Workplace exposure - Measurement of dustiness of bulk materials that contain or release respirable NOAA or other respirable particles - Part 4: Small rotating drum method

This document describes the methodology for measuring and characterizing the dustiness of bulk materials that contain or release respirable NOAA or other respirable particles, under standard and reproducible conditions and specifies for that purpose the small rotating drum method.
This document specifies the selection of instruments and devices and the procedures for calculating and presenting the results. It also gives guidelines on the evaluation and reporting of the data.
The methodology described in this document enables
a)   the measurement of the respirable dustiness mass fraction,
b)   the measurement of the number-based dustiness index of respirable particles in the particle size range from about 10 nm to about 1 µm,
c)   the measurement of the initial number-based emission rate and the time to reach 50 % of the total particle number released during testing,
d)   the measurement of the number-based particle size distribution of the released aerosol in the particle size range from about 10 nm to about 10 µm,
e)   the collection of released airborne particles in the respirable dustiness mass fraction for subsequent observations and analysis by analytical electron microscopy.
NOTE 1   The particle size range described above is based on the equipment used during the pre-normative research [8].
This document is applicable to the testing of a wide range of bulk materials including powders, granules or pellets containing or releasing respirable NOAA or other respirable particles in either unbound, bound uncoated and coated forms.
NOTE 2   Currently no number-based classification scheme in terms of particle number and emission rate has been established for powder dustiness. Eventually, when a large number of measurement data has been obtained, the intention is to revise the document and to introduce such a classification scheme, if applicable.
NOTE 3   The small rotating drum method has been applied to test the dustiness of a range of materials including nanoparticle oxides, nanoflakes, organoclays, clays, carbon black, graphite, carbon nanotubes, organic pigments, and pharmaceutical active ingredients. The method has thereby been proven to enable testing of a many different materials that can contain nanomaterials as the main component.

Exposition am Arbeitsplatz - Messung des Staubungsverhaltens von Schüttgütern, die alveolengängige NOAA oder andere alveolengängige Partikel enthalten oder freisetzen - Teil 4: Verfahren mit kleiner rotierender Trommel

Diese Europäische Norm enthält die Methodik für die Messung und Charakterisierung des Staubungsverhaltens von Schüttgütern, die Nanoobjekte oder Partikel im Submikrometerbereich enthalten oder unter wiederholbaren und Standardbedingungen freisetzen, und legt zu diesem Zweck das Verfahren mit kleiner rotierender Trommel fest.
Darüber hinaus legt diese Europäische Norm die Auswahl der Instrumente und Vorrichtungen sowie die Verfahren für die Berechnung und Präsentation der Ergebnisse fest. Des Weiteren enthält die Norm eine Anleitung für die Auswertung und Angabe der Daten.
Die in dieser Europäischen Norm festgelegte Methodik ermöglicht
a)   die Berechnung des Massenanteils an alveolengängigem Staub,
b)   die Messung des zahlenbasierten Staubindex alveolengängiger Partikel im Größenbereich zwischen ungefähr 10 nm und 1 000 nm,
c)   die Messung der zahlenbasierten Größenverteilung des freigesetzten Aerosols im Größenbereich zwischen ungefähr 10 nm und 10 µm,
d)   die Quantifizierung der ersten Staubemissionsrate und der Dauer bis zur Erreichung von 50 % der während der Prüfung freigesetzten Gesamtpartikelzahl und
e)   die Charakterisierung des Aerosols auf der Grundlage seiner Partikelgrößenverteilung und der Morphologie und chemischen Zusammensetzung seiner Partikel.
Diese Europäische Norm gilt für die Prüfung einer Vielzahl unterschiedlicher Schüttgüter einschließlich Pulver, Granulate oder Pellets, die Nanoobjekte oder Partikel im Submikrometerbereich in ungebundener, gebundener und unbeschichteter und beschichteter Form enthalten oder freisetzen.
ANMERKUNG 1   Bisher wurde noch kein zahlenbasiertes Klassifizierungsschema für das Staubungsverhalten von Pulver im Hinblick auf die Partikelzahl und das Emissionsverhalten entwickelt. Schließlich, wenn eine große Anzahl an Messdaten vorliegt, ist beabsichtigt, diese Europäische Norm zu revidieren und ein solches Klassifizierungsschema einzuführen.
ANMERKUNG 2   Das Verfahren mit kleiner rotierender Trommel wurde angewendet, um das Staubungsverhalten verschiedener Materialien, einschließlich Nanopartikeloxide, Nanoplättchen, Organokaolin, Ton, Kohlenschwarz, Graphit, Carbon-Nanoröhrchen, organischer Pigmente und pharmazeutischer aktiver Inhaltsstoffe zu prüfen. Das Verfahren ermöglicht daher nachweislich die Prüfung vieler verschiedener Materialien, die Nanomaterialien als Hauptkomponente enthalten können.

Exposition sur les lieux de travail - Mesurage du pouvoir de resuspension des matériaux en vrac contenant ou émettant des nano-objets et leurs agrégats et agglomérats (NOAA) ou autres particules en fraction alvéolaire - Partie 4: Méthode impliquant l'utilisation d'un petit tambour rotatif

Le présent document décrit la méthodologie permettant de mesurer et de caractériser le pouvoir de resuspension de matériaux en vrac contenant ou émettant des NOAA ou autres particules en fraction alvéolaire dans des conditions normalisées et reproductibles et spécifie, à cette fin, le but de la méthode du petit tambour rotatif.
Le présent document spécifie le choix des instruments et dispositifs ainsi que les procédures de calcul et d’expression des résultats. Il fournit également des lignes directrices concernant l’évaluation et la consignation des données.
La méthodologie décrite dans le présent document permet :
a)   le mesurage de la fraction massique des poussières alvéolaires ;
b)   le mesurage de l’indice du pouvoir de resuspension en nombre de particules alvéolaires dans la plage granulométrique comprise entre environ 10 nm et 1 µm ;
c)   le mesurage du taux initial d’émission en nombre et du temps nécessaire pour atteindre 50 % du nombre total de particules libérées au cours des essais ;
d)   le mesurage de la distribution granulométrique en nombre des particules d’aérosol libérées dans la plage granulométrique comprise entre environ 10 nm 10 µm ;
e)   la collecte des particules en suspension dans l’air libérées dans la fraction massique des poussières alvéolaires pour des observations et une analyse supplémentaires par microscopie électronique.
NOTE 1   La plage granulométrique décrite ci-dessus a été établie sur la base de l’équipement utilisé au cours des recherches préalables à la normalisation [8].
Le présent document est applicable aux essais relatifs à une gamme étendue de matériaux en vrac, y compris des matériaux granulaires, en poudre ou sous forme de pastilles contenant ou émettant des NOAA ou autres particules en fraction alvéolaire sous formes revêtues, non revêtues, liées et non liées.
NOTE 2   Jusqu’à présent, aucun système de classification basé sur le nombre en termes de nombre de particules et de taux d’émission n’a été établi concernant l’aptitude à l’empoussièrement des poudres. Dès lors que des données de mesure seront disponibles en grand nombre, il est prévu de réviser le présent document et d’introduire un tel système de classification, le cas échéant.
NOTE 3   La méthode du petit tambour rotatif a été employée pour déterminer le pouvoir de resuspension d’une gamme de matériaux parmi lesquels des nanoparticules d’oxydes, des nanoflocons, des argiles organiques, des argiles, du noir de carbone, du graphite, des nanotubes de carbone, des pigments organiques et des ingrédients pharmaceutiques actifs. Ainsi, il s’est avéré que la méthode était appropriée pour les essais relatifs à un grand nombre de matériaux différents pouvant contenir des nanomatériaux en tant que composant principal.

Izpostavljenost na delovnem mestu - Meritve prašnosti razsutih materialov, ki vsebujejo ali sproščajo respirabilne nanopredmete ter njihove agregate in aglomerate (NOAA) in druge respirabilne delce - 4. del: Metoda z majhnim vrtečim bobnom

Ta evropski standard določa metodologijo za merjenje in opredelitev prašnosti razsutih materialov, ki vsebujejo ali sproščajo nanopredmete ali submikrometrske delce v standardnih in ponovljivih pogojih, ter za ta namen določa metodo z majhnim vrtečim bobnom.
Poleg tega navaja ta evropski standard tudi izbiro instrumentov in naprav ter postopke za izračun in predstavitev rezultatov. Podaja tudi smernice za vrednotenje in poročanje podatkov.
Metodologija, ki je opisana v tem evropskem standardu, omogoča:
a)   merjenje masnega deleža pri respirabilni prašnosti,
b)   merjenje indeksa prašnosti respirabilnih delcev na podlagi števila v razponu velikosti od približno 10 nm to 1000 nm,
c)   merjenje porazdelitve velikosti sproščenega aerosola na podlagi števila v razponu velikosti od približno 10 nm to 10 µm,
d)   kvantifikacija začetne stopnje prašnih emisij in časa, dokler ni doseženih 50 % skupnega števila delcev, sproščenih med preskušanjem, in
e)   karakterizacijo aerosola na podlagi porazdelitve velikosti delcev ter morfologije in kemijske sestave njegovih delcev.
Ta evropski standard se uporablja za preskušanje širokega nabora razsutih materialov, vključno s praški, granulami in peleti, ki vsebujejo ali sproščajo nanopredmete ali submikrometrske delce v nevezani, vezani, prevlečeni ali neprevlečeni obliki.
OPOMBA 1:   Za prašnost praška v smislu števila delcev in stopnje emisij trenutno še ni vzpostavljena nobena klasifikacijska shema na podlagi števil. ko bo sčasoma pridobljenih veliko merilnih podatkov, je predvidena revizija evropskega standarda in uvedba take klasifikacijske sheme, če bo to ustrezno.
OPOMBA 2:   Metoda z majhnim vrtečim bobnom je bila uporabljena za preskušanje prašnosti več različnih materialov, vključno z oksidi nanodelcev, nanoluskami, organskimi glinami, glinami, oglenimi sajami, grafitom, ogljikovimi nanocevkami, organskimi pigmenti in aktivnimi farmacevtskimi sestavinami. S tem metoda dokazano omogoča preskušanje veliko različnih materialov, v katerih so lahko nanodelci glavna sestavina.

General Information

Status
Published
Publication Date
26-Mar-2019
Current Stage
6060 - Definitive text made available (DAV) - Publishing
Due Date
27-Mar-2019
Completion Date
27-Mar-2019

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SLOVENSKI STANDARD
SIST EN 17199-4:2019
01-september-2019
Izpostavljenost na delovnem mestu - Meritve prašnosti razsutih materialov, ki
vsebujejo ali sproščajo respirabilne nanopredmete ter njihove agregate in
aglomerate (NOAA) in druge respirabilne delce - 4. del: Metoda z majhnim vrtečim
bobnom
Workplace exposure - Measurement of dustiness of bulk materials that contain or

release respirable NOAA or other respirable particles - Part 4: Small rotating drum

method

Exposition am Arbeitsplatz - Messung des Staubungsverhaltens von Schüttgütern, die

Nanoobjekte oder Submikrometerpartikel enthalten oder freisetzen - Teil 4: Verfahren mit

kleiner rotierender Trommel

Exposition sur les lieux de travail - Mesurage du pouvoir de resuspension des matériaux

en vrac contenant ou émettant des nano-objets et leurs agrégats et agglomérats (NOAA)

ou autres particules en fraction alvéolaire - Partie 4: Méthode impliquant l'utilisation d'un

petit tambour rotatif
Ta slovenski standard je istoveten z: EN 17199-4:2019
ICS:
13.040.30 Kakovost zraka na delovnem Workplace atmospheres
mestu
SIST EN 17199-4:2019 en,fr,de

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

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SIST EN 17199-4:2019
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SIST EN 17199-4:2019
EN 17199-4
EUROPEAN STANDARD
NORME EUROPÉENNE
March 2019
EUROPÄISCHE NORM
ICS 13.040.30
English Version
Workplace exposure - Measurement of dustiness of bulk
materials that contain or release respirable NOAA or other
respirable particles - Part 4: Small rotating drum method

Exposition sur les lieux de travail - Mesurage du Exposition am Arbeitsplatz - Messung des

pouvoir de resuspension des matériaux en vrac Staubungsverhaltens von Schüttgütern, die

contenant ou émettant des nano-objets et leurs Nanoobjekte oder Submikrometerpartikel enthalten

agrégats et agglomérats (NOAA) ou autres particules oder freisetzen - Teil 4: Verfahren mit kleiner

en fraction alvéolaire - Partie 4: Méthode impliquant rotierender Trommel
l'utilisation d'un petit tambour rotatif
This European Standard was approved by CEN on 8 February 2019.

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, 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.
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. EN 17199-4:2019 E

worldwide for CEN national Members.
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SIST EN 17199-4:2019
EN 17199-4:2019 (E)
Contents Page

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

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

1 Scope .................................................................................................................................................................... 6

2 Normative references .................................................................................................................................... 6

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

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

5 Principle ............................................................................................................................................................. 8

6 Equipment ...................................................................................................................................................... 10

6.1 General ............................................................................................................................................................. 10

6.2 Test apparatus............................................................................................................................................... 10

7 Requirements ................................................................................................................................................ 13

7.1 General ............................................................................................................................................................. 13

7.2 Engineering control measures ................................................................................................................ 14

7.3 Conditioning of the test material ............................................................................................................ 14

7.4 Conditioning of the test equipment ....................................................................................................... 14

8 Preparation .................................................................................................................................................... 14

8.1 Weighing of filters ........................................................................................................................................ 14

8.2 Test sample .................................................................................................................................................... 14

8.3 Moisture content of the test material ................................................................................................... 15

8.4 Bulk density of the test material ............................................................................................................ 15

8.5 Preparation of test apparatus ................................................................................................................. 15

8.6 Aerosol instruments and aerosol samplers........................................................................................ 15

9 Test procedure .............................................................................................................................................. 16

9.1 General ............................................................................................................................................................. 16

9.2 Test sequence for running a dustiness test ........................................................................................ 17

9.3 Selection of the amount to be used for SRD dustiness triple test ............................................... 18

9.3.1 General ............................................................................................................................................................. 18

9.3.2 Selection of 6 g test material .................................................................................................................... 19

9.3.3 Selection of more than 6 g test material .............................................................................................. 19

9.3.4 Selection of less than 6 g test material ................................................................................................. 20

9.4 Cleaning in between runs .......................................................................................................................... 20

9.5 Cleaning of equipment after conclusion of a dustiness test ......................................................... 21

10 Evaluation of data ........................................................................................................................................ 21

10.1 Respirable dustiness mass fraction ....................................................................................................... 21

10.2 Use of CPC data .............................................................................................................................................. 21

10.2.1 General ............................................................................................................................................................. 21

10.2.2 Number-based emission rate ................................................................................................................... 22

10.2.3 Number-based dustiness index ............................................................................................................... 22

10.2.4 Dustiness kinetics ........................................................................................................................................ 23

10.2.5 Time needed to reach 50 % of the released number of particles during the test ................ 23

10.3 Use of ELPI data .......................................................................................................................................... 23

10.3.1 General ............................................................................................................................................................. 23

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SIST EN 17199-4:2019
EN 17199-4:2019 (E)

10.3.2 Modal aerodynamic equivalent diameters obtained by ELPI (aerodynamic D , µm) ....... 23

10.4 Morphology and chemical characterization of the particles ........................................................ 24

11 Test report ...................................................................................................................................................... 24

Annex A (informative) Example of a small rotating drum set-up .............................................................. 26

Bibliography ................................................................................................................................................................. 27

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SIST EN 17199-4:2019
EN 17199-4:2019 (E)
European foreword

This document (EN 17199-4:2019) 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 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 September 2019 and conflicting national standards shall

be withdrawn at the latest by September 2019.

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.

This document has been prepared under a mandate given to CEN by the European Commission and the

European Free Trade Association.

According to the CEN-CENELEC Internal Regulations, the national standards organizations of the

following countries are bound to implement this European Standard: 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

the United Kingdom.
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SIST EN 17199-4:2019
EN 17199-4:2019 (E)
Introduction

Dustiness measurement and characterization provide users (e.g. manufacturers, producers, occupational

hygienists and workers) with information on the potential for dust emissions when the bulk material is

handled or processed in workplaces. They provide the manufacturers of bulk materials containing NOAA

with information that can help to improve their products and reduce their dustiness. It allows the users

of the bulk materials containing NOAA to assess the controls and precautions required for handling and

working with the material and the effects of pre-treatment (e.g. modify surface properties or chemistry).

It also allows the users to select less dusty products, if available. The particle size distribution of the

aerosol and the morphology and chemical composition of its particles can be used by occupational

hygienists, scientists and regulators to further characterize the aerosol in terms of particle size

distribution and chemical composition and to thus aid users to evaluate and control the health risk of

airborne dust.

This document gives details on the design and operation of the small rotating drum method that can be

used to measure the dustiness of bulk materials that contain or release respirable NOAA or other

respirable particles in terms of dustiness indices or emission rates. Dustiness indices as well as particle

emission rates can be mass-based of the health-related respirable dustiness mass fraction using a cyclone

for the respirable dust fraction and by number using real-time sampling of particle number

concentrations. The particle size distribution of the released aerosol is measured using direct-reading

aerosol instruments. The released dust particles can be further sampled and characterized for, e.g.

physical size distribution, morphology and chemical composition by off-line analysis (as required).This

test uses the same dust generation principle as EN 15051-2 and EN 17199-2 [1], but the rotating drum

volume and diameter is smaller and the sampling design different, which allows testing of small sample

volumes and simultaneous sampling of all realtime data and dust for off-line analysis.

The small rotating drum method has been designed to simulate workplace scenarios and to represent

general bulk material handling processes, including processes where bulk material is tipped, poured,

mixed, scooped, dropped or similar, either mechanically or by hand.

The small rotating drum method presented here differs from the rotating drum, continuous drop and the

vortex shaker methods presented in EN 17199-2 [1], EN 17199-3 [2] and EN 17199-5 [3] respectively.

The rotating drum and small rotating drum methods perform, both, repeated pouring or agitation of a

bulk material. The continuous drop method simulates continuous feed of a bulk material while the vortex

shaker method simulates vigorous agitation of a bulk material.

This document was developed based on results in scientific literature [4,5,6,7] and pre-normative

research [8]. The pre-normative research project investigated the dustiness of ten bulk materials

(including nine bulk nanomaterials) with the intention to test as wide a range of bulk materials as

possible in terms of magnitude of dustiness, chemical composition and primary particle size distribution

as indicated by a large range in specific surface area.

Subsequently, the sampling line was optimized to improve dust transmission in the system and make the

sampling closer to the efficiency in the prototype by [4] and EN 15051-2 [9].
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SIST EN 17199-4:2019
EN 17199-4:2019 (E)
1 Scope

This document describes the methodology for measuring and characterizing the dustiness of bulk

materials that contain or release respirable NOAA or other respirable particles, under standard and

reproducible conditions and specifies for that purpose the small rotating drum method.

This document specifies the selection of instruments and devices and the procedures for calculating and

presenting the results. It also gives guidelines on the evaluation and reporting of the data.

The methodology described in this document enables
a) the measurement of the respirable dustiness mass fraction,

b) the measurement of the number-based dustiness index of respirable particles in the particle size

range from about 10 nm to about 1 µm,

c) the measurement of the initial number-based emission rate and the time to reach 50 % of the total

particle number released during testing,

d) the measurement of the number-based particle size distribution of the released aerosol in the

particle size range from about 10 nm to about 10 µm,

e) the collection of released airborne particles in the respirable dustiness mass fraction for subsequent

observations and analysis by analytical electron microscopy.

NOTE 1 The particle size range described above is based on the equipment used during the pre-normative

research [8].

This document is applicable to the testing of a wide range of bulk materials including powders, granules

or pellets containing or releasing respirable NOAA or other respirable particles in either unbound, bound

uncoated and coated forms.

NOTE 2 Currently no number-based classification scheme in terms of particle number and emission rate has

been established for powder dustiness. Eventually, when a large number of measurement data has been obtained,

the intention is to revise the document and to introduce such a classification scheme, if applicable.

NOTE 3 The small rotating drum method has been applied to test the dustiness of a range of materials including

nanoparticle oxides, nanoflakes, organoclays, clays, carbon black, graphite, carbon nanotubes, organic pigments,

and pharmaceutical active ingredients. The method has thereby been proven to enable testing of a many different

materials that can contain nanomaterials as the main component.
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.

CEN ISO/TS 80004-2, Nanotechnologies - Vocabulary - Part 2: Nano-objects (ISO/TS 80004-2)

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

EN 1540, Workplace exposure - Terminology

EN 13205-2, Workplace exposure - Assessment of sampler performance for measurement of airborne

particle concentrations - Part 2: Laboratory performance test based on determination of sampling efficiency

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SIST EN 17199-4:2019
EN 17199-4:2019 (E)

EN 15051-1, Workplace exposure - Measurement of the dustiness of bulk materials - Part 1: Requirements

and choice of test methods

EN 16897, Workplace exposure - Characterization of ultrafine aerosols/nanoaerosols - Determination of

number concentration using condensation particle counters

EN 17199-1, Workplace exposure - Measurement of dustiness of bulk materials that contain or release

respirable NOAA or other respirable particles - Part 1: Requirements and choice of test methods

ISO 15767, Workplace atmospheres - Controlling and characterizing uncertainty in weighing collected

aerosols

ISO 27891, Aerosol particle number concentration - Calibration of condensation particle counters

3 Terms and definitions

For the purposes of this document, the terms and definitions given in EN 1540, EN 15051-1,

CEN ISO/TS 80004-2 and EN 17199-1 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
CPC Condensation Particle Counter
d A lower particle size at which the counting or sampling efficiency is 50 %
Electrical Low Pressure Impactor
ELPI
EM Electron Microscopy
FTIR Fourier Transform Infra-Red Spectroscopy
GC Gas Chromatography
HEPA High Efficiency Particulate Arrestance
HPLC High Performance Liquid Chromatography
ICP Inductive Coupled Plasma
ID Inner Diameter
LOQ Limit Of Quantification
MS Mass Spectrometry
NOAA Nano-objects, and their aggregates and agglomerates > 100 nm

1) ELPI is the trade name or trademark of a product supplied by Dekati. This information is given for the

convenience of users of this European Standard and does not constitute an endorsement by CEN of the product

named. Equivalent products may be used if they can be shown to lead to the same results.

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SIST EN 17199-4:2019
EN 17199-4:2019 (E)
Raman Raman Spectroscopy
RH Relative Humidity
SEM Scanning Electron Microscopy
SRD Small Rotating Drum
TEM Transmission Electron Microscopy
XRF X-ray Fluorescence
5 Principle

The small rotating drum (SRD) method described in this document measures the dustiness of bulk

materials in terms of
— the respirable dustiness mass fraction,
— the number-based dustiness index,
— the number-based emission rates, and
— the time period to generate 50 % of the emitted particle numbers.

In addition, this document describes the procedures by which the aerosols can be further characterized

in terms of their particle size distributions and the morphology and chemical composition of their

airborne particles.

The sampling for the purpose of and the execution of qualitative or quantitative analysis of the

morphology and chemical composition of the collected airborne particles are described. Performing these

analyses is optional but can provide confirmation of the sizes of the particles generated and

complementary information to the real-time instruments.
Table 1 provides
— an overview of the different measurands,
— information on whether determining these measurands is mandatory or not, and
— the aerosol instruments and sampling devices needed to determine a measurand.
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SIST EN 17199-4:2019
EN 17199-4:2019 (E)

Table 1 — Measurands, aerosol instruments/sampling devices and associated recommendations

for the small rotating drum method
Method/Device specific to
Measurand Mandatory/optional
measurand
25 mm- or 37 mm- air
sampling cassette mounted
Respirable dustiness mass fraction Mandatory
on a cyclone for the
(mg/kg)
respirable dust fraction
Number-based dustiness index of
respirable particles in the particle size Condensation Particle
Mandatory
range from about 10 nm to about 1 µm Counter (CPC)
(1/mg)
Number-based average emission rate
of respirable particles in the particle Condensation Particle
Mandatory
size range from about 10 nm to about Counter (CPC)
1 µm (1/mg·s)
Number-based initial dustiness
kinetics considering the number of
Condensation Particle
particles released in the particle size Mandatory
Counter (CPC)
range from about 10 nm to about 1 µm
(1/mg·s )
Time-based dustiness kinetics
assessed as the time required to
generate 50 % of the total number of Condensation Particle
Mandatory
particles released in the particle size Counter (CPC)
range from about 10 nm to about 1 µm
(s)
Number of modes of the time-averaged
Mandatory
number-based particle size
Time- and size-resolving
distributionas dN/dlogD (-)
instrument covering the
Modal aerodynamic equivalent
particle size range from
diameters corresponding to the
about 10 nm up to about 10
highest mode (M1 ) and to the second
Mandatory
highest mode (M2 ) of the time-
averaged number-based particle size
distribution as dN/dlogD (µm)
Number of modes of the time-averaged
mass-based particle size distribution Optional
as dM/dlogD (-)
Cascade impactor covering
Modal aerodynamic equivalent
the particle size range from
diameters corresponding to the
about 10 nm up to about 10
highest mode (M1 ) and to the second
Optional
highest mode (M2 ) of the time-
averaged mass-based particle size
distribution as dM/dlogD (µm)
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SIST EN 17199-4:2019
EN 17199-4:2019 (E)
Method/Device specific to
Measurand Mandatory/optional
measurand
Optional
E.g. a TEM-grid holder
Particles on TEM-grids may be
Morphological characterization of the
equipped with porous carbon
analysed by transmission (TEM)
particles including NOAA
film TEM-grid
or scanning (SEM) electron
microscopy
25 mm- or 37 mm- air Optional
sampling cassette mounted
Filters may be analysed
on a cyclone for the
chemically after weighing using
respirable dust fraction
Chemical characterization of the
e.g. XRF, ICP-MS, GC-MS, HPLC-
particles including NOAA
MS, FTIR, and Raman
spectrometry depending on
needs and suitability of the
sample.

NOTE The particle size range described above is based on the equipment used during the pre-normative research.

6 Equipment
6.1 General

Figure 1 gives a schematic example for a small rotating drum set-up, which is configured with a bypass

tube to bypass the test atmosphere while preparing and cleaning the small rotating drum.

6.2 Test apparatus
The usual laboratory apparatus and, in particular, the following:
6.2.1 Small rotating drum

The small rotating drum consists of the components described in detail in 6.2.2 to 6.2.12. The small drum

consists of a cylindrical part with a radius of 8,15 cm and a length of 23 cm and two 45° truncated conical

ends with a centre depth of 6,3 cm (see Figure 1 and Figure A.1). These dimensions give a total volume of

about 5,675 l. The cylindrical part of the drum contains three powder lifter vanes (2 cm × 22,5 cm) placed

120° apart. The inner surfaces shall be polished to reach an arithmetical mean roughness profile of 0,19

µm, which can be obtained by vibratory finishing. The drum is rotated driven by a cogwheel belt

connected to a programmable electrical engine.
The volume-flow-balance shall be as follows:
— Q is 10 l/min to the ELPI ;
— Q = Q + Q +Q ;
A B1 B2 C
— Q + Q = Q = 10 l/min.
C D E

If measurement systems and sampling systems with different volume flows are applied, the entire

sampling line shall be redesigned to allow isokinetic (or at least near-isokinetic) sampling. See also 6.2.4.

Mass flow controllers should be used to ensure a stable volume flow of humidified air to deliver Q and

Q .
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SIST EN 17199-4:2019
EN 17199-4:2019 (E)
Key

1 temperature and RH-controlled test atmosphere directed into the test system at Q = 11 l/min

2 valves to direct air flow through or bypass the small rotating drum
3 small rotating drum (inlet and outlet tube inner diameters of 20,25 mm)
4 tight-fitting stainless steel tube connector (with inner diameter of 20,25 mm)

5 three-way aerosol flow splitter (connection to dust transfer line with an inner diameter of 20,25 mm)

6 sampling tube for the CPC and the electron microscopy sampler (optional) allowing isokinetic sampling from

the flow-splitter at 1 l/min (QB2)
7 Y-split connector

8 0,3 l/min (Q ) flow directed to the electron microscopy sampler and bypass filter.

B2a
9 0,7 l/min (QB2b) flow directed to the CPC

10 valve to direct the flow towards the electron microscopy sampler or the bypass filter

11 electron microscopy sampler
12 particle filter to protect the pump
13 pump enabling sampling at QB2a = 0,3 l/min
14 CPC sampling at Q = 0,7 l/min
B2b

15 sampling tube for the cyclone for the respirable dust fraction allowing (near-)isokinetic sampling from three-

way flow-splitter at QB1 = 4,2 l/min.

16 cyclone for the respirable dust fraction with pump sampling at QB1 = 4,2 l/min

17 sampling tube for the ELPI allowing (near-)isokinetic sampling of Q = 5,8 l/min

18 4,2 l/min (QD) temperature- and RH-controlled make-up air to balance the ELPI volume flow

19 T-split connector
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SIST EN 17199-4:2019
EN 17199-4:2019 (E)
20 10 l/min (Q ) volume flow to the ELPI
21 ELPI® sampling at Q = 10 l/min.

Figure 1 — Small Rotating Drum with sampling line in a configuration where sampling is made

using a CPC, a cyclone for the respirable dust fraction, an electron microscopy sampler and an

ELPI
6.2.2 System for minimizing the risk of human inhalation exposure
Examples of such a system are a safety cabinet, a fume-hood or an enclosure.
6.2.3 System for humidifying experimental air

The system for humidifying experimental air shall be capable of delivering 11 l/min through the drum

and 7,4 l/min dilution air or a total of 18,4 l/min air with highly controlled temperature at (21 ± 3) °C and

(50 ± 5) % RH (see Figure 1).

Humidifiers for this method should be designed to not transmit particles into the test atmosphere.

Testing should be possible under variable relative humidity conditions (20 % R
...

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