SIST EN 17289-1:2021

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

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

This draft European Standard is submitted to CEN members for enquiry. It has been drawn up by the Technical Committee

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

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,

Recipients of this draft are invited to submit, with their comments, notification of any relevant patent rights of which they are

Warning : This document is not a European Standard. It is distributed for review and comments. It is subject to change without

© 2019 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 17289-1:2019 E

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

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

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

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

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

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

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

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

The evaluation of bulk materials using SWFF is complementary to determining the dustiness according

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

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

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

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

This document gives also guidance on the preparation of the sample and determination of crystalline

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

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.

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.

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

prEN 17289-3:2019, Characterization of bulk materials – Determination of a size-weighted fine fraction

ISO 16258-2, Workplace air — Analysis of respirable crystalline silica by X-ray diffraction — Part 2:

ISO 24095, Workplace air — Guidance for the measurement of respirable crystalline silica

For the purposes of this document, the terms and definitions given in EN 1540:2011 and the following

ISO and IEC maintain terminological databases for use in standardization at the following addresses:

ratio of the mass of a quantity of dry granular material to the total volume of its grains, including the

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

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

k is the positive imaginary (absorption) part of the refractive index of a particle;

silicon dioxide with Si and O orientated in a fixed pattern as opposed to a nonperiodic, random

Note 1 to entry: The three most common crystalline forms of silica are quartz, tridymite, and cristobalite.

particle diameter corresponding to 10 % of the cumulative undersize distribution (by volume or by

particle diameter, where 50 % of the particles – by volume or by mass – are smaller than this diameter

particle diameter corresponding to 90 % of the cumulative undersize distribution (by volume or by

diameter of a sphere having the same rate of sedimentation and density as the particle for laminar flow

homogeneous substance with a well-defined set of physical and chemical properties; it defines a

proportion of mass of particles in a bulk material below a well-defined probability function

mass of a unit volume of the Diatomaceous Earth (DE) skeleton, inaccessible to Helium

measure of dispersion used in the assessment of proficiency, based on the available information

column of liquid that is separated from the total sedimentation liquid column which contains the solid

proportion of crystalline silica particles in a bulk material below a well-defined probability function

standardized measure of laboratory bias, calculated using the assigned value and the standard

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

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 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

done after experiments have shown that the results are accurate and consistently equal or higher than

The sedimentation method is a good approximation for the determination of SWFF and SWFF .

However, when samples have a narrow size distribution and a median diameter (D ) in the range 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

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

Figure 1 gives a flowchart to assist the user in selecting the appropriate test method.

NOTE Experiments were performed on a series of minerals in order to make recommendations on the use of

Samples shall be extracted from the bulk material using a method, which will result in a representative

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

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.

h) density of the crystalline silica polymorph of interest (e.g. quartz, cristobalite etc.), in kg/m

The test report shall also include specific minimum requirements for the calculation and/or

i) determination of PSD by laser diffraction analysis – LD-Fraunhofer, LD-Mie or Sedimentation X-

ii) an example of a calculation sheet for determining SWFF by calculation can be found on the

(https://www.crystallinesilica.eu/sites/crystallinesilica.eu/files/SWeRF%20calculation%

20sedimentation_version%202015%2004%2024.xlsx) and the SWFF calculation xls sheet.

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

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

Essentially the mass fraction of quartz 100 %, therefore in this case SWFF is equal to SWFF . Further,

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

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

In accordance with ISO 13528:2015, B.2 samples may be considered as homogenous, if they fulfil

Formula (A.1) compares s , which is the standard deviation between the random samples of the

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

The subsamples comply with this requirement of ISO 13528 (according to Table 1). Therefore, they are

Table A.1 — Homogeneity check (according to ISO 13528:2015, B.2) by laser diffraction

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,

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

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.