Accessed from 10.6.1.
1 by merck1 on Fri Jun 03 04:50:33 EDT 2016
6428 Zinc / Official Monographs
Salicylic Acid, in fine powder . . . . . . 20 g
Zinc Oxide Paste, a sufficient quantity
to make . . . . . . . . . . . . . . . . . . . . . 1000 g
Thoroughly triturate the Salicylic Acid with a
portion of the paste, then add the remaining
paste, and triturate until a smooth mixture is ob-
tained.
Packaging and storage—Preserve in well-closed contain-
ers.
Identification—
A: The residue obtained in the Assay for zinc oxide is yel-
low when hot and white when cool.
B: Shake 1 g of it with 10 mL of water, and filter. To the
filtrate add 1 mL of ferric chloride TS: an intense reddish
violet color is produced. To this solution add 1 mL of acetic
acid: the color is not dispersed. To this solution add 2 mL of
2 N hydrochloric acid: the color is dispersed and a white
crystalline precipitate is formed.
Minimum fill 〈755〉: meets the requirements.
Assay for zinc oxide—Weigh accurately in a tared porce-
lain crucible about 500 mg of Paste, heat gently until
melted, and continue the heating, gradually raising the tem-
perature until the mass is thoroughly charred. Ignite the
mass strongly until all of the carbonaceous material has
been dissipated, the residue is uniformly yellow, and the
weight of the cooled residue is constant. The weight of the
residue represents the quantity of ZnO in the weight of the
Paste taken for the assay.
Assay for salicylic acid—Transfer to a suitable beaker
about 5 g of Paste, accurately weighed. Add 40 mL of alco-
hol, previously neutralized with 0.1 N sodium hydroxide to
a phenol red endpoint, and heat on a water bath for 5 min-
utes, with frequent swirling. While still hot, add phenol red
USP Monographs
TS, and titrate with 0.1 N sodium hydroxide VS to a red
endpoint. Each mL of 0.1 N sodium hydroxide is equivalent
to 13.81 mg of salicylic acid (C7H6O3).
.
Zinc Stearate
Octadecanoic acid, zinc salt;
Zinc stearate [557-05-1].
DEFINITION
Zinc Stearate is a compound of zinc with a mixture of solid
organic acids obtained from fats, and consists chiefly of
variable proportions of zinc stearate and zinc palmitate. It
contains the equivalent of NLT 12.5% and NMT 14.0% of
ZnO.
IDENTIFICATION
• A. IDENTIFICATION TESTS—GENERAL, Zinc 〈191〉
Sample solution: Mix 25 g with 200 mL of hot water,
add 60 mL of 2 N sulfuric acid, and boil until the fatty
acids separate as a transparent layer. Cool the mixture,
and remove the solidified layer of fatty acids.
Acceptance criteria: A portion of the water layer meets
the requirements.
• B. CONGEALING TEMPERATURE 〈651〉
Analysis: Place the separated fatty acids obtained in
Identification test A in a filter wetted with water, and
wash with boiling water until free from sulfate. Collect
the fatty acids in a small beaker, allow to cool, pour off
the separated water, then melt the acids. Filter into a
dry beaker while hot, and dry at 105° for 20 min.
Acceptance criteria: The fatty acids congeal at a tem-
perature not below 54°.
Official from May 1, 2016
Copyright (c) 2016 The United States Pharmacopeial Convention. All rights reserved.
USP 39
ASSAY
• PROCEDURE
Sample solution: Boil 1 g of Zinc Stearate with 50 mL
of 0.1 N sulfuric acid for at least 10 min, or until the
fatty acids layer is clear, adding more water as neces-
sary to maintain the original volume. Cool, and filter.
Wash the filter and the flask thoroughly with water until
the last washing is not acid to litmus paper.
Analysis: Add to the combined filtrate and washings
15 mL of ammonia–ammonium chloride buffer TS and
0.2 mL of eriochrome black TS. Heat the solution to
about 40°, and titrate with 0.05 M edetate disodium VS
until the solution is deep blue in color. Each mL of 0.05
M edetate disodium is equivalent to 4.069 mg of ZnO.
Acceptance criteria: 12.5%–14.0% of ZnO
IMPURITIES
• ARSENIC, Method I 〈211〉
Test preparation: Mix 5.0 g with 50 mL of water. Cau-
tiously add 5 mL of sulfuric acid, and boil gently until
the fatty acids layer is clear and the volume is reduced
to about 25 mL. Filter while hot, cool the filtrate, and
dilute with water to 50 mL. Transfer a 20-mL aliquot to
the arsine generator flask, and dilute with water to
35 mL.
Acceptance criteria: NMT 1.5 ppm
• LEAD 〈251〉
Standard solution: To 20 mL of 0.2 N nitric acid add
5 µg of lead, 4 mL of Ammonia–Cyanide Solution, and
2 drops of Hydroxylamine Hydrochloride Solution, and
shake with 10.0 mL of Standard Dithizone Solution for
30 s. Pass through an acid-washed filter paper into a
color-comparison tube.
Test preparation: Ignite 0.50 g in a platinum crucible
for 15–20 min in a muffle furnace at 475°–500°. Cool,
add 3 drops of nitric acid, evaporate over a low flame
to dryness, and ignite again at 475°–500° for 30 min.
Dissolve the residue in 1 mL of 8 N nitric acid, add
3 mL of Ammonium Citrate Solution and 0.5 mL of Hy-
droxylamine Hydrochloride Solution, and render alkaline
to phenol red TS with ammonium hydroxide. Add
10 mL of Potassium Cyanide Solution. Immediately ex-
tract the solution with successive 5-mL portions of
Dithizone Extraction Solution, draining off each extract
into another separator, until the last portion of
dithizone solution retains its green color. Shake the
combined extracts for 30 s with 20 mL of 0.2 N nitric
acid, and discard the chloroform layer. Add to the acid
solution 4.0 mL of Ammonia–Cyanide Solution and
2 drops of Hydroxylamine Hydrochloride Solution. Add
10.0 mL of Standard Dithizone Solution, and shake the
mixture for 30 s. Pass the chloroform layer through an
acid-washed filter paper into a color-comparison tube.
Acceptance criteria: The color of the Test preparation
does not exceed that of the Standard solution (NMT
10 ppm).
• ALKALIES AND ALKALINE EARTHS
Sample solution: Mix 2.0 g with 50 mL of water, and
add 10 mL of hydrochloric acid. Boil until the solution is
clear, filter while hot, and wash the separated fatty
acids with about 50 mL of hot water. Render the com-
bined filtrate and washings alkaline with 6 N ammo-
nium hydroxide. Add ammonium sulfide TS to precipi-
tate the zinc completely, dilute with water to 200 mL,
mix, and filter.
Analysis: To 100 mL of the clear filtrate add 0.5 mL of
sulfuric acid, evaporate to dryness, and ignite to con-
stant weight.
Acceptance criteria: The weight of the residue does
not exceed 10 mg (1.0%).
ADDITIONAL REQUIREMENTS
• PACKAGING AND STORAGE: Preserve in well-closed
containers.
Accessed from 10.6.1.1 by merck1 on Fri Jun 03 04:50:33 EDT 2016
USP 39
.
Zinc Sulfate
ZnSO4 · xH2O
Sulfuric acid, zinc salt (1:1), hydrate;
Zinc sulfate (1:1) monohydrate 179.46
Zinc sulfate (1:1) heptahydrate 287.56
[7446-20-0].
Anhydrous 161.44
[7733-02-0].
DEFINITION
Zinc Sulfate contains one or seven molecules of water of
hydration. The monohydrate contains NLT 89.0% and
NMT 90.4% of zinc sulfate (ZnSO4), corresponding to
NLT 99.0% and NMT 100.5% of zinc sulfate monohy-
drate (ZnSO4 · H2O), and the heptahydrate contains NLT
55.6% and NMT 61.0% of zinc sulfate (ZnSO4), corre-
sponding to NLT 99.0% and NMT 108.7% of zinc sulfate
heptahydrate (ZnSO4 · 7H2O).
IDENTIFICATION
• A. IDENTIFICATION TESTS—GENERAL, Zinc 〈191〉: Meets the
requirements
• B. IDENTIFICATION TESTS—GENERAL, Sulfate 〈191〉: Meets
the requirements
ASSAY
• PROCEDURE
Sample: An amount of Zinc Sulfate equivalent to
170 mg of zinc sulfate (ZnSO4)
Analysis: Dissolve the Sample in 100 mL of water. Add
5 mL of ammonia–ammonium chloride buffer TS and
0.1 mL of eriochrome black TS, and titrate with 0.05 M
edetate disodium VS until the solution is deep blue in
color. Each mL of 0.05 M edetate disodium is equiva-
lent to 8.072 mg of zinc sulfate (ZnSO4).
Acceptance criteria
Monohydrate: 89.0%–90.4% of zinc sulfate (ZnSO4),
corresponding to 99.0%–100.5% of zinc sulfate mono-
hydrate (ZnSO4 · H2O)
Heptahydrate: 55.6%–61.0% of zinc sulfate (ZnSO4),
corresponding to 99.0%–108.7% of zinc sulfate
heptahydrate (ZnSO4 · 7H2O)
IMPURITIES
• ARSENIC, Method I 〈211〉
Test preparation: Dissolve a portion equivalent to
215 mg of zinc sulfate (ZnSO4) in 35 mL of water.
Acceptance criteria: NMT 14 ppm
• LEAD 〈251〉
Standard solution: Combine 5 mL of water, 0.50 mL of
standard lead solution TS, and 10 mL of Potassium Cya-
nide Solution (1 in 10) in a color-comparison tube.
Test preparation: Dissolve an amount equivalent to
0.25 g of zinc sulfate (ZnSO4) in 5 mL of water, and
transfer the solution to a similar, matched color-com-
parison tube. Add 10 mL of Potassium Cyanide Solution
(1 in 10), and allow the mixture to become clear.
Analysis: To the Standard solution and the Test prepara-
tion add 0.1 mL of sodium sulfide TS. Mix the contents
of each tube, and allow to stand for 5 min.
Acceptance criteria: Viewed downward over a white
surface, the Test preparation is not darker than the Stan-
dard solution (NMT 20 ppm of lead).
• ALKALIES AND ALKALINE EARTHS
Sample solution: Dissolve the equivalent of 1.12 g of
zinc sulfate (ZnSO4) in 150 mL of water contained in a
200-mL volumetric flask. Add sufficient ammonium sul-
fide TS to precipitate the zinc completely, and dilute
with water to volume. Pass through a dry filter, and
reject the first portion of the filtrate.
Analysis: To 100 mL of the Sample solution filtrate add a
few drops of sulfuric acid, evaporate to dryness in a
tared dish, and ignite to constant weight.
Official from May 1, 2016
Copyright (c) 2016 The United States Pharmacopeial Convention. All rights reserved.
Official Monographs / Zinc 6429
Acceptance criteria: The weight of the residue is NMT
5 mg (0.9%).
SPECIFIC TESTS
• ACIDITY
Sample solution: 28 mg/mL of zinc sulfate (ZnSO4)
Acceptance criteria: The Sample solution is not colored
pink by methyl orange TS.
ADDITIONAL REQUIREMENTS
• PACKAGING AND STORAGE: Preserve in tight containers.
• LABELING: The label indicates whether it is the monohy-
drate or the heptahydrate. Label any oral or parenteral
preparations containing Zinc Sulfate to state the content
of elemental zinc.
.
Zinc Sulfate Injection
DEFINITION
Zinc Sulfate Injection is a sterile solution of Zinc Sulfate in
Water for Injection. It contains NLT 90.0% and NMT
110.0% of the labeled amount of zinc (Zn).
IDENTIFICATION
• A. IDENTIFICATION TESTS—GENERAL, Zinc 〈191〉 and Sulfate
〈191〉: Meets the requirements
ASSAY
Change to read:
• PROCEDURE
[NOTE—The Standard solutions and the Sample solution
may be diluted quantitatively with water, if necessary,
to obtain solutions of suitable concentrations adaptable
USP Monographs
to the linear or working range of the instrument.]
Sodium chloride solution: 0.9 mg/mL of sodium chlo-
ride in water
Standard stock solution A: 10 mg/mL of zinc in water
prepared as follows. Transfer 3.11 g of zinc oxide to a
250-mL volumetric flask. Add 80 mL of 1 N sulfuric
acid, warm to dissolve, and cool. Dilute with water to
volume.
Standard stock solution B: 125 µg/mL of zinc in water,
from Standard stock solution A
Standard solution A: Transfer 2.0 mL of the Standard
stock solution B and 5 mL of Sodium chloride solution into
a 500-mL volumetric flask, and dilute with water
(0.50 µg/mL of zinc).
Standard solution B: Transfer 3.0 mL of the Standard
stock solution B and 5 mL of Sodium chloride solution into
a 500-mL volumetric flask, and dilute with water
(0.75 µg/mL of zinc).
Standard solution C: Transfer 4.0 mL of the Standard
stock solution B and 5 mL of Sodium chloride solution into
a 500-mL volumetric flask, and dilute with water (1.0
µg/mL of zinc).
Sample solution: Transfer a volume of Injection, equiv-
alent to 5 mg of zinc, to a 500-mL volumetric flask.
Dilute with water to volume. Transfer 10.0 mL of this
solution to a 100-mL volumetric flask. From the labeled
amount of sodium chloride, if any, in the Injection, cal-
culate the amount, in mg, of sodium chloride in the
10.0-mL portion and add sufficient Sodium chloride solu-
tion to bring the total sodium chloride content of the
100-mL volumetric flask to 0.9 mg. Dilute with water to
volume.
Instrumental conditions
(See •Atomic Absorption Spectroscopy 〈852〉.)• (CN 1-May-
.
2016)