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Gasometric assays

-Depends upon two type of operational concepts: i)measurement of the volume of a gas liberated under the conditions that are described in the assay. ii)Decrease in volume of a gas when a suitable reagent is used to remove one of the gases present.

-Apparatus: gas burette or nitrometer: -These are provided with two(or three)stopcock & two way outlet. -Properly connected with a balancing tube.

Assay of carbon dioxide: -Limit: Minimum 99.5 per cent V/V of CO2 in the gaseous phase. -The sample is absorbed in 50% potassium hydroxide & the volume of the residual gas is measured.

-It is carried out by the use of hempel apparatus: -It is composed of burette & absorption pipette. -Hempel burette is fitted with three-way tap. -Measuring tube & leveling tubes are connected by a rubber tube(about 3 feet).

-The three way tap is turned so as to connect the measuring tube to gas air. -The top tap is also opened. -A stream of the gas from the supply is passed through the measuring tube for about two minutes. -Both taps are closed. -The top of the measuring tube is connected to the absorption pipette(via a bent capillary & rubber tubes).

-The lower bulb of the pipette is filled with 50%w/v solution of potassium hydroxide. -The upper bulb is partly filled. -The connection is made such a way that the connecting tube becomes completely filled with the liquid. -The top tap of the burette is opened.

-The leveling tube is(filled with water) raised with so as to drive the whole of the gas into the lower bulb of the pipette. -Gentle rocking of the pipette is carried out(2-3 minutes). - It ensures complete absorption of carbon dioxide. -Then the leveling tube is lowered.

-The small volume of the residual gas is drawn back into the burette. -The tap is turned off as soon as the capillary has become filled with liquid. -The levels in the two burette are adjusted & the volume of unabsorbed gas is read.

Assay of oxygen:

-Limit: not less than 99.0 per cent v/v of O2. -The gas sample is exposed to the action of an ammonical copper solution. -The solution reacts with oxygen. -The residual gas volume is a measure of the impurities present.(Should not more than 1% of the original). 4NH4Cl+8CuNH3Cl+8NH3+2H2O+O2 = 4CuCl,CuCl2,4NH3+4NH4OH.

-Either Hempel or Franke burette can be used for measurement. -For rapid assay Franke burette is used. -The dry burette is filled with the gas by passing a stream through for two minutes as appropriate. -Then, taps are closed.

-The plug is removed & receiver is filled with alkaline pyrogallol solution. -The plug is replaced & the tap is closed. -By central tap the solution is allowed to flow into the burette. -The burette is gently shaken to ensure the complete absorption of oxygen. -The burette is then inverted & the central is opened.

-All the absorbent is flowed back into the receiver. -The central tap is closed. -The burette is turned right way up. -The burette is lowered into a cylinder of water. -The bottom tap is opened. -Water is adjusted to the same level inside & outside the burette.

-The volume of unabsorbed gas is read on the scale.

Assay of cyclopropane: Limit: not less than 99.0 per cent v/v of . -The sample is treated with Conc. sulphuric acid in a mercury-charged nitrometer. -Cyclopropane is absorbed by ring fission & formation of propyl hydrogen sulphate. CH2 | CH2 CH2 + H2SO4 CH3.CH2 .CH2.HSO4

References: -Bentley & drivers text book of pharmaceutical chemistry. -Alfonso R. Gennaro: Remington: the Science and Practice of Pharmacy