If other methods or test procedures are used to verify the conditions of stability prescribed above in this section, those methods shall lead to the same findings as could be reached by the methods specified below.
In carrying out the stability tests by heating described below, the temperature of the oven containing the sample under test shall not deviate by more than 2 °C from the prescribed temperature; the prescribed duration of a 30-minute or 60-minute test shall be observed to within two minutes. The oven shall be such that the required temperature is restored not more than five minutes after insertion of the sample.
Before undergoing the tests in 2.3.2.9 and 2.3.2.10, the samples shall be dried for not less than 15 hours at the ambient temperature in a vacuum desiccator containing fused and granulated calcium chloride, the sample substance being spread in a thin layer; for this purpose, substances which are neither in
powder form nor fibrous shall be ground, or grated, or cut into small pieces. The pressure in the desiccator shall be brought below 6.5 kPa (0.065 bar).
Before being dried as prescribed in 2.3.2.6 above, substances conforming to 2.3.2.2 shall undergo preliminary drying in a well-ventilated oven, with its temperature set at 70 °C, until the loss of mass per quarter-hour is less than 0.3% of the original mass.
Weakly nitrated nitrocellulose conforming to 2.3.2.1 shall first undergo preliminary drying as prescribed in 2.3.2.7 above; drying shall then be completed by keeping the nitrocellulose for at least 15 hours over concentrated sulphuric acid in a desiccator.
Test of chemical stability under heat
(a) Test of the substance listed in paragraph 2.3.2.1 above.
(i) In each of two glass test tubes having the following dimensions:
length 350 mm
internal diameter 16 mm
thickness of wall 1.5 mm
is placed 1 g of substance dried over calcium chloride (if necessary the drying shall be
carried out after reducing the substance to pieces weighing not more than 0.05 g each).
Both test tubes, completely covered with loose-fitting closures, are then so placed in an
oven that at least four-fifths of their length is visible, and are kept at a constant
temperature of 132 °C for 30 minutes. It is observed whether nitrous gases in the form of
yellowish-brown fumes clearly visible against a white background are given off during
this time;
(ii) In the absence of such fumes the substance is deemed to be stable;
(b) Test of plasticized nitrocellulose (see 2.3.2.2)
(i) 3 g of plasticized nitrocellulose are placed in glass test tubes, similar to those referred to
in (a), which are then placed in an oven kept at a constant temperature of 132 °C;
(ii) The test tubes containing the plasticized nitrocellulose are kept in the oven for one hour.
During this time no yellowish-brown nitrous fumes (nitrous gases) shall be visible.
Observation and appraisal as in (a).
Ignition temperature (see 2.3.2.1 and 2.3.2.2)
(a)The ignition temperature is determined by heating 0.2 g of substance enclosed in a glass test tubeimmersed in a Wood's alloy bath. The test tube is placed in the bath when the latter has reached100 °C. The temperature of the bath is then progressively increased by 5 °C per minute;
(b)The test tubes must have the following dimensions:length125 mminternal diameter15 mmthickness of wall 0.5 mmand shall be immersed to a depth of 20 mm;
(c)The test shall be repeated three times, the temperature at which ignition of the substance occurs,i.e., slow or rapid combustion, deflagration or detonation, being noted each time;
(d)The lowest temperature recorded in the three tests is the ignition temperature.
Tests relating to flammable liquids of Classes 3, 6.1 and 8
Determination of flash-point
The following methods for determining the flash-point of flammable liquids may be used:
International standards:
ISO 1516 (Determination of flash/no flash –Closed cup equilibrium method)
ISO 1523 (Determination of flash point –Closed cup equilibrium method)
ISO 2719 (Determination of flash point –Pensky-Martens closed cup method)
ISO 13736 (Determination of flash point –Abel closed-cup method)
ISO 3679 (Determination of flash point –Rapid equilibrium closed cup method)
ISO 3680 (Determination of flash/no flash –Rapid equilibrium closed cup method)
National standards:
American Society for Testing Materials International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, Pennsylvania, USA 19428-2959:
ASTM D3828-07a, Standard Test Methods for Flash Point by Small Scale Closed-Cup Tester
ASTM D56-05, Standard Test Method for Flash Point by Tag Closed-Cup Tester
ASTM D3278-96(2004)e1, Standard Test Methods for Flash Point of Liquids by Small Scale Closed-Cup Apparatus
ASTM D93-08, Standard Test Methods for Flash Point by Pensky-Martens Closed-Cup Tester
Association française de normalisation, AFNOR, 11, rue de Pressensé, F-93571 La Plaine Saint-Denis Cedex:
French standard NF M 07 -019
French standards NF M 07 -011 / NF T 30 -050 / NF T 66 -009
French standard NF M 07 -036
Deutsches Institut für Normung, Burggrafenstr. 6, D-10787 Berlin:
Standard DIN 51755 (flash-points below 65 °C)
State Committee of the Council of Ministers for Standardization, RUS-113813, GSP, Moscow, M-49Leninsky Prospect, 9:
GOST 12.1.044-84
To determine the flash-point of paints, gums and similar viscous products containing solvents, only
apparatus and test methods suitable for determining the flash-point for viscous liquids shall be used, in
accordance with the following standards:
(a) International Standard ISO 3679: 1983;
(b) International Standard ISO 3680: 1983;
(c) International Standard ISO 1523: 1983;
(d) International standards EN ISO 13736 and EN ISO 2719, Method B.
The standards listed in 2.3.3.1.1 shall only be used for flash-point ranges which are specified therein. The possibility of chemical reactions between the substance and the sample holder shall be considered when selecting the standard to be used. The apparatus shall, as far as is consistent with safety, be placed in a draught-free position. For safety, a method utilizing a small sample size, around 2 ml, shall be used for organic peroxides and self-reactive substances (also known as "energetic" substances), or for toxic substances.
When the flash-point, determined by a non-equilibrium method is found to be 23 ± 2 °C or 60 ± 2 °C, it shall be confirmed for each temperature range by an equilibrium method.
In the event of a dispute as to the classification of a flammable liquid, the classification proposed by the consignor shall be accepted if a check-test of the flash-point, yields a result not differing by more than 2 °C from the limits (23 °C and 60 °C respectively) stated in 2.2.3.1. If the difference is more than 2 °C, a second check-test shall be carried out, and the lowest figure of the flash-points obtained in either check-test shall be adopted.
Determination of initial boiling point
The following methods for determining the initial boiling point of flammable liquids may be used:
International standards:
ISO 3924 (Petroleum products – Determination of boiling range distribution – Gas chromatography method)
ISO 4626 (Volatile organic liquids – Determination of boiling range of organic solvents used as raw materials)
ISO 3405 (Petroleum products – Determination of distillation characteristics at atmospheric pressure)
National standards:
American Society for Testing Materials International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, Pennsylvania, USA 19428-2959:
ASTM D86-07a, Standard Test Method for Distillation of Petroleum Products at Atmospheric Pressure
ASTM D1078-05, Standard Test Method for Distillation Range of Volatile Organic Liquids
Further acceptable methods:
Method A.2 as described in Part A of the Annex to Commission Regulation (EC) No 440/20081.
________________
1 Commission Regulation (EC) No 440/2008 of 30 May 2008 laying down test methods pursuant to Regulation (EC) No 1907/2006 of the European Parliament and of the Council on the Registration, Evaluation, Authorisation and Restriction of Chemicals (REACH) (Official Journal of the European Union, No. L 142 of 31.05.2008, p.1-739 and No. L 143 of 03.06.2008, p.55).