009

ISO Compliance of the

Dry Jet Dispersion Technology
Introduction
CILAS Dry mode measurements use a new dispersion technology called
Dry Jet Dispersion (DJD). This technology provides you with:
- high dispersion efficiency,
- great reproducibility.
The DJD de-agglomeration concept guarantees particles will not break
apart and the results will be traceable.

Figure 1 : Software Simulation of the velocity distribution in the mixing chamber

Figure 2 : Visualisation of dry

particle flow

The ISO 13320 standard explains how to calibrate and verify a particle size analyzer using Certified
Reference Materials CRMs. CRMs are measured using 5 primary methods to be sure of the powder size.
The results are traceable to major international standards (NIST).
Validation should be done using spherical CRMs such as glass beads and using the Mie theory.

The ISO 13320 Standard

The standard requires that the manufacturer calibrate the instrument using Certified Reference Materials
(CRMs) of a known size distribution. The user must also verify operation of the instrument, both
repeatability and accuracy, at regular time intervals using CRMs. The main requirements of the standard
are presented in table 1.
Requirement

Target values

Test Method

Repeatability
(6.4 in the standard)

Coefficient of variation:
< 3% for X50
< 5%* for X10 & X90

The measurement is done on

at least 5 different samples
from the same batch

Accuracy
(6.5 in the standard)

Maximum deviation from the certified range:

< 3% for X50
< 5%* for X10 & X90

Mean value over 3

independent measurements

*below 10m, these values should be doubled

Table 1: Summary of the main requirements of the ISO 13320 standard.

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Available CRM
Certified Reference Materials (CRMs) (figure 3) are made of spherical
particles and the size distribution of these particles must be established
by using an absolute method.
There are 5 absolute methods for size characterization: Electroformed
Sieve, Gravitational Sedimentation, Centrifugal Sedimentation, Optical
Microscopy and Electrical Sensing Zone. The size distribution ratio of a
CRM is 1:10 (for example, a size distribution from 10 to 100 ms).
Several companies distribute CRMs : NIST and Whitehouse Scientific.
Whitehouse Scientific manufactures a single-shot glass microsphere
covering the complete range of measurement from 0.1 to 2,500 m.
Figure 3 : SEM Picture of
Certified Glass Beads

Whitehouse Glass Bead Measurements

The reproducibility of the measurements made using 10-100m
glass beads with Dry Jet Dispersion is better than 1% (see figure 5).
The ISO 13320 standard requires that reproducibility must be better
than 3% with respect to the median value.
All CILAS particle size analyzers are fully compliant with the 13320
standard.
Figure 4 : Vials from CILAS calibration kit

Calibration and verification of a CILAS particle size

analyzer in wet and/or dry modes are similar. Powders
traceable to international standard, called CILAS
Secondary Reference, are used: CSR1 and CSR2.
The validation is performed using glass bead CRM
from Whitehouse Scientific Ltd (figure 4).
The powders needed for calibration or validation are
available in a hard-sided case which contains single
shot vials used to perform the measurements.
The vials of CSR1, CSR2 and the Whitehouse glass
beads are traceable to international standards.
CILAS allows the user to self-perform the calibration
and verification with the powders provided in the
calibration kit.

Figure 5 : Measurement of the 10-100m CRM

with a CILAS 1064 Particle Size Analyser

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Dry Mode Calibration and Verification

Dry Jet Dispersion Calibration complies with the ISO 13320
standard. The goal of the calibration is to correct any possible
hardware deviations during the products lifetime.
All of the hardware components used in the acquisition system
(laser, lens, sample cell, electronic components, photodiodes)
have imperfections and manufacturing tolerances. The sum of
these tolerances can cause deviations in the reproducibility
and the accuracy of the results.
The system calibration takes into account all these deviations
and enables you to adjust the response of the instrument in
comparison with expected values from certified materials.

Figure 6 : Reproducibility (5 measurements)

of 10-100m glass beads from Whitehouse

Dry and Wet Mode Correlation

The same ISO Calibration method is used for both wet and dry mode. This results in an excellent
correlation between the two different modes with respect to the demands of the ISO standard (figure 6
and 7).
For the same instrument, CILAS can guarantee the following results:

- Accuracy: <3%
- Reproducibility: less than 1% on D50

Figure 7 : Dry and wet mode correlation for CSR2 powder

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Measurement of the CRM with a CILAS 1064

The CILAS 1064L instrument was used
to measure the Whitehouse Scientific
Certified Reference Material.
Data
collected using the CILAS 1064L showed
better repeatability and accuracy values
than required in the ISO 13320 standard.
Statistics from over 50 production
instruments have shown a reproducibility
of better than 1% (figure 8).
The following standards were measured:
Polydispersed standard 1-10m
Polydispersed standard 10-100m
Polydispersed standard 3-30m
Polydispersed standard 50-350m

Figure 8 : Reference Curve for 10-100 m

CRM (from Whitehouse Sc.)

Conclusion
CILAS is the only particle size analyzer manufacturer who calibrates the optical
bench and the dispersing system at the same time. Calibrating both systems at the
same time allows the user to eliminate measurement errors due to the powder
dispersion system.
Our instrument with DJD technology is completely ISO compliant.
The major advantage of CILAS technology is that both modes of dispersion
are calibrated and validated using the same procedure. This allows the user
good correlation between the two modes and a greater accuracy.

Bibliography
[1] The Development of New Reference Standards For Particle Size Instrument Calibration
Rideal, Dodds, Lechonski, Loyd, Mercus, World Congress on Particle Technology 3 (IchemE), 1998, Brighton,
England
[2] International Standard , ISO 13320-1, Particle Size Analysis-Laser Diffraction Methods, General Principles

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