Workplace atmospheres - Determination of diesel particulate matter - General requirements

This European Standard describes the analytical requirements for the determination of particulate diesel engine exhaust emissions in workplace atmospheres. The particulate concentration, averaged over the sampling duration is determined by the parameters total carbon, organic carbon and elemental carbon.
This European Standard enables users to determine occupational exposure to DPM according to a uniform approach and to obtain directly comparable results.
It is the responsibility of users to ascertain that the requirements of EN 482 under the given laboratory conditions are fulfilled.
Potential procedure-related cross sensitivities and interferences in particular workplaces mentioned in this European Standard have to be particularly considered.

Arbeitsplatzatmosphäre - Bestimmung von teilchenförmigen Emissionen von Dieselmotoren - Allgemeine Anforderungen

Air des lieux de travail - Dosage des matières particulaires émises par les moteurs diesel - Exigences générales

La présente Norme européenne spécifie les exigences d'échantillonnage et d'analyse pour déterminer les émissions particulaires des moteurs diesel dans l'air des lieux de travail. Les concentrations massiques moyennes pondérées dans le temps sont mesurées pour les composés des particules émises par les moteurs diesel (c'est à dire OC, CE, TC).
Les utilisateurs ont la responsabilité de s'assurer que les exigences de l'EN 482 dans les conditions de laboratoire sont respectées.

Zrak na delovnem mestu - Določevanje delcev iz dizelskih motorjev - Splošne zahteve

General Information

Status
Published
Publication Date
06-Apr-2004
Current Stage
9093 - Decision to confirm - Review Enquiry
Completion Date
01-Nov-2008

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SLOVENSKI STANDARD
SIST EN 14530:2004
01-junij-2004
=UDNQDGHORYQHPPHVWX'RORþHYDQMHGHOFHYL]GL]HOVNLKPRWRUMHY6SORãQH
]DKWHYH
Workplace atmospheres - Determination of diesel particulate matter - General
requirements
Arbeitsplatzatmosphäre - Bestimmung von teilchenförmigen Emissionen von
Dieselmotoren - Allgemeine Anforderungen

Air des lieux de travail - Dosage des matieres particulaires émises par les moteurs diesel

- Exigences générales
Ta slovenski standard je istoveten z: EN 14530:2004
ICS:
13.040.30 Kakovost zraka na delovnem Workplace atmospheres
mestu
SIST EN 14530:2004 en,fr,de

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

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SIST EN 14530:2004
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SIST EN 14530:2004
EUROPEAN STANDARD
EN 14530
NORME EUROPÉENNE
EUROPÄISCHE NORM
April 2004
ICS 13.040.30
English version
Workplace atmospheres - Determination of diesel particulate
matter - General requirements

Air des lieux de travail - Dosage des matières particulaires Arbeitsplatzatmosphäre - Bestimmung von

émises par les moteurs diesel - Exigences générales teilchenförmigen Emissionen von Dieselmotoren -

Allgemeine Anforderungen
This European Standard was approved by CEN on 2 February 2004.

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 Central Secretariat 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 Central Secretariat has the same status as the official

versions.

CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,

Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia,

Slovenia, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: rue de Stassart, 36 B-1050 Brussels

© 2004 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 14530:2004: E

worldwide for CEN national Members.
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SIST EN 14530:2004
EN 14530:2004 (E)
Contents page

Foreword............................................................................................................................................................. 3

1 Scope ..................................................................................................................................................... 5

2 Normative references ........................................................................................................................... 5

3 Terms and definitions........................................................................................................................... 5

4 Abbreviated terms ................................................................................................................................ 7

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

6 Requirements ........................................................................................................................................ 8

7 Test methods....................................................................................................................................... 10

8 Description of the procedures........................................................................................................... 10

8.1 General................................................................................................................................................. 10

8.2 Sampling.............................................................................................................................................. 11

8.3 Filter pre-treatment and storage........................................................................................................ 11

8.4 Processing........................................................................................................................................... 12

8.5 Determination of organic carbon (desorption) ................................................................................ 12

8.6 Determination of elemental carbon................................................................................................... 12

8.7 Determination of total carbon............................................................................................................ 12

9 Interferences and cross-sensitivities ............................................................................................... 12

10 Test report ........................................................................................................................................... 12

11 Examples of tested measuring procedures ..................................................................................... 13

Annex A (informative) Concrete descriptions of tested measuring procedures ....................................... 14

Bibliography ..................................................................................................................................................... 19

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SIST EN 14530:2004
EN 14530:2004 (E)
Foreword

This document (EN 14530:2004) 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 October 2004, and conflicting national standards shall be withdrawn at

the latest by October 2004.
Annex A is informative.

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

countries are bound to implement this European Standard: Austria, Belgium, Cyprus, Czech Republic,

Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,

Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland

and United Kingdom.
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SIST EN 14530:2004
EN 14530:2004 (E)
Introduction

Diesel engine exhaust emissions are a complex mixture consisting of gases and vapours such as carbon

monoxide, carbon dioxide, sulphur dioxide, nitrogen oxides, aldehydes and hydrocarbons, plus also diesel

particulate matter (DPM). DPM is the particulate phase of diesel engine exhaust emissions and contains

inorganic components (e.g. sulphates) as well as the ones described in the method. They occur in workplaces

where diesel engines operate, especially during tunnel and gallery construction, in freight and transport

facilities, in the mining industry and in workshops. The potentially carcinogenic effect of diesel engine exhaust

emissions is currently attributed to the particulate phase, especially to those particles that consist of a soot

core with associated adsorbed organic compounds. Therefore, these are the components of the total

particulate matter that are considered and referred to in this European Standard.

Since the target organ for the carcinogenic effect from DPM is the alveolar lung region, only the respirable

fraction as defined in EN 481 is sampled. Since the mass median aerodynamic diameter of DPM is

approximately 0,1 mm, sampling this fraction still guarantees complete trapping of all DPM.

NOTE Epidemiological studies from ambient air suggests that there can be other health effects associated with

exposure to diesel engine exhaust besides lung cancer.
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SIST EN 14530:2004
EN 14530:2004 (E)
1 Scope

This European Standard specifies the sampling and analytical requirements for the determination of

particulate diesel engine exhaust emissions in workplace atmospheres. Time weighed average mass

concentrations are measured for the components of particulate diesel engine exhaust emissions (i.e. OC, EC,

TC).

This European Standard enables users to select a procedure to determine occupational exposure to DPM

according to a uniform approach and to obtain directly comparable results.

It is the responsibility of users to ascertain that the requirements of EN 482 under the given laboratory

conditions are fulfilled.
2 Normative references

This European Standard incorporates by dated or undated reference, provisions from other publications.

These normative references are cited at the appropriate places in the text and the publications are listed

hereafter. For dated references, subsequent amendments to or revisions of any of these publications apply to

this European Standard only when incorporated in it by amendment or revision. For undated references the

latest edition of the publication referred to applies (including amendments).

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

EN 482: 1994, Workplace atmospheres — General requirements for the performance of procedures for the

measurement of chemical agents.

EN 689, Workplace atmosphere — Guidance for the assessment of exposure by inhalation to chemical agents

for comparison with limit values and measurement strategy.

EN 1232, Workplace atmospheres — Pumps for personal sampling of chemical agents — Requirements and

test methods.

EN 12919, Workplace atmospheres — Pumps for the sampling of chemical agents with a volume flow rate of

over 5 l/min — Requirements and test methods.

EN 13205: 2001, Workplace atmospheres — Assessment of performance of instruments for measurement of

airborne particle concentrations.
3 Terms and definitions

For the purposes of this European Standard, the following terms and definitions apply.

3.1
components of particulate diesel engine exhaust emissions

organic carbon, elemental carbon and total carbon referred to in this European Standard

NOTE These components are not defined via a specific bonding state of carbon in natural or synthetic substances,

but refer to carbon masses determined by performing specific analytical procedures in several subsequent measuring

steps. Thus, the components of particulate diesel engine exhaust emissions are directly defined via the analysis

procedure.
3.2
organic carbon

organic compounds that can be removed from the soot cores and which are a component of DPM

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SIST EN 14530:2004
EN 14530:2004 (E)

NOTE It is removed by thermal desorption in an inert gas flow at an appropriate temperature as described in one of

the procedures in this European Standard and in a further step is completely converted to carbon dioxide

3.3
elemental carbon
residual soot cores after the organic carbon has been removed

NOTE It is thermally converted to carbon dioxide by heating in an oxygen rich atmosphere at an appropriate

temperature as described in one of the procedures in this European Standard.
3.4
total carbon
sum of organic and elemental carbon.

NOTE It can either be determined by summing the components described in 3.2 and 3.3 or by complete conversion

to carbon dioxide by direct oxidation of the soot core with its adsorbed organic compounds by means of oxygen or an

oxygen rich atmosphere.
3.5
analytical determination

laboratory performed determination of OC, EC, and/or TC in filter samples of the respirable fraction of

particles
3.6
recovery rate
ratio of analytically determined value to target value expressed as a percentage

NOTE The recovery rate can be checked using quality control standards which have been used in round robin tests

or standards which have been produced using test atmospheres.
3.7
bias (relating to determination of DPM)

consistent deviation of the results of a measurement process from the true value of the air quality

characteristic itself
NOTE 1 Adapted from EN 1540: 1998 respectively ISO 6879.

NOTE 2 Because it is not possible to generate a reference atmosphere containing a known concentration of diesel

particulate matter no reference value exists. Additionally, there exists no independent analytical procedure for

determination of diesel particulate matter. Therefore, in all cases the bias should be considered to be zero.

3.8
overall uncertainty (of a measuring procedure)

quantity used to characterise as a whole the uncertainty of the result given by an apparatus or a measuring

procedure

NOTE 1 It is expressed as a percentage, by combination of bias and precision usually according to the formula.

x-x + 2s
ref
·100
ref
where
x is the mean value of results of a number n of repeated measurements;
x is the true or accepted reference value of concentration;
ref
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SIST EN 14530:2004
EN 14530:2004 (E)
s is the standard deviation of measurements.
[EN 1540 : 1998]

NOTE 2 For the determination of diesel particulate matter the bias is assumed to be zero (see 3.7). Therefore the

overall uncertainty equals to the precision of the overall procedure including sampling and analytical determination.

ref

Since there is no reference value for the overall procedure x is considered as being the mean of several repetitive

ref

measurements. These repetitive measurements should be of high quality originating from diesel aerosol test chamber

measurements and interlaboratory studies and should make use of thorough reference materials for the analytical

procedure.

NOTE 3 In strict mathematical terms there is no way to combine precision (a variance) and bias (an absolute number).

However by occupational hygiene precedent and time honoured convention they have been combined according to the

above formula.
3.9
limit of detection
LOD

three times the estimated standard deviation of the mass of the sample, accounting for the double weighing

(exposed vs. unexposed) and for the uncertainty associated with any correction blank used

NOTE 1 The value LOD can be used as a threshhold value to assert the presence of a substance with confidence in

the method.
[ISO 15767 : 2003]
NOTE 2 See also EN 13890:2002, 3.4.4
3.10
limit of quantitation
LOQ
ten times the estimated standard deviation of the mass of the sample

NOTE 1 The value LOQ can be used as a threshhold value to assure measurement of a substance accurarely.

[ISO 15767 : 2003]
NOTE 2 See also EN 13890:2002, 3.4.5
4 Abbreviated terms
DPM diesel particulate matter
OC organic carbon
EC elemental carbon
TC total carbon
LOD limit of detection
LOQ limit of quantitation
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SIST EN 14530:2004
EN 14530:2004 (E)
5 Principle

The respirable fraction of particulate diesel engine exhaust emissions is sampled according to EN 481. OC,

EC, or TC are determined by conversion into carbon dioxide and its subsequent analytical determination by a

suitable method.

NOTE Various analytical techniques have been demonstrated to be suited. Examples are coulometry, non-dispersive

infrared spectroscopy (NDIR) and gas chromatography with flame ionisation detection (GC-FID).

6 Requirements

This clause lists the requirements according to the steps involved in the procedure (particle sampling,

analytical determination, measuring procedure and other requirements, see Tables 1 to 4).

The whole analysis procedure shall meet the requirements of EN 482.
Exposure assessment of DPM shall follow the requirements of EN 689.
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SIST EN 14530:2004
EN 14530:2004 (E)
Table 1 — Particle sampling
No. Attribute Requirements Test methods

6.1.1 particle fraction to be sampled respirable fraction according to convention see 7.1

in EN 481
6.1.2 accuracy EN 13205: 2001, 4.2 see 7.2
6.1.3 filter blank values and use suitable material with regard to blank see 7.3
scattering value level and scattering
6.1.4 flow rate stability according to EN 1232 and EN 12919 —
Table 2 — Analytical determination
No. Attribute Requirements Test methods
6.2.1 maximum load of DPM on filter Determine maximum load of DPM on the see 7.4
filter.
6.2.2 limit of detection and documented by laboratory see 7.5.1 and
limit of quantitation 7.5.2
6.2.3 calibration function linear over the range of measuring see 7.6
procedure
6.2.4 coefficient of variation of 10% within the range of measuring see 7.7
procedure procedure (LOQ up to maximum load)
6.2.5 recovery rate 95 % to 105 % see 7.8
6.2.6 instrument blank value documented by laboratory; constant within see 7.9
20%
Table 3 — Overall measuring procedure
No. Attribute Requirements Test methods
6.3.1 overall uncertainty 30 % to 50 % according to EN 482 see 7.10
6.3.2 storage maximum storage time to be determined see 7.11
and documented by the laboratory. (The
maximum deviation after storage shall not
exceed 5 %.)
6.3.3 field blank values to be treated like samples, a minimum of see 7.12
three per measuring series is
recommended
6.3.4 result unit results in mg m —
6.3.5 specified measuring range according to EN 482 —
Table 4 — Other requirements
No. Attribute Requirements Test methods
6.4 sample identification sample labelling must be unambiguous —
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SIST EN 14530:2004
EN 14530:2004 (E)
7 Test methods
See Table 5.
Table 5 — Test methods
No. Attribute Test methods
7.1 particle fraction to be sampled see EN 13205:2001, clause 5
7.2 accuracy see EN 13205:2001, clause 5

7.3 filter blank values and scattering Apply overall measuring procedure for each new lot of blank

filters.

7.4 maximum load of DPM on the filter Repeat analytical procedure once and check for memory

effects.

7.5.1 limit of detection (LOD) Apply analytical determination step (see 8.5 to 8.7) completely

at least six times for blank filters. LOD is calculated as three
times the standard deviation of the results obtained.
7.5.2 Apply analytical determination step (see 8.5 to 8.7) completely
limit of quantitation (LOQ)
at least six times for blank filters. LOQ is calculated as ten
times the standard deviation of the results obtained.
7.6 calibration function Use suitable statistical test.

7.7 coefficient of variation of procedure Apply analytical determination step (see 8.5 to 8.7) completely

at least six times at identical concentrations of a suitable test
substance (e.g. oxalic acid) at three different “steps” (e
...

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