Microscale chemistry is an environmentally safe pollution prevention method of performing chennmical processes using small quantities of chemicals with

out compromising the quality and standard of chemical applications in education and industry. The best way to succeed in this effort is by eliminating chemical waste at the source. Traditional organic lab uses grams, Microscale uses milligrams.

Advantages
1. It offers vastly
Better Laboratory Air Quality. Least Exposure to Toxic Chemicals. No Fire and Explosion Hazards. No Spills and Accidents.

improved laboratory safety by

2. It sharply

reduces laboratory cost.

3. It requires

shorter experiment time.

It lowers glass breakage cost. 5. It is user friendly to people with physical disabilities.
4.

Ground-glass joints:
These are used to attach one piece of glass

equipment to another with an air-tight seal. They come in standard sizes, called "standard taper", and are identified by two numbers: 1. the first indicating the diameter of the joint . 2. the second indicating the length of the tapered part.

Conical Vials :
Chemical reactions usually are carried out

in these vials, and they can also be used for measuring and storing chemicals. Each one has an outer ground-glass joint and a threaded outer surface to allow attachment of other glassware. There are four sizes: 5.0 mL, 3.0 mL, 1.0 mL, and 0.3 mL capacity.

Air Condensers :
They are usually attached to a (conical vial)

and used to prevent vapors from escaping. The vapors contact the cool, inside surface of the tube and condense into the liquid phase,returning to the reaction mixture. The air condenser can also function as a simple mechanical extension to hold a conical vial in place in a cooling or heating bath.

Water-cooled or Jacketed Condensers :

These serve the For lower-boiling

same purpose as the air condensers, except that cooling is made more efficient by circulating cold tap water through an outer glass jacket.

liquids, this additional cooling is necessary to prevent the escape of vapors.

Claisen Head or Claisen Adaptor :

This allows introducing chemical

reagents (usually liquids) into a reaction mixture without taking apart the whole apparatus. Liquids can be introduced with a syringe without exposing the reaction mixture to the atmosphere. Thermometer can be introduced through the access hole.

Hickman Distilling Head :

The purpose of a still is to heat a liquid until is

passes into the gas (vapor) phase, and then allow the vapor to cool and condense back into the liquid phase, trapped in a second container. The Hickman still functions like the air condenser in condensing vapors with the cool glass surface. But the liquid drips down the inside to be trapped in a small circular depression, in the lower part of the tube.

Drying Tube :
The tube is used to protect the reaction from

moisture in the atmosphere while still allowing the passage of air to equalize pressure. To accomplish this the tube is packed with a glass wool plug, a quantity of drying agent, and another glass wool plug. It is important to remove the drying agent and clean the tube after each use, since drying agents can harden and swell with time and become impossible to remove.

Craig Tube :
The Craig tube is used for small-scale

recrystallization, which is a method for the purification of small quantities of solid compounds. It has two parts: 1. An outer body, which functions like a vial or test tube. 2. An inner plunger, which fits partly into the body and rests on a ground-glass surface. The ground-glass joint is not greased, so that liquids can leak through it but solids cannot pass.

Capillary Gas Delivery Tube :

It is placed on top of a reaction apparatus in

which gas is generated, and the gas passes through the tube to be collected in an inverted tube at the other end. Gas collection is used to: Measure the quantity of gas produced in a reaction. Or to prevent toxic gases from escaping to the atmosphere.

Syringe :
used to measure and transfer small volumes of

liquids, It consists of three parts: 1. the body, which is calibrated according to volume. 2. The plunger, which fits into the body so that liquid cannot escape between the ground-glass outer surface of the plunger and the groundglass inner surface of the body. 3. The needle, which is a hollow, pointed piece of stainless steel.

Micro-spatula :
This is one of the most useful devices in

your microscale kit. The flat, long blade can be used to weigh out solids, stir mixtures, scratch glass surfaces to induce crystallization, and generally poke at solutions to see what's going on. Keep it clean so that reactions and chemicals are not cross-contaminated.

Description :
In this experiment students do a microscale esterification reaction between 2-hydroxybenzoic acid (salicylic acid) and ethanoic anhydride using phosphoric acid as a catalyst.
salicylic acid

Chemicals
Phosphoric acid (85%)

Ethanoic anhydride

Procedure :
1-Put eight drops of aminobenzene in a beaker and add 30 drops of deionised water followed by 15 drops of concentrated acid, put it .hydrochloric in an ice bath 2-Weigh 0.15 g of sodium nitrite into another beaker and add 1 cm3 of deionised water.

Cool the beaker in the ice bath. Add one spatula of urea(this prevents side reactions occurring).
3-Mix the contents of the two beakers together and keep in the ice bath.

4-Weigh 0.45 g of 2naphthol into another beaker and add 3 cm3 of sodium hydroxide solution. Swirl to dissolve. 5-Take a piece of cotton cloth using tweezers, dip it into the 2-naphthol solution. Allow the solution to completely soak the cotton.

6-Dip the cloth completely into the diazonium salt solution.

References:
1. Grey, Egerton C (1928). Practical Chemistry by Micro-Methods. Cambridge: W Heffer & Sons Ltd. 2. El-Marsafy, M K (1989). "Microscale Chemistry Experimentation". MicrEcol. M.K.El-Marsafy. 3. Thompson, S. "Small-Scale Chemistry". National Small-Scale Chemistry Centre. Colorado State University.

1.Nada Essam Fahmy. 2.Nayera Muhammed Nagy.

385 402

3.Hager Ashraf Sobhy Ahmed.

4.Heba Salah eldeen Ramzy. 5.Huda Muhammed Emad.

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