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Plant – II, Alathur No: RST: RME 0013
apex RAW MATERIAL SPECIFICATION & Mat.Code: RME 0013
STANDARD TEST PROCEDURE Revision No.: 01
Effective date:
Material: POVIDONE IP
Review Period:

`1.0 SAMPLING AND HANDLING:

1.1 Storage conditions:

Store in airtight containers.

1.2 Precautions, Handling hazards & Special instructions for sampling if any:

Do not expose the material to moisture.

1.3 Total Quantity of Composite sample required for analysis:

30 grams

1.4 Quantity of Reserve sample:

2 x 30grams

1.5 Sampling Instructions:

Follow the Standard operating procedure number: QCGN:022

1.6 Destruction Instructions:

Follow the Standard operating procedure number: QCGN:028

1.7 Retest period:

12 months from the date of release.

1.8 Synonym/Brand Name:

Polyvinylpyrrolidone,Polyvidone.

1.9 Type of Material:

Excipient
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 apex laboratories private limited Page No.: 2 of 9
Plant – II, Alathur No: RST: RME 0013
apex RAW MATERIAL SPECIFICATION & Mat.Code: RME 0013
STANDARD TEST PROCEDURE Revision No.: 01
Effective date:
Material: POVIDONE IP
Review Period:

2.0 INSTRUMENTS REQUIRED:

2.1 Auto titrator

2.2 Muffle Furnace

2.3 Analytical Balance

2.4 FT-IR

2.5 pH meter

2.6 Capillary viscometer

3.0 CHEMICALS REQUIRED:

3.1 Ethanol.

3.2 Dimethylaminobenzaldehyde reagent.

3.3 Hydrochloric acid.

3.4 Sodium hydroxide

3.5 0.05 M Iodine

3.6 Hydrogen peroxide.

3.7 0.1 M Sodium thiosulphate

4.0 GLASSWARE REQUIRED:

4.1 100 ml beaker.

4.2 50 ml measuring cylinder.

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 apex laboratories private limited Page No.: 3 of 9
Plant – II, Alathur No: RST: RME 0013
apex RAW MATERIAL SPECIFICATION & Mat.Code: RME 0013
STANDARD TEST PROCEDURE Revision No.: 01
Effective date:
Material: POVIDONE IP
Review Period:

4.3 5 ml,10 ml Pipette.

4.4 Flat-bottomed test-tube.

4.5 50 ml burette.

4.6 100 ml, 250 ml conical flask.

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 apex laboratories private limited Page No.: 4 of 9
Plant – II, Alathur No: RST: RME 0013
apex RAW MATERIAL SPECIFICATION & Mat.Code: RME 0013
STANDARD TEST PROCEDURE Revision No.: 01
Effective date:
Material: POVIDONE IP
Review Period:

5.0 STANDARD SPECIFICATIONS:

S.No TEST SPECIFICATION METHODS

A White or yellowish-white powder
1.0 Description* or flakes.odourless or almost IP Follow 6.1
odourless ,hygroscopic.
2.0 Solubility Freely soluble in water, ethanol
(95.0%) and Chloroform, IP Follow 6.2
Practically in soluble in ether.
3.0 Identification:* First Identification: A and D
Second Identification:B,C and D
Concordant with the reference
IP Follow 6.3
Test A: IR Spectrum spectrum of Povidone.
Test B, C&D: Chemical
Should comply
reaction
4.0 Appearance of solution* Should comply IP Follow 6.4
5.0 Heavy metals Not more than 10 ppm IP Follow 6.5
6.0 Aldehydes (Acetaldehyde) Not more than 9.1 ml IP Follow 6.6
7.0 Vinyl pyrrolidone Not more than 3.6 ml IP Follow 6.7
8.0 Sulphated ash Not more than 0.1% w/w IP Follow 6.8
9.0 Water* Not more than 5.0%w/w IP Follow 6.9
Viscosity
10.0 IP Follow 6.10
(expressed as K-value)
11.0 Nitrogen*
11.5 % to 12.8 % w/w IP Follow 6.11
-on anhydrous basis

* Tests to be performed on Retesting.

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 apex laboratories private limited Page No.: 5 of 9
Plant – II, Alathur No: RST: RME 0013
apex RAW MATERIAL SPECIFICATION & Mat.Code: RME 0013
STANDARD TEST PROCEDURE Revision No.: 01
Effective date:
Material: POVIDONE IP
Review Period:

6.0 STANDARD TEST PROCEDURE:

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Plant – II, Alathur No: RST: RME 0013
apex RAW MATERIAL SPECIFICATION & Mat.Code: RME 0013
STANDARD TEST PROCEDURE Revision No.: 01
Effective date:
Material: POVIDONE IP
Review Period:

6.1 DESCRIPTION:

A White or yellowish-white powder or flakes, odourless or almost odourless,hygoscopic.

6.2 SOLUBILITY:

Procedure Observation Result

1.0 g of sample + 1ml of water If the material doesn’t dissolve
Add further 9ml of water in
If the material dissolved Freely soluble
portions.
1.0 g of sample + 1ml of ethanol If the material doesn’t dissolve
Add further 9ml of ethanol in
If the material dissolved Freely soluble
portions.
1.0g of sample + 1ml of
If the material doesn’t dissolve
Chloroform.
Add further 9ml of Chloroform in
If the material dissolved Freely soluble
portions.
10 mg of sample + 100 ml of Practically
If the material doesn’t dissolved
ether. insoluble

6.3 IDENTIFICATION:

Test A: By FTIR:< GAM0004>

Determine by infrared Spectrophotometry.Compare the spectrum with that obtained with

Povidone RS.

Test B:

Add 2.5 g in small portions to a suitable volume of carbon dioxide-free water, stirring with a
magnetic stirrer, and dilute to 25 ml with the same solvent (solution A). To 0.4 ml of solution
A add 10 ml of water, 5 ml of 2M hydrochloric acid and 2 ml of potassium dichromate
solution; an orange-yellow precipitate is produced.
Test: C:

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 apex laboratories private limited Page No.: 7 of 9
Plant – II, Alathur No: RST: RME 0013
apex RAW MATERIAL SPECIFICATION & Mat.Code: RME 0013
STANDARD TEST PROCEDURE Revision No.: 01
Effective date:
Material: POVIDONE IP
Review Period:

To 1 ml of solution A add 0.2 ml of Dimethylaminobenzaldehyde reagent and 0.1 ml of

Sulphuric acid; a pink colour is produced.

Test: D: ( test to be performed for individual container)

To 0.1 ml of solution A add 5 ml of water and 0.2 ml of 0.05M iodine; a red colour is
produced.

6.4 APPEARANCE OF SOLUTION:< GAM 0007>

Solution A is clear and not more intensely coloured than reference solution BS6 or BYS6.

6.5 HEAVY METALS: Limit: Not more than 10 ppm

Test solution: In a silica crucible, mix thoroughly 2.0g of the sample with 0.5 g of
magnesium oxide. Ignite to dull red until a homogeneous white or greyish white mass is
produced. Heat at 800º for about 1 hour ,dissolve the residue using two quantities, each of 5
ml, of 5 M hydrochloric acid, add 0.1 ml of phenolphthalein solution and strong ammonia
solution until a pink colour is produced. Cool, add glacial acetic acid until the solution is
decolorised and add a further 0.5 ml of glacial acetic acid. Filter if necessary and dilute the
solution to 20 ml with water.

Reference solution (standard): Prepare as described for the test solution using the 2ml of
lead standard solution (10 ppm Pb) instead of the sample .

Blank solution:  A mixture of 10 ml of water and 2 ml of the test solution.

Procedure : To 12 ml of each solution, add 2 ml of acetate buffer solution pH 3.5. Mix, add
1.2 ml of thioacetamide reagent, mix immediately and allow to stand for 2 minutes. The test
is invalid if the reference solution does not show a brown colour compared to the blank
solution.

Inference: The sample complies with the test if any brown colour in the test solution is not
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Plant – II, Alathur No: RST: RME 0013
apex RAW MATERIAL SPECIFICATION & Mat.Code: RME 0013
STANDARD TEST PROCEDURE Revision No.: 01
Effective date:
Material: POVIDONE IP
Review Period:

more intense than that in the reference solution.

6.6 ALDEHYDES ( ACETALDEHYDE):

Boil 20.0 g in 180 ml of a 25% v/v solution of sulphuric acid in a ground-glass-stoppered

flask under a reflux condenser for 45 minutes and allow to cool. Fit a distillation head, distil
and collect 60 ml of the distillate in 20 ml of a 7.0% w/v solution of hydroxylamine
hydrochloride, previously adjusted to pH 3.1 using 1M sodium hydroxide, and cooled in ice.
Titrate with 0.1M sodium hydroxide to pH 3.1. Perform a blank determination .

Limit: Not more than 9.1 ml of 0.1M sodium hydroxide is required.(0.2% calculated as
aldehyde)

6.7 VINYLPYRROLIDONE:

Dissolve 10.0 g in 80 ml of water and add 1 g of   sodium acetate. Titrate with 0.05M iodine
until a persistent colour is obtained and add a further 3.0 ml of the iodine solution. Allow to
stand for 10 minutes and titrate the excess of iodine with 0.1M sodium thiosulphate using 3
ml of starch solution, added towards the end of the titration, as indicator. Repeat the
operation without the substance being examined using the same total volume of 0.05M
iodine. The difference between the titrations represents the amount of iodine consumed by
the vinylpyrrolidone monomer that may be present.
Limit:Not more than 3.6 ml of 0.05 M iodine is required.( 0.2%)

6.8 SULPHATED ASH :< GAM 0013>

Determined on 1.0 g of the substance.

Limit: Not more than 0.1%

6.9 WATER: < GAM0012>

Not more than 5.0% determined on 0.5 g.

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 apex laboratories private limited Page No.: 9 of 9
Plant – II, Alathur No: RST: RME 0013
apex RAW MATERIAL SPECIFICATION & Mat.Code: RME 0013
STANDARD TEST PROCEDURE Revision No.: 01
Effective date:
Material: POVIDONE IP
Review Period:

6.10 VISCOSITY, EXPRESSED AS K-VALUE: < GAM0030>

Dissolve 1.0 g of sample in 100 ml of water. Allow to stand for 1 hour and determine the
viscosity of the solution at 25 ±°C, using viscometer No.1 with a minimum flow time of 100
seconds.. Calculate the K-value from the expression:

Where,

c = concentration of the sample, calculated with reference to the anhydrous substance, in

grams per 100 ml. => C = Weight of sample in g x (100 – Water)
100

Z = viscosity of the solution relative to that of water.

6.11 Nitrogen content : Perform in duplicate

Weigh accurately 0.3 g of the substance , equivalent to about 15 mg of nitrogen into a 200-ml
long-necked flask and add 1g of a powdered mixture of 10 parts of anhydrous sodium
sulphate or potassium sulphate and 1 part of cupric sulphate. Add 11 ml of nitrogen-free
sulphuric acid, mix and carefully. For complete destruction of organic matter,add hydrogen
peroxide ofd 10 vol of until a clear,light green solution is obtained,then heat for further 4
hours. Cool, carefully add 20 ml of water-cool again and connect the flask to a distillation
apparatus.

Add 50 ml of 10M sodium hydroxide and distill immediately by passing steam through the
flask. Collect the distillate in 25.0 ml of 0.1 M hydrochloric acid and titrate the excess of
acid with 0.1 M sodium hydroxide using methyl red-methylene blue solution as indicator.
Repeat the operation using 0.025 g of anhydrous dextrose in place of the substance being
examined. The difference between the titrations represents the ammonia liberated by the
substance being examined. Each ml of 0.1M hydrochloric acid is equivalent to 0.001401 g of
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 apex laboratories private limited Page No.: 10 of 9
Plant – II, Alathur No: RST: RME 0013
apex RAW MATERIAL SPECIFICATION & Mat.Code: RME 0013
STANDARD TEST PROCEDURE Revision No.: 01
Effective date:
Material: POVIDONE IP
Review Period:

Nitrogen.
 
Blank: Repeat the test using about 0.025 g of anhydrous dextrose in place of the substance
to be examined.

Variation for duplicate results: NMT1.0% Declare the are

average
thetheassay.

7.0 REVISION HISTORY:

Date of Revision Change Effective

Changes Made
Revision No. Control No. Date

NA 00 New NA

Revised to correct the volume

01 of ethanol and chloroform in the 09/112
solubility test.

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