GB/T 39090-2020.Adiabatic storage test method for dangerous goods.
1 Scope
GB/T 39090 specifies the safety measures, test equipment, test procedures, data processing and test report for adiabatic storage test of dangerous goods.
GB/T 39090 is applicable to adiabatic 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 may occur in the container used for transport.
[GB 21178-2007 ,3.3]
Note: The adiabatic storage test for dangerous goods is used to determine the heating rate of dangerous goods as a function of temperature. The heating parameters obtained together with the heat loss data of the relevant packaging are used to determine the self-accelerating decomposition temperature of dangerous goods in their containers. It is applicable to each type of container, including intermediate bulk containers and tanks.
3 Safety measures
3.1 If the cooling system is turned on when the heating rate exceeds the cooling capacity of the cooling system, the sample may explode. Therefore, the cooling system should be turned on in time and a safe test site should be selected to minimize the possible explosion hazard and the risk of gas explosion (secondary explosion) caused by the decomposition products.
3.2 After the test, the sample should be handled safely and harmlessly as soon as possible. The sample may become more unstable and more sensitive after the test and should be handled with caution.
4 Test Equipment
4.1
The test equipment for the adiabatic storage of dangerous goods consists of a glass Dewar flask (1.0 L or 1.5 L) for the sample, an insulated oven capable of maintaining a temperature difference of ±0.1 °C from the sample, and an inert Dewar flask cover. In special cases, the sample container may be made of other materials. The coil-shaped internal heater and cooling tube made of inert material are inserted into the sample through the flask cover. A 2m long polytetrafluoroethylene capillary is inserted into the insulated flask cover to prevent the pressure in the Dewar flask from rising. The heating power of the internal heater is adjustable and is used to heat the sample to a preset temperature or for calibration. When the sample in the Dewar flask reaches the preset temperature, the internal heating can be automatically stopped or cooling can be started. In addition to the cooling system, the equipment should also be equipped with an auxiliary safety device to cut off the power supply to the oven when the safety temperature limit is exceeded. See Appendix A for a schematic diagram of the adiabatic storage test.
4.2 The sample temperature is measured at the center of the sample using an armored thermocouple or platinum resistance sensor with an accuracy of at least 0.1°C. The ambient temperature in the oven is also measured using a thermocouple or platinum resistance sensor at the same height as the sample temperature point. Continuous temperature measurement and recording equipment is required to monitor the sample temperature and the ambient temperature in the oven. The test equipment should be placed in a separate isolated observation area. For samples with a self-accelerating decomposition temperature lower than the ambient temperature, the test should be carried out in a cooling room or the oven should be cooled with solid carbon dioxide.
This standard specifies the safety measures, test equipment, test procedures, data processing and test reports for the adiabatic storage test of hazardous materials. This standard applies to the adiabatic storage test of hazardous materials.

ICS13.300
National Standard of the People's Republic of China
GB/T39090—2020
Adiabatic storage test method for dangerous goods
Issued on 2020-09-29
State Administration for Market Regulation
National Administration of Standardization
Implementation on 2021-04-01
Terms and definitions
Safety measures
Test equipment
Test procedures
Data processing
Test report
Appendix A (informative)
Appendix B (informative)
Appendix C (informative)|| tt||Appendix D (Informative Appendix)
Adiabatic Storage Test Apparatus
Calculation of Heat Loss Rate per Unit Mass (L) of Package, IBC or Tank Example of Determining Self-Accelerating Decomposition Temperature
Example of Adiabatic Storage Test Results for Dangerous Goods
GB/T39090—2020
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 Dangerous Chemicals Management (SAC/TC251). GB/T39090—2020
Drafting organizations 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, Dangerous Goods and Packaging Testing Center of Nanjing Customs, and China Chemical Economic and Technological Development Center. The main drafters of this standard: Gan Yaqin, Huang Fei, Zhang Jinmei, Guo Lu, Kang, Zhang Huiguang, Wu Baoyi, Xu Sen, Gan Hongsong, Cao Mengran Test method for adiabatic storage of hazardous goods
GB/T39090—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 of explosion.
1 Scope
This standard specifies the safety measures, test equipment, test procedures, data processing and test reports for the adiabatic storage test of hazardous goods. This standard applies to adiabatic storage tests of hazardous goods. 2 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 a substance in a container used for transport may undergo self-accelerating decomposition. [GB211782007, 3.3
Note: The adiabatic storage test for dangerous goods is used to determine the temperature-dependent heating rate of dangerous goods. The heating parameters obtained are used together with the heat loss data of the relevant packaging to determine the self-accelerating decomposition temperature of dangerous goods in their containers. It is applicable to every type of container, including intermediate bulk containers and tanks. 3 Safety measures
3.1 If the cooling system is turned on when the heating rate exceeds the cooling capacity of the cooling system, the sample may explode. Therefore, the cooling system should be turned on in time and a safe test site should be selected to minimize the possible explosion risk and the risk of gas explosion (secondary explosion) caused by the decomposition products.
3.2 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.
4 Test Equipment
4.1 The test equipment for adiabatic storage of dangerous goods consists of a glass Dewar flask (1.0L or 1.5L) for holding the sample, an insulated oven capable of maintaining a temperature difference of ±0.1°C from the sample, and an inert Dewar flask cover. In special cases, the sample container may be made of other materials. The coil-shaped internal heater and cooling tube made of inert material are inserted into the sample through the flask cover. A 2m long polytetrafluoroethylene capillary is inserted into the insulated flask cover to prevent the pressure in the Dewar flask from rising. The heating power of the internal heater is adjustable and is used to heat the sample to a preset temperature or for calibration. When the sample in the Dewar flask reaches the preset temperature, the internal heating can be automatically stopped or the cooling can be started. In addition to the cooling system, the equipment should also be equipped with auxiliary safety devices to cut off the power supply to the oven when the safety temperature limit is exceeded. The schematic diagram of the adiabatic storage test is shown in Appendix A.
4.2 The sample temperature is measured at the center of the sample using an armored thermal couple or platinum resistor sensor with an accuracy of at least 0.1°C. Similarly, use a thermocouple or platinum resistance sensor to measure at the same height as the temperature point of the sample to obtain the ambient temperature in the oven. Continuous temperature measurement and recording equipment is required to monitor the sample temperature and the ambient temperature in the oven. The test equipment should be placed in a separate isolated observation area. For samples with a self-accelerating decomposition temperature lower than the ambient temperature, the test should be carried out in a cooling room or the oven should be cooled with solid carbon dioxide. GB/T39090-2020
4.3 The adiabatic storage test of dangerous goods can be carried out in a temperature range of -20℃ to 220℃. The minimum detectable temperature rise rate is equivalent to a heat generation rate of 15mW/kg. The maximum detectable temperature rise rate depends on the ability of the cooling system to safely cool the sample (up to 500W/kg if water is used as a coolant). Although the test is not completely hot, the heat loss is less than 10mW. At a heat generation rate of 15mW/kg, the maximum error is 30%, and at a heat generation rate of 100mW/kg10W/kg, the maximum error is 10%. 5 Test Procedure
5.1 Calibration
The calibration procedure is to determine the heat loss rate and heat capacity of the Dewar flask at various temperature points by heating and cooling the Dewar flask and the inert calibration material of known heat capacity in the flask under the test environment and monitoring the temperature change rate of the calibration material in the Dewar flask. The calibration procedure is as follows: a) The Dewar flask is filled with calibration materials, such as analytical grade sodium chloride and dibutyl phthalate, and placed on the bottle rack of the insulated storage test oven;
b) The calibration material is heated to multiple temperature points at intervals of 20°C, such as 40°C, 60°C, 80°C and 100°C, using an internal heater with an appropriate power (e.g. 0.333W or 1.000W) to obtain the temperature rise rate of the calibration material during internal heating. After the calibration material is heated to the predetermined temperature, the heating is stopped and the temperature change of the calibration material with time is recorded to determine the temperature drop rate of the calibration material and finally determine the heat loss rate at each temperature point;
c) The heat capacity and heat loss of the Dewar flask are determined according to the methods described in 6.2 and 6.3. 5.2 Test
The test procedure is as follows:
a) The weighed sample is placed in the Dewar flask. If the packaging material is metal, a representative amount of packaging material should also be added. The Dewar flask is placed on the bottle rack of the insulated storage test oven; Note: The representative amount of packaging material, that is, the amount of metal packaging material added and the contact area with the contents can reflect the mass ratio and contact area of ​​metal to contents in the actual packaging.
b) Start temperature monitoring and use the internal heater to heat the sample to a preset temperature where self-heating may be detected. The specific heat capacity of the sample can be calculated from the sample temperature rise, heating time and heating power; c) Stop internal heating and monitor the temperature. If no temperature rise due to self-heating of the sample is observed within 24 hours, increase the sample temperature by 5°C and repeat this procedure until self-heating is detected; d) When self-heating of the sample is detected, keep the ambient temperature of the Dewar flask, that is, the oven temperature, consistent with the sample temperature in the Dewar flask, and allow the sample to heat up to a preset temperature under adiabatic conditions where the heat generation rate is less than the cooling capacity. Once the preset temperature is reached, start the cooling system;
e) Measure the mass loss of the sample immediately after cooling and determine the composition change if necessary. The tested sample should be safely destroyed as soon as possible after the test.
6 Data Processing
6.1 Calculate the rate of temperature drop of the Dewar flask containing the calibration material at different temperatures in the calibration test. Plot a curve using these values ​​to determine the rate of temperature drop at any temperature. 6.2 Use formula (1) to calculate the heat capacity of the Dewar flask: H = 3600 × E
Where:
-(M,×C)
H—heat capacity of the Dewar flask, in joules per Kelvin (J/K); 2
—power of the internal heater during heating, in watts (W); E,
GB/T39090—2020
—temperature drop rate of the calibration material at the calculated temperature point after the internal heating stops, in Kelvin per hour (K/h); —temperature rise rate of the calibration material at the calculated temperature point during internal heating, in Kelvin per hour (K/h); M,—mass of the calibration material, in kilograms (kg); Cpl
specific heat capacity of the calibration material, in joules per kilogram Kelvin [J/(kg·K)]. 6.3 Use formula (2) to calculate the heat loss of the Dewar flask containing the calibration material at each specific temperature, and use these values ​​to draw a curve of heat loss versus temperature.
Where:
K=A×(H+M,×C)
Heat loss of the Dewar flask, in watts (W); ——The temperature drop rate of the calibration material at the calculated temperature point after the internal heating stops, in Kelvin per hour (K/h); H——The heat capacity of the Dewar flask, in joules per Kelvin (J/K); The mass of the calibration material, in kilograms (kg); M
Specific heat capacity of the calibration material, in joules per kilogram Kelvin [J/(kg·K)]. 6.4 Calculate the specific heat capacity of the sample using formula (3): Cp2 =
Wherein:
3600X(E2+K)
is the specific heat capacity of the sample, in joules per kilogram Kelvin [J/(kg·K)]; Cp2
E2 is the power of the internal heater, in watts (W); K is the heat loss of the Dewar flask, in watts (W); HbZxz.net
is the heat capacity of the Dewar flask, in joules per Kelvin (J/K); When internal heating is applied, calculate the temperature rise rate of the sample at the temperature point, in Kelvin per hour (K/h); and the mass of the sample, in kilograms (kg). 5 Use formula (4) to calculate the heat generation rate per unit mass of the sample at each temperature every 5°C: 6.5
(M2×C+H)×D/3600-K
Wherein:
Qt——heat generation rate per unit mass of the sample, in watts per kilogram (W/kg); M,——mass of the sample, in kilogram (kg); Ce——specific heat capacity of the sample, in joules per kilogram Kelvin [J/(kg·K)]; H
-d Dewar flask heat capacity, in joules per Kelvin (J/K); the temperature rise rate of the sample at the calculated temperature point during the self-heating stage, in Kelvin per hour (K/h); Dewar flask heat loss, in watts (W), · (2)
(3)
(4)
6.6 Take the calculated unit mass heat generation rate as a function of temperature, plot each data point in a linear coordinate, and draw a best fit curve through these marked points, i.e., the sample heat generation curve. Determine the unit mass heat loss rate L (see Appendix B) of the sample package (including IBC or tank) in actual transportation, and draw a straight line tangent to the heat generation curve with a slope equal to L. The intersection of this line and the abscissa is the critical ambient temperature, i.e., the highest temperature at which the substance in the package does not self-accelerate decomposition. The self-accelerating decomposition temperature is the critical ambient temperature rounded up to an integer multiple of 5 (°C). See Appendix C for an example of determining the self-accelerating decomposition temperature, and see Appendix D for an example of the results of the adiabatic storage test of dangerous goods. 7 Test report
The test report shall include at least the following contents:3
GB/T39090—2020
--Test sample name and quality;
Name of manufacturer;
——Test equipment;
Critical ambient temperature;
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. 4
See Figure A.1 for the adiabatic storage test device.
Description:
A—Multi-point recorder and temperature controller:
B—External zero adjustment device:
C—High-precision recorder;
Appendix A
(Informative Appendix)
Adiabatic storage test device
D—Controller:
E—Relay;
F—Internal heater
Figure A.1 Adiabatic storage test device
GB/T39090—2020
GB/T39090—20 20
Appendix B
(Informative)
Calculation of the rate of heat loss per unit mass (L) of packagings, IBCs or tanks B.1 The rate of heat loss per unit mass of a specific packaging, IBC or tank is calculated using formula (B.1): L = ln2 ×
where:
rate of heat loss per unit mass, in watts per kilogram Kelvin [W/(kg·K)]; half time of cooling, in seconds (s);
specific heat capacity of the substance, in joules per kilogram Kelvin [J/(kg·K)]. .......(B.1)
2 Table B.1 gives examples of the rate of heat loss per unit mass of typical packagings, IBCs and tanks. The actual value of the heat loss rate characteristic B.2
depends on the shape, wall thickness and surface coating of the container. Table B.1
Container type
3H1 (black)
Tank container (insulated)
Examples of unit mass heat loss rate for packaging, IBC and tank Contents
Isododecane
Content state
Nominal capacity
Container type code Refer to the test requirements of the United Nations Recommendations on the Transport of Dangerous Goods.
Dimethyl phthalate.
Calculated using thermal conductivity = 5W/m2·K.
Dicyclohexyl phthalate (solid). 6
Loading
Unit mass heat loss rate
mW/kg·K
Model Regulations (21st revised edition) Chapter 6.1 Manufacture and use of containers1.
Description:
A—Multi-point recorder and temperature controller:
B—External zero adjustment device:
C—High-precision recorder;
Appendix A
(Informative Appendix)
Adiabatic storage test device
D—Controller:
E—Relay;
F—Internal heater
Figure A.1 Adiabatic storage test device
GB/T39090—2020
GB/T39090—20 20
Appendix B
(Informative)
Calculation of the rate of heat loss per unit mass (L) of packagings, IBCs or tanks B.1 The rate of heat loss per unit mass of a specific packaging, IBC or tank is calculated using formula (B.1): L = ln2 ×
where:
rate of heat loss per unit mass, in watts per kilogram Kelvin [W/(kg·K)]; half time of cooling, in seconds (s);
specific heat capacity of the substance, in joules per kilogram Kelvin [J/(kg·K)]. .......(B.1)
2 Table B.1 gives examples of the rate of heat loss per unit mass of typical packagings, IBCs and tanks. The actual value of the heat loss rate characteristic B.2
depends on the shape, wall thickness and surface coating of the container. Table B.1
Container type
3H1 (black)
Tank container (insulated)
Examples of unit mass heat loss rate for packaging, IBC and tank Contents
Isododecane
Content state
Nominal capacity
Container type code Refer to the test requirements of the United Nations Recommendations on the Transport of Dangerous Goods.
Dimethyl phthalate.
Calculated using thermal conductivity = 5W/m2·K.
Dicyclohexyl phthalate (solid). 6
Loading
Unit mass heat loss rate
mW/kg·K
Model Regulations (21st revised edition) Chapter 6.1 Manufacture and use of containers1.
Description:
A—Multi-point recorder and temperature controller:
B—External zero adjustment device:
C—High-precision recorder;
Appendix A
(Informative Appendix)
Adiabatic storage test device
D—Controller:
E—Relay;
F—Internal heater
Figure A.1 Adiabatic storage test device
GB/T39090—2020
GB/T39090—20 20
Appendix B
(Informative)
Calculation of the rate of heat loss per unit mass (L) of packagings, IBCs or tanks B.1 The rate of heat loss per unit mass of a specific packaging, IBC or tank is calculated using formula (B.1): L = ln2 ×
where:
rate of heat loss per unit mass, in watts per kilogram Kelvin [W/(kg·K)]; half time of cooling, in seconds (s);
specific heat capacity of the substance, in joules per kilogram Kelvin [J/(kg·K)]. .......(B.1)
2 Table B.1 gives examples of the rate of heat loss per unit mass of typical packagings, IBCs and tanks. The actual value of the heat loss rate characteristic B.2
depends on the shape, wall thickness and surface coating of the container. Table B.1
Container type
3H1 (black)
Tank container (insulated)
Examples of unit mass heat loss rate for packaging, IBC and tank Contents
Isododecane
Content state
Nominal capacity
Container type code Refer to the test requirements of the United Nations Recommendations on the Transport of Dangerous Goods.
Dimethyl phthalate.
Calculated using thermal conductivity = 5W/m2·K.
Dicyclohexyl phthalate (solid). 6
Loading
Unit mass heat loss rate
mW/kg·K
Model Regulations (21st revised edition) Chapter 6.1 Manufacture and use of containers
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