PFN 99/117

Method for the determination of acid insoluble sieve residues on

raw meals and raw materials.

(i) Take a representative sample of about 10 g and weigh this quantity accurately to three
decimal places. Wet sieve on the required mesh (normally 170 mesh, aperture 90
um). If the sieve residue itself is required it may be dried and weighed as usual.

(ii) Transfer residues completely to evaporating basin, if necessary inverting the sieve and
washing off with water. Add further water to make up to approximately 100 ml, and
then add 20 ml of 50% technical HC1, making sure to wear appropriate PPE.

(iii) Warm the evaporating basin over a bunsen, taking care not to boil the contents. Stir
occasionally with a glass rod and after a few minutes remove the bunsen. Add a little
more acid, and if effervescence occurs, continue adding acid until there is no more
effervescence and, after warming and stirring, the liquid turns blue litmus paper red.

(iv) Remove the evaporating basin from the heat, dilute with 100 ml of cold water and
pour the evaporating basin contents through the sieve, transferring the residue by
rinsing with water. Rinse the sieve with a little water to remove any acid and briefly
wet sieve the residue. Any quantity of residue should be transferred to a dish by
washing off with water, and excess water decanted off through the sieve. The acid
insoluble residue can then be rinsed with acetone, (to speed up the drying process),
the rinsings being decanted through the sieve, and both dish and sieve dried off. (See
Safety comment below)

(v) The contents of sieve and dish should be combined and weighed, to give the acid
insoluble sieve residue.

Safety

Acetone is a highly flammable substance and adequate precautions should be taken to restrict
Acetone vapour to the surrounding atmosphere, eg a fume cupboard or vapour removal
system. If this is not available then acetone should not be used and the dish and sieve should
have the resultant washings evaporated in an oven at ~ 105 °C until dry.
Worked example:

M1 = original sample weight [para (i)]

M2 = residue weight after initial wet sieving [para (ii)]
M3 = insoluble residue weight on sieve [para (v)]
M4 = insoluble residue weight on dish [para (v)]

M2
Sample Residue = x 100 %
M1

M3 M4
Insoluble Residue = x 100 %
M1

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