11/7/2020 USP-NF Polyvinyl Alcohol

Printed on: Sat Nov 07 2020, 16:03:37 pm

Printed by: Shruti Kharidia
O cial Status: Currently O cial on 07-Nov-2020
O cial Date: O cial as of 1-May-2020
Document Type: USP & NF
DocId: 1_GUID-294AEB93-6C94-45BA-B4DD-DFC666C2EB11_6_en-US
Printed from: https://online.uspnf.com/uspnf/document/1_GUID-294AEB93-6C94-45BA-B4DD-DFC666C2EB11_6_en-US
© 2020 USPC

Polyvinyl Alcohol

(C2H4O)n
Ethenol, homopolymer;
Vinyl alcohol polymer
[9002-89-5].

DEFINITION
Polyvinyl Alcohol is a water-soluble synthetic resin, represented by the formula (C2H4O)n, in which the average value of n lies between
500 and 5000. It is prepared by 85%–89% hydrolysis of polyvinyl acetate. The apparent viscosity, in mPa · s, at 20°, of a 4% (w/w)
aqueous solution is NLT 85.0% and NMT 115.0% of that stated on the label.

IDENTIFICATION
Change to read:
• A. ▲SPECTROSCOPIC IDENTIFICATION TESTS 〈197〉, Infrared Spectroscopy: 197K▲ (ERR 1-May-2020)
• B. It meets the requirements in the test Viscosity—Capillary Methods 〈911〉, Viscosity—Rotational Methods 〈912〉, or Viscosity—Rolling
Ball Method 〈913〉.
• C.

L
Sample solution: Dissolve 0.5 g of Polyvinyl Alcohol in 10 mL of water, with heat if necessary, and let the solution cool to room
temperature.
IA
Analysis 1: Transfer 5 mL of the Sample solution to a test tube, add 1 drop of iodine TS, mix, and allow to stand.
Acceptance criteria 1: A dark red to blue color is produced.
Analysis 2: Transfer 2 mL of the remaining Sample solution to a test tube, add 10 ml of Alcohol, and mix.
Acceptance criteria 2: A white, turbid, or occulent precipitate is formed.
IC

IMPURITIES
• RESIDUE ON IGNITION 〈281〉: NMT 1.0%
• WATER-INSOLUBLE SUBSTANCES
Analysis: Wash the tared 100-mesh screen used in the test for Viscosity immediately after with two 25-mL portions of water, and dry
FF

at 110° for 1 h.
Acceptance criteria: NMT 6.4 mg of water-insoluble substances are found (corresponding to NMT 0.1%).
• LIMIT OF METHANOL (METHYL ALCOHOL) AND METHYL ACETATE
Standard solution: In a 100-mL screw-cap bottle, prepare a 100-mL solution containing 0.24 µL/mL of USP Methyl Alcohol RS and 0.24
µL/mL of USP Methyl Acetate RS. Add 30 µL of USP Acetone RS to the screw-cap bottle. Close the bottle tightly with the screw cap,
and heat it in a water bath, stirring continuously. Remove the bottle from the water bath, and allow it to cool to room temperature.
O

Sample solution: Transfer a quantity of Polyvinyl Alcohol, equivalent to 2.0 g on the dried basis, to a 100-mL screw-cap bottle, and add
a magnetic stirrer. Add 98 mL of water and 30 µL of USP Acetone RS. Close the bottle tightly with the screw cap, and heat it in a
water bath, stirring continuously. Once the solution becomes clear, remove the bottle from the water bath, and allow it to cool to
room temperature.
Chromatographic system
(See Chromatography 〈621〉, System Suitability.)
Mode: GC
Detector: Flame ionization
Column: 3.2-mm × 2-m glass, phase S3
Temperatures
Injection port: 160°
Column: 160°
Detector: 160°
Carrier gas: Nitrogen
Flow rate: 30 mL/min
Injection volume: 0.4 µL
System suitability
Sample: Standard solution

https://online.uspnf.com/uspnf/document/1_GUID-294AEB93-6C94-45BA-B4DD-DFC666C2EB11_6_en-US?source=TOC 1/3
11/7/2020 USP-NF Polyvinyl Alcohol

Suitability requirements
Relative standard deviation: NMT 2.0%
Analysis
Samples: Standard solution and Sample solution
Calculate the percentages of methanol and methyl acetate in the portion of Polyvinyl Alcohol taken:

Result = (RU/RS) × (CS/W) × V × D × F × 100

RU = peak response ratio of the methanol or methyl acetate peak relative to the acetone peak from the Sample solution

RS = peak response ratio of the methanol or methyl acetate peak relative to the acetone peak from the Standard solution

CS = concentration of methanol (methyl alcohol) or methyl acetate in the Standard solution (µL/mL)

W = weight of Polyvinyl Alcohol on the dried basis taken to prepare the Sample solution (g)

V = volume of the Sample solution, 100 mL

D = density of methanol (methyl alcohol) or methyl acetate, 0.79 and 0.93 g/mL, respectively

F = conversion factor, 10−3 mL/µL

Acceptance criteria
Methanol (methyl alcohol): NMT 1.0%
Methyl acetate: NMT 1.0%

SPECIFIC TESTS
• LOSS ON DRYING 〈731〉
Analysis: Dry at 110° to constant weight.
Acceptance criteria: NMT 5.0%
• VISCOSITY—CAPILLARY METHODS 〈911〉, VISCOSITY—ROTATIONAL METHODS 〈912〉, or VISCOSITY—ROLLING BALL METHOD 〈913〉

L
Sample: After performing Loss on Drying, weigh undried Polyvinyl Alcohol, equivalent to 6.00 g on the dried basis.
Analysis: Over a period of seconds, transfer the Sample with continuous slow stirring to 140 mL of water contained in a suitable tared
IA
ask. When the specimen is well wetted, increase the rate of stirring, avoiding mixing in excess air. Heat the mixture to 90°, and
maintain the temperature at 90° for about 5 min. Discontinue heating, and continue stirring for 1 h. Add water to make the mixture
weigh 150 g. Resume stirring to obtain a homogeneous solution. Filter the solution through a tared 100-mesh screen into a 250-mL
conical ask, cool the ltrate to 15°, mix, and proceed as directed in the chapter. Determine its viscosity at 20 ± 0.1°, using an
appropriate viscometer.
IC

Acceptance criteria: 85.0%–115.0% of the labeled value.

• PH 〈791〉
Sample solution: 40 mg/mL
Acceptance criteria: 5.0–8.0
FF

• DEGREE OF HYDROLYSIS
Sample: 1 g of Polyvinyl Alcohol, previously dried at 110° to constant weight
Analysis: Transfer the Sample to a wide-mouth, 250-mL conical ask tted by means of a suitable glass joint to a re ux condenser.
Add 35 mL of dilute methanol (3 in 5), and mix gently to ensure complete wetting of the solid. Add 3 drops of phenolphthalein TS,
and add 0.2 N hydrochloric acid or 0.2 N sodium hydroxide if necessary, to neutralize. Add 25.0 mL of 0.2 N sodium hydroxide VS,
and re ux gently on a hot plate for 1 h. Wash the condenser with 10 mL of water, collecting the washings in the ask, cool, and
O

titrate with 0.2 N hydrochloric acid VS. Concomitantly perform a blank determination in the same manner, using the same quantity
of 0.2 N sodium hydroxide VS.
Calculation of saponi cation value: Calculate the saponi cation value:

Result = [(VB − VS) × N × Mr]/W

VB = volume of 0.2 N hydrochloric acid VS consumed in the titration of the blank (mL)

VS = volume of 0.2 N hydrochloric acid VS consumed in the titration of the Sample solution (mL)

N = actual normality of hydrochloric acid VS

Mr = molecular weight of potassium hydroxide, 56.11

W = weight of the portion of Polyvinyl Alcohol taken (g)

Calculation of degree of hydrolysis: Calculate the degree of hydrolysis, expressed as a percentage of hydrolysis of polyvinyl
acetate:

Result = 100 − [7.84 × S/(100 − 0.075 × S)]

https://online.uspnf.com/uspnf/document/1_GUID-294AEB93-6C94-45BA-B4DD-DFC666C2EB11_6_en-US?source=TOC 2/3
11/7/2020 USP-NF Polyvinyl Alcohol
S = saponi cation value of the Polyvinyl Alcohol

Acceptance criteria: 85%–89%

• ACID VALUE
Sample: 10.0 g
Analysis: Add 200 mL of water to a borosilicate round-bottom ask attached to a re ux condenser. Heat the water on a water bath
with constant stirring. Add the Sample to the water, and continue heating for 30 min with continuous stirring. Remove the ask from
the water bath, and continue stirring until room temperature is reached. Quantitatively transfer this solution to a 250-mL volumetric
ask, dilute with water to volume, and mix. Add 0.5 mL of phenolphthalein TS to 50 mL of this solution, and titrate with 0.05 N
potassium hydroxide VS until the pink color persists for 15 s.
Calculate the acid value:

Result = D × Mr × [(N × V)/W]

D = dilution factor

Mr = molecular weight of potassium hydroxide, 56.11

N = normality of potassium hydroxide VS used

V = volume of 0.05 N potassium hydroxide used (mL)

W = weight of the Sample (g)

Acceptance criteria: NMT 3.0

ADDITIONAL REQUIREMENTS
• PACKAGING AND STORAGE: Preserve in well-closed containers, and store at room temperature in a dry place.
• LABELING: Label it to indicate the viscosity, giving the viscosity measurement parameters, the concentration of the solution, and the type
of equipment used.
• USP REFERENCE STANDARDS 〈11〉
USP Acetone RS
USP Methyl Acetate RS
L
IA
USP Methyl Alcohol RS
USP Polyvinyl Alcohol RS
IC

Auxiliary Information- Please check for your question in the FAQs before contacting USP.

Topic/Question Contact Expert Committee

POLYVINYL ALCOHOL Sean P Delaney CE2020 Complex Excipients

FF

Assistant Scienti c Liaison

Chromatographic Database Information: Chromatographic Database

O

Most Recently Appeared In:

Pharmacopeial Forum: Volume No. 33(6)

Page Information:

USP43-NF38 - 3593
USP42-NF37 - 3566
USP41-NF36 - 3352

Current DocID: GUID-294AEB93-6C94-45BA-B4DD-DFC666C2EB11_6_en-US

https://online.uspnf.com/uspnf/document/1_GUID-294AEB93-6C94-45BA-B4DD-DFC666C2EB11_6_en-US?source=TOC 3/3