Deepak Fertilisers and Petrochemicals Corporation Ltd.- Testing for distillation range

Deepak Fertilisers & Petrochemicals Corporation Ltd.

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A leading manufacturer of industrial chemicals including methanol, nitric acid and carbon dioxide.

The largest Indian manufacturer of ammonium nitrate.

"Mahadhan" brand fertilisers are effective for a wide variety of crops.

Test method for analysis of acidity in volatile solvents and chemical intermediates

Scope
This method covers a procedure for the determination of total acidity as acetic acid, in concentration below 0.05 per cent, organic compounds and hydrocarbon mixtures used in paint, varnish and lacquer solvents and diluents. It is known to be applicable to such mixture as low molecular weight saturated and unsaturated alcohols, ketone, ether, ester, hydrocarbon diluents, naphtha, and other light distillate petroleum fraction.

Summary of the Method
The sample is mixed with either an equal volume of water or an equal volume of alcohol and titrated with aqueous sodium hydroxide solution to the phenolphthalein end point.

Reagents

a) Alcohol, Refined, ethyl or iso-propyl.
b) Phenolphthalein Indicator Solution. : (10 gm per litre) Dissolves 1.0 gm phenolphthalein in isopropyl alcohol (99 percent) and dilute to 100 ml with the alcohol.
c) Sodium hydroxide, standard solution (0.05N).

Apparatus

a) Buret, 10 ml, graduated in 0.05 ml subdivisions
b) Erlenmeyer Flask, 250 ml capacity.
c) Pipet, capable of delivering 2.0 ml of solution.
d) Interval Timer and clock, capable of measuring a time interval of 120 min or more. An alarm arrangement may be desirable.

Procedure

(a) Measure in to a 250-ml Erlenmeyer flask 50 ml water, or 50 ml of alcohol, if the sample is not completely water-soluble.
(b) Add 0.5 ml of phenolphthalein indicator solution. Titrate the water or alcohol with 0.05 N NaOH solution to the first perceptible pink colour.
(c) Pipet 50 ml of the sample in to the flask. Titrate with the 0.05 N NaOH solution to the same first perceptible pink colour originally obtained glass constant-temperature bath is employed, it should be wrapped or coated with an opaque material.

Fill a 50 ml Nessler tube beyond the mark with the sample to be tested and place in the constant-temperature bath. Maintain the water level in the bath approximately 1 in. (25 mm) below the top of the tube. When the sample has reached the specified temperature, being the level to the 50 - ml mark. With a pipet, add 2 ml of the KMnO4 solution. Stopper the tube, invert once to mix the contents, return to the bath and note the time. At the end of the minimum time specified for the material being tested, remove the tube and compare it to the colour standard by viewing downward through the tube against a white background from which diffused white light is reflected.

The following time and temperature conditions should be employed:

Temperature Of Test	Permanganate time mm
Acetone	25C	ASTM Specification D 329
Methanol	15 C	ASTM Specification D 1152

Report
If the residual pink colour of the sample is greater than the standard, report the permanganate time as "greater than X minutes". If the residual pink colour of the sample is equal to that of the standard, report the permanganate time as "X minutes". If the residual pink colour of the sample is less than the standard report as "less than X minutes". Where "X minutes" is the minimum time specified for the material being tested.

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