General Test Procedure Identification by IR

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7 months ago

General Test Procedure Identification by IR

1.0 Purpose
1.1 This procedure is applicable to all incoming raw materials.
2.0 Apparatus
2.1 Infrared Spectrophotometer
2.2 Hydraulic Pellet Press
2.3 Lab Oven
2.4 Analytical Balance
3.0 Reagents
3.1 Potassium Bromide spectroscopic grade
3.2 Liquid Paraffin AR grade
3.3 Sodium chloride

4.0 Procedure
4.1 Substance being examined is mixed intimately with potassium

bromide IR grade and compressed into Pellets.
4.1.1 Triturate 1 to 2mg of the substance with approximately 300-400mg

of dry finely powdered Potassium bromide

(Dry the KBr for minimum one hour at 105°C).
4.1.2 Grind the mixture thoroughly, spread it uniformly in a

suitable die and compress at a pressure of about 5 tons.
4.1.3 Carefully remove the pellet from the disc.
4.1.4 If pellet is not transparent then prepare one more pellet in the same way.
4.1.5 Mount the pellet in the sample holder.
4.1.6 Take IR absorption in the range between 4000-1 to 650-1 cm.

In the same way make a pellet of RS and take IR.
4.1.7 Store the reference spectrum of RS in the hard disc of the

computer and compare (Superimpose) spectrum of sample with

the reference standard.
4.2 For liquids use sodium chloride cell having thickness of 2mm path

length, procedure same as above.

4.2.1 Make slurry of substance with Mineral Oil and suspend neatly

between sodium chloride plates.
4.2.2 Take IR absorption spectrum between 4000 and 650cm-1
4.2.3 In the same way prepare the slurry of WS and take IR.
4.2.4 The IR absorption spectrum of sample should be concordant

with spectrum obtained with WS.
4.2.5 The working standard used should be authenticated against a current

Pharmacopoeia standard.
4.2.6 This authentication should be repeated once in every 6 months.
4.2.7 If sample and standard are not concordant then recrystallization

for both the standard working and the sample, using the same solvent method is used.

4.3 The IR of the modified WS and the sample should be concordant.

5.0 Reference I.P.

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