Volumetric Analysis Iodometric Titration (thiosulfate S2O32- & I2)

● Pre-calc from expected titre reading
- Usually to find % purity (take note of total V)
Standard Solution
1. Using the electronic mass balance, measure the mass of
a clean, dry weighing bottle and tare
2. Weigh out accurately __ g of X
3. Transfer X into a small clean beaker
4. Rinse the weighing bottle and pour washings into the
beaker, do this at least twice
5. Stir gently to dissolve as much of X as possible, pour
mixture into clean 250cm3 graduated flask using a funnel
and a glass rod to guide the flow
6. Rinse the beaker a few times and add washings into the
graduated flask
7. Remove the funnel and make up to mark with distilled
water using a dropper for the last few drops
8. Mix solution thoroughly by shaking and inverting the flask
Dilution
● Using a burette, add __cm3 of stock solution into
250cm3 graduated flask
● Add 50cm3 of excess KI into conical flask
● Gradually add Na2S2O3 from the burette to the
conical flask, swirling continuously, until a pale
yellow colour is observed
● Add 10 drops of starch solution
● Continue titrating until solution changed from dark
blue to colourless
Back Titration
- Add A (insoluble solid) to excess B (acid)
- Titrate with C (alkali) to find remaining B
Gravimetric Analysis
Heating
1. Using an electronic mass balance, measure and record
the mass of a dry crucible/boiling tube
2. Add between__g to __g of solid and re-weigh
3. Record weighings in table
Mass of crucible/boiling tube and solid /g
Mass of empty crucible/boiling tube /g

General Titration Mass of solid /g

1. Pipette 25.0cm3 of FA1 into 250cm3 conical flask 4. Heat strongly to decompose the solid
2. Add 1 to 3 drops of indicator to the conical flask 5. Place the crucible on heat proof mat to cool
3. Fill the burette with FA2 6. Reweigh the crucible and contents, recording results in
4. Titrate the mixture in the conical flask with FA2 from the the table. Repeat steps 4 to 6 until mass of the crucible and
burette, swirling continuously to ensure mixing residue remains constant (within 0.05g)
5. The end point is indicated by a sharp/permanent colour
change from __ to __ (follow indicator) Mass of crucible/boiling tube and residue after heating /g
6. Repeat steps 1 to 5 until 2 consistent results are achieved,
Mass of empty crucible/boiling tube /g
both readings within ±0.10cm3
Mass of residue after heating /g
Indicators
Indicator Lower Upper End-point Precipitation
1. Weigh accurately about __g of solid in a clean and dry
Methyl Orange 2.8 Red 4.3 Yellow Orange
weighing bottle (do not use max amt)
Screened Methyl 2.8 Red 4.2 Green Grey 2. Transfer the contents into a 500cm3 beaker and reweigh
Orange the weighing bottle and residue
Mass of bottle and solid /g
Thymolphthalein 9.4 10.6 Blue Pale Blue
Colourless
Mass of bottle and residue /g
Phenolphthalein 9.4 10.6 Pink Pale Pink
Colourless Mass of solid added /g
3. Completely dissolve the solid in suitable solvent
Thymol Blue 1.2 Red 2.8 Yellow Orange 4. Using a 50cm3 measuring cylinder, add 10cm3 of FA3
5. Continue adding dropwise, stirring until no more ppt forms
Thymol Blue 8.0 Yellow 9.6 Violet Grey
6. Weigh a dry filter paper and line a funnel
7. Filter the mixture
Double Indicator Titration 8. Use a dropper to add FA3 to the filtrate. If no more ppt
● Add indicator 1 → 1st end-point volume A forms, discard filtrate. If more ppt forms, repeat steps 4-7.
● Add indicator 2 → 2nd end-point volume B 9. Wash the residue with cold deionised water
- Vol of Y reacted for 2nd reaction = B-A 10. Dry the ppt using an infra-red lamp/oven
11. Weigh the dried ppt with the filter paper
Redox Titration 12.. Repeat steps 10-11 until constant mass obtained
● Using a 10cm3 measuring cylinder, add 10cm3 of
Mass of filter paper and residue after drying /g
H2SO4 into conical flask (excess acid)
● Titrate with KMnO4 until one drop gives the first Mass of filter paper /g
permanent pale pink
Mass of residue after drying /g
Energetics
Mixing
- Different proportions of substances
- 2 varying solutions = graph is X
- V not varying = graph is horizontal after Tmax
○ varying mass of solid dissolved BUT
constant V of reactant
○ varying V reactant BUT + H2O to keep
total V constant
Mixing 2 Solutions
1. Using a 50cm3 measuring cylinder, measure __cm3 of
FA4 into a polystyrene cup supported in a 250cm3 beaker
2. Using a 0.2॰C thermometer, place in the polystyrene cup
and cover with lid, measure and record initial Ta
3. Using another 50cm3 measuring cylinder, measure __cm3
of FA5. Using the same but clean 0.2॰C thermometer,
measure and record the initial Tb
4. Calculate ave initial T using <T> = (Ta+Tb)/2
5. Add FA5 quickly into the polystyrene cup and cover with
the lid. Stir the mixture vigorously with thermometer
6. Record the highest T reached and calculate ∆T
7. Wash and dry polystyrene cup
8. Repeat steps 1 to 7 for the other sets of volumes
Mixing Solid in Solution
● Pre-calc to find min mass of solid
- 2.5g of solid + 40.00cm3 of FA4 = ∆5.0॰C
- 5.0g of solid + 40.00cm3 of FA4 = ∆10.0॰C
● Using an electronic mass balance, weigh accurately
about __g of solid in a clean and dry weighing bottle
● Tip the contents…
● Reweigh the weighing bottle with residue and
calculate the mass of solid reacted
Thermometric Titration
● Pre-calc to determine the range of V to include
- __cm3 (fixed) of FA6 w known conc
- Determine Vn FA7 for neutralisation
- 3 V below Vn, 3 V above Vn (Tmax @ Vn)
1. Using a burette, measure __cm3 (fixed) of FA6 into a
styrofoam cup supported in a 250cm3 beaker
2. Using a 0.2॰C thermometer, place in the styrofoam cup,
measure and record initial T
3. From second burette, top up with FA7
4. Gradually add FA7 at a constant rate to FA6, using the
thermometer to stir gently
5. Record T when 5.00cm3 of FA7 is added
6. Progressively add FA7 at a constant rate and record T at
every 5.00cm3 of FA7 added until 30.00cm3 has been
added
7. Calculate the ∆T
8. Plot graph of ∆T vs V(FA7). Draw 2 straight, best fit lines
9. Equivalence point has been passed once T decreasing
10. ∆Tmax and equivalence point V can be determined from
intersection of the 2 lines
Combustion of liquid fuels
1. Pour fuel into a spirit lamp until it is about ⅔ full. Using an
electronic mass balance, weigh and record the mass of fuel
and spirit lamp
2. Using a 100cm3 measuring cylinder, measure 100cm3 of
water and transfer into a copper can
3. Using a 0.2॰C thermometer, measure and record the initial
T of the water, Tw, in the copper can
4. Place copper can on tripod stand with wire gauze and the
spirit lamp just below the copper can
5. Light the wick. Stir the water vigorously with the
thermometer and monitor its temperature
6. Extinguish the flame when the water temp has risen by
5॰C. Continue to observe temp rise and record Tmax
7. Reweigh and record mass of the spirit lamp with remaining
fuel immediately. Calculate mass of fuel combusted
8. Repeat steps 1-7 using the other fuels
Temperature Correction
● Pre-calc mass of excess solid (or V solution)
- __cm3 (fixed) of FA8 w known conc
- Determine M of solid for reaction
- Use whole number > M
1. Using an electronic mass balance, weigh accurately about
__g of solid in a clean and dry weighing bottle
2. Using a burette, measure __cm3 FA8 into a styrofoam cup
supported in a 250cm3 beaker
3. Using a 0.2॰C thermometer, place in the styrofoam cup
and cover with a lid, measure and record initial T at t=0 min
4. Start the stopwatch and at regular time intervals of 0.5
minute, measure and record T for 2.5 minutes
5. At 3 min, tip the contents of the weighing bottle into the
styrofoam cup and cover with a lid. Stir the mixture
vigorously with the thermometer
6. Measure and record T of the mixture from 3.5 min for
every 0.5 min for the next 10 minutes
7. Reweigh and record the mass of weighing bottle with
residual solid and calculate the mass of solid reacted
8. Plot a graph of T against t and extrapolate to get Tmax at
t=3min. Calculate ∆T
Kinetics
Non-continuous Precipitation (acidification S2O32-, form S)
Continuous Titration
V(Na2S2O3) V(HCl) / V(H2O) Time 1/
● Using appropriate apparatus, add required volume /cm3 cm3 /cm3 taken/s time /s-
of solution, add NY1 followed by catalyst, followed 1
by NY2 (other reactant)
- Note dilution factor to ensure reasonable end point 1 40 40 0
of titration & sufficient stock solution for titration
2 20 40 20
- Calc new conc using total vol of solution in conical
flask after all the addition (can add water to dilute) 3 20 20 40
…
3. Using a 100cm3 measuring cylinder, add __cm3 of NY2 1. Using a 50cm3 measuring cylinder, add 40cm3 of
into the 250cm3 conical flask. Start the stopwatch and swirl Na2S2O3 into a 250cm3 conical flask on a paper with an X
the mixture thoroughly to mix its contents 2. Using a 50cm3 measuring cylinder, add 40cm3 of HCl to
4. Using another 20cm3 measuring cylinder, measure 20cm3 the conical flask and start the stopwatch
of quenching agent 3. Measure and record the time taken such that the X cannot
5. When stopwatch shows t=3min, using a 10cm3 pipette, be seen from the top of the conical flask
transfer 10.00cm3 aliquot mixture of the reaction mixture into 4. Repeat steps 1 to 3 with varying V from the table keeping
a 100cm3 conical flask total V the same
6. Add in 20cm3 of quenching agent and record time of
addition, swirl the mixture Non-continuous Iodine Clock (small & limiting Na2S2O3)
7. Immediately titrate mixture with NY3 (redox/iodometric) ● Pre-calc V for all
8. Wash out the 100cm3 conical flask with water - Plan for the formation of I2 (excess KI added to e.g.
9. Repeat steps 4 to 8, 5 more times at 3 min intervals when H2O2 (NY5) for I2 to remain soluble)
stopwatch shows 6, 9 ,12, 15, 18 - Plan for 1/10 of I2 to react with NaS2O3 (exact V)
10. Plot graph of V(NY3) against time (V(NY3) ∝ to [NY1]) 1. Using a 50cm3 measuring cylinder, add __cm3 (excess)
of KI into a 250cm3 conical flask
Continuous Change in Gas 2. Using another 50cm3 measuring cylinder, add __cm3 of
● Pre-calc m limiting solid and V excess NY4 from (acid) followed by 10 drops of starch solution
fixed V of gas collected 3. From a burette, run __cm3 (exact) of Na2S2O3 into the
1. Using a 50cm3 measuring cylinder, add __cm3 of NY4 conical flask
into stoppered test tube and connect the 100cm3 gas 4. Using another 50cm3 measuring cylinder, add __cm3 of
syringe via its delivery tube to its side-arm NY5 into the conical flask and start the stopwatch
2. Using an electronic mass balance, weigh accurately about 5. Swirl the mixture and place the conical flask on a white tile
__g of solid into a weighing bottle then tie a cotton thread 6. Measure and record the time taken for the solution to turn
around the weighing bottle and lower into stoppered test- dark blue
tube till it is just above liquid level and tighten the stopper 7. Repeat steps 1 to 6 for the volumes in the table below
3. Tilt the stoppered test tube so that solid will mix into NY4 V(KI) V(acid) V(NY5) V(H2O) V(Na2 t/ 1/
and start the stopwatch /cm3 /cm3 /cm3 /cm3 S2O3) s t /s-
4. At 1 min intervals, record V gas collected in syringe /cm3 1
5. Take at least 6 readings and plot graph of V gas against
1 20 20 20 0 4.00
time, extrapolate to 100cm3 of gas for complete reaction
2 20 20 10 10 4.00
Continuous Spectrometry
1. Spectrometer calibrated using diff known conc of I2 3 20 20 20 10 4.00
solution before experiment
● Using appropriate apparatus, add required volume 4 10 20 20 10 4.00
of solutions into cuvette placed in spectrometer and
start the stopwatch
…
4. Measure and record absorption level in 1 min time
intervals
5. Use the calibration curve to convert absorbance into [I2]
and plot graph of [I2] against time
Chem Equilibria
Determining Equilibrium Concentration
1. Form equilibrium mixture (method given in qn)
● Pre-calc from expected titre reading
● E.g. leave separating funnel to stand for one hour at
constant room temperature, drain aqueous layer to
use for titration
● E.g. form standard solution and leave mixtures in
fume cupboard for 1 week
2. Titrate with known concentration of acid/alkali
3. Calculations
● Initial conc from initial amt of each reactant added
● Equilibrium conc of reactant from titre value
● ICE table to find equilibrium conc of other all other
components at equilibrium
Determining Solubility/Conc for ppt/ Ksp
(max amt of substance that can dissolve in a solvent as a
given temp to form a saturated solution)
- Dissolve solid until some left undissolved
- Analyse residue (heat, cool, weigh)
- Analyse filtrate (evap to dryness/ titration)
Saturated Solution
1. Using a __cm3 burette/pipette, add__cm3 of water into a
clean, dry 250cm3 beaker
(OR) using an electronic mass balance, weigh 100g of water
2. Place the beaker in a thermostated water bath controlled
at __ ॰C
3. Using an electronic mass balance, weigh accurately about
__g of sparingly soluble salt in a clean and dry weighing
bottle
4. Add the salt into the beaker of water
5. Stir the solution with a glass rod continuously until no
more salt dissolves
6. Allow the mixture to stand for 30 min to establish
equilibrium
7. Reweigh and record the mass of weighing bottle with
residual salt and calculate the mass of salt added
Collecting Residue
8. Using an electronic mass balance, measure and record
the mass of piece of dry filter paper
9. Filter the mixture using dry filter paper and dry filter funnel
10. Dry the filter paper and residue under IR lamp or in oven
11. After 10 min, allow to cool down in a desiccator
12. Using an electronic mass balance, measure and record
the mass of the residue with the filter paper
13. Repeat the process of heating, cooling and weighing until
a constant mass of ±0.05g is obtained
Mass weighing bottle + salt /g
Mass weighing bottle + residue /g
Mass salt added /g A
Mass filter paper + residue after drying /g
Mass filter paper /g
Mass of salt residue after drying /g B
Mass of salt dissolved /g A-B
- Calculation: mass of salt dissolved/V(solvent) =
solubility in gdm-3
Collecting Filtrate
8. Using an electronic mass balance, measure and record
the mass of a dry evaporating dish/crucible
9. Filter the mixture using a dry filter paper and dry filter
funnel and collect the filtrate in an evaporating dish/crucible
or dry 250cm3 conical flask
10. A. Evaporate to dryness (GA)
B. Titration (VA)
- Calculation:
A. mass of salt dissolved/V(solvent) =
solubility in gdm-3
B. n(salt) dissolved/V(pipette) =
solubility in moldm-3
Electrochem
Electrochemical/Galvanic/Voltaic Cell
- Use eqns e.g. ΔG = -nFEcell, ΔG = ΔH - TΔS
- Form linear eqn and plot graph
● Draw diagram
● Standard solutions (given in question)
● Appropriate quantities (dilute such that conc of each
solution is the same e.g. 0.100moldm-3)
● Thermostated water bath (if varying temp)
● Record Ecell using Voltmeter
- Use gradient/vertical-int for calc
Electrolytic Cell
- Use eqns e.g. Q=n(e-)F, Q=It
- Form linear eqn and plot graph
- E.g. mass deposited vs time/current
● Draw diagram
1. Using electronic mass balance, measure and record the
initial mass of the clean and dry metal object
2. Connect metal object (cathode) to be plated to -ve end
and pure metal (anode) to +ve end of battery
3. Ensure voltage/current is set to zero before turning on the
power source
4. Turn on the power source and start stopwatch
5. At t=1200s, turn off the power source
6. Remove plated object and wash it with distilled water to
remove traces of electrolyte
7. Rinse with propanone to dissolve the water
8. Allow propanone to evaporate from surface
9. Using an electronic mass balance, measure and record
final mass of dry cathode
10. Calculate mass deposited
11. Repeat for different pieces of metal for different
durations/different charge by adjusting rheostat
12. Plot graph of mass deposited against time/charge. Draw
line of best fit through the origin
13. Calculate gradient (use for determination of unknown)
Organic
Synthesis
● Draw reflux diagram
● Add appropriate quantities as stated in question
● Note duration of reflux, added to X for precipitation,
recrystallisation from X
A. Preparation of Crude Product
…
4. Swirl the mixture in the flask to ensure thorough mixing
5. Add boiling chips
6. Attach reflux condenser (+ other apparatus) vertically
7. Allow mixture to reflux in hot water bath for (duration)
8. (follow any other instructions) Allow mixture to cool and
dismantle apparatus
9. Slowly add into X, stirring well to precipitate solid
B. Purification (recrystalisation)
11. Add just enough X to dissolve most of the impure product
12. Using a dry funnel, dry filter paper and dry conical flask,
filter the solution
13. Filter again under reduced pressure, when a reasonable
quantity of crystals has formed, using a Buchner funnel and
flask. Use cold distilled water to wash all contents of the flask
into the funnel
14. Wash the residue with little cold distilled water
15. Place residue under IR lamp for drying
C. Confirmation of Yield/Purity
16. Using an electronic mass balance, measure and record
the mass of dry solid
17. Check purity by doing a melting point test