7
 Hydrochloric acid; pH = 1.2
 Citric acid; pH = 2.9
 Ethanoic acid; pH = 3.3
– Sulfuric acid has the lowest pH of all the solutions as it is a diprotic strong acid, where was
hydrochloric acid is a monoprotic strong acid. Citric and ethanoic acid are weak acids.
 PRACTICAL – Choose equipment and perform a first-hand investigation to identify the pH of
a range of salt solutions:
– In this practical, the pH of a range of salt solutions was estimated by examining the parent acids and
bases.
– The actual pH was then measured using a pH meter.
– Salts:
 Sodium acetate - CH3COONa:
 Parent acid is CH3COOH (weak) and parent base is NaOH (strong).
 Predicted pH is slightly basic.
 True pH = 8.9
 Sodium nitrate - NaNO3:
 Parent acid is HNO3 (strong) and parent base is NaOH (strong)
 Predicted pH is neutral.
 True pH = 7
 Other salts:
 NaHCO3 - pH = 8
 MgCl2 - pH = 3
 PRACTICAL – Perform a first-hand investigation to determine the concentration of a
domestic acidic substance using computer-based technologies:
– 50 mL of household vinegar was placed in a small beaker.
– A pH probe was attached to the laboratory computer; the probe was rinsed with distilled water, and
then rinsed with left-over solution.
– The probe was then placed in the solution, and the pH measured.
– The probe was rinsed again, and pH was measured twice more.
– The average pH was calculated, and using this, the concentration of H+ ions found
– Given the fact that food-grade ethanoic acid only has about 0.4% ionisation, the concentration of
ethanoic acid was then calculated.
– RESULTS:
 The average pH measured was 2.5
 [H+] = 10-pH = 10-2.5 = 0.00316 mol/L
 But [H+] = 0.4% × c ; (where c = concentration of ethanoic acid)
 Hence c = 0.00316 ÷ 0.004 = 0.79
 Therefore vinegar is 0.79 M ethanoic acid.
 PRACTICAL – Identify data, plan, select equipment and perform a firsthand investigation to
prepare an ester using reflux:
– A functional group is a specific group of atoms within a molecule that is responsible for the
characteristic chemical properties of that molecule.
– Polarity occurs within a bond when one of the atoms is more electronegative than the other; the
bond has a slight charge.

– The ester prepared was ethyl ethanoate.


– Ethanol and ethanoic acid were used as the reactants.
 ethanol + ethanoic acid ethyl ethanoate + water
– In a round-bottom flask, 40 mL of ethanol, 30 mL of ethanoic acid and 10
drops of concentrated sulfuric acid were placed.
– Boiling chips were also dropped into the flask.
– The condenser attachment of the reflux apparatus was attached to the
flask, and secured onto a retort stand; water was passed into the condenser.
– The flask was placed in a water-bath in a large beaker.
– A Bunsen-burner was used to bring the water to a gentle boil, which
brought the reflux apparatus to a temperature of 100ºC; it was left to reflux
for 30 minutes.
– Heating was stopped and the entire apparatus was left to cool, with the water still flowing.
– Disassemble the apparatus, carefully holding on to the flask.
– The refluxed contents were poured into a separating funnel; the mixture was washed with 50 mL of
distilled water and shaken. The lower aqueous layer was drained off, and this washing was repeated
twice more.
– Finally 15 mL of saturated NaHCO3 solution and 35 mL of distilled water was added, the mixture
shaken, and the aqueous layer drained off.
– The final product is relatively pure ethyl ethanoate.
– JUSTIFY the method:
 See ABOVE for the justification for refluxing.
 See ABOVE for the justification of the addition of sulfuric acid.
 Boiling chips were added to facilitate a slow and gentle heating.
 A water bath was also used to allow for gentle heating
 The use of the separating funnel for extracting the ester was justified because all the reactants and
products except the ester are water soluble; ethanol, ethanoic acid, and of course water, are all
water soluble. Hence they are all immiscible with the ester.
 The ester also is less dense and floated on top, allowing the aqueous reactants to be drained off.
 Washing with distilled water was used to remove as much ethanol, ethanoic acid and sulfuric
acid from the ester as possible; multiple washings increased the purity of the ester.
 Finally, the sodium hydrogen carbonate was used to neutralise any remaining sulfuric acid in the
mixture.
Chemical monitoring and management
 PRACTICAL – Perform first-hand investigations to carry out a range of tests, including
flame tests, to identify the following ions:-
 Cations: Barium, calcium, lead, copper and iron:
 Anions: Phosphate, sulfate, carbonate and chloride:
– In this practical, students were given vials of unknown solutions; vials were labelled as ‘mixtures of
ions’ or ‘only one ion’.
– Using both precipitation and flame tests, the contents of the vials were determined.
– Precipitation Tests:
 Please see ABOVE for a very in-depth coverage of precipitation tests used to determine anions
and cations present in a sample.
– Flame Tests:
 Flame tests were only used to identify cations.
 Anions cannot be identified by flame tests.
 Out of the given list of cations, only barium, calcium, and copper produce a distinctive flame
colour when sprayed into a flame:
 Ba2+ gives a pale-green flame.
 Ca2+ gives a brick-red flame.
 Cu2+ gives a blue-green flame.
 PRACTICAL – Identify data, plan and select equipment and perform first-hand
investigations to measure the sulfate content of lawn fertiliser and explain the chemistry
involved:
– In this practical, the sulfate content of a lawn fertiliser was calculated.
– This is an example of gravimetric analysis; it is a quantitative analysis.
– METHOD:
 In a dry beaker, 5 grams (±0.01%) of fertilizer was electronically weighed.
 All the fertilizer was carefully transferred to a mortar and pestle, where it was ground into a fine
powder.
 The powder was transferred into a beaker; using a wash bottle with distilled water, all the residue
was washed into the beaker up to the 200 mL mark.
 50 mL of 0.1 M hydrochloric acid was added, and the mixture stirred until all of the fertilizer
dissolved.
 The mixture was then heated to its boiling point; the flame was turned off, and barium chloride
was added in drops, which formed a precipitate:
 BaCl2 (aq) + SO42- (aq) BaSO4 (s) + 2Cl- (aq)
 Barium chloride was added until no more precipitate formed.
 The mixture was digested (heated just below boiling point) for 30 minutes, stirring every now
and then, and then the precipitate was allowed to settle.
 The beaker and its contents was then cooled in an ice-bath.
 Using a sintered-glass crucible (which had its mass recorded), connected to a vacuum pump, the
mixture was filtered.
 The crucible was washed with water, and then ethanol, and then dried in an oven to a constant
mass.
 The difference between the crucible’s original weight and weight after drying (which was the
mass of BaSO4) was found to be 5.92 g.
– CALCULATING SULFATE CONTENT:
mass of BaSO4 formed = 5.92 g
percentage of sulfate in BaSO4 = molar mass sulfate / molar mass BaSO4
= (32.1 + 4×16.0) / (137.3 + 32.1 + 4×16.0)
= 41.2 %
mass of sulfate in BaSO4 = 5.92 × 41.2 %
= 2.44 g
percentage of sulfate in fertilizer = mass of SO4 / mass of fertilizer × 100
= 2.44 / 5.0 × 100
= 48.9 %
 Analyse information to evaluate the reliability of the results of the above investigation and to
propose solutions to problems encountered in the procedure:
– RELIABILITY:
 The use of a very precise electronic scale ensured accurate measurement.
 The fertilizer was ground into a powder to ensure that all of it dissolved; if some sulfate stayed in
solid form, the measurements would be inaccurate.
 The washing of the mortar and pestle into the beaker was to ensure all of the fertiliser was
transferred into the beaker.
 Hydrochloric acid was added to aid in the dissolving of the fertiliser.
 Slowly forming precipitates (using a dropper) at a high temperature ensures the formation of large
particles.
 Also, the mixture was digested for half an hour to allow the particles to grow.
 Large particle size meant fewer loses of BaSO4 through the filter.
 The mixture was cooled in ice-water to greatly reduce the solubility of BaSO4 to ensure that
virtually all of the sulfate precipitated out.
 A sintered-glass crucible was used instead a filter-paper as filter paper pores are too large; they
allow an unacceptable level of BaSO4 through.
 The washing with water and ethanol removed any traces of contaminants.
– SOLUTIONS to Problems Encountered:
 Human errors in measurement were the main source of inaccuracies; more careful measurement
of fertilizer mass, would ensure better results.
 There were small losses of barium sulfate due to its very small solubility. This was why the
beaker was cooled in ice-water before filtering (solubility decreases at low temperatures).
However, due to time constraints, cooling did not occur to a great extent.
 Longer digestion times would allow larger particles to form, and less loss of barium sulfate
through the filter would occur.
 There was possibly some barium sulfate left on the beaker walls before filtering; this would be
solved by washing out the beaker with distilled water.
 An incomplete drying of the sintered glass crucible (due to moist environment, as well as time
constraints) would be solved by a longer period of heating, as well as by using a dessicator.
 PRACTICAL – Perform first-hand investigations to use qualitative and quantitative tests to
analyse and compare the quality of water samples:
– In this practical, water samples were taken from the local Cook’s River and using a ‘StreamWatch’
kit the water quality tests were performed on-site.
– Water samples were taken from various parts of the river, and the results were compared to the same
tests performed on distilled water.
– Pollutants:
 This was a qualitative test performed on the water samples to detect pollution.
 Any sort of colouration of the water (any deviation from ‘clear’) indicated the presence of a form
of pollution; any ‘rainbow streaks’ meant hydrocarbons.
 The water was smelt to detect any odours (another sign of pollution).
 A sample bottle was filled half-way with sample water, and another bottle was filled with
distilled water; both were shaken at the same time for equal periods of time. If the bubbles
remained longer on the sample, this indicated the presence of detergents.
 The presence of heavy metal pollution was performed in the laboratory; 1 mL of sodium sulfide
was placed in 5 mL of sample water. Any precipitate indicated the presence of a heavy metal.
– Turbidity:
 This test was a relatively quantitative test, with turbidity measured in NTU.
 Firstly, distilled water was poured into the turbidity tube, and it was clear all the way to the top of
the tube. It was given a turbidity of <10 NTU.
 The sample water was collected in a bottle using a telescoping handle, and this water was poured
into the tube; it had a much higher turbidity, and clouded the view of the cross on the bottom of
the tube.
– Temperature:
 A thermometer (with a rubber handle) was placed directly into the water way to accurately
measure the temperature of the water; it was found to be within acceptable ranges.
– pH:
 pH of water samples was done using strips of pH paper.
 Firstly, the pH of distilled water was measured and found to be 7.
 The pH of the water sample was then measured and found to be 7.5.
– TDS:
 The total dissolved solids was measured using an electrical conductivity meter that measured in
μS/cm (mircosieverts per centimetre).
 The sample water had only slightly more ions that distilled water.
– DO/BOD:
 The levels of dissolved oxygen was easily measured using an oxygen sensing metre found in the
StreamWatch kit.
 Two sample bottles were filled; one was capped air-free and sealed tightly, and the DO level in
the other was measured immediately.
 The other sample had the levels of DO measured 5 days later, and the difference was the BOD.
– Hardness:
 For hardness, a titration method was used.
 To a 100 mL sample, 1 mL of buffer solution (pH 10) was added, and 2-3 drops of Eriochrome
Black T indicator was added.
 This red-violet solution was titrated against a solution of EDTA until a permanent blue colour
occurred.
 A lack of definite change in colour meant there were no magnesium ions.