EN 17199-4:2019
(Main)Workplace exposure - Measurement of dustiness of bulk materials that contain or release respirable NOAA or other respirable particles - Part 4: Small rotating drum method
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
Standards Content (Sample)
SLOVENSKI STANDARD
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
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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.
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 ®
10.3.2 Modal aerodynamic equivalent diameters obtained by ELPI (aerodynamic D , µm) . 23
p
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
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.
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].
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
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 %
)
®1
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.
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.
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 (-)
i
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
N
µm
Mandatory
highest mode (M2 ) of the time-
N
averaged number-based particle size
distribution as dN/dlogD (µm)
i
Number of modes of the time-averaged
mass-based particle size distribution Optional
as dM/dlogD (-)
i
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
M
µm
Optional
highest mode (M2 ) of the time-
M
averaged mass-based particle size
distribution as dM/dlogD (µm)
i
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 ;
E
— 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
A
Q .
D
Key
1 temperature and RH-controlled test atmosphere directed into the test system at Q = 11 l/min
A
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
C ®
18 4,2 l/min (QD) temperature- and RH-controlled make-up air to balance the ELPI volume flow
19 T-split connector ®
20 10 l/min (Q ) volume flow to the ELPI
E
21 ELPI® sampling at Q = 10 l/min.
E
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 % RH to 80 % RH).
6.2.4 Sampling line with isokinetic sampling outlets
The drum is connected to the aerosol samplers and the aerosol instruments by using a three-way aerosol
flow splitter. This allows particle sampling of respirable dust, electron microscopy samples, and real-time ®
measurement using the CPC and ELPI aerosol monitoring devices (see Figure 1).
It is important that the sampling line is configured in a manner that prevents particle losses in the
respirable particle size range to ensure interlaboratory comparability.
6.2.5 Electrically conductive tubing
To minimize losses in sampling lines during the measurement of airborne particle size distributions and
number concentrations, electrically conductive tubing should be used.
Transition tube lengths and bent in tubing should be kept to a minimum to minimize particle losses.
If diffusion chargers are connected to the sampling line, these should be connected using the types of
tubes distributed with the instruments or similar.
6.2.6 Cyclone for the respirable dust fraction
Cyclone with a flow rate of 4,2 l/min and mounted with filters with 25 mm- or 37 mm- cassettes, enabling
sampling of the respirable dust, according to EN 481 and validated according to EN 13205-2.
NOTE Sampling is performed using an individual pump.
6.2.7 Collection filter, 25 mm or 37 mm, preferably made of polytetrafluorethylene (PTFE)
The user may select a filter type of another material with a lower limit of quantification.
6.2.8 Direct-reading size-resolved aerosol instrument for time-averaged number-based particle
size distribution
Number-based particle size distribution shall be measured using a direct reading number-based low
pressure cascade impactor and the number of modes and the modal aerodynamic
equivalentdiameter(s)of the time-averaged particle number shall be derived from the data. The device
shall be able to count and classify particles in the particle size range from at least 10 nm to 10 µm.
The measurement of the number-based particle size distribution in aerodynamic equivalent diameter
shall be preferred and shall be performed with a time step of 1 s.
) ®
An Electrical Low Pressure Impactor (ELPI ) has been selected as the benchmark equipment for this
measurement. ®
NOTE 1 In the ELPI , the number concentration in each channel is calculated from the measured current by
applying the charger efficiency curve which is dependent on mobility-equivalent diameter, itself related to the
aerodynamic diameter. Therefore, it is necessary that the density which relates these two equivalent diameters is
known to calculate the number concentration in each channel. The density mentioned here corresponds to the
effective density of airborne particles, which is theoretically dependent on particle diameter (the larger the
agglomerates and aggregates, the smaller their effective density; the closer to the primary particle diameter, the ®
closer to the material density of the compound), see [5] and [6]. Concerning the ELPI , the value considered for the ®
density can have a strong impact on the number concentration. Over the particle size range covered by the ELPI
3 3
and a range of density from 0,1 g/cm to 10 g/cm , the under estimation or overestimation can reach up to a factor
of 25. Despite this, the effect on relative particle size distributions is limited and the modal aerodynamic equivalent
diameters are therefore less affected.
6.2.9 Direct-reading aerosol instrument for particle number concentration, with a detectable
particle size range from 10 nm to 1 µm
Particle number concentration shall be measured at 1 s resolution using a condensation particle counter
(CPC). The CPC shall be able to count particles in the particle size range from at least 10 nm to 1 µm and
3 3
to 100 000 particles/cm in single particle counts. The
at concentrations ranging from 0 particles/cm
working fluid of the instrument shall be alcohol.
The CPC shall be calibrated in accordance with ISO 27891 and its response checked following EN 16897.
6.2.10 Sampler for analytical electron microscopy (optional), where sampling air is drawn by an
individual pump
NOTE It is advised to mount a valve to enable bypassing air through a millipore filter cassette during the time
when electron microscopy sampling is not performed. Thereby the volume flow is balanced throughout the test.
6.2.11 Flow meters, capable of measuring and monitoring volume flows ranging from 0,3 l/min to
11 l/min with a measurement uncertainty of 5 % or less.
6.2.12 Equipment for gravimetric analysis, capable of weighing at 0,1 µg resolution or lower and with
a limit of quantification (LOQ) of filter weight less than 1 µg, under temperature- and % RH-controlled
conditions, if temperature is (22 ± 1) °C and relative humidity (50 ± 3) %.
Using the balance in the weighing atmosphere with the selected filter material and particle size shall have
an LOQ less than 15 μg according to ISO 15767.
NOTE Using a dedicated temperature- and % RH-controlled weighing room ensures accuracy in weighing.
7 Requirements
7.1 General
The general procedures outlined in EN 17199-1 shall be applied.
Fundamental requirement for standard testing is a stable rotation speed of the SRD at eleven revolutions
per minute, a stable flow of controlled relative humidity (50 % RH) high efficiency particulate arrestance
2) See Footnote 1.
(HEPA) filtered air through the drum at 11 l/min and an isokinetic to near-isokinetic sampling line with
no or minimal and well-characterized particle loss for sampling and quantification of the end points a) to
e) mentioned in the Scope. To test powders under general use conditions testing of dustiness should be
enabled in the range from 20 % RH to 80 % RH.
The volume flow through the sampling line shall not exceed 11 l/min, which is sufficient to the indicated
samplers and real-time monitors for air sampling. For instruments, which require higher volume-flows
than those provided from the 11 l/min flow through the dustiness system itself, make-up air needs to be
supplied between the monitor and the sampling line (see Figure 1).
7.2 Engineering control measures
Appropriate engineering control measures (e.g. enclosure, use of local exhaust ventilation) shall be
implemented to prevent exposure of the operator during the tests, but also during disassembly and
cleaning sequences between individual test runs.
Occupational risks should be assessed according to national regulations.
7.3 Conditioning of the test material
Because powders and the number-based dustiness index can be sensitive to the relative humidity during
storage, the test powder samples shall be conditioned at least 12 h (overnight) before testing. In standard
test conditions, the samples shall be stored at room temperature with air conditioned at (50 ± 5) % RH.
NOTE The storage at controlled % RH test conditions can be done in different ways. One possibility is to use
the same humidifier, which is used to condition the air for dustiness testing, and connect this to a chamber suitable
in size. Alternatively, a humidity-controlled laboratory room or a separate humidity-controlled chamber can be
used.
7.4 Conditioning of the test equipment
For testing under standard conditions, the average conditions for temperature and relative humidity
inside the drum shall be (21 ± 3) °C and (50 ± 5 % RH), respectively, and shall be stable throughout the
entire test period. These conditions are provided by the air from the humidifier feeding the test
atmosphere into the drum (see Figure 1).
The test apparatus shall be electrically grounded to prevent charge accumulation.
8 Preparation
8.1 Weighing of filters
At least four filters (depending on which filter type has lowest limit of quantification in the specific
laboratory) shall be prepared for each powder sample for collection of respirable dust with the cyclone
for the respirable dust fraction. The four filters include one backup, if a fourth sample will be needed to
reduce uncertainty or errors. For each weighing round (e.g., one-week-sets of tests) three blank filters
shall be included to take into account filter variations and handling.
Before weighing (before and after use in test), the filters shall be conditioned, at least overnight, in a
climate-controlled weighing room and weighed.
8.2 Test sample
One 2 g sample for “conditioning testing” and four at least 6 g samples for quantitative dustiness testing
are incubated for 24 h at the intended test conditions (i.e. (21 ± 5) °C; (50 ± 5) % RH).
For the determination of moisture content and bulk density (see 8.3 and 8.4) sufficient sample amounts
are incubated at the desired test conditions.
8.3 Moisture content of the test material
The moisture content of the test material shall be determined and documented according to the
procedure given in EN 17199-1.
8.4 Bulk density of the test material
The bulk density of the test material shall be determined and documented according to the procedure
given in EN 17199-1.
8.5 Preparation of test apparatus
Prior to the tests being carried out, the rotating drum is cleaned thoroughly using a suitable vacuum
cleaner, wiped with a damp cloth (e.g. alcohol-wetted cloths) and allowed to dry. For test materials that
stick to the internal surfaces, it can also be necessary to wash the surfaces with a solution of a detergent
in water followed by thorough washing with water, or to clean with a suitable solvent (e.g. propanol).
The tube connecting the drum (item number 1 in Figure 1) and the sampling line (item number 4 in Figure
1) is attached to the outlet stage of the drum using a rotating coupling device. The dust transmission line
is connected to the sampling line using a tight fitting stainless connecter (item number 3 in Figure 1).
The volume flow rates of air provided by the humidifiers and all the pumps, devices and real-time
instruments are checked using air volume flow meters and adjusted, if necessary, to balance the total
collection air volume flow to the total volume flow of 11 l/min into the drum as depicted in Figure 1.
The instruments are connected to the sampling line using stainless metal or alloy tubes or conductive
tubing as shown in Figure 1. Bends in tubing shall be avoided to the extent possible.
8.6 Aerosol instruments and aerosol samplers
Instruments shall be switched on in due time to allow equilibration of the real-time monitors. For ®
is used, it shall be switched on several hours before any measurements take place,
example, if the ELPI
preferably the day before. This allows the electrometers to fully stabilize. ®
Sintered collection plates shall be prepared as recommended by the manufacturer of the ELPI . In case
Al-plates are used, greasing shall be done using one to two drops of vacuum pump oil per plate. When a
new powder sample is being tested, the plates and insulators need to be cleaned in an ultrasonic bath
with alcohol. ®
The ELPI leak test and zeroing procedure shall take place prior to any measurements. The “zeroing”
procedure shall be performed with the drum empty, the instrument connected to the drum and the other
instruments and devices operating. The external HEPA-filter to the air inlet may be used and the charger
shall be on during the “zeroing” procedure.
At the start of a test day, a zero check of the CPC shall be carried out by applying HEPA-filters to the
sampling line.
All devices and instruments flow rates shall be checked using in-line air flowmeters before and after the
test, and the values shall be recorded. ®
Sintered ELPI plates shall be checked between testing powder replicates and only cleaned or wiped if
necessary between replicates.
9 Test procedure
9.1 General
The test procedure starts with a conditioning run to coat the drum and sampling tube surfaces with dust
(see 9.1). The real-time monitoring data from the pre-conditioning test is also used to assess whether the
standard 6 g powder used for the test is suitable to generate quantitative respirable mass and real-time
monitoring data (see 9.2). The conditioning run is followed by a minimum of three tests to establish the
quantitative dustiness data (see 9.3). The SRD is cleaned by gentle vacuum cleaning in between runs (see
9.4) and thoroughly cleaned after completion of the dustiness test for one material and before starting
testing the dustiness testing on the next material (see 9.5).
The test procedure consists of the following steps:
1) Set the direction of the test atmosphere to by-pass the drum.
2) Start the humidified air-flow for the test-line and lead it through the bypass tubing. Follow the
instructions for directing the air-flow carefully.
3) Start all real-time monitoring instruments to be used in the test as well as humidifiers ensuring the ®
test atmosphere and the make-up air to the ELPI . ®
4) Start the ELPI in due time as explained in 8.6.
5) Ensure that the test atmosphere and make-up air is at the correct conditions (standard conditions:
(21 ± 3) °C and (50 ± 5) % RH) and recorded.
6) Ensure all instruments are time synchronized to the extent possible and set to log data
simultaneously.
7) Start the controller and program it to rotate the drum at eleven revolutions per min for 60 s, if not
already pre-programmed. Follow the instructions given for programming the controller.
8) Mount the filter cassette in the cyclone for the respirable dust fraction; connect all instruments,
samplers and make-up air pump to the sampling line as shown in Figure 1.
9) Use a clean filter cassette mounted with an unexposed filter in the cyclone for the respirable dust
fraction for each run.
10) Zero the mounted drum to position a lifter vane in bottom position.
11) Start all pumps and ensure that all monitoring devices are attached to the sampling line and running;
12) Set the valves of the system to direct the test atmosphere through the drum. ®
13) Perform the “zeroing” procedure of the ELPI as described in 8.6. Perform a “blank” measurement
with the drum empty and rotating on to check the level of “background” particles within the drum. A
background of less than 20 particles/cm measured using the CPC shall be achieved inside the drum.
14) Set the direction of the test atmosphere back to by-pass the drum. ®
15) Disconnect the ELPI and switch off the pumps to the respirable dust sampler and EM samplers.
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