Accessed from 203.130.214.
106 by regis22 on Sat Apr 12 01:31:32 EDT 2014
USP 36
Acceptance criteria: Meets the requirements
ASSAY
Change to read:
• PROCEDURE
▲Edetate disodium titrant: Prepare and standardize as
directed in Reagents, Volumetric Solutions, Edetate Diso-
dium, Twentieth-Molar (0.05 M).▲USP36
Sample: 800 mg of Ammonium Alum
Analysis: Transfer the Sample to a 400-mL beaker, mois-
ten with 1 mL of glacial acetic acid, and add 50 mL of
water, 50.0 mL of Edetate disodium titrant and 20 mL of
acetic acid–ammonium acetate buffer TS. Warm on a
steam bath until the solution is complete, and boil gen-
tly for 5 min. Cool, add 50 mL of alcohol and 2 mL of
dithizone TS, and titrate ▲the excess edetate diso-
dium▲USP36 with 0.05 M zinc sulfate VS to a bright rose-
pink color. Perform a blank determination, and make
any necessary correction. Each mL of 0.05 M Edetate
disodium titrant is equivalent to 11.86 mg of
AlNH4(SO4)2.
Acceptance criteria: 99.0%–100.5% on the dried basis
IMPURITIES
• HEAVY METALS, Method I 〈231〉
Test preparation: Dissolve 1 g in 20 mL of water, and
add 5 mL of 0.1 N hydrochloric acid. Evaporate the so-
lution in a porcelain evaporating dish to dryness. Treat
the residue with 20 mL of water, and add 50 mg of
hydroxylamine hydrochloride. Heat the solution on a
steam bath for 10 min, cool, and dilute with water to
25 mL.
Analysis: Proceed as directed in the chapter, except add
50 mg of hydroxylamine hydrochloride to the Standard
Preparation.
Acceptance criteria: 20 ppm
• IRON
Sample solution: 6.7 mg/mL
Analysis: Add 5 drops of potassium ferrocyanide TS to
20 mL of the Sample solution.
Acceptance criteria: No blue color is produced
immediately.
SPECIFIC TESTS
• LOSS ON DRYING 〈731〉
Sample: 2.0 g
Analysis: Transfer the Sample, in a tared porcelain cruci-
ble, to a muffle furnace at 200°. Increase the tempera-
ture to 300°, and dry at 300° to a constant weight.
Cool in a desiccator, and weigh.
Acceptance criteria: 45.0%–48.0%
• LIMIT OF ALKALIES AND ALKALINE EARTHS
Sample: 1 g
Analysis: Completely precipitate the aluminum from a
boiling solution of the Sample in 100 mL of water by
the addition of sufficient 6 N ammonium hydroxide to
render the solution distinctly alkaline to methyl red TS,
and filter. Evaporate the filtrate to dryness, and ignite.
Acceptance criteria: The weight of the residue is NMT
5 mg (0.5%).
Potassium Alum
.
AlK(SO4)2 · 12H2O 474.39
Sulfuric acid, aluminum potassium salt (2:1:1),
dodecahydrate.
Aluminum potassium sulfate (1:1:2) dodecahydrate
[7784-24-9].
Anhydrous 258.21 [10043-67-1].
Official from December 1, 2013
Copyright (c) 2014 The United States Pharmacopeial Convention. All rights reserved.
Official Monographs / Alumina 2389
» Potassium Alum contains not less than
99.0 percent and not more than 100.5 percent of
AlK(SO4)2, calculated on the dried basis.
Packaging and storage—Preserve in tight containers, and
store at room temperature.
Identification—
A: Add 1 N sodium hydroxide dropwise to a solution of it
(1 in 20): a precipitate is formed that dissolves in an excess
of the reagent. Ammonia is not evolved (distinction from Am-
monium Alum).
B: Hold it in a nonluminous flame: a violet color is im-
parted to the flame.
C: Add 10 mL of sodium bitartrate TS to 5 mL of a satu-
rated solution of it: a white, crystalline precipitate is formed
within 30 minutes.
D: A solution (1 in 20) responds to the tests for Alumi-
num 〈191〉 and for Sulfate 〈191〉.
Loss on drying 〈731〉—Transfer 2.0 g, in a tared porcelain
crucible, to a muffle furnace at 200°. Increase the tempera-
ture to 400°, and dry at 400° to constant weight. Cool in a
desiccator, and weigh: it loses between 43.0% and 46.0%
of its weight.
Heavy metals, Method I 〈231〉—Dissolve 1 g in water to
make 20 mL, and add 5 mL of 0.1 N hydrochloric acid.
Evaporate the solution in a porcelain evaporating dish to
dryness. Treat the residue with 20 mL of water, and add
50 mg of hydroxylamine hydrochloride. Heat the solution
on a steam bath for 10 minutes, cool, dilute with water to
25 mL, and proceed as directed, except to add 50 mg of
hydroxylamine hydrochloride to the Standard Preparation:
the limit is 0.002%.
Iron—Add 5 drops of potassium ferrocyanide TS to 20 mL
of a solution (1 in 150): no blue color is produced immedi-
ately.
Assay—
Edetate disodium titrant—Prepare and standardize as di-
rected in the Assay under Ammonium Alum.
Procedure—Transfer about 800 mg of Potassium Alum, ac-
curately weighed, to a 400-mL beaker, moisten with 1 mL
of glacial acetic acid, and add 50 mL of water, 50.0 mL of
Edetate disodium titrant, and 20 mL of acetic acid–am-
monium acetate buffer TS. Warm on a steam bath until so-
lution is complete, and boil gently for 5 minutes. Cool, add
50 mL of alcohol and 2 mL of dithizone TS, and titrate 0.05
M zinc sulfate VS to a bright rose-pink color. Perform a
blank determination, and make any necessary correction.
Each mL of 0.05 M Edetate disodium titrant is equivalent to
12.91 mg of AlK(SO4)2.
Alumina and Magnesia Oral Suspension
.
» Alumina and Magnesia Oral Suspension is a
mixture containing aluminum hydroxide
[Al(OH)3] and Magnesium Hydroxide [Mg(OH)2].
It contains the equivalent of not less than
90.0 percent and not more than 110.0 percent of
the labeled amounts of aluminum hydroxide
[Al(OH)3] and magnesium hydroxide [Mg(OH)2].
It may contain a flavoring agent, and may con-
tain suitable antimicrobial agents.
Packaging and storage—Preserve in tight containers, and
avoid freezing.
Labeling—Oral Suspension may be labeled to state the alu-
minum hydroxide content in terms of the equivalent
 Accessed from 203.130.214.106 by regis22 on Sat Apr 12 01:31:32 EDT 2014
2390 Alumina / Official Monographs
amount of dried aluminum hydroxide gel, on the basis that
each mg of dried gel is equivalent to 0.765 mg of Al(OH)3.
Identification—
A: To a solution of 5 g in 10 mL of 3 N hydrochloric acid
add 5 drops of methyl red TS, heat to boiling, add 6 N am-
monium hydroxide until the color of the solution changes
to deep yellow, then continue boiling for 2 minutes, and
filter: the filtrate responds to the tests for Magnesium 〈191〉.
B: Wash the precipitate obtained in Identification test A
with hot ammonium chloride solution (1 in 50), and dis-
solve the precipitate in hydrochloric acid: the solution re-
sponds to the tests for Aluminum 〈191〉.
Microbial enumeration tests 〈61〉 and Tests for speci-
fied microorganisms 〈62〉—Its total aerobic microbial
count does not exceed 100 cfu per mL, and it meets the
requirements of the test for absence of Escherichia coli.
Acid-neutralizing capacity 〈301〉—The acid consumed by
the minimum single dose recommended in the labeling is
not less than 5 mEq, and not less than the number of mEq
calculated by the formula:
0.55(0.0385A) + 0.8(0.0343 M)
in which 0.0385 and 0.0343 are the theoretical acid-neutral-
izing capacities, in mEq, of Al(OH)3 and Mg(OH)2, respec-
tively, and A and M are the quantities, in mg, of Al(OH)3
and Mg(OH)2 in the specimen tested, based on the labeled
quantities.
pH 〈791〉: between 7.3 and 8.5.
Chloride 〈221〉—Dissolve 5.0 g in the minimum volume of
nitric acid required to achieve complete solution, add 1 mL
of acid in excess, then add water to make 100 mL, and
filter: a 10-mL portion of the filtrate shows no more chloride
than corresponds to 1.0 mL of 0.020 N hydrochloric acid
(0.14%).
Sulfate 〈221〉—Dissolve 5.0 g in 5 mL of 3 N hydrochloric
acid, with gentle heating. Cool, add water to make 250 mL,
mix, and filter: a 20-mL portion of the filtrate shows no
more sulfate than corresponds to 0.40 mL of 0.020 N sulfu-
ric acid (0.1%).
Other requirements—It meets the requirements of the
tests for Arsenic and Heavy metals under Aluminum Hydroxide
Gel.
Assay for aluminum hydroxide—
Edetate disodium titrant—Prepare and standardize as di-
rected in the Assay under Ammonium Alum.
Assay preparation—Transfer an accurately measured quan-
tity of Oral Suspension, previously well shaken in its original
container, equivalent to about 1200 mg of aluminum hy-
droxide, to a suitable beaker. Add 20 mL of water, stir, and
slowly add 10 mL of hydrochloric acid. Heat gently, if neces-
sary, to aid solution, cool, and filter into a 200-mL volumet-
ric flask. Wash the filter with water into the flask, add water
to volume, and mix.
Procedure—Pipet 10 mL of Assay preparation into a
250-mL beaker, add 20 mL of water, then add, in the order
named and with continuous stirring, 25.0 mL of Edetate di-
sodium titrant and 20 mL of acetic acid–ammonium acetate
buffer TS, and heat near the boiling point for 5 minutes.
Cool, add 50 mL of alcohol and 2 mL of dithizone TS, and
mix. Titrate with 0.05 M zinc sulfate VS until the color
changes from green-violet to rose-pink. Perform a blank de-
termination, substituting 10 mL of water for the Assay prepa-
ration, and make any necessary correction. Each mL of 0.05
M Edetate disodium titrant consumed is equivalent to
3.900 mg of Al(OH)3.
Assay for magnesium hydroxide—
Assay preparation—Prepare as directed in the Assay for
aluminum hydroxide.
Procedure—Pipet a volume of Assay preparation, equiva-
lent to about 40 mg of magnesium hydroxide, into a
Official from December 1, 2013
Copyright (c) 2014 The United States Pharmacopeial Convention. All rights reserved.
USP 36
400-mL beaker, add 200 mL of water and 20 mL of trietha-
nolamine, and stir. Add 10 mL of ammonia-ammonium
chloride buffer TS and 3 drops of an eriochrome black indi-
cator solution prepared by dissolving 200 mg of eriochrome
black T in a mixture of 15 mL of triethanolamine and 5 mL
of dehydrated alcohol, and mix. Cool the solution to be-
tween 3° and 4° by immersion of the beaker in an ice bath,
then remove, and titrate with 0.05 M edetate disodium VS
to a blue endpoint. Perform a blank determination, substi-
tuting 10 mL of water for the Assay preparation, and make
any necessary correction. Each mL of 0.05 M edetate diso-
dium consumed is equivalent to 2.916 mg of Mg(OH)2.
Alumina and Magnesia Tablets
.
» Alumina and Magnesia Tablets contain not less
than 90.0 percent and not more than 110.0 per-
cent of the labeled amounts of aluminum hy-
droxide [Al(OH)3] and magnesium hydroxide
[Mg(OH)2].
Packaging and storage—Preserve in well-closed contain-
ers.
Labeling—Tablets prepared with the use of Dried Alumi-
num Hydroxide Gel may be labeled to state the aluminum
hydroxide content in terms of the equivalent amount of
dried aluminum hydroxide gel, on the basis that each mg of
dried gel is equivalent to 0.765 mg of Al(OH)3.
Identification—
A: To a 0.7-g portion of finely powdered Tablets add
10 mL of 3 N hydrochloric acid and 5 drops of methyl red
TS, heat to boiling, and add 6 N ammonium hydroxide until
the color of the solution changes to deep yellow. Continue
boiling for 2 minutes, and filter: the filtrate responds to the
tests for Magnesium 〈191〉.
B: Wash the precipitate obtained in Identification test A
with a hot solution of ammonium chloride (1 in 50), and
dissolve the precipitate in hydrochloric acid: the solution re-
sponds to the tests for Aluminum 〈191〉.
Disintegration 〈701〉: 10 minutes, simulated gastric fluid
TS being substituted for water in the test.
Uniformity of dosage units 〈905〉: meet the require-
ments for Weight Variation with respect to alumina and to
magnesia.
Acid-neutralizing capacity 〈301〉—The acid consumed by
the minimum single dose recommended in the labeling is
not less than 5 mEq, and not less than the number of mEq
calculated by the formula:
0.55(0.0385A) + 0.8(0.0343 M)
in which 0.0385 and 0.0343 are the theoretical acid-neutral-
izing capacities, in mEq, of Al(OH)3 and Mg(OH)2, respec-
tively, and A and M are the quantities, in mg, of Al(OH)3
and Mg(OH)2 in the specimen tested, based on the labeled
quantities.
Assay for aluminum hydroxide—
Edetate disodium titrant—Prepare and standardize as di-
rected in the Assay under Ammonium Alum.
Assay preparation—Weigh and finely powder not fewer
than 20 Tablets. Transfer an accurately weighed portion of
the powder, equivalent to about 1200 mg of aluminum hy-
droxide, to a 150-mL beaker, add 20 mL of water, stir, and
slowly add 30 mL of 3 N hydrochloric acid. Proceed as di-
rected for Assay preparation in the Assay for aluminum hy-
droxide under Alumina and Magnesia Oral Suspension, begin-
ning with “Heat gently, if necessary.”