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EPHECT is co-funded by European Union (Executive Agency for Health and Consumers- EAHC) framework of the Health Programmes 2006-2013

QUANTIFICATION OF THE PRODUCT

EMISSIONS BY LABORATORY TESTING

WP6

PART I CONSUMER PRODUCT TEST PROTOCOL

Marianne Stranger, Frederick Maes, Eddy Goelen (VITO)

Asger W. Nørgaard, Peder Wolkoff (NRCWE)

Gabriela Ventura, Eduardo de Oliveira Fernandes (IDMEC)

Evangelos Tolis, John Bartzis (UOWM)

January 2012

“© VITO, NRCWE, IDMEC, UOWM All rights on the materials described in this document rest with VITO, NRCWE, IDMEC and UOWM. This document is produced in the frame of the EPHECT –project. The EPHECT-project is co-funded by the European Union in the framework of the health Programmes 2006-2013. The information and views set out in this document are those of the author(s) and do not necessarily reflect the official opinion of the European Union. Neither the European Union institutions and bodies nor any person acting on their behalf, nor the authors may be held responsible for the use which may be made of the information contained herein. Reproduction is authorized provided the source is acknowledged.”

Distribution List

III

DISTRIBUTION LIST

Vlaamse Instelling voor Technologisch Onderzoek , Mol, Belgium

University of Western Macedonia Research Comitee, Athens, Greece

Agence Nationale de Sécurité Sanitaire, Alimentation, Environnement, Travail, Paris,

France

Technische Universität München, Germany

The National Research Centre for the Working Environment, Copenhagen, Denmark

Instituto de Engenharia Mecanica Environment, Porto, Portugal

Universita Degli Studi di Milano, Italy

Ipsos Belgium, Waterloo, Belgium

Table of contents

V

TABLE OF CONTENTS

Distribution List _________________________________________________________________ III

Table of contents ________________________________________________________________ V

List of figures ___________________________________________________________________ VI

List of tables ___________________________________________________________________ VII

List of acronyms _______________________________________________________________ VIII

CHAPTER 1 Introduction ________________________________________________________ 1

CHAPTER 2 EPHECT Umbrella for Consumer Product Testing ___________________________ 3

2.1 Consumer product emission testing versus Building product emission testing 3

2.2 Internal versus external diffusion in consumer product testing 5

2.3 EPHECT Umbrella for consumer product testing 8

2.3.1 Start-up conditions: emission test chamber system 10

2.3.2 Initial test conditions 10

2.3.3 Product specific test chamber conditions 11

2.3.3.1 Liquid consumer and personal care products 12

2.3.3.2 Solid consumer and personal care products 14

CHAPTER 3 EPHECT priority compounds ___________________________________________ 16

3.1 Strategy for the identification of key and emerging pollutants 16

3.1.1 Inclusion and exclusion criteria for the selection of key and emerging pollutants 16

3.1.2 Selection of key pollutants 17 3.1.3 Selection of emerging pollutants _______________________________________ 17

3.2 Overview of the key and emerging pollutants per consumer product category 18

CHAPTER 4 EPHECT Analytical Methods ___________________________________________ 20

4.1 Identification of the EPHECT analytical methods 20

CHAPTER 5 EPHECT QA/QC _____________________________________________________ 22

CHAPTER 6 EPHECT plan of work _________________________________________________ 24

6.1 Test chamber experiments of 15 product classes in 4 different labs 24

6.2 Translation into an operational plan of work 25

6.3 Reporting data for BUMAC imputation 26

References_____________________________________________________________________ 31

List of figures

VI

LIST OF FIGURES

Figure 1 Diagram of the kinetic processes involved in the mass transfer model of VOCs from material surfaces (adopted from Sparks et al. 1996). _________________________________________ 6

Figure 2 EPHECT Umbrella for consumer product testing __________________________________ 9 Figure 3 Operational plan of work for spray consumer product testing at VITO ________________ 26 Figure 4 Datasheet for WP6 emission data _____________________________________________ 30

List of tables

VII

LIST OF TABLES

Table 1 Selection of EPHECT consumer products _________________________________________ 3 Table 2 Units of emission test results from EPHECT consumer and personal care products ________ 5 Table 3 Start-up conditions EPHECT consumer product emission testing _____________________ 10 Table 4 Initial conditions for EPHECT consumer product emission testing ____________________ 10 Table 5 The ideal room dimensions and loading factors according to CEN TC 351 WG2 __________ 11 Table 6 Experimental conditions to test liquids, packed in a flask ___________________________ 12 Table 7 Experimental conditions to test liquids, packed in a spray bottle _____________________ 13 Table 8 Experimental conditions to test liquids, packed to be volatilized _____________________ 14 Table 9 Experimental conditions to test solid products; candle emissions ____________________ 15 Table 10. Selected key pollutants. ____________________________________________________ 17 Table 11 Selected emerging pollutants. _______________________________________________ 18 Table 12 Primary and secondary key pollutants, and liq. phase quantification. ________________ 18 Table 13 Specification of selected pollutants. ___________________________________________ 19 Table 14 Overview of the EPHECT analytical methods ____________________________________ 20 Table 15 Test chamber experiments of the EPHECT consumer and personal care products _______ 24 Table 16 EPHECT work division sheet _________________________________________________ 27

List of acronyms

VIII

LIST OF ACRONYMS

WP Work package quats Quaternair amonium salts THC Total Hydrocarbon

Chapter 1 Introduction

1

CHAPTER 1 INTRODUCTION

EPHECT work package 6 (WP6) involves 4 different laboratories that will perform lab testing

experiments in product test chambers of different dimensions. The main aim of this document is to

tune the laboratory activities of these research institutes for obtaining meaningful emission data.

Several aspects of the laboratory work are addressed and described in this document. These include:

The formulation of consumer product test protocols (chapter 2)

The assessment of priority compounds, studied in WP6 and further WPs (chapter 3)

The detailed description of analytical methods, used by the different involved laboratories (chapter 4)

The QA/QC strategy, applied in the EPHECT lab testing activities (chapter 5)

The EPHECT plan of work (Chapter 6)

Secondly this document may contribute to the definition and formulation of a general consumer

product test protocol, to assess emissions related to the use and typical use scenarios of consumer

and personal care products in households. It can be considered as a first step to obtain harmonized

lab testing experiments of consumer products. Since different laboratories are involved, using

emission test chambers of various dimensions, attention is also put to analyse products in more than

one lab. The latter experiments will provide valuable information concerning the error of emission

rates from consumer products, which are calculated based on this consumer product test protocol

presented in this document.

This document addresses a strategy to assess product emissions, related to the household use of

consumer products. This is based on available open literature and on pre-screening experiments,

performed by the laboratories involved in WP6. The strategy presented in this document is

optimized, updated and fine-tuned, based on the results of the EPHECT lab experiments that are

organised based on this protocol. The strategy presented here, more specifically applies to the 15

EPHECT product classes that comply with the 6 EPHECT criteria, defined in the EPHECT project

proposal. These selection criteria are the following:

- The product is used in households - The use of the product causes an exposure related to the use - The product emits key or emerging pollutants - The product has a considerable indicative household use frequency - The product mainly causes inhalation exposure - The use causes a health end point

Chapter 2 Ephect umbrella for consumer products testing

3

CHAPTER 2 EPHECT UMBRELLA FOR CONSUMER PRODUCT TESTING

2.1 Consumer product emission testing versus Building product emission testing

In the recent decades, research activities on product emissions were mainly focused on building

material emissions. The resulting emission test procedures, evaluation protocols (e.g. AgBB, Afsset

2009, GEV testing method, etc… ) and standards on emission test chamber procedures and sampling

techniques (ISO 16000-3, ISO 16000-6, ISO 16000-9) are well-established. ASTM D6670-01 (2007)

describes a more generic strategy for (VOC) emission testing from materials, products and

equipment (building materials, furniture, consumer products, printers, air cleaners etc.) typically

used in office and residential buildings, in full-scale chambers for VOC emission testing. However,

specifically for the consumer and personal care products studied in EPHECT, dedicated standards for

emission tests are currently not available. Test protocols as well as the results, reported in the open

literature, vary between laboratories and are difficult to compare, mainly due variable test conditions

(Derudi et al. 2012; Salthammer et al. 2009). Therefore, EPHECT aims at a maximal overlap between

the proposed consumer and personal care product test protocols and existing ISO standards and

other relevant emission test/evaluation protocols and standards for building materials.

Table 1 Selection of EPHECT consumer products

1 all purpose cleaner

2 kitchen cleaning agent

3 floor cleaning agent

4 glass and window cleaner

5 bathroom cleaning agent

6 furniture polish

7 floor polish

8 combustible air fresheners

9 air fresheners (spray)

10 passive units

11 electric units

12 coating products

13 hair styling products

14 deodorants (sprays)

15 perfumes


4

In building material emission testing, the products are typically installed as a static object in the test

chamber, with respect to relevant ISO standard (ISO 16000-9), test chamber dimensions, and

reported loading factors; the product emissions are assessed respecting valid emission test protocols.

The selection of EPHECT consumer and personal care products (listed in Table 1), consists of products

characterized by exposures which are related to the household uses and use scenarios (resulting

from EPHECT criterion nr. 2). Certain aspects of the emission test protocols proposed in EPHECT may

therefore differ from the well-established building material test protocols, because the emissions will

only occur when a certain interaction between the product and the user takes place: a certain use

scenario should thus be simulated in the test chamber.

An important aspect of an emission test protocol is its repeatability and applicability in emission test

chambers of various dimensions. For building material emission testing, the repeatability will mainly

be function of the product dimensions with respect to the loading factor and the test conditions

(respecting chamber start-up conditions and test conditions). For consumer product testing, the

repeatability of the use scenario can additionally have a considerable impact on the emission test

results.

The list of EPHECT consumer and personal care products, shown in Table 1, implies a variety of use

scenarios. These use scenarios are typically function of the product package (sprays, flasks, etc.) and

of the purpose of the product (floor cleaning agent to be diluted, floor polish to be used undiluted,

etc.). The product package on the other hand is closely related to the aggregation state of the

product (solid, liquid or gaseous). Each package and product purpose combination thus implies a

specific use scenario that should be simulated in the test chamber protocol, in a reproducible way, in

order to assess the emission characteristics and factors of the consumer product.

When assessing building product emissions in emission test chambers, the emission test result is

typically obtained as specific emission rate per hour and per m² surface (or per kg or per m³ product

or per unit). It is then used to model its concentration in a reference room. For consumer and

personal care product testing, the units of the emission factors are typically related to the amount of

used products. Depending on the product package (spray, flask, ..) this parameter can be expressed

per hour (passive units), and per grams aerosols or product (spray, electric units² ) or product as well

as per square meters surface covered with the product (if used on a surface). They are thus reported

in dimensions of µg/h per unit, in case no dosage is possible, and in µg per hour and per mass aerosol

for a spray product. Emission factors of liquid products applied on a surface are typically reported in

µg per hour and per m2, referring to the reference surface in the test room. An overview hereof is

shown in Table 2.


5

Table 2 Units of emission test results from EPHECT consumer and personal care products

Use and use scenario Emission Rate units Normalized Emission Rate units

Applied on a surface

all purpose cleaner

µg/h

(dilutions according to

manufacturer or market study)

Area specific emission rate

µg/(h.g.m2)

kitchen cleaning agent

floor cleaning agent

glass and window cleaner

bathroom cleaning agent

furniture polish

floor polish

Combustible, active or passive units

passive units µg/h

Mass specific emission rate

µg/(h.g)

electric units

combustible air fresheners

Sprayed on a surface or in the air

air fresheners (spray)

µg/h

(±0,5 sec or 0.5g automatic spray)

Mass specific emission rate

µg/(h.g aerosol)

(±0,5 sec or 0.5g automatic spray)

hair styling products

deodorants (sprays)

coating products (sprays)

perfumes

glass and window cleaner (spray)

2.2 Internal versus external diffusion in consumer product testing

The important questions about emission testing of building and consumer products are a) what specific pollutants are emitted that may affect occupants; b) how their emission profiles changes over time; and c) are the emission test results meaningful – i.e. are the results independent of test conditions In general, the emission can be characterized by two fundamental physical processes (see Figure 1), partly taken from Salthammer et al. 2009.

a) Gas-phase mass transfer (i.e. external diffusion) b) Source-phase mass transfer (i.e. internal diffusion)


6

Figure 1 Diagram of the kinetic processes involved in the mass transfer model of VOCs from material surfaces (adopted from Sparks et al. 1996).

The gas-phase mass transfer model (a) is based on molecular diffusion across a laminar boundary layer as described in equation (1), external diffusion.

)CC(k)CC(D

SER iSgiS

(1)

SER is the specific emission rate, D is the diffusion coefficient, is the thickness of the boundary layer, CS is the concentration of the target VOC at the source surface and Ci is the concentration of the target VOC in the air and kg is the gas-phase mass transfer coefficient. Process (b) is limited by internal diffusion from the interior of the source to the surface and can be described by equation (2).

)mm(kSER iSs (2)

Here, ms is the mass of the target VOC in the source, mi is the mass of the target VOC at the surface and ks is the source-phase mass transfer coefficient. Comparing emission test results from different chambers, three different scenarios have to be considered.

For kg >> ks: the emission is controlled by the external diffusion process and the thickness of the boundary

layer is directly related to the air velocity above the surface and turbulence, if it is a point source or activity related emission (e.g. spray). This applies to most wet-applied or liquid building products and certain consumer products during the drying/curing phase. Thus, the external diffusion is significantly affected by both surface air velocity/turbulence and the sample loading factor (m2/m3) (and associated vapour concentration within the chamber). The exact timing of the emissions testing is also critical for wet samples, in particular for temporary point sources. During this phase it is therefore paramount to control both air velocity (and/or turbulence), in order to prevent them from influencing/changing the test result. However, for temporary (activity related) point sources like spray products, the air velocity/turbulence becomes difficult to define and measure (which direction), and no

air

boundary layer

source

Ci

Cs

mi

ms

surface

gas-phase mass transfer(external diffusion)

source-phase mass transfer(internal diffusion)

kg

ks

Figure 3


7

harmonized practice exists. Thus, any comparison of such temporary sources will by nature be rather difficult to compare between laboratories with quite different chambers without applying rigorous control of all parameters prior to and during testing. However, the extreme sensitivity of the results to such a multitude of variables, does call into the question the validity of testing wet samples and point sources during the curing/drying stage or use. Further, a vapour pressure effect for such wet-like products cannot be ruled out; thus, some agreed upon test condition is helpful, but not a guarantee for obtaining comparable emission data.

For kg << ks: the emission is controlled by the internal diffusion process and the influence of the air flow condition in the chamber should be negligible. This applies to most solid building materials and to wet and liquid products after a surface film have been formed. There will be a transition phase where kG and ks compete together; thus, a more difficult situation arises for

kg ks or if the ratio ks/kg changes over time. For an ageing product, ks/kg will normally reach infinity over time. Thus, VOC emissions controlled by internal diffusion (dry products/materials) are largely independent of surface air velocity and loading, provided the exchange rate is fast enough to prevent a vapour pressure effect.

Thus, for consumer product testing, that is characterized by short-term or temporary activity related emission profiles and dominated by external diffusion any comparison of emission data obtained from different chambers (and even only slightly different test conditions) is by nature encumbered, even if harmonized test conditions are attempted. Two often quoted questions about the outcome of emission testing of building materials in a given chamber are: “does the chamber provide correct” SERs” and “how comparable are the round-robin testing results with other chambers”. These questions lead to the implicit assumption that SER data obtained from that particular chamber may be less reliable. These questions are deceptive, especially in view of round-robin testing, because a successful test requires that the results are independent of test conditions, i.e. the emission data are comparable. This is only the case for emissions where the mass transfer rate within the material is slower than in the boundary layer (i.e. “internal” versus “external” diffusion control). However, many other factors influence the SER, of which the most important ones are material homogeneity and laboratory performance (Oppl, 2008; Wolkoff et al., 2005). For consumer products with short-term emission profiles the issue becomes even more difficult, because of the difficulty of defining and controlling exactly identical test and activity conditions. In theory, under well controlled environmental conditions and satisfactory recovery (minimal sink (wall) effect) and adequate sampling (according to the objective) and analytical performance, comparable SERs should be obtainable for “internal” diffusion controlled emissions from homogeneous materials, independent of type of chamber. Thus, a third frequently asked question is “whether there exists an ideal chamber providing SER data that would be identical in real scenarios”, i.e. a golden chamber standard. One may ask how meaningful is it to predict (model) externally controlled SERs of VOCs and SVOCs from building materials and consumer products in real life indoor scenarios, in view of the inherent difficulties associated with the use of climate chambers. These include all the factors that influence the SERs and external factors. Thus, measured SER in a climate chamber, even with adequate recovery and low wall sink effects, may not be representative of the actual SER from the exact same building material/product in a real indoor setting. Well-knowing that chambers versus chambers may differ, in some cases for reasons outside of the performance of chamber itself, one should consider the objective of the emission test itself. Thus, the sampling strategy should reflect the objective of the testing. This in EPHECT means that the emission data should accommodate requirements set by the risk assessment objective. The important issue here is


8

that the risk assessment focuses on acute effects, semi-acute effects or longer-term (respiratory) effects. Thus, the sampling strategy should be adopted accordingly, where applicable. With this in mind, one may contemplate the feasibility and meaningfulness of transforming emission data, at least of short-term temporary (point source) emissions to a given model room. Other emission decay models are available simply by use of the known in the product.

2.3 EPHECT Umbrella for consumer product testing

Aiming at an EPHECT test protocol that implies a maximal overlap between the test scenario for the

various selected consumer product classes, as well as a maximal overlap with existing knowledge on

building material emission testing, the consumer product test protocols are presented in the EHPECT

umbrella.

This umbrella, pictured in Figure 2, shows common as well as different steps between the proposed

test scenarios for the different EPHECT product classes. The upper level of Figure 2 indicates the

generic aspects of the test protocol, whilst the lower levels are more specifically dedicated to the

specific consumer product package, use scenario and purpose. The reported test conditions result

from a review of existing open literature on consumer and personal care product emission testing

and from pre-screening experiments, performed in EPHECT. These pre-screening experiments have

addressed several practical issues on test performance, feasibility and repeatability of tests and test

results.

The resulting EPHECT umbrella consists of 3 levels:

- Start-up conditions

- Initial test chamber conditions

- Product specific test chamber conditions

These 3 levels are discussed more in detail in the following paragraphs.


9

Figure 2 EPHECT Umbrella for consumer product testing

EPHECT umbrella for Consumer Product Emission Testing

- AIR FLOW: deviation of exhaust flow with intake flow < 5%

- TVOC (ISO 16000-9) < 20 µg.m-3

; individual VOC < 2 µg.m-3

(radiello code 130 -min 48h, max 5d)

- collect/sample up to 80% of the intake flow

- AIR EXCHANGE RATE: 0.5/h ± 5% deviation and ±3% accuracy

- RECOVERY AND SINK permeation or diffusion tube - known concentration toluene and n-dodecane in the chamber - conc after 72h in room - recovery > 80%Start-up

conditions

(ISO 16000-9)

Initial test

chamber

conditions

(ISO 16000-9)

- AIR VELOCITY above the sample 0.1-0.3 m/s and accuracy 0.1m/s

- RH 50% ± 5% and ±3% accuracy

- T 23°C ± 2 and accuracy ±1°C

- VOC level (FID)

Liquid

(fluid, cream or gel)Solid

Aggregation

state of the

product?

- weigh before and after test

Flask

Spray To

volatilize

To burn

- Chamber < 20L, 20L - 50 m3

- Weigh before and after test

- weigh before and after

test

- ideally: automatic spray

of 0.5 sec

Use

diluted

Use

undiluted

Rinse

after use Don't rinse

after use

Rinse

after use

Don't rinse

after use

- quantity/dilution: function

of real use scenario and

expected (T)VOC levels

- Rinse + wet mop outside

test chamber

- Sample collection:

t0: application (0-1h)

t1: 1h-3h

t2: 3h-5h

t3: 5h-7h

- quantity/dilution: function of

real use scenario and

expected (T)VOC levels

- Wet mop outside test

chamber



t1: 1h-3h

t2: 3h-5h

t3: 5h-7h

- quantity: function of real

use scenario and expected

(T)VOC levels

- Rinse + wet mop outside

test chamber



t1: 1h-3h

t2: 3h-5h

t3: 5h-7h

Spray on

a surface

Spray in

the air

- # sprays is function of real use scenario’s and expected (T)VOC levels

- Sample collection:t0: spray (0-1h)t1: 1h-3h t2: 3h-5h t3: 5h-7h

- PM monitoring

- spray at time t0

spray orientation: angle 45°,

upwards to air movement

- sprayed quantity is

approx. 0.5g per 1m3 or 1

automatic spray at max

position if electric device

- Sample collection:t0: spray (0-1h)t1: 1h-3h t2: 3h-5h t3: 5h-7h

- PM monitoring

- weigh before and after test

- light during at least 6h (taken

burning time of candle in

consideration)

- light with a gas lighter


t0: 0-3h after installation and lighting

t2: 3h-4h

t2: 4h-5h

t3: 5h-6h (extinguish candle after 5h)

- THC monitoring, PM monitoring,

EC/OC assessment, O2 monitoring at

inlet and outlet

Passive

Active

Electric

unit

To be

heated by

a candle

- electricity supply in room

- run test until at least 3h after

equilibrium

- position max

Sample collection:

t0: 0-3h after installation

t2: 3h-4h

t2: 4h-5h

t3: 5h-6h

- PM Monitoring

- run test until at least 3h

after equilibrium

- dimensions (distance

candle, quantity, dilution)

Sample collection:


t2: 3h-4h

t2: 4h-5h

t3: 5h-6h

- THC monitoring

Product specific

test chamber

conditions

- run test until at least 3h

after equilibrium

Sample collection:


t2: 3h-4h

t2: 4h-5h

t3: 5h-6h

LF ideal room ‘Arrêté sur l’etiquettage (NOR :

DEVL1104875A); CEN TC 351 WG2

if surface = window:LF = 0.07 m

2/m

3

if surface = floor:

LF = 0.4 m2/m

3

if other surface = adapted m2/m

3

- quantity: function of real

use scenario and expected

(T)VOC levels

- Wet mop outside test

chamber



t1: 1h-3h

t2: 3h-5h

t3: 5h-7h

Test ends when

THC =< 5%

deviation of initial

concentration

Test ends when

THC =< 5%


concentration

Test ends when

THC =< 5%


concentration

Test ends when

THC =< 5%


concentration

Test ends when

THC =< 5%


concentration

Test ends when

THC =< 5%


concentration

After 6h

After 6hAfter 6h

After 6h

LF ideal room ‘Arrêté sur l’etiquettage (NOR :

DEVL1104875A); CEN TC 351 WG2

if surface = window:LF = 0.07 m

2/m

3

if surface = floor:

LF = 0.4 m2/m

3

if other surface = suitable

surface m2/m

3

Chamber dimensions in

relation to spray strength

(> 0.5 m3)


10

2.3.1 Start-up conditions: emission test chamber system

The test chamber start-up conditions in the EPHECT consumer product testing procedures are the

same as those reported in ISO 16000-9 (Indoor Air – Part 9: determination of the emission of volatile

organic compounds from building products and furnishing – emission test chamber method). This

implies the installation settings summarized in Table 1. The listed parameters have been measured or

set before the experiment takes place and will be kept constant during the experiment.

Table 3 Start-up conditions EPHECT consumer product emission testing

Aspect Conditions

Air supply The emission test chamber has facilities capable of continuously controlling the air change rate at a fixed value with an accuracy of ± 5%

Air flow The deviation of the exhaust flow with the intake flow is < 5%

Air Exchange rate 0.5/h ± 5% deviation and ± 3% accuracy

Sample collection limit The sum of sampling air flows can be up to 80% of the intake flow

Recovery and sink Using a permeation of diffusion tube, insert a known concentration of toluene and n-dodecane in the chamber, measure the concentration after 72h in the room. The recovery should be > 80%

2.3.2 Initial test conditions

The initial test conditions are also established in agreement with ISO 16000-9. In consumer product

testing these test conditions are labeled as ‘initial’ conditions, since the emission tests of certain

products might disturb one or more of the initial conditions. This could for instance occur when

assessing the emissions of a diluted floor cleaning agent: applying the product in the chamber will

increase the relative humidity that was initially set at 50%. They are however considered to be less

critical when realistic user scenarios are simulated.

Table 3 summarizes the initial test conditions for EPHECT consumer product testing.

Table 4 Initial conditions for EPHECT consumer product emission testing

Aspect Conditions

Temperature 23°C ± 2°C (accuracy of 1.0°C)

Relative humidity 50% ± 5% (accuracy of 3%)

Air velocity The air velocity above the sample is 0.1-0.3 m/s (accuracy 0.1 m/s) (with an averaging time of 1 minute)

Supply air & background concentrations (TVOC and VOCS)

The concentration of TVOC is below 20 µg.m-3

; Individual VOCs occur at concentrations below 2 µg.m

-3

(radiello code 130 – at least 48h, maximal 5 days)


11

During the experiments, temperature, relative humidity and air flow rate are monitored

continuously.

2.3.3 Product specific test chamber conditions

This lower level of the EPHECT umbrella describes more specific test conditions for consumer and

personal care product emission testing.

All emission data measured in the test chamber are recalculated to the ideal room dimensions

(CEN/TS 16516 and CEN TC 351 WG2). This implies a room with a total volume of 30 m3, and an air

change rate of 0,5 h-1. This ideal room consists of a floor of 12 m2, a ceiling of 12 m2, one door of 1,6

m2, walls of 31,4 m2 (excluding door and window) and joints (or small surfaces) of 0,2 m2. Table 5

shows an overview of these dimensions. For the windows, reference is made to l’Arrêté sur

l’étiquettage’ NOR : DEVL1104875A and CEN TC 351 WG2, with a surface of one window equal to 2

m2. In case a product can be used on several types of surfaces, the most important surface will be

taken into account (in agreement with NOR: DEVL1104875A). Using the dimensions of this ideal

room in the generation of emission data, will also enable us to refer to EU LCI values. However, a

direct comparison should be carried out with some caution, because LCI values refer to the emission

after 28 days only. Further, it is probable that LCI values in the future will consider multiple-source

contribution.

Whenever applicable, the loading factors, related to the ideal room dimensions, are respected in the

EPHECT test protocols. This implies that e.g. a floor cleaning agent will be tested respecting a loading

factor of 0.4 m2/m3 and a window cleaning agent will be applied respecting a loading factor of 0.07

m2/m3. Products to be applied on surfaces (other than floor, ceiling, door, window or walls) will be

tested respecting the loading factor included in Table 5 as ‘joints or small surfaces’, as far as this is a

representative loading factor for the use of that product in a room.

Table 5 The ideal room dimensions and loading factors according to CEN TC 351 WG2 and CEN/TS 16516

Surface [m

2]

Loading factor [m

2/m

3]

Floor 12 0,4

Ceiling 12 0,4

1 door 1,6 0,05

1 window* 2 0,07

Walls (excl. window & door) 31,4 1

Joints (or small surfaces) 0,2 0,007

* only in CEN TC 351 WG 2

Because the major influence of the aggregation state on the use and use scenario of a product, the

first division is made between liquid and solid consumer and personal care products.


12

2.3.3.1 Liquid consumer and personal care products

Liquid consumer and personal care products include fluids, creams and gels. Depending of the

product purpose, they can be found in different packages. They can be stored (1) in a flask, (2) in a

spray bottle (pistol spray, continuous spray or automatic spray), or (3) in a format to be volatilized.

The test protocol scenarios, proposed in the EPHECT umbrella depend on this product package. All 3

options are discussed below in detail:

Products packed in a flask

Liquid products, stored in a flask, may involve products to be used in a diluted as well as in an

undiluted concentration. They are typically applied on a surface. The type of surface on which the

product is tested will be of a representative material, typical for the purpose of the product.

Throughout the EPHECT project, similar products tested in more than one lab will be tested on the

same surface material. However, for full scale chambers, a metal surface (steel) may be preferable to

be able to obtain an even surface. After the application, the surface may need to be rinsed. For

practical purposes an additional rinsing process after surface drying will interfere in a full scale

experiment. Thus, data obtained from full scale testing might be considered a worst case scenarion,

because there is no information about the effect of rinsing effect. For small chamber testing both

application and eventually rinsing may have to be carried out outside the chamber. The

interpretation from outside conditioning should be carried out with caution due to lost volatiles.

EPHECT consumer and personal care products on which this section applies are all purpose cleaners,

kitchen cleaning agent, floor cleaning agent, (no spray) window cleaner, (no spray) bathroom

cleaning agent, (no spray) furniture polish and floor polish. Table 6 gives an overview of the

conditions for emission experiments of liquids, stored in a flask.

Table 6 Experimental conditions to test liquids, packed in a flask

Aspect Conditions

Room dimensions No restrictions

Loading factor In agreement with Table 5

Quantity If diluted use: dilution according to the results from the market study on EU uses and use patterns (WP5) and according to expected (T)VOC levels

*.

If undiluted use: quantity according to the results from the market study on EU uses and use patterns (WP5) and according to expected (T)VOC levels

*.

Scenario Rinse if use scenario prescribes to do so

Wet mop out room

Sampling t0: during the application (0-1h) t1: 1h – 3h t2: 3h – 5h t3: 5h – 7h

End of the test When THC has less than 5% deviation from the initial concentration

* This implies that the used quantity may be multiplied if a first test leads to values below the detection limits of the used

techniques. After the experiments this multiplication should be taken into account.


13

Products packed in a spray bottle

Liquid products packed in a spray bottle will, depending on the product purpose, be sprayed in the

air or on a surface. The type of spraying bottle, and thus the use scenario, will be related to the

product purpose. Products to be sprayed on a surface are packed in a pistol spray bottle; products to

be sprayed in the air will be packed in a bottle to allow continuous or automatic (with electricity

supply) spraying.

In order to avoid spraying on the test chamber walls, the allowed test chamber dimensions to study

these products are restricted to 0.5 m3 or larger.

EPHECT consumer and personal care products, on which this section applies are air freshener sprays

(manual spray or automatic spray), hair styling products (sprays), deodorant sprays, coating product

sprays, and perfumes.

Table 7 gives an overview of the conditions for emission experiments of liquids, packed in a spray

bottle.

Table 7 Experimental conditions to test liquids, packed in a spray bottle

Aspect Conditions

Room dimensions Larger than 0.5 m3

Loading factor If spraying pistol (to be sprayed on a surface) in agreement with Table 5

Quantity If spraying in the air: spray quantity is limited to approximately 0.5g of product ( 0.5s of spraying per m

3 test chamber), or one automatic spray at maximum

capacity) and according to expected (T)VOC levels*.

If spraying on a surface: quantity according to the results from the market study on EU uses and use patterns (WP5) and according to expected (T)VOC levels

*.

The product is weight before and after the experiment.

Scenario If sprayed on a surface: representative selection of the surface material to be sprayed on

Sampling t0: during the application (0-1h) t1: 1h – 3h t2: 3h – 5h t3: 5h – 7h PM monitoring

End of the test When THC has less than 5% deviation from the initial concentration



Products packed to be volatilized

Products to be volatilized can be passive units that volatilize without any user interaction, or active

units, that require a source of heating. Both types of products, packed to be volatilized, need time to


14

equilibrate with the surrounding air, before any assessment of the product emissions can take place.

In EPHECT, this period to equilibrate is set on 3 hours (equal to 1.5 air changes).

The only restriction on test chamber dimensions is the size of the product to be tested, that should fit

in the test cell.

EPHECT consumer and personal care products, on which this section applies, are passive and electric

units. These units may be air freshener units as well as insect repellent devices.

Table 8 gives an overview of the test conditions for liquid products, packed to be volatilized.

Table 8 Experimental conditions to test liquids, packed to be volatilized

Aspect Conditions

Room dimensions No restrictions (the product should fit)

Loading factor Maximum one unit per full scale chamber

Quantity If passive unit: not applicable If active unit: position max The product is weighed before and after the experiment.

Scenario Passive units should be placed on a board, minimum twice the area of the unit Active units may need electrical supply in the exposure chamber

Sampling t0: 0 h – 3h after installation t1: 3h – 4h t2: 4h – 5h t3: 5h – 6h Full scale chamber: Sample in quadruplicate after establishment of chamber equilibrium (by PID). PM monitoring when active units

End of the test After 6 hours

2.3.3.2 Solid consumer and personal care products

Solid consumer products, considered in EPHECT, are candles. This strategy is based on available open

literature (Derudi et al. 2012), and on the AISE candle emission test protocol (AISE, Development of a

standard methodology for measuring emissions from candles, 2012) that was made available for

EPHECT. The candle should be inserted in the test chamber with the air flow on and should be lighted

with a gas lighter. Then the test chamber must be closed. The candle emissions expected to

equilibrate during 3 hours. Sampling however starts in the period of 0h to 3h after lighting the

candle. The sampling is performed in the following three hours. When the last sampling hour starts,

the candle should be extinguished, and the emissions are monitored during one more hour. For small

test chambers the air flow should be 0.5 m³/h per candle. In case of large test chambers an air

exchange rate of 0.5 h-1 should be used. The air velocity (speed) in the test chamber in the vicinity of


15

the candle should be measured without the candle being lighted and should be lower than 0.30 m/s.

The air velocity (speed) with a lighted candle is higher, due to the convection movements caused by

the thermal gradients. The burning rate should be determined after the test, and should be

compared with the burning rate of a duplicate candle burned in a normal room. The two values

should not differ by more than 15%.

The only restriction on test chamber dimensions is the size of the product to be tested.

For candle emissions special attention should be put on relative humidity and oxygen supply. Relative

humidity should be kept below 75%, in order to avoid wall condensation in the room (AISE protocol

for candle emission). The outlet oxygen concentration shouldn’t not decrease more than 2.5%

compared to the inlet oxygen concentration (AISE protocol for candle emission; this number ).

Table 9 shows an overview of the experimental conditions to test candle emissions.

Table 9 Experimental conditions to test solid products; candle emissions

Aspect Conditions

Room dimensions No restrictions – the candle should fit in

Loading factor Small test chambers - air flow of 0.5 m³/h per candle Full scale test chambers - air exchange rate of 0.5 h

-1

Quantity 1 candle; more than one taking into account expected (T)VOC levels*.

The product is weighted before and after the experiment.

Scenario The candle is placed on a preconditioned surface in the test chamber. It is lighted using a gas lighter.

Sampling t0: 0 h – 3h after lighting the candle t1: 3h – 4h t2: 4h – 5h t3: 5h – 6h (with the candle extinguished) PM monitoring EC/OC assessment O2 monitoring at inlet and outlet

End of the test After 6 hours



Chapter 3 Ephect priority compounds

16

CHAPTER 3 EPHECT PRIORITY COMPOUNDS

3.1 Strategy for the identification of key and emerging pollutants

3.1.1 Inclusion and exclusion criteria for the selection of key and emerging pollutants

The main focus of EPHECT is the identification and quantification of air pollutants that potentially

may be associated with adverse respiratory effects, i.e. (chemo-) sensory irritation in the airways,

asthma and pulmonary effects.

Although it is well-established that a number of fragrances are known to cause dermal effects by

contact (skin allergy), there is no supporting evidence that such compounds in ozone poor

environments are associated with airway effects (1).

A large number of common industrial chemicals have been assessed for risk of airway effects, like

asthma. In general, except for acid anhydrides and isocyanates, e.g. (2), industrial chemicals have not

been identified to cause asthma (1;3;4). This also goes for chemicals like phthalates (1;5) although

they have received much publicity in the literature. Further, polyethylene glycol ethers are not

considered to be airway sensitizers, e.g. (4;6), in agreement with international scientific guidelines

(7;8); however, recent focus on this type of pollutants (9;10) have prompted the selection of 2-

butoxyethanol as a pollutants of some general interest; further, this common solvent has also been

proposed as a potential proxy for terpene-containing consumer products, cf. (11).

Formaldehyde have previously been associated with asthma in children, however, supporting

evidence has not been identified (12;13) and this is further strengthened by lack of biological

plausibility (14).

A number of reviews argue that increase of airway health effects in cleaning personnel is associated

with the use of cleaning agents, e.g. (15-17). Suspected product categories and pollutants that have

been suggested as important contributors to health effects among cleaning personnel are products

in spray-form, amines (e.g. ethanolamine), chlorine bleach and other disinfectants like quaternary

ammonium compounds and glutaraldehyde (15;17). It has been argued that quaternary ammonium

compounds only have occupational relevance (1), however, the concern may be extended in indoor

environments to new types of quaternary compounds.

Fragrances like pinenes and limonene have also been suggested as airway sensitizers and sensory

irritants; this, however, is judged only to be relevant in ozone-enriched environments, e.g. (18). Thus,

more research into cause-effect relationships is recommended for this group of pollutants, e.g. (13).

In summary, chemically non-reacting VOCs in general are not considered to cause respiratory effects

at indoor concentrations. The ozone-initiated reactions with carbon-carbon unsaturated VOCs

(alkenes), present in a number of fragrances, need to be investigated further, cf. (18); not only


17

because of the formation of a host of new oxygenated species (e.g. formaldehyde) of which there is

concern about their airway effects, e.g. (19;20), but also the concern about the formation of ultrafine

particles, see below.

Ultrafine particles have received much focus and concern about respiratory and cardio-pulmonary

effects during the last decade (21). More recently, the focus has been on spray products and

reported respiratory effects, e.g. (22-24) and combustion of e.g. candles and incense. Another

relevant issue of concern is the ultrafine particle formation in the ozone-initiated alkene (e.g.

terpenoids) reactions, e.g. (18).

3.1.2 Selection of key pollutants

The selection procedure for key pollutants has been depending on the Index project (25), WHO

indoor air guidelines (26), WHO air quality guidelines (27), and SCHER (28), see Table 10.

Table 10. Selected key pollutants.

Key pollutants INDEX 2005 WHO 2010 WHO 2000 SCHER

Ammonia x

Benzene x x x

Naphthalene x x x

Formaldehyde x x x

Ultrafine particles x x

-pinene x

Limonene x

Carbon monoxide x x x

Nitrogen dioxide x x x

Ozone (18)

3.1.3 Selection of emerging pollutants

The selection of emerging pollutants has partly been depending on the outcome of the EPHECT WP4

deliverable ‘Literature review on product composition, emitted compounds, emissions rates and

health end points from consumer products’, partly from a compiled selection of relevant emission

literature from the product categories, close to 100 papers (Appendix 1), including recent literature

findings deemed to be of potential interest and concern as a research gap, and identified jointly with

WP7. The selection is further supported by the pre-screening process carried out in winter 2010-

spring 2011. Table 11 shows the selected emerging compounds.

In addition to the above listed compounds others will also be identified during the lab testing

experiments, although they are not assessed to pose respiratory effects, e.g. aromatic compounds,

phthalates, PAH, and chlorinated compounds.


18

Table 11 Selected emerging pollutants.

Potential source Odour Sensory irritant

Potential Lung effects

Examples literature

Acrolein Combustion x

Butoxyethanol Common solvent x (x) (10)

Terpenoids Fragrances x (x)* (x)a

(18)

QUATsb

Biocides x (29;30)

Chloramines Disinfectants x x (30)

Perfluorinated siloxanes Coatings x (22-24)

ROSc

Ozone-initiated reactions Particles

x (31)

a) In ozone enriched environments. b) Quaternary ammonium compounds. c) Reactive oxygen species.

3.2 Overview of the key and emerging pollutants per consumer product category

The selection of key and emerging pollutants for the different product categories are briefly listed in

Table 12 and further specified in Table 13. This selection is based on open literature and on pre-

screening experiments, performed in EPHECT. For a complete list, see Appendix 2. Products listed in

column ‘1. Primary Priority key pollutants, gas phase’ must be quantified in gas phase for each

product. Also the major VOCs with a relative intensity above 10% must be quantified. The

compounds listed in the column ‘2. Secondary priority key pollutants’ may be emitted by certain

products, they are detected quantitatively if possible. The 3rd column lists the compounds that will be

detected in the liquid phase of the product. Since up to now little or no literature is available on the

presence of miscellaneous compounds in the various consumer product classes, this set of

compounds is being assessed for any product tested in EPHECT.

Table 12 Primary and secondary key pollutants, and liq. phase quantification.

1. Primary priority key pollutants, gas phase 2. Secondary priority key

pollutants, gas phase

Selected pollutants

(%), liq phase

A1 All purpose cleaner Terpenoids, aldehydes, particles, quats, NH3, disinfectants

Micl. Compounds Terpenoids, aromates, aldehydes

A2 Kitchen cleaning agent Terpenoids, aldehydes, particles, quats, NH3, disinfectants

Micl. Compounds Terpenoids, aromates, aldehydes

A3 Hard surface (floor) cleaner Terpenoids, aldehydes, particles, quats, NH3, disinfectants

Terpenoids, aromates, aldehydes

A4 Glass and window cleaner Terpenoids, aldehydes, particles, quats, NH3, disinfectants


A5 Bathroom cleaning agents Terpenoids, aldehydes, particles, quats, NH3, disinfectants


A6 Furniture polish Terpenoids, aldehydes, particles Silanes/siloxanes Terpenoids, aromates, aldehydes

A7 Floor polish Terpenoids, aldehydes, particles Terpenoids, aromates, aldehydes

A8 Combustible air freshener Terpenoids, aldehydes, particles, aromates, CO, NO2, EC/OC, oxiPAH

A9 Air freshener (spray) Terpenoids, aldehydes, particles Terpenoids, aromates, aldehydes


19

A10 Passive units (air freshener) Terpenoids, aldehydes, particles Terpenoids, aromates, aldehydes

A11 Electric units (air freshener, insecticide)

Terpenoids, aldehydes, particles Terpenoids, aromates, aldehydes

A12 Coating products for (hard surfaces, leather, textiles)

Terpenoids, aldehydes, particles Silanes/siloxanes Terpenoids, aromates, aldehydes

13 Hair styling products (sprays, gel)

Terpenoids, aldehydes, particles Silanes/siloxanes Terpenoids, aromates, aldehydes

A14 Deodorants (sprays) Terpenoids, aldehydes, aromates particles Terpenoids, aromates, aldehydes

15 Perfumes Terpenoids, aldehydes, aromates particles Terpenoids, aromates, aldehydes

A17 Deodorizers Terpenoids, aldehydes, particles Terpenoids, aromates, aldehydes

A18 Toys Terpenoids, aldehydes, aromates Micl. Compounds

A19 Magazines Aldehydes

The consumer product classes written in italics are not compulsory in EPHECT

Table 13 Specification of selected pollutants.

Generic name Compounds

Terpenoids limonene

-pinene

geraniol

a-terpineol linalool Aldehydes: formaldehyde acrolein

glutaraldehyde

acetaldehyde Aromates benzene

toluene

xylenes

Styrene

PAHs (naphthalene and benz-a-pyrene)

Disinfectants chloroamines hypochlorite

H2O2

CO

NO2

Ammonia

Silanes/siloxanes/polymers +/- fluorinated

Quaternary ammonium chlorides

Particles (spray and combustible products only)

Micl. compounds (not associated with respiratory diseases)

PCBs

PCDDs

Phthalates

Chapter 4 Ephect analytical methods

20

CHAPTER 4 EPHECT ANALYTICAL METHODS

4.1 Identification of the EPHECT analytical methods

For each compound to be identified, including the EPHECT priority compounds, details on the

analytical method for compound identification and quantification are established. An overview of the

methods is shown in Table 14.

Table 14 Overview of the EPHECT analytical methods

Terpenoids: Tenax TA tubes C6-C16 ISO 16000-6 limonene alpha-pinene geraniol a-terpineol linalool

TD GC MS sample max. 5 l; 20-200 ml/min column: slightly polar, (5 % phenyl / 95 % methyl poly siloxane capillary column) calibration: methanolic solution of these compounds; spike +/- 5 µl on Tenax tube n

Aldehydes: sampling on DNPH tubes; ISO 16000-3

formaldehyde acrolein glutaraldehyde acetaldehyde

check effective sampling range (Waters booklet): 50 l for 10-1000 ppb calibration with hydrazon standards analysis: HPLC-UV or DAD

Aromates:

Benzene toluene xylenes Styrene PAHs: naphthalene & benz-a-pyrene

See terpenoids ISO 16000-12: not possible for test chamber samples Alternative: PDMS/Tenax 150 ml/min – 60 min; TD-GC-MS with cold trap for high boilers

Disinfectants:

chloroamines hypochlorite (H2O2)

Hery et al. (1995) sampling on filter cassette (Teflon filter and 2 impregnated filters with As2O2 and Na2CO3); 1 l/min; 2 hours; IC; result = sum of chloroamines + ClO

-

Micl. compounds (not associated with respiratory diseases)

PCBs PCDDs Phthalates Isothiazolinones

see PAHs (Alternative: PDMS/Tenax 150 ml/min – 60 min; TD-GC-MS with cold trap for high boilers)

Chapter 4 Ephect analytical methods

21

CO

NDIR monitor method: EN 14626; or continious low cost logger Both methods need calibration

NH3

Sampling on Orbo 554 tubes (conform OSHA method ID-188 Analysis: ion selective electrode

NO2

ISO 16000-15: short term measurements; continuous analytical monitor chemo luminescence ISO7996; alternative manual photometric reference methods with impinger (Saltzman method) ISO 6768


1. Sampling on tenax tubes (see terpenoids) and analysis by GC-MS/MS using both EI and CI. 2. Sampling on quartz filters (e.g. Whatman Grade GF/C - 1.2 um retention, Cat No. 1822-025). Extraction of filters by PLE and subsequent analysis of extracts by LC-MS

Quaternary ammonium chlorides (QUATs)

Sampling on quartz filters e.g. (Whatman Grade GF/C - 1.2 um retention, Cat No. 1822-025). Extraction of filters by PLE and subsequent analysis of extracts by LC-MS.


Primary aerosols: Optical method (Grimm), aerodynamic and electric mobility (TSI, Dekati). Size distribution, concentration or particle number Secondary aerosol filter sampling

Chapter 5 Ephect QA/QC

22

CHAPTER 5 EPHECT QA/QC

The strategy for quality control of the results obtained under EPHECT focuses on a quality control of the activities performed by laboratories that currently perform chemical analysis of air sampling. It is assumed that all the labs have an internal quality control system; however for EPHECT it is necessary to evidence this control. That will be assured by the following actions:

1) Field blanks should be performed. Before the realization of an emission test experiment a blank of the test chamber should be taken. The concentration values of the blanks should be reported.

2) The analysis of the compounds sampled on adsorbents should be performed in duplicate. For continuous monitoring (such as THC, PMx, NO2 and CO) this concept is not applicable.

It may not be feasible to sample all cartridges in duplicate, since the tests are of short duration, several cartridges should be loaded at the same time and room dimensions, thus intake air flows, may differ. It will for instance be possible to sample two Tenax tubes simultaneously, but it may then be difficult to sample two DNPH cartridges simultaneously as well, because the EPHECT emission test protocol sets a sample collection limit at maximum 80% of the total intake flow (with respect to ISO-16000-9). In such a case the one DNPH cartridge will be analyzed in duplicate. So, whenever possible, sampling and/or the analysis should be performed in duplicate; a maximum deviation of 20% between the results is allowable.

3) To control the VOCs quantification, a blind solution containing terpenes and aromatic

hydrocarbons with a certain concentration will be prepared by IDMEC, and will be sent to the other partners. IDMEC will also participate in this control, but the analysis will be done by a researcher without access to the true values.

4) To control aldehyde quantification, a blind solution containing formaldehyde, acetaldehyde,

acrolein and glutaraldehyde will be prepared by IDMEC and sent to all partners. IDMEC will also participate in this control, but the analysis will be done by a researcher without access to the true values.

For the calculation of the total uncertainty of the analysis procedure, the following formula is

proposed:

Chapter 5 Ephect QA/QC

23

Where: Xr = the reference value

x = is the average of the analysis performed in the laboratory

s = the standard deviation of the individual results

(This formula is extracted from EN 482:2005)

5) The compounds listed in Table 16b as ‘2nd level: complex’ (ammonia / Silanes / siloxanes / polymers / fluorinated and Quaternary ammonium chlorides (QUATs) / phthalates) will be sampled by the respective labs who perform the emission tests, but the analysis will be performed centrally by one selected lab (which is part of WP6). This lab is selected based on the experience and equipment of the laboratories.

For these compounds only one sample will be collected at the peak concentration. QA/QC will be performed using (C)RM if available (external).

6) Whenever applicable calibration records should be presented.

7) The heterogeneity of a products is an aspect that should be considered. Where possible, a

product test is performed in duplicate. This implies that two different product packages should be bought, and each should be subjected to an independent test. The results should be presented individually.

8) The product to be tested should be ‘new’ (the package cannot be opened, the product cannot be

used before).

9) The activities of preparation of the products to be tested shall have no or as little as possible,

impact on the integrity of the sampled product. This relates to minimising:

a) evaporation of volatile substances

b) deterioration of the product due to heat production during sampling or sub-sampling;

c) contamination of the sample(s) by the sampling devices, the other sample(s);

To control these potential influences of the preparation activities of the product, all preparatory

steps should be taken in a short period of time.

Chapter 6 Ephect Plan of work

24

CHAPTER 6 EPHECT PLAN OF WORK

The previous chapters have described (1) EPHECT protocols for test chamber experiments per

product type/package, (2) EPHECT priority compounds per product class focussing on respiratory

health, (3) EPHECT methods for sampling and analysis and (4) EPHECT methods for quality control

and assurance. This chapter combines the previous sections in one overall plan of work, distributing

the lab testing experiments and the sample analysis amongst WP6 associated partners.

6.1 Test chamber experiments of 15 product classes in 4 different labs

Table 15 shows the EPHECT consumer product classes that are analysed in the different involved

laboratories in WP6.

Table 15 Test chamber experiments of the EPHECT consumer and personal care products

NRCWE (10)

VITO (6)

UOWM (5)

IDMEC (5)

Analysed in more than 1 lab

all purpose cleaner

X X X

kitchen cleaning agent X X

floor cleaning agent X

X

X

glass and window cleaner

X

bathroom cleaning agent X

furniture polish X

X X

floor polish X

X X

combustible air fresheners

X

X

air fresheners (spray) X X

X

passive units X X

X

electric units X X

coating products X

hair styling products

X

deodorants (sprays)

x

X X

perfumes X X X

this product class is tested in all laboratories (same brand) X this product class is tested by one or a few laboratories (may be different brands)

The brand and product type selection for EPHECT lab testing experiments is based on the IPSOS

market study. This market study was part of EPHECT and took place in 4 EU regions. It led to the

identification of the most used product brand and type in all 4 regions, as well as to the identification

of the EU most used brand per product class. The following strategy will be followed:


25

Selection of product 1: EU most used

For each EPHECT product class, the EU most used brand (according to the EPHECT IPSOS market

study) is tested applying the above specified emission test protocol, in at least one of the

involved labs.

Selection of product 2

For the majority of the products (11 out of 15; excluding glass and window cleaner, bathroom

cleaning agent, coating products, hair styling spray), a second product brand is tested, applying

the above specified emission test protocol. This second product is then the brand, which

according to the IPSOS market study, is most used in the region of the analysing lab.

Inter-lab study

For 3 product classes (kitchen cleaning agent, electric air freshener, and perfume), the same

product brand and type is exchanged and tested in all 4 involved laboratories, allowing a

comparison of the emission test results within the participating labs.

Complementary to the lab testing experiment to assess the product emissions, TUM is responsible

for quantification of selected compounds (terpenoids, aromates and aldehydes) in 15 of the tested

liquid products.

In agreement with the available techniques in the 4 involved laboratories, the analysis of the

compounds that have to be identified and/or quantified is distributed between the different involved

laboratories. Table 16 shows this work division sheet, which clarifies whether samples are analysed in

the laboratory where the experiment took place, or is sent to another laboratory that is responsible

for the analysis of the samples from the whole team.

6.2 Translation into an operational plan of work

Combining Tables 12 and 13 on key and emerging pollutants expected to be present in the tested

consumer products, together with the work division and QA/QC (table 16) as well as the EPHECT

emission test umbrella, a detailed operational plan of work for consumer product emission testing

can be formulated for each product class.

This plan of work then schedules the successive sampling phases during each emission test

experiment and specifies the different samples to be collected in each phase; adapted to the

preconditions of each laboratory (test chamber dimensions and related total intake flow). An

example of the operational plan for the VITO lab testing experiments on spray type consumer

products (types A9, A13 and A14) is shown in Figure 4. Each lab has developed an operational plan of

work, adapted to their emission test chamber dimensions (with respect to the EPHECT umbrella

start-up condition on a sample collection limit smaller than 80% of the intake flow) and their

chamber facilities to collect samples.


26

Figure 3 Operational plan of work for spray consumer product testing at VITO

6.3 Reporting data for BUMAC imputation

Data generated in WP6 are not only used in WP7 for details exposure and health risk assessment. All

emission data, generated in this work package, are included in BUMAC. Therefore, the emission data

and experimental details are collected in datasheets, per product class tested. An example of the

datasheet is shown in Table 16.


27

Table 16 EPHECT work division sheet

Complexity of the analysis

QA/QC EPHECT key, gap and emerging pollutants

# samples per

product

NCRWE (1) VITO (2) UOWM (3) IDMEC (4)

Sampling Analysis Sampling Analysis Sampling Analysis Sampling Analysis

Basic Terpenoids:

limonene 4 (1) (1) (2) (2) (3) (3) (4) (4)

level 1 duplicate collection - max 20% deviation

alpha-pinene 4 (1) (1) (2) (2) (3) (3) (4) (4)

level 2 (C)RM (external) geraniol 4 (1) (1) (2) (2) (3) (3) (4) (4)

a-terpineol 4 (1) (1) (2) (2) (3) (3) (4) (4)

linalool 4 (1) (1) (2) (2) (3) (3) (4) (4)

Aldehydes:

formaldehyde 4 (1) (1) (2) (2) (3) (3) (4) (4)

acrolein 4 (1) (1) (2) (2) (3) (3) (4) (4)

glutaraldehyde 4 (1) (1) (2) (2) (3) (3) (4) (4)

acetaldehyde 4 (1) (1) (2) (2) (3) (3) (4) (4)

Aromates:

benzene 4 (1) (1) (2) (2) (3) (3) (4) (4)

toluene 4 (1) (1) (2) (2) (3) (3) (4) (4)

xylenes 4 (1) (1) (2) (2) (3) (3) (4) (4)

styrene 4 (1) (1) (2) (2) (3) (3) (4) (4)

PAHs: naphthalene 4 (1) (1) (2) (2) (3) (3) (4) (4)


28

Complexity of the analysis

QA/QC EPHECT key, gap and emerging pollutants

# samples per product

NCRWE (1) VITO (2)

UOWM (3) IDMEC (4)


Primary aerosols (analysed in real time by FMPS,

SMPS, dust monitors etc.)

(1) (1) (2) (2) (3) (3) (4) (4)

Secondary aerosols (filter sampling)

(1) (1) (2) (2) (3) (3) (4) (4)

Complex 1 lab for analysis Disinfectants: chloroamines 1 (@peak) (1) (2) (2) (2) (3) (2) (4) (2) level 1 (C)RM if available

(external) hypochlorite 1(@peak) (1) (2) (2) (2) (3) (2) (4) (2)

(H2O2) 1

Micl. compounds (not respiratory health)

(PCBs) 1

(PCDDs) 1

on PDMS tenax Phthalates benz-a-pyrene

1 (1) (1) identification

(2) quantification

(2) (2) (3) (2) (4) (2)

Isothiazolinones 1

CO - - - - - - (4) (4)

CRM NO2 - - - - - - (4) (4)

Ammonia (1) (4) (2) (4) (3) (4) (4) (4)


(1) (1) (2) (1) (3) (1) (4) (1)

Quat. ammonium chlorides (QUATs) (1) (1) (2) (1) (3) (1) (4) (1)

VOC Identification&analysis

1 (3/4 samples)

(1) (1) (2) (1) (3) (1) (4) (1)


29


30

Figure 4 Datasheet for WP6 emission data

References

31

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Appendix 1 Literature compilation Appendix 2 Complete list of key and emerging compounds

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