Tremco Illbrück

Route de Gray
21850 Saint Appolinaire

Att. M. Jean François ANGONIN

Vitry, , October 29th , 2015

Our ref: Estimate # 201420756.1

Your ref: Order # 15/2227
Subject: Study report # V430024B

Dear sir,

Enclosed please find the results of the tests carried out according to the agreed
program, concerning sealant JS 680.

Remaining at your disposal for any information you may require, we look forward to
hearing from you.

Florence BRUNO Jerôme DELAFOY

Unit Manager Technician
bruno@lrccp.com delafoy@lrccp.com

Materials & Processes Unit

 Tremco Illbrück
Route de Gray
21850 Saint Appolinaire

Report study # V430024B

October 29th , 2015

Report study in accordance with

CEKAL standards
Sealant JS 680

CONFIDENTIAL

DQ15V03
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October 29th , 2015

Tremco Illbrück
Route de Gray
21850 Saint Appolinaire

Report study in accordance with

CEKAL standards
Sealant JS 680

References : Quotation # 201420756.1

Order # 15/2227

Analyses and tests results included in this report only concern the samples, products or materials which
were provided and tested. They do not prejudge of the representativeness of these objects compared to
manufacture products.

The reproduction of this report is authorized only in its integral form.

It contains 10 pages.

Samples relating to this study are kept for six months. Beyond this period, they will be eliminated unless
otherwise specified.
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October 29th , 2015

CONTENTS

I. References of samples tested ...................................................................................... 4

II. Synthesis of results ..................................................................................................... 4
III. Results....................................................................................................................... 5
III.1 Fogging ............................................................................................................... 5
III.2 Thermogravimetric analysis ................................................................................... 5
III.3 Infrared Spectrometry ........................................................................................... 6
III.4 Pyrolysis gas chromatography mass spectrometry analysis ....................................... 7
IV. Tests conditions.......................................................................................................... 9
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I. REFERENCES OF SAMPLES TESTED

Reference Lot number Production date Place of taking

Gomaverre
JS 680 7383/15 March 17th 2015
(22/05/2015)

II. SYNTHESIS OF RESULTS

Reference results
Test Specification 2014 Results 2015
Report# V430001B
Fogging specification CEKAL no visible condensation no visible condensation

61,5 % pyrolyzable 61,5 % pyrolyzable

TGA NFT 46047 26,0 % oxidizable 26,0 % oxidizable
12,5 % mineral residue 12,5 % mineral residue

FTIR NF ISO 4650 IIR or/and PIB IIR or/and PIB

PY/GC/MS NF ISO 17257 / IIR or/and PIB

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October 29th , 2015

III. RESULTS

III.1 FOGGING

After 24 hours of test no visible condensation on the glass surface was observed.

III.2 THERMOGRAVIMETRIC ANALYSIS

Reference results 2014 Results 2015

Figure 1 : Thermogram of sample in the state of reception

Reference results
Results 2015
2014
Pyrolyzable 61,5 % 61,5 %

Oxidizable 26,0 % 26,0 %

Mineral residue at 900 °C 12,5 % 12,5 %

Tableau 1 –Weight composition of sample in the state of reception

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October 29th , 2015

III.3 INFRARED SPECTROMETRY

Reference
results 2014

Results 2015

Figure 2 : IR spectrum of sample in the state of reception

Wave number cm-1 Functional group

1230 >C<

1370 and 1390 >C(CH3)2

1460 -CH2-

Tableau 2 – Functional groups isobutene (butyl rubber or PIB)

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III.4 PYROLYSIS GAS CHROMATOGRAPHY MASS SPECTROMETRY ANALYSIS

Figure 3 : First step : Pyrolysis at 250 °C of sample in the state of reception

Retention time
Identified Compound CAS number Origin
(min)
Residue of amino
5.02 1-Butanamine, N-butyl- 111-92-2
accelerator
12.55 Butylated Hydroxytoluene 128-37-0 Antioxidant

Tableau 3 –Pyrolysis products at 250 °C

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Figure 4 : Second step : Pyrolysis at 550 °C of sample in the state of reception

Retention time
Identified Compound CAS number Origin
(min)
1.88 Isobutylene 115-11-7
Specifics products of
6.34 Diisobutylene 107-39-1
isobutene (butyl
12.62 Triisobutylene 7756-94-7
rubber and/or PIB)
16.44 Tetraisobutylene 15220-85-6
Tableau 4 –Pyrolysis products at 550 °C

Florence BRUNO Jerôme DELAFOY

Unit Manager Technician
bruno@lrccp.com delafoy@lrccp.com

Materials & Processes Unit

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October 29th , 2015

IV. TESTS CONDITIONS

Fogging :

Standard: Method CEKAL

Temperature of oil: 90 ± 2 °C
Temperature of the cooled plate: 10 ± 2 °C
Time of test: 24 h
Weight of sample: 100 ± 40 g
Beaker in Stainless steel: Ø 65 mm, height 85 mm
Glass plate: 100 x 100 mm

The mastic sample coated with a non-stick paper is put in a stainless steel beaker.
The beaker is placed on a support and introduced into oil silicone bath (see picture).
The beaker is closed by a glass plate, with a refrigerated plate, controlled by a cooling system
at 10 °C.

Cooling plate

Insulating
Glass plate

Support
Sample

Oil bath

After 24 hours, the glass is examined by eye to detect condensation of volatile substances from
the sealant sample.
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Experimental conditions for TGA:

Standards: NF ISO 11358 and NFT 46-047 procedure A

Equipment: Thermal analyser, Perkin Elmer TGA 7
Sample weight: > 10 mg
Uncertainty of measurement (absolute) : ± 0,2 %

Thermal programme under nitrogen (pyrolyzable phase):

 initial temperature: 35 °C
 final temperature: 600 °C
 cooling: 600 °C to 400 °C
 heating rate: 20 °C / min
Thermal programme under air (oxidizable phase):
 initial temperature: 400 °C
 isotherm at 400 °C: 2 min
 final temperature: 900 °C
 isotherm at 900 °C: 5 min
 heating rate: 20 °C / min

Experimental conditions for FTIR :

Standard: NF ISO 4650

Used technique: attenuated total reflexion (ATR)
Sampling method: surface analysis
Equipments: Thermo Nicolet Avatar 730 Spectrometer
Accessory ATR: Thunderdome single crystal germanium reflexion

Experimental conditions for PY/GC/MS :

Standard: NF ISO 17257

Used technique: Pyrolysis /gas chromatography /mass spectrometry)
Sampling method: Pyrolysis (2 Temperatures) of rubber
Equipments: Pyrolyseur CDS 5150
GC/MS: Thermo Focus DSQ II
Capillary column: HP-1MS 30m – 0,25 mm – 1 µm