Particle Size Determination

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1.0 Purpose 
 
 The purpose of this procedure is to define the process for determining particle size and relative
 quantity. 
 
 2.0 Scope 
 
 This procedure applies to raw material and finished product samples for which there is a
 specification for the percentage of particles that will pass through a screen of a specified size.
 
 This procedure does not apply to materials intended for use in pharmaceuticals.
 
 3.0 Responsibility 
 
 3.1 It is the responsibility of QC Laboratory Analysts to follow this procedure.
 
 3.2 It is the responsibility of QC Laboratory Management to implement this procedure and
 to ensure that the procedure is being followed. 
 
 3.3. It is the responsibility of QC Laboratory Management and/or Analytical Development
 to keep this procedure aligned with current practices. 
 
 4.0 Definitions 
 
 4.1 QC - Quality Control 
 
 4.2 | ASTME — American Society of Tool Manufacturing Engineers 
 
 4.3. NIST — National Institute of Standards and Technology 
 
 4.4 ISO - International Organization for Standardization 
 
 
 

[SOP 

 Standard Operating Procedure SOP No | Rev —_— 
 Particle Size Determination D-724 7 s 
 
 5.0 References 
 
 5.1 USP<786>, monograph, Particle Size Distribution Estimation by Analytical Sieving
 
 5.2. D-724-F1, Form, Particle Size Test Ticket 
 
 6.0 Procedure 
 
 6.1 Perform the procedure using form D-724-F1 Particle Size Test Ticket.
 
 6.2 All sieves used must be traceable to ASTME, NIST, or ISO 3310-1 specifications and
 have a placard with the specified gauge. 
 
 6.3 Verify that the sieves used have the correct gauges specified for the material.
 
 6.4 Inspect sieve to verify that there are no broken, bent, or missing wires in the mesh.
 
 Replace sieve if any damage if found. 
 
 6.5 When more than one gauge of sieve is being used place in order of coarsest (top) to
 finest (bottom). Pre-weigh each sieve and document their initial weights.
 
 6.6 Weigh each test sieve to the nearest 0.1 g. Record Weight. 
 
 6.7. Weigh a representative portion of the test material and document the initial sample
 
 weight. 
 
 6.7.1 Sample size is dependent upon the density of the powder or granule, and the
 
 diameter of test sieves being used, typically between 25 — 100 grams.
 
 6.7.2 If the test material is prone to picking up or losing significant amounts of water
 
 with varying humidity, the test must be carried out in an appropriately
 controlled environment. 
 
 6.7.3 If the test material is known to develop an electrostatic charge, careful
 
 observation must be made to ensure that such charging is not influencing the
 
 
 

[SOP 

 Standard Operating Procedure SOP No | Rev oan dots 
 Particle Size Determination D-724 7 % 
 
 analysis. An antistatic agent, such as colloidal silicon dioxide and/or aluminum
 
 oxide, may be added at a 0.5 percent (m/m) level to minimize this effect.
 
 6.7.4 Agglomerations may be manually broken apart without pressing sample through
 
 the screen. 
 
 6.8 Place an accurately weighed quantity of test specimen on the top (coarsest) sieve, and
 replace the lid. Agitate the nest of sieves for 5 minutes. Then carefully remove each
 
 from the nest without loss of material. Reweigh each sieve, and determine the weight of
 material on each sieve. Determine the weight of material in the collecting pan in a
 
 similar manner 
 
 6.9 Calculate the %weight of a particle size by: 
 
 6.9.1 Subtract the pre-weight of the sieve from the final sieve containing sifted
 
 sample. 
 
 6.9.2 Divide the difference in by the original sample tare weight then multiply by 100.
 
 The result is the % weight by particle size. 
 
 6.9.3. Report % weight as the percentage of the initial sample weight.
 
 6.9.4 Calculations can be repeated for each gauge screen as needed.
 
 6.10 Alternatively, weigh the amount passed through the sieve directly and report the
 percentage passed as a percentage of the initial sample weight. 
 
 
 

[SOP 

 Standard Operating Procedure SOP No | Rev cape 
 Partiec le Sie ze Determien atie on a= e ! :€ 0 
 
 7.0 Revision History 

| Rev | Date | Description of Changes | CCR # | By |
|-----|----------|------------------------|-------|----|
| 0 | 05/06/10 | New - - 01/26/12 Updated SOP. - - | - | - |
| 2 | 02/23/13 | Reformatted SOP. | 13-114 | B. Johns |
| 3 | 02/06/15 | Biennial review. Update SOP format. Expanded calculation description. Expanded sieve standardization traceability. Excluded | 15-0144 | B. Johns |
| 4 | 04/10/17 | pharmaceutical materials. Changed responsibilities. Added USP <786> reference. | 17-0394 | B. Johns |
| 5 | 07/20/20 | Added definition and changed responsibilities. CC- | 20-0517 | J. Maignan |
| 6 | 06/09/22 | Updated to reflect current practice and align with USP. CC- | 22-0266 | J. Sassman |
| 7 | 01/30/23 | Updated to add reference to new form D-724-F1. Created new CC- form D-724-F1 that can accept up to three tests per page. | 23-0053 | J. Nicholson |

 
 

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