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A laser diffraction system is made up of two main components, the optical bench,
PARTICLE SIZE which collects the scattering data from a sample, and a dispersion unit which
must accurately deliver the sample to the optical bench. This technical note
describes how the optical bench and dispersion units are tested and how system
to system reproducibility of laser diffraction instruments can be assessed.
During production each optical bench is tested with a range of latex standards,
generating a significant data set from which the reproducibility of the optical
benches can be assessed. In this section the results of measurements of a
range of latex sizes, on 100 optical benches, are presented to demonstrate the
reproducibility of the optical benches.
2 Assessing the reproducibility of particle size measurements using the Mastersizer 3000
TECHNICAL NOTE
Malvern has developed a Quality Audit Standard (QAS) which meets all of the
requirements of ISO 13320 for a certified reference material. Glass beads are an
appropriate reference material for laser diffraction as they are spherical particles
with well-known optical properties.
The particle size distribution of the sample must be greater than one decade in
size. The width of the size distribution is specified as the ratio of the Dv90/Dv10
which must be between 1.5 and 10. For QAS the Dv90/Dv10 is approximately 2.3,
see Table 2.
Sampling bias is removed from the measurement process by using a single shot
sample. These single shot vials are produced by riffling down from a master batch
into appropriate masses for each dispersion unit.
A full measurement procedure is defined for each dispersion unit [2] setting such
parameters as measurement duration, stir speed, air pressure and vibration rate
to ensure full dispersion of the material.
The target size and pass/fail criteria for QAS have been measured on a reference
laser diffraction system which has been verified using NIST -traceable polystyrene
latex standards. Therefore, as a reference material, QAS is indirectly traceable
to NIST. The pass/fail criteria have been set, according to the ISO standard as
follows; the Dv10 must be within 3% of the target value, the Dv50 within 2.5% and
the Dv90 within 4%.
The reproducibility of the dry dispersion units, Aero S, was assessed by measuring
QAS samples using 100 dispersion units. In Figure 3 the scatter plot shows Dv50
from these 100 measurements vs accessory number, a line has been added to
3 Assessing the reproducibility of particle size measurements using the Mastersizer 3000
TECHNICAL NOTE
show the target value and the size axis extends to ± 2.5% of the target value. The
same data is also represented in a box plot in Figure 3.
The average values and RSDs from these QAS measurements using the Aero S are
shown in Table 1. The RSDs are less than 1% for all parameters, demonstrating
system to system reproducibility better that the repeatability of a laser diffraction
measurement, as stated in the ISO standard.
The reproducibility of the wet dispersion units was tested by measuring 100 QAS
samples on each of the wet dispersion units, Hydro MV, Hydro LV and Hydro EV.
The Dv50 vs. accessory number for all 300 wet QAS measurements is shown in
Figure 4
Figure 3 : Scatter plot and box plot of 100 QAS measurements using the Aero S
The statistics from the wet measurements are shown in Table 2. When the data
from all wet units is combined the RSDs are less than 1% showing excellent
reproducibility across the range of dispersion units. The RSDs for individual
dispersion units are even lower.
This level of reproducibility between the dispersion units simplifies the process of
transferring methods and specifications between sites and different dispersion
units.
4 Assessing the reproducibility of particle size measurements using the Mastersizer 3000
TECHNICAL NOTE
Conclusions
The reproducibility of laser diffraction instruments requires both the optical bench
and dispersion units to be tested. A range of latex standards have been measured
on 100 optical benches in order to test bench to bench reproducibility. The results
show a relative standard deviation over the one hundred measurements of less
than 1%.
The reproducibility of the dispersion units have been tested by measuring QAS
samples on one hundred of each type of dispersion units. This showed a relative
standard deviation of less than 1% for the 100 measurements on each dispersion
unit, and across all of the wet dispersion units combined.
References
• ISO13320 (2009). Particle Size Analysis - Laser Diffraction Methods, Part 1:
General Principles
• QAS measurement procedure
5 Assessing the reproducibility of particle size measurements using the Mastersizer 3000
TECHNICAL NOTE
Malvern Instruments Malvern Instruments is part of Spectris plc, the Precision Instrumentation and Controls Company.
Limited
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