Chemistry Practical

Chemistry Practical- Exercise 1

June 2006:- Reactions of metal ions- observations

June 2005:- Reactions of organic compounds- observations
June 2004:- Titration of a solution of iron (II) sulphate.
June 2003:- Titration of a solution of potassium iodate(V).

Likely to be a titration again.

Chemistry Practical- Exercise 2

Concordant=within 0.1 of each other.

Equipment error % = (error/value) * 100

Generally one result that is anomalous. This must be identified in the evaluation
and a reason given if possible.

% difference in K = (K1 – K2 / <K>) * 100

June 2006:- Analysis of a hydrogen peroxide solution

 Deduce an equation
 Identify concordant titration results/give average
 Calculating number of mols
 Work out equipment error.
 Comment on consistency
 Calculate % difference in values and comment on its value.
 Comment on improvements:-
o Hydrogen peroxide decomposes and therefore the solution is less
concentrated than it should be.
o Burette was read incorrectly/is hard to read
o Hydrogen peroxide solution diluted too much- made beyond the mark.

June 2005:- Determining equilibrium constant

 Deduce equilibrium constant equation

 Work out number of mols remaining in the equilibrium mixture and therefore
the equilibrium constant.
 Equipment error
 Calculate % difference in expected Kc and measured Kc.
 Comment that % equipment error < % difference.
 Comment on improvements:-
o Decrease concentration of sodium hydroxide added so that more is
added. This reduces burette error.
o Maintain a constant temperature using an ice bath- Kc is temperature
dependant.

June 2004:- measuring rate of reaction.

 Plot log VOL against log TIME .Identify that one point is anomalous and ignore
it. Draw a line of best fit and work out gradient.

Matthew Swallow Pg 1 of 10 Welbeck Defence College

 Work out apparatus error.
 Comment on consistency of results- generally good, one anomalous.
 Comment on improvements:-
o Spectroscopy to identify the colour change so that it is identified
immediately rather than relying on humans to spot it.
o Water bath to keep temperature constant as increasing temp increases
the rate of reaction.
o Smaller concentrations meaning that the reaction took longer- this would
reduce the inaccuracy in the stop watch.
o (OR) Larger volumes so that inaccuracies in measuring the liquids is
reduced.
o (OR) Use more accurate instruments to measure- e.g. pipette.

June 2003:- Titration

 Write an equation for redox titration

 Calculate mean titre from concordant values
 Work out mols and % iron in the iron tablet.
 Calculate equipment error.
 Comment on consistency- first one=rough titration otherwise good etc.
 Work out % difference and compare to apparatus error
 Explain that it is necessary to filter of unwanted zinc- zinc will act to reduce
dichromate ions and will reduce Iron (III) ions once they have reacted.
Otherwise an inaccurate titre will occur.
 Explain how errors may have occurred:-
o Small particles of zinc may get through
o Filter paper may absorb some solution
o Fe (II) may oxidise to Fe (III) in air.

June 2002:- Determining dissociation constant of a weak acid

 Draw a pH curve and use it to find out pKa therefore Ka

 Identify this unknown acid by comparing Ka values
 Work out apparatus error.
 Calculate difference from expected value and comment on the size of this.
 Suggest improvements:-
o % error in pH meter is very high- therefore use a 2dp pH meter
o Increase the number of readings by doing smaller additions by the end
point.
o Water bath to keep at a constant temperature as Ka is temperature
dependant.
o Calibrate pH meter before use and wash with distilled water before
using.
o Data logger to record data and plot graph.
o Repeat experiment.

I predict that the analysis is likely to be something that involves drawing a graph.
This could easily be determining the Ka value.

Matthew Swallow Pg 2 of 10 Welbeck Defence College

Chemistry Practical- Exercise 3

June 2006:- Determining order of reaction.

June 2005:- Redox titration
June 2004:- Determining Ka of an acid.
June 2003:- Organic Purification.
June 2002:- Organic Preparation (Aspirin).

Other possible plans:-

 Colorimeter
 Measuring cell EMF

General Tips:-

How fast do you need to add stuff?

What conditions are you using?
What accuracy of equipment- e.g. 2dp balance or 3dp balance?

Colour changes:-

Methyl orange Yellow to red when adding acid.

Phenylphaline Pink to colourless when adding
acid.
Manganate (not an Solution remains light pink.
indicator)

Matthew Swallow Pg 3 of 10 Welbeck Defence College

June 2006:- Finding the order of a chemical reaction

Appreciation of scale


100cm3 gas syringes in college- thus collect 100cm3

Calculate moles required for volume, and correct dilution factors.

Method

 Equipment:- MUST BE IN DIAGRAM THIS TIME

o Stoppered boiling tube with gas outlet
o Gas syringe for collecting gas
o Pipettes for measuring volumes of solution
o Water bath to control temp of solution
 Measure out 40cm3 of ion using a pipette- keeping mixture at 20C
 Measure time taken to collect 25cm3 of gas- work out rate
 Dilute solution by half to give two concentrations and repeat with this
concentration- work out rate. Concentration of ion must remain constant.
 Use the equation

[B]^n is constant since concentration of ion did not change. Thus Rate=k[A]^n

Safety:-

 phenol toxic/corrosive wash spillages with cold water/ wear gloves

 eye protection/pipette filler

Matthew Swallow Pg 4 of 10 Welbeck Defence College

June 2005- Titration

Appreciation of scale:-

 Construction of appropriate redox equation.

 Ration 5:2 and appreciation we want approx same vol of both reactants-
therefore calculate correct dilution factor.
 Description of how you would work out concentration of hydrogen peroxide
from the titration.

Method:-

 Rinse a burette with a little manganate. Fill the burette ensuring that the jet
space is filled and funnel is removed. Record the initial burette reading from
the bottom of the meniscus. Illuminating the burette may help with this
reading.
 Rinse the pipette with hydrogen peroxide and the transfer 25cm3 of
hydrogen peroxide into a conical flask. Let the pipette empty under gravity
and touch the end to the water once draining has finished to remove surface
tension.
 Add a couple of drops of sulphuric acid.
 Place the conical flask on a white tile under the burette.
 Add manganate from the burette whilst swirling the flask. Add manganate
drop wise towards the end point- continue until permanent pink colour
remains.
 Note the final burette reading in the same manner described above and
record.
 Repeat until two concordant results are achieved.

Safety:-

 Hydrogen peroxide irritant linked to eye protection/ pipette filler

 Sulphuric acid corrosive linked to gloves/ flood affected area
 Manganate (VII) oxidising linked to avoid flammable materials

Matthew Swallow Pg 5 of 10 Welbeck Defence College

June 2004- Determining Ka

Appreciation of scale:-

1:1 reaction therefore the same concentration of acid/alkali is wanted. A standard

solution of around 250cm3 is wanted. Do appropriate calculations.

Method:-

 Equipment:-
o pH meter
o Distilled water
o Burette
o Pipette
o HA and NaOH solutions.
o Beaker
 Standardize/calibrate pH meter and rinse with distilled water.
 Rinse burette with a little NaOH. Fill up the burette ensuring that the jet
space is filled and the funnel is removed.
 Rinse a pipette with HA and then use it to transfer 25cm3 of the standard
solution to a beaker. Make sure you touch the surface of the liquid with the
pipettes tip to remove surface tension- and empty under gravity.
 Record the pH of HA
 Add 2cm3 of HA from the burette. Stir/swirl the solution and then record the
new pH value. Continue until NaOH is in excess (i.e. pH of 12-14 is
reached.) Using a data logger would make this easier.
 Add the HA in smaller increments near the end point.
 Repeat this until concordant results are gained for each increment of NaOH
added. Take an average of the pH of the solution for each value NaOH added
and then plot a graph of pH (y-axis) against volume of NaOH added (x-axis.)
 Use this graph to work out pKa. i.e. half equivalence point etc. From this
work out pH.

Equivalence point is when mols acid = mols alkali.

Safety:-

 Use pipette filler when filling the pipette.

 Alkali and acid may be corrosive/irritant- protective clothing/gloves/flood
skin with water if contact made with skin. Eye protection.
 Clear up spills immediately.
 Glass wear is breakable- be careful when using it.

Matthew Swallow Pg 6 of 10 Welbeck Defence College

June 2003- Organic Purification

Appreciation of scale:-

 1:1 reaction/calculation of scale.

Method:-

 Equipment:-
o Beaker for original solution and Beaker for pure crystals
o Water bath and Ice bath
o Funnel and Filter Paper
o Buchner Funnel/Filter Apparatus + suction system
o Reflux apparatus
 Add the minimum amount of hot methylbenzene
 Filter the solution hot using filter paper and funnel.
 Cool the hot solution by placing in an ice bath for 15minutes.
 Filter the crystals from the solution using the Buchner apparatus.
 Dry under suction and then with filter paper.
 Weigh the dried sample.

Safety:-

 Methyl benzene is toxic and flammable

 Therefore organic compound can also be toxic
 Avoid naked flames
 Use a fume cupboard
 Use skin protection or flood areas with water straight away.
 Mop up any spills
 Wear safety goggles and protective clothing

Matthew Swallow Pg 7 of 10 Welbeck Defence College

June 2002- Organic Preparation/Purification (Aspirin)

Appreciation of scale:-

 1:1 reaction/calculation of yield.

Method:-

 Equipment:-
o 100 cm3 conical flask
o 2dp scales
o Pipette + filler
o Water bath
o Funnel and Filter Paper
o Buchner Funnel/Filter Apparatus + suction system
o Reflux apparatus
o Beaker for pure crystals.
 Weigh out, using weighing by difference, a sensible mass of 2-
hydroxybenzoic acid using a 2dp scale. Place this in a 100cm3 conical flask.
 Measure out 7.0cm3 of redistilled ethanoic anhydride using a pipette and
filler. Empty this into the 100cm3 conical flask allowing the pipette to empty
by gravity and touching the surface with the end of the pipette to remove
surface tension. Place in a water bath as reaction can initially be violent.
 Add 2-3 drops of concentrated sulphuric acid and swirl contents of the flask
to ensure thorough mixing.
 Transfer the conical flask to a water bath set at 50°C. Heat under reflux for
15minutes.
 Add a few drops of water to the hot mixture with care.
 Allow the mixture to cool and then add 40cm3 of cold water to precipitate
the aspirin.
 Add minimum amount of hot water to dissolve the aspirin.
 Filter the solution whilst it is still hot using a piece of filter paper and funnel.
 Place the solution in an ice bath for 15 minutes whilst allowing crystals to
form.
 Using a Buchner funnel filter the crystals and allow them to dry under
suction. Dry the crystals using filter paper and record the mass achieved.
 Check purity by doing a melting point test.

If mass of yield is greater than original mass then something has gone wrong!
Normally the crystals are not dry.

Safety:-

 Ethanoic acid/phosphoric acid corrosive therefore organic product is also

likely to be corrosive.
 Wear gloves, safety goggles, protective clothing and flood any areas that
contact material with water. Clean up and spills.
 Use a fume cupboard.
 Use pipette filler.
 Sulphuric acid reacts violently with water- therefore keep away from water.
 Ethanoic anhydride is flammable- therefore do not use naked flames.

Matthew Swallow Pg 8 of 10 Welbeck Defence College

Measuring the EMF of electrochemical cells:-

Circuit consists of two halves. In each half the metal ions are in contact with the
metallic element. Each metal is connected to a crocodile clip and this clamped in
place by passing the electron through a clamped cork. The salt bridge is a
conducting piece of filter paper soaked in a solution of potassium nitrate or
potassium chloride. However chloride precipitates may interfere with the
experiment.

Determining equilibrium constant:-

Allow a mixture to reach equilibrium. React the remaining reactants away with an
exact amount of another chemical- and use this exact amount to calculate number
of mols of each chemical in the equilibrium mixture.

Measuring an unknown concentration of transition metal using colorimetry:-

Solutions containing transition metal complexes appear coloured because they

absorb visible light of specific frequencies. The amount of light absorbed depends
on the concentration of the complex in solution. To determine the concentration of
an unknown solution you must measure the absorbance of a known value for
several known solution and plot an absorbance vs concentration calibration curve.

Use a suitable reference cell which must be the complexes complementary colour-
and use a reference cell containing distilled water each time. Cuvettes must be kept
as clean as possible.

Calculating % of iron in an iron tablet:-

 Record mass of two iron tablets using a 2dp scale

 Using pestle and mortar grind the tablets- make sure none leaves mortar
 Once in fine powder add 20cm3 dilute sulphuric acid and stir the tablet into
the acid with the pestle; being careful not to lose any.
 Pour solution into a volumetric flask using a funnel. Add more sulphuric acid
to mortar to remove remaining iron. Make the volumetric flask up to 100cm3
with sulphuric acid and shake to ensure good mixing.
 Rinse a pipette with the solution
 Extract 10cm3 using a pipette/filler and place in a conical flask.
 Wash out burette with potassium manganate of known concentration- fill up
burette taking care to remove the funnel. Make sure the jet space is filled.
Record the starting volume.
 Keep titrating, drop wise towards the end point, until a pale pink coloured
solution exists permanently in the conical flask. Record the final burette
volume.
 Repeat until two concordant results are achieved. Record the average
volume of the good titres. This can be used to work out % Iron in the
tablets.

NB:- most likely to be something that involves number manipulation (calculation of

concentrations, mols etc) at the beginning. This could be something to do with %
iron as this hasn’t been done before.

Matthew Swallow Pg 9 of 10 Welbeck Defence College

Matthew Swallow Pg 10 of 10 Welbeck Defence College