Ethylene Glycol and Vinyl Alcohol Graft Copolymer
Polyethylene glycol-graft-polyvinyl alcohol;
Graft-copoly(ethylene glycol-vinyl alcohol) [121786-16-1].
Ethylene Glycol and Vinyl Alcohol Graft Copolymer is a graft copolymer of ethylene glycol and vinyl alcohol. It consists of about 75% of vinyl alcohol (CH2CH(OH)) units and 25% of ethylene glycol (CH2CH2O) units. The Copolymer is produced by using polyethylene glycol and vinyl acetate as starting materials. Polyethylene glycol forms the polymer backbone on which polyvinyl acetate is grafted. Hydrolysis of polyvinyl acetate side chains leads to formation of polyvinyl alcohol grafted chains. Ethylene Glycol and Vinyl Alcohol Graft Copolymer may contain glidant to improve flowability.
• Infrared Absorption
Sample: 200 mg of Ethylene Glycol and Vinyl Alcohol Graft Copolymer
Analysis: Dissolve the Sample in 510 mL of water. Spread 1 mL of this solution on a thallium bromoiodide window.1 Totally moisten the surface area of the window. Dry the window at 110 for approximately 30 min, and allow the window to cool to room temperature.
Acceptance criteria: The IR absorption spectrum of Ethylene Glycol and Vinyl Alcohol Graft Copolymer exhibits maxima corresponding to the same wavelengths as those of a similar preparation of USP Ethylene Glycol and Vinyl Alcohol Graft Copolymer RS treated in the same manner.
• Residue on Ignition 281
Sample: 10.0 g
Acceptance criteria: NMT 3.0%
• Procedure 1: Ethylene Oxide and Dioxane
[CautionEthylene oxide is toxic and flammable. Prepare these solutions in a well-ventilated fume hood, using great care. Protect both hands and face by wearing polyethylene protective gloves and an appropriate face mask. Store all solutions in hermetic containers, and refrigerate at a temperature between 4 and 8. ]
[NoteBefore using polyethylene glycol 200 in this test, remove any volatile components from it by placing 500 mL of polyethylene glycol 200 in a 1000-mL round-bottom flask, and attaching the flask to a rotary evaporator maintained at a temperature of 60 and under a vacuum of 1020 mm Hg for 6 h. ]
Acetaldehyde solution: 10 µg/mL of acetaldehyde. [NotePrepare the Acetaldehyde solution immediately before use. ]
Ethylene oxide stock solution: Introduce 300 µL (corresponding to 250 mg) of gaseous ethylene oxide to the polyethylene glycol 200. Determine the absorbed mass of ethylene oxide via the weight of the solution before and after the absorption. Dilute the solution with the polyethylene glyol 200 to 100 g. This stock solution contains 2.5 mg/g of ethylene oxide. [NotePrepare this stock solution immediately before use, and store in a refrigerator after preparation. ]
Ethylene oxide solution: 100 µg/g of ethylene oxide in polyethylene glycol 200 from Ethylene oxide stock solution. Transfer 5 g of 100 µg/g ethylene oxide in polyethylene glycol 200 to a 50-mL volumetric flask filled with 30 mL of water. Dilute with water to volume, and mix to obtain a solution containing 10 µg/mL of ethylene oxide. [NotePrepare this solution immediately before use, and use the solution directly after preparation. ]
Dioxane solution: 500 µg/mL of dioxane
Standard solution A: Transfer 0.1 mL of Ethylene oxide solution to a 10-mL pressure headspace vial. [NoteOther sizes, such as 22-mL, may be used, depending on the operating conditions; however, the same size must be used for Standard solution A, Standard solution B, and the Sample solution. ] Add 0.1 mL of Acetaldehyde solution and 0.1 mL of Dioxane solution, seal the vial, and mix.
Standard solution B: Transfer 1.0 g of Ethylene Glycol and Vinyl Alcohol Graft Copolymer to a 10-mL pressure headspace vial. Add 0.1 mL of Ethylene oxide solution, 0.1 mL of Dioxane solution, and 1.0 mL of N,N-dimethylacetamide, seal the vial, and mix.
Sample solution: Transfer 1.0 g of Ethylene Glycol and Vinyl Alcohol Graft Copolymer to a 10-mL pressure headspace vial. Add 1.0 mL of N,N-dimethylacetamide and 0.2 mL of water, seal the vial, and mix.
[NoteUse a headspace apparatus that automatically transfers a measured amount of headspace. ]
Detector: Flame ionization
Detector temperature: 250
Column: 0.25-mm × 30-m glass or quartz capillary column; 1.0-µm layer of phase G1
Column temperature: See the temperature program table below.
Carrier gas: Helium
Flow rate: 0.8 mL/min
Injection size: 1 mL (the gaseous headspace)
Injection type: Split ratio 20:1
Injection port temperature: 250
Equilibration time: 45 min
Standard solution A: 70
Standard solution B: 90
Sample solution: 90
Transfer line temperature: 150
Pressurization time: 1 min
Final headspace pressure: 0.7 bar
Injection time: 12 s
Sample: Standard solution A
[NoteThe relative retention times for acetaldehyde and ethylene oxide are 0.94 and 1.0, respectively. ]
Resolution: NLT 1.5 between acetaldehyde and ethylene oxide
Signal-to-noise: NLT 5 determined from the dioxane peak
Relative standard deviation: NMT 15%
Samples: Standard solution B and Sample solution
Calculate the content of ethylene oxide, in ppm, in the portion of Ethylene Glycol and Vinyl Alcohol Graft Copolymer taken:
Result = AE × rU/[(rS × WU) (rU × WS)]
Calculate the content of dioxane, in ppm, in the portion of Ethylene Glycol and Vinyl Alcohol Graft Copolymer taken:
Result = AD × rU/[(rS × WU) (rU × WS)]
Acceptance criteria: NMT 1 ppm of ethylene oxide; NMT 10 ppm of dioxane
• Procedure 2: Vinyl Acetate
Solution A: Acetonitrile, methanol, and water (5:5:90)
Solution B: Acetonitrile, methanol, and water (45:5:50)
Mobile phase: See the gradient table below.
System suitability solution: Transfer 50 mg of vinyl acetate and 50 mg of 1-vinylpyrrolidin-2-one to a 50-mL volumetric flask, add 10 mL of methanol, and sonicate or gently shake the flask to dissolve the materials. Dilute with Solution A to volume. Dilute 10 mL of this solution with Solution A to 100 mL. Dilute 5 mL of this solution with Solution A to 100 mL. The System suitability solution contains about 5 µg/mL each of vinyl acetate and 1-vinylpyrrolidin-2-one.
Standard solution: Transfer 50 mg of vinyl acetate to a 100-mL volumetric flask, dissolve in and dilute with methanol to volume, and mix well. Dilute 5.0 mL of the solution with Solution A to 100 mL. Dilute 10.0 mL of this solution with Solution A to 100 mL. The Standard solution contains about 2.5 µg/mL of vinyl acetate. [NoteThis solution should be analyzed within 1 h when stored at room temperature. ]
Sample solution: Transfer 250 mg of Ethylene Glycol and Vinyl Alcohol Graft Copolymer to a 10-mL volumetric flask, and add 12 mL of methanol, using an ultrasonic bath if necessary. After cooling to ambient temperature, dilute with water to volume, and mix. Pass through a 0.2-mm membrane filter. [NoteThis solution should be analyzed within 1 h when stored at room temperature. ]
Detector: UV 205 nm
Column: 4.0-mm × 25-cm analytical column; 5-µm packing L1. A 4.0-mm × 3-cm pre-column; 5-µm packing L1 may be used if a matrix effect is observed. [NoteThe matrix effect may result in poor reproducibility of the retention times and of the peak shapes. ]
Column temperature: 30
Flow rate: 1 mL/min
Injection size: 10 µL
Sample: System suitability solution
[NoteThe relative retention times for vinyl acetate and 1-vinylpyrrolidin-2-one are 1.0 and 1.4, respectively. ]
Resolution: NLT 5.0 between vinyl acetate and 1-vinylpyrrolidin-2-one
Relative standard deviation: NMT 5.0% determined from the 1-vinylpyrrolidin-2-one peak
Samples: Standard solution and Sample solution
Acceptance criteria: The response of the vinyl acetate peak from the Sample solution is NMT that of the vinyl acetate peak from the Standard solution, corresponding to NMT 100 ppm of vinyl acetate.
• Procedure 3: Acetic Acid/Acetate
Mobile phase: 5 mM sulfuric acid
Standard solution: 0.3 mg/mL for each of acetic acid and citric acid in Mobile phase
Sample solution: 20 mg/mL of Ethylene Glycol and Vinyl Alcohol Copolymer
Detector: UV 205 nm
Column: 4.6-mm × 25-cm; 5-µm packing L1
Column clean: After each injection, rinse the column with a mixture of equal volumes of Mobile phase and acetonitrile.
Column temperature: Ambient
Flow rate: 1 mL/min
Injection size: 20 µL
Sample: Standard solution
[NoteThe relative retention times for acetic acid and citric acid are 1.0 and 1.3, respectively. ]
Resolution: NLT 2.0 between acetic acid and citric acid
Relative standard deviation: NMT 5.0% determined from the acetic acid peak
Samples: Standard solution and Sample solution
Acceptance criteria: The response of the acetic acid peak from the Sample solution is NMT that of the acetic acid peak from the Standard solution, corresponding to NMT 1.5% of acetic acid.
• Fats and Fixed Oils, Ester Value 401: 1075
• Loss on Drying 731: Dry 1.0 g of Ethylene Glycol and Vinyl Alcohol Graft Copolymer in a vacuum at 140 for 1 h: it loses NMT 5.0% of its weight.
• pH 791: 5.08.0, in a solution of 20% (w/w) in carbon dioxide-free water
• Viscosity 911: After determining the Loss on Drying, weigh a quantity of undried Ethylene Glycol and Vinyl Alcohol Graft Copolymer, equivalent to 100.0 g on the dried basis. Transfer the sample to a short form, 600-mL beaker (internal diameter about 80 mm and height 120 mm), and add water to make the mixture weigh 500 g. Ensure a homogeneous solution by gently stirring at room temperature for 48 h. Afterwards allow the container to stand for 24 h to let the entrapped air dissipate. [NoteEnsure that the concentration of this solution is 20% (w/w). ] Determine the viscosity of this solution at 23 ± 0.1 using a suitable rotational viscometer with a spindle having a cylinder 4.7 cm in diameter and 0.2 cm high attached to a shaft 0.3 cm in diameter, the distance from the top of the cylinder to the lower tip of the shaft being 2.7 cm, and the immersion depth being 4.9 cm.2 Operate the viscometer at 100 rpm. Follow the instrument manufacturer's directions to measure the apparent viscosity.
Acceptance criteria: 25250 mPa·s
• Packaging and Storage: Preserve in well-closed containers, and store at a temperature below 25.
• Labeling: Label it to indicate the viscosity, giving the viscosity measurement parameters, concentration of the solution, and the type of equipment used. The labeling also indicates the name and quantity of any added glidant.
• USP Reference Standards 11
USP Ethylene Glycol and Vinyl Alcohol Graft Copolymer RS
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