SIST EN 17289-1:2021
(Main)Characterization of bulk materials - Determination of a size-weighted fine fraction and crystalline silica content - Part 1: General information and choice of test methods
Characterization of bulk materials - Determination of a size-weighted fine fraction and crystalline silica content - Part 1: General information and choice of test methods
The purpose of this document is to allow users to evaluate bulk materials with regard to the
amount of fine fraction of potentially hazardous substances, especially crystalline silica. This Part
1 describes the requirements and choice of test method. It provides the user with guidance on
how to select the method as well as the preparation of the sample and determination of
crystalline silica by XRD and FTIR.
This document is applicable for bulk materials that contain particles in the size range from 0,1
μm to 125 μm satisfying with the criteria given in Part 2 and Part 3 of this document series. The
current industrial minerals within the scope of this method are: quartz, clay, kaolin, talc, feldspar,
mica, cristobalite, vermiculite, diatomaceous earth, barite and andalusite. The method may be
applicable to other bulk materials, following full investigation and validation.
Charakterisierung von Schüttgütern - Bestimmung einer größengewichteten Feinfraktion und des Anteils an kristallinem Quarz - Teil 1: Allgemeine Information und Auswahl der Prüfverfahren
Dieses Dokument legt die Anforderungen und die Auswahl des Prüfverfahrens für die Bestimmung der größengewichteten Feinfraktion (SWFF) und der größengewichteten Feinfraktion von kristallinem Quarz (SWFFCS) in Schüttgütern fest.
Dieses Dokument gibt auch Hinweise zur Vorbereitung der Probe und zur Bestimmung von kristallinem Quarz durch Röntgenpulverdiffraktometrie (XRD) und Fourier-Transformations-Infrarotspektrometrie (FT IR).
ANMERKUNG EN 17289-2 legt ein Verfahren zur Berechnung der größengewichteten Feinfraktion aus einer gemessenen Partikelgrößenverteilung fest und geht davon aus, dass die Partikelgrößenverteilung der kristallinen Quarzpartikel die Gleiche ist wie die der anderen Partikel im Schüttgut. EN 17289-3 legt ein Verfahren fest, bei dem eine Sedimentationstechnik in Flüssigkeit zur Bestimmung der größengewichteten Feinfraktion von kristallinem Quarz verwendet wird. Beide Verfahren basieren auf einer Reihe von Einschränkungen und Annahmen, die in EN 17289- bzw. EN 17289-3 angegeben sind. Das Verfahren nach EN 17289-3 kann auch für andere Bestandteile als CS verwendet werden, wenn diese untersucht und validiert werden.
Dieses Dokument ist für kristallinen Quarz enthaltende Schüttgüter anwendbar, die zur Bewertung der größengewichteten Feinfraktion und des kristallinen Quarzes untersucht und validiert wurden.
Caractérisation des matériaux en vrac - Détermination de la fraction fine pondérée par taille et de la teneur en silice cristalline - Partie 1 : Informations générales et choix des méthodes d’essai
Le présent document spécifie les exigences et le choix d’une méthode d’essai pour la détermination de la fraction fine pondérée par taille (SWFF) et de la fraction fine de silice cristalline pondérée par taille (SWFFCS) dans des matériaux en vrac.
Le présent document donne également des recommandations relatives à la préparation de l’échantillon et au dosage de la silice cristalline par analyse de poudre par diffraction de rayons X (XRD) et par spectroscopie infrarouge à transformée de Fourier (FT-IR).
NOTE L’EN 17289-2 spécifie une méthode permettant de calculer la fraction fine pondérée par taille à partir d’une distribution granulométrique mesurée et part de l’hypothèse que la distribution granulométrique des particules de silice cristalline est identique à celle des autres particules présentes dans le matériau en vrac. L’EN 17289-3 spécifie une méthode utilisant une technique de sédimentation dans un liquide pour déterminer la fraction fine de silice cristalline pondérée par taille. Les deux méthodes sont fondées sur un certain nombre de limites et d’hypothèses, qui sont respectivement énumérées dans l’EN 17289-2 et l’EN 17289-3. La méthode décrite dans l’EN 17289-3 peut également être utilisée pour d’autres constituants que la silice cristalline, s’ils sont étudiés et validés.
Le présent document s’applique aux matériaux en vrac contenant de la silice cristalline, qui ont été entièrement étudiés et validés pour l’évaluation de la fraction fine pondérée par taille et de la silice cristalline.
Karakterizacija razsutih materialov - Določanje velikostno utežene fine frakcije in deleža kristaliničnega kremena - 1. del: Splošne informacije in izbira preskusnih metod
General Information
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN 17289-1:2021
01-februar-2021
Karakterizacija razsutih materialov - Določanje velikostno utežene fine frakcije in
deleža kristaliničnega kremena - 1. del: Splošne informacije in izbira preskusnih
metod
Characterization of bulk materials - Determination of a size-weighted fine fraction and
crystalline silica content - Part 1: General information and choice of test methods
Charakterisierung von Schüttgütern - Bestimmung einer größengewichteten Feinfraktion
und des Anteils an kristallinem Quarz - Teil 1: Allgemeine Information und Auswahl der
Prüfverfahren
Caractérisation des matériaux en vrac - Détermination de la fraction fine pondérée par
taille et de la teneur en silice cristalline - Partie 1 : Informations générales et choix des
méthodes d’essai
Ta slovenski standard je istoveten z: EN 17289-1:2020
ICS:
13.040.30 Kakovost zraka na delovnem Workplace atmospheres
mestu
SIST EN 17289-1:2021 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST EN 17289-1:2021
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SIST EN 17289-1:2021
EN 17289-1
EUROPEAN STANDARD
NORME EUROPÉENNE
December 2020
EUROPÄISCHE NORM
ICS 13.040.30
English Version
Characterization of bulk materials - Determination of a
size-weighted fine fraction and crystalline silica content -
Part 1: General information and choice of test methods
Caractérisation des matériaux en vrac - Détermination Charakterisierung von Schüttgütern - Bestimmung
de la fraction fine pondérée par taille et de la teneur en einer größengewichteten Feinfraktion und des Anteils
silice cristalline - Partie 1 : Informations générales et an kristallinem Quarz - Teil 1: Allgemeine Information
choix des méthodes d'essai und Auswahl der Prüfverfahren
This European Standard was approved by CEN on 4 October 2020.
CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this
European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references
concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN
member.
This European Standard exists in three official versions (English, French, German). A version in any other language made by
translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management
Centre has the same status as the official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,
Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and
United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2020 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 17289-1:2020 E
worldwide for CEN national Members.
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SIST EN 17289-1:2021
EN 17289-1:2020 (E)
Contents Page
European foreword . 3
Introduction . 4
1 Scope . 6
2 Normative references . 6
3 Terms and definitions . 6
4 Symbols and abbreviations . 9
5 Test methods . 9
6 Guidelines for the determination of crystalline silica . 11
6.1 Preparation of sample to be analysed . 11
6.2 Sample preparation for further analysis by XRD and FT-IR . 11
7 Test report . 11
Annex A (informative) Bias and uncertainties . 13
A.1 General . 13
A.2 Bias between EN 481 and sedimentation SWFF probability function and influence of
density and mineral phase mass fraction . 13
A.3 Uncertainty . 16
Annex B (informative) Round robin test to establish a SWFF reference sample . 18
B.1 General . 18
B.2 Test material . 18
B.3 Evaluation and appraisal method . 19
B.4 Results . 20
Annex C (informative) Determination of crystalline silica in bulk samples using X-Ray
diffraction (XRD) or FT-IR spectroscopy . 23
C.1 General . 23
C.2 Preparation of bulk samples for determination of CS using XRD . 23
C.3 Preparation of bulk samples for determination of CS using FT-IR . 26
Annex D (informative) Calculating SWFF and SWFFCS from a given particle size distribution
using a spreadsheet . 29
D.1 Spreadsheet setup . 29
D.2 Example . 30
Bibliography . 33
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EN 17289-1:2020 (E)
European foreword
This document (EN 17289-1:2020) has been prepared by Technical Committee CEN/TC 137
“Assessment of workplace exposure to chemical and biological agents”, the secretariat of which is held
by DIN.
This European Standard shall be given the status of a national standard, either by publication of an
identical text or by endorsement, at the latest by June 2021, and conflicting national standards shall be
withdrawn at the latest by June 2021.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN shall not be held responsible for identifying any or all such patent rights.
According to the CEN-CENELEC Internal Regulations, the national standards organisations of the
following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria,
Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland,
Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Republic of
North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the
United Kingdom.
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EN 17289-1:2020 (E)
Introduction
A method was developed in the industrial minerals industry for the purpose of determining the “size-
weighted relevant fine fraction” within the bulk material. This document sets out the methods
which can be used to measure and calculate the fine fraction of the bulk material and the fine fraction
of the crystalline silica, in several types of bulk materials. This information provides additional
information to users for their risk assessment and to compare bulk materials. It has been used
in the industry and by institutes previously under the acronym SWeRF. EN 17289 (all parts) is based
on that industrial method and specifies the analytical methods to determine the difference between
materials with coarse quartz and fine quartz, for example, sands versus flour.
As further activities with the material (intentional or otherwise) can change the particle size
distribution, the size-weighted fine fraction can also change. Therefore, the method reports (in terms of
the mass fraction in the bulk material in percent) both, the total crystalline silica (CS) and the estimated
size-weighted fine fraction of CS.
Conventions as specified in EN 481 [1] can be used as input for this document. However, the output
of this document is not related to the respirable fraction and cannot be used to replace workplace
exposure measurements.
EN 17289 (all parts) specifies two procedures that can be used to estimate the size-weighted fine
fraction (SWFF) in bulk materials. It also specifies how the SWFF, once separated, can be further
analysed to measure the content of crystalline silica (SWFFCS). The method can be used for comparing
the fine fraction in different bulk samples. EN 17289 (all parts) uses the term fine fraction to indicate
that it does not analyse airborne particles, but it evaluates the proportion of particles in a bulk material
that, based on their particle size, have a potential to be respirable if they were to become airborne.
EN 17289 (all parts) also allows for the size-weighted fine fraction of crystalline silica (SWFFCS)
particles in bulk materials to be evaluated in terms of mass fraction in percent, if the fraction separated
is subsequently analysed by a suitable method.
In a comparison of similar bulk materials, in which the particle size distribution is the only variable,
the SWFF can provide useful information to guide material selection. For example, leaving all other
factors aside, a bulk material with a lower SWFF value can pose less of a risk in terms of potential
occupational exposure. For the actual exposure at the workplace, the handling etc. of the material,
will play a major role.
Concentrations of respirable dust, or respirable crystalline silica (RCS), in the workplace air, resulting
from processing and handling of bulk materials, will depend on a wide variety of factors and these
concentrations cannot be estimated using SWFF or SWFFCS values. SWFF and SWFFCS values are not
intended for workplace exposure assessments as they have no direct relationship with occupational
exposure.
The evaluation of bulk materials using SWFF is complementary to determining the dustiness according
to EN 15051-1 [2].
The difference between EN 17289 (all parts) and EN 15051-1 is that SWFF quantifies the fine fraction in
a bulk material while dustiness quantifies the respirable, thoracic and inhalable dust made airborne
from the bulk material after a specific activity (dustiness characterizes the material with relation to the
workplace atmosphere when working with the bulk material).
4
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EN 17289-1:2020 (E)
EN 17289 Characterization of bulk materials — Determination of a size-weighted fine fraction
and crystalline silica content consists of the following parts:
— Part 1: General information and choice of test methods;
— Part 2: Calculation method;
— Part 3: Sedimentation method.
NOTE This document is intended for use by laboratory experts who are familiar with FT-IR, XRD methods,
PSD measurements and other analytical procedures. It is not the intention of this document to provide instruction
in the fundamental analytical techniques.
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EN 17289-1:2020 (E)
1 Scope
This document specifies the requirements and choice of test method for the determination of the size-
weighted fine fraction (SWFF) and the size-weighted fine fraction of crystalline silica (SWFFCS) in bulk
materials.
This document gives also guidance on the preparation of the sample and the determination of
crystalline silica by X-ray Powder Diffractometry (XRD) and Fourier Transform Infrared Spectroscopy
(FT-IR).
NOTE EN 17289-2 specifies a method to calculate the size-weighted fine fraction from a measured particle
size distribution and assumes that the particle size distribution of the crystalline silica particles is the same as the
other particles present in the bulk material. EN 17289-3 specifies a method using a liquid sedimentation
technique to determine the size-weighted fine fraction of crystalline silica. Both methods are based upon a
number of limitations and assumptions, which are listed in EN 17289-2 and EN 17289-3, respectively. The method
in EN 17289-3 can also be used for other constituents than CS, if investigated and validated.
This document is applicable for crystalline silica containing bulk materials which have been fully
investigated and validated for the evaluation of the size-weighted fine fraction and crystalline silica.
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements of this document. For dated references, only the edition cited applies. For
undated references, the latest edition of the referenced document (including any amendments) applies.
EN 1540, Workplace exposure — Terminology
EN 17289-2, Characterization of bulk materials — Determination of a size-weighted fine fraction and
crystalline silica content — Part 2: Calculation method
EN 17289-3:2020, Characterization of bulk materials — Determination of a size-weighted fine fraction
and crystalline silica content — Part 3: Sedimentation method
ISO 16258-2:2015, Workplace air — Analysis of respirable crystalline silica by X-ray diffraction — Part 2:
Method by indirect analysis
3 Terms and definitions
For the purposes of this document, the terms and definitions given in EN 1540 and the following apply.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— IEC Electropedia: available at http://www.electropedia.org/
— ISO Online browsing platform: available at http://www.iso.org/obp
3.1
10th–percentile particle diameter
d
10
particle diameter corresponding to 10 % of the cumulative undersize distribution (by volume or by
mass)
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3.2
90th–percentile particle diameter
d
90
particle diameter corresponding to 90 % of the cumulative undersize distribution (by volume or by
mass)
3.3
between-samples standard deviation
S
s
standard deviation between the random samples used for homogeneity check
3.4
bulk sample
portion that is representative of the bulk material
3.5
coefficient of variation of the reproducibility
CV
R
ratio of standard deviation to the mean of test results produced under reproducibility conditions,
i.e. conditions where test results are obtained with the same method on identical test items in different
laboratories with different operators using different equipment
3.6
complex refractive index
n
p
refractive index of a particle, consisting of a real and an imaginary (absorption) part
Note 1 to entry: The complex refractive index of a particle can be expressed mathematically as
nn−×i k
pp p
where
i
is the square root of −1;
is the positive imaginary (absorption) part of the refractive index of a particle;
k
p
is the positive real part of the refractive index of a particle
n
p
[SOURCE: ISO 13320:2020, 3.1.5, [3] modified – Note 2 to entry deleted]
3.7
crystalline silica
SiO
2
silicon dioxide with Si and O orientated in a fixed pattern as opposed to a nonperiodic, random
molecular arrangement defined as amorphous
Note 1 to entry: The three most common crystalline forms of silica are quartz, tridymite, and cristobalite.
7
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3.8
equivalent Stokes diameter
equivalent spherical diameter
diameter of a sphere having the same rate of sedimentation and density as the particle for laminar flow
in a liquid
3.9
mass fraction of crystalline silica
w
CS
mass fraction of crystalline silica in the bulk sample, in percent (%)
3.10
median particle diameter
d
50
particle diameter, where 50 % of the particles, by volume or by mass, are smaller than this diameter
and 50 % are larger
3.11
mineral phase
homogeneous substance with a well-defined set of physical and chemical properties; it defines a
uniquely identifiable mineral
3.12
particle density
ratio of the mass of particles to the volume of the particles, in which closed pores are included
in the volume while open pores and volume between particles are excluded
3
Note 1 to entry: Particle density is typically determined using a pycnometer and has the dimension kg/m .
3.13
size-weighted fine fraction
SWFF
w
SWFF
fraction of the mass of a bulk material as determined by the size and density of the particles and a well-
defined probability function, in percent (%)
3.14
size-weighted fine fraction of crystalline silica
SWFFCS
w
SWFFCS
fraction of the mass of crystalline silica particles in the SWFF, in percent (%)
3.15
skeletal density
mass of a unit volume of the diatomaceous earth (DE) skeleton, inaccessible to Helium
3.16
standard deviation for proficiency assessment
σ
measure of dispersion used in the assessment of proficiency, based on the available information
[SOURCE: ISO 13528:2015, 3.4 [4]]
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3.17
supernatant
column of liquid that is separated from the total sedimentation liquid column which contains the solid
particles of interest
Note 1 to entry: See EN 17289-3:2020, Figure A.2.
3.18
z-score
z
standardized measure of laboratory bias, calculated using the assigned value and the standard
deviation for proficiency assessment
[SOURCE: ISO 13528:2015, 3.7]
4 Symbols and abbreviations
CS crystalline silica
DE diatomaceous earth
LD laser diffraction
PSD particle size distribution
FT-IR Fourier transform infrared spectroscopy
MMAD mass median aerodynamic diameter
RCS respirable crystalline silica
RI refractive index
SWFF size-weighted fine fraction
SWFFCS size-weighted fine fraction of crystalline silica
XRD X-ray powder diffractometry
5 Test methods
There are two ways to determine the SWFF and SWFFCS:
a) by calculation, as specified in EN 17289-2;
b) by sedimentation in a liquid, as specified in EN 17289-3.
The calculation method requires that the aerodynamic particle size distribution of the bulk material
is known. When SWFFCS needs to be determined this is often not possible since the PSD of the CS
in the sample cannot be determined separately from the rest of the sample. The CS can be finer
or coarser than the bulk of the sample. Instead, in this case the sedimentation method shall be used
to determine the SWFFCS.
The calculation method is easier and faster to perform. This can be a reason to choose the calculation
method over the sedimentation method; the assumption is then made that the size distributions
are the same so that SWFFCS can be calculated from the PSD of the whole sample. However, this can
only be done after experiments have shown that the results are accurate and consistently equal
or higher than the results from sedimentation for that particular bulk material.
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The sedimentation method is a good approximation for the determination of SWFF and SWFFCS.
However, when samples have a narrow size distribution and a median diameter ( d ) in the range
50
from 6 µm to 12 µm (aerodynamic) the method shall not be used since results will be too low.
Instead the calculation method shall be applied. This is possible because of the narrow size distribution.
In this case the difference in PSD between CS and bulk of the sample is small.
The analytical approach specified in these methods fulfils the expanded uncertainty requirements
of EN 482 [5]. Guidance on bias and uncertainties is given in Annex A.
Figure 1 gives a flowchart to assist the user in selecting the appropriate test method for the
determination of SWFF and SWFFCS. Both calculation and sedimentation methods are based
upon a number of assumptions, which are listed in EN 17289-2 and EN 17289-3, respectively.
Figure 1 — Selection of test method for SWFF and SWFFCS
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NOTE Experiments were performed on a series of minerals in order to make recommendations on the use
of the different methods (see Annex B).
6 Guidelines for the determination of crystalline silica
6.1 Preparation of sample to be analysed
Samples shall be extracted from the bulk material using a method, which will result in a representative
sample (for example, ISO 14488 [7], BS 3406-1 [6]), respecting the limitations of the analytical methods.
6.2 Sample preparation for further analysis by XRD and FT-IR
Sample preparation is specified in Annex C using XRD and FT-IR.
The content of crystalline silica of the sample shall be determined using techniques such as X-ray
Powder Diffractometry (XRD) as specified, for example, in EN 13925-1, EN 13925-2 and EN 13925-3
[8], [9], [10] and ISO 16258-2 or Fourier Transform Infrared Spectroscopy (FT-IR) as specified in
ISO 19087 [11].
NOTE 1 The sample preparation step in EN 13925-2 is applicable for both analytical methods.
NOTE 2 All paragraphs related to sampling in ISO 16258-2 and ISO 19087 are not applicable to this document.
NOTE 3 Omotoso et al. [12] and Chipera and Bish [13] specify quantitative mineral analysis.
7 Test report
The test report shall contain at least the following information:
a) reference to this document (“EN 17289-1”);
b) date of testing;
c) identification of test facility;
d) identification of contractor or subcontractor, if applicable;
e) identification of the test method used – calculation or sedimentation method;
f) identification of the method of sampling and sample preparation used;
g) identification of samples of test materials;
3
h) particle density of the sample, in kilograms per cubic metre (kg/m );
i) density of the substance of interest (for example, quartz, cristobalite), in kilograms per cubic metre
3
(kg/m );
j) the mass fraction of the substance of interest (for example, quartz, cristobalite) in the bulk sample,
in percent (%);
k) the mass fraction of SWFF and/or SWFFCS in the bulk sample, in percent (%).
The test report shall also include specific minimum requirements for the calculation and/or
sedimentation methods as follows:
1) For the calculation method:
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a) method of determination of PSD (for example, by laser diffraction (LD) analysis (specify wet or
dry and Mie or Fraunhofer), gravitational sedimentation method, particle time-of-flight
(TOF) method)
b) an example of a calculation sheet for determining SWFF by calculation can be found in Annex D
and on the Safe Silica website (https://safesilica.eu/safety-and-measurement/).
2) For the sedimentation method:
a) total sample mass that was dispersed, in grams [g];
b) type and volume of sedimentation liquid, in millilitres (ml);
c) temperature, density and viscosity of the liquid;
d) type of dispersants (if used);
e) method of dispersion;
f) sedimentation time, in seconds (s);
g) depth of the separated liquid column, in metres (m);
h) supernatant residue, in grams (g);
i) method of determination of substance of interest e.g. Quartz XRD or FT-IR;
j) fine fraction of CS in the supernatant, in percent (%).
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Annex A
(informative)
Bias and uncertainties
A.1 General
As with any method of analysis there are biases and uncertainties. These are investigated in this Annex.
A.2 looks at the biases arising from the size distribution measurement and in particular: the biases
arising from the different probability functions and the issues associated with the density of
multicomponent particles. The biases arising from three scenarios of increasing complexity are
compared with the ideal powder of a single mineral phase of crystalline silica. A.3 lists the uncertainties
associated with the calculation method (EN 17289-2) and sedimentation method (EN 17289-3).
With any method of analysis representative sampling is extremely important. A recognized method or
standard should be followed. The use of the methods specified in the sampling standards referenced in
ISO 14488 and BS 3406-1, will allow the sampling uncertainty to be calculated.
A.2 Bias between EN 481 and sedimentation SWFF probability function
and influence of density and mineral phase mass fraction
A.2.1 Bias between EN 481 and sedimentation SWFF probability curve
A.2.1.1 General
This subclause specifies the theoretical comparison between the respirable sampling convention
and the SWFF probability function.
A.2.1.2 Ideal powder, one mineral phase of known density and ideal SWFF measurement
The SWFF and respirable sampling conventions have been compared theoretically for an ideal
dispersed powder and ideal SWFF measurement (without bias or uncertainties) for which the particles
have the following characteristics:
— all particles are spherical;
— all particles have an identical and known density;
— all particles (independent of size) are completely dispersed in air and test liquid, respectively;
— no particle is attached to (agglomerated with) any other particle, neither when dispersed in air
nor when dispersed in the test liquid.
The comparison was carried out by calculating a bias map of the SWFF probability function / fraction
relative to the respirable fraction for the aerodynamic mass-weighted particle size distributions
specified in EN 13205-2 [14]. For such an ideal powder and an ideal measurement, it does not matter
whether the SWFF was determined using EN 17289-2 or EN 17289-3.
For this ideal situation, the bias between the two sampling conventions is small, generally within ± 5 %
except for particles greater than 6 μm where the bias is in the range from −5 % to −20 %. This is due
to the sedimentation method not sampling particles of more than 6 μm aerodynamic diameter ( d ).
ae
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A.2.2 Internal SWFF sedimentation bias
A.2.2.1 General
This subclause specifies the bias between SWFF 1 sedimentation (spherical non-agglomerated particles,
one mineral phase, density of quartz mixture) and SWFF 2 sedimentation (spherical non-agglomerated
particles, two mineral phases one of them being quartz, identical mass fraction of quartz to total mass
of the particle for all particles independently of particle size).
A.2.2.2 Ideal powder, two mineral phases of known density and ideal SWFF sedimentation
measurement
The SWFF 1 and SWFF 2 have been compared theoretically for ideal dispersed powders and ideal SWFF
measurement (without bias or uncertainties) for which the particles have the following characteristics:
SWFF 1:
— all particles are spherical;
— all particles have one mineral phase;
— all particles have an identical and known density (quartz density);
— all particles (independent of size) are completely dispersed in air and test liquid, respectively;
— no particle is attached to (agglomerated with) any other particle
...
SLOVENSKI STANDARD
oSIST prEN 17289-1:2019
01-februar-2019
[Not translated]
Characterization of bulk materials - Determination of a sizeweighted fine fraction and
crystalline silica content - Part 1: General information and choice of test methods
Charakterisierung von Schüttgütern - Bestimmung einer größengewichteten Feinfraktion
und des Anteils an kristallinem Quarz - Teil 1: Allgemeine Information und Auswahl der
Prüfverfahren
Ta slovenski standard je istoveten z: prEN 17289-1
ICS:
13.040.30 Kakovost zraka na delovnem Workplace atmospheres
mestu
oSIST prEN 17289-1:2019 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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oSIST prEN 17289-1:2019
DRAFT
EUROPEAN STANDARD
prEN 17289-1
NORME EUROPÉENNE
EUROPÄISCHE NORM
January 2019
ICS 13.040.30
English Version
Characterization of bulk materials - Determination of a
sizeweighted fine fraction and crystalline silica content -
Part 1: General information and choice of test methods
Charakterisierung von Schüttgütern - Bestimmung
einer größengewichteten Feinfraktion und des Anteils
an kristallinem Quarz - Teil 1: Allgemeine Information
und Auswahl der Prüfverfahren
This draft European Standard is submitted to CEN members for enquiry. It has been drawn up by the Technical Committee
CEN/TC 137.
If this draft becomes a European Standard, CEN members are bound to comply with the CEN/CENELEC Internal Regulations
which stipulate the conditions for giving this European Standard the status of a national standard without any alteration.
This draft European Standard was established by CEN in three official versions (English, French, German). A version in any other
language made by translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC
Management Centre has the same status as the official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey and United Kingdom.
Recipients of this draft are invited to submit, with their comments, notification of any relevant patent rights of which they are
aware and to provide supporting documentation.
Warning : This document is not a European Standard. It is distributed for review and comments. It is subject to change without
notice and shall not be referred to as a European Standard.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2019 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 17289-1:2019 E
worldwide for CEN national Members.
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Contents Page
European foreword . 3
Introduction . 4
1 Scope . 6
2 Normative references . 6
3 Terms and definitions . 6
4 Symbols and abbreviations . 9
5 Test methods . 9
6 Guidelines for the determination of crystalline silica . 11
6.1 Preparation of sample to be analysed . 11
6.2 Sample preparation for further analysis by XRD and FT-IR . 11
7 Test report . 11
Annex A (informative) Round robin test to establish a SWFF reference sample . 13
A.1 General . 13
A.2 Test material . 13
A.3 Evaluation and appraisal method . 14
A.4 Results . 15
Annex B (informative) Determination of CS in bulk samples using X-Ray diffraction (XRD)
or FT-IR spectroscopy . 17
B.1 General . 17
B.2 Preparation of bulk samples for determination of CS using XRD . 17
B.2.1 General . 17
B.2.2 Method 1: Bulk method . 17
B.2.2.1 General . 17
B.2.2.2 Preparation . 18
B.2.2.3 Measurement . 18
B.2.2.4 Calculation . 18
B.2.3 Method 2: Deposition method . 19
B.3 Preparation of bulk samples for determination of CS using FT-IR . 19
B.3.1 Identification of the interfering minerals . 19
B.3.2 Interferences removal . 20
B.3.3 Standards and sample preparation . 20
B.3.4 Operating conditions . 20
B.3.5 Measurement . 20
B.3.6 Determination of the quartz content . 21
Bibliography . 23
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European foreword
This document (prEN 17289-1:2019) has been prepared by Technical Committee CEN/TC 137
“Assessment of workplace exposure to chemical and biological agents”, the secretariat of which is held
by DIN.
This document is currently submitted to the CEN Enquiry.
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Introduction
A method was developed in the industrial minerals industry for the purpose of determining the “size
weighted relevant fine fraction” within the bulk material. This method provides the necessary
information to the users and allows them to compare bulk materials, by measuring the fine fraction, in
order for them to select the safest materials. It has been used in the industry and by institutes
previously under the acronym SWeRF. EN 17289 (all parts) is based on that industrial method and
describes the analytical methods to determine the difference between materials with coarse quartz and
fine quartz, e.g. sands versus flour.
As further activities with the material (intentional or otherwise) might change the particle size
distribution, the size weighted fine fraction might also change. Therefore, the method reports (in terms
of the mass percentages in the bulk material) both, the total CS and the estimated size weighted fine
fraction of CS.
Conventions as described in EN 481 can be used as input for this document. However, the output of this
document is not related to the respirable fraction and cannot be used for workplace exposure
measurements.
EN 17289 (all parts) describes two procedures that can be used to estimate the size weighted fine
fraction (SWFF) in bulk materials. It also describes how the SWFF, once separated, can be further
analysed to measure the content of crystalline silica (SWFF ). The method can be used for comparing
cs
the fine fraction in different bulk samples. EN 17289 (all parts) uses the term fine fraction to indicate
that it does not analyse airborne particles, but it evaluates the proportion of particles in a bulk material
that, based on their particle size, have a potential to be respirable if they were to become airborne.
EN 17289 (all parts) also allows for the size weighted fine fraction of crystalline silica (SWFF ) particles
cs
in bulk materials to be evaluated in terms of mass fraction in percent, if the fraction separated is
subsequently analysed by a suitable method.
In comparison of similar bulk materials, in which the particle size distribution is the only variable, the
SWFF can provide useful information to guide material selection. For example, leaving all other factors
aside, a bulk material with a lower SWFF value can pose less of a risk in terms of potential occupational
exposure. For the actual exposure at the workplace, the handling etc of the material, will play a major
role.
Concentrations of respirable dust, or respirable crystalline silica (RCS), in the workplace air, resulting
from processing and handling of bulk materials, will depend on a wide variety of factors and these
concentrations cannot be estimated using SWFF or SWFFcs values. SWFF and SWFFcs values are not to
be used for occupational exposure assessments as they have no relationship with occupational
exposure.
The evaluation of bulk materials using SWFF is complementary to determining the dustiness according
to EN 15051-1 [1].
The difference between EN 17289 (all parts) and EN 15051-1 is that SWFF quantifies the fine fraction in
a bulk material while dustiness quantifies the respirable, thoracic and inhalable dust made airborne
from the bulk material after a specific activity (it characterizes the material with relation to the
workplace atmosphere when working with the bulk material).
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EN 17289 Characterization of bulk materials — Determination of a size-weighted fine fraction and
crystalline silica content consists of the following parts:
— Part 1: General information and choice of test methods;
— Part 2: Calculation method;
— Part 3: Sedimentation method.
Part 1 gives information on how to choose the most appropriate method as well as a guideline for the
determination of crystalline silica. A calculation method based on particle size distribution is described
in Part 2. Part 3 describes a method using sedimentation.
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1 Scope
This document specifies the the requirements and choice of test method for the determination of the
size weighted fine fraction (SWFF) and the size weighted fine fraction of crystalline silica (SWFF ) in
CS
bulk materials.
This document gives also guidance on the preparation of the sample and determination of crystalline
silica by XRD and FT-IR.
NOTE prEN 17289-2:2019 specifies a method to estimate the size-weighted fine fraction from a measured
particle size distribution and assumes that the particle size distribution of the crystalline silica particles is the
same as the other particles present in the bulk material. prEN 17289-3:2019 specifies a method using a liquid
sedimentation technique to determine the size-weighted fine fraction of crystalline silica. Both methods are based
upon a number of limitations and assumptions, which are listed in prEN 17289-2:2019 and prEN 17289-3:2019,
respectively. The method in prEN 17289-3:2019 can also be used for other constituents, if investigated and
validated.
This document is applicable for bulk materials which have been fully investigated and validated. The
criteria for the materials are described in prEN 17289-2:2019 and prEN 17289-3:2019. This includes
industrial minerals which can contain crystalline silica such as quartz, clay, kaolin, talc, feldspar, mica,
cristobalite, vermiculite, diatomaceous earth, barite, andalusite, iron ore, chromite etc.
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements of this document. For dated references, only the edition cited applies. For
undated references, the latest edition of the referenced document (including any amendments) applies.
EN 1540:2011, Workplace exposure - Terminology
prEN 17289-2:2019, Characterization of bulk materials – Determination of a size-weighted fine fraction
and crystalline silica content — Part 2: Calculation method
prEN 17289-3:2019, Characterization of bulk materials – Determination of a size-weighted fine fraction
and crystalline silica content — Part 3: Sedimentation method
ISO 16258-2, Workplace air — Analysis of respirable crystalline silica by X-ray diffraction — Part 2:
Method by indirect analysis
ISO 24095, Workplace air — Guidance for the measurement of respirable crystalline silica
3 Terms and definitions
For the purposes of this document, the terms and definitions given in EN 1540:2011 and the following
apply.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— IEC Electropedia: available at http://www.electropedia.org/
— ISO Online browsing platform: available at http://www.iso.org/obp
3.1
between-samples standard deviation
Ss
standard deviation between the random samples used for homogeneity check
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3.2
bulk density
ratio of the mass of a quantity of dry granular material to the total volume of its grains, including the
volume of any closed pores within the grains
[SOURCE: ISO 836: 2001[3]]
3.3
bulk sample
portion that is representative of the bulk material
3.4
coefficient of variation of the reproducibility
CV
R
ratio of standard deviation to the mean of test results produced under reproducibility conditions, i.e.
conditions where test results are obtained with the same method on identical test items in different
laboratories with different operators using different equipment
[SOURCE: ISO 5725-1[4]]
3.5
complex refractive index
n
p
refractive index of a particle, consisting of a real and an imaginary (absorption) part
Note 1 to entry: The complex refractive index of a particle can be expressed mathematically as
n m−×ik
pp p
where
i is the square root of −1;
k is the positive imaginary (absorption) part of the refractive index of a particle;
p
m is the positive real part of the refractive index of a particle
p
[SOURCE: ISO 13320] [5]
3.6
crystalline silica
SiO
2
silicon dioxide with Si and O orientated in a fixed pattern as opposed to a nonperiodic, random
molecular arrangement defined as amorphous
Note 1 to entry: The three most common crystalline forms of silica are quartz, tridymite, and cristobalite.
3.7
D
10
particle diameter corresponding to 10 % of the cumulative undersize distribution (by volume or by
mass)
[SOURCE: ISO 13320]
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3.8
D median particle diameter
50
particle diameter, where 50 % of the particles – by volume or by mass – are smaller than this diameter
and 50 % are larger
[SOURCE: Adapted from ISO 13320]
3.9
D
90
particle diameter corresponding to 90 % of the cumulative undersize distribution (by volume or by
mass)
[SOURCE: ISO 13320]
3.10
equivalent Stokes diameter
equivalent spherical diameter
diameter of a sphere having the same rate of sedimentation and density as the particle for laminar flow
in a liquid
3.11
mineral phase
homogeneous substance with a well-defined set of physical and chemical properties; it defines a
uniquely identifiable mineral
3.12
relative density
ratio of the density of a substance to the density of a given reference material
3.13
size weighted fine fraction
SWFF
proportion of mass of particles in a bulk material below a well-defined probability function
3.15
skeletal density
mass of a unit volume of the Diatomaceous Earth (DE) skeleton, inaccessible to Helium
3.16
standard deviation for proficiency assessment
σ
measure of dispersion used in the assessment of proficiency, based on the available information
[SOURCE: ISO 13528[6]]
3.17
supernatant
column of liquid that is separated from the total sedimentation liquid column which contains the solid
particles of interest
Note 1 to entry: See prEN 17289-3:2018, Figure A.2.
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3.18
SWFF
CS
proportion of crystalline silica particles in a bulk material below a well-defined probability function
3.19
z-score
z
standardized measure of laboratory bias, calculated using the assigned value and the standard
deviation for proficiency assessment
[SOURCE: EN ISO/IEC 17043[7]]
4 Symbols and abbreviations
CS Crystalline Silica
DE Diatomaceous Earth
PSD Particle Size Distribution
FT-IR Fourier Transform Infrared Spectroscopy
XRD X-ray Powder Diffractometry
SWFF Size Weighted Fine Fraction
SWFF Size Weighted Fine Fraction of crystalline silica
CS
5 Test methods
There are two ways to determine the SWFF and SWFF :
CS
a) by calculation, as described in prEN 17289-2:2019;
b) by sedimentation in a liquid, as described in prEN 17289-3:2019.
The calculation method requires that the aerodynamic particle size distribution of the bulk material is
known. When SWFF needs to be determined this is often not possible since the PSD of the CS in the
cs
sample cannot be determined separately from the rest of the sample. The CS can be finer or coarser
than the bulk of the sample. Instead, in this case the sedimentation method shall be used to determine
the SWFF .
cs
The calculation method is easier and faster to perform. This can be a reason to choose the calculation
method over the sedimentation method; the assumption is then made that the size distributions are the
can be calculated from the PSD of the whole sample. However, this can only be
same so that SWFFcs
done after experiments have shown that the results are accurate and consistently equal or higher than
the results from sedimentation for that particular bulk material.
The sedimentation method is a good approximation for the determination of SWFF and SWFF .
cs
However, when samples have a narrow size distribution and a median diameter (D ) in the range from
50
6 µm to 12 µm (aerodynamic) the method shall not be used since results will be too low. Instead the
calculation method shall be applied. This is possible because of the narrow size distribution. In this case
the difference in PSD between CS and bulk of the sample is small.
NOTE The method given in prEN 17289-2:2018 (first measuring the particle size distribution and thereafter
calculate the SWFF based on this size distribution), overestimates the SWFF if the laser diffraction measurements
are accurate, otherwise the bias is unknown. For non-spherical particles, the liquid sedimentation method (see
prEN 17289-3:2018) overestimates the SWFF.
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Figure 1 gives a flowchart to assist the user in selecting the appropriate test method.
Figure 1 — Selection of test method
NOTE Experiments were performed on a series of minerals in order to make recommendations on the use of
the different methods (see Annex A).
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6 Guidelines for the determination of crystalline silica
6.1 Preparation of sample to be analysed
Samples shall be extracted from the bulk material using a method, which will result in a representative
sample (e.g. DIN 51701-3 [8], BS 3406-1 [9]).
6.2 Sample preparation for further analysis by XRD and FT-IR
Sample preparation is described in Annex B using XRD and FT-IR.
The content of crystalline silica of the sample shall be determined using techniques such as X-ray
Powder Diffractometry (XRD) as described e.g. in EN 13925-1, EN 13925-2 and EN 13925-3 [10, 11, 12]
and ISO 16258-2 [13] or Fourier Transform Infrared Spectroscopy (FT-IR) as described in ISO 19087
[14].
NOTE 1 The sample preparation step in EN 13925-2 is applicable for both analytical methods.
NOTE 2 All paragraphs related to sampling in ISO 16258-2 and ISO 19087 are not applicable to this document.
NOTE 3 Omotoso et al. [15] and Chipera and Bish [16] describe quantitative mineral analysis.
7 Test report
The test report shall contain at least the following information:
a) reference to this document (“EN 17289-1”)
b) date of testing;
c) identification of test house and test personnel;
d) identification of contractor or subcontractor, if applicable;
e) identification of the test method used – calculation or sedimentation method;
f) identification of samples of test materials;
3
g) average bulk density of the sample, in kg/m ;
3
h) density of the crystalline silica polymorph of interest (e.g. quartz, cristobalite etc.), in kg/m
i) the mass fraction of total CS in the bulk sample, in %;
j) the mass fraction of SWFF in the bulk sample, in %.
cs
The test report shall also include specific minimum requirements for the calculation and/or
sedimentation methods as follows:
1) For the calculation method:
i) determination of PSD by laser diffraction analysis – LD-Fraunhofer, LD-Mie or Sedimentation X-
Ray;
ii) an example of a calculation sheet for determining SWFF by calculation can be found on the
crystalline silica website
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(https://www.crystallinesilica.eu/sites/crystallinesilica.eu/files/SWeRF%20calculation%
20sedimentation_version%202015%2004%2024.xlsx) and the SWFF calculation xls sheet.
2) For the sedimentation method:
i) total sample mass that was dispersed, in g;
ii) type and volume of sedimentation liquid;
iii) temperature, density and viscosity of the liquid;
iv) type of dispersants (if used);
v) method of dispersion;
vi) sedimentation time, in s;
vii) depth of the separated liquid column, in m;
viii) supernatant residue, in g;
ix) method of determination of substance of interest e.g. Quartz XRD or FT-IR
x) fine fraction of CS in the supernatant, in %.
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Annex A
(informative)
Round robin test to establish a SWFF reference sample
A.1 General
The IMA-Europe Metrology Working Group has arranged a round robin test in order to make a SWFF
reference sample available. In this Annex, the most relevant results are summarized.
NOTE A full report (Examination Report No. 20100437, not published) on this work is available from the IMA
Metrology WG.
A.2 Test material
Typical quartz flour from a German quartz production company was used as the test material. It was
produced from processed silica sand of Frechen deposit by iron-free grinding with subsequent air
separation.
Essentially the mass fraction of quartz 100 %, therefore in this case SWFF is equal to SWFF . Further,
cs
because the test material consists only of quartz, hence the particle density is constant and in case of
this round robin the mass fraction (w/w-%) is equal to the volume fraction (v/v-%).
A 75 kg sample was homogenized and divided by coning and quartering to give a number of
representative portions, in accordance with ISO 14488 [17]. Reference samples are still available upon
request.
For further material data of the flour sample, see A.1, Note. Sample homogeneity was checked by laser
diffraction at the central laboratory of the German quartz production company. A random sample from
each of the 50 subsamples was measured and evaluated (Fraunhofer approximation).
In accordance with ISO 13528:2015, B.2 samples may be considered as homogenous, if they fulfil
Formula (A.1):
s ≤×0,3 δ (A.1)
s
where
s is the between-samples standard deviation;
s
δ is the standard deviation for proficiency assessment.
Formula (A.1) compares s , which is the standard deviation between the random samples of the
s
50 subsamples, with δ . According to ISO 13528, the standard deviation for proficiency assessment was
derived from the requirements for repeatability of laser diffraction devices given in ISO 13320. This
document claims for samples with particles smaller than 10 μm that the coefficient of variation for d
50
should be smaller than 6 % and for d and d smaller than 10 %.
10 90
The subsamples comply with this requirement of ISO 13528 (according to Table 1). Therefore, they are
adequately homogeneous.
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Table A.1 — Homogeneity check (according to ISO 13528:2015, B.2) by laser diffraction
(Fraunhofer) with 50 subsamples of the SWFF reference sample
Passing Passing Passing
Parameter
D D D
10 50 90
Mean (µm) 0,83 3,18 9,70
abs
Between-samples standard deviation (s ), absolute
s
0,01 0,02 0,04
(µm)
rel
Between-samples standard deviation (s ), relative
s
1,2 0,6 0,4
(%)
Standard deviation for proficiency assessment (δ )
10 6 10
(%)
0,3× δ (%) 3 1,8 3
rel
Fulfil requirement: s ≤ 0,3 × δ (%) yes yes yes
s
A.3 Evaluation and appraisal method
The main focus of the round robin test is the estimation of SWFF by laser diffraction and gravitational
liquid sedimentation method analysis. For the gravitational liquid sedimentation method analyses,
automated X-ray sedimentation was used according to ISO 13317-3 [18].
For laser diffraction, results based on the Fraunhofer theory were requested in a first run. The Mie
theory provides that particles “are homogeneous, isotropic and their optical properties are known”
(according to ISO 13320). Because these data, especially effects depending on shape and kind of surface
(e.g. rough or smooth, transparent or opaque) of the used quartz flour were not known, the Fraunhofer
theory was in principle preferred. Nevertheless, some laboratories sent in results using the Mie theory.
The initial laser diffraction data using the Mie theory showed large differences between the data of the
different laboratories. When the results were evaluated it became clear that the participants used
different optical data. Therefore, it was decided that analyses with harmonized Mie parameters from
literature (e.g. ISO 13320) should be carried out in a second run. The following parameters were
defined:
— Refractive index of quartz (n ): 1,54;
p
— Imaginary index of quartz (kp): 0,10;
): 1,33.
— Absorption coefficient of medium/water (nm
The mean values of each participating laboratory were used as the basis of the evaluation. The results
were first checked for outliers after Dixon (according to DIN 53804-1 [19]) with significance of α = 0,05.
The statistical model is based on the means and standard devi
...
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