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-49
Leninsky 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).

 

Test for determining peroxide content

To determine the peroxide content of a liquid, the procedure is as follows:
A quantity p (about 5 g, weighed to the nearest 0.01 g) of the liquid to be titrated is placed in an
Erlenmeyer flask; 20 cm3 of acetic anhydride and about 1 g of powdered solid potassium iodide are
added; the flask is shaken and, after 10 minutes, heated for 3 minutes to about 60 °C. When it has
been left to cool for 5 minutes, 25 cm3 of water are added. After this, it is left standing for half an
hour, then the liberated iodine is titrated with a decinormal solution of sodium thiosulphate, no
indicator being added; complete discoloration indicates the end of the reaction. If n is the number of
cm3 of thiosulphate solution required, the percentage of peroxide (calculated as H2O2) present in the
sample is obtained by the formula:
17n
-------
100p

Test for determining fluidity

To determine the fluidity of liquid, viscous or pasty substances and mixtures, the following test
method shall be used.

Test apparatus

Commercial penetrometer conforming to ISO 2137:1985, with a guide rod of 47.5 g ± 0.05 g; sieve
disc of duralumin with conical bores and a mass of 102.5 g ± 0.05 g (see Figure 1); penetration vessel
with an inside diameter of 72 mm to 80 mm for reception of the sample.

Test procedure

The sample is poured into the penetration vessel not less than half an hour before the measurement.
The vessel is then hermetically closed and left standing until the measurement. The sample in the
hermetically closed penetration vessel is heated to 35 °C ± 0.5 °C and is placed on the penetrometer
table immediately prior to measurement (not more than two minutes). The point S of the sieve disc is
then brought into contact with the surface of the liquid and the rate of penetration is measured.

Evaluation of test results

A substance is pasty if, after the centre S has been brought into contact with the surface of the sample,
the penetration indicated by the dial gauge:
(a) after a loading time of 5 s ± 0.1 s, is less than 15.0 mm ± 0.3 mm; or
(b) after a loading time of 5 s ± 0.1 s, is greater than 15.0 mm ± 0.3 mm, but the additional
penetration after another 55 s ± 0.5 s is less than 5.0 mm ± 0.5 mm.
NOTE: In the case of samples having a flow point, it is often impossible to produce a steady level
surface in the penetration vessel and, hence, to establish satisfactory initial measuring conditions for
the contact of the point S. Furthermore, with some samples, the impact of the sieve disc can cause an
elastic deformation of the surface and, in the first few seconds, simulate a deeper penetration. In all
these cases, it may be appropriate to make the evaluation in paragraph (b) above.
 
Figure 1 – Penetrometer
Tolerances not specified are ± 0.1 mm.

Classification of organometallic substances in Classes 4.2 and 4.3

Depending on their properties as determined in accordance with tests N.1 to N.5 of the Manual of
Tests end Criteria, Part III, section 33, organometallic substances may be classified in Class 4.2 or 4.3,
as appropriate, in accordance with the flowchart scheme given in Figure 2.3.5.
NOTE 1: Depending on their other properties and on the precedence of hazard table
(see 2.1.3.10), organometallic substances may have to be classified in other classes as appropriate.
NOTE 2: Flammable solutions with organometallic compounds in concentrations which are not
liable to spontaneous combustion or, in contact with water, do not emit flammable gases in dangerous
quantities, are substances of Class 3.
 
Figure 2.3.5: Flowchart scheme for the classification of organometallic substances
in Classes 4.2 and 4.3ab
 
 
a If applicable and testing is relevant, taking into account reactivity properties, class 6.1 and 8 properties should
be considered according to the precedence of hazard table of 2.1.3.10.
b Test methods N.1 to N.5 can be found in the Manual of Tests and Criteria, Part III, Section 33.

 

3

Dangerous goods list, special provisions and exemptions related to limited and excepted quantities

3.1

GENERAL

Previous Matter Next Matter

adrbook.com - Copyright all rights reserved. © 2015-2018