Experiment # 3


Preparation of Acetic acid

Date: 12-10-10

Muhammad Usman (2008-chem-02-B)

1. Ethanol: Harmful:
Pure Ethanol will irritate the skin and eyes. Nausea, vomiting and intoxication are symptoms of ingestion. Long term use by ingestion can result in serious liver damage. Death from Ethyl alcohol consumption is possible when blood alcohol level reaches 0.4%. A blood level of 0.5% or more is commonly fatal. Levels of even less than 0.1% can cause intoxication, with unconsciousness often occurring at 0.3–0.4%

Highly flammable:
It has a flash point of 13 oC. It can readily catch fire. So care should be taken while handling it because its combustion products include Acetaldehyde which is a strongly carcinogenic substance. However, ethanol itself is not cancer causing.

Properties of Ethanol:
IUPAC Name Ethanol

Other names

Absolute alcohol Drinking alcohol Ethyl alcohol Ethyl hydrate Grain alcohol Hydroxy-Ethane


Colorless liquid


Molecular formula Molar mass Density Melting point Boiling point Solubility in water Acidity (Pka) Flash point Auto-ignition temperature

C2H6O 46.07 g mol-1 0.789 g cm-3 -114.3 oC 78.4 oC Miscible 15.9 13 oC 422 oC

Sodium Di-chromate:

Sodium di-chromate is a strong oxidizing agent. It will readily oxidize anything that will come into contact with it. Precautionary measures are necessary while handling it.

It is a strongly corrosive compound as it readily oxidizes anything.

Dangerous to Environment:
It is a Hexa-valent chromium ion so is considered hazardous. It can contaminate potable water as it is of carcinogenic properties.

Very toxic:
If swallowed, this compound can even cause death because it is very toxic compound. It is carcinogenic in nature. Potable water should especially be treated which may contain Hexa-valent chromium compounds.

It is a very harmful substance. Its contact with skin should be avoided.

Properties of sodium di-chromate:
IUPAC name Other names Sodium dichromate Chromic acid, (H2Cr2O7), disodium salt


Molecular formula Molar mass

Na2Cr2O7 261.97 gmol-1 (anhydrous) 298.00 gmol-1(di-hydrate)


Density Melting point Boiling point Solubility in water

2.52 g cm-3 356.7 oC 400 oC decomposes 730 g/ l (25 oC)

Sulphuric acid:

It is a strongly corrosive compound as it readily oxidizes anything.

Dangerous to Environment:
Although sulfuric acid is non-flammable, contact with metals in the event of a spillage can lead to the liberation of hydrogen gas. The dispersal of acid aerosols and gaseous sulfur dioxide is an additional hazard of fires involving sulfuric acid.

Very toxic:
Sulfuric acid is not considered toxic besides its obvious corrosive hazard, and the main occupational risks are skin contact leading to burns and the inhalation of aerosols. Exposure to aerosols at high concentrations leads to immediate and severe irritation of the eyes, respiratory tract and mucous membranes.

Properties of sulfuric acid:
IUPAC name Other names Sulfuric acid Oil of vitriol


Molecular formula


Molar mass

98.06 g/gmol


Density Melting point Boiling point Solubility in water Acidity (Pka) Viscosity Flash point

1.84 g/cm3 (liquid) 10 oC 337 oC Miscible -3 26.7 cP (20 oC) Non- flammable

It is a non-hazardous compound.

Environmentally safe:
Water is an essential part of life. Life cannot be sustained without water. Food & eatables contain some amount of water in them. It is a nonhazardous compound.

IUPAC name

Water Oxidane

Other names

Hydrogen oxide Dihydrogen monoxide Hydrogen monoxide Hydroxylic acid Hydrogen hydroxide R-718 Oxygen dihydride

Oxygen hydride Oxane


Molecular formula Molar mass

H2O 18.0152833 gmol-1


Density Melting point Boiling point Acidity (Pka) Basicity (Pkb) Viscosity

1000 kg m-3 (liquid) 917 kg m-3 (solid) 0 oC 99.98 oC 15.74 15.74 0.001 Pa.S (20 oC)

Preparation of Acetic Acid

Chemicals required:
1) Ethanol 3) Concentrated H2SO4 2) Sodium di-chromate 4) Water

Apparatus Required:
Bolt head flask Knee tube Adopter Stirrer Dropping funnel Water condenser Conical flask beaker

Chemical Equation:

CH3CH (OH) 3

[-H O]




1) Place 15 ml of water into the Bolt head flask. Add 10 ml of concentrated H 2SO4slowly with shaking. Finally add 10.5 g of Na-Dichromate & some fragments of porcelain. 2) Place a mixture of 4.5 ml of ethanol & 18ml of water in dropping funnel. 3) Fit a bolt head flask with reflux H2O condenser to the top of which a dropping funnel is fixed. 4) Add Ethanol-H2O mixture drop by drop down the condenser into the flask. A vigorous reaction occurs & mixture becomes green. 5) When the addition is complete & reaction is subsided, heat the flask on a boiling H 2O bath for 1520 minutes. 6) Detach & reverse the condenser & re-connect it to the flask through a knee tube for direct distillation & distill the mixture by direct heating.

Uses of Acetic acid:
Acetic acid is used: As a coagulant for latex in rubber industry In the manufacture of plastics (polyvinyl acetate) rayon (cellulose acetate) and silk In medicine as a local irritant

As a solvent in laboratory for carrying out reactions In the manufacture of pickles In the manufacture of many organic compounds like acetone, acetates and esters

Industrial preparation of acetic acid: Feed tank:
Weak acetaldehyde is fed into this tank. Cooling brine is used to remove heat of acetaldehyde.

Heat exchanger:
From storage CH3CHO is fed to next unit via a heat exchanger where the feed stream is heated by exchange of heat with steam coming out of acetaldehyde still.

Acetaldehyde still:
In this unit the acetaldehyde is heated to remove any water contents or other volatile materials. Pure acetaldehyde is cooled with cooling brine in coils and is sent to the pure acetaldehyde storage tank.

Oxidizing kettle:
This is the reaction zone. Here air at a pressure of 70 Psi is introduced and catalyst is added. Acetaldehyde is converted into acetic acid. Off gases like nitrogen are collected at the top and sent to a scrubber where it is washed with water and vented to atmosphere and un-reacted material is sent back via recycle stream again into the process.

Acetic acid still:
Crude acetic acid is again refined via a still and stored in a refined acetic acid tank.

References: 1. Shreve’s chemical process industries by George T. Austin 2nd edition, page 947-948 2. Unit processes in organic synthesis by P.H. Groggins 5th edition, page 509-510 3. Wikipedia http://en.wikipedia.org/wiki/acetic_acid/

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