Decree of the Ministry of Interior No. 85 / 1999 Coll.
Decree of the Ministry of the Interior laying down methods for the detection of flammable and oxidising properties of chemicals and chemical preparations
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85
DECLARATION
Ministry of Interior
of 16 April 1999
laying down methods for the detection of flammable and oxidising properties of chemicals and chemical preparations
According to Article 4 (1) (b) of Act No. 157 / 1998 Coll., on Chemicals and Chemical Products and on the amendment of certain other laws, hereinafter referred to as "the Act":
This Decree sets out the methods by which tests are carried out to detect the flammable and oxidising properties of hazardous chemicals and chemicals referred to in § 2 (8) (b) to (e) of the Act. The methods are set out in the Annex and their numerical labelling is made following the numerical labelling of methods for the detection of toxicity of chemicals and chemical products and for the detection of the properties of chemicals and chemical products dangerous to the environment as laid down in specific legislation. 1)
This Decree shall take effect on 1 July 1999.
Minister:
PhDr. Grulich v. r.
Annex to Decree No 85 / 1999 Coll.
Methods for detecting flammable and oxidising properties of chemicals and chemical preparations
A. 9.
1 METHOD
1.1 Introduction
Prior to the start of the test, the test worker should have at his disposal preliminary information on the flammable properties of the substance.
The test procedure shall be applied to liquids whose vapours can be ignited by ignition sources.
The test methods listed in this text are only reliable for the flash point range specified in each method.
The choice of the method to be used shall consider the possibility of chemical reactions between the substance and the test cup.
1.2 Definitions and units
The flash point is the lowest temperature corrected to the pressure of 101,325 kPa at which the liquid releases the explosive mixture under the conditions defined in the test method of steam in such a quantity that it is formed by air in the test vessel.
Temperature units:
result from the relationship t = T - 273,15,
where t is in ° C and T is in Kelvin (K).
1.3. Reference substances
Reference substances need not be used in all cases when a new substance is tested. Reference substances are primarily used for periodic control of the correct implementation of the method and allow comparison with the results of other methods.
1.4. Principle of method
The substance is placed in a test vessel in which it is heated or cooled to a test temperature according to the procedure described in each test method. In order to determine whether or not the sample ignites at this temperature, ignition tests shall be carried out.
1.5. Quality criteria
1.5.1 Repeatability limit (r)
The repeatability limit is changed according to the flash point range and the test method used. The maximum is 2 ° C.
1.5.2. Sensitivity
Sensitivity depends on the test method used.
1.5.3. Specification
The test methods determine the span of the flash point, the subject of the test and the data related to the substance (e.g. high viscosity).
1.6. Description of method
1.6.1 Preparation
A sample of the test substance shall be inserted into the test apparatus in accordance with 1.6.3.1 or 1.6.3.2. From a safety point of view, it is recommended to apply a method using a small sample of approximately 2 cm3 for toxic substances or high calorific substances.
1.6.2. Test conditions
The test equipment shall be placed in accordance with the working safety requirements at a place where there is no excessive air flow.
1.6.3. Perform the test
1.6.3.1. Steady method
The determination of the flash point is described in detail in ISO 1516, ISO 3680, ISO 1523, ISO 3679 (EN 456).
1.6.3.2. Unbalanced methods
- Abel test equipment: determination of flash point is described in detail in BS 2000 - Part 170 (BS EN ISO 13 736), NF M 07-011, NF T 66-009 and ISO 13 736 (CSN EN ISO 13 736),
- Abel-Pensky test equipment: determination of flash point is detailed in EN 57 (EN 57), DIN 51 755 - Part 1 (for temperatures from 5 to 65 ° C), DIN 51 755 - Part 2 (for temperatures below 5 ° C), (CSN 65 6065, Method B) and NF M 07- 036,
- TAGa test equipment: determination of flash point is detailed in ASTM D 56,
- Pensky-Martense test equipment: the determination of the flash point is detailed in ISO 2719 (CSN EN 22 719), DIN 51 758, ASTM D 93, BS 200-34 (BS EN 22 719) and NF M 07-019.
Notes:
If the flash-point value determined by the imbalance method according to 1.6.3.2 is within the range (0 ± 2) ° C, (21 ± 2) ° C or (55 ± 2) ° C, the equilibrium method shall be confirmed by the same test equipment. The same procedure is recommended for the range (100 ± 2) ° C and (250 ± 2) ° C, i.e. for flammable liquids III and IV hazard classes according to ČSN 65 0201. If the classification is contested, e.g. if more than 2 ° C differs, a new control test shall be carried out and the lowest value of the flash point detected shall be considered decisive. Only those methods that can reach flash-point temperatures are used for notification.
Only test equipment and test methods suitable for determining the flash point of viscous liquids (colours, adhesives, etc.) containing solvents may be used to determine the flash point of viscous liquids: ISO 3679 (ČSN EN 456), ISO 3680, ISO 1523 and DIN 53 213 - Part 1 (ČSN 67 3015).
In determining the flash point according to this method, the applicable test standard shall be used.
2 PARTICULARS
For the evaluation of a substance or preparation, the value of the flash point determined in accordance with 1.6.3 is decisive.
3 PROTOCOL ON TEST AND INTERPRETATION OF RESULTS
The test report shall contain the following known data:
- precise specification of the substance (identification and impurities),
- reference to the test method used and to any possible deviation from the specified test procedure,
- the date of the test,
- the results and any additional comments that are important and necessary to interpret the results.
A. 10. HOSTERY OF THE LIVE SUBSTANCES
1 METHOD
1.1 Introduction
Before starting the test, the test worker should have at his disposal preliminary information on the potential explosive properties of the substance.
This test method is used only for powdered, granular or grazing substances. In order not to consider all substances that can be ignited as highly flammable but only those that burn rapidly or whose burning behaviour is particularly dangerous in some way, only those for which the burning rate exceeds the limit value are considered to be highly flammable.
The spread of burning can be particularly dangerous by burning metal dust for its difficult extinguishing. Metal money is considered to be highly flammable if the ignition is extended by its specific mass for the prescribed time (1.6.1 and 1.6.2.3).
1.2 Definitions and units
The burning time shall be expressed in seconds and the burning rate in millimetres per second.
1.3. Reference substances
They're not intended.
1.4. Principle of method
The substance is formed into an intact tape or powder caterpillar with a length of 250 mm. A preliminary indicative test shall be carried out to determine whether the flame propagation or ignition occurs after igniting the test sample with a gas burner flame. If the combustion is extended to 200 mm of its length over the prescribed period, a proper test shall be performed to determine the burning rate.
1.5. Quality criteria
Not intended.
1.6. Description of method
1.6.1 Preliminary indicative test
The substance is formed into an intact tape or powder caterpillar with a length of 250 mm, a width of 20 mm and a height of 10 mm on a non-flammable, non-porous and low thermal conductive backing plate.
At the end of the test sample, the flame of a gas burner with a minimum mouthpiece diameter of 5 mm shall be applied until the dust is ignited but no more than 2 minutes (5 minutes for metal or metal alloys). It shall be determined whether the burning spreads over 200 mm of test sample length over the test period for 4 minutes (or 40 minutes for metal dust). If the substance does not ignite and the burning does not spread either by flame or by burning 200 mm of the length of the test sample within 4 minutes (or 40 minutes for metallic dust) of the test period, it cannot be considered highly flammable and no further test is required. If the powder is spread over 200 mm over a period of less than 4 minutes (or 40 minutes for metallic dust), the test described below shall be performed.
1.6.2. Burning speed test
1.6.2.1 Preparation
Powdered or granular substances are freely poured into a 250 mm long form with a triangular cross-section of an internal height of 10 mm and a width of 20 mm. 2 metal plates of the frame with a base shall be fixed to both longitudinal sides of the form as sidewalls which extend 2 mm above the upper edge of the inner section (Figure 1). The product is then started three times from a height of 2 cm to a solid surface. If necessary, the form shall be subsequently supplemented. The frame will be removed and the excess material scraped off. A non-flammable, non-porous and low thermal conductive plate shall be placed on the top of the mould, the assembly shall be inverted and the mould removed. The traps shall be spread over a non-flammable, non-porous and low-heat conductive plate in the shape of a 250 mm rope and a cross-section of approximately 1 cm2.
1.6.2.2. Test conditions
In the case of a moisture sensitive substance, the test shall be carried out as quickly as possible after removal of the substance from the container.
1.6.2.3. Testing
The test sample shall be formed in the digestors perpendicular to the direction of withdrawal.
The flow rate of the exhaust air shall be sufficient to prevent the smoke leak to the laboratory and shall not be changed during the test. It is necessary to place protective curtains around the test equipment against excessive air flow.
A flame of a gas burner with a minimum mouth diameter of 5 mm shall be used to ignite the test sample at the end of the test. After burning 80 mm of test sample length, the burning rate shall be measured to a further 100 mm. The test shall be performed six times, each time using a clean and cold plate, unless a positive result has been found.
2 PARTICULARS
For evaluation, the burning time from the preliminary indicative test according to 1.6.1 and the shortest burning time or maximum burning rate from 6 tests according to 1.6.2.3 are important.
3 PROTOCOL ON TEST AND INTERPRETATION OF RESULTS
3.1 Test report
The test report shall contain the following known data:
- precise specification of the substance (identification and impurities),
- reference to the test method used and to any possible deviation from the specified test procedure,
- the date of the test,
- a description of the test substance, its physical state, including moisture content,
- results from the preliminary indicative test and from the burning rate test (if any), any other comments that are relevant and necessary for the interpretation of the results.
3.2 Interpretation of the result
Powdered, grained or pasteurised substances are considered to be highly flammable when the burning time in each test carried out according to the test procedure described in 1.6.2 is less than 45 seconds or the burning speed is greater than 2,2 mm.s-1. The dust of metals or metal alloys is considered to be highly flammable when it can be ignited and the flame or reaction zone spreads over the entire test sample in 10 minutes or less.
Figure 1
Form and accessories (frame and base) for preparing the test sample (all dimensions are in millimetres)
A. 11. GAS HOWEVER
1 METHOD
1.1 Introduction
This test method determines whether gases mixed with air at room temperature (approximately 20 ° C) and atmospheric pressure are explosive and, if so, in which concentration area. Mixtures which gradually increase the concentration of the test gas in the air are ignited by an electric spark. At the same time, it shall be observed that the gaseous mixture is ignited.
1.2 Definitions and units
The explosive area is a range of concentrations of flammable gas mixed with air between the lower and upper limits of the explosive. The lower and upper limits of the explosive are such limiting concentrations below and above which the flame will not spread.
1.3. Reference substances
They're not intended.
1.4. Principle of method
The concentration of the gas in the air is gradually increased and at each step the mixture is ignited by an electric spark.
1.5. Quality criteria
Not intended.
1.6. Description of method
The test is described in detail in NF T 20-041 Chemical products for industrial use - Determination of flammable gas (or CSN 65 0322 and CSN EN 720-2).
1.6.1. Test equipment
The test equipment consists of a vertical glass cylinder with a minimum inside diameter of 50 mm and a minimum height of 300 mm. The ignition electrodes are 3 mm to 5 mm apart and are located at a height of 60 mm above the cylinder floor. The cylinder is equipped with a pressurised safety fuse. The test equipment shall be provided with a cover to prevent any risk of explosion. A static induction spark is used as a ignition source, with a duration of 0,5 s, generated from a high voltage transformer with an output voltage of between 10 kV and 15 kV (maximum power input is 300 W).
1.6.2. Test conditions
The test is performed at room temperature (approximately 20 ° C).
1.6.3. Perform the test
A gas with a known concentration in the mixture with air is driven into the glass cylinder by a dosing pump. When igniting a mixture, it shall be monitored whether the flame is separated from the ignition source and whether it spreads spontaneously. The gas concentration shall be increased by 1% in degrees until the ignition described above occurs. If, according to the chemical composition and the structural formula of the gas, it appears that it could be non-flammable, and if it is possible to calculate the stoichiometric composition of mixtures with air, it is sufficient to test mixtures only within a range of 10% lower than stoichiometric concentration to a concentration of 10% higher than the stoichiometric degree of 1%.
2 PARTICULARS
The occurrence of flame propagation is the only relevant and necessary information to determine this property.
3 PROTOCOL ON TEST AND INTERPRETATION OF RESULTS
The test report shall contain the following known data:
- precise specification of the substance (identification and impurities),
- reference to the test method used and to any possible deviation from the specified test procedure,
- the date of the test,
- a description of the test equipment used with dimensions,
- the temperature at which the test was carried out,
- test concentrations and results obtained,
- test result: non-flammable gas or extremely flammable gas,
- a concentration range which has been tested with a step of 1% (if the gas is found to be non-flammable),
- all information and comments which are important and necessary for the interpretation of the results.
A. 12. HOSTACY OF SUBSTANCES REAGAINST WATER FOR THE DEVELOPMENT OF HOT GAS
1 METHOD
1.1 Introduction
This test method determines whether the reaction of a substance with water or air ingestion results in the development of dangerous quantities of gas or gases which may be highly flammable.
The test method is applicable to solids and liquids. It cannot be applied to substances that spontaneously ignite when they come into contact with air.
1.2 Definitions and units
Highly flammable substances are substances which, when in contact with water or air humidity, release highly flammable gases in dangerous quantities at a rate of at least 1 dm3 of 1 kg of this substance per hour.
1.3. Principle of method
The substance is tested in the sequence of successive steps described below. If an ignition step occurs, further tests are not necessary. If it is known that the water substance is not responding sharply, proceed according to 1.3.4.
Step 1
The test substance is carried into a rectangular container (tank) with distilled water at a temperature of 20 ° C and it is monitored whether or not the released gas ignites.
Step 2
The test substance shall be placed on filter paper floating on the surface of a bowl of distilled water at a temperature of 20 ° C and shall be monitored whether or not the released gas ignites. In order to increase the potential for ignition, the substance is to be placed only in 1 place of filter paper.
Step 3
The test solids shall be moulded into a cylinder of approximately 2 cm height and 3 cm diameter. A few drops of water are added to it to see if the released gas ignites or not.
1.3.4 Step 4
The test substance shall be mixed with distilled water at a temperature of 20 ° C and the gas development rate measured for 7 hours at one hour intervals. If the rate of gas development is irregular or increases after 7 hours, the measurement time shall be extended to a maximum of 5 days. The test may be interrupted if the rate of gas development exceeds 1 dm3 per kg of substance per hour during the measurement.
1.4. Reference substances
They're not intended.
1.5. Quality criteria
Not intended.
1.6. Description of method
The test is described in detail in NF T 20-040 Chemical products for industrial use - Determination of flammable gases resulting from hydrolysis of solid or liquid products.
Step 1
1.6.1.1. Test conditions
The test is performed at room temperature (approximately 20 ° C).
1.6.1.2. Testing
A small amount of the test substance (approximately 4 mm3) shall be introduced into the distilled water bowl and monitored for release of any gas and for ignition. If ignition occurs, further tests are no longer necessary and the substance is considered dangerous.
Step 2
1.6.2.1. Test equipment
The test equipment consists of a suitable container, e.g. a evaporation dish approximately 100 mm in diameter with distilled water and filter paper on the surface.
1.6.2.2. Test conditions
The test is performed at room temperature (approximately 20 ° C).
1.6.2.3. Testing
A small amount of the test substance (approximately 4 mm3) shall be placed in the centre of the filter paper and shall be monitored for release of any gas and for ignition. If ignition occurs, further tests are no longer necessary and the substance is considered dangerous.
1.6.3 Step 3
1.6.3.1. Test conditions
The test is performed at room temperature (approximately 20 ° C).
1.6.3.2. Perform the test
The test solids shall be adjusted to a cylindrical shape approximately 2 cm high and a diameter of approximately 3 cm at the top. A few drops of water are added to the test sample, while checking for gas development and ignition. If ignition occurs, further tests are no longer necessary and the substance is considered dangerous.
Step 4
1.6.4.1 Test equipment
The assembly of the test equipment is shown in Figure 2.
1.6.4.2. Test conditions
The test substance container shall be checked for dust with a particle size below 500 mm. If this dust is more than 1% of the content or when the sample is crumbled, all the substance shall be ground to dust before the test to take account of the reduction of particle size during transport and handling. Otherwise, the substance shall be tested in its original form. The test shall be carried out at room temperature (approximately 20 ° C) and atmospheric pressure.
1.6.4.3. Perform the test
The drip funnel of the test equipment shall be filled with 10 cm3 to 20 cm3 water and 10 g conical flask. The volume of gas released shall be measured by any appropriate means. The tap of the drip funnel opens, the water flows into the conical flask and simultaneously begins to measure the time (e.g. stoppers). The volume of gas generated shall be measured every hour for 7 hours. If the gas development is unstable during this period or the rate of development increases at the end of the test, the measurement shall be continued for 5 days. If during the measurement the rate of gas development exceeds 1 dm3 per kg of substance per hour, the test may be interrupted. The test shall be carried out three times.
If the chemical identity of the gas is unknown, a chemical analysis shall be carried out. If the gas contains highly flammable components and if it is not known whether the mixture is highly flammable, a mixture of the same composition shall be prepared and tested according to method A. 11.
2 PARTICULARS
A substance is considered dangerous if:
- spontaneous ignition occurs in any step of the test procedure, or
- if the flammable gas is produced at a rate of more than 1 dm3 per kg of substance per hour.
3 PROTOCOL ON TEST AND INTERPRETATION OF RESULTS
The test report shall contain the following known data:
- precise specification of the substance (identification and impurities),
Sign in for notes, favorites and notifications
Regulation Information
| Citation | Decree of the Ministry of the Interior No. 85 / 1999 Coll., laying down methods for the detection of flammable and oxidising properties of chemicals and chemical preparations |
|---|---|
| Regulation Type | Order |
| Author | - |
| Collection | Code of Laws |
| Date of Promulgation | 11.05.1999 |
|---|---|
| Effective from | 01.07.1999 |
| Effective until | - |
| Status | Valid |
The regulation text is for informational purposes only.
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