Vanillin

Particle size distribution (Granulometry)

Administrative data

Endpoint:

particle size distribution (granulometry)

Type of information:

experimental study

Adequacy of study:

key study

Study period:

February-March 2010

Reliability:

1 (reliable without restriction)

Rationale for reliability incl. deficiencies:

other: Standardised method performed on all internal powders and flakes.

Data source

Reference

Reference Type:

study report

Title:

Unnamed

Year:

2010

Materials and methods

Test guideline

Qualifier:

no guideline followed

Principles of method if other than guideline:

Particle size distribution was performed on bulk powders by laser diffraction. Sieving analysis was performed on flakes. Fine fractions (particles < 100 µm) coming from sieving analysis were characterized by laser diffraction.

GLP compliance:

no

Type of method:

Laser scattering/diffraction

Type of distribution:

volumetric distribution

Test material

Test material information

Constituent 1

Reference substance name:

Vanillin

EC Number:

204-465-2

EC Name:

Vanillin

Cas Number:

121-33-5

Molecular formula:

C8H8O3

IUPAC Name:

1-butoxypropan-2-ol

Details on test material:

- Name of test material (as cited in study report): Rhovanil extrapure and vaniltek flakes
- Substance type:
- Physical state: solid/ powder and flakes
- Analytical purity: see confidential details below
- Impurities (identity and concentrations): see confidential details below
- Purity test date: see below
- Lot/batch No.: see below
- Expiration date of the lot/batch: see below
- Other: the product was sampled from standard commercial packaging (25 kg). A representative sampling is first produced according to DIN 51701/Pt 4 - "Testing of solid fuels - Sampling and sample preparation - Part 4: equipment" with a Retsch rotating tube divider PK1000 and then a Retsch sample rotating divider PT100.

Results and discussion

Particle size

Particle size 1

Percentile:

D50

Mean:

220.3 µm

Remarks on result:

other: Above is D50 for Rhovanil SFC; D50 = 247,8 µm for Rhovanil BTR(migrated from fields under 'Mass median diameter' as D50 percentile. No source field for Standard deviation.)

Particle size 2

Percentile:

D10

Mean:

100.7 µm

Remarks on result:

other: Rhovanil SFC

Particle size 3

Percentile:

D10

Mean:

121.2 µm

Remarks on result:

other: Rhovanil BTR

Particle size 4

Percentile:

D90

Mean:

393.1 µm

Remarks on result:

other: Rhovanil SFC

Particle size 5

Percentile:

D90

Mean:

401.4 µm

Remarks on result:

other: Rhovanil BTR

Any other information on results incl. tables

Picture digital camera: Rhovanil: white powder of fine crystals with some agglomerates. Vaniltek: white to pale yellow flakes presenting a heterogeneity of sizes and shapes, most are large flakes in the range 1 mm to 5 mm.

Microscope pictures: Rhovanil: plate and some needles like crystals from 50 to > 500 µm. Vaniltek: flakes presenting some fine particles agglomerated to bigger particles.

Sieving of the flakes: 91.0% weight > 1000 µm, 6.5% weight in the range from 500 to 1000 µm; it was not possible to collect fine particles < 100 µm, so no analysis on laser Sympatec was further performed.

Fragility test: the attrition of particles or flakes is realized with insertion of two rubber balls (diameter 35 mm, weight 23 +/- 1g) on the 1 mm sieve. Results on fragility are the particle size distribution compared with standard sieve analysis described above. Average result from 2 measurements: vaniltek flakes are somewhat fragile, 65.1% weight keep their initial size. A low level for generation of fine particles < 100 µm is observed (around 0.2 % weight).

Applicant's summary and conclusion

Conclusions:

Particle size distribution of vanilline powders were characterized through laser diffraction analysis and by sieving for flakes. D10 were 100.7 µm and 121.2 µm respectively for the two powders tested. As concerning the flakes: no flakes above 5000 µm and no particles below 100 µm were collected. The finest particles collected were in the range 100 to 200 µm (0.2 %), 91% of weight was above 1000 µm.