Printed on: Fri Jan 05 2024, 09:43:49 PM(EST) Status: Currently Official on 06-Jan-2024 DocId: GUID-350DC704-A573-404F-A435-E257AE27F908_5_en-US

Printed by: USP NF Official Date: Official as of 01-Jun-2023 Document Type: NF @2024 USPC
Do Not Distribute DOI Ref: 7a9ho DOI: https://doi.org/10.31003/USPNF_M46650_05_01
1

sodium chloride, dilute each with water to volume,

Magnesium Aluminum Silicate and mix.
DEFINITION Sample stock solution: Transfer 0.200 g of Magnesium
Magnesium Aluminum Silicate is a blend of colloidal Aluminum Silicate to a 25-mL platinum crucible
montmorillonite and saponite that has been processed to containing 1.0 g of lithium metaborate, and mix. Using a
remove grit and nonswellable ore components. muffle furnace or a suitable burner, heat slowly at first, and
The requirements for viscosity and ratio of aluminum content ignite at 1000°–1200° for 15 min. Cool, place the crucible
to magnesium content differ for the several types of in a 100-mL beaker containing 25 mL of dilute nitric acid
Magnesium Aluminum Silicate, as set forth in the table (50 mg/mL), and add an additional 50 mL of the dilute
below. acid, filling and submerging the upright crucible. Place a
polyfluorocarbon-coated magnetic stirring bar into the
crucible, and stir gently with a magnetic stirrer to dissolve.
Viscosity Al Content/ Pour the contents into a 250-mL beaker, and remove the
Type (mPa · s) Mg Content Appearance
crucible. Warm the solution, transfer through a rapid-flow
Min. Max. Min. Max. filter paper with the aid of water into a 200-mL volumetric
flask, dilute with water to volume, and mix.
Fine
granules or Sample solution: Pipet 20 mL of the Sample stock solution
IA 225 600 0.5 1.2 flakes into a 100-mL volumetric flask. Add 20 mL of a solution
of sodium chloride (10 mg/mL), dilute with water to
Microfine
IB 150 450 0.5 1.2 powder volume, and mix.
Instrumental conditions
Fine (See Atomic Absorption Spectroscopy á852ñ.)
granules or
Mode: Atomic absorption spectrophotometer equipped

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IC 800 2200 0.5 1.2 flakes
with a single-slot burner
Fine Analytical wavelength: 309 nm
granules or Lamp: Aluminum hollow-cathode
IIA 100 300 1.4 2.8 flakes
Flame: Oxidizing acetylene–air–nitrous oxide
Analysis
IDENTIFICATION
• A.
Sample: 2 g
ci Samples: Aluminum standard solutions and Sample
solution
Determine the absorbances of the Aluminum standard
Analysis 1: Add the Sample in small portions to 100 mL of solutions and the Sample solution. From a linear
water with intense agitation. Allow to stand for 12 h to regression equation calculated from the absorbances
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ensure complete hydration. Place 2 mL of the resulting and concentrations of the Aluminum standard solutions,
mixture on a suitable glass slide, and allow to air-dry at determine the aluminum content in the magnesium
room temperature to produce an oriented film. Place the aluminum silicate.
slide in a vacuum desiccator over a free surface of ethylene Magnesium content
glycol. Evacuate the desiccator, and close the stopcock so Lanthanum solution: Stir 88.30 g of lanthanum chloride
that the ethylene glycol saturates the desiccator chamber. (LaCl3) with 500 mL of 6 N hydrochloric acid to dissolve,
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Allow to stand for 12 h. Record the X-ray diffraction pattern transfer with the aid of water to a 1000-mL volumetric
(see X-Ray Powder Diffraction á941ñ), and calculate the d flask, dilute with water to volume, and mix.
values. Magnesium standard stock solution: Place 1.000 g of
Acceptance criteria 1: The largest peak corresponds to a d magnesium in a 250-mL beaker containing 20 mL of
value between 15.0 and 17.2 Å. water, and carefully add 20 mL of hydrochloric acid,
Analysis 2: Prepare a random powder specimen of warming, if necessary, to complete the reaction. Transfer
Magnesium Aluminum Silicate, record the X-ray diffraction the solution to a 1000-mL volumetric flask, dilute with
pattern, and determine the d values in the region between water to volume, and mix. This solution contains the
1.48 and 1.54 Å. equivalent of 1 mg/mL of magnesium. Transfer 10.0 mL
Acceptance criteria 2: Peaks are found at 1.492–1.504 Å of this solution to a 1000-mL volumetric flask, dilute with
and at 1.510–1.540 Å. water to volume, and mix.
• B. It meets the requirements of the test for Viscosity in Magnesium standard solutions: Transfer 5-, 10-, 15-, and
Specific Tests. 20-mL aliquots of the Magnesium standard stock solution
• C. It meets the requirements for Ratio of aluminum content to separate 100-mL volumetric flasks. To each flask add
to magnesium content in the test for Aluminum Content and 20.0 mL of Lanthanum solution, dilute with water to
Magnesium Content. volume, and mix.
• D. Its appearance corresponds to the description in the table Sample stock solution: Use the Sample stock solution
in the Definition. prepared as directed for Aluminum content.
ASSAY Sample solution: Transfer 25 mL of the Sample stock
• ALUMINUM CONTENT AND MAGNESIUM CONTENT solution to a 50-mL volumetric flask, dilute with water to
Aluminum content volume, and mix. Transfer 5.0 mL of this solution to a
Aluminum standard stock solution: Dissolve 1.000 g of 100-mL volumetric flask, add 20.0 mL of Lanthanum
aluminum in a mixture of 10 mL of hydrochloric acid and solution, dilute with water to volume, and mix.
10 mL of water by gentle heating. Transfer the solution Instrumental conditions
to a 1000-mL volumetric flask, dilute with water to (See Atomic Absorption Spectroscopy á852ñ.)
volume, and mix. This solution contains the equivalent of Mode: Atomic absorption
1 mg/mL of aluminum. Analytical wavelength: 285 nm
Aluminum standard solutions: Transfer 2-, 5-, and 10-mL Lamp: Magnesium hollow-cathode
aliquots of the Aluminum standard stock solution to Flame: Reducing flame of acetylene–air
separate 100-mL volumetric flasks containing 200 mg of

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Printed on: Fri Jan 05 2024, 09:43:49 PM(EST) Status: Currently Official on 06-Jan-2024 DocId: GUID-350DC704-A573-404F-A435-E257AE27F908_5_en-US
Printed by: USP NF Official Date: Official as of 01-Jun-2023 Document Type: NF @2024 USPC
Do Not Distribute DOI Ref: 7a9ho DOI: https://doi.org/10.31003/USPNF_M46650_05_01
2

Analysis concentrated extracts through a rapid-flow filter paper

Samples: Magnesium standard solutions and Sample into a 50-mL volumetric flask. Transfer the remaining
solution contents of the 400-mL beaker through the filter paper and
Determine the absorbances of the Sample solution and the into the flask with water. Dilute with water to volume.
Magnesium standard solutions. From a linear regression Instrumental conditions
equation calculated from the absorbances and (See Atomic Absorption Spectroscopy á852ñ.)
concentrations of the Magnesium standard solutions, Mode: Atomic absorption spectrophotometer equipped
determine the magnesium content in the magnesium with a deuterium arc background correction and a
aluminum silicate. single-slot burner
Ratio of aluminum content to magnesium content Analytical wavelength: 284 nm
Analysis: Using the results from the Aluminum content and Lamp: Lead hollow-cathode
the Magnesium content, determine the ratio of aluminum Flame: Oxidizing flame of air and acetylene
content to magnesium content. Acceptance criteria: The absorbance of the Test preparation
Acceptance criteria is NMT that of the Standard preparation (15 µg/g).
Type IA: 0.5–1.2
Type IB: 0.5–1.2 SPECIFIC TESTS
Type IC: 0.5–1.2 • MICROBIAL ENUMERATION TESTS á61ñ and TESTS FOR
Type IIA: 1.4–2.8 SPECIFIED MICROORGANISMS á62ñ: Its total aerobic
microbial count does not exceed 103 cfu/g, and it meets
IMPURITIES the requirements of the test for absence of Escherichia coli.
• PH á791ñ
Change to read: Sample suspension: 50 mg/mL
• ▲ARSENIC á211ñ, Procedures, Procedure 1▲ (CN 1-Jun-2023) Acceptance criteria: 9.0–10.0

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Standard preparation: Transfer 5.0 mL (5 µg of arsenic) • LOSS ON DRYING á731ñ
of the Standard Arsenic Solution to a 25-mL volumetric flask, Analysis: Dry at 110° to constant weight.
and add dilute hydrochloric acid (1:25) to volume. Acceptance criteria: NMT 8.0%
Test preparation: Transfer 13.3 g of Magnesium Aluminum • VISCOSITY
Silicate to a 250-mL beaker containing 100 mL of dilute
ci Sample: After determining the Loss on Drying, weigh a
hydrochloric acid (1:25), mix, cover with a watch glass, and quantity of Magnesium Aluminum Silicate, equivalent to
boil gently with occasional stirring for 15 min without 25.0 g on the dried basis. Over a period of a few seconds,
allowing excessive foaming. Allow the insoluble material to transfer the undried test specimen to a suitable 1-L blender
settle, and decant the hot supernatant through a rapid-flow jar containing an amount of water, maintained at a
filter paper into a 200-mL volumetric flask, retaining as temperature of 25 ± 2°, that is sufficient to produce a
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much sediment as possible in the beaker. Add 25 mL of hot mixture weighing 500 g. Blend for 3 min, accurately timed,
dilute hydrochloric acid (1:25) to the residue in the beaker, at 14,000–15,000 rpm (high speed).1
stir, and heat to boiling. Allow the insoluble material to [NOTE—Heat generated during blending causes a
settle, and decant the supernatant through the filter into temperature rise to above 30°.]
the 200-mL volumetric flask. Repeat the extraction with Analysis: Transfer the contents of the blender to a 600-mL
four additional 25-mL portions of hot dilute beaker, and allow to stand for 5 min. The sample
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hydrochloric acid (1:25), decanting each hot supernatant temperature should be 33 ± 3°. Using a suitable rotational
through the filter into the volumetric flask. At the last viscometer2 equipped with a spindle as specified below,
extraction, transfer as much of the insoluble material as operate the viscometer at 60 rpm for 6 min, accurately
possible onto the filter. Cool the combined filtrates to room timed, and record the scale reading.
temperature, add dilute hydrochloric acid (1:25) to For Type IA, use a spindle with a cylinder 1.87 cm in
volume, and mix. Use 25 mL for the test. diameter and 0.69 cm high attached to a shaft 0.32 cm
Acceptance criteria: NMT 3 µg/g; the absorbance due to in diameter, the distance from the top of the cylinder to
any red color from the Test preparation does not exceed the lower tip of the shaft being 2.54 cm, and the
that produced by the Standard preparation. immersion depth being 5.00 cm (No. 2 spindle). If the
• LEAD scale reading is greater than 90% of full scale, repeat the
Standard preparation: On the day of use, dilute 3.0 mL of measurement, using a spindle similar to the No. 2 spindle
lead nitrate stock solution TS with water to 100 mL. Each but with the cylinder 1.27 cm in diameter and 0.16 cm
mL contains the equivalent of 3 µg of lead. high instead (No. 3 spindle).
Sample: 10.0 g For Type IC, use a No. 3 spindle. If the scale reading is
Test preparation: Transfer the Sample to a 250-mL beaker greater than 90% of full scale, repeat the measurement
containing 100 mL of dilute hydrochloric acid (1:25), stir, using a spindle consisting of a cylindrical shaft 0.32 cm in
cover with a watch glass, and boil for 15 min. Cool to room diameter and with an immersion depth of 4.05 cm (No.
temperature, and allow the insoluble matter to settle. 4 spindle).
Decant the supernatant through a rapid-flow filter paper For Types IB and IIA, use a No. 2 spindle.
into a 400-mL beaker. Add 25 mL of hot water to the Acceptance criteria
insoluble matter in the 250-mL beaker, and stir. Allow the Type IA: 225–600 mPa · s
insoluble matter to settle, and decant the supernatant Type IB: 150–450 mPa · s
through the filter into the 400-mL beaker. Repeat the Type IC: 800–2200 mPa · s
extraction with two additional 25-mL portions of water, Type IIA: 100–300 mPa · s
decanting each supernatant portion through the filter into
the 400-mL beaker. Wash the filter with 25 mL of hot water,
collecting this filtrate in the 400-mL beaker. Concentrate 1 A suitable blender is available from Waring as Waring Commercial Blender
the combined extracts by gentle boiling to approximately Model 7009G or equivalent with 1-L glass jar and tachometer adapter,
20 mL. If a precipitate appears, add 2–3 drops of nitric acid, Model CAC24 or equivalent.
2 A suitable viscometer is available from Brookfield as Viscometer Model
heat to boiling, and cool to room temperature. Filter the
LVF or LVT, or equivalent.

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Printed on: Fri Jan 05 2024, 09:43:49 PM(EST) Status: Currently Official on 06-Jan-2024 DocId: GUID-350DC704-A573-404F-A435-E257AE27F908_5_en-US
Printed by: USP NF Official Date: Official as of 01-Jun-2023 Document Type: NF @2024 USPC
Do Not Distribute DOI Ref: 7a9ho DOI: https://doi.org/10.31003/USPNF_M46650_05_01
3

• ACID DEMAND 185, 245, 305, 365, 425, 485, 545, 605, 665, and 725 s,
Sample: After determining the Loss on Drying, weigh a and add a 1.0-mL portion at 785 s. Determine the pH
quantity of Magnesium Aluminum Silicate equivalent to potentiometrically at 840 s.
5.00 g. Acceptance criteria: NMT 4.0
Analysis: Disperse the Sample in 500 mL of water with the
aid of a suitable blender fitted with a 1-L jar. Using a ADDITIONAL REQUIREMENTS
stopwatch, designate zero time. With constant mixing, add • PACKAGING AND STORAGE: Preserve in tight containers.
3.0-mL portions of 0.100 N hydrochloric acid at 5, 65, 125, • LABELING: Label it to indicate its type.

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