Global Standard Test Method Procedure

Title: Dispersion Test for Finished Goods

Procedure Number: GLO-QC-TM-0729 Content Revision Number: 11
Written by Neil Jones Departments: Global Quality Control & Technical Services
Page 1 of 6
The information contained in this document is proprietary to Colorcon and may not be used or disseminated inappropriately.

I. SCOPE: This SOP is effective at the following manufacturing sites:

All Sites No-Tox – US Bazainville – FR Shanghai – CN x
Dartford UK x Humacao – PR x Indianapolis – US Shizuoka - JP x
West Point US x Stoughton – US GOA - IN x Indaiatuba - BR x

II. INTRODUCTION The dispersion test involves evaluating a sample of the material itself or also evaluating
a hydrated mixture prepared from the sample (dry film coating systems).
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Some dry film coating systems contain a liquid ingredient that is introduced to the dry powder blend during the
manufacturing process. Inherently in this process, the formation of soft agglomerates or small flakes may
occur. This test outlines the methods and acceptance criteria in performing an evaluation to ensure the
product is dispersed adequately and considering some inherent physical variability that may be present from
the manufacturing process. A hydrated mixture best replicates the end usage of dry film coating systems. Dry
Pigment Blends and Liquid dispersions are simply evaluated as “neat” samples.

III. DEFINITIONS:
Retained Material: Material retained on a test sieve that is characteristic in color of the sample being
evaluated. This would not include undispersed pigment specks.
Foreign Matter: Anything found that is not inherent with the finished formulation or its ingredients.

IV. RESPONSIBILITIES: QC/Analyst/Technician: It is the responsibility of the analyst or technician to

perform the analysis according to this procedure.

V. OUTLINE OR FLOW CHART: N/A

VI. EQUIPMENT
■ 600 micrometer testing sieve (U.S. #30 Standard)
■ 150 micrometer testing sieve (U.S. #100 Standard)
■ 250 micrometer testing sieve (U.S. #60 Standard)

VII. SAFETY REQUIREMENTS:

■ Dye blend batches must be screened under a hood for dust-containment
■ Dust containment should be considered when dry sieving film coating systems
■ Gloves must be worn when contacting product
■ Coating mixtures prepared with organic solvents must be mixed under a hood

This document is valid at the time of distribution. Distributed automatically on 14-JUL-2022 (US EST)
 Global Standard Test Method Procedure
Title: Dispersion Test for Finished Goods
Procedure Number: GLO-QC-TM-0729 Content Revision Number: 11
Written by Neil Jones Departments: Global Quality Control & Technical Services
Page 2 of 6
The information contained in this document is proprietary to Colorcon and may not be used or disseminated inappropriately.

VIII. PROCEDURE:
A. USE OF TEST SIEVES
1. Verify that the sieve is within calibration/certification period prior to use.
2. Inspect test sieve prior to each use to ensure it is still in proper working condition
a. No residue from previous use is visible
b. No stretching or tearing of the wire mesh
c. If applicable, sieve gaskets (O-ring gaskets that fit on sieve flanges between test sieves to
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prevent sample or fluid loss during wet-sieving operations) are not cracked and seal
properly.
3. If the sieve is not in calibration/certification OR in proper working order, take sieve out of service
and inform Quality Management.
4. After each use, clean and dry sieve.
a. Dry sieve test - brush clean with a sieve brush.
b. Wet sieve test – rinse clean using water and use soft bristle brush if needed.
c. If further cleaning is required to remove residue, clean gently with a detergent soap, water
and a soft bristle brush. For deep cleaning the sieve can be placed in a sonicator bath with
a soap solution.
d. Dry sieve prior to further use.

B. DRY DISPERSION FILM COATING SYSTEMS

1. Dry Sieve Test (All Formulations)
a. Place about 100g of powder sample onto a 600-micrometer testing sieve (U.S. #30
Standard).
b. Manually shake sieve, allowing powder to fall through. Shake until all material has passed
through or until only retained material remains. Soft agglomerations as described in the
Introduction may be broken up by applying soft pressure with a gloved fingertip.
c. Examine retained material.
d. Guidelines for approval:
e. If all criteria pass, proceed to Section B-2 (Coating Mixture Test).
f. If one or more criteria fails, refer to notes in part g. below before proceeding further.

This document is valid at the time of distribution. Distributed automatically on 14-JUL-2022 (US EST)
 Global Standard Test Method Procedure
Title: Dispersion Test for Finished Goods
Procedure Number: GLO-QC-TM-0729 Content Revision Number: 11
Written by Neil Jones Departments: Global Quality Control & Technical Services
Page 3 of 6
The information contained in this document is proprietary to Colorcon and may not be used or disseminated inappropriately.

Criteria PASS (all must apply) FAIL (one or more applies – see note (1))
Foreign Matter None Present

Undispersed ingredients
(Pigments/other ingredients in Not more than 5 specks (See note (2)) >5 specks
the formula)
Small, soft agglomerates, typically uniform in
size, break up easily with slight fingertip Hard pieces that do not break up at all
pressure
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Retained Material Particles do not dissolve/disperse in

Non-uniform lumps, aggregates, hard pieces,
(see notes (3), (4) and (5)) recommended solvent
etc. that do not break up easily BUT
dissolve/disperse in recommended solvent as
per the reconstitution sheet Unusually large lumps

g. Notes to Approval Guidelines:

(1) A sample with a failing result during the Colorcon internal manufacturing process
shall have additional processing to fix the product dispersion uniformity.
(2) Undispersed ingredients and Retained Material: If greater than 5 specks or
particles that are not uniform in size persist after several attempts of additional
processing according to internal Colorcon work instructions, then proceed to
Section B-2 and assess a hydrated mixture (Coating Mixture Test). A passing
result in Section B-2 is more indicative of the end application, so this result
overrides that of Section B-1.
(3) Retained Material (A): Oversized particles are seen in products containing some
small fine ‘grain-like’ particles of Sucrose, HPC, solid PEG, Methacrylic Acids or
Ethylcellulose, as well as lumps formed after the addition of liquid ingredients to the
dry product. For these reasons, it is not expected to see 100% of the product go
through the sieve.
(4) Retained Material (B): For Acryl-EZE® formulations, it is inherent in the product
that some small fine ‘grain-like’ particles will be present in the powder (Section B-1,
this test) and when the powder is hydrated (Section B-2). Colorcon’s coating
mixture preparation recommendations for Acryl-EZE products includes filtering
prepared mixtures through a 250-micron sieve prior to coating.
(5) Retained Material (C): Where doubt exists, review product history of this or similar
formulations and/or evaluate previously acceptable batches.

This document is valid at the time of distribution. Distributed automatically on 14-JUL-2022 (US EST)
 Global Standard Test Method Procedure
Title: Dispersion Test for Finished Goods
Procedure Number: GLO-QC-TM-0729 Content Revision Number: 11
Written by Neil Jones Departments: Global Quality Control & Technical Services
Page 4 of 6
The information contained in this document is proprietary to Colorcon and may not be used or disseminated inappropriately.

2. Coating Mixture Test (Pigmented Formulations only)

a. Prepare coating dispersion according to the appropriate method used for color testing (see
GLO-QC-TM-0576 and Document No. 0927)1. Part of this solution is used for color
measurement. The remainder is poured through a 150-micrometer testing sieve (U.S. #100
Standard). For Acryl-EZE formulations, a 250-micrometer testing sieve is used (U.S #60
Standard).
b. Wash with sufficient solvent to ensure all the dispersion has passed through.
c. Examine retained material.
d. Guidelines for approval:
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(1) Passing Result (Parts (a) and (b) must pass; (c) must pass for specified product)
(a) The sieve should be essentially free from oversize material
(b) Soft and break up easily with fingertip pressure
(c) For Acryl-EZE products, a small amount of fine hardened retained material
will be present on the 250-micrometer sieve. This is inherent in the
formulations
(2) Failing Result: Any test noted in (a) through (c) above did not pass. (see note (1))
e. Notes to Approval Guidelines:
(1) A sample with a failing result during the Colorcon internal manufacturing process
shall have additional processing to fix the product dispersion uniformity.
(2) Retained Material: Where doubt exists, review product history of this or similar
formulations and/or evaluate previously acceptable batches.

C. DRY PIGMENT BLENDS

1. Dry Sieve Test:
a. Place about 50g of powder sample onto a 600-micrometer testing sieve (U.S. #30
Standard).
b. Manually shake sieve, allowing powder to fall through.
c. Examine retained material.
d. Guidelines for approval:

Criteria PASS FAIL

Foreign Matter None Present

1An alternative is to prepare a coating mixture using the solvent and concentration as recommended in the Colorcon reconstitution
sheet, available at www.colorcon.com . This would apply to non-pigmented formulas (if necessary, based on outcome in Section B-1)
or if the color testing method preparation is not performed.

This document is valid at the time of distribution. Distributed automatically on 14-JUL-2022 (US EST)
 Global Standard Test Method Procedure
Title: Dispersion Test for Finished Goods
Procedure Number: GLO-QC-TM-0729 Content Revision Number: 11
Written by Neil Jones Departments: Global Quality Control & Technical Services
Page 5 of 6
The information contained in this document is proprietary to Colorcon and may not be used or disseminated inappropriately.

2. Pigment Speck Evaluation:

a. Pour approximately 10 grams of the blend onto a piece of white paper or paper towel.
Using a spatula, spread it over the paper towel or white piece of paper, examining for
pigment specks or streaks.
b. Guidelines for Approval:
(1) Passing Result: Completely dispersed product with no pigment specks or streaks.
(2) Failing Result: Multiple undispersed pigment specks or lumps.
3. Notes to Approval Guidelines:
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a. A sample with a failing result during the Colorcon internal manufacturing process shall have
additional processing to fix the product dispersion uniformity.
b. Some blends cannot appear completely uniform due to its compatibility with other
ingredients, so where doubt exists, use a previously acceptable batch for comparison.

D. LIQUID DISPERSIONS
1. Pour approximately 10 grams of product onto a piece of white paper.
2. Examine for foreign matter.
3. Using a spatula, spread it over the paper, examining for pigment specks or streaks.
4. Formulas containing dye only: Pour sample into secondary container and examine the residue of
the primary container for undispersed dye, specifically at the bottom of the container for dye
settlement.
5. Guidelines for approval:

Criteria PASS FAIL

Foreign Matter None Present
Pigment Specks/Streaks None Observed
Undispersed Dye None Observed

6. Notes to Approval Guidelines:

a. A sample with a failing result during the Colorcon internal manufacturing process shall have
additional processing to fix the product dispersion uniformity.
b. Where doubt exists, review product history of this or similar formulations and/or evaluate
previously acceptable batches.

This document is valid at the time of distribution. Distributed automatically on 14-JUL-2022 (US EST)
 Global Standard Test Method Procedure
Title: Dispersion Test for Finished Goods
Procedure Number: GLO-QC-TM-0729 Content Revision Number: 11
Written by Neil Jones Departments: Global Quality Control & Technical Services
Page 6 of 6
The information contained in this document is proprietary to Colorcon and may not be used or disseminated inappropriately.

IX. CALCULATIONS: N/A

X. ATTACHMENTS: N/A

XI. REFERENCES:
■ GLO-QC-TM-0576 – Sample preparation and color assessment of Colorcon dispersion products
■ Document No. 0927 – Reconstitution method for preparing dispersion drawdown films

XII. CHANGE HISTORY:

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M-Files Content Date Comments

Version Revision
N/A 0 16-JAN-2001 New Document Issue
N/A 1 08-JUN-2001 Update to include dry pigment blends and liquid dispersions
N/A 2 05-SEP-2003 Formatted. Added option to use paper or paper towel.
Added Acryl-eze statement (US 60 mesh sieve) as per
GLO-QC-TM-0576.
N/A 3 20-AUG-2008 Updated test for undispersed pigments. (D. Greene)
N/A 4 13-JAN-2010 Clarified information related Acryl-EZE products and this
procedure in steps 1A and 1B.
N/A 5 19-APR-2012 New document format, responsibility added
N/A 6 22-NOV-2013 Change of owner. Amendment made under the heading
Retained material. Point 4 added to Section B. Coating
Mixture Test
N/A 7 25-FEB-2014 Amendment made to VII Procedure – Retained Material
section – point 2 & 3
N/A 8 02-DEC-2016 Amendment to section VII Procedure – clarification of
screening process and applicability of Undispersed
Pigments examination for Dry Dispersion
N/A 9 07-FEB-2018 Edit applied (Sucrose) to reflect new product line
N/A 10 02-JUL-2019 Added section relating to Test Sieves, updated Section VII
Procedure to make acceptance criteria and notes more
understandable and pertinent to products
11-current 11 13-JUL-2021 New M-Files format.

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