Experiment of preparation of a compound

Reflux

Called condenser

AIM:
 heat reaction with slow rxr to increase rxr
 Vapourised r/p are condensed to prevent escape of r/p and return to flask.
 Prevents loss of volatile r/p
 Enables flammable liquids to be heated safely

Possible evaluation:
 Top of condenser should not be sealed
 For condenser, inner tube and outer water jacket should be shown
 Pear shape flaks not conical flask
 Heating source is water bath or electrical heater
 Anti-bumping granules allows smooth boiling

Purification by Washing

Purification of Solid:
1. Impure solid is removed by normal filtration
2. Soluble solid is removed by suction filtration

Purification of liquid:
1. Solvent Extraction
2. Distillation

Solvent extraction

AIM:
Properties of solvent:a
 immiscible in water
 low boiling temperature

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Recrystallisation

Step 1: The solid was dissolved in the minimum amount of hot ethanol
 To minimize amount of solid left in solution when it recrystallizes

Step 2: The hot solution was filtered

 (HOT) so most of solid remains in hot solution
OR to prevent premature formation of crystals in the funnel
 (Filter) to remove insoluble impurities

Step 3: The filtrate was cooled in an ice bath

 To ensure maximum amount of solid crystalizes

Step 4: The mixture was filtered using suction filtration

 To remove soluble impurities

Step 5: Crystals are washed with cold solvent and Dry crystal between filter papers

Suction Filtration: Filtration under reduced pressure

Advantages of suction filtration compared to normal filtration

1. Faster
2. Crystals are drier

Possible evaluation of suction filtration (can be drawn for modification)

 Butcher Funnel should have perforated base shown as dotted line under filter paper
 Suction pump is needed
 Filter paper should be trimmed so that it does not go up at the sides of funnel

How to identify crystal? Solid impurities: reduces MP

Liquid Impurities: increases BP
Measure melting temperature and compare to data booklet
 Pure crystals have sharper melting temp, consistent to literature value
 Impure crystals have larger range of melting temp and have range start at lower temp

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Normal Filtration:

Advantage of using above funnel

1. Product cannot crystallise in the funnel
2. Block the stem of the funnel

Distillation

Steam distillation

AIM:
 Separation an insoluble liquid from an aqueous solution
 Can be used to purify some compound / molecules

Advantage:
1. Insoluble liquid is removed from the reaction mixture at a temperature below its normal BP
2. Less decomposition occurs

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Melting temperature determination

The Capillary tube is sealed at one end… HOW?

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

Crystals are often stick in the top of capillary tube.

Describe how to ensure crystals reach the bottom of capillary tube
By gently tapping the tube

Properties of Liquid used in thiele tube

- High BP
- Does not decompose
- Mobile

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Tips from User Guide and etc…

Inorganic Compounds and elements

Appearance of solid
 Coloured crystalline substances are usually hydrated salts of transition metals
e.g) green solid : Cu(II), Cr(III), Ni(II) salts

Flame test with metal

 Ca2+ : yellow-red
 Li+ or Sr+ : red

Heating of compound
 Metal Carbonate other than Group 1 : Carbon dioxide gas
 Group 1 nitrates (not Li) : Oxygen gas
 Nitrates : Oxygen gas and nitrogen dioxide gas
 Hydrated salts: water

Recognition and identification of common gas

Gas Observations
oxygen colourless gas which relights a glowing splint
colourless gas which gives a white precipitate with limewater (calcium hydroxide
carbon dioxide
solution)
colourless gas which turns moist red litmus paper blue and forms white smoke
ammonia
with hydrogen chloride
nitrogen dioxide brown gas*
hydrogen colourless gas which ignites with a ‘pop’
steamy fumes on exposure to moist air, acidic and forms white smoke with
hydrogen chloride
ammonia
chlorine pale green gas which bleaches moist litmus paper
bromine brown gas*
iodine purple vapour
water vapour Add water to blue cobalt chloride to pink
Sulfate ion Add Barium Chrloide and diluted HCl(aq) and form a white precipitate (BaSO4)
Thiosulfate Acidic gas of sulfur dioxide and pale yellow ppt of Sulfur formed

* Bromine dissolves in organic solvents to form a brown solution whereas nitrogen dioxide is
insoluble.

Add dilute acids onto compound and elements

 Chromate(VI) becomes dichromate (VI), yellow solution turn orange

 Thiosulfate (𝑆2 𝑂32−): Sulfur dioxide acidic gas and pale yellow Sulfur ppt formed

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Hydrogen Peroxide solution

 Can act as both an oxidizing agent and reducing agent

Observation of adding H2O2 Inference Oxidation/Reduction

manganate(VII), brown precipitate Reduction
brown precipitate
is MnO2
purple solution is Reduction
manganate(VII) in acid solution
decolourised
pale green solution turns Oxidation
iron(II) to iron(III) in acid solution
yellow
green precipitate turns iron(II) hydroxide to iron(III) Oxidation
brown hydroxide
green alkaline solution goes Oxidation
Cr(III) to chromate(VI)
yellow
brown solution or black Oxidation
iodine from iodide in acid solution
precipitate

Precipitate

Barium Chloride(aq) Solution

 Test for Sulfate (SO42-), Sulfite (SO32-), Carbonate (CO32-)

 Add BaCl2 and then add dilute HCl

 When dilute HCl is added first, only sulfate forms ppt

Silver Nitrate solution

 Test for halides

 Add dilute nitric acid to remove any anions like carbonate and then add silver nitrate
 Then, add aqueous ammonia.

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Concentrated sulfuric acid
 Test for halides

Bad egg smell for H2S

Organic Compound

Solubility

Ignition

Chemical Test
 Ester has characteristic smell

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Tips from Paper 6

Apparatus

Perform at constant temperature

 Apparatus in water bath with thermometer

Advantage of water bath

 Water bath is used to make organic compound not to boil/evaporate
 Prevent compounds to ignite/explode

Dry organic molecule with

 Anhydrous CaCl2
 Should be compound that does not react with reaction mixtures

Complete decomposition
 Heat to constant mass

Pipette
 Use pipette with pipette filler
 Used for accurate calculation. For approximate volume, use measuring cylinder
 For 10cm^3 pipette, 10.0cm^3 of solution is insufficient volume of the reaction mixture left
in the flaks to pipette exactly 10.0cm^3

Burette:
 Before taking initial burette reading, check whether nozzle is full.

Meniscus
 Top of meniscus for pipette
1. volume of solution is lower than measured
2. So, pipette is calibrated to be measured from bottom of meniscus
 Top of meniscus for burette
1. Volume is same
2. as volume from burette is difference between two readings

Why is ice cube not used instead of ice bath?

 Ice cubes have less contact for cooling

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How to calibrate pH meter?
 Use pH meter to measure pH of alkaline buffer solution and acidic buffer solution

pH of solution is measured by…

 pH meter and Universal indicator.
 pH meter is more accurate as
1. universal indicator is difficult to match colour of indicator to pH
2. the colour of universal indicator covers a range of pH.

Why is water added before the sulfuric acids?

 Sulfuric acid reacts very exothermically with water

For stating impurities…

 Try to be precise
1. Identify the impurities if possible
2. Physical state (solid, liquid)
3. Soluble or Insoluble

Crystallization
1. Evaporate solution until reach to crystallization point
2. Cover solution and allow to coo
3. Dry crystals between filter paper

Graphs
 Scale of axis can start from not zero. So suitable scale can be from 8 – 22

Safety Precaution
 Wear lab coat and safety googles
 Flammable: use electrical heating or use water bath
 Corrosive: Wear gloves
 Toxic: Perform in fume cupboard
 Hydrogen is explosive

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Rate of Reaction

Give reason why it is acceptable for reaction mixture to be quenched at times other than every 5
minutes, like 4minutes and 30 seconds?
 If the time is accurately known, then it can still be plotted correctly and give same gradient

When should time be stopped for measuring rate of reaction with quenching?
 When half of reaction mixture has been pipetted into quenching solution

Rate
−𝑐ℎ𝑎𝑛𝑔𝑒 𝑖𝑛 [𝑟𝑒𝑎𝑐𝑡𝑎𝑛𝑡] 𝑐ℎ𝑎𝑛𝑔𝑒 𝑖𝑛 [𝑝𝑟𝑜𝑑𝑢𝑐𝑡]
𝑟𝑎𝑡𝑒 = =
𝑐ℎ𝑎𝑛𝑔𝑒 𝑖𝑛 𝑡𝑖𝑚𝑒 𝑐ℎ𝑎𝑛𝑔𝑒 𝑖𝑛 𝑡𝑖𝑚𝑒

Find order w.r.t… using graph:

1. State order
 For zero: [x] is independent to rate; change in [x] does not affect the rate
 For first: [x] is proportional to rate; increase/double in [x] increases/doubles rate

2. State, features of gradient, half-life and relate to rate of reaction.

e.g) gradient is constant so rate is constant

Redox and Electrochemical Cell

Titration:
 Transition metal ions can be oxidized by air.
 Continuous monitoring is better than sampling method (quenching) due to
1. Reaction does not need to be quenched (stopped)
2. Timing of data points is much more accurate
3. Small amount of reaction mixture is used

Compound for acidifying solution in half-cells for redox to occur

 Sulfuric acid not hydrochloric acid as HCl might be oxidized by strong oxidizing
agent(reduced)

Positive electrode shows

 Electron flows from negative electrode to positive electrode.
 So, reduction occurs at positive electrode, species gain electrons

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Transition Metal

Manganese (II) solution

 Colorless not pale pink
 For colourless to pale pink in titration, pale pink is for diluted manganate(VII) ion

Adding insoluble transition metal hydroxides, ammonia complexes to diluted acid

 When acid is added, reaction is reversed

 Hence, CuCl2(aq) forms aqua ion of Cu2+ shown as blue solution, not Cu-ammonia complex
shown as deep-blue solution

Anion of FeCl2 is tested with silver nitrate. Further test is addition of ammonia solution. Why is
this not a useful procedure?
 Ammonia reacts with iron ions to form a iron(II) hydroxide ppt
 Which obscures the dissolving of white ppt

Organic Chemistry

Phenol
 Test: add bromine water and a white ppt with antiseptic smell is formed
 Phenol cannot react with carboxylic acid as phenol is less reactive than alcohol but with acyl
chloride it can form ester

For nitration…
 Only H atom in 2 or 4 C atom is substituted.

Oxidation of Aldehyde
 Tollen’s reagent: aqueous ammoniacal silver nitrate/heat and clean test tube/silver mirror
 Benedict’s Fehling’s Solution: Copper(II) Sulfate Na2CO3 or NaOH / heat and clean test tube/
red ppt

O-H group test:

1. PCl5 -> steamy fume
2. Na -> effervescence
 These tests shows that OH group present. As it is given by both group, it odes not show that
an alcohol group is present

IR/MS/NMR
 TMS: Tetramethylsilan
 Fragmentation is made by loss of a radical.

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