GB/T 39093-2020.Heat accumulation storage test method for dangerous goods.
1 Scope
GB/T 39093 specifies the test principle, safety measures, test equipment, test procedures, result evaluation and test report for the heat accumulation storage test of dangerous
goods. GB/T 39093 is applicable to the heat accumulation storage test of dangerous goods.
2 Terms and definitions
The following terms and definitions apply to this document.
2.1
Self-accelerating decomposition temperature; SADT
The lowest ambient temperature at which self-accelerating decomposition of a substance may occur in the container used for transportation.
[GB/T 21178-2009,3.3]
3 Test Principle
According to the Semenov Theory of thermal explosion, the main resistance to heat flow propagation in a thermal runaway system is concentrated on the container wall. Therefore, a Dewar flask with a small volume but large thermal resistance of the container wall is used to simulate the thermal environment in which a large volume of dangerous goods undergoes self-accelerating decomposition. It is used to determine the lowest constant ambient temperature for self-accelerating decomposition of dangerous goods in containers, including medium bulk containers and small tanks with a volume of less than 2m3, i.e., the self-accelerating decomposition temperature. The effectiveness of the test depends on whether the heat loss rate per unit mass of the selected Dewar flask is similar to the heat loss rate per unit mass of the packaging used for dangerous goods.
4 Safety Measures
4.1 Safety precautions should be taken during the test to avoid catastrophic accidents caused by failure of the test container, and to avoid the escape of toxic decomposition products produced by the accident, as well as the ignition of a mixture of flammable vapor and air to cause secondary accidents. Special precautions should be taken for substances that may explode before testing.
4.2 After the test, the sample should be handled safely and harmlessly as soon as possible. The sample may become more unstable and sensitive after the test and should be handled with caution.
5 Test equipment
5.1 The test equipment includes a thermostat, a Dewar flask and its closure, a temperature sensor and a measuring device.
5.2 The thermostat should be fire-resistant and pressure-resistant, and an effective pressure relief system, such as an explosion venting panel, should be installed. The recording system should be placed in a separate observation area.
This standard specifies the test principle, safety measures, test equipment, test steps, result evaluation and test report of the heat accumulation storage test of hazardous goods. This standard applies to the heat accumulation storage test of hazardous goods.

ICS13.300
National Standard of the People's Republic of China
GB/T39093—2020
Heat accumulation storage test method for dangerous goods
Heat accumulation storage test method for dangerous goods2020-09-29Issued
State Administration for Market Regulation
National Administration of Standardization
2021-04-01Implementation
GB/T39093—2020
Terms and Definitions
Test Principle
Safety Measures
Test Equipment
Test Procedures
Result Evaluation
8 Test Report
Appendix A (Informative Appendix)
Appendix B (Regulatory Appendix) Appendix C (Informative Appendix)
Appendix D (Informative Appendix)
Schematic diagram of Dewar flask and its closure device for testing liquids and semi-solids Test and calculation of unit mass heat loss rate of Dewar flask Example of unit mass heat loss rate of packaging, intermediate bulk containers and bodies Example of heat accumulation storage test results of dangerous goods Before
This standard was drafted in accordance with the rules given in GB/T1.1-2009 This standard was proposed and managed by the National Technical Committee for Standardization of Hazardous Chemicals Management (SAC/TC251). GB/T39093—2020
Drafting units of this standard: Chemical Registration Center of the Ministry of Emergency Management, Qingdao Safety Engineering Research Institute of Sinopec, Nanjing University of Science and Technology, Nanjing Customs Dangerous Goods and Packaging Testing Center, China Chemical Economic and Technological Development Center. The main drafters of this standard: Zhang Jinmei, Huang Fei, Gan Yaqin, Guo Lu, Kang, Zhang Huiguang, Wu Baoyi, Xu Sen, Gan Hongsong, Cao Mengran I
Test method for heat accumulation storage of dangerous goods
GB/T39093—2020
Warning: This test has potential explosion hazard. The test equipment should be guaranteed to provide adequate protection for test personnel to avoid catastrophic consequences caused by explosion.
1 Scope
This standard specifies the test principle, safety measures, test equipment, test procedures, result evaluation and test report of the heat accumulation storage test of dangerous goods.
This standard applies to the heat accumulation storage test of dangerous goods. Terms and definitions
The following terms and definitions apply to this document. 2.1
Self-accelerating decomposition temperature; SADT is the lowest ambient temperature at which self-accelerating decomposition of a substance may occur in a container used for transportation. [GB/T21178-2009, 3.3]]
Test principle
According to the Semenov Theory of thermal explosion, the main resistance to heat flow propagation in a thermal runaway system is concentrated on the container wall. Therefore, a Dewar flask with a small volume but large thermal resistance of the container wall is used to simulate the thermal environment in which a large volume of dangerous goods undergoes self-accelerating decomposition. It is used to determine the dangerous goods in the container, including medium bulk containers and small containers below 2m". Type tank, the lowest constant ambient temperature at which self-accelerating decomposition occurs is the self-accelerating decomposition temperature. The effectiveness of the test depends on whether the heat loss rate per unit mass of the selected Dewar flask is similar to the heat loss rate per unit mass of the packaging used for dangerous goods. 4 Safety measures
4.1 Safety precautions should be taken during the test to avoid catastrophic accidents caused by failure of the test container, and to avoid the escape of toxic decomposition products produced by the accident, as well as secondary accidents caused by ignition of the mixture of flammable vapor and air. Special precautions should be taken for testing of substances that may explode.
4.2 After the test, the sample should be handled safely and harmlessly as soon as possible. The sample may become more unstable and sensitive after the test and should be handled with caution.
5 Test equipment|| tt||5.1 The test equipment includes a thermostat, a Dewar flask and its closure device, a temperature sensor and a measuring device. 5.2 The thermostat should be fire-resistant and pressure-resistant, and should be equipped with an effective pressure relief system, such as an explosion venting panel. The recording system should be placed in a separate observation area. 5.3 When the test temperature is higher than the ambient temperature, a thermostat with a jacketed outer wall can be used. The temperature inside the thermostat is controlled by circulating a heat-conducting liquid in the jacket. 1
GB/T39093—2020
The door or lid of the thermostat should be insulated, but it does not have to be sealed. A thermostat without a jacketed outer wall can also be used for testing, especially when the test temperature exceeds 75°C. The volume of the thermostat should be large enough to allow air to circulate around the Dewar flask. Magnetic door buckles can be used, or loosely mounted The insulated cover replaces the door. The thermostatic chamber is protected by a suitable steel lining and the Dewar flask is placed in a metal mesh cage. When testing with both equipment, the temperature of the liquid sample in the Dewar flask should be controlled to not deviate from the predetermined temperature by more than ±1°C within 10 days, and the temperature of the air in the thermostatic chamber should be measured and recorded.
5.4 When the test temperature is lower than the ambient temperature, a double-walled thermostatic chamber of appropriate size, such as a refrigerator, may be used for the test. The thermostatic chamber is equipped with a loose-fitting door or cover, such as a magnetic cover. The temperature of the air in the thermostatic chamber should be controlled to within ±1°C of the predetermined temperature. 5.5 The unit mass heat loss rate of the Dewar flask and its closure device should be representative of the unit mass heat loss rate of the largest size packaging actually used for dangerous goods. The closure device of the Dewar flask should be made of inert material. For solids, cork or rubber stopper can be used. Dewar flasks and closure devices for low-volatile or medium-volatile liquids and semi-solids can be found in Appendix A. Samples with high volatility at the test temperature should be tested using a pressure-resistant metal container equipped with a pressure relief valve. During the test, the pressure-resistant metal container is placed in the Dewar flask, and the influence of its heat capacity is taken into account.
5.6 Before the test, the heat loss rate per unit mass of the Dewar flask and its closure device should be determined, see Appendix B. The closure device has a great influence on the heat loss rate per unit mass of the Dewar flask, and the heat loss rate per unit mass of the Dewar flask can be adjusted to a certain extent by changing the closure device. In order to obtain the required level of sensitivity, the capacity of the Dewar flask should not be less than 0.5L. 5.7 A Dewar flask containing 0.4L of sample and a heat loss rate per unit mass of 80mW/kg·K)~100mW/(kg·K) can usually represent the heat loss rate per unit mass of a 50kg package. For larger packaging, intermediate bulk containers or small tanks, a larger capacity Dewar flask with a smaller heat loss per unit mass should be used to represent its heat loss rate per unit mass. For example, a 1L spherical Dewar flask with a heat loss rate per unit mass of 16mW/(kg·K)~34mW/(kg·K) can be used to represent intermediate bulk containers and small tanks. See Appendix C for examples of heat loss per unit mass of packages, IBCs and tanks. 6 Test Procedure
6.1 Set the thermostat to a predetermined temperature. Fill the Dewar flask with the sample to 80% of its capacity and record the mass of the sample. Solid samples should be compacted appropriately so that their density is close to the density in the actual transportation or storage state. Insert the temperature sensor into the center of the sample. Cover the Dewar flask with a lid and place it in the thermostat, connect the temperature recording system and close the thermostat door. 6.2 Heat the sample and continuously measure the sample temperature and the thermostat temperature. Record the time point when the sample temperature reaches 2 °C below the thermostat temperature. The test is then continued for a further 7 days, and the test is terminated early when the sample temperature rises to at least 6 °C above the thermostat temperature within 7 days. Record the time it takes for the sample temperature to rise from 2 °C below the thermostat temperature to its maximum temperature. 6.3 After the test, if there is any sample left in the Dewar flask, remove it after cooling, record the percentage of mass loss and determine whether the composition has changed.
6.4 Change the test temperature in steps of 5°C and repeat the above test with a new sample. If the purpose of the test is to determine whether temperature control is required, a sufficient number of tests should be conducted to determine whether the self-accelerating decomposition temperature is to the nearest 5°C or whether it is 60°C or higher; if the purpose of the test is to determine whether the dangerous goods meet the self-accelerating decomposition temperature standard for self-reactive substances and mixtures, a sufficient number of tests should be conducted to determine whether the self-accelerating decomposition temperature of a 50 kg package is 75°C or lower. 7 Evaluation of results
The lowest isothermal oven temperature that can cause the sample temperature to exceed the isothermal oven temperature by at least 6°C is recorded as the self-accelerating decomposition temperature of the sample in the corresponding packaging. If the sample temperature does not exceed the isothermal oven temperature by at least 6°C in any test, the self-accelerating decomposition temperature is recorded as greater than the highest isothermal oven temperature used. Examples of self-accelerating decomposition temperature results measured by the dangerous goods heat accumulation storage test method are shown in Appendix D.
Test report
The test report shall include at least the following contents: name and mass of the test sample;
Name of the manufacturer;
Test equipment;
Heat loss rate per unit mass of the Dewar flask;
- Self-accelerating decomposition temperature;
Record any phenomena observed during the test that are helpful in explaining the test results;- Test date, signature of the tester, and seal of the testing unit GB/T39093—2020
GB/T39093—2020
Appendix A
(Informative Appendix)
Schematic diagram of the Dewar flask and its closure device used for liquid and semi-solid testingThe schematic diagram of the Dewar flask and its closure device used for liquid and semi-solid testing is shown in Figure A.1. Description:
PTFE capillary:
Special screw fittings with O-ring (PTFE or aluminum): Metal strip;
Glass cover;
Glass beaker bottom;
A spring;
G——Glass protection tube;
H—Dewar flask;
A steel clamping device.
Figure A.1 Schematic diagram of Dewar flask and its closure device for liquid and semi-solid testing Appendix B
(Normative Appendix)
Test and calculation of unit mass heat loss rate of Dewar flask GB/T39093—2020 www.bzxz.net
The unit mass heat loss rate of Dewar flask is determined by measuring the change of temperature difference between the contents of Dewar flask and the surrounding environment over time. For example, for liquids, the container can be filled with dibutyl titanate or dimethyl titanate and then heated to about 80°C. Water should not be used as the content. Measure the temperature drop at the center of the contents within a certain temperature range, which should include the expected self-accelerating decomposition temperature. Continuously measure the temperature of the contents and the surrounding environment, and perform a linear regression on the logarithm of the difference between the contents temperature and the ambient temperature, i.e., In(TT,) with respect to time t according to formula (B.1), and obtain the slope c in formula (B.1), and then obtain the heat loss rate per unit mass of the Dewar flask L according to formula (B.2): In(TT.)=c. +cXt
L=c×C,
Where:
---content temperature, in degrees Celsius (℃); T. ——ambient temperature, in degrees Celsius (℃); C
the natural logarithm of the difference between the initial temperature of the contents and the initial ambient temperature; the slope of the straight line obtained by linear regression;
time, in seconds (s);
...........( B.)
..(B.2)
-heat loss rate per unit mass of the Dewar flask, in watts per kilogram Kelvin [W/(kg·K)]; -specific heat capacity of the contents, in joules per kilogram Kelvin [J/(kg·K)]. 5
GB/T39093—2020
Appendix C
(Informative Appendix)
Examples of unit mass heat loss rate of packaging, intermediate bulk containers and tanks Table C.1 gives examples of unit mass heat loss rate of packaging, intermediate bulk containers and tanks. The actual unit mass heat loss rate depends on factors such as the shape, wall thickness and surface coating of the container. Table c.1
Container type"
3H1 (black)
Rattan container (insulated)
Examples of unit mass heat loss rate for packaging, intermediate bulk containers and tanks Contents
Isododecane
Content state
Nominal capacity
Loading amount
Unit mass heat loss rate
mW/(kg·K)
Container type code Refer to Chapter 6.1 of the United Nations "Recommendations on the Transport of Dangerous Goods Model Regulations" (21st revised edition) for the construction and test requirements of containers.
Dimethyl phthalate.
. Calculated using thermal conductivity = 5W/(m·K). d Dicyclohexyl phthalate (solid). 6
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