Decree No. 164 / 2004 Coll.
Decree laying down basic methods for the testing of hazardous properties of chemicals and chemical preparations with regard to flammable and oxidative properties
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164
DECLARATION
of 31 March 2004
laying down the basic methods for testing the hazardous properties of chemicals and chemical preparations with regard to flammable and oxidative properties
According to § 8 (5) (a) of Act No 356 / 2003 Coll., on Chemicals and Chemical Products and on the amendment of certain other laws, hereinafter referred to as "the Act":
This Decree sets out basic methods (hereinafter referred to as "methods') for the testing of hazardous properties of chemicals (hereinafter referred to as" substances') and chemical preparations (hereinafter referred to as "preparations') with regard to flammable and oxidative properties which are classified in accordance with § 2 (5) (b) to (e) of the Act and specific legislation.
(1) Methods for the testing of hazardous properties of substances and preparations with regard to flammable properties and oxidising capacity shall be carried out to detect:
(a) flash points;
(b) flammable substances and preparations;
(c) flammable gases;
(d) the flammable properties of substances and preparations which react with water for the development of flammable gases;
(e) pyrophoric properties of solids and liquid substances and preparations,
(f) ignition temperatures of liquid and gaseous substances and preparations;
(g) relative ignition temperatures of solids and preparations;
(h) the oxidative properties of solids and preparations; and
(i) the oxidation properties of liquids.
(2) The methods are set out in the Annex.
Decree No. 85 / 1999 Coll., laying down methods for the detection of flammable substances and oxidising properties of chemicals and chemical preparations, is hereby repealed.
This decree shall take effect on the date of the entry into force of the Treaty of Accession of the Czech Republic to the European Union.
Minister:
Mgr. Gross v. r.
Annex to Decree No 164 / 2004 Coll.
Methods for testing hazardous properties of substances and preparations in terms of flammable and oxidative capacity
I. METHODS FOR DETERMINING THE EXAMINATION POINT - Method A.9 taken from the Annex to Commission Directive 92 / 69 / EEC of 31 July 1992 adapting for the seventeenth time to technical progress Council Directive 67 / 548 / EEC on the approximation of laws, regulations and administrative provisions relating to the classification, packaging and labelling of dangerous substances (hereinafter referred to as "the Directive")
I. 1 INTRODUCTION
These methods are applied to liquids whose vapours can be ignited.
In order to ensure safety, it is necessary to have information on the flammable properties of the substance or preparation.
The choice of the method for determining the flash point shall take into account the possibility of chemical reaction between the substance and the test cup.
I. 2 DEFINITIONS AND UNIT
The flash point is the lowest temperature t (° C) corrected to a pressure of 101,325 kPa, at which the liquid releases vapours in such a quantity under conditions defined in the test methods, in a test cup when mixed with air. For the conversion of absolute temperature T (K) to ° C the relationship: t = T - 273,15.
I. 3 REFERENCE SUBSTANCES
Reference substances shall be used to periodically check the correct implementation of the method, where appropriate, to compare with the results of other methods or to verify the accuracy of the measured result for the new substance or preparation.
I. 4 PRINCIPLE OF METHODS
The substance or preparation shall be placed in a test cup in which it is heated or cooled to the test temperature according to the procedure described in the individual test method. In order to determine whether or not the sample ignites at the test temperature, the tests shall be carried out by ignition.
I. 5 QUALITATIVE CRITERIA METHOD
I. 5.1 The reproducibility of the method varies according to the flash point range and test methods used; not more than 2 ° C.
I. 5.2 The applicability of the method for determining the flash point is defined by a certain span of the flash point and data relating to the substance or preparation as the subject of the test (e.g. high viscosity).
I. 6 DESCRIPTION OF THE METHOD
I. 6.1 A sample of the test substance or preparation is inserted into the test apparatus in accordance with section I.6.1 or I.6.3.2. From a safety point of view, approximately 2 cm3 is recommended for toxic substances or preparations and / or high calorific substances or products.
I.6.2 The test equipment shall be placed in a draught-free area where the leakage of harmful substances does not endanger the operator's health.
I. 6.3 Types of test methods
I. 6.3.
ISO 1516 Determination will ignite / not ignite. Steady method of closed cup.
ISO 3680 Determination will ignite / not ignite. Quick equilibrium method of a closed cup.
ISO 1523 Determination of flash point. Steady method of closed cup.
ISO 3679 Determination of flash point. Quick equilibrium method of a closed cup.
I.6.2 Unbalanced test methods
Abel test equipment:
BS 2000 - Part 170 Flame point by Abel,
NF M 07-011 Flammable liquids. The flash point by means of the closed cup device according to Abel,
NF T 66-009 The point of ignition of bitumens by a closed cup machine according to Abel,
Abel-Pensky test equipment:
EN 57 Petroleum products. Determination of flash point with closed cup according to Abel-Pensky,
DIN 51 755 - Part 1 (for temperatures from 5 ° C to 65 ° C) Testing of mineral oils and other flammable liquids. Determination of flash point in closed cup by Abel-Pensky method,
DIN 51 755 - Part 2 (for temperatures below 5 ° C) Testing of mineral oils and other flammable liquids. Determination of flash point in closed cup by Abel-Pensky method,
NF M 07-036 Flammable liquids. The flash point by the Abel-Pensky method in a closed cup,
Taga test equipment:
ASTM D 56 Standard test method for flash point by a closed cup instrument according to Taga
Test equipment according to Pensky - Martens:
ISO 2719 Determination of flash point. Method of closed cup according to Pensky - Martens,
DIN 51 758 Testing of mineral oils and other flammable liquids. Determination of flash point in closed cup by Pensky - Martens method
ASTM D 93 Standard test method for flash point with closed cup according to Pensky - Martens,
BS 2000- 34 Flash point closed by Pensky-Martens cup,
NF M 07-019 Flammable liquids. Determination of flash points above 50 ° C by means of a closed cup device according to Pensky - Martens.
Note:
If the flash-point value determined by the unequilibrium method in point I.6.3.2 is within the range (0 ± 2) ° C, (21 ± 2) ° C or (55 ± 2) ° C, the equilibrium method shall be confirmed on the same test device. 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 (e.g. colours, adhesives) containing solvents may be used for determining the flash point of viscous liquids: ISO 3679, ISO 3680, ISO 1523 and DIN 53 213 - Part 1 Testing of paints, varnishes and similar products containing solvents.
Determination of flash point using a closed cup.
If the above technical standards are issued as CSN, they may also be used to determine the flash point.
I. 7 INTRODUCTION RESULTS
The test report shall contain the following information:
(a) the precise identification of the substance or preparation, including the indication of the impurities contained;
(b) the reference to the method used and the indication of any deviations;
(c) the results and any other data relevant to the interpretation of the results (e.g. the contracting entity of the test, the method of sampling, the date of the test which performed the test).
II. METHODOLOGY FOR DETERMINATION OF FULL SUBSTANCES AND PRODUCTS - Method A.10 of the Directive
II. 1 INTRODUCTION
This method is used only for powdered, granular and pasteurised substances and preparations.
Information on their explosive properties shall be obtained before the test of the substance or preparation is started. At the same time, it is necessary to provide a suitable extinguishing agent with regard to the difficult extinguishing of radiant metals or metal alloys.
II. 2 DEFINITIONS OF FIXING AND UNIT
The burning time is the time at which 100 mm of the sample is burned under test conditions; Expresses in seconds (s).
The burning rate is expressed in millimetres per second by the length of the burnt sample and calculated from the burning time; is expressed (mm.s-1).
II. 3 PRINCIPLE OF METHODS
The substance or preparation shall be formed into an intact tape or powder caterpillar of 250 mm length. 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 burning time specified in Article II (4) is extended to 200 mm of the length of the test sample, a proper test shall be performed to determine the burning rate.
II. 4 PREVIOUS ORIENTATION TEST
The substance or preparation shall be formed into an intact tape or powder caterpillar of 250 mm length, 20 mm width and 10 mm height on a non-flammable, non-porous and low thermal conductive backing plate. At one 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 not more than 2 minutes or 5 minutes for metal or metal alloy dust. It shall be determined whether the burning is extended to 200 mm of test sample length over a test period of 4 minutes or 40 minutes for metallic dust. If the substance or preparation is not lit and burning either by flame or ignition does not extend to 200 mm of test sample length within 4 minutes or 40 minutes for metallic dust, it cannot be considered highly flammable and no further test is required. If the burning of the powder spreads to 200 mm in length over a period of less than 4 minutes or 40 minutes for metal dust, the test described below shall be carried out.
II.5 PREPARATION, CONDITIONS AND IMPLEMENTATION OF THE FIRE TEST
II. 5.1 Powdered or granular substances or preparations shall be freely poured into a 250 mm shape with triangular cross-section of an internal height of 10 mm and a width of 20 mm. The two metal plates of the frame with the base shall be fixed to both longitudinal sides of the form as side walls 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 is removed and the excess substance or preparation 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. Paste substances or preparations shall be spread over a 250 mm length rope with a cross-section of approximately 1 cm2 on a non-flammable, non-porous and low thermal conductive plate.
II. 5.2 For a moisture sensitive substance or preparation, the test shall be carried out as quickly as possible after removal from the container.
II5.3 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 change during the test. A protective curtain against draught shall be installed around the test equipment. The sample is ignited at one end. A flame of a gas burner with a mouthpiece diameter of 5 mm or more is used to ignite the test sample. 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, with the help of a clean and cool plate, unless a positive result has previously been found.
II.6 DATA FOR EVALUATION OF TEST RESULTS
For evaluation, the burning time from the preliminary indicative test referred to in point II.4 and the shortest burning time or maximum burning rate from the six tests referred to in point II.5 are significant.
II. 7 INTRODUCTION RESULTS
The test report shall contain the following information:
(a) the precise identification of the substance or preparation, including the indication of the impurities contained;
(b) the reference to the method used and the indication of any deviations;
(c) a description of the test substance or preparation, its physical state, including moisture content;
(d) results from the preliminary indicative test and from the burning rate test and any other data relevant to the interpretation of the results (e.g. the contracting authority of the test, the sampling method, the date of the test which performed the test).
II. 8 INTERPRETATION OF RESULTS
Powdered, grained or pasteurised substances or preparations shall be considered to be highly flammable if the burning time in each test carried out in accordance with point II.5 is less than 45 s or the burning speed is greater than 2,2 mm.s-1 Metal or metal alloy powder shall be considered as highly flammable when it can be ignited and the flame or reaction zone spread over the whole test sample for a period of less than or equal to 10 minutes.
Figure 1
Form and accessories (frame and base) for preparing the test sample (all dimensions are in millimetres)
III. METHOD FOR DETERMINING GAS FLOW - Method A.11 of the Directive
III. 1 INTRODUCTION
The combustion of gases shall be determined by this method by establishing whether gases mixed with air at room temperature (approximately 20 ° C) and atmospheric pressure are explosive and in what 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.
III. 2 DEFINITIONS AND SINGLE FIELDS OF EXPLOSITY AND BETWEEN EXPLOSIVES
The explosive area is a range of concentrations of flammable gas mixed with air between the lower and upper limits of the explosive; is expressed as volume percentage (% vol.). The lower and upper limits of the explosive are those limiting concentrations below which and over which the flame propagation does not occur under test conditions; are expressed in volume percentages (% vol.).
III. 3 PRINCIPLE OF METHODS
The concentration of gas in the mixture with air is gradually increased and at each step the mixture is ignited by an electric spark.
III. 4 PREPARATION, CONDITIONS AND IMPLEMENTATION OF THE TEST
III. 4.1 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 continuous induction spark of 0,5 s is used as the ignition source, generated from a high voltage transformer with an output voltage of between 10 kV and 15 kV with a maximum power input of 300 W.
III. 4.2 The test shall be carried out at room temperature.
III 4.3 A gas with a known concentration contained in a mixture with air is driven by a dosing pump into a glass cylinder. When igniting a mixture, it shall be monitored whether the flame breaks away from the ignition source and whether it spreads spontaneously. The gas concentration increases with a 1% v / v step until the ignition described above occurs.
If the chemical structure of the gas indicates that it could be non-flammable and can calculate the stoichiometric composition of the mixture with air, it is sufficient to test the mixtures only between 10% and 10% lower than the stoichiometric concentration and 10% higher than the stoichiometric concentration with a step of 1% vol.
III. 5 DATA FOR EVALUATION OF TEST RESULTS
The occurrence of flame propagation is the only important indication for determining the accelerability of the gas.
IMPLEMENTATION RESULTS
The test report shall contain the following information:
(a) the precise identification of the substance or preparation, including the indication of the impurities contained;
(b) the reference to the method used and the indication of any deviations;
(c) a description of the test substance or preparation, its physical state, including moisture content;
(d) a description of the test equipment used and its dimensions;
(e) temperature and atmospheric pressure at which the test was carried out;
(f) the test concentrations and results obtained in each step;
(g) test result of "non-flammable gas" or "highly flammable gas";
(h) a concentration range which has been tested with a step of 1% vol; if it is concluded that the gas is non-flammable,
(i) any other data relevant to the interpretation of the results (e.g. the test contracting entity, the method of sampling, the date of the test which performed the test).
IV. METHOD FOR DETERMINING THE HOSSITY OF SUBSTANCES AND WATER REAGENTS FOR THE DEVELOPMENT OF GAS - Method A.12 of the Directive
IV. 1 INTRODUCTION
This method is intended for solids and liquid substances and preparations. It is not intended for substances or preparations that spontaneously ignite when they come into contact with air.
This method is used to determine the reaction of a substance or preparation with water or air humidity if it leads to the development of dangerous quantities of gas or gases which may be highly flammable.
IV. 2 DEFINITIONS AND SINGLE COLLECTION OF SUBSTANCES OR PRODUCTS
Highly flammable substances or preparations are substances or preparations which, when in contact with water or air humidity, release highly flammable gases in dangerous quantities at a rate of at least 1 dm3 per kg of substance or preparation per 1 hour.
IV.3 PRINCIPLE OF METHODS
The substance or preparation shall be tested in the following steps:
IV. 3.1 Step 1
The test substance or preparation shall be placed in a container of distilled water at a temperature of 20 ° C and shall be monitored for ignition.
IV. 3.2 Step Two
The test substance or preparation shall be placed on filter paper floating on the surface of distilled water at a temperature of 20 ° C in the container and shall be monitored for ignition of the released gas. In order to increase the potential for ignition, the substance is to be placed in one place only.
IV. 3.3 Step Three
The test solid or preparation shall be formed 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.
IV. 3.4 Step 4
The test substance or preparation shall be mixed with distilled water at a temperature of 20 ° C and measured at one hour intervals for 7 hours. If the rate of gas development is irregular or increases after seven 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.
If an ignition step occurs, further test steps shall not be carried out. If the substance or preparation does not react rapidly, follow IV.
IV. 4 PREPARATION, CONDITIONS AND IMPLEMENTATION OF TESTS
IV. 4.1 Step 1
IV, 4.1 The test shall be carried out at room temperature.
IV. A small amount of the test substance or preparation (approximately 4 mm3) shall be placed in a distilled water container and monitored for release of any gas and ignition.
If gas ignition is set, further tests are no longer necessary and the substance or preparation is considered highly flammable.
IV. 4.2 Step Two
IV. The test equipment consists of a suitable container, e.g. a laboratory evaporation bowl approximately 100 mm in diameter, with distilled water and filter paper on the surface.
IV4.2 The test shall be carried out at room temperature.
IV. A small amount of the test substance or preparation (approximately 4 mm3) is inserted into the centre of the filter paper and it is monitored whether any gas is released and ignited. If gas ignition is set, further tests are no longer necessary and the substance or preparation is considered highly flammable.
IV. 4.3 Step Three
IV. The test shall be carried out at room temperature.
IV. The test solid or preparation shall be adjusted to the shape of a cylinder approximately 2 cm high and a diameter of approximately 3 cm high with a propagation at the top. A few drops of water shall be added to the sample and it shall be observed that the gas is developed and ignited. If gas ignition is set, further test steps shall not be carried out and the substance or preparation shall be considered highly flammable.
IV. 4.4 Step 4
IV. The assembly of the test equipment is shown in Figure 2.
IV. The container with the test substance or preparation shall be checked for dust with a particle size below 500 μm. If this dust constitutes more than 1% by weight of content (% by weight) or if the sample is crumbled, all the substance or preparation shall be ground to dust before the test. Otherwise, the substance or preparation shall be tested in its original form.
IV. The test shall be carried out at room temperature and atmospheric pressure.
IV. The drip funnel of the test equipment shall be filled with 10 cm3 to 20 cm3 water and 10 g conical flask. The faucet of the drip funnel opens and simultaneously begins to measure the time The volume of gas generated shall be measured every hour for seven 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 it is not known whether the mixture is highly flammable, a mixture of the same composition shall be prepared and the test shall be carried out according to method III.
IV. 5 DATA FOR EVALUATION OF TEST RESULTS
A substance or preparation is considered highly flammable if:
(a) spontaneous ignition occurs at any step of the test procedure; or
(b) if the flammable gas is produced at a rate exceeding 1 dm3 per kg of substance per hour.
IV. 6 INTRODUCTION RESULTS
The test report shall contain the following information:
(a) the precise identification of the substance or preparation, including the indication of the impurities contained;
(b) the reference to the method used and the indication of any deviations;
(c) the temperature at which the test was carried out;
(d) details of each initial preparation of the test substance or preparation;
(e) the results of the test steps carried out;
(f) the chemical identity of the gas released;
(g) the rate of gas development when step 4 is performed as described in section 1.6.4,
(h) all other data relevant to the interpretation of the results (e.g. the sponsor of the test, the method of sampling, the date of the test which performed the test).
Figure 2
Test equipment
V. METHOD FOR DETERMINING THE PYROFORTIC PROPERTIES OF FULL AND CAPABLE SUBSTANCES AND PRODUCTS - Method A.13 of the Directive
V. 1 INTRODUCTION
This method is intended for solid and liquid substances or preparations which, in small quantities, spontaneously ignite shortly after contact with air at room temperature.
This method does not apply to substances or preparations which are required to ignite the air at room temperature (about 20 ° C) or at a higher temperature for several hours or days.
V. 2 DEFINITIONS OF THE PYROFORTIC SUBSTANCE OR PRODUCT
Pyrophoric are substances or preparations if they spontaneously ignite or cause carbon leakage within 5 minutes under the conditions described in section V. 3. If a specific ignition temperature value needs to be known from a safety point of view, this shall be determined according to Method VI.
V. 3 PRINCIPLE OF METHODS
The substance or preparation shall be applied on an inert carrier and exposed to air at room temperature for 5 minutes. If the liquid or preparation does not ignite, it is subsequently absorbed into dry filter paper and exposed to air for 5 minutes at room temperature.
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Regulation Information
| Citation | Decree No. 164 / 2004 Coll., laying down the basic methods for testing the hazardous properties of chemicals and chemical preparations with regard to flammable and oxidative properties |
|---|---|
| Regulation Type | Order |
| Author | - |
| Collection | Code of Laws |
| Date of Promulgation | 14.04.2004 |
|---|---|
| Effective from | 01.05.2004 |
| Effective until | - |
| Status | Valid |
The regulation text is for informational purposes only.
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