Flame Test

- Use a clean nichrome/platinum wire

- Dip in concentrated hydrochloric acid first and then dip the wire in salt to be tested
- Hold over a non-luminous Bunsen flame and observe the colour of flame

Titration (5 or 6 marks)
- Pipette 25 cm3 / 10 cm3 / Take the whole solution of [X] into a conical flask.
- Fill the burette with [Y] and take the initial burette reading.
- Add [Y] drop by drop (at the end point) into the conical flask.
- When colour changes [state the colour change], end point is reached and final burette
reading is read. Titre value is calculated from the two burette readings.

Along with any 2 or 3 of the following:

- Use a white tile underneath the conical flask to observe the colour change clearly.
- When burette content is being dropped, always keep swirling the conical flask.
- Always take burtette reading from eye level and bottom of the meniscus.
- Rinse burette with [Y] first.
- Rinse pipette with distilled water and then [X] first.
- Addition of (dilute) sulfuric acid [if context permits]

Recrystallization
- Dissolve crystals in a minimum volume of hot/ boiling (named) solvent (solvent
depends on context).
- Filter the hot solution using hot fluted filter paper and a pre-heated stemless filter
funnel to remove insoluble impurities.
- Wash with cold solvent/ice bath to form crystals.
- Filter using Buchner funnel and vacuum filtration to remove soluble impurities.
- Crystals formed are then dried between filter paper / left in a desiccator.

***Why minimum volume is used → to minimise the amount of [X] left in solution when it
crystallises / to give saturated solution

**why is the funnel preheated

To prevent the premature crystallization of the (solute) upon contact with funnel

*why is a cold solvent used before filtration under reduced pressure

- To form a saturated solution→ otherwise hot solvent would dissolve the crystals

— compiled by Progga Paromita

Describe how you would ignite the sample of solid P to show that it burned with a smoky
flame. [3 marks]

- the use of a crucible lid

- on a tripod and gauze / pipe-clay triangle and
ignition from above
- use of a Bunsen burner

Thiele Tube - Method used for melting point of a solid [5 marks]:

- Diagram adjacent scores first 4 marks.

- 5th Mark - Note the temperature when the solid just
changes into a liquid.

Thiele Tube - Method used for boiling temperature of liquid [5 marks]:

Step 1: Place a capillary tube,

sealed at one end and with the open
end facing down into 0.5 cm3 of
compound A into the micro test
tube. Attach the micro test tube to a
thermometer with a rubber band

Step 2: Clamp the micro test tube

and the thermometer in the mineral
oil, making sure neither test tube nor
the thermometer bulb is in contact

— compiled by Progga Paromita

with the glass walls of the Thiele tube

Step 3: Move a small Bunsen flame back and forth along the lower part of the side- arm of the
Thiele tube, for even heat distribution. An initial stream of bubbles will come from the open end
of the capillary tube.

Step 4: Continue heating until a rapid and continuous stream of bubbles comes from the
capillary tube. Stop heating and record the temperature as soon as compound A is drawn up
into the capillary tube.

Vacuum filtration
- Removes soluble impurities
- So that the filtered solid is dry
- This type of filtration is faster and dries the solid

How pure crystals are obtained from the filtrate

- Evaporate the solution to the crystallisation point
- Cover solution and cool→ dry the crystals between filter paper

Dilution technique
- Transfer solution to a volumetric flask.
- Wash the previous container with distilled water and transfer washings as well.
- Makeup to 250 cm3 with distilled water and then stopper the flask and shake.

Higher value for mass of crystal → the crystals was not dry

Outlet in steam distillation → prevents the buildup of pressure by allowing vapours to

escape

Process after steam distillation is done and the aqueous and organic products are in the
separation funnel
- The separating funnel is used to remove the organic layer
- The organic layer is dried
- Using anhydrous calcium chloride

Toxic and flammable → vent goes into the fume cupboard

Why flammability might not be a problem

- The sample was used in small amounts
- And/or the sample had a high boiling temperature

— compiled by Progga Paromita

Why a water bath is used when reacting organic acid with metal
- At high temperatures, the metal might ignite

CO2 identification
- Pass gas through lime water
- Turns cloudy

Why infrared spectra cannot be used to distinguish between carboxylic acid isomers
- The two isomers will have the same functional group
- But different absorption groups in the fingerprint region

Advantage of using continuous monitoring rather than a sampling method

- The reaction does not need to be quenched

Phenol is extremely caustic (corrosive). Safety precautions used here

- Eye protection
- Laboratory coat
- Wear gloves to prevent contact with skin

Using a filter paper without a stem → so that the X cannot crystallize upon contact with the
stem of the funnel

In rate order determining reaction, why are some reactants given in large excess?
- So that the concentration of those reactants (eg. propanone and HCl) will be relatively
constant
- So that only the (another reactant, eg. iodine) changes during the reaction

When should the starch be added in the iodine-thiosulfate reaction? And why?
- Add the indicator when the reaction mixture is pale yellow
- To prevent the formation of an insoluble starch-iodine complex if it is added at the
beginning.

*smallest titre → greatest %uncertainty

*doubling the concentration of the acid, double the rate of the reaction
*so the reaction is first order

Explain, in terms of change in state, how the process of heating under reflux works and give two
reasons why it is often necessary to heat chemicals under reflux
- As the liquid vaporizes, the vapour is cooled and condensed back to liquid
- Prevents the escape of volatile products/ reactants
- Allows for a complete reaction

Heat - increase the rate of reaction

— compiled by Progga Paromita

Refluxing - prevents the loss of volatile reactants or products

*water is used to remove excess ethanoyl chloride

Identifying pure crystals

- There is a sharp melting temperature / very small range of melting temperature
- The value/range of the melting temperature is close to / consistent with the literature
value

Explain, in terms if standard electrode potentials, why manganate (VI) ions can be prepared in a
concentrated alkaline solution
- The higher the concentration of OH- ions, the lower the Ecell value of MnO42-
- So Ecell becomes more positive and the reaction becomes thermodynamically feasible

*reaction with sulfuric acid is very exothermic that’s why an ice bath is used

Describe how the melting temperature range of a crystal is found using given apparatus
- Heat water gently/ stir the water to distribute the heat evenly
- Note the temperature at which crystals start to melt
- Note the temperature at which crystals are completely melted

Why a compound is not coloured

- The 3d subshells did not split so no d-d electron transitions
- No colour as no ligands are present

Describe how to calibrate a pH metre

- Use equal volumes of alkaline buffer solution
- And an acidic buffer solution

Why is the ethoxyethane layer washed with sodium hydroxide solution

- To neutralise the HBr formed

Thiele tube:

The capillary tube must be sealed at one end. Describe how this is done.

- While rotating the tube, heat one end of the tube in a Bunsen flame until the glass starts
to melt

When crystals are placed in the capillary tube they often stick to the top. Describe how to
ensure the crystals reach the bottom of the capillary tube
- Gently tapping the tube

— compiled by Progga Paromita

Two properties of dibutyl phthalate that make it a suitable liquid for the Thiele tube:
- High boiling point
- Does not decompose

Taking upper meniscus reading effect on titre value: No effect since titre value is the
difference between two readings.

Effect on pipette:-
- Volume is less
- Should be read from the lower meniscus

Effect on burette:-
- The volume will be the same
- As the volume in a burette is found from the difference between two readings

*in thermal decomposition, observation could be that colourless liquid condenses at the
mouth of the boiling tube referring to water produced

Test for water:

- Add anhydrous cobalt (ii) chloride
- Blue solid turns pink

Combustion Analysis in U Tubes:

- Tube 1 → For absorbing H2O - anhydrous CaCl2 [Clarifies milky solution if added in one]
- Tube 2 → For absorbing CO2 - Soda Lime

To show decomposition is complete → heat to constant mass

Using this method, (above one), how is the formula of the compound confirmed
- Mass of compound measured before the experiment
- Measure the change in mass in tubes 1 and 2

The cause of the initial stream of bubble from the capillary tube
- Expansion of trapped air

Why is the side-arm of the Thiele tube heated rather than the lowest point?
- For more even distribution of heat

Why might the results vary using a thiele tube, even though al the experimental procedure is
accurate?
- Difference in atmospheric pressure day to day.

— compiled by Progga Paromita

Iodoform test
- Warm gently
- With iodine solution
- And sodium hydroxide solution
- Formation of pale yellow precipitate for positive result

*to quench sulfuric acid → sodium hydrogen carbonate

When should the time be recorded during quenching?

- When half of the reaction mixture has been pipetted into the quenching solution

Compound needed to allow redox reaction to occur (dichromate vi and chromium iii in LHS
beaker and manganate vii and manganese ii in the RHS beaker)
- Dilute sulfuric acid

Why KMnO4 is a stronger oxidising agent than K2Cr2O7?

- Electrons flow to the positive
- Reduction occurs at the RHS electrode and so KMnO4 is the stronger oxidising agent

Phenol test
- Add Br2 solution and shake.
- Solution decolourises and a white ppt with antiseptic smell forms.

*top of the condenser should never be sealed in heat under reflux to prevent buildup of
pressure

Geometric isomers- Each of the double bonded C=C atoms have different groups on them.
Optical isomers- One chiral carbon centre which is attached to 4 different groups

*anti-bumping granules- to prevent flash boiling/ to enable smooth boiling / prevent the
formation of large bubbles.

Give the reason why the organic layer is washed with sodium hydrogencarbonate solution and
suggest how the alkalinity of the aqueous layer should be confirmed (in a separating funnel)
- To neutralise any remaining sulfuric acid [context specific]
- The aqueous layer turns damp red litmus blue

*lower yield of esterification reaction → the reaction is reversible / is in equilibrium

Pipette preparation
- Rinse with distilled water
- Rinse with the solution that is to be measured (eg. hydrogen peroxide)

— compiled by Progga Paromita

Burette check
- Vertical
- Securely clamped
- The jet of the burette is full and there are no bubbles

*hydrogen peroxide slowly decomposes over time

*sodium hydrogen carbonate is used as a solution and not a solid because….

- The solid does not have a high surface area

Give a reason why it is acceptable for a sample of the reaction mixture to be quenched at times
other than every 5 minutes, for example at 4 minutes and 30 seconds
- If the time is known accurately, then it can still be plotted correctly, so time doesnt matter.

Explain why it is not possible to remove the sixth sample by pipette and state how it would still
be possible to titrate the sixth sample
- There is an insufficient volume of the reaction mixture left in the flask to pipette exactly
10 cm3
- Add sodium hydrogen carbonate directly to the flask with the reaction mixture and titrate
the mixture

*compound used as a base value for chemical shifts- tetramethylsilane

Why is ice water used for cooling rather than ice cubes?
- Ice cubes have a lower surface area

*remember to give perforations on a Buchner funnel

*remember to give AND LABEL filter paper on the Buchner funnel
*Pipe out of apparatus must go to a vacuum pump and LABELLED as such
*filter paper should be trimmed so that the edges do not go up the sides of the funnel

*why potassium hydroxide solution should not be used for the salt bridge.
- The hydroxide would react with Zn in zinc half cell [context specific] to form insoluble salt
Zn(OH)²

How to make distillate from separating funnel go from cloudy to clear→ add anhydrous CaCl2

Bromine clock experiment

Purpose of phenol
- Phenol reacts rapidly with the bromine formed in this reaction
- When all the phenol is used up- the excess bromine bleaches the methyl red indicator

- Reacts with bromine

— compiled by Progga Paromita

 - To delay colour change

*remember that if the methyl orange is in aqueous solution- then the initial colour will be pink,
which is then bleached colourless by bromine

*the temperature is also measured at the same time as taking other measurements→ as the
temperature also affects the rate

How to obverse colour change of indicator

- Track progress against a white background

Why is the total volume kept constant

- So that the volume of BrO3- is proportional to the concentration

Give a reason why the potassium bromate (v) solution is first measured into a separate boiling
tube rather than directly into the reaction mixture
- The burette would transfer the liquid too slowly so the titre would be inaccurate

To determine the overall rate equation, what changes should be made to the procedure?
- Repeat the experiments for various concentrations of Br- ions and then for H+ ions
- Varying the value for each, adding the appropriate volume of water and keeping all the
other values constant

*adding small amounts of sample

- Use a pipette
- Add drop by drop by tapping pipette

*make sure that the ppt is washed properly

- If it isn’t, the moles of the ppt calculated will be higher, and hence the value of the
calculated concentration of the solution will be higher than actual

*benzene is volatile and carcinogenic, so it is always heated under reflux in procedures

*ammonia is toxic so always carried out procedures under fume cupboard
*SO2 is toxic, so use a fume cupboard here as well

During nitration, why is the reaction mixture stirred continuously?

- Reactants are immiscible
- The reactants need to be mixed to ensure enough contact for a reaction to take place

Why a solid is dried in a dessicator rather than heated in an oven?

- To avoid thermal decomposition if dried in an oven

*No matter the volume used, a measuring cylinder is used instead of a pipette when precise
measurements are not needed.

— compiled by Progga Paromita

Why - since it is quicker to add the chemical from a measuring cylinder.

(Context specific) why the addition of ethanol results in the precipitation of crystals
- Less soluble in ethanol than in water- easier to form crystals

Sulfate ion test:

- Add dilute hydrochloric acid (used in order to react with carbonate and sulfite impurities
that might be present in the sample), followed by BaCl2 (aq)
- White ppt forms

TItration procedure using LiCl as an example.

- A stopwatch is used to monitor the temperature of the water every 30 seconds for 2.5
minutes
- The LiCl is added at exactly 3 minutes
- The change in temperature is measured and the measurements are continued to be
taken at the same interval for a further 5 minutes
- A graph of temperature against time is plotted
- Two lines of best fit are then extrapolated to meet at the time of the mixing to determine
the maximum rise in temperature

Test for -OH group

- Add PCl5(s)
- Observe misty/steamy fumes

****Note that this is true if there are -COOH groups present as well.

Role of Sn in the preparation of nitrobenzene to phenylamine

[Sn + conc. HCl(aq) + HUR; reduction occurs]

- Acts as a reducing agent (it is a catalyst that undergoes oxidation, the reaction here
required the answer to be this)

The initial ppt when NaOH is added to reducing nitrobenze to phenylamine - Sn(OH)2
Ppt. then dissolves.

Why is NaCl added to a separating funnel? [Context Specific]

- To aid the separation of the layers (by increasing density of aqueous layer)

How to relieve the pressure in a separating funnel?

- Invert the funnel and open the tap

*ether is highly flammable, so heat using water bath

— compiled by Progga Paromita

What happens to the calculated percentage impurity when the student forgets to rinse the
beaker?
- The volume of titre would decrease as there is a lower mass of the sample in 100 cm^3
volumetric flask so less amount of (iodate v) in reaction. Less (iodine) produced, and the
titre needed is lower
- Since the amount of (KIO3) used is less, percentage purity decreases as it appear mass
is lower of KIO3

*gentle reminder that benzenes generally prefer electrophilic substitution

*when acid reacts with thiosulfate, an yellow solid of sulfur is observed

*if starch was not used in thiosulfate reaction → colour would change from pale yellow to
colourless

*both aromatic compounds and cycloalkanes undergo incomplete combustion to form a black/
yellow sooty flame.
**Always prioritise presence of benzene ring in writing conclusions.
***If asked what else also leads to smoky flames, only then write cycloalkane.

*Fehling’s Test ppt. → Cu2O [red ppt.]

Given X is a transition metal compound.

Colorimetry as a continuous method of monitoring

- Using a colorimeter (mark to identify process as it was asked in the question)
- Measuring the absorbance values at various times
- Using a calibration curve to obtain concentration

Explain why the front window of the fume cupboard must be below the safety line with the
exhaust fan switched on.
- If the window is above the safety line, the exhaust system is not strong enough to draw
in the fumes
- So the toxic fumes will escape into the lab

— compiled by Progga Paromita

— compiled by Progga Paromita
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ALWAYS USE A PEAR SHAPED FLASK FOR HEAT UNDER REFLUX

— compiled by Progga Paromita