Some standard content:
Chemical Industry Standard of the People's Republic of China
HG 2341 - 92
Brominated Bisphenol
Published on June 1, 1992
Ministry of Chemical Industry of the People's Republic of China
Implemented on July 1, 1993
Chemical Industry Standard of the People's Republic of China
Subject Content and Scope of Application
HG2341-92
This standard specifies the technical requirements, test methods, inspection rules, as well as marking, packaging, transportation and storage of tetrabromobisphenol A. This standard applies to tetrabromobisphenol A made from bisphenol A and bromine. This product is mainly used as a flame retardant for polymer materials. Molecular formula: Cr5H,2BrO2
Relative molecular mass: 543.86 (according to the international relative atomic mass in 1989)Molecular structure:
2 Reference standards
GB6678
GB6682
3 Technical requirements
Packaging, storage and transportation pictorial signs
Chemical reagents
Chemical reagents
Chemical reagents
Preparation of standard solutions for titration analysis (volume analysis) Preparation of preparations and products used in test methods General method for colorimetric determination
Chemical reagents General method for determination of melting point range General rules for sampling of chemical products
Specifications for laboratory water
3.1 Appearance: white or light yellow crystalline powder 3.2 Tetrabromobisphenol A should comply with Table 1 Requirements:
Bromine content, %
Melting point (initial melting point),
Heating loss, %
Chroma, fumigation
Approved by the Ministry of Chemical Industry of the People's Republic of China on June 1, 1992Superior product
First-class product
Qualified product
Implemented on July 1, 1993
4 Test method
HG2341-92
The reagents and water used in this standard, unless otherwise specified, refer to analytical reagents and meet the specifications of grade 3 water in GB6682.
The preparation of standard titration solutions used in this standard shall be carried out in accordance with GB601. The preparation of indicators used in this standard shall be carried out in accordance with GB603. 4.1 Appearance -
Visual inspection.
4.2 Determination of bromine content
4.2.1 Alkali fusion mercury method (arbitration method)
Reagents and solutions
95% ethanol (GB.679);
Sodium hydroxide (GB629) and 4g/L solution; nitric acid (GB626): 1+1 and 1+160 solutions; diphenylazocarbohydrazide ethanol solution: 5g/L; bromophenol blue indicator solution: 4g/L;
Chlorine Standard titration solution of sodium chloride: c(NaCl)=0.1mol/L; Standard titration solution of mercuric nitrate: c(1/2Hg(NO,)2)=0.1mo1/L g
Weigh 16.2g mercuric nitrate (accurate to 0.1g), add 6mL1+1 nitric acid and 50mL water in a 200mL beaker, stir to dissolve, filter if necessary, transfer to a volumetric flask, dilute to the scale with water, mix well, and calibrate. : Pipette 20mL of sodium chloride standard titration solution into a 250mL conical flask, add 50mL of water, add three drops of bromophenol blue indicator solution, neutralize with 1+160 nitric acid until it turns yellow, and add 6 to 8 drops in excess, add 1mL of diphenylazocarbonyl hydrazide, and titrate with mercuric nitrate standard titration solution until the color changes from yellow to purple-red. The actual concentration (c) of the mercuric nitrate standard titration solution is calculated according to formula (1): C
Wherein: V is the volume of mercuric nitrate standard titration solution consumed Volume, mL.4.2.1.2 Instruments and equipment
General laboratory instruments and high temperature furnace, 30mL nickel pot, 25mL brown burette.(1)
4.2.1.3 Determination steps
Weigh 0.2 (accurate to 0.0001g) of the sample, add 3g of sodium hydroxide to 30mL nickel alkali, add 8-10 drops of water, shake the crucible so that the sample is wrapped in the alkali solution, and place it on an electric furnace with a voltage regulator. Dissolve with slight heat and evaporate the water. Gradually increase the furnace temperature. When the sample decomposes and carbonizes, do not let it splash out with carbon dioxide bubbles. When the sample is basically carbonized and stops bubbling, move the crucible into a high-temperature furnace at 300℃, continue to raise the temperature to 700℃, and melt for another 10 minutes. Take it out, cool it, put it in a 200mL beaker, add 40mL water, heat it slightly to dissolve it, wash it, make the total volume about 80mL, add 3 drops of bromophenol blue indicator solution, use 1+1 nitric acid solution to neutralize the excess alkali, then use 4g/L sodium hydroxide solution and 1+160 nitric acid solution to neutralize it until it turns slightly yellow and add 6~8 drops of 1+160 nitric acid solution in excess, add 1mL of diphenylamine carbohydrazide indicator solution, and titrate it with mercuric nitrate standard titration solution until the color changes from yellow to purple-red as the end point. At the same time, do a blank test.
4.2.1.4 Expression and calculation of results
The mass percentage of bromine x is calculated according to formula (2): (V, -V,) c× 0. 799
HG2341-92
Wherein: Y—the volume of the standard mercuric nitrate solution consumed in the titration of the blank test solution, mL; V—the volume of the standard mercuric nitrate solution consumed in the titration of the sample solution, mL; —-the actual concentration of the standard mercuric nitrate solution, mol/L; m-—the mass of the sample, g;
0.0799——the mass of bromine expressed in c grams per 1.00mL of the standard mercuric nitrate solution.
Hg(NO）=1.000mol/L, the difference between the parallel determination results in 4.2.1.5 allowable difference
shall not exceed 0.3%, and the arithmetic mean shall be taken as the determination result. 4.2.2 Oxygen bottle combustion mercury method
4.2.2.1 Reagents and solutions
Hydrogen peroxide (GB6684):
Sodium hydroxide (GB629) solution: 20g/L; b.
Nitric acid (GB626) solution: 1+30;
Standard mercuric nitrate titration solution: c (1/2Hg(NO3)2) = 0.01mol/L (quantitatively dilute the standard mercuric nitrate solution in 4.2.1.1g by 10 times).
4.2.2.2 Apparatus and equipment
Oxygen combustion bottle: 500mL, with platinum wire (mesh) or nickel-chromium wire (mesh) welded on the standard ground-mouth plug; a.
Analytical balance: minimum scale value 0.01mgbZxz.net
Oxygen cylinder with pressure gauge (filled with oxygen): c.
d.25mL brown burette
4.2.2.3 Determination steps
Weigh 0.015g of the sample (accurate to 0.00001g), put it in a small piece of ash-free filter paper and wrap it up, lead out a paper tail, clamp it on the platinum wire (mesh) or nickel-chromium wire (mesh), then ignite the paper tail, and quickly put it into 2mL sodium hydroxide solution (20g/L) and 10mL water (with 1mL of industrial peroxide added in it) in advance. Put the sample in a combustion bottle filled with oxygen and filled with hydrogen, cover the bottle stopper, let the sample burn completely, shake and leave for 30 minutes to make it completely absorbed (complete absorption means no smoke in the bottle), open the bottle stopper, rinse the platinum wire (net) and the bottle wall with about 15mL of water, heat on an electric furnace to decompose the excess hydrogen peroxide, and concentrate the test solution to about 5mL, cool to room temperature, add three drops of bromophenol blue indicator solution (4.2.1.1.e), neutralize the excess alkali with 1+30 nitric acid solution, then neutralize with 1+160 nitric acid solution and 4g/L sodium hydroxide solution until it turns slightly yellow, add 4~6 drops of excess 1+160 nitric acid solution, add 20mL of ethanol (95%), add 7~8 drops of diphenylazocarbohydrazide indicator solution, and titrate with standard mercuric nitrate titration solution until the color changes from yellow to purple-red. Perform a blank test at the same time. 4.2.2.4 Expression and calculation of results
The calculation of mass percentage of bromine is the same as that in 4.2.1.4. 4.2.2.5 Allowable difference
The difference between the results of two parallel determinations shall not exceed 0.5%. The arithmetic mean shall be taken as the determination result. 4.3 Determination of melting point
According to GB617, use the round-bottom flask instrument in Figure 3 and read the initial melting temperature. 4.4 Determination of heating loss
4.4.1 Instruments and equipment
4.4.1.1 Electric drying oven: capable of controlling the temperature at 105~110℃4.4.1.2 Weighing bottle: 50mm in diameter, 30mm in height, 4.4.2 Determination steps
Weigh 5g of the sample (accurate to 0.0001g), place it in a constant-weight weighing bottle, place it in an electric drying oven at 105~110℃, keep it for 2h, take it out and place it in a desiccator, cool it to room temperature (about 30min) and weigh it. 4.4.3 Expression and calculation of results
The percentage of mass loss on heating x is calculated according to formula (3): m,-m
wherein: mo is the mass of the empty weighing bottle, g;
m,—the mass of the weighing bottle and the sample before heating, g,- The mass of the weighing bottle and the sample after heating, g.m2
4.4.4 Allowable difference
The difference between the two measurement results shall not be greater than the allowable difference in Table 2, and the arithmetic mean shall be taken as the measurement result. Table 2
Heating loss
4.5 Determination of chromaticity
4.5.1 Sample preparation
Weigh 10g of sample (accurate to 0.1g), dissolve it in 50mL of methanol and shake well. 4.5.2 Determination steps
Perform according to GB605,
4.5.3 Allowable difference
%(m/m)
When the chromaticity is not greater than 80 dark blues and the difference between two determination results is not greater than 5 dark blues, take the arithmetic mean as the determination result. 5 Testing rules
5.1 Tetrabromobisphenol A shall be inspected by the quality inspection department of the manufacturer in accordance with this standard. The manufacturer shall ensure that each batch of products leaving the factory meets the requirements of this standard. Each batch of products leaving the factory shall be accompanied by a quality certificate, the contents of which shall include: manufacturer name, product name, quality grade, date of manufacture, batch number, net weight and number of this standard. 5.2 The user shall have the right to conduct quality inspection on the received products in accordance with the provisions of this standard to check whether they meet the requirements of this standard. If one indicator of the inspection result does not meet the requirements of this standard, samples shall be taken from twice the amount of packaging for re-inspection. If even one indicator of the re-inspection result does not meet the requirements of this standard, the whole batch of products shall not be accepted. 5.3 When the supply and demand parties have objections to the product quality, the national statutory monitoring unit shall conduct arbitration in accordance with the provisions of this standard (the determination of bromine content shall be based on the alkali fusion mercury method).
5.4 The weight of each batch of products shall not exceed 5t.
5.5 Sampling method
The number of sampling bags shall be selected as specified in Table 3,
Total number of packages in each batch
82~101
102125
126~151
152~181
182~216
HG2341-92
Minimum number of sampling bags selected
Total number
Insert the sampler (GB6679 Figure A, sampling probe) into the selected package along the vertical center line at half its depth for sampling. The total amount of sampling shall not be less than 1000g. After mixing the samples, select 250g of the sample by quartering method and divide it into two clean and dry wide-mouth bottles or plastic bottles, seal them, stick labels, indicate the manufacturer's name, product name, grade, batch, sampling date and name of the sampler, one bottle is inspected by the quality inspection department, and the other bottle is kept for three months for future reference. 5.6 The inspection results shall be determined according to the rounded value comparison method in GB1250. 6 Marking, packaging, transportation and storage
6.1 The packaging bag should have a firm mark, which includes: manufacturer's name, product name, batch number, quality grade, production date, net weight, this standard number and trademark, and printed with Figure 6 "moisture-averse mark" specified in GB191. 6.2 Tetrabromobisphenol A is packaged in plastic woven bags lined with plastic bags, and the net weight of each bag is 25kg. 6.3 This product should be protected from moisture, rain and bag breakage during transportation. 6. 4 This product should be stored in a dry warehouse to prevent rain and sunlight. The storage period is 2 years. After the storage period, it can still be used after passing the quality re-inspection.
Additional instructions:
This standard was proposed by the Science and Technology Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Shanxi Chemical Research Institute. This standard was drafted by the Tainan Salt Field Chemical Plant of Jiangsu Province. The main drafters of this standard are Cheng Dewen, Li Guangguo, and Xue Jianhua.
Chemical Industry Standard of the People's Republic of China
Bromobisphenol A.
HG 234192
Editor: Chemical Industry Standards Editorial Department
(Standardization Research Institute of the Ministry of Chemical Industry)
Postal Code: 100013
Printer: Standardization Research Institute of the Ministry of Chemical Industry
Copyright reserved. No reproduction allowed
Format: 880×12301/16 Number of words on a sheet: 10000 First edition in December 1992
First printing in December 1992
Print run: 1500
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