Some standard content:
HG2683—1995
Chemical Industry Standard of the People's Republic of China
Food Additives
Phytic Acid (Inositol Hexaphosphate)
1 Subject Content and Scope of Application
HG2683—1995
This standard specifies the technical requirements, test methods, inspection rules, and marking, packaging, transportation and storage of food additive phytic acid (Inositol Hexaphosphate). This standard applies to products extracted, purified and concentrated by chemical methods using rice bran, corn and other plants as raw materials. This product is mainly used in the food industry as an antioxidant, preservative, fermentation promoter and chelating agent.
Molecular formula: C6H18O24P6
Structural formula:
OP(UH)2
(OH),FC
OP(OH)a
QP(OH)
OP(OH):
Relative molecular mass: 660.04 (according to the international relative atomic mass in 1991) 2 Reference standards
GB/T602 Preparation of standard solutions for determination of impurities in chemical reagents GB/T603 Preparation of reagents and products used in chemical reagent test methods GB/T6678 General rules for sampling of chemical products
GB/T6680 General rules for sampling of liquid chemical products GB/T8450 Determination method in food additives GB/T8451 Test method for limits of heavy metals in food additives GB/T9728 General method for determination of sulfate in chemical reagents GB/T9729 General method for determination of chloride in chemical reagents 3 Technical requirements
3.1 Appearance: Light yellow or light brown viscous liquid. Approved by the Ministry of Chemical Industry of the People's Republic of China on April 5, 1995 and implemented on January 1, 1996
HG2683-1995
Food additive phytic acid should meet the requirements of the following table: 3.2
Phytic acid (CeHi8O24P), %
Inorganic phosphorus (as P), %
Chloride (as CI), %
Sulfate (as SO4), %
Calcium salt (as Ca), %
Arsenic (as As), %
Heavy metal (as Pb), %
4 Test method
The reagents and water used in this standard, unless otherwise specified, shall use the analytical reagents of the current national standards or industry standards and meet the specifications of Grade 3 water in GB/T6682. The impurity standard solutions, preparations and products required in the test shall be prepared in accordance with the provisions of GB/T602 and GB/T603 unless otherwise specified.
4.1 Identification test
4.1.1 Reagents and materials
a. Sulfuric acid:
b. Hydrogen peroxide;
c. Ammonia solution: (2+3);
d. Calcium chloride solution: 75g/L;
e. Ammonium molybdate solution: 25g/L.
4.1.2 Analysis steps
a. Take a small amount of this product, neutralize it with ammonia solution, add a few drops of calcium chloride solution, and a white precipitate will occur. b. Take 0.2mL of this product, add 1mL of sulfuric acid, heat until completely carbonized, then add hydrogen peroxide until it is colorless and transparent, and add ammonium molybdate solution to turn yellow. 4.2 Determination of phytic acid content
4.2.1 Summary of method Quinmolybdate gravimetric method
Phytic acid is digested by perchloric acid and nitric acid to form phosphoric acid. In nitric acid medium, phosphoric acid reacts with quinmolybdate reagent to form yellow precipitate of quinoline phosphomolybdate. The phytic acid content in the sample can be calculated by filtering, washing, drying and weighing.
4.2.2 Reagents and Materials
a. Nitric acid;
b. Perchloric acid;
c. Nitric acid solution: (1+1);
d. Preparation of quinomolybdate reagent:
Weigh 70g of sodium molybdate and add 150mL of water to dissolve, which is solution I; weigh 60g of citric acid and add 150mL of water and 85mL of nitric acid to dissolve, and pour solution I into it under stirring, which is solution II; measure 100mL of water, add 35mL of nitric acid and 5mL of quinoline, slowly pour the mixture into solution II, let it stand for 24h, filter it into a 1L volumetric flask, add 280mL of acetone, dilute it to the scale with water, mix it well and store it in a plastic bottle, with a validity period of half a year.
4.2.3 Instruments
Sand core glass funnel or: G440mL.
4.2.4 Analysis steps
Approved by the Ministry of Chemical Industry of the People's Republic of China on April 5, 1995, and implemented on January 1, 1996
HG2683-1995
Weigh about 0.3g of the sample (accurate to 0.0002g), place it in a 300mL conical flask, add 10mL of nitric acid and 5mL of perchloric acid, heat it on an electric furnace in a fume hood, gradually increase the temperature to allow white smoke to escape until the solution is transparent and nearly dry, and cool it. Rinse the bottle wall with a small amount of water, transfer it quantitatively to a 100mL volumetric flask, and dilute it to the scale with water to obtain solution A.
Measure 20.0mL of solution A in a 300mL conical flask, add 80mL of water, 10mL of nitric acid solution, and 50mL of quinoline molybdate reagent, heat it in boiling water until the solution is clear, and cool it to room temperature. Filter by pouring method on the suction filtration device, transfer the precipitate quantitatively to the sand core glass funnel with constant weight, and wash the precipitate and the bottle wall with a small amount of water several times. Place the funnel in an oven at 120±2℃ and dry for 1h, cool to room temperature in a desiccator, and weigh.
4.2.5 Expression of analysis results
The percentage content (X) of phytic acid (CH1sO24P) is calculated according to formula (1): mX0.01400X3.552
-mass of precipitate, g;
Where: m
mass of sample, g;
Conversion coefficient of quinoline phosphomolybdate and phosphorus:
3.552Conversion coefficient of phosphorus and phytic acid:
The result should be expressed to one decimal place.
42.6Allowance
30.974×6).
The difference between the results of two parallel determinations shall not exceed 0.3%. The arithmetic mean shall be taken as the determination result. 4.3 Determination of inorganic phosphorus
4.3.1 Method Summary
Phosphombohedral blue colorimetric method
In the presence of a certain acidity and a reducing agent, the phosphomolybdenum yellow generated by the free phosphate in the phytic acid solution is reduced to phosphomolybdenum blue. The limit value of inorganic phosphorus is determined by visual colorimetry. a.4.3.2 Reagents and materials
b. Ammonia solution; (2+3);
c. Sulfuric acid solution: (1+6);
d. Ammonium molybdate solution: 25g/L;
e. Ascorbic acid solution: 100g/L, prepared immediately before use; f. Phosphorus standard solution: 0.01mgP/mL;
4.3.2 Analysis steps
Weigh 0.1g of the sample (accurate to 0.01g), place it in a 25mL colorimetric tube, add 5mL of water, and neutralize it with ammonia solution to pH=7 (pH test paper test). Add 1mL of sulfuric acid solution, 1mL of ammonium molybdate solution, and 1mL of ascorbic acid solution, dilute to the scale with water, place it in an ice bath (0~5℃) for 30min, and compare the colors visually. The blue color of the sample shall not be darker than the limit standard. The limit standard is to take 2.0 mL of phosphorus standard solution (each mL is equivalent to 0.01 mgP), add water to 5 mL, approved by the Ministry of Chemical Industry of the People's Republic of China on April 1, 1995 and implemented on January 1, 1996
HG2683-1995
and treat it in the same way as the test solution.
4.4 Determination of chloride
4.4.1 Reagents and materials
Ammonia solution: (2+3).
4.4.2 Analysis stepsWww.bzxZ.net
Weigh 0.5 g of the sample (accurate to 0.01 g), place it in a 25 mL colorimetric tube, add 20 mL of water, and neutralize it with ammonia solution to pH = 7 (pH test paper test). The rest is carried out in accordance with the provisions of GB/T9729. The limit standard is to take 1.0 mL of chloride standard solution (each mL is equivalent to 0.1 mgCl), add water to 20 mL, and treat it in the same way as the test solution.
4.5 Determination of sulfate
4.5.1 Reagents and materials
Ammonia solution: (2+3).
4.5.2 Analysis steps
Weigh 0.5g of the sample (accurate to 0.01g), place it in a 25mL colorimetric tube, add 20mL of water, and neutralize it with ammonia solution to pH=7 (pH test paper test). The rest is carried out in accordance with the provisions of GB/T9728. The limit standard is to take 1.0mL of sulfate standard solution (each mL is equivalent to 0.1mgSO4), add water to 20mL, and treat it in the same way as the test solution.
4.6 Determination of calcium salt
4.6.1 Method Summary
Calcium Oxalate Turbidimetric Method
In acetic acid medium, trace calcium ions and oxalate ions form insoluble calcium oxalate suspension, and the limit value of calcium is determined by visual turbidimetry.
4.6. 2 Reagents and Materials
a. Acetic acid 36%;
b. Ammonia solution: (2+3);
c. Ammonium oxalate solution: 40g/L;
d. Calcium standard solution: 0.1mgCa/mL.
4.6.3 Analysis Steps
Weigh 0.5g of the sample (accurate to 0.01g), put it in a 25mL colorimetric tube, add 10mL of water, and neutralize it with ammonia solution to pH=7 (pH test paper test). Add 1mL of acetic acid and 5mL of calcium oxalate solution, dilute to the scale with water, and let it stand for 10min before turbidity measurement. The turbidity presented shall not be greater than the standard. The limit standard is to take 1.0mL of calcium standard solution (each mL is equivalent to 0.1mgCa), add water to 10mL, and treat it in the same way as the test solution.
4.7 Determination of arsenic
Analysis steps:
Weigh 1.0g of the sample, place it in a 100mL ground-mouth conical flask, add 10mL of water, and the limit standard is to take 3.0mL of arsenic standard solution (each mL is equivalent to 0.001mgAs), add water to 10mL. The rest is carried out according to the arsenic spot method in GB/T8450.
4.8 Determination of heavy metal content
4.8.1 Reagents and solutions
a. Acetic acid 36%;
b. Ammonia solution: (2+3);
c. Sodium sulfide solution: weigh 5g of sodium sulfide, add 10mL of water and 30mL of glycerol to dissolve, valid for three months;
d. Lead standard solution: 0.01mgPb/mL. Take 0.1mgPb/mL in a 100mL volumetric flask, approved by the Ministry of Chemical Industry of the People's Republic of China on April 1, 1995, and implemented on January 1, 1996
HG2683-1995
dilute to the scale.
4.8.2 Sample treatment shall be carried out according to the wet digestion method in 5.2.1 of GB/T8451. 4.8.3 Analysis steps
Take 5mL of the sample solution in 4.8.2 and place it in a 25mL colorimetric tube, dilute it with water to 20mL, add ammonia solution to neutralize it to pH=7~8 (pH test paper test), add 0.2mL of acetic acid, and filter it if necessary. Add 2 drops of sodium sulfide solution, dilute it with water to the scale, shake it well, place it in a dark place for 5min, and compare the color on a white background. The dark color should not be greater than the limit standard.
The limit standard is to take 2.0mL of lead standard solution (each mL is equivalent to 0.01mgPb), add water to 20mL, and treat it in the same way as the test solution.
5 Test rules
5.1 Food additive phytic acid should be inspected by the quality inspection department of the manufacturer. The manufacturer should ensure that the quality of all products shipped meets the requirements of this standard and be accompanied by a quality certificate in a certain format. The contents include: product name, manufacturer name, factory address, batch number, production date, product net weight, this standard number, production license number and warranty period.
5.2 The user has the right to inspect and accept the received products according to this standard, and the inspection and acceptance should be carried out within 10 days after arrival.
5.3 Uniform products produced at one time are considered a batch. 5.4 The sampling volume and sampling method shall be implemented in accordance with Article 6.6 of GB/T6678 and Chapter 2 of GB/T6680. The 200g sample taken shall be divided into two clean and dry ground-mouth or plastic bottles, the bottle mouths shall be sealed, and labels shall be attached to the bottles. Indicate: manufacturer name, product name, batch number, sampling date and sampler. One bottle is for inspection and one bottle is kept for three months for future reference. 5.5 If one of the indicators in the test results does not meet the requirements of this standard, samples should be taken from twice the amount of packaging for re-inspection. If one of the indicators still does not meet the requirements of this standard after re-inspection, the entire batch of products will not 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
61 The words "food additive" and the following content should be marked on the outer packaging of this product: manufacturer name, factory address, product name, trademark, specification, batch number, net weight, production date, this standard number and production license number.
6.2 Food additive phytic acid is packaged in polyethylene plastic barrels. The net weight of each barrel is 1, 5, 10 and 20kg, plus corrugated paper boxes or wooden boxes, and can also be packaged according to user needs. 6.3 Do not turn the barrel upside down during transportation, prevent it from being exposed to the sun and rain, load and unload it gently, prevent the packaging from being damaged, and do not mix it with toxic and harmful items.
6.4 This product should be stored in a cool, dark, ventilated place. It should not be piled in the open air and should not be mixed with toxic and harmful substances to avoid contamination. The shelf life is one year. If the sampling test results still meet the requirements of this standard after one year, it can continue to be used.
Additional instructions:
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 technical jurisdiction of the Beijing Chemical Research Institute of the Ministry of Chemical Industry and the Food Hygiene Supervision and Inspection Institute of the Ministry of Health. This standard was drafted by Yixing Shanjuan Phytic Acid Factory and approved by the Ministry of Chemical Industry of the People's Republic of China on April 5, 1995 and implemented on January 1, 1996.
HG2683—1995
The main drafters of this standard are: Zhang Hailiang, Ma Dan, Bai Hongyu, and Zhang Zuming. Approved by the Ministry of Chemical Industry of the People's Republic of China on April 5, 1995 and implemented on January 1, 1996.6 and Chapter 2 of GB/T6680. The 200g sample is divided into two clean and dry ground-mouth or plastic bottles, the bottle mouths are sealed, and labels are affixed to the bottles. Note: manufacturer name, product name, batch number, sampling date and sampler. One bottle is for inspection and one bottle is kept for three months for future reference. 5.5 If one indicator of the inspection result does not meet the requirements of this standard, re-samples should be taken from twice the amount of packaging for re-inspection. If one item still does not meet the requirements of this standard after re-inspection, the entire batch of products will not 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
61 The words "food additives" and the following content should be marked on the outer packaging of this product: manufacturer name, address, product name, trademark, specification, batch number, net weight, production date, this standard number and production license number.
6.2 Food additive phytic acid is packaged in polyethylene plastic barrels. The net weight of each barrel is 1, 5, 10 and 20 kg, plus corrugated boxes or wooden boxes, and can also be packaged according to user needs. 6.3 Do not turn the barrel upside down during transportation, prevent it from being exposed to the sun and rain, and load and unload it gently to prevent the packaging from being damaged. It cannot be transported together with toxic and harmful items.
6.4 This product should be stored in a cool, dark, ventilated and dark place. It should not be piled in the open air, and it must not be mixed with toxic and harmful substances to avoid contamination. The shelf life is one year. If the sampling test results still meet the requirements of this standard after one year, it can continue to be used.
Additional instructions:
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 technically managed by the Beijing Chemical Research Institute of the Ministry of Chemical Industry and the Food Hygiene Supervision and Inspection Institute of the Ministry of Health. This standard was drafted by Yixing Shanjuan Phytic Acid Factory. Approved by the Ministry of Chemical Industry of the People's Republic of China on April 5, 1995 and implemented on January 1, 1996.
HG2683-1995
The main drafters of this standard are Zhang Hailiang, Ma Dan, Bai Hongyu and Zhang Zuming. Approved by the Ministry of Chemical Industry of the People's Republic of China on April 5, 1995 and implemented on January 1, 1996.6 and Chapter 2 of GB/T6680. The 200g sample is divided into two clean and dry ground-mouth or plastic bottles, the bottle mouths are sealed, and labels are affixed to the bottles. Note: manufacturer name, product name, batch number, sampling date and sampler. One bottle is for inspection and one bottle is kept for three months for future reference. 5.5 If one indicator of the inspection result does not meet the requirements of this standard, re-samples should be taken from twice the amount of packaging for re-inspection. If one item still does not meet the requirements of this standard after re-inspection, the entire batch of products will not 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
61 The words "food additives" and the following content should be marked on the outer packaging of this product: manufacturer name, address, product name, trademark, specification, batch number, net weight, production date, this standard number and production license number.
6.2 Food additive phytic acid is packaged in polyethylene plastic barrels. The net weight of each barrel is 1, 5, 10 and 20 kg, plus corrugated boxes or wooden boxes, and can also be packaged according to user needs. 6.3 Do not turn the barrel upside down during transportation, prevent it from being exposed to the sun and rain, and load and unload it gently to prevent the packaging from being damaged. It cannot be transported together with toxic and harmful items.
6.4 This product should be stored in a cool, dark, ventilated and dark place. It should not be piled in the open air, and it must not be mixed with toxic and harmful substances to avoid contamination. The shelf life is one year. If the sampling test results still meet the requirements of this standard after one year, it can continue to be used.
Additional instructions:
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 technically managed by the Beijing Chemical Research Institute of the Ministry of Chemical Industry and the Food Hygiene Supervision and Inspection Institute of the Ministry of Health. This standard was drafted by Yixing Shanjuan Phytic Acid Factory. Approved by the Ministry of Chemical Industry of the People's Republic of China on April 5, 1995 and implemented on January 1, 1996.
HG2683-1995
The main drafters of this standard are Zhang Hailiang, Ma Dan, Bai Hongyu and Zhang Zuming. Approved by the Ministry of Chemical Industry of the People's Republic of China on April 5, 1995 and implemented on January 1, 1996.
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