GB/T 15814.3-1995 Fireworks and firecrackers thermal compatibility test Differential thermal analysis or differential scanning calorimetry
Some standard content:
National Standard of the People's Republic of Chinabzxz.net
Reagent of fireworks and firecrackersThermal compatibility test
Differential thermal analysis or differential scanning calorimetry
Reagent of fireworks and firecrackersThermal compatibil ity test
-Method of DTA and DSC
1 Subject content and applicable scope
GB/T 15814.3-1995
This standard specifies the instruments, equipment, test conditions, test procedures and result processing methods required for the thermal compatibility test of fireworks and firecrackers using differential thermal analysis (DTA) or differential scanning calorimeter (ISC). This standard is used for rapid screening tests of thermal compatibility of fireworks and firecrackers. 2 Terminology
2.1 Internal compatibility: compatibility between components in the agent 2.2 External compatibility: compatibility between the agent as a system and related contact substances (another agent or binding material). 3 Basic Principles
The sample is at a program-controlled temperature, and the sample temperature changes due to the thermal effect of chemical or physical changes. The temperature difference between the sample and the reference material, the energy integration and the response temperature are recorded by a differential thermal analyzer or a differential scanning calorimeter, which is the DTA or DSC curve. In the mixed system composed of mutually incompatible substances on the DTA or DSC curve, the exothermic peak temperature drifts toward the low temperature direction, and the activation energy generally changes greatly. This standard mainly uses the change in the decomposition peak top temperature (T) of the mixed system relative to the single system of the determined reference substance on the DTA or DSC curve, and the change in the reference activation energy (A/) to evaluate the thermal compatibility of fireworks and firecrackers. 4 Instruments
4.1 Differential thermal analyzer or differential scanning calorimeter, the temperature division value is less than or equal to 0.5℃. 4.2 Tablet press: made of aluminum, stainless steel, nickel or platinum, etc. 4.3 Manual tablet press.
4.4 Analytical balance: maximum weighing 20g, graduation value 0.01mg. 4.5 Calculator: Calculator capable of logarithmic regression processing. 5 Materials
5.1 Powdered alumina (HGB3413) + analytically pure, treated at 1350℃ to become α-AlO. 5.2 Standard substances for temperature calibration: steel, tin, lead, zinc, lead, etc., with a purity of 09.999%. 6 Experimental preparation
6.1 Verification of instrument temperature measurement accuracy
Approved by the State Administration of Technical Supervision on December 8, 1995 and implemented on August 1, 1996
6.1.1 Weighing samples
GH/T 15814:3—1995
Weigh 510mg of standard substances, accurate to 0.01mg. 6-1.2 Make ITA or ISC thermogram
Make ITA or DSC thermogram according to the operating procedures in the instrument manual. 6.1.3 Temperature measurement error calculation
Compare the melting temperature value of the standard substance obtained in the graph with the standard temperature value. The temperature accuracy should be within 5℃. 6-1.4 Calibration cycle
Calibration cycle is every six months.
6.2 Determination of actual heating rate
The actual heating rate of the instrument with no less than four heating rate gears is generally 2, 5, 10.20℃/min. Its value is calculated according to the formula ():
Wherein, 1-actual heating rate,/minTemperature line 1 is the temperature difference between two non-returning temperature points on the straight line segment; BT
·corresponding time interval, min
6.3 Determination of base substance
6.3.1 Determination of reference substance for compatibility test Clearly define the chemical composition of the test agent and its content, understand the decomposition reaction temperature, phase change and melting point of each component, and through comparison of the above data, determine the component with the highest decomposition temperature as the reference substance for this group of compatibility tests. 6.3.2 Determination of reference material for external compatibility test Make TA or I>SC spectra of the agent and the contact material respectively, compare their first exothermic peaks, and the one with the lower first exothermic peak temperature shall be the reference material for this group of compatibility tests. 6.4 Sample preparation
The sample must be the raw material used in production, and the contact material should be made into powder or cut into pieces to ensure full contact after mixing. 7 Test procedure
7.1 Put the instrument in standby state according to the instrument operating procedures, select the thermal range or differential scanning range, and set it aside. 7.2 If the internal compatibility of the agent is to be determined, follow the following procedures. 7.2.1 Weigh ±~10mg of a-Al,0, in the reference medium and set it aside. 7.2.2 Weigh 2~10mg of the selected reference material in the sample medium and set it aside. 7.2.3 Instrument operating conditions Make DTA or DSC spectrum of the reference substance at a heating rate of 5°C/min and determine its first exothermic peak temperature.
Weigh 2-10 mg of the test agent in the sample culture medium for use. 7.2.4
7.2.5 Instrument operating conditions Make DTA or DSC spectrum of the test agent at a heating rate of 5°C/min and determine its first exothermic peak temperature.
Compare the temperature values of the first exothermic peak of the reference substance and the agent. If △T.≤5°C, fill in the analysis report directly. 7-2.6
7.2.7 If △T.≤5°C, the reference substance and the agent should be made DTA or DSC spectrum at three other appropriate heating rates, generally 2, 10, 20°C/min, and determine the first exothermic peak temperature. 7.3 If the external compatibility of the agent and the contact material is to be determined, the following procedures shall be followed: 7.3.1 Weigh 310 mg of -Al0 in a reference crucible and set aside. 7.3.2 Weigh 2-10 ng of the selected reference material in a sample crucible. 7.3.3 Instrumental conditions: Make ITA or DSC spectrum of the reference material at 5 °C/min to determine the first exothermic value temperature. GB/T 15814.3-1995
7.3.4 Mix the agent and the contact material in a ratio of 1:1. 7.3.5 Weigh 2-10 mg of the mixed mixture in a sample crucible. 7.3.6 Instrumental conditions: Make DTA or DSC spectrum of the mixture at a heating rate of 5 °C/min to determine the first exothermic peak temperature. 7.3.7 Compare the first exothermic peak temperature of the reference substance and the mixture. If △T, ≥ 5℃, fill in the analysis report directly; 7.3.8 If △T < 5℃, the reference substance and the mixture should be heated at two other appropriate rates, generally 2.10 and 20℃/min, to make IDTA or DSC spectra and determine their first exothermic peak temperatures. 8 Data processing
8.1 Calculate the test data according to formula (2):
△Tm=Tml-Tm2
The change in the first exothermic peak temperature of the agent or the mixture of the agent and the contact substance relative to the quasi-substance The first exothermic peak temperature of the reference substance;
The first exothermic peak temperature of the mixture of the agent or the contact substance 8.2 Calculation of apparent activation energy ()
Substitute the test data into test (3):
2.315 --0.4567
LRF(X)L
G-1.2.3.4.
Wherein: A-
refers to the antecedent-
mechanism function;
E.-.-apparent activation energy, kJ/mol;
gas constant, 8.314J/K·mol:
the first decomposition peak of the white when the heating rate is 2, 5, 10, 20C/min, K;Φ,-:-the actual heating rate when the heating rate is 2, 5, 10, 20℃/min, ℃/in. .(2)
（3）
Perform logarithmic regression on 1g history, and 1/T. to obtain the apparent activation energy E,. When the absolute value of the data processing correlation coefficient (r) is less than 0.97, four different heating degrees of the TA or DSC spectra should be repeated. 8.3 Calculation of the apparent activation energy change rate (△E/E,) A/(%)
Where: AF/F.
The change rate of the apparent activation energy of the agent or the mixture of the agent and the contact material relative to the reference material; the apparent activation energy of the agent or the mixture of the agent and the contact material relative to the reference material; E
E: The apparent activation energy of the reference material, kJ/mol: F: The apparent activation energy of the agent or the mixture of the agent and the contact material, kJ/mol. 8.4 Result expression
Report the thermal compatibility test results of TA or DSC in the format of A (reference). (4)
Heating rate, centimeters/min
Method power
Electrical data
Tester signature
Measured value
Es.kJ/mal
Additional instructions:
GB/r 15814.3—1995
Appendix A
Fireworks and firecrackers thermal compatibility test results report sheet (reference)
Name of the agent
Signature of the reviewer
This standard is proposed by the China Light Industry Federation.
This standard is under the jurisdiction of the National Fireworks and Firecrackers Standardization Technical Committee, Agents and Related Materials
Agents and Related Materials
This standard is drafted by the Second and Third Research Institute of China Ordnance Industry, Shaanxi Fireworks and Firecrackers Product Quality Supervision and Inspection Station 1, and Fengzheng County Fireworks and Firecrackers Research Institute of Suixi Province.
The main drafters of this standard: Yao Pu, Zhang Zang, Yin Kaixian,
Tip: This standard content only shows part of the intercepted content of the complete standard. If you need the complete standard, please go to the top to download the complete standard document for free.