1,6-Bis(methoxybenzoyloxy)hexane

Particle size distribution (Granulometry)

Link to relevant study record(s)

Reference

Endpoint:

particle size distribution (granulometry)

Type of information:

experimental study

Adequacy of study:

key study

Study period:

10th March 2004

Reliability:

2 (reliable with restrictions)

Rationale for reliability incl. deficiencies:

other: Carried out in a GLP laboratory but no OECD or equiavlent test method is referenced, only an internal laboratory test method.

Qualifier:

no guideline followed

Principles of method if other than guideline:

Test Objective
To characterise the particle size distribution of the powder. The analysis is conducted initially using a visual microscope and is then undertaken more formally using a Laser Diffraction Particle Size Analyser.

Optical Microscope Analysis
Sample Setafix X 11342
Date 10/03/2004
Operator D.Baker
SOP Reference CTL SOP 417 (current version)

The sample is observed under 3 conditions.
•· Direct observation
• Under a microscope with ·100 x magnification
• Under a microscope with 400 x magnification
The physical characteristics of the material are recorded, noting such items as shape and size distribution.

Standard visual observation
Sample observed to be a coarse, crystalline, white powder with a small number of clusters.

Observation at 100 x magnification
The particles appeared to be large, round edged, irregular shaped crystals. The smallest particle size was approximately 48.0 μm and the largest size was approximately 874.7 μm.

Observation at 400 x magnification
The sample was observed to be made up of single crystalline particles.

Manual Sieve Analysis
Standard Operating Procedum No. 417
Sample Setafix X 11342
Preparation Sample tested as received.
Quantity 114.6g
Date 10/03/2004
Operator D.Baker

LASER DIFFRACTION PARTICLE SIZE ANALYSIS
Test Objective and Information
The test is conducted to determine the particle size distribution of Setafix X 11342. The sample is initially observed to determine whether sieving of the material is required. The final sample is then analysed using the Coulter Laser Diffraction Analyser fitted with a dry powder module. It is normal practice to complete 3 runs to ensure repeatability of results, but in the case of Setafix X 111342 only 2 runs were performed, due to limited sample being available. The test was conducted to BS ISO 13320-1 : 1999.

Date 10/03/2004
Operator D.Baker
Preparation Sample tested as received.
SOP Reference CTL SOP 417 (current version)

Note : Due to the small quantity of suitable sample being available, only two 30 second runs were able to be performed. However, excellent reproducibility was observed suggesting reliable results haive been obtained from this reduced analysis.

GLP compliance:

yes (incl. QA statement)

Remarks:

GLP certificate dated 31st July 2003 and attached to report

Type of method:

other: GLP protocols and following guidelines stated in Chilworth Technology Limited standard operating procedure No 417

Type of distribution:

counted distribution

Geometric standard deviation:

1.7

Percentile:

D50

Mean:

509.2 µm

Remarks on result:

other: Results from Laser diffraction Particle Size Analysis(migrated from fields under 'Mass median diameter' as D50 percentile. No source field for Standard deviation.)

Percentile:

D10

Mean:

ca. 212.1 µm

Remarks on result:

other: Results from Laser Diffraction Particle Analysis

Percentile:

D50

Mean:

ca. 509.2 µm

Remarks on result:

other: Results from Laser Diffraction Particle Analysis

Percentile:

D90

Mean:

ca. 811.2 µm

Remarks on result:

other: Results from Laser Diffraction Particle Analysis

Conclusions:

The testing conducted to determine the Particle size analysis produced the following results:

Manual sieve analysis indicated that 43.5 % by weight of the sample had a particle size of < 850 μm.
A subsequent laser diffraction analysis on the < 850 μm sample produced the following results:

Average
Volume %                                     100.0
Mean (micrometeres)                   452.1
Median (micrometers)                    509.2
Mode (micrometers)                       859.9
95 % Conf. limit (micrometers)      160 -1270
S.D.                                               1.7
< 10 % of material is                     212.1 micrometers
< 25 % of material is                     333.5 micrometers
< 50 % of material is                     509.2 micrometers
< 75 % of material is                     688.8 micrometers
< 90 % of material is                     811.2 micrometers

Executive summary:

The testing conducted to determine the Particle size analysis produced the following results:

Manual sieve analysis indicated that 43.5 % by weight of the sample had a particle size of < 850 μm.

A subsequent laser diffraction analysis on the < 850 μm sample produced the following results:

Average

Volume %                                     100.0

Mean (micrometeres)                   452.1

Median (micrometers)                    509.2

Mode (micrometers)                       859.9

95 % Conf. limit (micrometers)      160 -1270

S.D.                                               1.7

< 10 % of material is                     212.1 micrometers

< 25 % of material is                     333.5 micrometers

< 50 % of material is                     509.2 micrometers

< 75 % of material is                     688.8 micrometers

< 90 % of material is                     811.2 micrometers

Description of key information

Manual sieve analysis indicated that 43.5 % by weight of the sample had a particle size of < 850 μm.
A subsequent laser diffraction analysis on the < 850 μm sample produced the following results:
Average
Volume %                                     100.0
Mean (micrometers)                    452.1
Median (micrometers)                    509.2
Mode (micrometers)                       859.9
95 % Conf. limit (micrometers)      160 -1270
S.D.                                               1.7
< 10 % of material is                     212.1 micrometers
< 25 % of material is                     333.5 micrometers
< 50 % of material is                     509.2 micrometers
< 75 % of material is                     688.8 micrometers
< 90 % of material is                     811.2 micrometers