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Particle size distribution (Granulometry)

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Reference
Endpoint:
particle size distribution (granulometry)
Type of information:
experimental study
Adequacy of study:
key study
Study period:
March 2010
Reliability:
1 (reliable without restriction)
Rationale for reliability incl. deficiencies:
other: Well conducted study with Internal Management System and according to OECD and ISO guidelines, certificate of analysis included in the report.
Qualifier:
according to
Guideline:
OECD Guideline 110 (Particle Size Distribution / Fibre Length and Diameter Distributions)
Deviations:
no
Qualifier:
according to
Guideline:
other: ISO 2591-1, Test sieving - Part 1: Methods using test sieves of woven wire cloth and perforated metal plate, December 1988
Deviations:
no
Qualifier:
according to
Guideline:
other: ISO 3310-1, Test sieves - Technical requirements and testing - Part 1: Test sieves of metal wire cloth, July 1990
Deviations:
no
Qualifier:
according to
Guideline:
other: Intern AkzoNobel SMA 721.02, Determination of the particle size distribution of powders and granular products, June 2001
Deviations:
no
Qualifier:
according to
Guideline:
other: Intern AkzoNobelSMA 743.02, Distribution of powders and granulated products in representative portions, August 1993 SMA Gr/86.4-3, Determination of the sieve residue (air-jet method) in particulate solids, January 1996
Deviations:
no
GLP compliance:
no
Remarks:
Internal Management System
Type of method:
sieving
Type of distribution:
counted distribution
Percentile:
D10
Mean:
21.5 µm
St. dev.:
1
Remarks on result:
other: From fraction <100µm
Percentile:
D50
Mean:
68.8 µm
St. dev.:
0.5
Remarks on result:
other: From fraction <100µm
Percentile:
D90
Mean:
132 µm
St. dev.:
3
Remarks on result:
other: From fraction <100µm
No.:
#1
Size:
< 100 µm
Distribution:
3.1 %

 Light microscopic examinations

 

Pictures of a small amount of the samples A and B were taken with the Stemi 2000-c microscope equipped with an AxioCam ICc 3 digital camera. The pictures are in the attachment.

From the digital pictures it can be concluded that the shape of the particles is non fibrous. Besides flakes the product contains small particles.

Sieving

 

The sample was sieved over a 100 µm sieve according to SMA 271.02, after splitting the sample according to SMA 743.

Sieve analysis of Perkadox 14S-FL

 

Perkadox 14S-FL

Batch No.:

0909144588

Intake

(g)

Fraction > 100 µm

Fraction < 100 µm

(g)

(% m/m)

(g)

(% m/m)

A-1

84.51

82.09

97.14

2.02

2.39

A-2

84.14

81.79

97.21

2.23

2.65

B-1

83.26

80.94

97.21

2.22

2.67

B-2

84.52

82.19

97.24

2.22

2.63

Average

 

 

97.20

 

2.58

 

Remark:           A large part of the fraction < 100 µm of the Perkadox 14S-FL adhered to the underside of the sieve and remained in the sieve mesh. In order to quantify the remaining fines in the > 100 µm product and on the 100 µm sieve additional sieving was performed via air jet sieving for 10 minutes. Remaining fines are removed then via vacuum.

 

The Perkadox 14S-FL sample fraction > 100 µm was sieved by air jet sieving for 10 minutes with a pressure of 4000 Pa according to SMA Gr/86.4-3.

 

Air-jet sieve analysis of Perkadox 14S-FL

 

Perkadox 14S-FL

Batch No.:

0909144588

Intake

(g)

Fraction > 100 µm

Fraction < 100 µm

(g)

(% m/m)

(g)

(% m/m)

A-1

82.09

81.71

99.54

0.38

0.46

A-2

81.79

81.44

99.57

0.35

0.43

B-1

80.94

80.44

99.38

0.50

0.62

B-2

82.19

81.70

99.40

0.49

0.60

Average

 

 

99.47

 

0.53

 

For the total amount of fraction < 100 µm the results have to be calculated back to the first intake of the sample. In the following table these results are reported.

 


Total results of fraction < 100 µm of Perkadox 14S-FL

 

Perkadox 14S-FL

Batch No.:

0909144588

Intake

(g)

Fraction < 100 µm

Traditional sieving

(g)

Air-jet

sieving

(g)

Total

(g)

Total

(% m/m)

A-1

84.51

2.02

0.38

2.40

2.84

A-2

84.14

2.23

0.35

2.58

3.07

B-1

83.26

2.22

0.50

2.72

3.27

B-2

84.52

2.22

0.49

2.71

3.21

Average

 

 

 

 

3.10

 

This means that the average fraction < 100 µm of 3.1% (m/m) is significantly more than the limit value of 1.0% m/m. The PSD of the fraction < 100 µm has to be determined and also the relative density of Perkadox 14S-FL

 Relative density

 

The relative density of Perkadox 14S-FL is reported separately in Physico-Chemical Properties Report number 2.416.361 (see Reference 9).

 

The relative density of Perkadox 14S-FLis 1.042 with a standard deviation of 0.001.

 PSD by laser diffraction

In the following table the PSD characteristics of the fraction smaller than 100 µm are reported

PSD-characteristics of Perkadox 14S-FL fraction < 100 µm

 

Perkadox 14S-FL

Batch No.: 0909144588

d10

(µm)

d50

(µm)

d90

(µm)

A-1

20.2

68.5

136

A-2

21.2

68.7

134

B-1

22.4

69.6

130

B-2

22.1

68.4

129

Average

21.5

68.8

132

Standard Deviation

1.0

0.5

3

RSD

4.6%

0.8%

2.6%

 

Remark:           The definition of dxis that equivalent diameter (usually in µm) where x volume-% of the powder has a smaller diameter.

 The PSD curve of the fraction < 100 µm of Perkadox 14S-FL is in the attachment.

 

 

Conclusions:
Light microscopic examination showed a flake type granular product, no fibres were observed.

The fraction < 100 µm of [1,3-phenylenebis(1-methylethylidene)]bis[tert-butyl] peroxide is 3.1% (m/m). The PSD-characteristics determined via laser light diffraction analysis are : d10 is 22µm, d50 is 69µm and d90 is 132µm.

Executive summary:

Well conducted study with Internal Management System and according to OECD and ISO guidelines, certificate of analysis included in the report.

Light microscopic examination showed a flake type granular product, no fibres were observed.

The fraction < 100 µm of [1,3-phenylenebis(1-methylethylidene)]bis[tert-butyl] peroxide is 3.1% (m/m). The PSD-characteristics determined via laser light diffraction analysis are : d10 is 22µm, d50 is 69µm and d90 is 132µm.

Description of key information

Light microscopic examination showed a flake type granular product, no fibres were observed.

The fraction < 100 µm of [1,3-phenylenebis(1-methylethylidene)]bis[tert-butyl] peroxide is 3.1% (m/m). The PSD-characteristics determined via laser light diffraction analysis are : d10 is 22µm, d50 is 69µm and d90 is 132µm.

Additional information

See Light microscopic images in attached document.