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TEST METHOD

D49 3027 / - - B

VOLATILE ORGANIC COMPONENTS ANALYSIS

PRODUCED BY CABIN PARTS

Renault Automobiles Standardization


RE-DS / Department 67210
Standards and Specifications Section
RENAULT D49 3027 / - - B

This document must be treated as a whole; its elements must not be separated.

© RENAULT 2011.
Reproduction is not permitted without the approval of the publishing department.
Communication forbidden without prior approval from Renault.

FIRST ISSUE

September 2005 --- This issue originates from project NC 2002 0512 / - - -.

MODIFICATION

May 2006 - - A Update.


This issue originates from project NC 2006 0287 / - - -.
May 2011 - - B Update
This issue originates from project NC 2011 0367 / - - -.

REFERENCE DOCUMENTS

Recommendation : VDA 276

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CONTENTS

Page

1. PURPOSE AND SCOPE 5

2. PRINCIPLE 5

3. EQUIPMENT 5

3.1. Instrumentation 5

3.1.1. Injection and dynamic pre-concentration system (Turbomatrix from Perkin Elmer,
for example) 5

3.1.2. Gas chromatography (Clarus 500 from Perkin Elmer, for example) 5

3.1.3. Mass spectrometer (Clarus MS Gold from Perkin Elmer, for example) 5

3.1.4. Another possible detector type: FID 5

3.1.5. Test chamber: Weiss VCE 1000 climatic chamber 5

3.2. Equipment 6

3.2.1. Sampling pumps (Smart Automatic Sampling System (SASS) from TERA, for
example) 6

3.2.2. Scales accurate to 1/10 of a milligram (Mettler AE 240, for example) 6

3.2.3. 50 ml gauged phials (class A) 6

3.2.4. 0.5 µl, 1µl and 5µl syringe 6

3.2.5. Swagelock ¼" Screws 6

3.2.6. Freezer which can reach a temperature of -18°C 6

3.2.7. Tubes for thermal desorption in steel containing Tenax TA (SUPELCO Ref: 25055
for example) 6

3.2.8. Calibrated flow meter 6

3.2.9. Oven for cleaning tubes of adsorbent (RTA from TERA Environment, for example) 6

3.2.10. Reference sample injection system 6

3.2.11. Equipment for the storage of test pieces before analysis 6

3.3. CONSUMABLES 6

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3.3.1. 99.5% minimum pure nitrogen (sweeping out gas) 6

3.3.2. 99.9% pure toluene 6

3.3.3. Analysis quality methanol 6

3.3.4. Exacanal tubing or other non-pollutant flexible materials. 6

4. SETTING UP OF TEST 6

4.1. storage of test pieces before analysis 6

4.2. preparation of tubes 7

4.3. preparing the pumps 7

5. PROCEDURE 7

5.1. launching the VDA 276 test and sampling 7

5.2. STORAGE of sampling tubes 8

5.3. Analysis of the test pieces by TDS/CG/SM 8

5.3.1. Conditions for analysis 8

5.3.2. Calibration 10

5.3.3. Analysis of the tubes 11

6. USE OF THE RESULTS 11

6.1. Calibration line 12

6.2. individual VOC dosage (pure compounds) 12

6.2.1. Qualitative analysis 12

6.2.2. Quantitative analysis 12

6.3. Total VOC dosage 13

7. Test report 13

APPENDIX 1 VDA 276 RECOMMENDATION 15

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1. PURPOSE AND SCOPE

The aim of this method is to identify and quantify in toluene equivalent the main volatile organic
compounds (VOC) released by parts or cabin functions due to the effect of temperature and climatic
conditions. The test relates to cabin parts or functions which are subject to incoming air flow.

2. PRINCIPLE
3
The VDA 276 recommendation describes a method for the assessment, using a 1m test chamber, of
VOCs produced by the functions or sub-assemblies of the passenger vehicle of a motor vehicle.

The VOCs present in the test chamber atmosphere are sampled in a steel tube containing an
adsorbent (TENAX: 2.6-diphenyl-phenylene based porous polymer). They are thermally desorbed
(TDS) and then separated by chromatography in the gaseous phase (CG). Detection is done by mass
spectrometry (SM) or by a flame ionization detector (FID).

The quantification of the total and individual VOCs is done by toluene equivalent using external
calibration.

3. EQUIPMENT

3.1. INSTRUMENTATION

3.1.1. Injection and dynamic pre-concentration system (Turbomatrix from Perkin Elmer, for
example)

3.1.2. Gas chromatography (Clarus 500 from Perkin Elmer, for example)

Helium 5.0. may be used as the carrier gas.

3.1.3. Mass spectrometer (Clarus MS Gold from Perkin Elmer, for example)

The software used to process the spectrums (Turbomass, for example) can be complemented with
one or several spectrum libraries (Wiley or NIST, for example).

3.1.4. Another possible detector type: FID

3.1.5. Test chamber: Weiss VCE 1000 climatic chamber

The test chamber must be air tight, chemically inert and have a recirculation facility to ensure the
circulation of air and the homogeneity of the mixture. Furthermore, the chamber must be capable of
accurately regulating temperature and relative humidity.

In order to define and quantify the VOCs produced by the test piece, the test chamber must be
equipped with an air tapping enabling a sample to be taken from the atmosphere during the VDA 276
cycle.

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3.2. EQUIPMENT

3.2.1. Sampling pumps (Smart Automatic Sampling System (SASS) from TERA, for example)

3.2.2. Scales accurate to 1/10 of a milligram (Mettler AE 240, for example)

3.2.3. 50 ml gauged phials (class A)

3.2.4. 0.5 µl, 1µl and 5µl syringe

3.2.5. Swagelock ¼" Screws

3.2.6. Freezer which can reach a temperature of -18°C

3.2.7. Tubes for thermal desorption in steel containing Tenax TA (SUPELCO Ref: 25055 for
example)

3.2.8. Calibrated flow meter

3.2.9. Oven for cleaning tubes of adsorbent (RTA from TERA Environment, for example)

3.2.10. Reference sample injection system

3.2.11. Equipment for the storage of test pieces before analysis

Choose chemically inert, watertight, odourless packaging, either household foil, cling film or heat-
sealed bags (made by VALSEM –BP 30 – 6, lieu dit ruelle Compiègne – 60190 LACHELLE, reference
Valsem S 156 type H, for example).

3.3. CONSUMABLES

3.3.1. 99.5% minimum pure nitrogen (sweeping out gas)

3.3.2. 99.9% pure toluene

3.3.3. Analysis quality methanol

3.3.4. Exacanal tubing or other non-pollutant flexible materials.

4. SETTING UP OF TEST

4.1. STORAGE OF TEST PIECES BEFORE ANALYSIS

The samples must be packaged 7 days after production. Then in order to reduce the risk of
contamination during transportation, the samples must be packaged. Use different packaging for each
sample reference. An example of a sample reference is cited in paragraph 3.2.11.

The samples must be stored, before and after packaging, in a place where they do not risk being
contaminated. The maximum storage temperature recommended is 20°C +/- 3°C and the average
recommended humidity rate is 50% ± 10% relative humidity.

The time between the date of packaging and the date of analysis of the part (VDA 276 test) must not
exceed 28 days.

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4.2. PREPARATION OF TUBES

Cleaning the tubes of adsorbent is essential before each series of tests.

This is done by placing the tubes of adsorbent (3.2.7) in the RTA oven (3.2.9.) at 300 °C ± 5 °C and
sweeping out with a neutral gas (3.3.1.) for at least 1 hour. After they return to ambient temperature
(always under gas flow), the tubes are taken out of the oven and immediately plugged with the
Swagelock screws (3.2.5.)

To verify the cleanliness of the adsorbent, perform an analysis using TDS/CG/SM. The adsorbent is
considered "clean" when no residual peaks appear on the chromatogram.

The tubes are then stored at an ambient temperature (2 weeks maximum).

Note: cleaning the tubes can also be done with the thermal desorber (3.1.1), on "tube heating" mode.

4.3. PREPARING THE PUMPS

Make a watertight connection between a tube of adsorbent and the pump (3.2.1) (for SASS, insert the
tube fully into the sample ramp).

Set the flow rate to 50ml/min.

Check the flow with a calibrated flow meter (3.2.8).

Then make a watertight connection between the tube + pump and the test chamber branching pipe
(3.1.5) using exacanal or Teflon tubing (3.3.4)

5. PROCEDURE

5.1. LAUNCHING THE VDA 276 TEST AND SAMPLING

The VDA 276 test procedure is described in appendix 1 of this document.

Follow the instructions below:

- launch the VDA 276 pre-conditioning cycle,

- once the temperature, humidity and air replacement rate has been conditioned within the
chamber, remove the part from its packaging and place it into the chamber ensuring that it does
not touch the chamber walls and start the VDA 276 test,

- wait 2½ hours after the start of the VDA 276 test, and then start taking samples from the test
chamber atmosphere. Each sample must be duplicated (simultaneous or successive samples).

As the concentrations of VOC produced by the sample is not known, at least two samples need to
be taken with different sampling volumes.

The recommended sampling volumes are as follows:

- 0.5 L of air (flow rate: 50ml/min for 10 minutes)

- 1.5 L of air (flow rate: 50ml/min for 30 minutes)

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The VOC sampling phase in tubes containing Tenax can be illustrated as follows:

Start pre- Introduce part + heating 65°C


conditioning End of the
70°C cycle
-1h 0 +0h30 +1h30 +2h30 +3h30 +4h30

50ml/min
VOC sample Tenax tube 1 Tenax tube 3
and 2 and 4
10min 30min

VDA 276 Heating cycle

- once the sampling is finished, plug the sample tubes with the Swagelock screws (3.2.5).

- Note the value of the air volume sampled for each tube.

5.2. STORAGE OF SAMPLING TUBES

The sample tubes must be stored in the freezer (3.2.6.) at -18°C until they are analyzed. The analysis
must be done as quickly as possible, within a maximum time limit of 2 weeks.

5.3. ANALYSIS OF THE TEST PIECES BY TDS/CG/SM

5.3.1. Conditions for analysis

The analytic conditions (valid for a Perkin Elmer apparatus) are summarized in the table below
(conditions taken from the VDA 278 recommendation):

VOC analysis Calibration

T Valve temperature 280°C

H Tube temperature 280°

E Tube desorption 30 min 15min


time
R (2-stage desorption procedure) (2-stage desorption
procedure)
M
Purge tube 1 min
A
Inlet split flow rate 40 ml/min
L
Outlet split flow 40 ml/min
rate

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D Desorption flow 40 ml/min


rate
E
Column head 14 psi
S pressure
25 psi when MSvent is used
O
Trap phase Air monitoring (carbopack C and Carobosieve III)
R
Cryogenics - 30°C
P temperature
T Trap heating 300°C
temperature
I
Trap heating ramp 40°C/s
O
Trap heating time 20 min
N
Carrier gas Helium 5.0

Capillary column non-polar capillary column stationary phase: 5% phenyl-methyl


siloxane)

(HP Ultra 2 50m column X 0.32mm X 0.52µm, for example)


G
GC temperature 40°C for 2min
C programming
3°C/min. up to 92°C

5°C/min. up to 160°C

10°C/min. up to 280°C

280°C for 10 min

Transfer line T° 280°C

scan 29 to 520 uma

M Inter scan 0.4 s

S Inter scan time 0.1 s

MS threshold 100

F FID temperature 320°C

I Flame O2: 450 ml/min

D H2: 45 ml/min

Attenuation Attenuation 6

Range: 1

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The qualitative and semi-quantitative analysis of VOCs is done on the complete chromatogram (TIC)
obtained by mass spectrometry.

(The semi-quantitative analysis can also be done with the chromatogram obtained with the FID
detector).

It is advisable to complete a blank analysis of the system before each series and between each
sample reference.

The calibration of the mass spectrometer must be verified before each series (the calibration ratio
must be printed and filed with the rest of the analyses).

5.3.2. Calibration

An external calibration is performed by injecting a known quantity of toluene under the same analysis
conditions as the sample (adsorption on Tenax tube, then thermal desorption).

The calibration must be done with a molecule with an analytic response close to the response from the
compounds sought (example: the response from toluene is close to that of BTXES: Benzene, Toluene,
Ethyl benzene, Xylene, Styrene). In our case, toluene is used to quantify all of the molecules present
in the sample. An estimate is made since the response from the molecules present can be different
from the response from the toluene.

Electronic storage of the calibration line must be carried out.

5.3.2.1. Preparation of standard solutions:

The solutions must be prepared in compliance with laboratory protection rules inherently linked to the
use of chemical products (protective eyewear, gloves and overalls must be worn and fume hood
used).

Prepare 3 standard solutions as follows:

S1: in a 50ml (3.2.3.) graduated flask, weigh 5mg of toluene using precision scales (3.2.2). Complete
with methanol up to the gauge line and homogenize.(3.3.3)

S2: in a 50ml graduated flask, weigh 25mg of toluene using precision scales. Complete with methanol
up to the gauge line and homogenize.

S3: in a 50ml graduated flask, weigh 250mg of toluene using precision scales. Complete with
methanol up to the gauge line and homogenize.

The solutions must be stored in the refrigerator (between 4 and 10°C). They are usable for 3 months.

5.3.2.2. Preparation of the standard tubes

The standard solutions are injected in tubes containing Tenax TA (3.2.7) using the system described
below:

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Standard
solution

flow meter
helium

Gas meter

helium
TENAX Tube

The thermal desorption tube containing the Tenax is connected to an injection system that makes it
possible to guarantee a controlled flow of helium (approx. 50ml/min.) through the tube while the
standard solution is flowing.

At the end of the tube, a gas meter measures the volume of gas that has passed through the tube (2.5
to 3L).

At the end of each injection, the tubes must be quickly closed.

Complete at least five calibration points with three repetitions for each point.

The volumes for each solution to inject into the tubes of adsorbent are summarized in the table below:

Solution Volume to inject (µl) Mass of toluene injected (µg)


S1 0.5 0.05
S1 1 0.1
S2 1 0.5
S2 2 1
S3 1 5

5.3.3. Analysis of the tubes

The tubes (standards and samples) are installed in the thermal desorber carousel. Each tube is then
heated to 280°C by the thermal desorber. The substa nces trapped by the Tenax TA are then released
and sent via a flow of helium to the cold trap cooled to -30°C. The cold trap is then heated (flash
heating to 300°C) in a few seconds. The VOCs are de sorbed in the carrier gas flow and led to the top
of the capillary column.

The VOCs are then separated by the capillary column and detected by the mass spectrometer.

Note: The detection can also be done with a flame ionization detector.

6. USE OF THE RESULTS

The results are expressed in toluene-equivalent.

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6.1. CALIBRATION LINE

Include the surfaces of each peak of toluene and create the calibration line for which the equation is
as follows:

Stoluene = F.Mtoluene
With Stoluene: Surface of the toluene peak

Mtoluene: mass of toluene injected (µg)

F: slope of the calibration line

6.2. INDIVIDUAL VOC DOSAGE (PURE COMPOUNDS)

6.2.1. Qualitative analysis

The identification of peaks present on the chromatogram is done by mass spectrometry by comparing
the mass spectrum for the compound observed to the mass spectrums referenced in the libraries
(Wiley or NIST, for example).

The characterization of the molecules analyzed must include at least:

- the retention time

- its name (if the molecule could not be identified, indicate its chemical family (e.g. amine, alkane,
etc.) or the fragments characteristic of this molecule)

- the CAS number

- indicate possible co-elutions

6.2.2. Quantitative analysis

Verify the purity of the peaks obtained on the chromatogram. Include the peaks and calculate the
masses for pure compounds in toluene equivalent by using the following ratio:

SVOC
mVOC =
F
Where:

mVOC: individual VOC mass in toluene equivalent (µg),

SVOC: individual VOC peak area,

F: slope of the calibration line completed with the toluene,

Then calculate the individual VOC concentration in the atmosphere sampled:

CVOC= mVOC
V sampled air

Where:
3
CVOC: individual VOC concentration in toluene equivalent (µg/m ),

mVOC: individual VOC mass in toluene equivalent (µg),


3
Vsampled air : volume of sampled air (m ).

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6.3. TOTAL VOC DOSAGE

Include the surface peaks eluting between hexane (n-C6) and hexadecane (n-C16).

Calculate the equivalent toluene mass by using the following ratio:

Stotal VOC
mtotal VOC = F

Where:

MtotaL VOC: Total VOC mass (VOC eluting nC6 and nC16) in toluene equivalent (µg),

Stotal VOC: area of all of the VOC peaks eluting between nC6 and nC16),

F: slope of the calibration line completed with the toluene,

Then calculate the total VOC concentration released by the test piece:

mtotal VOC
Ctotal VOC =
Vsampled air

Where:

CtotaL VOC: total VOC concentration in toluene equivalent (µg/m3),

MtotaL VOC: total VOC mass in toluene equivalent (µg),

Vsampled air: volume of air sampled from the cabin (m3).

For the same sample, the deviations in total VOC concentration obtained from the 4 samples must not
exceed 15%.

If a deviation> 15% is observed, take the following action:

Results observed Possible cause Procedure to be followed

Detector saturation for 1.5 L Only take results obtained from


samples 0.5 L samples into consideration

Drilling of tubes (1.5 L samples): Only take results obtained from


the quantity of VOC samples is 0.5 L samples into consideration
too high or the sampling lasted too
-results obtained with similar 1.5 L long
samples
Insufficient detector sensitivity of Only take results obtained from
-results obtained with similar 0.5 L 0.5 L samples (quantity of VOC 1.5 L samples into consideration
samples sampled too low)
Changes in the nature and/or Indicate the results for each
- however variation in results
quantity of VOC produced by the volume of air sampled (1 result for
depending on volume of air
part over time 0.5 L samples and 1 result for
sampled
1.5L samples)

1 Anomalous result Analytical problem Delete the anomalous result

Changes in the nature and/or Only take the highest C total


quantity of VOC produced by the VOCresult
into account.

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part over time


No repeatability of results To be specified in the test report

Analytical problem Restart the test

7. TEST REPORT

The test report must include:

- the chromatogram of the tested sample (sample of which the total CVOC is the highest)

- a table containing the list of substances observed and their semi-quantifications (sample of which
the total CVOC is the highest)

- the calibration line

- reference of this method

- reference of the tested sample (name, reference no., supplier, composition, mass, colour,
production date, date of packaging)

- the atmospheric sampling date from the climatic chamber

- the TDS/GC/MS analysis date

- procedural details not specified in this test method, together with any incidents that might have
affected the results.

- the name and address of the laboratory that carried out the tests

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APPENDIX 1
VDA 276 RECOMMENDATION

Characterization of organic substances produced by components installed


3 VDA
inside the cabin of a motor vehicle using a test chamber with a volume of 1 m .
276

Determination of organic substances as emitted from


automotive interior products using a 1 m3 test cabinet.

Foreword

These test methods enable the quantity of chemical organic substances produced, in the specified
conditions, by components located inside the cabin of a motor vehicle to be measured.

The results obtained using these methods are unsuitable for:

- making conclusive estimates relating to any kind of health and hygiene assessment of these
substances,

- being used, in any form, as a basis for evaluating the concentrations which may be encountered
in the cabin of a vehicle at a complete stop, on the move or in a similar state.

The two following sections are included in these recommendations:


1)
Part 1: Standard emissions tests

Part 2: Characterization of formaldehyde, ammonia and carbolic acid emissions in


1
accordance with the balancing concentration method. moulded parts used within
2
the cabin of motor vehicles )

1)
by:
"Institute for the study and testing of Environmental protection association TÜV
plastic materials (IKP)" Nord mbh
Pfaffenwaldrind 32 Institute of chemistry and environmental
D - 70569 Stuttgart protection
Grosse Bahnstrasse 31
22525 Hambourg
2)
by:
"Fraunhofer institute for wood research
Wilhem Klauditz Institute (WKI)
Bienroder Weg 54 E
38108 Brunswick

Note from translator: error in German text

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APPENDIX 1 (continued)

Characterization of organic substances produced by components installed


3 VDA
inside the cabin of a motor vehicle using a test chamber with a volume of 1 m .
Part 1: Standard emissions tests
276-1

Determination of organic substances as emitted from


3
automotive interior products using a 1 m test cabinet.
Part 1: Standard-Emission test

Contents

1. INTRODUCTION 17
2. REFERENCES TO OTHER STANDARDS; LITERATURE 17
3. DEFINITIONS 18
4. SYMBOLS AND UNITS 19
5. TEST METHOD PRINCIPLE 19
6. EMISSIONS TEST BENCH 19
6.1. TEST CHAMBER 20
6.2. TEMPERATURE BALANCING IN THE TEST CHAMBER 21
6.3. AIR HUMIDIFICATION 21
6.4. FRESH AIR SUPPLY 21
6.5. MEASURING THE CUMULATED CONCENTRATION OF HYDROCARBON
COMPOUNDS 21
6.6. COOLING OF THE ATMOSPHERE FOR FOGGING 22
7. GENERAL QUALITY ASSURANCE MEASURES 22
8. TEST PIECE 24
8.1. RECEIPT OF TEST PIECE 24
8.2. TEST PIECE PACKAGING, TRANSPORT AND STORAGE 25
9. PERFORMING A STANDARD EMISSIONS TEST 25
9.1. CLEANING 25
9.2. TEST 26
10. CALCULATION AND PRESENTATION OF TEST RESULTS 29
11. TEST REPORT 30

Appendix 1: Laboratory report

Appendix 2: Emissions tests inspection list (example)

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APPENDIX 1 (continued)

1. INTRODUCTION

This VDA recommendation describes a method enabling the characterization, using a test chamber,
the volatile organic substances produced by the sub-assemblies or construction elements used within
the cabin of motor vehicles. On the one hand, it describes the characteristics and the general quality
3
assurance measures to be taken for a chamber with a volume of 1m used for the standard emissions
tests carried out on products located in the cabins of motor vehicles, and on the other hand it
describes the overall test procedure, from the provision of the test pieces to taking samples from the
test chamber.

For successive chemical analysis methods, we recommend the application of methods that have been
1)
drawn up in the context of the FAT/BMBF project, by an approved body for the technical inspection
of safety standards, "Technischer Überwachungsverein" (TÜV), North Germany division in Hamburg,
and by the Institute for the study and testing of plastic materials “Institut für Kunststoffprüfung und
Kunststoffkunde” (IKP) in Stuttgart. Where different analysis methods have been applied, it will be
necessary to demonstrate that the values obtained according to these methods are equivalent and to
document in the test report, the variations in relation to the recommended methods.

2. REFERENCES TO OTHER STANDARDS; LITERATURE

This paragraph includes the standards and directives to which this document refers to in the relevant
passages. If the quotation refers to a document without indicating its date or edition, the most recent
version of the document is applicable. The references to standards concerning specific editions or
versions are also valid when more recent versions of these documents are available and where
appropriate, should be integrated into a revised version of this document.

- European Collaborative Action (ECA) "Indoor Air Quality And Its Impact on Man" Report No. 8
"Guideline for the Characterization of Volatile Organic Compounds Emitted from Indoor Materials
and Products Using Small Test Chambers" (European Collaborative Action "Indoor Air Quality
And Its Impact on Man", report no. 8 "Recommendations relating to the characterization of volatile
organic substances produced indoors by materials and products using small test chambers").

- European Collaborative Action (ECA) "Indoor Air Quality And Its Impact on Man" Report No. 18
"Evaluation of VOC Emissions from Building Products" (European Collaborative action “Indoor Air
quality and its impact on man”, report no.18 “Evaluation of volatile organic substances produced
by construction materials”).

- DIN EN 45001, General criteria for the use of test laboratories.

- DIN EN ISO 9001, Quality management systems – quality assurance model/Quality management
of design/development, production, assembly and maintenance.

- DIN 50011-11, Climates and their technical applications; facilities for climatic tests; terminology
and general requirements.

- DIN 5011-13, Climates and their technical applications; facilities for climatic tests; Climatic
properties: Air humidity and temperature.

-----------------
1)
Final report: "Development and testing of standard measurement methods enabling the assessment of air
pollution contribution by motor vehicle components through the emission of organic substances inside the
cabin" (BMBF, Fkz:. 07INR27A8 and 07INR27B0);
- Volume III (document available from: TÜV Nord eV, Grosse Bahnstrasse 31, 22525 Hambourg)
- Volume V (document available from: IKP, Pfaffenwaldring 32, 70569 Stuttgart)

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APPENDIX 1 (continued)

3. DEFINITIONS

The following characterizations are applicable within the context of this present VDA recommendation:

Air evacuation flow: Air flow leaving the test chamber through a previously defined opening.

Loading: Relationship between the volume, surface, length or the mass of the test piece and the
volume of the test chamber.

Emissions: Organic substances released by the test piece in the specified test conditions.

Emission rate: Rate of organic substances released by the test piece during a specified time unit; the
characterization is carried out either in relation to the mass, volume, surface or length or as an
absolute value for each test piece.

Fogging: Precipitation of generally organic, condensable, volatile substances.

Air replacement rate: Incoming air flow and test chamber volume quotient per time unit.

Air velocity: Average speed of air flow caused by the mixing of air inside the test chamber; it is
measured at the centre of the test chamber.

Air sample: Sampling of a volume previously defined and representative of the atmosphere inside of
the test chamber.

Ideal mixture: A substance introduced to a zone which has an ideal mix is divided immediately and
completely to create a homogenous mix in the whole zone.

Condensation sample: Enrichment of condensable substances (fogging) from the test chamber
atmosphere on a cooled manifold device.

Concentration in the test chamber: Concentration defined by the chemical/analytical/physical values


of one or more chemical substances found in a gaseous sample taken from a place representative of
the test chamber.

Test piece surface: Surface formed by the contours of the test piece from which organic substances
may also be produced.

Test chamber: Chamber which may be sealed in an airtight manner to define the emission of organic
volatile substances in pre-defined climatic conditions.

Test chamber volume: Actual volume of the test chamber minus the volume of all technical facilities
and devices located inside the test chamber.

Mass comparison: Relationship between the mass percentage of a defined substance in the
outgoing airflow and the loss of mass of this same substance in the test chamber over the same
period of time.

Incoming air flow: All of the gaseous volumic flows introduced to the test chamber per time unit.

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APPENDIX 1 (continued)

4. SYMBOLS AND UNITS


3
C [µg/m ] Concentration of a substance in the test chamber
5
(for 1.01310 Pa and 293K)
R [µg/h] Emission rate
2
RA [µg/m h] Emission rate in relation to the test piece surface
3
RV [µg/m h] Emission rate in relation to the test piece volume
Rm [µg/kgh] Emission rate in relation to the test piece mass
n Air replacement rate
-1)
defined as air replacement per hour (h
2 3
LA [m /m ] Loading by surface
3 3
LV [m /m ] Loading by volume
3
Lm [kg/m ] Loading by mass

5. TEST METHOD PRINCIPLE


3
The test piece is placed in the test chamber with a volume of 1m where the air mixture is almost ideal;
It is stored in this chamber in pre-defined conditions regarding temperature, air humidity and the air
replacement rate. The organic substances produced by the test piece enrich the atmosphere of the
test chamber from which they are then evacuated by a current of air.

At specific, pre-defined moments, samples of air or condensation are taken which enable us to define,
using qualitative or quantitative chemical analysis methods; the concentration of gaseous substances
in the air of the test chamber.

6. EMISSIONS TEST BENCH

A test bench used to define gaseous emissions includes the following functional elements:

- Test chamber - Fresh air supply system

- Air mixing facility - Control and


regulation system

- Temperature balancing thermostat - Overall CH Monitor


in the test chamber

- Air humidifier - Fogging cooling system

The design type, availability, combination and technical design of these different functional elements
may be freely selected. The minimum requirements to be complied with are defined in the following
chapters. In addition, it is necessary to demonstrate (by systematic testing carried out in several
laboratories for example) that the test bench used enables comparable results for chemical
substances to be analyzed to be obtained.

Chapter 7 includes the specifications relating to ongoing quality assurance activities.

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APPENDIX 1 (continued)

6.1. TEST CHAMBER

The test chamber is an enclosure which can be closed in order to ensure air tightness. Inside the
chamber, there is an air mixing facility, as well as a support enabling the positioning of the test piece to
avoid contact with the chamber walls.

To control the air exchange and to take air samples, this chamber must be equipped with air intake
and output manifolds (diameter < 50mm), these two manifolds must be placed in diametrically
opposed places to prevent the air current from short circuiting.

Materials

The inner walls of the test chamber and the test piece support must be made of reinforced steel or
glass.

Any test pieces or elements situated inside the test chamber which cannot be made of reinforced steel
or glass, for technical reasons, must be made of materials with minimum emission and adsorption of
organic substances characteristics. All test piece surfaces and elements in contact with the test
chamber atmosphere, must under no circumstance exceed 5% of the test chamber wall surfaces.

Sealing

To prevent any non-controlled air exchange, the air leakage produced during testing from air
exchange at an overpressure of 1,000Pa must be lower than 1%0 of the volume of the test chamber
per minute or lower than 1% of the incoming air flow.

To prevent any external air intake, the emission tests must in all cases be carried out with a low
overpressure inside the chamber in relation to the atmospheric pressure of the laboratory and/or by an
excess volumic flow.

Air mixing

The almost ideal test chamber air mixing constitutes the basis of this test method. To obtain this
almost ideal mixture, the chamber must be equipped with an air mixing facility which also guarantees
these conditions for large and/or bulky samples.

The mixing needs to be adjusted in order to obtain an air flow speed greater than 0.1m/s at the centre
of the empty test chamber.

NOTE: Reports no.8 and 18 from the "Indoor Air Quality And Its Impact on Man" document of
European Collaborative Action (ECA) describe methods for the definition of the “sealing”
and “air mixing” parameters.

Cleaning

An appropriate cleaning method, by desorption at high temperatures for example, will ensure that the
test chamber is perfectly clean in between tests. Chapter 9.1. includes a detailed description for this
purpose.

The cleaning must be checked before each test by a test control.

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APPENDIX 1 (continued)

6.2. TEMPERATURE BALANCING IN THE TEST CHAMBER

Due to the close link between emissions and temperature, the temperature adjustment facility inside
the test chamber must comply with strict requirements.

As required, this facility must be able to cover a wide range of temperatures to comply with the test
conditions. The spatio-temporal temperature deviation must not exceed ± 0.5K.

6.3. AIR HUMIDIFICATION

The humidification of incoming air in the test chamber must be carried out ensuring that no vapour
and/or aerosols form. The humidification facility must enable a dew point temperature between 10.4°C
and 65°C in the incoming air flow, which correspond s to a relative humidity between 45% for 23°C and
5% for 65°C.

6.4. FRESH AIR SUPPLY

The tests involving air replacement, as well as air sampling require an ultra pure gas supply to the test
-1
chamber. To set the air replacement rate to 0.5 h , the volumic air flow must be able to be set to
6.67l/mn ± 0.35l/mn in the test conditions (65°C, a mbient atmospheric pressure), with an accuracy of ±
3%.

Before the test, the total concentrations of organic volatile hydrocarbon compounds in the incoming air
3 3
must not exceed 50µg/m in total or 5µg/m for an individual substance.

The fine dust rate must be reduced to 7µm using a particulate filter to prevent any adsorption of
analytes.

6.5. MEASURING THE CUMULATED CONCENTRATION OF HYDROCARBON COMPOUNDS

To ensure a qualitative evaluation of the nature of the cumulated concentration of hydrocarbon


compounds in the test chamber during a test cycle, an online analyzer based on a flame ionization
detector (FID) will be used enabling the detection of a large range of organic substances in the form of
a cumulated signal. Calibration is performed with the aid of a test gas mixture including approximately
100ppmv propane of synthetic air. The zero test gas to be used for this purpose is nitrogen with a
purity rate of 5.0.

The conversion formula which gives the mass concentration is described in chapter 10.

NOTE: The technical equipment specifications which define the quantitative properties based on a
cumulated FID signal are described in the section “Definition of the cumulated
concentration of hydrocarbon compounds using a flame ionization detector (FID)” which
will be drawn up at a later date.

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APPENDIX 1 (continued)

6.6. COOLING OF THE ATMOSPHERE FOR FOGGING

The qualitative characterization of condensable components of organic substances produced by a test


piece is undertaken with the aid of a cooling body positioned inside the test chamber. This cooling
body must be maintained at a temperature of 21°C ± 1°C for a temperature of 100°C inside the test
chamber. It should be noted that the use of a cooling body could affect the temperature balancing
within the test chamber. The materials to be used for this cooling body are specified in chapter 6.1.
Figure 1 schematically illustrates an example of test chamber emissions:

3
Figure 1: Diagram of a test chamber with a volume of 1 m
(for example: HCE/S 1000, manufactured by Vötsch Industrietechnik GmbH, Balingen)

7. GENERAL QUALITY ASSURANCE MEASURES

The integration of a large number of technical functions within this type of test bench carries a certain
risk of error, which therefore requires careful, regular checks of the overall system. Due to the fact that
these errors may have an immediate effect on the test results, the test bench must be integrated into a
quality assurance system that has been certified compliant or into a comparable ongoing monitoring
system.

The following chapters describe a number of important test methods for measuring the test
parameters.

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APPENDIX 1 (continued)

Sealing:

The air tightness of the test chamber is verified using an overpressure of 1,000Pa by measuring the
pressure drop after 2 hours. The pressure sensor sensitivity must be lower than 100Pa and its
accuracy must be ± 5%. The average leakage rate of this interval is calculated using the following
formula:

 o  1000 o
v  oo  = oo •  p1 − 1
 
 h  t [h]  p2 
 

where:
. specific leakage rate defined in relation to the volume of the test chamber, as a %0 per
V
hour
p1 Absolute pressure of the test chamber at the start of the test, in Pa
p2 Absolute pressure of the test chamber at the end of the test, in Pa
t duration of leakage rate characterization interval, in hrs

Alternative method:

The air tightness of the test chamber is defined using an overpressure of 1,000Pa by measuring the
half-value t1/2 of the pressure drop in the test chamber. The half-value is the time required to reduce
the overpressure in the test chamber to half its initial value. This enables the calculation of the specific
leakage rate according to the following formula:

 o  100 o
v  oo  = oo . ∆p . In2
 h  t [h] p t 1/ 2
 

where:
. specific leakage rate defined in relation to the volume of the test chamber, as a %0 per hour
V
∆p/p relative overpressure in relation to the ambient atmospheric pressure
t1/2 reduction interval of overpressure to half its initial value, in hrs.

According to the two methods described above, airtightness is measured for a temperature of 65 °C in
the test chamber.

Air velocity:

Air velocity is measured at the centre of the empty test chamber. The measuring device may be an
anemometer with a heated pin, film or plate.

Incoming air flow:

Due to its significant impact on the test results, the incoming air flow must be checked at regular
intervals. The volume of incoming air flow is measured to a pressure which corresponds approximately
to the ambient atmospheric pressure at the entrance of the test chamber. These measurements are
taken using a gas meter with an accuracy of ± 2% that has been certified for a range specified in
article 6.4 above. The minimum volume to be specified is 200 times greater than the accuracy of the
gas meter measurement. In this case, the incoming air flow can be calculated as the quotient of the
incoming volume and the measurement duration. To calculate the air replacement rate in test
conditions; the calculated incoming flow must be corrected in compliance with the law of perfect gases
based on the temperature and pressure values measured in the test chamber.

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APPENDIX 1 (continued)

Control values

The incoming air flow and ambient air control values as well as other sources of emissions in contact
with the test chamber atmosphere must be able to be defined by regular inspections.

For the control values required for quantitative analysis methods, proceed in accordance with the
specifications of these methods as previously described.

Carry out a semi-quantitative check of the control value using a “screening” process such as the
3
"tenax/thermal desorption" process for example, where sensibility is < 2µg/m for individual
substances.

It is preferable that the cumulated concentrations of organic volatile substances defined by this
3
process be lower than 50 µg/m , and the concentration of individual substances not exceeding 5
3
µg/m .

Temperature and humidity:

The temperature and relative humidity tolerances must be checked using a combined temperature and
humidity sensor with an accuracy of ± 0.5 K and/or ± 5%.

Air humidity can also be measured in the incoming air flow if the department has enough experience in
dealing with the possible effects of humidified incoming air condensation.

8. TEST PIECE

The conditions to which the test piece has been exposed before the volatile organic substances
emissions testing may have a considerable effect on the results, especially if the test involves
quantitative measurements. Consequently, it is necessary to standardize as much as possible the test
piece history until the test.

8.1. RECEIPT OF TEST PIECE

For standardized tests intended for the characterization of new part behaviour and emissions, the test
pieces must be analyzed in the state in which they came when the goods are received. It may be
necessary to take into account the adsorption of substances contained in the surrounding environment
and not included in the test piece at the origin. Consequently, it will be necessary to document the test
piece history as thoroughly as possible up until the moment that it is subject to testing.

If the test piece needs to be partially removed, disassembled or modified in any way whatsoever for
the test, these operations must also be documented. All clogging must be avoided during these
operations.

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APPENDIX 1 (continued)

8.2. TEST PIECE PACKAGING, TRANSPORT AND STORAGE

On receipt, the test piece must be packaged and remain in its packaging until the start of the tests so
that it cannot be contaminated by any chemical substances from the surroundings and to retain as
much as possible the test piece emission potential and/or to prevent any alteration of the material from
radiation (such as solar radiation for example).

NOTE: On receipt, the test piece should be packaged in a film made of a weldable composite
material and a layer of aluminium not only ensuring gas tightness and circulation but also
protection against damage risks during transportation (E.g. film made by Flöter, D-71735
Eberdingen-Nußdorf).

The test piece must be kept at a maximum temperature of 23°C during storage and transportation.

9. PERFORMING A STANDARD EMISSIONS TEST

This chapter describes the procedures, specifications and requirements of a standard emissions test
in the test chamber. This test provides a general overview of the test piece emissions spectrum in
harsher climatic conditions.

During the first conditioning phase, the test temperature is set to 65 °C and the relative humidity of
incoming air is approximately 5%. (corresponding to 45% relative humidity for 23°C). The air
-1
replacement rate is 0,4 h .
2
The test starts with the characterization of BTXE/S aromatic concentrations aldehydes and ketones,
as well as a GC-MS analysis. If necessary, the test may be supplemented by an additional air analysis
to determine the concentration of amines, glycolic ethers, phtalates or n-nitrosamines for example, in a
sampling window of 2.5 hours.

During the second conditioning phase, the temperature inside the test chamber is set to 100°C
(without humidification of incoming air); at the same time, the sampling of condensation resulting from
fogging is carried out on a cooling body set to 21°C.

The testing must be documented as a report (see example in appendix 1). The overall temperature,
humidity and concentration of organic components in the test chamber defined using the FID must be
documented throughout the whole test.

9.1. CLEANING

Before each test, all test chamber surfaces exposed to pollutants must be carefully cleaned. Any
possible background concentrations must be maintained at the lowest possible value so that they do
not affect the quality of the air analysis results.

Test chamber

Initially, all residual particles and substances from previously analyzed test pieces in the test chamber
shall be eliminated by mechanical cleaning (using an industrial vacuum cleaner for example). Any
condensation deposits produced from drying must be eliminated using steel wool or highly volatile
solvents.

2
benzene, toluene, xylene p-m, xylene o, ethyl benzene and styrene

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APPENDIX 1 (continued)

If the test chamber is cleaned by the heating and application of hot rinsing air, a process which
reaches all surfaces that have been in contact with the test chamber atmosphere should be used, the
rinsing air should be >200°C. This cleaning process will be complete after 10 air replacement cycles
from the moment that the specified temperature has been reached.

If the cleaning of the test chamber surfaces is carried out using alkaline cleaning products, this
washing must be supplemented by rinsing twice with demineralized water. To end, the test chamber
must be dried to the test temperature by applying a rinsing air current.

Other elements

All elements that have come into contact with the test chamber atmosphere and not directly involved in
its cleaning process must be subject to a separate cleaning process which is as effective as the
process described above.

NOTE: For all elements that have been installed inside the test chamber where thermal constraints
must not exceed 200°C (e.g. the seals), a washing s upplemented by a vacuum drying at
120°C for 2 to 3 hours is generally sufficient.

9.2. TEST

The actual test includes the period between the installation of test pieces into the test chamber and
their removal after having carried out all of the conditioning and sampling operations.

9.2.1. Prior conditioning

Condition the test chamber before installing the test piece, to a temperature of 70°C ± 1°C and relati ve
air humidity of 5 % ± 2 %.

9.2.2. Preparation

Inspect the whole test bench carefully before each test by verifying all of the required functions to
ensure that the test cycle is fully carried out and with a high level of safety. These checks carried out
through visual inspections and functional checks must include the verification of the fresh air
generation system, test chamber, climatic regulator, total CH monitor, the data recording system and
all other necessary accessories.

NOTE: Appendix 2 includes, as an example, a list of activities to be carried out before the test.

9.2.3. Test piece installation

The test piece must be placed on its support in the centre of the test chamber avoiding all contact with
the walls of the chamber. If the test is carried out on a batch of several test pieces, these must be
placed in a way that ensures optimum air mixing and prevents the movement of test pieces throughout
the test.

The test chamber must be closed immediately after the installation of test pieces.

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APPENDIX 1 (continued)

9.2.4. Conditioning phase

Immediately after the closing of the test chamber, the test must be initiated by the selection of an
automatic test programme or by manually setting the test conditions. The table below summarizes the
climatic parameters and the sampling operations for different phases of the test; figure 2 illustrates the
temperature curve and the sampling windows.

Standard emissions test performance table

Line Momen Nominal Air replacement Incoming air Operation


-1
t [h: temperature [h ] humidity [°C/%
1)
mn] [°C] H.R.]
Prior conditioning
1 70 Max 10.4/4.0
2 - 0:30 70 Max 10,4/4.0 Possibly: preparation in the
test chamber
Test
3 0:00 65 0.40 10.4/5.0 Conditioning phase 1
4 2:00 65 0.40 10.4/5.0 Start of air sampling
- BTXE/S aromatics
- aldehydes and ketones
- overall analysis
- if required: other samples
5 4:30 100 0.44 Conditioning phase 2
- start of fogging sampling
- end of fogging sampling
6 8:00 100 0.44
1) 5
Dew point temperature/relative humidity for 65/°C and 1.013 X 10 Pa

Additional notes

Line 1: The humidification of incoming air must start early to ensure the humidity required at the
start of the test in the test chamber
Line 2: Preparation of the test chamber must start early to ensure that pre-conditioning conditions
can be retrieved in the tolerance range the moment the test starts
Line 3: to ensure that the test temperature of 65 ± 0.5°C within the test chamber is reached again
after 30 minutes at the latest.
Line 4: The air sampling phase is designed so that there is enough time, after the specified air
sampling operations to take additional air samples in order to define the concentration of
amines, glycolic ethers, phtalates or n-nitrosamines for example.

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APPENDIX 1 (continued)

Figure 2 Standard emissions test cycle enabling the characterization of easily or not easily
volatile substances emitted from the test pieces using a test chamber with a volume
3
of 1 m

Air sampling

Air sampling should be carried out at pre-defined intervals. Consequently, the time and order of
sampling must be complied with during the sampling phase of several analytes.

The air sampling operating procedure is described in the corresponding air analysis method.

NOTE: The number of identical air samples is limited to a maximum of 6 per minute due to the air
replacement rate programme for the test (65°C, ambi ent atmospheric pressure).

Condensation sampling

Condensation sampling starts after the application of the cooling current at 21°C on the cooling body.
Due to the fact that the condensation sampling requires the opening of the test chamber, the test must
be terminated after this sampling.

The condensation sampling operational mode must be described in standard working instructions.

9.2.5. End of test

The emissions test is terminated by cutting the climatic regulation system and by opening the test
chamber. The test chamber must be immediately cleaned after the tests (see chapter 9.1).

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APPENDIX 1 (continued)

10. CALCULATION AND PRESENTATION OF TEST RESULTS

The tests provide quantitative values relating to the concentration of substances in the air of the test
chamber, enabling the calculation of emission rates and conclusions to be drawn relating to the
presence of chemical substances in the test chamber atmosphere.

The type, characterization and calculation of these test results are an integral part of a
chemical/analytic analysis method defined by standard work instructions that have been drawn up for
each test type. The reference volume to be used is the volume of the empty test chamber in a
3
standardized state ; this risks obtaining calculated concentration values which are lower than the
actual values.

Concentrations in the test chamber


3
Standard emissions test 65 °C Toluene (108-88-3) 10 µg/m
3)
Test Phase Substance (CAS no.) Concentration (µg/m

Qualitative detection of substances

Standard emissions test 65 °C Toluene (108-88-3) id entified


Test Phase Substance (CAS no.) Detection

Total carbon volumic concentration per FID


3
Standard emissions test 180 mn Total CH 10 mgCH/m
3)
Test Moment Substance Concentration (mgCH/m

Due to the fact that recording is ongoing, the concentration curve in the test chamber is generally
reproduced in the form of a concentration/time diagram. In this case, moment t= 0mn must be the
moment of closing of the test chamber after the installation of the test piece.

The total carbon concentration is calculated based on the volumic concentration of a FID according to
the following formula (calibration from a propane test gas mixture)

Molar propane mass


Volumic concentration = ⋅ Volume concentration
Molar propane volume

44.094 [Kg / Kmol ]


mCH[mg / Nm3 ]= ⋅C [ppmv ]
24.055 [m3 / Kmol ] FID
= 1.833. CFID[ppmv]

Emission rate

The mass concentration enables the calculation of the emission rate at the moment of sampling
(ignoring the end of test chamber accumulation):

Emission rate = volumic air flow X concentration


. .
mCH [mg / h]= V[m 3 / h ]⋅ C [mg / m 3 ]
CH

3 5
Standardized state: pressure of 1.013 x 10 PA, temperature of 293K for the relevant volume of gas

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APPENDIX 1 (continued)

Emission rate calculated in relation to the surface

Emission rateA = volumic air flow X concentration


test piece surface
.
.m V[m 3 / h ]⋅ C CH [mg / m 3 ]
[mg / m h ]=
A[m 2 ]
CH;A 2

Emission rate calculated in relation to the mass

Emission ratem = volumic air flow X concentration


test piece mass
.
. V [m3 / h ]⋅ CCH [mg / m3 ]
mCH;m [mg / kgh]=
m[kg]

11. TEST REPORT

Compliant with the specifications of standards DIN ISO 9001 and/or DIN EN 45001, the test report
must contain the following information:

- Name and address of the testing laboratory,

- Name and address of the customer,

- Date test piece received and type of packaging at delivery,

- Clear description(s) of the test piece so that it can be identified,

- Detailed description of the test piece,

- Manufacturing date of the test piece,

- Storage and air-conditioning between receiving the test piece and the start of the tests,

- Modifications carried out on the test piece (for example: disassembly, surface sealing, etc.),

- Test parameters: temperature, relative humidity and air replacement rate throughout the test,

- Moments, type and time of sampling,

- Analysis method and work instructions,

- Short description of the analysis method,

- Accuracy and dependability of the analysis method,

- Comparison of substance masses to be defined,

- Reference to the present standard,

- Variations in relation to the test method and particularities during the test,

- Date and signature.

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APPENDIX 1 (continued)

Appendix 1 Characterization of organic substances produced by components


Laboratory installed inside the cabin of a motor vehicle using a test chamber VDA
3
report with a volume of 1 m .
Page 1/1 Part 1: Standard emissions tests 276 - 1

Order number Test piece description

Manager, department Prior treatment,


see section B

Date Test air-conditioning,


see section C
Inspection tool – No.

A. Properties
Manufacturer Manufacturing date

B. Storage
Storage date Location
Temperature °C Packaging PE
Relative humidity % PE-Al
open

C. 3D Measurements
Start of measurements End
EPS Total CH

C1. Packaging
AUTOMATIC MANUAL

Programme No. Temperature °C


Dew point °C
Incoming air flow Nl/mn

C2. Sampling

Date/description of samples Categories of substances


1 2 3 4 5 6 7 8 9

D. Storage removal

Date test piece removed from storage Location

Date Signature

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APPENDIX 1 (continued)

Characterization of organic substances produced by components


installed inside the cabin of a motor vehicle using a test chamber
3
with a volume of 1 m . VDA
Part 1: Standard emissions tests 276 - 1

Appendix 2: Emissions tests inspection list (example)

Periodic check OK
Fresh air supply filter with carrier gas (handling, loading)
Air humidifier water tank sufficiently filled
Resistance to splitting (operation, sealing)
Visual inspection of the test chamber, air mixing
Functioning of fogging cooling system (air mixing, sealing, temperature)

Before test piece installation


Correct adjustment of incoming air flow (actual value)
Fogging cooling system connection, installation of plates
Installation and correct status of test chamber door sealing joints
Correct calibration and connection of total CH analyzer

At the start of the test


Correct plugging of all unnecessary openings within the test chamber
Activation of data recording system
Compliance of test parameters

VDA = Federation of automotive manufacturers

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APPENDIX 1 (continued)

Characterization of organic substances produced by components


installed inside the cabin of a motor vehicle using a test chamber
3
with a volume of 1 m . VDA
Part 2: Characterization of formaldehyde, ammonia and carbolic acid 276 - 2
emissions in accordance with the balancing concentration method.

Determination of organic substances as emitted from automotive


3
interior products using a 1 m test cabinet.
Part 2: Determination of the release of Formaldehyde, Ammonia
and Phenole – measurement by method of steady-state
concentration

1. AIM

These VDA test methods describe a test method enabling the characterization of formaldehyde,
ammonia and carbolic acid emissions from moulded parts installed within the cabin of a vehicle.

2. SCOPE

This method enables the measurement of moulded part emissions in extreme climatic conditions.

3. REFERENCE TO OTHER TEST METHODS

ENV 717-1 Components made of wood - Definition of formaldehyde emission - Part 1: characterization
of formaldehyde emission using the test chamber method

4. PRINCIPLE

To determine the emission rate of pollutants, such as formaldehyde, ammonia or carbolic acids, from
moulded parts made of fabric or wood fibres used within the context of automotive manufacturing, a
3
test method referred to as “method for a 1m test chamber” is applied which takes into account the
least favourable conditions which may be encountered within the cabin of a motor vehicle.

To simulate the exposure conditions of the cabin of a motor vehicle to solar radiation, the temperature
of the test chamber must be maintained to 65°C. Fur thermore, the “cabin loading/air replacement rate”
ratio has been defined as value 4 based on preliminary tests relating to the characterization of the air
replacement rates for various types of vehicles, with the ventilation valves closed taking into account
the generally high proportion of fabric coatings within the cabin. The relative air humidity is
approximately 11%, which corresponds to the vapour saturation of the air at ambient temperature,
which is then heated to 65°C in the test chamber. T he test piece is placed so that it is exposed in the
best possible way to the air flow.

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APPENDIX 1 (continued)

5. SAMPLING

A test piece with a total surface area of 2m² in relation to all of the main surfaces should be prepared.
For large format moulded parts, the test piece shall be taken from a place representative of the part.
Directly after manufacture or after it has been removed from its packaging for transportation, it should
be protected by airtight packaging such as polyethylene film, and stored at a maximum temperature of
25°C maximum until testing. To prevent the formatio n of condensation on its surface, the test piece
must be kept at a temperature > 20°C until it is pl aced in the test chamber.

6. TEST METHOD

6.1. TEST PARAMETERS


3
The test piece is placed in a test chamber with a total volume of 1m in the following climatic
conditions:

- Test temperature (65 ± 1) °C,

- Relative humidity (11 ± 5) %,


-1
- Air replacement rate 0,5 h ,
2 3
- Test chamber loading rate 2 m /m .*

* A reduced loading rate is also possible provided that the air replacement rate is also reduced to
ensure the same ratio between the chamber loading rate and the air replacement rate, i.e. coefficient
4.

6.2. DESCRIPTION OF A TEST CHAMBER WITH A VOLUME OF 1 M3

6.2.1. Glass test chamber (example)

The internal dimensions of this chamber are 1.00 m. X 0.80 m. X 1.25 m (figure 1). The outer walls of
the test chamber are made of glass with a thickness of 8mm. The temperature is set using a heating
thermostat made of reinforced steel and the air mixing is carried out using two ventilators connected to
the thermostat.

The introduction of water-saturated air at 23 °C in to the test chamber which has been heated to 65 °C
leads to a reduction of the relative humidity rate to (11 ± 5) %.

6.2.2. Reinforced steel chamber

This type of test chamber includes the conditioning chamber and the actual test chamber (1.78 m. X
0.75 m. X 0.75 m). The test chamber is made up of a welded inner panel which is gas tight with
smooth surfaces made of reinforced steel with low surface roughness. Air humidity is adjusted in the
incoming air flow according to the dew point principle. See chapter 6 of Section 1 of this VDA
recommendation for a detailed description of a reinforced steel test chamber.
3
NOTE: Other test chambers with a volume of 1m are also acceptable if it is proven that they are
compliant with the measurement method described in this document.

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RENAULT D49 3027 / - - B

APPENDIX 1 (continued)

6.3. EQUIPMENT USED FOR THE OPERATION OF THE TEST CHAMBER


3
- Test chamber with a volume of 1 m .
- 1 Air flowmeter, capacity 50-300l/h.
- Equipment for gas sampling.
- Thermo-hydrograph.
- Barograph.
- 3 air washers.
- Compressed air connection or pump/compressor.
- Active carbon turn.
- Oil separator in fine spray mode.
- Insulation materials (for a glass chamber only).
7. PERFORMING THE TESTS

7.1. PREPARATION OF TEST EQUIPMENT

The chamber must be regulated to a temperature of (65 ± 1) °C. Fresh air may be provided by a
compressed air circuit for example. Prior cleaning of the air is carried out using active carbon. Before
carrying out the test, the concentrations of the following individual substances must be checked to
ensure that they do not exceed the values mentioned below within the test chamber:

3
ppm µg/m
Formaldehyde < 0.005 6.3
Carbolic acids < 0.003 11.4
Ammonia < 0,.1 13,.

3
Figure 1: Structural diagram of a test chamber with a volume of 1m (E.g. chamber made of glass
with external thermal protection)

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RENAULT D49 3027 / - - B

APPENDIX 1 (continued)

7.2. TEST

Remove the test pieces from their packaging and place them in the pre-heated chamber. At the same
time, introduce the thermo-hydrograph used to record the temperature and relative humidity during
testing and then close the test chamber. Two bottles of air wash are installed in series to enable the
regulation of relative air humidity. Adjust the flow rate after closing the chamber using a regulation
transformer and a throttle valve set to the specified value, for example to (500 ± 5) l/h for an air
-1
replacement coefficient of 0.5 h .

7.3. SAMPLING CARRIED OUT TO DETERMINE THE RATE OF FORMALDEHYDE, AMMONIA


AND CARBOLIC ACIDS

Measure on a daily basis the concentration of formaldehyde, ammonia, carbolic acids until the
corresponding balancing concentration has been obtained.

NOTE: At the start of the test, sampling must be carried out twice a day for at least 3 consecutive
working days. Allow time for the suitable installation of test pieces into the test chamber.
3
A 0.1m sample of gas from the test chamber air is taken, using an appropriate gas sampling device
(figure 2), where the gas passes through the bottles of gas wash which are filled with absorption liquid
and analyzed using the corresponding methods.

Figure 2: Structural diagram of the sampling system

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RENAULT D49 3027 / - - B

APPENDIX 1 (continued)

7.3.1. Analysis methods used

7.3.1.1. Formaldehyde

To characterize the formaldehyde concentration, the test chamber air passes through the bottles of
gas wash which have been filled with distilled water at a sampling speed of 2l/mn. The formaldehyde
rate measured in the adsorption solution is defined by an acetone acetyl-based photometric and/or
fluorimetric method (VDI 3484 directive, page 2, 1999 project). The detection limit of the applied
3
method is 0.005ppm of formaldehyde (1ppm = approx. 1.25mg of HCHO/m ).

As an alternative, the characterization of the concentration of formaldehyde may be carried out using
the DNPH method. The corresponding sampling, analysis and assessments are defined in the VDI
Directive, page 3, October 1999 project.

7.3.1.3. Carbolic acids

The concentration of carbolic acids is defined using the p-nitraniline method (VDI Directive 3485,
December 1988). The absorption solution used for this purpose is caustic soda (0.1mol), the sampling
speed is 1l/mn. The detection limit of this analysis method occurs, in these sampling conditions, at
ppm ∧ approximatively 3.8 mg / m ).
3
approximately 0.003ppm of carbolic acid ( 1

7.3.1.4. Ammonia

The photometric characterization of the ammonia concentration at ambient temperature is carried out
using 0.1 mol of sulphuric acid as an absorption solution; the sampling speed is l/mn; 1ml of
absorption solution is dissolved in 5ml of solution A (dissolve 25mg of sodium nitroprusside and
9.975g of carbolic acid in the distilled water and then add more distilled water to 500ml) and B
(dissolve 2.5g of sodium hydroxide in distilled water, add 2.5ml of sodium chloride solution and then fill
to 500ml with distilled water). Balance the temperature to 40°C (thermostat) in a bain-marie for 30
mins. Then measure the extinction of the indophenol complex by photometry for a wavelength of
1 ppm ∧ 1.39 mg / m ).
3
5800nm in relation to the distilled water (detection limit: 0.01ppm ammonia;

NOTE: Other analysis methods are acceptable if it is proven that the results are compliant with the
methods described above.

8. CALCULATION OF RESULTS

Corrected sample volume calculation (20 °C, 1013 hP a):


3
Vcorr = Vp.PL. 293 [m ]
(273 + tG). 1013
3
Vcorr = corrected sample volume (20 °C, 1018 hPa) (m ).
3
Vp = recorded sample volume (m ).

PI = average air pressure during measurement (hPa).

tG = average air pressure in the gas meter during measurement (°C).

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RENAULT D49 3027 / - - B

APPENDIX 1 (continued)

Formaldehyde concentration calculation:

KCH2O = (E.g. – EXBW). A. 3 [µg/30ml]


3
K’CH2O = KCH2O [mg/m ]
1000. vcorr
3
K’’CH2O = KCH2O [ml/m ] ou. [ppm]
1.248

KCH20: Formaldehyde quantity in the sample (µg)


E.g. Termination of the absorption solution
ExBW : Termination of the reference solution
A: Coefficient of the slope of the calibration line (µg/10 ml)
3
K’CH20: Concentration of formaldehyde (mg/m )
3
K’’CH20: Concentration of formaldehyde (ppm) or (ml/m )

Ammonia concentration calculation:


(Exst – EXBW) Cst


(ExNH3 – EBW) KNH3

K’NH3 = KNH3. 30 [mg/m3]


vcorr

K’’NH3 = K’NH3. [ppm] or. [ml/m3]


1.39

ExSt: Termination of the buffer solution


ExNH3: Extinction of the reference solution
ExBW: Termination of the reference solution
KSt: Concentration of the buffer solution (mg/ml)
KNH3: Concentration of the analysis solution (mg/ml)
3
K’NH3: Concentration of ammonia (mg/m )
3
K’NH3: Concentration of ammonia (ppm) or (ml/m )

Carbolic acid concentration calculation:

Kph = (Ex-ExBW)B3 [mg/30ml]


3
K’ph = Kph [mg/m ]
Vcorr

K’’ph = Kph
3.8

E.g. Extinction of the reference solution


ExBW : Termination of the reference solution
B: Coefficient of the slope of the calibration line (mg/10 ml)
Kph: Concentration of carbolic acids (mg)
3
K’ph: Concentration of carbolic acids (mg/m )
3
K’’ph: Concentration of carbolic acids (ppm) or ml/m )

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RENAULT D49 3027 / - - B

APPENDIX 1 (continued)

9. TEST REPORT

The test report must refer to this VDA recommendation and contain the following information:

- test piece origin,

- location, position and state of the material at the moment of sampling, particularly the humidity,

- manufacturing date of the test piece,

- date of sampling,

- test date,

- test conditions,

- test chamber loading rate,

- calculated value of formaldehyde, ammonia and carbolic acid concentration (in ppm for example),
1)
- additional details .
1)
Description of all operations non-compliant with this VDA recommendation (removal of test piece,
conditioning, etc.).

© RENAULT 2011 Page 39/39

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