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Inalfa Engineering Standard

Page 1 of 19
IES 60.020
Volatile Organic Components
(Emission Testing)
Revision 02 2013/12 (yyyy/mm)
First published 2012/04 (yyyy/mm)

Index:

1. Scope. 2

2. Standards referred to. 3

3. Specification on Drawing. 3

4. General 3

5. Sample collection. 4

6. Odor Test. 4

7. Formaldehyde Emission Test. 4

8. Fogging Test. 5

9. Total Volatile Organic Components Test. 5

10. Attachment A – English translation VDA 275. 6

11. Attachment B – English translation VDA 277. 14

12. Attachment C – Test Waiver. 18

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Inalfa Engineering Standard
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IES 60.020
Volatile Organic Components
(Emission Testing)
Revision date: 2013/12 (yyyy/mm)

1. Scope

The purpose of this standard is to define emission tests and limit values on component level
parts so that the components and systems will meet most OEM requirements. Tests results
need to be provided with PPAP approval. Testing can also provide early material verification
during the development phase.

This document also includes an English translation (attachment) for referenced VDA
standards where no English version exists.

Testing must be repeated before any material changes can be approved.

SERIAL PRODUCTION PHASE

DEVELOPMENT PHASE PRODUCTION VALIDATION PRODUCTION CONFIRMATION


PRODUCT CONFIRMATION PHASE
SYSTEMATIC PRODUCT
DESIGN VERIFICATION TESTING PROCESS VALIDATION TESTING VERIFICATION (SPV)
(DV) (PV) (Ref. IES 60.033)
(Time Required)

(Time Required)

(Time Required)
SEQUENCE

SEQUENCE

SEQUENCE
DURATION

DURATION

DURATION
TEST REQUIREMENT
TEST REQUIREMENT TEST REQUIREMENT
Sample Quantity = See
Sample Quantity = 0 Sample Quantity = 0
Test for Quantities

1
1 Odor Test
PPAP

Day
Formaldehyde 1
2
Emission Test Day
1
3 Fogging Test
Day

Total Volatile Organic 1


4
Component Test Day

For materials that are already validated (listed in IES 10.012 Material Emission Compliance
Overview List), a waiver can be used. For further details on evaluating if new testing is
required, refer to “Attachment C – Test Waiver”

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Inalfa Engineering Standard
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IES 60.020
Volatile Organic Components
(Emission Testing)
Revision date: 2013/12 (yyyy/mm)

2. Standards referred to

Reference standards:

Standard Number Standard Name


VDA 270, October 1992 Determination of the odor characteristics of trim materials in motor vehicles
VDA 275, July 1994 Determination of formaldehyde emission of components in vehicle interiors
ISO 6452, June 2007 Determination of fogging characteristics of trim materials in interior of automobiles
VDA 277, January 1995 Determination of organic emissions from non metallic materials in vehicle interiors

3. Specification on the Drawing

The following information shall be specified on the drawing:

“Part must comply with emission requirements according to IES 60.020”.

Deviations from this standard must be specified explicitly on the drawing. Drawing
specifications override specifications in this standard.

Emission tests and requirements in this standard only apply to parts having a weight greater
than 20 grams or, in case of POM greater than 5 grams. All parts having a surface area
greater than 100 cm2 require conformance to this standard.

4. General

The testing and requirements of this standard apply only to homogeneous materials. For
components consisting of multiple materials, this standard applies to each of the individual
materials. The weight and surface area values shown in section 3 apply to each specific
material used in the component.

For coated polymeric materials, testing may be done on the coated material ensuring that a
representative amount of coated surface is used for the test specimen.

For coated non-polymeric substrates (e.g. metals), the weight and surface area values
shown in section 3 refer to the coating only. If the coating cannot be separated from the
substrate, the coating is to be applied on a glass substrate; the coating and its application
process should represent that of the original component.

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Inalfa Engineering Standard
Page 4 of 19
IES 60.020
Volatile Organic Components
(Emission Testing)
Revision date: 2013/12 (yyyy/mm)

5. Sample collection

Unless otherwise approved by Inalfa, samples are to be taken from actual parts, produced
using production representative process conditions.

Samples shall be collected directly from the manufacturing or packaging line and packed
within 24-hours of production unless otherwise specified. Seal the samples with two layers
of heavy-duty aluminum foil so the air space within the package is minimized, crimping the
seams to create an airtight seal. Use clear packaging tape to assure that the package is
airtight. Label the foil package and place in a clear polyethylene or polyester bag.

6. Odor Test

This test evaluates the odor characteristics of materials under the influence of temperature
and climate conditions.

The odor test is performed according to VDA 270 C3.

Requirement: grade ≤3

7. Formaldehyde Emission Test

This test evaluates the formaldehyde characteristics of materials.

The formaldehyde emission test is performed according to VDA 275.


Since no English version exists for this standard, an English translation is included in
attachment A.

In case the in the VDA 275 specified specimen size (40mm x 100mm x thickness) is not
available in the part to verified, take 10 grams instead (if 10 grams of materials is not
available in one part, more parts can be used to collect 10 grams of material). The form of
this material is irrelevant.

Requirement: ≤10mg/kg.

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Inalfa Engineering Standard
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IES 60.020
Volatile Organic Components
(Emission Testing)
Revision date: 2013/12 (yyyy/mm)

8. Fogging Test

This test evaluates the fogging characteristics of materials. Fogging refers to volatile organic
components released from automotive interior materials that can condensate elsewhere in
the vehicle, such as on the windscreen.

The fogging test is performed according to ISO 6452.

Requirement (gravimetric): ≤2mg.

9. Total Volatile Organic Components (TVOC) Test

This test evaluates the emission characteristics of materials, measuring the sum of all
released organic substances.

The TVOC test is performed according to VDA 277.


Since no English version exists of this standard, an English translation is included in
attachment B.

Requirement: ≤20μg Carbon/g


Below detection limit: Benzene, N-nitrosamines, NMP (N-Methyl-2-pyrrolidone).

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Inalfa Engineering Standard
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IES 60.020
Volatile Organic Components
(Emission Testing)
Revision date: 2013/12 (yyyy/mm)

Attachment A – English translation VDA 275

Below is an English translation of relevant parts of standard VDA 275, July 1994.
The reason for including this English translation in this standard is because an English
version of VDA 275 is not available.
The translation is for reference only; the original VDA standard takes precedence over this
translated version.

Form part for the cabin interior.


Determination of the formaldehyde content.
Measuring process according to the modified flask method.

Principle:

With this test samples with a defined mass and size are being stored for a defined period in
a 1 liter polyethylene flask over distilled water at constant temperature. This is followed by
cooling the flask and determining the absorbed amount of formaldehyde in the distilled
water. The measured formaldehyde is referred to dry part weight (mg/kg).

Reagents:

For the analysis reagents, analytically pure quality and distilled or demineralized water
should be used.

The formaldehyde measurement is done photometrically according to the acetyl acetone


method. Other methods however are allowed provided they their specifications are in
accordance with the reference method for the analysis.

Acetyl acetone p.a.


Ammonium nitrate p.a.

Remark:
prepared solutions available on the market can be used, if they provide the same result.

Test apparatus:

Precision scale ±1mg

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Inalfa Engineering Standard
Page 7 of 19
IES 60.020
Volatile Organic Components
(Emission Testing)
Revision date: 2013/12 (yyyy/mm)

Well ventilated thermostatically controlled chamber capable of maintaining a


temperature of (103±2) ˚C.

Circulating air chamber, capable of maintaining a temperature of (60±2) ˚C.

Spectral photometer

Test apparatus:
> Polyethylene flask with a volume of 1 liter with lid. See picture below.

> Hook of stainless steel sealed at the attachment point of the lid to the flask.

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IES 60.020
Volatile Organic Components
(Emission Testing)
Revision date: 2013/12 (yyyy/mm)

Laboratory Test Apparatus:


> Precision burette 50 ml, calibrated at 20˚C
> 2 volumetric flasks, 1000 ml, calibrated at 20˚C
> 6 volumetric flasks, 100 ml, calibrated at 20˚C
> Volumetric pipette, 5 ml, calibrated at 20˚C
> Volumetric pipette, 10 ml, calibrated at 20˚C
> Volumetric pipette, 15 ml, calibrated at 20˚C
> Volumetric pipette, 20 ml, calibrated at 20˚C
> Volumetric pipette, 25 ml, calibrated at 20˚C
> Volumetric pipette, 50 ml, calibrated at 20˚C
> Volumetric pipette, 100 ml, calibrated at 20˚C
> Erlenmeyer flasks, 250 ml
> Flasks, 50 ml with plug
> Watch glass with a diameter of approximately 120 mm
> Desiccator
> Cuvettes with suitable thickness for the spectral photometer

Test Samples:
> sampling:
the samples are to taken distributed over the width of the cooled part at appropriate
and suitable locations.
> The size of the samples should be 40 mm x 100 mm x thickness. Per part at least 6
samples are to be taken; 5 samples for formaldehyde measurement, 1 sample for
measuring moisture content.

Test Procedure:

Number of tests:
5 evaluations are to be carried out.

Measuring moisture content:


Moisture content is measured according to DIN EN 322.

Measurement of the formaldehyde emission:


The samples are measured prior to the analysis within 0.01g precision. 50 ml of
distilled water is added to the polyethylene flasks.

> In every sample at the center top a hole of 1 to 2 mm is drilled for fixation.

> After fixating the sample to the hook in the flask, the flask is closed and heated for
3 hours at a constant temperature of 60˚C in a circulating air chamber.

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IES 60.020
Volatile Organic Components
(Emission Testing)
Revision date: 2013/12 (yyyy/mm)

> After the test period, the flasks are taken from the chamber. Samples are to be
removed from the flasks after 60 minutes at room temperature.

Blank Test:
The test is carried out in parallel without samples.

Measuring the formaldehyde concentration in the aqueous solution:


The measurement of the formaldehyde concentration of the aqueous solution is done
photometrically following the acetylene acetone method.

> Principle:
Measurement based on the so called Hantzsch-reaction (see below) where the
formaldehyde in the aqueous solution reacts with ammonium ions and acetyl acetone
to form diacetyl-dihydrolutidin (DDL). DDL has an absorption maximum at 412 nm.
The reaction is specific for formaldehyde.

Reagents:
> Acetyl acetone solution
4 ml acetyl acetone is added to a 1000 ml volumetric flask, add distilled water to 1000
ml. The solution has a durability of 4 weeks if sealed air tight and stored in the dark.

> ammonium nitrate solution


200 g ammonium nitrate are weighed in a 1000 ml volumetric flask, dissolved in
distilled water, filled up to 1000 ml.

Procedure:
10 ml of the aqueous formaldehyde solution are being dosed with a pipette and in a
50 ml volumetric flask, adding 10 ml acetyl acetone solution and 10 ml ammonium
nitrate. The flask is closed, shaken, and heated for 15 minutes in a water bath at
40˚C. The green-yellow solution is cooled down to room temperature, shielded from
sun light (approximately 1 hour). The extinction of this solution is being measured at a
wave length of 412 nm against distilled water with spectral photometer. A blank test

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Inalfa Engineering Standard
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IES 60.020
Volatile Organic Components
(Emission Testing)
Revision date: 2013/12 (yyyy/mm)

with distilled water is evaluated in parallel and is taken into account when calculating
the flask value.

Remark:
After every measurement the polyethylene flasks must be cleaned in a laboratory
dishwasher. If this is insufficient, it is advised to put the flasks opened in a circulating
air chamber at 70˚C for 16 hours.

Calibrating Curve:
The calibration curve (see below) is established over a formaldehyde standard
solution, of which its concentration is measured using iodometric titration. The
calibration curve is to be verified at least once a week.

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IES 60.020
Volatile Organic Components
(Emission Testing)
Revision date: 2013/12 (yyyy/mm)

Formaldehyde Standard Solution:


Reagent solutions:

> Iodine c (I2) = 0.05 mol/l


> Sodium thiosulfate c (Na2S2O3) = 0.1 mol/l
> Caustic soda c (NaOH) = 1 mol/l
> Sulphuric acid c (H2SO4) = 1 mol/l
> Dilute solution 1 % m/m

The titer of the solutions are to be verified before use.

Approximately 1 g formaldehyde solution (concentration 35 to 40%) is dissolved in


distilled water in a 1000 ml volumetric flask and filled up to the mark. The exact
formaldehyde concentration is measured as follows:

20 ml of the formaldehyde solution are mixed with 25 ml iodine solution and 10 ml


caustic soda. After 15 minutes rest, shielded from light, 15 ml of sulphuric acid is
added. The excess of iodine is being titrated with the thiosulfate solution. When
finished titration add a few drops of dilute solution as indicator. A blank test is done in
parallel using distilled water.

The formaldehyde concentration is being calculated using following formula:

c (HCHO) formaldehyde concentration in mg/l


V0 volume of thiosulfate solution for blank test in ml
V volume of thiosulfate solution in ml
c (Na2S2O3) concentration of thiosulfate solution in mol/l

Remark:
1 ml 0.1 mol/l thiosulfate solution equals 1 ml 0.05 mol/l iodine solution and 1.5 mg
formaldehyde.

Formaldehyde Calibration Solution (cuvette layer thickness: 1cm):


Pipette from a micro burette a volume containing 15 mg formaldehyde of the
formaldehyde standard solution into a 1000 ml volumetric flask and fill up with
distilled water up to the mark. 1 ml of this solution contains 15 µg formaldehyde.

Establishing the calibration curve:


Pipette 0, 5, 10, 20, 50 or 100 ml of formaldehyde calibration solution into six 100 ml

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IES 60.020
Volatile Organic Components
(Emission Testing)
Revision date: 2013/12 (yyyy/mm)

volumetric flasks and fill them up to the mark with distilled water. 10 ml of each
dilatation is measured using the same method as described under “Measurement of
the formaldehyde emission” photometrically. The extinctions are plotted against the
formaldehyde concentrations (between 0 and 15 µg/ml) on millimeter paper. The
slope is derived graphically or calculated.

Formaldehyde Calibration Solution (cuvette layer thickness: 5cm):


Pipette from a micro burette a volume containing 3 mg formaldehyde of the
formaldehyde standard solution into a 1000 ml volumetric flask and fill up with
distilled water up to the mark. 1 ml of this solution contains 3 µg formaldehyde.

Establishing the calibration curve:


Pipette 0, 5, 10, 20, 50 or 100 ml of formaldehyde calibration solution into six 100 ml
volumetric flasks and fill them up to the mark with distilled water. 10 ml of each
dilatation is measured using the same method as described under “Measurement of
the formaldehyde emission” photometrically. The extinctions are plotted against the
formaldehyde concentrations (between 0 and 3 µg/ml) on millimeter paper. The slope
is derived graphically or calculated.

Calculating Results:

Moisture content:
Moisture content H (in Mass % m/m) of the part is calculated with the following
formula:

m1 = mass of the sample before drying in grams


m0 = mass of the sample after drying in grams

Formaldehyde emission following the flask method:


The total amount of absorbed formaldehyde is being derived from the slope factor of
the photometric analysis and the total volume of water in the absorption liquid (in this
case: 10 ml). This formaldehyde content in mg/kg is being calculated related to the
sample weight corrected for dry state.

Calculation of the formaldehyde emission in mg/kg:

AS : the extinction of the analyzed solution

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IES 60.020
Volatile Organic Components
(Emission Testing)
Revision date: 2013/12 (yyyy/mm)

AB : the extinction of the analysis with distilled water


f : the slope factor of the calibration function (in µg/ml)
m : sample mass in g
H : moisture content of sample material in %
V : volume of the absorption solution (50 ml)
bd : bone dry
F : factor for calculating the analysis result in kg [mg/kg]; F = 10

Test Report:
In the test report, if available, following information is to be reported under reference
to VDA 275:

> Origin of sample material


> Location, condition and state of the material at time of sampling,
especially the humidity
> Date and manufacturing of the material
> Date of sampling
> Date of formaldehyde content analysis
> Moisture content (%) at the time of analysis
> Formaldehyde emission according the flask method
(mg formaldehyde/kg bd material)
> Description of any other relevant details
Report on all aspects that are not in accordance with VDA 275 (sampling,
conditioning, etc.).

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Inalfa Engineering Standard
Page 14 of 19
IES 60.020
Volatile Organic Components
(Emission Testing)
Revision date: 2013/12 (yyyy/mm)

10. Attachment B – English translation VDA 277.

Below is an English translation of relevant parts of standard VDA 277, January 1995.
The reason for including this English translation in this standard is because an English
version of VDA 277 is not available.
The translation is for reference only; the original VDA standard takes precedence over this
translated version.

Non-metallic automotive interior trim parts.


Determination of the emission of organic compounds.

Goal:
VDA 277 test standard measures the emission of organic components from non-
metallic materials, having an influence on the interior air quality of the passenger cell.
Measurement of the emission potential for a material is the sum of all values of the
emitting substances, separated with a gas chromatograph and detected by flame
ionization detector. The sample delivery using head-space technology at tempering at
120˚C.

Requirements:
The associated sampling locations, the respective requirements as well as the
specific executions per referred specification or drawing are to be taken respected.
If components consist of multiple materials, a separate test for each individual
material may be requested.

Sample preparation:
Transport and storage of samples must be done in an aluminum coated polyethylene
bag.
The sampling must be done immediately when parts are received or in a condition
that reflects this state. The time of receipt of the components and the sampling time
must be recorded.
Generally samples are not conditioned. Exceptions are natural materials (cotton,
wood, leather, wool). These materials are before weighing-in dried as chopped
pieces for 24 hours over calcium chloride (CaCl2).
The sample is to be taken from the specified location sample form the total parts
section. The sample is to be chopped to small pieces between 10 and 25 mg without
heating the sample. When needed another sample preparation method may be
specified. This should then be reported with the results.

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IES 60.020
Volatile Organic Components
(Emission Testing)
Revision date: 2013/12 (yyyy/mm)

The sample weight is depending on the size of the head space flask, which volume
has to be at least 5 ml. Per 10 ml flask volume 1.000 g ± 0.001 g (weighing error
maximum 0.1%) sample material is required. Metal parts are to be removed before
weighing-in.
Organic substances that adhere to metal parts, e.g. paints, adhesives, etc. are to be
mechanically separated before weighing-in.
The sample particles are weighed in a head space flask (at least 3 flasks per test).
The flasks are sealed gas tight using a septum with a teflon coating pointing inward.

Test Apparatus, Test Conditions:

Test apparatus:
Gas chromatograph for capillary column operation with head space sampler, flame
ionization detector (FID) and computer/integrator.

WCOT-capillary separation column with 100% polyethylene glycol separation phase


(so called wax-type, e.g. DB-wax, carbo wax…)
0.25 mm I.D., 0.25 µm film thickness, and 30 m length.

Analytical balances, precision 0.1 mg

Microsyringe, 5 µl, sampling in glass-body

Measuring conditions:
GC oven temperature:
3 minutes isothermal at 50 ˚C
Heating to 200 ˚C with rate of 12 K / min
4 minutes isothermal at 200 ˚C
Injector temperature: 200 ˚C
Detector temperature: 250 ˚C
Split ratio: approximately 1 : 20
Carrier gas: helium
Average carrier gas speed: approximately 22 – 27 cm / s
Remark: the substance 2,6-di-tert-butyl-4-methylphenol (BHT) should have a
retention time below 16 minutes.

Test:
For adsorption of the substances, directly before measuring the flasks are to be
conditioned in the head space sampler in the air over the samples for 5 hours ± 5
minutes at 120 ˚C ± 1 ˚C and immediately after analysis. 3 Samples are to be
analyzed.

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IES 60.020
Volatile Organic Components
(Emission Testing)
Revision date: 2013/12 (yyyy/mm)

The blank value is determined by averaging the signal of at least 3 measurements


with empty flasks.
The dosage must be reproducible and identical during all analysis of samples, blank
values and calibration solutions.
The separation column is for heating to be heated to it maximum temperature at least
once a week for 15 minutes.

Calibration:
For the quantitative measurement of the total carbon emission as well as the amount
of specific individual substances, the calibration curves are to be established
according to the method of external standards.
Acetone is used for calibration for the total carbon emission, for the individual
substances the respective substances themselves.
After installation of a new column and after each change in the apparatus a basic
calibration with 7 calibration concentrations is to be performed. In addition, a check
calibration with at least 3 calibration concentrations is to be performed every 4 weeks.
For acetone for the basic calibration 7 calibration concentrations 0.1 / 0.5 / 1 / 5 / 10 /
50 and 100 g acetone per liter n-butanol need to be prepared.
For the check calibrations at least three concentration 0.5 / 5 and 50 g acetone per
liter need to be prepared. It is to be verified that the n-butanol used does not produce
peaks at the same time as acetone.
For the specific individual substances calibration solutions in similar concentration
need to be prepared, where a solvent is to be used that, with the retention time of the
respective substance does not produce peaks, and of which the boiling point is below
120 ˚C.
The various substances used for calibration should be at least of analytically pure
quality.
For the calibration measurements a 5 µl syringe is used, to inject each time 2 µl ±
0.02 µl (injection error maximum 1%) per 10 ml flask volume into an empty, non-
sealed head space flask.
The calibration samples are conditioned 1 hour at 120 ˚C in the head space sampler
after which they are analyzed in accordance with the general guide lines, at which the
temperature program of the gas chromatograph can be terminated after elution of the
solvent.
When plotting the for the respective calibration substance established area against
the concentration of the calibration solutions (in g/l) a best-fit straight line can be
created, of which the slope represents the calibration factor k (k (G) for the total
emission and k (i) for the individual substance emission). This should be done using
the least squares method. The correlation coefficient k needs to be greater than
0.995.

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IES 60.020
Volatile Organic Components
(Emission Testing)
Revision date: 2013/12 (yyyy/mm)

Evaluation:
From the registered gas chromatograph data, the total peak area as well as areas for
the peaks for the specified individual substances needs to be analyzed.
For the calculation of the total peak area only peaks are taken into account,
> of which the height exceeds the 3-fold value of the basic noise level
> of which the area exceeds 10% of the acetone peak of the calibration solution with
a concentration 0.5 g/l

The detection limit of the analysis method should result a peak height and peak area,
that is below 10% of the actual value that is found with the analysis of an acetone
calibration solution with a concentration of 0.5 g/l acetone.

The emission values are calculated from the measuring results as follows:

> total carbon emission EG:


calculated from the total peak area as found in the sample analysis and calibration
factor k(G) of the acetone calibration

Unit in “µg carbon per g sample”.

The factor two relates to “g sample”, and is given by the fact that for each g of sample
material, 2 µl of calibration solution is dosed in the 10 ml flask.
The factor 0.6204 is representing the carbon weight content in acetone.

> Individual substance emission Ei:


calculated from the total peak area as found in the sample analysis for the individual
substance and calibration factor k (i) of the individual substance calibration

Units in “µg substance i per g sample”.

The factor two relates to “g sample”, and is given by the fact that for each g of sample
material, 2 µl of calibration solution is dosed in the 10 ml flask.

From the results of 3 samples are not be averaged, but all should meet the
requirement. This is to ensure that all locations of the component meet the
requirement.

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IES 60.020
Volatile Organic Components
(Emission Testing)
Revision date: 2013/12 (yyyy/mm)

Attachment C – Test Waiver

Test Waiver:

This section allows waiving certain emission tests based on a risk assessment using earlier
validation evidence and material behavior.
Decision flow chart below applies to all individual emission requirements:
- Odor
- Formaldehyde
- Fogging
- Total Volatile Organic Components

The supplier remains in all cases responsible that the material complies with the emission
requirements.

A test report from a certified laboratory may be used as performance reference.

A waiver for the formaldehyde emission test can be given based on an explicit statement of
the supplier that the nature of the materials used cannot lead to formaldehyde emission.

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IES 60.020
Volatile Organic Components
(Emission Testing)
Revision date: 2013/12 (yyyy/mm)

Do not use this waiver if any reasonable doubt exists regarding its usage.

When this waiver applies, reference to earlier validation results must be provided.

Material:

The term “Material” in the flow chart refers to the components’ material.

Referring to the exact grade (same trade name) of the material the supplier is using.

In case a component consists of multiple materials, the above statements apply to every
individual material used in the final component.

In case of multiple material components, the waiver option needs to be assessed for each
individual material.

In case of coated materials, the coating specification must be the same as earlier validated
(material, thickness)

02 Section 7: Formaldehyde 10 grams weight intake specified Dec. 2013 T. Nabuurs


Correct translation error VDA277 detector temperature to
01 “250ºC”. Sept. 2013
T. Nabuurs
Change fogging test temperature from 85⁰C to 100⁰C and
requirement raised from ≤0.3mg to ≤2mg.
Approval and Release with Integration of IES 60.012
00 “Determination of the odour characteristics of trim materials in April 2012 T. Nabuurs
motor Vehicles”
REVISION CHANGE DESCRIPTION APPROVAL APPROVED
DATE BY

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