Stage 4 Harmonization Sodium 1

Official May 1, 2021

ASSAY
Sodium Lauryl Sulfate
Portions of this monograph that are national USP text, and are Change to read:
not part of the harmonized text, are marked with symbols • CONTENT OF SODIUM ALKYL SULFATES
(◆◆) to specify this fact. ▲
Dimidium bromide–sulfan blue mixed solution: Dissolve
Sulfuric acid monododecyl ester sodium salt; separately 0.5 g of dimidium bromide and 0.25 g of sulfan
Sodium monododecyl sulfate [151-21-3]. blue in 30 mL of a hot solution of 10% ethanol in water,
combine these solutions, and dilute with 10% ethanol to
DEFINITION 250 mL. Mix 20 mL of this solution with 20 mL of a 14.0%
Sodium Lauryl Sulfate is a mixture of sodium alkyl sulfates (v/v) solution of sulfuric acid previously diluted with about
consisting chiefly of sodium lauryl sulfate (C12H25NaO4S). It 250 mL of water, and dilute with water to 500
contains NLT 85.0% of sodium alkyl sulfates calculated as mL.▲ (NF 1-May-2021)
sodium lauryl sulfate (C12H25NaO4S). Sample: ▲1.15 g▲ (NF 1-May-2021) of Sodium Lauryl Sulfate
IDENTIFICATION Titrimetric system
(See Titrimetry á541ñ.)
Change to read:
Mode: Direct titration
Titrant: 0.004 M benzethonium chloride VS
• ▲
▲ (NF 1-May-2021)A.
SPECTROSCOPIC IDENTIFICATION TESTS Endpoint detection: Visual
á197ñ, Infrared Spectroscopy: 197A or 197K▲▲ (NF 1-May-2021) Analysis: Dissolve the Sample in water, warming if
• B. SODIUM necessary, and dilute with water to exactly 1000.0 mL.
Potassium pyroantimonate solution: To 2 g of potassium
▲
Mix 20.0 mL of the solution with 15 mL of methylene
pyroantimonate add 100 mL of water. Boil the solution for chloride and 10 mL of Dimidium bromide–sulfan blue mixed
about 5 min, cool quickly, and add 10 mL of a solution of solution.▲ (NF 1-May-2021)Titrate with Titrant, shaking
potassium hydroxide (3 in 20). Allow to stand for 24 h, and vigorously and allowing the layers to separate before each
filter. addition, until ▲the pink color of the methylene chloride
Sample: 2.5 g layer is completely discharged and a greyish-blue color is
Analysis: Place the Sample in a silica or platinum crucible, obtained.▲ (NF 1-May-2021) One milliliter of Titrant is equivalent
and add 2 mL of 10 N sulfuric acid. Heat on a water bath, to 1.154 mg of sodium alkyl sulfates, calculated as sodium
then cautiously raise the temperature progressively over an lauryl sulfate (C12H25NaO4S).
open flame. Ignite, preferably in a muffle furnace, at 600 Acceptance criteria: NLT 85.0%, calculated as sodium
± 25°. Continue heating until all black particles have lauryl sulfate (C12H25NaO4S)
disappeared. Cool, add a few drops of 2 N sulfuric acid, and
heat and ignite as above. Add a few drops of ammonium IMPURITIES
carbonate TS, evaporate to dryness, and ignite as above.
Cool, dissolve the residue in 50 mL of water, and mix. To a Change to read:
2-mL portion of this solution, add 4 mL of Potassium • SODIUM CHLORIDE
pyroantimonate solution. If necessary, rub the inside of the Fluorescein sodium solution: Dissolve 0.2 g of fluorescein
test tube with a glass rod. sodium in water to 100 mL.
Acceptance criteria: A white, crystalline precipitate is Dilute nitric acid: Dilute 105 mL of nitric acid with water to
formed. 1000 mL.
• C. SULFATE Sample solution: 100 mg/mL of Sodium Lauryl Sulfate in
Sample: Solution (1 in 10) water
Analysis: After acidification with hydrochloric acid and Analysis: Neutralize 50 mL of Sample solution with Dilute
boiling for 20 min, no precipitate is formed. Add barium nitric acid, using litmus paper as the indicator, if necessary.
chloride TS; a white precipitate is produced. Add exactly 5.0 mL of 0.1 N sodium chloride and titrate,
Acceptance criteria: Meets the requirements ▲
under vigorous stirring (to disperse silver
chloride),▲ (NF 1-May-2021) with 0.1 N silver nitrate VS
Delete the following: (indicator: 2 drops of Fluorescein sodium solution) to the first
▲
• D. appearance of turbidity with solution color change from
Sample: 0.1 g yellow-green to orange through yellow. Perform a blank
Analysis: Dissolve the Sample in 10 mL of water and shake. determination, and make any necessary correction. Each
Acceptance criteria: A copious foam is milliliter of 0.1 N silver nitrate is equivalent to 5.844 mg of
formed.▲ (NF 1-May-2021) sodium chloride.
Acceptance criteria: The combined content of sodium
chloride and sodium sulfate is NMT 8.0%.
Delete the following:
▲
• E. Change to read:
Sample: Solution prepared for Identification D
Analysis: To 0.1 mL of the Sample, add 0.1 mL of a 1-g/L • SODIUM SULFATE
solution of methylene blue and 2 mL of diluted sulfuric Sample solution: 100 mg/mL of Sodium Lauryl Sulfate in
acid. Add 2 mL of methylene chloride and shake. water
Acceptance criteria: An intense blue color develops in the Analysis: To 10 mL of Sample solution, add 100 mL of
methylene chloride layer.▲ (NF 1-May-2021) alcohol and heat at a temperature just below the boiling
point for 2 h. Pass through a glass ▲or
porcelain▲ (NF 1-May-2021) filter ▲(pore size equivalent to 4–10
µm)▲ (NF 1-May-2021) while hot, and wash with 100 mL of
boiling alcohol. Dissolve the precipitate by washing with
150 mL of water, collecting the washings in a beaker. Add

© 2020 The United States Pharmacopeial Convention All Rights Reserved.

2 Sodium Stage 4 Harmonization
Official May 1, 2021
10 mL of diluted hydrochloric acid, heat to boiling, add 25 to a 500-mL separator, rinsing the flask twice with ether and
mL of barium chloride TS, and allow to stand overnight. adding the washings to the separator. Extract the solution
Collect the precipitate ▲by filtration through a filter with two 75-mL portions of ether, evaporate the combined
(maximum pore size of 16 µm)▲ (NF 1-May-2021) and wash with ether extracts in a tared beaker on a steam bath, dry the
water until the last washing shows no opalescence with residue at 105° for 30 min, cool, and weigh.
▲
0.1 N silver nitrate VS▲ (NF 1-May-2021). Dry the precipitate, Acceptance criteria: The residue represents the total
ignite to constant mass between 500° and 600° by raising alcohols and is NLT 59.0% of the weight of Sodium Lauryl
the temperature gradually, and weigh as barium sulfate Sulfate taken.◆
(BaSO4; 233.39). • UNSULFATED ALCOHOLS
Sample solution: Dissolve 10 g in 100 mL of water, and add
Amount (mg) of sodium sulfate (Na2SO4) = amount (mg) of 100 mL of alcohol.
barium sulfate (BaSO4) × 0.6086 Analysis: Transfer the solution to a separator, and extract
with three 50-mL portions of petroleum ether. If an
Acceptance criteria: The combined content of sodium emulsion forms, sodium chloride may be added to promote
chloride and sodium sulfate is NMT 8.0%. separation of the two layers. Wash the combined petroleum
ether extracts with three 50-mL portions of water, and dry
SPECIFIC TESTS with anhydrous sodium sulfate. Filter the petroleum ether
• ALKALINITY extract into a tared beaker. Evaporate on a water bath until
Sample solution: Dissolve 1.0 g in 100 mL of water, add 0.1 the odor of petroleum ether no longer is perceptible, dry
mL of phenol red TS, and titrate with 0.10 N hydrochloric the residue at 105° for 30 min, cool, and weigh.
acid. Acceptance criteria: The weight of the residue is NMT 4.0%
Acceptance criteria: NMT 0.5 mL for neutralization of the weight of Sodium Lauryl Sulfate taken.
• ◆TOTAL ALCOHOLS: Transfer 5 g to an 800-mL Kjeldahl flask,
and add 150 mL of water, 50 mL of hydrochloric acid, and ADDITIONAL REQUIREMENTS
a few boiling chips. Attach a reflux condenser to the • ◆PACKAGING AND STORAGE: Preserve in well-closed
Kjeldahl flask, heat carefully to avoid excessive frothing, and containers.◆
boil for 4 h. Cool the flask, rinse the condenser with ether, • USP REFERENCE STANDARDS á11ñ
collecting the ether in the flask, and transfer the contents USP Sodium Lauryl Sulfate RS

© 2020 The United States Pharmacopeial Convention All Rights Reserved.