ALUMINIUM SULFATE (ANHYDROUS)

Prepared at the 55th JECFA (2000) and published in FNP 52 Add 8

(2000), superseding tentative specifications prepared at the 22nd
JECFA (1978) and published in FNP 7 (1978) and in FNP 52 (1992).
No ADI was allocated at the 22nd JECFA (1978).

SYNONYMS INS No. 520

DEFINITION
Chemical names Aluminium sulfate

C.A.S. number 10043-01-3

Chemical formula Al2(SO4)3

Formula weight 342.13

Assay Not less than 99.5% on the ignited basis

DESCRIPTION White powder, shining plates, or crystalline fragments; odourless

FUNCTIONAL USES Firming agent

CHARACTERISTICS
IDENTIFICATION

Solubility (Vol. 4) Freely soluble in water, insoluble in ethanol

pH (Vol. 4) 2.9 or above ( 5% solution )

Test for aluminium Passes test

(Vol. 4)

Test for sulfate (Vol. 4) Passes test

PURITY

Loss on ignition (Vol. 4) Not more than 5% (about 500o, 3 h)

Alkalis and alkaline earths To a boiling solution of 2 g of the sample in 150 ml of water add a few
(Vol. 4) drops of methyl red TS. Then add ammonia TS until the colour of the
solution just changes to a distinct yellow. Add hot water to restore the
original volume, and filter while hot. Evaporate 75 ml of the filtrate to
dryness, and ignite to constant weight. Not more than 4 mg of residue
remains (about 0.4%).

Fluoride Not more than 30 mg/kg

 See description under TESTS

Lead Not more than 5 mg/kg

Determine using an atomic absorption technique appropriate to the
specified level. The selection of sample size and method of sample
preparation may be based on the principles of the method described in
VOLUME 4, "Instrumental Methods"

Selenium (Vol. 4) Not more than 30 mg/kg

Test 0.2 g of the sample as directed in the Limit Test (Method II)

TESTS
Fluoride Lime Suspension
Carefully slake about 56 g of low-fluoride calcium oxide (about 2 mg/kg
F) with 250 ml of water, and add 250 ml of 60% perchloric acid slowly
and with stirring. Add a few glass beads, and boil to copious fumes of
perchloric acid, then cool, add 200 ml of water, and boil again. Repeat
the dilution and boiling once more, cool, dilute considerably, and filter
through a fritted glass filter, if precipitated silicon dioxide appears. Pour
the clear solution, with stirring, into 1000 ml of a 1 in 10 sodium
hydroxide solution, allow the precipitate to settle, and siphon off the
supernatant liquid. Remove the sodium salts from the precipitate by
washing 5 times in large centrifuge bottles, shaking the mass
thoroughly each time. Finally, shake the precipitate into a suspension
and dilute to 2000 ml. Store in paraffin-lined bottles and shake well
before use. 100 ml of this suspension should give no appreciable
fluoride blank when evaporated in a platinum dish and treated as
directed below under "Procedure", beginning with "Ignite briefly at
600o,...".

Distillation Apparatus
Connect a 125-ml distillation flask with a condenser. Equip also with a
thermometer and a capillary tube, both of which must extend into the
liquid. Connect a small dropping funnel or a steam generator to the
capillary tube. Support the flask on an asbestos mat with a hole which
exposes about one-third of the flask to the flame. To minimize the
distillation blank resulting from fluoride leached from the glassware, the
distillation apparatus should be treated as follows: treat the glassware
with hot 10% sodium hydroxide solution, followed by flushing with tap
water and rinsing with distilled water. At least once daily, treat in
addition by boiling down 15-20 ml of a 1 in 2 sulfuric acid solution until
the still is filled with fumes; cool, pour off the acid, treat again with 10%
sodium hydroxide solution, and rinse thoroughly.

Procedure
Add to the distilling flask 1.67 g of the sample, accurately weighed, and
25 ml of a 1 in 2 sulfuric acid solution. Distil until the temperature
reaches 160o, then maintain at 160o to 165o by adding water from the
funnel, collecting 300 ml of distillate. Oxidize the distillate by the
cautious addition of 2 or 3 ml of fluoride-free 30% hydrogen peroxide
 (to remove sulfites), allow to stand for a few min, and evaporate in a
platinum dish with an excess of Lime Suspension. Ignite briefly at 600o,
then cool and wet the ash with about 10 ml of water. Cover the dish
with a watch glass, and cautiously introduce under cover just sufficient
60% perchloric acid to dissolve the ash. Add the contents of the dish
through the dropping funnel of a freshly treated distilling apparatus (the
distilling flask should contain a few glass beads), using a total of 20 ml
of 60% perchloric acid for dissolving the ash and transferring the
solution. Add 10 ml of water and a few drops of a 1 in 2 silver
perchlorate solution through the dropping funnel. Continue as directed
in the Limit Test, Method I, Thorium Nitrate Colorimetric Method,
beginning with "Distil until the temperature reaches 135o ...".

METHOD OF ASSAY Weigh accurately about 4 g of the sample, transfer into a 250-ml
volumetric flask. Dissolve in water, dilute to volume with water, and mix.
Pipet 10 ml of this solution into a 250-ml beaker, add 25.0 ml of 0.05 M
disodium ethylenediaminetetra-acetate, and boil gently for 5 min. Cool,
and with continuous stirring add in the order given: 20 ml of pH 4.5
buffer solution (77.1 g of ammonium acetate and 57 ml of glacial acid in
1000 ml), 50 ml of ethanol, and 2 ml of dithizone TS. Titrate with 0.05 M
zinc sulfate until the colour changes from green-violet to rose-pink, and
perform a blank determination, substituting 10 ml of water for the
sample. Each ml of 0.05 M disodium ethylenediaminetetraacetate is
equivalent to 8.553 mg of Al2(SO4)3.