Some standard content:
Chemical Industry Standard of the People's Republic of China
Azodicarbonamide (Blowing Agent ADC)
Subject Content and Scope of Application
HG2097-91
This standard specifies the technical requirements, test methods, inspection rules, marking, packaging, transportation and storage of azodicarbonamide. This standard applies to azodicarbonamide, namely blowing agent ADC, which is prepared by condensation and chlorination of urea and hydrazine hydrate as raw materials. Trade Name: Blowing Agent ADC
Chemical Name: Azodicarbonamide
Molecular Formula: C, H40, N4
Structural formula:
Relative molecular mass: 116.08 (according to the international relative atomic mass in 1987) 2 Reference standards
Chemical reagents
Preparation of standard solution for titration analysis (volumetric analysis) GB603 Preparation of preparations and products used in chemical reagent test methods GB11409.5 Determination method of sieve residue of rubber antioxidant and vulcanization accelerator 3 Technical requirements
3.1 Appearance
Azodicarbonamide should be light yellow powder (visual inspection). 3.2 Azodicarbonamide shall meet the requirements of the following table: Item
Gas generation, mL/g
Decomposition temperature, ℃
Heating loss, %
Ash content, %
Purity (ADC), %
Sieve residue (sieve hole 38um), %
Average particle size (D), um
Note: Purity is only tested during type inspection. Other items are factory inspection items. Approved by the Ministry of Chemical Industry of the People's Republic of China on July 31, 19914
Superior product
200210
First-class product
Qualified product
Implemented on March 1, 1992
Test method
HG2097-91
Unless otherwise specified, the reagents and water used in this standard refer to analytical reagents and distilled water or water of corresponding purity; the titration solutions, preparations and products of this standard are prepared in accordance with the provisions of GB601 and GB603. 4.1 Determination of gas emission
4.1.1 Summary of method
The gas emission of the sample is measured by the water displacement gas collection method under the condition of heating decomposition temperature. 4.1.2 Instruments and equipment
4.1.2.1 Gas generation measurement device (see Figure 1)o0S
Figure 1 Gas generation measurement device diagram
1-Voltage regulator (1kVA)2-Electric furnace (300W);3-Density bottle (25mL):4-Latex tube;5-Level bottle (250mL);6-Straight gas measuring tube (100mL);7-Glass three-way piston (@2mm);8-Glass tube (34mm);9-Thermometer (0~250℃)10-Beaker (400mL)4.1.2.2 Mercury thermometer: 0~250℃, graduation value is 1℃;4.1.2.3 Gas measuring tube: scale value is 0.2mL;4.1.2.4 Barometer
4.1.3 Reagents
4.1.3.1 Dioctyl phthalate;
4.1.3.2 Glycerol heat transfer fluid.
4.1.4 Operating steps
Weigh 0.3g of the sample (accurate to 0.0002g), place it in a 25mL density bottle, add 2mL of dioctyl phthalate, install the instrument according to Figure 1, and open the three-way piston to the atmosphere. Raise the level bottle to adjust the zero point of the gas pipe (at room temperature), close the three-way piston, check that the zero point remains unchanged, and heating can be carried out only when there is no leakage. Put 150-200mL of heat transfer liquid in a 400mL beaker, immerse the density bottle in the heat transfer liquid, and the depth should be 15-20mm from the bottom of the density bottle to the surface of the heat transfer liquid. When the heat transfer liquid is heated to 180℃, adjust the heat source, 5
HG2097—91
Put a small amount of sample into a clean and dry capillary, take a dry glass tube about 800mm high and stand it on a porcelain plate or glass plate, throw the capillary containing the sample on it several times, so that the sample in the capillary is compressed to 6-10mm high, turn on the magnetic stirrer and electric heater, heat and raise the temperature to 190±2℃, and attach the capillary containing the sample to the temperature. On the thermometer, the middle layer of the sample is at the same height as the middle of the mercury ball. Adjust the heat source to keep the heating rate at 3-4℃/min. The moment when the sample liquefies, cracks or decomposes and turns white is the decomposition temperature.
4.3.5 Representation of results
If a full immersion thermometer is used, the measured decomposition temperature is calculated according to formula (2): T-r+0.00016h(tt)
Where:, the temperature indicated by the measuring thermometer,; - the temperature indicated by the auxiliary thermometer, C;
0.00016-the apparent expansion coefficient of mercury volume; h-the height of mercury exposed to the liquid surface (expressed in temperature), 4.4 Determination of heating loss
4.4.1 Summary of the method
The mass percentage of the sample reduced after heating under specified conditions. 4.4.2 Instruments and equipment
Electric constant temperature drying oven: the temperature fluctuation range is ±2C; a.
b. Weighing bottle: 40mm in diameter, 25mm in height; c. Desiccator: filled with color-changing silica gel or anhydrous calcium chloride. 4.4.3 Operation steps
Weigh about 2g of the sample (accurate to 0.000.2g), place it in a weighing bottle that has been kept at a constant weight at 105±2℃, dry it in a drying oven at 105±2℃ for 2h, move it into a desiccator, cool it to room temperature (about 30min), and weigh it. 4.4.4 Expression of results
Heating loss expressed as mass percentage (knife) is calculated according to formula (3): J
Where: m
Mass of sample before drying, g
Mass of sample after drying, g-
4.5 Determination of ash content
4.5.1 Summary of method
The ash content of foaming agent ADC is determined by high-temperature burning method. 4.5.2 Apparatus
Porcelain: 30mL;
Electric furnace: 600-800W;
Voltage regulator: 1kVA;
d High-temperature furnace.
4.5.3 Operating steps
Weigh 5g of sample (accurate to 0.1g) and place it in a crucible that has been kept constant at 800℃, then put it in an electric furnace equipped with a voltage regulator and gradually heat it up until the test After the sample is decomposed and carbonized, it is transferred to a high-temperature furnace at 800℃ and burned for 2h. The crucible is taken out, cooled slightly, transferred to a desiccator, and continued to cool to room temperature (about 30min). It is weighed (accurate to 0.0002g). 8
4.5.4 Expression of results
HG2097-91
The ash content (H) expressed as mass percentage is calculated according to formula (4): H-
Where: m is the mass of the empty crucible, g;
m2 is the mass of the added ash, g
m—the mass of the sample, g
4.6 Purity determination
4.6.1 Summary of the method
Quantitative hydrazine hydrate and diaminodicarbonamide are reacted to form biurea, and the remaining hydrazine is titrated with iodine standard solution to calculate the content of the foaming agent ADC.
4.6.2 Reagents and solutions
4.6.2.1 Sodium bicarbonate (GB640);
4.6.2.2 Hydrazine hydrate (hydrazine hydrate): 1% (V/V) solution; 4.6.2.3 Iodine standard solution: c(I)=0.1mol/L; 4.6.2.4 Starch indicator solution: 10g/L solution. 4.6.3 Operation steps
Weigh 0.15g of the sample (accurate to 0.0002g) and place it in a 100mL iodine volumetric flask, then add 10mL of water and use a pipette to draw 5.0mL of hydrazine hydrate solution (4.6.2.2) and heat it in a 60±2℃ water bath for 20min. When the sample turns completely white, cool it to 15-20℃. Add 1g of sodium bicarbonate and use iodine standard solution (4.6.2.3 ) titration, add 1mL starch indicator solution when near the end point, continue titration until purple-red color does not fade for 30S as the end point, and carry out blank test at the same time. 4.6.4 Expression of results
The purity of azodicarbonamide expressed as mass percentage (4) is calculated according to formula (5): A
(VV).cx0.05804
Wherein: V-the volume of iodine standard solution (4.6.2.3) consumed in blank test, mL; -the volume of iodine standard solution (4.6.2.3) consumed by sample, mL; 2
-the concentration of iodine standard solution (4.6.2.3), mol/L; the mass of sample, g;
the mass of azodicarbonamide equivalent to 1.00mL iodine standard solution [c (1) = 1.000mol/L) expressed in grams.
4.6.5 Allowable difference
The difference between parallel measurement data shall not exceed 0.5%. The arithmetic mean of the two data shall be taken as the measurement result. 5 Inspection rules
5.1 Azodicarbonamide shall be inspected by the quality supervision and inspection department of the manufacturer. The manufacturer shall ensure that all azodicarbonamide shipped out of the factory meets the requirements of this standard and shall be accompanied by a quality certificate in a certain format. 5.2 The user has the right to inspect and accept the azodicarbonamide received in accordance with the provisions of this standard to verify whether it meets the requirements of this standard.
5.3 Each batch of products shall not exceed 10t.
HG2097—91
5.4 Sampling method
5.4.1 Select the number of random sampling bags (barrels) according to the table below. When the total number of bags (barrels) is greater than 500, the number of bags (barrels) selected is 3×VN (N is the total number of bags (barrels)), the total number of ADC (barrels) produced
82~101
102~125
126~151
152~181
182~216
217~254
255~296
297.～343
344~394
395~450
451~512
The minimum number of bags (barrels) selected
All bags (oranges)
5.4.2 Extend the sampling probe into the upper and middle of the bag (catch). Take equal amounts of samples from each part, mix them evenly, and use the quartering method to take out no less than 100 samples, and place them in two clean and dry ground-mouth bottles (or plastic bottles, plastic bags). Paste labels on the bottles, indicate the product name, batch number, quantity and sampling date, send one bottle to the inspection department for inspection, and keep the other bottle for two months for future reference. 5.5 If one of the test results does not meet the requirements of this standard, re-sample from 2 times the amount of packaging for verification. If the verification results show that even if only one item does not meet the requirements of this standard, the entire batch of azodicarbonamide cannot be accepted. 5.6 When the supply and demand parties have objections to the product quality, the two parties shall negotiate to resolve the dispute. If arbitration is required, it shall be conducted in accordance with the provisions of this standard. 6 Marking, packaging, transportation and storage
6.1 The packaging shall indicate the manufacturer's name, product name, trademark, production date, grade, batch number and net weight. 6.2 Azodicarbonamide is available in bags and barrels. Bags are packed in plastic woven bags lined with polyethylene film bags, with a net weight of 25±0.2kg per bag. Barrels are packed in iron barrels lined with polyethylene film bags, with a net weight of 40±0.2kg per barrel. If special packaging is required, the supply and demand parties shall negotiate separately.
During transportation and storage, it should not be close to any heat source, and should be protected from violent impact and water ingress, 10
atmospheric pressure
906667
909333
912000
914667
917333
920000
922667
925333
928000
930 667
933333
936000
938667
941333
944000
946667
952000
954 667
957333
960000
962667
965333
HG2097—91
Appendix A
Gas volume conversion factor
(Supplement)
Table A1 Gas volume conversion to 20℃, 101325P18c
0:9342
HG2097-91
Appendix A
Gas volume conversion factor
(Supplement)
The conversion factor of this volume into 20℃, 101325Pa (1atm) is 8
0-8674
968000
970667
973 333 | | tt | | 976000 | :000
100267
100533
100800
101067 | | tt | 03733
104000
0.96130.9570
0.9716 10.9667
0.98120.9761
HG2097—91
Continued Table A1
0.94490.9397
0.9475 /0.9423
0.9663:0.961c
.0.9930
IHG2097-91
Continued Table A1
23 ℃
1:0042
Additional Notes
HG2097-91
This standard is proposed by the Department of Science and Technology of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of Shanxi Chemical Research Institute. This standard is drafted by Shanghai Xiangyang Chemical Factory. The main drafters of this standard are Zeng Guangmo, Lin Shengqi, Xu Wenqi, Cai Dan and Xue Weijing. From the date of implementation of this standard, the former Ministry of Chemical Industry of the People's Republic of China Standard HG2-1187-78 "Azodimethylamine (AC Foaming Agent)" will be invalidated.
People's Republic of China
Chemical Industry Standards
Vulcanization Accelerator CBS
Azodicarbonamide (Blowing Agent ADC)
HG2096~2097-91
Chemical Industry Standards Editorial Department
(Standardization Research Institute of Ministry of Chemical Industry)
Postal Code: 100013
Printing Standardization Research Institute of Ministry of Chemical Industry
Copyright reserved. No reproduction allowed
Book size 880×12301/16
Printing sheet 1V
Word count 27000
First edition in December 1991
First printing in December 1991
Print count 1500The barrel is an iron barrel lined with a polyethylene film bag, with a net weight of 40±0.2kg per barrel. If special packaging is required, the supply and demand parties shall negotiate separately.
During transportation and storage, it should not be close to any heat source, and should be protected from violent impact and water ingress, 10
atmosphere pressure
906667
909333
912000
914667
917333
920000
922667
925333
928000
930 667
933333
936000
938667
941333
944000
946667
952000
954 667
957333
960000
962667
965333
HG2097—91
Appendix A
Gas volume conversion factor
(Supplement)
Table A1 Gas volume conversion to 20℃, 101325P18c
0:9342
HG2097-91
Appendix A
Gas volume conversion factor
(Supplement)
The conversion factor of this volume into 20℃, 101325Pa (1atm) is 8
0-8674
968000
970667
973 333 | | tt | | 976000 | :000
100267
100533
100800
101067 | | tt | | 101325 | 03733
104000
0.96130.9570
0.9716 10.9667
0.98120.9761
HG2097—91
Continued Table A1
0.94490.9397
0.9475 /0.9423
0.9663:0.961c
.0.9930
IHG2097-91
Continued Table A1
23 ℃
1:0042
Additional Notes
HG2097-91
This standard is proposed by the Department of Science and Technology of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of Shanxi Chemical Research Institute. This standard is drafted by Shanghai Xiangyang Chemical Factory. The main drafters of this standard are Zeng Guangmo, Lin Shengqi, Xu Wenqi, Cai Dan and Xue Weijing. From the date of implementation of this standard, the former Ministry of Chemical Industry of the People's Republic of China standard HG2-1187-78 "Azodimethylamine (AC Foaming Agent)" will be invalidated.
People's Republic of China
Chemical Industry Standards
Vulcanization Accelerator CBS
Azodicarbonamide (Blowing Agent ADC)
HG2096~2097-91
Chemical Industry Standards Editorial Department
(Standardization Research Institute of Ministry of Chemical Industry)
Postal Code: 100013
Printing Standardization Research Institute of Ministry of Chemical Industry
Copyright reserved. No reproduction allowed
Book size 880×12301/16
Printing sheet 1V
Word count 27000
First edition in December 1991
First printing in December 1991
Print count 1500The barrel is an iron barrel lined with a polyethylene film bag, with a net weight of 40±0.2kg per barrel. If special packaging is required, the supply and demand parties shall negotiate separately.
During transportation and storage, it should not be close to any heat source and should be protected from violent impact and water ingress, 10
atmosphere pressure
906667
909333
912000
914667
917333
920000
922667
925333
928000
930 667
933333
936000
938667
941333
944000
946667
952000
954 667
957333Www.bzxZ.net
960000
962667
965333
HG2097—91
Appendix A
Gas volume conversion factor
(Supplement)
Table A1 Gas volume conversion to 20℃, 101325P18c
0:9342
HG2097-91
Appendix A
Gas volume conversion factor
(Supplement)
The conversion factor of this volume into 20℃, 101325Pa (1atm) is 8
0-8674
968000
970667
973 333 | | tt | | 976000 | :000
100267
100533
100800
101067 | | tt | 03733
104000
0.96130.9570
0.9716 10.9667
0.98120.9761
HG2097—91
Continued Table A1
0.94490.9397
0.9475 /0.9423
0.9663:0.961c
.0.9930
IHG2097-91
Continued Table A1
23 ℃
1:0042
Additional Notes
HG2097-91
This standard is proposed by the Department of Science and Technology of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of Shanxi Chemical Research Institute. This standard is drafted by Shanghai Xiangyang Chemical Factory. The main drafters of this standard are Zeng Guangmo, Lin Shengqi, Xu Wenqi, Cai Dan and Xue Weijing. From the date of implementation of this standard, the former Ministry of Chemical Industry of the People's Republic of China Standard HG2-1187-78 "Azodimethylamine (AC Foaming Agent)" will be invalidated.
People's Republic of China
Chemical Industry Standards
Vulcanization Accelerator CBS
Azodicarbonamide (Blowing Agent ADC)
HG2096~2097-91
Chemical Industry Standards Editorial Department
(Standardization Research Institute of Ministry of Chemical Industry)
Postal Code: 100013
Printing Standardization Research Institute of Ministry of Chemical Industry
Copyright reserved. No reproduction allowed
Book size 880×12301/16
Printing sheet 1V
Word count 27000
First edition in December 1991
First printing in December 1991
Print count 1500
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