### Test Report - Copy

This report shall not be reproduced except in full without the written approval of the testing laboratory. Result survey

- Page 3

Test Fire p ropagation rate (UN)

- Page 4

Flashpoint according DIN EN ISO 2719

- Page 5
Autoignition temperature

- Page 6
Differential Scanning Calorimetry (DSC)

- Page 8

Assessment

- Page 11

### Test Report - Copy

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### Test Report - Copy

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## Result survey

Fire propagation rate (UN) Because of the result of the preliminary test the test substance is not considered a flammable solid of division 4.1.

Flashpoint

DIN EN ISO 2719: Flashpoint: 79.5 °C

Autoignition temperature Autoignition temperature (corrected): 480 °C Temperature class: T1

Differential Scanning Calorimetry (DSC)

in V4A

No exothermic reaction has been found in the stated temperature interval.

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## Fire propagation rate (UN)

Principle of the method The burning time of a powder train 250 mm in length is measured and it is observed whether the flame passes a wetted zone. A gas flame or a hot wire is used as igniter.

Test method Recommendations on the Transport of Dangerous Goods, Manual of Tests and Criteria, 2nd revised edition, Part III, Test N.1, Section 33.2.1.4 Preparation The crystllin solid was pulverized before the measurement.

Result 1. Preliminary test: Burning time ( 200 mm test distance): The product melts in contact with the hot wire. The resulting liquid flared briefly in contact with the hot wire. Local burning without propagation. The preliminary test is negativ. Because of the result of the preliminary test the test substance is not considered a flammable solid of division 4.1.

Remarks The test results relate only to the items tested.

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## Flashpoint according DIN EN ISO 2719

Principle of the method The closed crucible containing the sample is heated. While the temperature is slowly increased, an attempt is made from time to time to ignite the vapour/air mixture with an ignition flame introduced through a cover aperture.

Test method
DIN EN ISO 2719, method A (comparable to ASTM D 93)

Test conditions The test was made following the standard procedure. Instrument error of the thermometer according to the calibration certificate (registration number 579 ): 0.1 °C The test was performed under a barometric pressure of 1006 mbar. Prior to the measurement, the sample was liquefied at 50.0 °C.

Results

Initial test: 80.0 °C

Main test Corrected value in °C 79.3

The corrected flashpoint to the nearest 0.5°C is

79.5 °C

Remarks The test results relate only to the items tested.

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## Autoignition Temperature of Gases and Vapours

Definition The autoignition temperature (AIT) of a flammable gas or vapour is the lowest temperature of a hot surface (in this case the heated wall of a 200-ml conical flask) at which under specified test conditions an ignition of a flammable gas or flammable vapour in mixture with air or air/inert gas occurs with the production of flames and/or deflagration.

Test method The AIT was determined in accordance with the method prescribed in DIN EN 14522 (Method S).

Automatic test.

Test conditions Ambient pressure during the test: 1005 mbar to 1013 mbar Ambient temperature during the test: 23 °C to 23 °C Oxidiser: atmospheric air

Results

test run no. lowest temperature leading to autoignition

°C quantity of sample

ml ignition delay

time

sec 1 496 0.07 14

2 487 0.07 16

3 492 0.07 18

Autoignition temperature (corrected)*: 480 °C

* The lowest observed auto ignition temperature is reduced by a factor of 1.5% in order to take into account all uncertainties (calibration, temperature measuring system, amount of substance, etc.), this value is then rounded to the next 1 K

. Electrical and non-electrical equipment, which may be in contact with explosive mixtures of the test substance and air, has to be of a temperature class T1 or higher.

Te mperature classes according to EN 60079- 0:

Temperature class of electrical and non

- electrical equipment Maximum surface temperature in °C T1 T2 T3 T4 T5 T6 450 300 200 135 100 85

### Test Report - Copy

This report shall not be reproduced except in full without the written approval of the testing laboratory. Remarks The results apply only to the samples tested. In the interior of large heated containers or reactors, flammable gases and vapours can be ignited in a range up to 50 °C below their AIT measured according to the cited standard (DIN EN 14522). Where there are catalytic effects, the temperature effects can be even greater.

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## Differential Scanning Calorimetry (DSC)

Test Method The test complies with DIN 51007. Apparatus: heatflux differential scanning calorimeter

Results
No exothermic reaction has been found in the stated temperature interval.

The result(s) is(are) shown in fig. DSC-1

.

Test conditions

instrument: Mettler TA 8000 test cell (inliner ): closed high pressure cell, V4A sample mass: 27.3 mg sample atmosphere: nitrogen reference: empty cell evaluated temperature interval: 30 - 500 °C heating rate: 2.5 K/min sensitivity: 20 mW

Definitions Differential scanning calorimetry, DSC - a technique in which the difference in energy inputs into a substance and a reference material is measured as a function of temperature, while the substance and the reference material are subjected to a controlled temperature program
Onset temperature - the temperature at which a deflection from the established baseline is first observed Peak temperature - the temperature corresponding to the maximum deflection of the DSC

curve
Remarks The DSC is a rapid screening test useful for detecting potentially hazardous reactions and for estimating the temperatures at which these reactions occur. Decomposition pressures and gas evolution rates cannot be obtained from a DSC test. The results refer exclusively to the investigated sample. Catalytically active impurities (inclusive the material of the sample cell), although in general not changing the energy content, may affect the onset temperature significantly. Samples should be representative of the material being analysed including particle size and purity. Inhomogeneous samples may yield incorrect results, as a very small portion of typically 10 mg is investigated. The large surface to volume ratio of the sample cell may either favour (surface catalysed) or inhibit (chain radical) reactions.

### Test Report - Copy

This report shall not be reproduced except in full without the written approval of the testing laboratory. The energy content of mixtures already starting to react around ambient temperature will not be recorded quantitatively by the standard DSC method. In this case isothermal reaction calorimetric tests are recommended. According to TRAS 410 (German guideline for plant safety) the handling of thermally unstable material is considered safe, if the difference between the onset temperature and the maximum attainable process temperature is greater than 100 K. This safety margin*) can be decreased if there is enough knowledge for example about the activation energy and the sensitivity of the used DSC apparatus and if these facts are considered in a competent way. The safety margin is approximately equivalent with an adiabatic induction time of 24 hours. In general, this period leaves sufficient time for an incipient runaway to be detected and for counteraction to be taken. If storage of large amounts is considered, the time required for detection of and counteraction to disturbed process conditions may not be short compared to 24 h. In such cases, as well as with gassy systems, the safety margin must be increased significantly.

The rule fails in the case of self-accelerating reactions , where a safety margin of even 100 K may not be sufficient. The test result that a particular reaction shows no self-accelerating behavior in isothermal DSC measurements is only valid for periods of approx. one day. Weak self-accelerating reactions which may be safety relevant for long-term storage will not be detected using this method. The decision whether further measurements (adiabatic calorimetry, reaction calorimetry with larger samples) have to be made, depends on a comparison of the temperature region of the observed exothermic event and its magnitude together with the intended process conditions. According TRAS 410 an exotherm of less than 100 J/g, which is equivalent to an adiabatic temperature rise of about 50 K, will generally present no safety problem. From experience, reactions with an energy content of less than 200 J/g may be considered as safe, if the process is open to atmosphere or an appropriate venting system is present. Exothermal reactions with an energy release below 200 J/g will not be tested for selfaccelerating behaviour. According to transportation regulations further tests are required if the decomposition energy is greater than 300 J/g. According to handling regulations further tests are required if the decomposition energy is greater than 500 J/g. *) The former stated safety margin of 50 K referred to usual activation energies and onset temperatures less than 200 °C.