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IES 60.020
Volatile Organic Components
(Emission Testing)
Revision 02 2013/12 (yyyy/mm)
First published 2012/04 (yyyy/mm)
Index:
1. Scope. 2
3. Specification on Drawing. 3
4. General 3
5. Sample collection. 4
6. Odor Test. 4
8. Fogging Test. 5
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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.
(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
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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2. Standards referred to
Reference standards:
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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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.
Requirement: grade ≤3
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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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.
This test evaluates the emission characteristics of materials, measuring the sum of all
released organic substances.
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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.
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.
Remark:
prepared solutions available on the market can be used, if they provide the same result.
Test apparatus:
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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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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.
> 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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> 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.
> 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.
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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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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Remark:
1 ml 0.1 mol/l thiosulfate solution equals 1 ml 0.05 mol/l iodine solution and 1.5 mg
formaldehyde.
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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.
Calculating Results:
Moisture content:
Moisture content H (in Mass % m/m) of the part is calculated with the following
formula:
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Test Report:
In the test report, if available, following information is to be reported under reference
to VDA 275:
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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.
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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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:
Gas chromatograph for capillary column operation with head space sampler, flame
ionization detector (FID) and computer/integrator.
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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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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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:
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.
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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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 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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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)
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