The purpose of this document is to allow users to determine the fine fraction with the calculation
method. It also describes the assumptions and preconditions to be met in order for this method
to be valid. This calculation method is applicable only after experiments have shown that the
results are accurate and consistently equal or higher than the results from sedimentation, as
described in Part 2, for that particular bulk material.
For preparation of the sample and determination of crystalline silica by XRD and FTIR
the users
can refer to Part 1.
An informative annex describes a specific method for the evaluation of the FF recommended for
diatomaceous earth bulk materials. Due to the internal porosity of diatomaceous earth, the
general instructions given in this part of the standard are adapted in order to take into account
the material’s effective density.
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 this part and Part 2. 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 3: Sedimentationsverfahren

Dieses Dokument legt die Bestimmung der größengewichteten Feinfraktion (SWFF) und der größen-gewichteten Feinfraktion von kristallinem Quarz (SWFFCS) in Schüttgütern mit einem Sedimentations-verfahren fest, bei dem eine Sedimentationstechnik mit Flüssigkeit eingesetzt wird.
Der Zweck dieses Dokuments besteht darin, Anwendern die Bewertung von Schüttgütern hinsichtlich deren größengewichteter Feinfraktion und des Gehalts an kristallinem Quarz zu ermöglichen.
ANMERKUNG   Zur Probenvorbereitung und zur Bestimmung von kristallinem Quarz durch Röntgenpulverdiffrakto-metrie (en: X-ray powder diffractometry, XRD) oder Fourier-Transformations-Infrarot-Spektroskopie (FT-IR) siehe EN 17289-1.
Spezielle Verfahren für die Bewertung der SWFF bestimmter Schüttgüter werden in mehreren Anhängen festgelegt.
Dieses Dokument ist für kristallinen Quarz enthaltende Schüttgüter anwendbar, die zur Bewertung der größengewichteten Feinfraktion und des kristallinen Quarzes vollständig 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 3 : Méthode par sédimentation

Le présent document spécifie 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 au moyen d’une méthode par sédimentation en utilisant une technique de sédimentation dans un liquide.
L’objectif du présent document est de permettre aux utilisateurs d’évaluer des matériaux en vrac en ce qui concerne leur fraction fine pondérée par taille et leur teneur en silice cristalline.
NOTE   Pour la préparation de l’échantillon et le dosage de la silice cristalline par l’analyse de poudre par diffraction de rayons X (XRD) et la spectroscopie infrarouge à transformée de Fourier (FT-IR), voir le FprEN 17289-1.
Des méthodes spécifiques pour l’évaluation de la SWFF de matériaux en vrac particuliers sont décrites dans plusieurs annexes.
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 - 3. del: Metoda sedimentacije

General Information

Status
Published
Public Enquiry End Date
04-Mar-2019
Publication Date
11-Jan-2021
Technical Committee
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
05-Jan-2021
Due Date
12-Mar-2021
Completion Date
12-Jan-2021

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SLOVENSKI STANDARD
SIST EN 17289-3:2021
01-februar-2021

Karakterizacija razsutih materialov - Določanje velikostno utežene fine frakcije in

deleža kristaliničnega kremena - 3. del: Metoda sedimentacije

Characterization of bulk materials - Determination of a size-weighted fine fraction and

crystalline silica content - Part 3: Sedimentation method

Charakterisierung von Schüttgütern - Bestimmung einer größengewichteten Feinfraktion

und des Anteils an kristallinem Quarz - Teil 3: Sedimentationsverfahren

Caractérisation des matériaux en vrac - Détermination de la fraction fine pondérée par

taille et de la teneur en silice cristalline - Partie 3 : Méthode par sédimentation

Ta slovenski standard je istoveten z: EN 17289-3:2020
ICS:
13.040.30 Kakovost zraka na delovnem Workplace atmospheres
mestu
SIST EN 17289-3:2021 en,fr,de

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

---------------------- Page: 1 ----------------------
SIST EN 17289-3:2021
---------------------- Page: 2 ----------------------
SIST EN 17289-3:2021
EN 17289-3
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 3: Sedimentation method

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 3 : Méthode par sédimentation an kristallinem Quarz - Teil 3:

Sedimentationsverfahren
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 17289-3:2020 E

worldwide for CEN national Members.
---------------------- Page: 3 ----------------------
SIST EN 17289-3:2021
EN 17289-3:2020 (E)
Contents Page

European foreword ....................................................................................................................................................... 4

Introduction .................................................................................................................................................................... 5

1 Scope .................................................................................................................................................................... 7

2 Normative references .................................................................................................................................... 7

3 Terms and definitions ................................................................................................................................... 7

4 Symbols and abbreviations ......................................................................................................................... 7

5 Assumptions ...................................................................................................................................................... 8

6 Determination of SWFF and SWFFCS by sedimentation ................................................................ 10

6.1 Determination of sedimentation time .................................................................................................. 10

6.2 Selection of sedimentation liquid .......................................................................................................... 10

6.3 Sample preparation, sedimentation and SWFF determination ................................................... 11

6.4 Use of a dispersant of deflocculant ........................................................................................................ 13

6.5 Determination of the SWFF and SWFFCS of mixtures of phases with different particle

densities .......................................................................................................................................................... 13

6.6 SWFF of mixtures ......................................................................................................................................... 13

6.7 SWFFCS of mixtures of homogeneous particles ................................................................................ 13

6.8 SWFFCS of mixtures of heterogeneous particles .............................................................................. 14

Annex A (normative) Separation of the SWFF by sedimentation .............................................................. 16

A.1 Derivation for calculating the sedimentation parameters ........................................................... 16

A.2 Calculation of the SWFF after sedimentation ..................................................................................... 20

Annex B (normative) Determination and isolation of the size-weighted fine fraction (SWFF)

of kaolins and kaolinitic clays by sedimentation ............................................................................. 22

B.1 General ............................................................................................................................................................. 22

B.2 Use range ......................................................................................................................................................... 22

B.3 Equipment and consumables ................................................................................................................... 22

B.4 Method ............................................................................................................................................................. 23

B.5 Figures .............................................................................................................................................................. 25

Annex C (normative) Other minerals which can be treated in a similar way to

kaolins/kaolinitic clays for SWFF and SWFFCS determination ................................................... 28

C.1 General ............................................................................................................................................................. 28

C.2 Andalusite ....................................................................................................................................................... 28

C.3 Mica ................................................................................................................................................................... 29

C.4 Vermiculite ..................................................................................................................................................... 30

C.5 Talc .................................................................................................................................................................... 30

Annex D (normative) Determination of the size-weighted fine fraction (SWFF and SWFFCS)

of Diatomaceous Earth (DE) by sedimentation ................................................................................. 32

D.1 General ............................................................................................................................................................. 32

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SIST EN 17289-3:2021
EN 17289-3:2020 (E)

D.2 Categories of diatomaceous earth .......................................................................................................... 32

D.3 Equipment and consumables ................................................................................................................... 32

D.4 Method .............................................................................................................................................................. 32

D.5 Determination of SWFF by sedimentation .......................................................................................... 33

D.6 Determination of SWFFCS .......................................................................................................................... 33

D.7 Example ............................................................................................................................................................ 33

Annex E (normative) Determination of the size-weighted fine fraction (SWFF) of feldspar

products by sedimentation ....................................................................................................................... 35

E.1 General ............................................................................................................................................................. 35

E.2 Use range ......................................................................................................................................................... 35

E.3 Consumables .................................................................................................................................................. 35

E.4 Method .............................................................................................................................................................. 35

Bibliography ................................................................................................................................................................. 40

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SIST EN 17289-3:2021
EN 17289-3:2020 (E)
European foreword

This document (EN 17289-3:2020) 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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SIST EN 17289-3:2021
EN 17289-3:2020 (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, e.g. 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 can be used as input for this document. However, the output of this

document is not related to the respirable fraction at the workplace 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 [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 (dustiness characterizes the material with relation to the

workplace atmosphere when working with the bulk material).
---------------------- Page: 7 ----------------------
SIST EN 17289-3:2021
EN 17289-3:2020 (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.
---------------------- Page: 8 ----------------------
SIST EN 17289-3:2021
EN 17289-3:2020 (E)
1 Scope

This document specifies the determination of the size-weighted fine fraction (SWFF) and the size-

weighted fine fraction of crystalline silica (SWFFCS) in bulk materials by means of a sedimentation

method using a liquid sedimentation technique.

The purpose of this document is to allow users to evaluate bulk materials with regard to their size-

weighted fine fraction and crystalline silica content.

NOTE For preparation of the sample and determination of crystalline silica by X-ray Powder Diffractometry

(XRD) or Fourier Transform Infrared Spectroscopy (FT-IR) see EN 17289-1.

Specific methods for the evaluation of SWFF for specific bulk materials are specified in several annexes.

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 481, Workplace atmospheres — Size fraction definitions for measurement of airborne particles

EN 1540, Workplace exposure — Terminology

EN 17289-1, Characterization of bulk materials — Determination of a size-weighted fine fraction and

crystalline silica content — Part 1: General information and choice of test methods

EN 17289-2:2020, Characterization of bulk materials — Determination of a size-weighted fine fraction

and crystalline silica content — Part 2: Calculation method
3 Terms and definitions

For the purposes of this document, the terms and definitions given in EN 1540 and EN 17289-1 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
4 Symbols and abbreviations
CS crystalline silica
PSD particle size distribution
SWFF size-weighted fine fraction
SWFFCS size-weighted fine fraction of crystalline silica
---------------------- Page: 9 ----------------------
SIST EN 17289-3:2021
EN 17289-3:2020 (E)
5 Assumptions
The sedimentation method is based on the following assumptions:

a) all liquid that is extracted from the sedimentation vessel only comes from the space above the

extraction nozzle, and not from the space below the extraction nozzle. If this is not the case this will

result in a higher SWFF.

b) the particle size distribution of the bulk material is constant over the particle size range of interest,

i.e. from 1 µm to 12 µm (aerodynamic).

A constant particle size distribution is a PSD with a function that has a derivative which is constant,

see Formula (1). It is considered constant when classes of the same size contain the same fraction

of the total amount.
dd−
( )
min
fd × 100 (1)
( )
dd−
( )
max min
where
is the cumulative particle size distribution;
( )
d is the particle size, in micrometres (µm);
is the minimum particle size, in micrometres (µm);
min
is the maximum particle size, in micrometres (µm).
max
NOTE d ≤ d ≤ d . See Figure 1 for an example.
min max
---------------------- Page: 10 ----------------------
SIST EN 17289-3:2021
EN 17289-3:2020 (E)
Key
X particle diameter (µm)
Y fraction (%)
1 constant cumulative particle size distribution
Figure 1 — Example of a constant cumulative PSD with d = 0,5 µm and d = 25 µm
min max

c) the particle size distribution of the sample does not have a narrow size distribution (relative span

d − d / dd× < 1,5) and at the same time, have a d in the range from 2 µm to
( )
90 10 90 10 ae,50

12 µm. Otherwise the error made could be more than 1 % (absolute value).For a relative span less

than 1,5 µm and d in the range from 2 µm to 6 µm, sedimentation overestimates the SWFF.

ae,50

For a relative span less than 1,5 µm and d in the range from 6 µm to 12 µm SWFFCS is

ae,50

underestimated. It is therefore recommended in these cases to use the calculation method instead

to determine SWFF. The mean reason for determining the SWFF using sedimentation is because,

although the PSD of the whole sample is known, the PSD of the crystallin silica is not. The CS can

either be in the coarse part of the PSD or in the fine part. However, in the case of a narrow

distribution it is likely to assume the CS practically has the same PSD as the whole sample. Since the

PSD is so narrow, sample and CS particles are automatically close to each other.

d) Stokes law is only valid for particles settling in a medium at low Reynolds number. The velocity of a

particle settling in a medium is limited by the drag force and this depends on the Reynolds number

for that particle. Although the density of liquids is much higher, so is their viscosity so that in the

end the difference between the Reynolds number of a particle in air and, for example, in water is

only a factor of 5. And although the constants for calculating the drag coefficient of particles depend

on the Reynolds number, the variation with Reynolds number within this range is very small and

can be neglected. Therefore, the dynamic form factor is assumed to be equal in both air and liquid.

e) in the material of interest all particles have the same and known particle density.

f) the sub sample is representative of the bulk material.

If these assumptions are not met, the calculation method shall be used as specified in EN 17289-2.

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SIST EN 17289-3:2021
EN 17289-3:2020 (E)
6 Determination of SWFF and SWFFCS by sedimentation
6.1 Determination of sedimentation time

The sedimentation time shall be calculated by Formula (2), which is based on Stokes’ law and the

convention given in EN 481. The derivation of it is given in Annex A.
18η 0
(2)
th=××
sup
ρρ− g
( ) 
× I
where

is the time, in seconds (s), at which the size-weighted particle fraction of the collected

supernatant in an optimal way approaches the fraction collected according to the sampling

convention of respirable dust (see EN 481);

is the height of the column of supernatant liquid that is extracted at the calculated time, in

sup
metres (m);
is the viscosity of the fluid, in kilograms per metre per second (kg/m·s);
is the acceleration due to gravity, in metres per square seconds (m/s );
is the particle density of the particles, in kilograms per cubic metre (kg/m );
is the density of the liquid medium, in kilograms per cubic metre (kg/m );
3 3
is the unit density (1 000 kg/m [ = 1 g/cm ]);
I is the respirable convention integral: 4,281 × 10 m.

For determining the SWFF of a sample, the particle density of that sample shall be used for ρ .

When SWFFCS is determined, the density of the crystalline silica polymorph of interest

(quartz or cristobalite) shall be used.

SWFFCS shall be used when the CS is the constituent of only interest. For the SWFFCS only the

sedimentation rate for the quartz (cristobalite etc.) particles are relevant. The fact that the

sedimentation time for other particles is not correct is not important since SWFFCS is needed. When the

SWFF of material with a different particle density is needed the procedure shall be repeated

with a sedimentation time as calculated by Formula (1) with the particle density of that material.

The height h to be separated is usually set at 0,1 m, but other heights can be used depending on the

sup

nature of the sample. In any case, the height h shall be less than half the total height h of the

sup tot
sedimentation liquid in the measuring cylinder (see B.4).
6.2 Selection of sedimentation liquid

A suitable sedimentation liquid shall be selected in order to meet the following requirements:

— the particles in the sample shall be completely de-agglomerated;
— the particles in the sample shall not dissolve, swell or disintegrate;
---------------------- Page: 12 ----------------------
SIST EN 17289-3:2021
EN 17289-3:2020 (E)
— the particles in the sample shall not react.
NOTE 1 Water is in most cases a suitable sedimentation liquid.

When necessary, a dispersant or deflocculant additive shall be used in appropriate quantities.

NOTE 2 De-agglomeration is the process where particles are separated from each other without breaking the

particles. Disintegration is the process in which particles are broken.
6.3 Sample preparation, sedimentation and SWFF determination

In order to ensure that the sedimentation is performed correctly, the Andreasen pipette method is used

[2], [3].

The following steps shall be executed to determine the SWFF or SWFFCS of a sample.

a) take a representative subsample of the bulk sample of approximately 1,0 g;

For coarse bulk material a pre-preparation is required to respect the limitations of the Andreasen

pipette method, e.g. sieving.
b) determine the mass m of the sample with a precision of 0,001 g;
tot

c) disperse the sample in 50 ml of sedimentation liquid in a 100 ml pre-weighted, dry and clean

beaker. The mass of the beaker shall also be determined with a precision of 0,001 g (see also

ISO 13317-2);

d) treat the sample in an ultrasonic bath or shaker until completely de-agglomerated;

NOTE 1 The de-agglomeration time will depend on the type of material.

e) if necessary, based on the characterization of the bulk material, add a suitable dispersant or

deflocculant to keep the particles from flocculating or coagulating. The use of this product will lead

to additional steps specified in 6.4;
For unknown bulk materials a full characterization is needed.

f) pour the dispersed sample in a graduated cylinder with 250 ml volume. Rinse out the sample jar

using the sedimentation liquid to ensure that no residue remains. Fill the cylinder up to 250 ml

with sedimentation liquid. Seal the open end of the cylinder and shake the contents thoroughly.

Then replenish the cylinder up till 250 ml and homogenize;

NOTE 2 The volume of solids is maximum 0,2 % of the volume of the total liquid to ensure unhindered

sedimentation of the separate particles.

For some minerals it can be required to use a plunger agitator. With the cylinder in place, agitate.

Then remove the plunger to replenish the cylinder up till 250 ml and homogenize.

g) place the cylinder in a location where it is at constant temperature and free from effects that could

cause currents in the liquid. The constant temperature can be achieved when using a water bath.

Leave to settle for the calculated time ( t ). Determine the height of the liquid column (m);

tot
---------------------- Page: 13 ----------------------
SIST EN 17289-3:2021
EN 17289-3:2020 (E)

h) from the cylinder, after calculated time ( t ), lower a pipette to h below the surface, draw the

sup

volume of the supernatant ( V ) above the tip of the pipette with a siphon or pipette and transfer

into the pre-weighed beaker.

Make sure that, whilst using the pipette, the tip of the pipette remains in the same place in the

cylinder; do not insert it deeper as the level descends;

NOTE 3 Placing a clip on the pipette and attaching it to the edge of the cylinder makes it easier to keep the

pipette in the right place.

i) place the beaker containing the supernatant on a hot plate to evaporate the liquid and heat gently

until dry. Then place the beaker in the oven at about 103 °C for at least 1 h or longer until

completely dry and transfer into a desiccator, leaving it to cool down to ambient temperature;

j) re-weigh the beaker to within an accuracy of 0,001 g and note the post-weight. Determine the mass

of the residue m by subtracting the mass of the pre-weighted beaker;

NOTE 4 The above procedure is repeated three times in order to check the reproducibility of the sedimentation

method for SWFF determination.
k) determine the SWFF of the sample by using Formula (3):
hm×
tot r
w × 100 (3)
SWFF
hm×
sup tot
where
is the size-weighted fine fraction, in percent (%);
SWFF

is the height of the total column of fluid that is used for sedimentation, in metres (m);

tot

is the height of the column of supernatant liquid that is extracted at the calculated time, in

sup
metres (m);
is the total mass that was dispersed, in grams (g);
tot

is the mass of the residue in the extracted supernatant, in grams (g) (see Figure A.2).

l) the SWFFCS of the sample shall be calculated by using Formula (4):
hm×
tot r
w × w (4)
SWFFCS CS
hm×
sup tot
where
is the size-weighted fine fraction of crystalline silica, in percent (%);
SWFFCS

is the height of the total column of fluid that is used for sedimentation, in metres (m);

tot

is the height of the column of supernatant liquid that is extracted at the calculated time, in

sup
metres (m);
---------------------- Page: 14 ----------------------
SIST EN 17289-3:2021
EN 17289-3:2020 (E)
is the total mass that was dispersed, in grams (g);
tot
is the mass of the residue in the extracted supernatant, in grams (g);
is the mass frac
...

SLOVENSKI STANDARD
oSIST prEN 17289-3:2019
01-februar-2019
[Not translated]

Characterization of bulk materials - Determination of a sizeweighted fine fraction and

crystalline silica content - Part 3: Calculation method

Charakterisierung von Schüttgütern - Bestimmung einer größengewichteten Feinfraktion

und des Anteils an kristallinem Quarz - Teil 3: Berechnungsverfahren
Ta slovenski standard je istoveten z: prEN 17289-3
ICS:
13.040.30 Kakovost zraka na delovnem Workplace atmospheres
mestu
oSIST prEN 17289-3:2019 en,fr,de

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oSIST prEN 17289-3:2019
DRAFT
EUROPEAN STANDARD
prEN 17289-3
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 3: Calculation method
Charakterisierung von Schüttgütern - Bestimmung
einer größengewichteten Feinfraktion und des Anteils
an kristallinem Quarz - Teil 3: Berechnungsverfahren

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 17289-3:2019 E

worldwide for CEN national Members.
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Contents Page

European foreword ....................................................................................................................................................... 6

Introduction .................................................................................................................................................................... 7

1 Scope .................................................................................................................................................................... 9

2 Normative references .................................................................................................................................... 9

3 Terms and definitions ................................................................................................................................... 9

4 Symbols and abbreviations ......................................................................................................................... 9

5 Assumptions ................................................................................................................................................... 10

by sedimentation .................................................................. 11

6 Determination of SWFF and SWFFCS

6.1 Determination of sedimentation time .................................................................................................. 11

6.2 Selection of sedimentation liquid .......................................................................................................... 12

6.3 Sample preparation, sedimentation and SWFF determination ................................................... 12

6.4 Use of a dispersant of deflocculant ........................................................................................................ 13

6.5 Determination of the SWFF and SWFF of mixtures of phases with different densities .... 14

6.6 SWFF of mixtures ......................................................................................................................................... 14

6.7 SWFF of mixtures of homogeneous particles .................................................................................. 14

6.8 SWFFcs of mixtures of heterogeneous particles ............................................................................... 14

Annex A (informative) Separation of the SWFF by sedimentation .......................................................... 16

A.1 Derivation for calculating the sedimentation parameters ........................................................... 16

A.1.1 General ............................................................................................................................................................. 16

A.1.2 Integral of R(D) .............................................................................................................................................. 17

A.1.3 Integral of S(D) .............................................................................................................................................. 17

A.2 Calculation of the SWFF after sedimentation ..................................................................................... 19

Annex B (informative) Determination and isolation of the size-weighted fine fraction

(SWFF) of kaolins and kaolinitic clays by sedimentation .............................................................. 21

B.1 General ............................................................................................................................................................. 21

B.2 Application range ......................................................................................................................................... 21

B.3 Equipment and consumables ................................................................................................................... 21

B.3.1 Beakers, (preferably glass) or similar containers to hold, about3 l by volume .................... 22

B.3.2 Buchner vacuum flask, (preferably glass) of more than 2 l volume with implosion

protection ....................................................................................................................................................... 22

B.3.3 Water bath, with temperature control to ± 1°C to accommodate the 3-l-glass beakers

(a bath that holds three to four beakers gives a good compromise between taking up

too much bench space and adversely affecting sample throughput) ........................................ 22

B.3.4 Siphon tube, as described and shown in Figures B.1 to B.3 (alternatively, a curved

glass-siphon can be used as well) ........................................................................................................... 22

B.3.5 Demineralized (deionised) water .......................................................................................................... 22

B.3.6 Analytical balance, capable for weighing with an accuracy of 0,001 g ..................................... 22

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B.3.7 Ultrasonic bath or shaker .......................................................................................................................... 22

B.3.8 Dessicator ........................................................................................................................................................ 22

B.3.9 Oven, with temperature control to maintain at temperature of (105 ± 5) °C ......................... 22

B.3.10 Buchner filter assembly, flask and funnel for filtering fine fraction ......................................... 22

B.3.11 Filter papers, with slow speed and hardened high retention (fine crystalline) ................... 22

B.3.12 Filter assembly, suitable for use with mixed cellulose ester filter membranes .................... 22

B.3.13 Filter membranes, 0,8 µm (or finer) mixed cellulose ester filter membranes ...................... 22

B.3.14 Evaporating basins ....................................................................................................................................... 22

B.3.15 Dispersant, e.g. sodium hexametaphosphate (calgon), sodium polyacrylate ........................ 22

B.3.16 Sodium carbonate solution, diluted, about 10 % volume concentration, for pH

adjustment ...................................................................................................................................................... 22

B.3.17 Sulphuric acid, diluted, about 10 % volume concentration, for pH adjustment ................... 22

B.4 Method .............................................................................................................................................................. 22

B.4.1 Step 1 ................................................................................................................................................................. 22

B.4.2 Step2 .................................................................................................................................................................. 22

B.4.3 Step 3 ................................................................................................................................................................. 23

B.4.4 Step 4 ................................................................................................................................................................. 23

B.4.5 Step 5 ................................................................................................................................................................. 23

B.4.6 Step 6 ................................................................................................................................................................. 23

B.4.7 Step 7 ................................................................................................................................................................. 23

B.4.8 Step 8 ................................................................................................................................................................. 24

B.5 Figures .............................................................................................................................................................. 24

Annex C (informative) Other minerals which can be treated in a similar way to

kaolins/kaolinitic clays for SWFF and SWFF determination ..................................................... 27

C.1 General ............................................................................................................................................................. 27

C.2 Andalusite ....................................................................................................................................................... 27

C.2.1 General ............................................................................................................................................................. 27

C.2.2 Sedimentation procedure .......................................................................................................................... 27

C.2.2.1 Steps .................................................................................................................................................................. 27

C.2.2.2 Example ............................................................................................................................................................ 28

C.3 Mica .................................................................................................................................................................... 28

C.4 Vermiculite...................................................................................................................................................... 28

C.5 Talc ..................................................................................................................................................................... 29

C.5.1 General ............................................................................................................................................................. 29

C.5.2 Surfactant/Dispersant preparation ....................................................................................................... 29

C.5.3 Sedimentation procedure .......................................................................................................................... 29

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Annex D (informative) Determination of the size weighted fine fraction (SWFF) and SWFF

of Diatomaceous Earth (DE) by sedimentation ................................................................................. 30

D.1 General ............................................................................................................................................................. 30

D.2 Categories of diatomaceous earth .......................................................................................................... 30

D.3 Equipment and consumables ................................................................................................................... 30

D.3.1 Mercury porosimeter .................................................................................................................................. 30

D.3.2 Mercury of high purity, hexadistilled ................................................................................................... 30

D.3.3 Analytical balance, capable of weighing with an accuracy of 0,001 g ....................................... 30

D.3.4 Gas pycnometer ............................................................................................................................................ 30

D.3.5 Helium gas, quality class 2-1°A ............................................................................................................... 30

D.4 Method ............................................................................................................................................................. 30

D.4.1 Determination of the skeletal density .................................................................................................. 30

D.4.2 Determination of the intra-particular pore volume and intra-particle porosity ................. 30

D.4.3 Calculation of the effective density ........................................................................................................ 31

D.5 Determination of SWFF by sedimentation .......................................................................................... 31

D.5.1 Preparation of the sample ........................................................................................................................ 31

D.5.2 Determination of sedimentation time .................................................................................................. 31

D.6 Determination of SWFF ........................................................................................................................... 31

D.7 Example ........................................................................................................................................................... 31

Annex E (informative) Determination of the size weighted fine fraction (SWFF) of feldspar

products by sedimentation ....................................................................................................................... 33

E.1 General ............................................................................................................................................................. 33

E.2 Application range ......................................................................................................................................... 33

E.3 Consumables .................................................................................................................................................. 33

E.3.1 Measuring cylinders, of 250 ml volume or equivalent height ..................................................... 33

E.3.2 Demineralized (deionised) water .......................................................................................................... 33

) , 0,05 % or 50 g/l .............................................................. 33

E.3.3 Sodium hexametaphosphate Na(PO3 6

E.3.4 Analytical balance, capable of weighing with an accuracy of 0,001 g ....................................... 33

E.3.5 Ultrasonic bath or shaker ......................................................................................................................... 33

E.3.6 Desiccator ....................................................................................................................................................... 33

E.3.7 Oven with an automatic temperature control set to (103 ± 5) °C ............................................... 33

E.3.8 Sedimentation Excel sheet for calculations of sedimentation time ........................................... 33

E.4 Method ............................................................................................................................................................. 33

E.4.1 General ............................................................................................................................................................. 33

E.4.2 Step1 ................................................................................................................................................................. 34

E.4.3 Step 2 ................................................................................................................................................................ 34

E.4.4 Step 3 ................................................................................................................................................................ 34

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E.4.5 Step 4 ................................................................................................................................................................. 35

E.4.6 Step 5 ................................................................................................................................................................. 35

E.4.7 Step 6 ................................................................................................................................................................. 35

Bibliography ................................................................................................................................................................. 37

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European foreword

This document (prEN 17289-3:2019) 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

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

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 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 determination of the size weighted fine fraction (SWFF) and the size

weighted fine fraction of crystalline silica (SWFF ) in bulk materials by means of a sedimentation

method using a liquid sedimentation technique.

The purpose of this document is to allow users to evaluate bulk materials with regard to their size-

weighted fine fraction and crystalline silica content.

For preparation of the sample and determination of crystalline silica by XRD and FT-IR see

prEN 17289-1:2018.

Annex A to Annex E describe specific methods for the evaluation of SWFF for specific bulk materials.

This document is applicable for bulk materials which have been fully investigated and validated. The

criteria for the materials are described in this document and prEN 17289-2:2018. 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, Workplace exposure - Terminology

EN 481, Workplace atmospheres - Size fraction definitions for measurement of airborne particles

prEN 17289-1:2019, Characterization of bulk materials – Determination of a size-weighted fine fraction

and crystalline silica content — Part 1: General information and choice of test methods

prEN 17289-2:2019, Characterization of bulk materials – Determination of a size-weighted fine fraction

and crystalline silica content — Part 2: Calculation method
3 Terms and definitions

For the purposes of this document, tthe terms and definitions given in in EN 1540 and prEN17289-

1:2019 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
4 Symbols and abbreviations
CS Crystalline Silica
PSD Particle Size Distribution
PSCD Particle Size Cumulative Distribution
SWFF Size Weighted Fine Fraction
SWFF Size Weighted Fine Fraction of crystalline silica
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5 Assumptions
The sedimentation method is based on the following assumptions:

a) All liquid that is extracted from the sedimentation vessel only comes from the space above the

extraction nozzle, and not from the space below the extraction nozzle. If this is not the case this will

result in a higher SWFF.

b) The particle size distribution of the bulk material is constant over the particle size range of interest,

i.e. from 1 µm to 12 µm (aerodynamic).

A constant particle size distribution is a PSD with a function that has a derivative which is constant,

see Formula (1).
DB−
( )
PSD D ×100 (1)
( )
AB−
( )
where
D is the particle size;
B is the minimum particle size;
A is the maximum particle size;
NOTE ≤ ≤ . See Figure 1 for an example.
B D A
cummulative
Figure 1 — Example of a constant PSCD with A = 25 µm and B = 0,5 µm

c) The particle size distribution of the sample does not have a mean diameter (D ) in the range from

6 µm and 12 µm (aerodynamic), and has a too narrow distribution. The distribution is considered

too narrow when the relative span of the distribution is less than 1,5. Relative span is calculated as

((D -D )/D ). In case the sample has a narrow size distribution SWFF and SWFF should be

90 10 50 CS
calculated from the particle size distribution.
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d) Stokes law is only valid for particles settling in a medium at low Reynolds number. The velocity of a

particle settling in a medium is limited by the drag force and this depends on the Reynolds number

for that particle. Although the density of liquids are much higher, so is their viscosity so that in the

end the difference between the Reynolds number of a particle in air and in e.g. water is only a factor

of 5. And although the constants for calculating the drag coefficient of particles depend on the

Reynolds number, the variation with Reynolds number within this range is very small and can be

neglected. Therefore, the dynamic form factor is assumed to be equal in both air and liquid.

e) In the material of interest all particles have the same and known density.
f) The sub sample is representative of the bulk material.
6 Determination of SWFF and SWFF by sedimentation
6.1 Determination of sedimenta
...

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