Some standard content:
Chemical Industry Standard of the People's Republic of China
Food Additives
1 Subject Content and Scope of Application
Potassium Bromate
HG 2681-95
This standard specifies the technical requirements, test methods, inspection rules, and marking, packaging, transportation, and storage of potassium bromate, a food additive. This standard applies to potassium bromate, a food additive produced by electrolysis, which is mainly used as a flour improver. Molecular formula: KBrO:
Relative molecular mass: 167.00 (according to the international relative atomic mass in 1991)2
Cited standards
GB 190
GB 191
Dangerous goods packaging markingbZxz.net
Pictorial marking for packaging storage and transportation
GB/T601
GB/T 602
GB/T603
GB 2760
Preparation of standard solutions for titration analysis (volume analysis) of chemical reagentsPreparation of standard solutions for determination of impurities of chemical reagentsPreparation of preparations and products used in chemical reagent test methodsHygienic standards for the use of food additives
GB/T 6678
GB/T 6682
GB8450
GB8451
3 Technical requirements
General rules for sampling of chemical products
Specifications and test methods for water used in analytical laboratories Determination of arsenic in food additives
Test method for limits of heavy metals in food additives 3.1 Appearance: white crystalline granules or crystalline powder. 3.2 The food additive potassium bromate shall meet the requirements of the following table: Item
Potassium bromate (KBrO,) content, %
Bromide content
Free acid or free base content
Heating loss (105±2℃), %
As content, %
Heavy metal (as Pb) content, %
Approved by the Ministry of Chemical Industry of the People's Republic of China on April 5, 1995 578
99.0~101.0
Implementation on January 1, 1996
4 Test method
HG 2681—95
The reagents and water used in this standard, unless otherwise specified, refer to analytical pure reagents and grade 3 water specified in GB/T6682. The standard titration solution, impurity standard solution, preparation and product used in the test, unless otherwise specified, shall be prepared in accordance with the provisions of GB/T601, GB/T602 and GB/T603. 4.1 Identification test
4.1.1 Identification of potassium salt
Potassium salt is lavender in the flame color reaction test. When the flame is yellow, it is reddish purple when observed with cobalt glass. 4.1.2 Identification of bromate
When 5-6 drops of freshly prepared sodium nitrite solution (1+10) are added to the nitric acid solution (1+20) of bromate, it turns yellow to reddish brown; add 1 mL of chloroform to the mixed solution and shake it, and the chloroform layer turns yellow to reddish brown. 4.2 Determination of potassium bromate content
4.2.1 Method summary
After potassium bromate reacts with potassium iodide in an acidic solution to precipitate iodine, it is titrated with a sodium thiosulfate standard titration solution. The reaction formula is as follows:
BrO:+61-+6H+=312+3H2O+Br
12+2S20-=S,0-+21
4.2.2 Reagents and materials
4.2.2.1 Potassium iodide (GB/T1272);
4.2.2.2 Hydrochloric acid (GB/T622): 1+1 solution; 4.2.2.3 Sodium thiosulfate (GB/T637): c(NazS,O3)=0.1mol/L standard titration solution; 4.2.2.4 Soluble starch: 5g/L solution. 4.2.3 Analysis steps
Weigh about 1g of sample (accurate to 0.0002g), place in a 250mL beaker, dissolve with water, transfer to a 250mL volumetric flask, dilute to scale, and shake well. Use a pipette to transfer 25mL of the test solution into a 500mL iodine volumetric flask, add 2g of potassium iodide, 5mL of hydrochloric acid solution, shake well, add water to seal the bottle and place in a dark place for 5min, add 150mL of water below 10℃, titrate with sodium thiosulfate standard titration solution, add 3mL of starch solution when close to the end point, and continue titrating until the blue disappears. Perform a blank test at the same time. 4.2.4 Expression of analytical results
The potassium bromate content (X,) expressed as mass percentage shall be calculated according to formula (1): X1 - c(VV)X0. 027 83 x
-the volume of sodium thiosulfate standard titration solution consumed in titrating the test solution, mL; Wherein: Vi—
V2-the volume of sodium thiosulfate standard titration solution consumed in titrating the blank test solution, mL; (1)
-the actual concentration of the sodium thiosulfate standard titration solution, mol/L; 0.02783-.-the mass of potassium bromate in grams equivalent to 1.00 mL of sodium thiosulfate standard titration solution Cc(NazS,O)=1.000 mol/LJ;
the mass of the sample, g.
4.2.5 Allowable difference
The arithmetic mean of the parallel determination results shall be taken as the determination result, and the absolute difference of the parallel determination results shall not exceed 0.3%. 4.3 Determination of bromide content
4.3.1 Reagents and materials
4.3.1.1 Sulfuric acid (GB/T625): 1+32 solution; 579
4.3.1.2 Methyl orange: 1g/L solution;
4.3.2 Analysis steps
HG 2681---95
Weigh 2.00g of sample (accurate to 0.01g), place it in a 100ml beaker, add 40ml of water to dissolve, add 0.25mL of sulfuric acid solution, add 1 drop of methyl orange indicator solution to show red, and shake the solution again until the color does not disappear immediately. 4.4 Determination of free acid or free base content
4.4.1 Reagents and materials
4.4.1.1 Sodium hydroxide (GB/T629): c(NaOH) about 0.01mol/L solution; 4.4.1.2 Hydrochloric acid (GB/T 622): c(HCI) about 0.01mol/L solution; 4.4.1.3 Phenol: 10g/L ethanol solution.
4.4.2 Analysis steps
Weigh 5.00g of sample (accurate to 0.01g), place it in a 100mL beaker, add 60mL of freshly boiled and cooled water, and heat to dissolve. After cooling, add 3 drops of phenolphthalein indicator solution, and treat the solution as follows: a. If the solution is colorless, add 1.2mL of sodium hydroxide solution, it will turn red; b. If the solution is red, add 0.4mL of hydrochloric acid solution, and the red color will disappear. 4.5 Determination of heating loss
4.5.1 Instruments and equipment
Weighing bottle: Φ50mm×30mm.
4.5.2 Analysis steps
Weigh about 2g of sample (accurate to 0.0002g), place it in a weighing bottle with constant weight, move it into an electric constant temperature drying oven, heat it at 105±2C for 2h, take it out and put it in a desiccator to cool to room temperature, and weigh it. 4.5.3 Expression of analysis results
The heating loss (X,) expressed as mass percentage is calculated according to formula (2): X,=mi=m2×100
Where: m-mass of weighing bottle and sample before heating, g; mass of weighing bottle and sample after heating, g; mz—
m——mass of sample, g.
4.5.4 Allowable difference
The arithmetic mean of the parallel determination results shall be taken as the determination result. The absolute difference of the parallel determination results shall not exceed 0.1%. 4.6 Determination of arsenic content
(2)
Weigh 0.50g of sample (accurate to 0.01g). Add 5mL of water and heat to dissolve, add 5mL of hydrochloric acid, evaporate to dryness on a water bath, and add 5mL of water to dissolve, as the test solution.
The following determination is carried out according to the arsenic spot method in GB8450. Preparation of standard color spots: Use a pipette to transfer 1.50mL of arsenic standard solution (1mL of solution contains 1.0μgAs), place it in the wide-mouth bottle of the arsenic analyzer, and treat it in the same way as the sample. 4.7 Determination of heavy metal content
Weigh 2.00g sample (accurate to 0.01g), add 10mL water and heat to dissolve, add 10mL hydrochloric acid, evaporate to dryness on a water bath, add 20ml, dissolve in water, add 2mL acetic acid (1+19) solution, add water to 50mL, as the test solution. The following determination is carried out according to GB8451.
Preparation of standard colorimetric solution: Use a pipette to transfer 2mL of lead standard solution (1mL solution contains 10μgPb), and treat it in the same way as the sample.
5 Inspection rules
5.1. Potassium bromate, a food additive, shall be inspected by the quality supervision and inspection department of the manufacturer in accordance with the provisions of this standard. The manufacturer shall ensure that all products shipped out of the factory meet the requirements of this standard. Each batch of products shipped out of the factory shall be accompanied by a quality certificate. The content includes: manufacturer name, factory address, product name and "food additive", net weight, batch number or production date, food hygiene license number, production license number, proof that product quality complies with this standard and this standard number. 5.2 The user has the right to accept the received food additive potassium bromate in accordance with the provisions of this standard: 5.3 Each recrystallization product is a batch. 5.4 Determine the number of sampling units in accordance with Article 6.6 of GB/T6678. When sampling, insert the sampler from the vertical line of the center of the packaging bag to ?3/4 of the depth of the material layer. After mixing the sample, reduce it to about 500g by quartering method and pack it in two clean and dry wide-mouth bottles with stoppers and seal them. Stick labels on the bottles and indicate: manufacturer name, product name, batch number, sampling date and name of the sampler. One bottle is used for inspection and the other bottle is kept for three months for reference.
5.5 If any index of the inspection result does not meet the requirements of this standard, the sample should be taken from the double amount of packaging for verification. If even one index of the inspection result does not meet the requirements of this standard, the whole batch of products cannot be accepted. 5.6 When the supply and demand parties have objections to the product quality, they shall be handled in accordance with the provisions of the "Product Quality Law of the People's Republic of China". 6 Marking, packaging, transportation and storage
6.1 The packaging of potassium bromate, a food additive, shall be firmly and clearly marked, including: the name of the manufacturer, the address of the factory, the name of the product and the words "food additive", net weight, batch number or production date, shelf life, trademark, food hygiene license number, production license number, proof that the product quality meets this standard and the number of this standard, as well as the mark 11 "oxidant" specified in GB190 and the mark 4 "heat-afraid" and mark 7 "moisture-afraid" specified in GB191.
6.2 Potassium bromate, a food additive, is packaged in three layers. The inner packaging is a two-layer polyethylene plastic film bag for food, and the thickness shall not be less than 0.05mm. Specification size: 1000mm×800mm, net weight of each bag is 50kg. The outer packaging is iron drum, and its performance and inspection method shall comply with relevant regulations. If the user has other requirements for packaging, they shall be negotiated to resolve. 6.3 For the packaging of food additive potassium bromate, the inner bag shall be tied tightly with two layers of binding rope; the outer packaging shall be sealed with a cover. 6.4 Food additive potassium bromate shall be covered during transportation to prevent rain and moisture. It shall not be mixed with toxic and hazardous substances. Transportation requirements: According to the secondary oxidant, hazard regulation No. 23019 shall be implemented. 6.5 Food additive potassium bromate shall be stored in a cool and dry place to prevent rain and moisture. Prevent sun exposure and heat. It shall not be mixed with toxic and hazardous substances. 6.6 The shelf life of the product is two years from the date of production. If it is overdue, it shall be re-inspected to see if it meets the requirements of this standard. 7 Safety requirements
7.1 Potassium bromate is a strong oxidant. Potassium bromate solid cannot be mixed and ground with organic matter, sulfide and other easily oxidized substances. 7.2 According to GB2760, the maximum usage is 0.05g/kg. 581
A1 Instruments and equipment
HG 2681--95
Appendix A
Measurement of fineness
(reference)
A1.1 Test sieve (GB6003): R40/3 series, Φ200mmX50mm/0.180mm, with sieve bottom and sieve cover. A2 Analysis steps
Weigh about 50g of sample, accurate to 0.01g, put it in the test sieve with sieve bottom, cover the sieve cover, sieve manually at a frequency of 90 times/min for 2min, weigh the mass of the sieve residue, accurate to 0.01g. A3 Expression of analysis results
The fineness expressed as mass percentage (X.) is calculated according to formula (A1): X.
Where: m1——mass of sieve residue, g;
m-——mass of test material, g.
A4 allowable difference
The arithmetic mean of the parallel determination results is taken as the determination result, and the absolute difference of the parallel determination results shall not exceed 1.0%. Additional remarks:
This standard is proposed by the Technical Supervision Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Tianjin Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by the Tianjin Chemical Research Institute and Beijing Chemical Plant No. 4. The main drafters of this standard are Wang Shumin, Zhao Mingshan, Li Wenqiang and Liu Youruo. This standard is equivalent to the fifth edition (1986 edition) "Potassium Bromate" of the "Japanese Food Additive Code". 582
(AI)0%. Additional remarks:
This standard was proposed by the Technical Supervision Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of Tianjin Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by Tianjin Chemical Research Institute and Beijing Chemical Plant No. 4. The main drafters of this standard are Wang Shumin, Zhao Mingshan, Li Wenqiang and Liu Youruo. This standard is equivalent to the fifth edition (1986 edition) of "Potassium Bromate" of the "Japanese Food Additive Code". 582
(AI)0%. Additional remarks:
This standard was proposed by the Technical Supervision Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of Tianjin Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by Tianjin Chemical Research Institute and Beijing Chemical Plant No. 4. The main drafters of this standard are Wang Shumin, Zhao Mingshan, Li Wenqiang and Liu Youruo. This standard is equivalent to the fifth edition (1986 edition) of "Potassium Bromate" of the "Japanese Food Additive Code". 582
(AI)
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