Polacrilin Potassium - USPNF2024

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Printed on: Fri Jan 05 2024, 09:10:34 PM(EST) Status: Currently Official on 06-Jan-2024 DocId: GUID-A2CB3410-4938-494B-AB7C-4714570F541F_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: 73txn DOI: https://doi.org/10.31003/USPNF_M66040_05_01
1

has fumed off, moisten the residue with a few drops of


Polacrilin Potassium sulfuric acid, and ignite strongly. Allow to cool, transfer,
with the aid of water, to a 1000-mL volumetric flask, dilute
with water to volume, and mix. Transfer 1.00 mL of this
solution to a 100-mL volumetric flask, add 20.0 mL of
Diluted sodium solution, dilute with water to volume, and
mix gently to prevent foaming.
Instrumental conditions
Mode: Flame photometry
Analytical wavelength: 766 nm
Analysis
Samples: Standard solutions and Sample solution
Concomitantly determine the emittances of the Standard
solutions and Sample solution, adjusting the instrument
so that the most concentrated Standard solution gives a
reading near 100%.
2-Propenoic acid, 2-methyl-, potassium salt, polymer with Prepare a standard curve by plotting the readings from
diethenylbenzene; the Standard solutions versus the square root of the
Potassium methacrylate–divinylbenzene, copolymer potassium concentrations. From the curve, determine
CAS RN®: 65405-55-2. the concentration of potassium in the Sample solution.
Calculate the percentage of potassium in the portion of
DEFINITION sample taken:
Polacrilin Potassium is the potassium salt of a unifunctional

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low-cross-linked carboxylic cation-exchange resin prepared Result = (C O/C U) × 100
from methacrylic acid and divinylbenzene. When previously
dried at 105° for 6 h, it contains NLT 20.6% and NMT 25.1% CO = concentration of the Sample solution determined
of potassium (K). from the standard curve (µg/mL)
CU = concentration of Polacrilin Potassium in the
IDENTIFICATION
• A. SPECTROSCOPIC IDENTIFICATION TESTS á197ñ, Infrared
Spectroscopy: 197K
• B. IDENTIFICATION TESTS—GENERAL, Potassium á191ñ
ci Sample solution (µg/mL)

Acceptance criteria: 20.6%–25.1%


Sample solution A: Shake 1 g with 10 mL of water. IMPURITIES
Sample solution B: Shake 1 g with 10 mL of 0.1 N
ffi
hydrochloric acid. Change to read:
Analysis: Use the aqueous phase from Sample solution A and
• ▲IRON á241ñ, Procedures, Procedure 1▲ (CN 1-Jun-2023)
Sample solution B.
Acceptance criteria Sample: 0.10 g
Sample solution A: Does not meet the requirements Analysis: Transfer the Sample to a suitable crucible, and
Sample solution B: Meets the requirements ignite at a low heat until thoroughly ashed. Add to the
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carbonized mass 2 mL of nitric acid and 5 drops of sulfuric


ASSAY acid, and heat cautiously until white fumes are no longer
• CONTENT OF POTASSIUM evolved. Ignite, preferably in a muffle furnace, at 500°–
Sodium stock solution: 14.612 mg/mL of sodium chloride, 600°, until the carbon is completely burned off. Cool, add
previously dried at 125° for 30 min. This solution contains 4 mL of 6 N hydrochloric acid, cover, digest on a steam
5.76 mg/mL of sodium (Na). bath for 15 min, uncover, and slowly evaporate on a steam
Potassium stock solution: 745.5 µg/mL of potassium bath to dryness. Moisten the residue with 1 drop of
chloride, previously dried at 125° for 30 min. This solution hydrochloric acid, add 10 mL of hot water, and digest for
contains 391 µg/mL of potassium (K). 2 min. Dilute with water to 25 mL. Filter, if necessary. Rinse
Surfactant solution: Transfer 5.0 g of a suitable nonionic the crucible and the filter with 10 mL of water, combining
surfactant to a 250-mL beaker, add 200 mL of water, and the filtrate and rinsing in a 50-mL color-comparison tube,
stir to dissolve. Transfer this solution to a 500-mL volumetric add 2 mL of hydrochloric acid, dilute with water to 45 mL,
flask, dilute with water to volume, and mix. [NOTE—To and mix.
prevent foaming when using this solution, gently run the Acceptance criteria: NMT 0.01%
solution down the sides of the vessel, and use gentle action • LIMIT OF SODIUM
when mixing.] Sample solution: Transfer 2 g to a 400-mL borosilicate
Diluted sodium solution: Transfer 50.0 mL of Sodium stock beaker, add 20 mL of sulfuric acid, cover with a borosilicate
solution and 10.0 mL of Surfactant solution to a 100-mL watch glass, and heat until charring is complete. While
volumetric flask, dilute with water to volume, and mix continuing to heat the beaker, add 20 mL of nitric acid
gently to prevent foaming. dropwise. Continue to heat, and add nitric acid until all of
Standard solutions: To three separate 500-mL volumetric the organic material has been destroyed as indicated by the
flasks transfer, respectively, 3.0-, 4.0-, and 5.0-mL contents of the beaker turning from brown to a very pale
portions of Potassium stock solution. To each flask add straw-colored or colorless solution. Continue to evaporate
50.0 mL of Sodium stock solution and 10.0 mL of Surfactant the solution, and if it turns brown during the evaporation,
solution, dilute with water to volume, and mix gently to add nitric acid dropwise until the brown color disappears.
prevent foaming. Each mL of these solutions contains Evaporate just to dryness, cool, and dissolve the residue in
2.346, 3.128, and 3.910 µg of K, respectively. 40 mL of water and 10 mL of 6 N hydrochloric acid. Heat
Sample solution: Transfer 1.4 g of Polacrilin Potassium, to boiling, cool, transfer to a 100-mL volumetric flask, dilute
previously dried, to a 50-mL silica crucible, moisten with with water to volume, and mix.
4 mL of sulfuric acid, heat over a small flame until the acid

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Printed on: Fri Jan 05 2024, 09:10:34 PM(EST) Status: Currently Official on 06-Jan-2024 DocId: GUID-A2CB3410-4938-494B-AB7C-4714570F541F_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: 73txn DOI: https://doi.org/10.31003/USPNF_M66040_05_01
2

Standard solutions: To three separate 100-mL volumetric concentration. From this standard curve, determine the
flasks add, respectively, 1.00, 2.00, and 3.00 mL of a sodium content in the sample taken.
solution containing 254.2 mg of sodium chloride in Acceptance criteria: NMT 0.20%
1000 mL of water. Add water to volume, and mix to obtain
sodium chloride solutions having concentrations equivalent SPECIFIC TESTS
to 1, 2, and 3 µg/mL of Na, respectively. • POWDER FINENESS á811ñ
Instrumental conditions Sample: 4 g
Mode: Flame photometry Analysis: Transfer the Sample to a No. 100 standard sieve
Analytical wavelength: 589 nm placed on top of a No. 200 standard sieve and pan. Using a
Analysis soft 2-cm brush, brush the sample lightly across the No.
Samples: Standard solutions and Sample solution 100 sieve until no more particles pass through. By brushing
Adjust the instrument so that the emission of the Standard and tapping, dust off the particles on the underside of the
solution with a concentration of 3 µg/mL reads close to No. 100 sieve into the No. 200 sieve. Obtain the weight of
100% at 589 nm. the material retained on the No. 100 sieve. Similarly,
Determine the readings of the three Standard solutions at determine the weight of material retained by the No. 200
589 nm. Readjust the wavelength setting to 580 nm, and sieve.
determine the background emission reading for one of Acceptance criteria: NMT 1.0% is retained on the No. 100
these Standard solutions. sieve, and NMT 30.0% is retained on the No. 200 sieve.
Pipet 5 mL of the Sample solution into a 100-mL volumetric • LOSS ON DRYING á731ñ
flask, add water to volume, and mix. Observe the emission Analysis: Dry at 105° for 6 h.
reading of this solution at 589 nm, using the same Acceptance criteria: NMT 10.0%
instrument settings, then readjust the wavelength setting ADDITIONAL REQUIREMENTS
to 580 nm, and observe the background emission

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• PACKAGING AND STORAGE: Preserve in well-closed
reading. containers.
Subtract the corresponding background readings from the • USP REFERENCE STANDARDS á11ñ
readings of Standard solutions and Sample solution. USP Polacrilin Potassium RS
Prepare a standard curve by plotting the corrected Standard
solution readings versus the square root of the sodium
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