Some standard content:
National Standard of the People's Republic of China
Food additives
Food additive-Calcium acetate1Subject content and scope of application
GB 15572-1995
This standard specifies the technical requirements, test methods, inspection rules and marking, packaging, transportation and storage conditions of food additive calcium acetate (calcium acetate).
This standard applies to calcium acetate obtained by reacting high-quality limestone with edible glacial acetic acid (fermentation method), which is used as a nutritional enhancer in the food industry.
2 Reference standards
Part II of the 1990 edition of the Pharmacopoeia of the People's Republic of China GB8450 Determination of arsenic in food additives 3 Chemical name, molecular formula, structural formula, molecular weight Chemical name: calcium acetate
Calcium acetate
Molecular formula: C, HOCa
Structural formula:
Molecular weight: 158.17 (according to the 1987 international atomic weight) 4
Technical requirements
4.1 Properties
This product is white needle-shaped crystals or crystalline powder, odorless, with acetic acid smell, and is very hygroscopic. This product is easily soluble in water and slightly soluble in ethanol. 4.2 Items and indicators
C, HO, Ca (anhydrous), %
Approved by the State Administration of Technical Supervision on June 2, 1995 280
98. 0~102. 0
1995-12-01Implementation
Sulfate, %
Chloride, %
Heavy metal (in terms of Pb), %
Arsenic salt (in terms of As), %
Magnesium salt and alkali metal salt, %
Water, %
Fluoride, %
5Test method
GB15572-1995
Comply with regulations
The reagents used in the tests of this standard are analytical reagents, water is distilled water or water of corresponding purity, and the solution is an aqueous solution. When the solution required for the determination is not specified, it shall be prepared according to the Appendix of Part II of the 1990 edition of the Pharmacopoeia of the People's Republic of China. The test instruments such as burettes, pipettes, and volumetric flasks used in the tests of this standard shall comply with the provisions of the current national standards and verification procedures for measuring instruments.
5.1 Identification
5.1.1 Reagents and solutions
5.1.1.1 Hydrochloric acid (GB 622).
Sulfuric acid (GB625).
Ferrous chloride (HG 3—1085).
5.1.1.4 Ammonium oxalate (HG3—976): 4% solution. 5.1.1.5 Preparation of sample solution
Weigh 0.1 g of sample and dissolve it in 20 mL of water. 5.1.2 Identification methodWww.bzxZ.net
5.1.2.1 Take 2 mL of sample solution (5.1.1.5) and add 1 drop of ammonium oxalate test solution to generate a white precipitate. 5.1.2.2 Take a platinum wire, wet it with hydrochloric acid, burn it on a colorless flame until it is colorless, then dip it in the sample solution (5.1.1.5), burn it on a colorless flame, the flame is brick red.
5.1.2.3 Take 0.2g of the sample, add 0.5mL of sulfuric acid, heat it, and the special odor of acetic acid will be generated. 5.1.2.4 Take 2mL of the sample solution (5.1.1.5), add 1 drop of ferric chloride test solution, the solution is dark red, add dilute hydrochloric acid, and the red color will fade. 5.2 Content determination
5.2.1 Principle
Add triethanolamine solution to the sample to mask Fe3+, A13+, Mn2+ ions, add sodium hydroxide test solution to make the solution pH greater than 12, Mg2+ forms Mg(OH)z precipitation, after eliminating interference, add calcipurpurogen indicator to this alkaline solution, and titrate calcium ions with disodium ethylene monoaminetetraacetic acid standard titration solution. Reaction formula: Ca2+→+H2Y2
5.2.2 Reagents and solutions
→CaY2-+2H+
5.2.2.1 Sodium hydroxide (GB629).
5.2.2.2 Triethanolamine (chemically pure): 20% solution. GB15572—1995
5.2.2.3 Disodium ethylenediaminetetraacetate (GB1401): 0.05 mol/L standard titration solution. 5.2.2.4 Calcium purpurogen.
5.2.3 Determination method
Weigh about 0.2 g of sample, accurate to 0.0002 g, add 100 mL of water to dissolve, add 5 mL of triethanolamine test solution, 15 mL of sodium hydroxide test solution, about 0.1 g of calcium purpurogen indicator, and then titrate with disodium ethylenediaminetetraacetate standard titration solution (0.05 mol/L) until the solution changes from red to pure blue.
5.2.4 Expression of analysis results
Calcium acetate content is expressed as mass percentage (X) and is calculated as follows: X - V + X0.158 2 × 100
m(1 - X2)
Wherein: X. Mass percentage of calcium acetate content, %; V - volume of disodium ethylenediaminetetraacetic acid standard titration solution, mL; C
Actual concentration of disodium ethylenediaminetetraacetic acid standard titration solution, mol/L; m - mass of sample, g;
Xz - mass percentage of water, %,
0.1582 - mass of calcium acetate expressed in grams equivalent to 1.00mL disodium ethylenediaminetetraacetic acid standard titration solution [c(EDTA)=1.00mol/L].
Note: The mass percentage of water is the result of 5.10. The result obtained shall be the arithmetic mean of two parallel determinations, retaining four significant figures. 5.2.5 Permissible difference
The relative deviation of the results of two parallel determinations shall not exceed 0.3%. 5.3 Determination of pH value of solution
Weigh 2.0g of sample and dissolve it in 100mL of water that has been freshly boiled and cooled to room temperature, and determine it according to page 44 of Appendix II of the 1990 edition of the Pharmacopoeia of the People's Republic of China.
5.4 Determination of sulfate
Weigh 0.1g of sample and dissolve it in 40mL of water, and check it according to page 48 of Appendix II of the 1999 edition of the Pharmacopoeia of the People's Republic of China. If turbidity occurs, its turbidity shall not exceed the turbidity of the control solution made with 1mL of standard potassium sulfate. 5.5 Determination of chloride
Weigh 0.1g of sample and dissolve it in 25mL of water, and check it according to page 48 of Appendix II of the 1991 edition of the Pharmacopoeia of the People's Republic of China. Compared with the control solution made with 5.0mL of standard sodium fluoride solution, it shall not be more concentrated. 5.6 Determination of heavy metals
Weigh 0.4g of sample, add 2mL of acetate buffer (pH 3.5) and appropriate amount of water to make 25mL, and check according to the first method on page 51 of the Appendix of Part II of the 199th edition of the Pharmacopoeia of the People's Republic of China. 5.7 Determination of arsenic salts
Weigh 1.0g of sample, and determine according to the arsenic spot method in GB8450. Sample treatment adopts nitric acid-sulfuric acid method. 5.8 Determination of magnesium salt and alkali metal salt
5.8.1 Reagents and solutions
5.8.1.1 Ammonium chloride (GB658).
5.8.1.2 Ammonium oxalate test solution: Take 3.5g of ammonium oxalate (HG3-976) and add water to dissolve it into 100mL. 5.8.1.3 Sulfuric acid (GB625).
5.8.2 Determination method
Weigh 1.0g of sample, add 40mL of water to dissolve, add 0.5g of ammonium chloride and boil for 1min, add 40mL of excess ammonium oxalate test solution to completely precipitate calcium, place in a water bath and heat for 1h. Let cool, add water to dilute to 100mL, filter, take 50mL of the clear filtrate, add 0.5mL of sulfuric acid, evaporate to dryness, and ignite to constant weight. The weight of the residue shall not exceed 5mg. 5.9 Determination of barium salt
5.9.1 Reagents and solutions
5.9.1.1 Calcium sulfate test solution: Take an appropriate amount of calcium sulfate (HG3903) and add water to make a saturated solution. 5.9.2 Determination method
Weigh 2.0g of sample, add 20mL of water to dissolve, filter, and divide the filtrate into two equal parts. Add 5mL of fresh calcium sulfate test solution to one part and 5mL of water to the other part. Let stand for 1h. It should be equally clear when compared with the control tube. 5.10 Determination of moisture
Weigh about 0.2g of sample, accurate to 0.0002g, and determine according to the Fischer method on page 55 of Appendix II of the 1990 edition of the Pharmacopoeia of the People's Republic of China.
5.11 Determination of fluoride
5.11.1 Reagents and solutions
5.11.1.1 Acetone.
5.11.1.2 70% perchloric acid.
5.11.1.3 10% sodium hydroxide solution.
5.11.1.4 0.2mol/L acetic acid standard solution. 5.11.1.51% phenolic acid indicator solution.
5.11.1.6 Dilute perchloric acid solution
Use 70%~72% perchloric acid and water to prepare a solution with a volume ratio of (1+100). 5.11.1.7 Alizarin aminocarboxylic acid complex solution
Weigh 0.04g of alizarin aminocarboxylic acid complex, add a small amount of 0.1mol/L sodium hydroxide solution to dissolve, neutralize with dilute perfluoric acid to orange-red (but not to form emulsion), dilute with water to 200mL, and shake to mix. 5.11.1.8 Acetic acid-sodium acetate buffer solution
Weigh 11.0g of anhydrous sodium acetate, add 30mL of 99% acetic acid and 170mL of water, and shake to dissolve. 5.17.1.9 Perchloric acid solution
Weigh 0.04g of lanthanum oxide, add 0.25mL of 70%~72% perchloric acid, dissolve in warm water, dilute with water to 50mL, and shake well. 5.11.1.10 Composite reagent
Measure 60.0ml of alizarin aminocarboxylate complex solution, 6.0ml of lanthanum perchlorate solution, and 20.0ml of acetic acid-sodium acetate buffer, and dilute to 200ml with water.
5.11.1.11 Fluoride impurity standard solution
Weigh 0.0221g of dry analytical pure sodium fluoride, dissolve, dilute to 1000ml, and store in a polyethylene plastic bottle. 5.11.2 Determination method
Weigh 5g of sample, accurate to 0.01g, and put it into a 50mL branch tube distillation flask, add 5mL70% perchloric acid, 15mL water and a few glass beads, connect the branch tube to the condenser, install a double-hole rubber stopper in the distillation flask, insert a 200℃ thermometer in each hole, the thermometer should be inserted into the liquid surface, install a small separating funnel in one hole, connect a capillary tube below, and insert the capillary tube below the liquid surface. Distill until the temperature reaches 135℃, accept One end of the tube is connected to the outlet of the condenser, and the other end is inserted below the liquid level of the receiving bottle. Keep the liquid temperature below 135-140℃ (controlled by adding water to the separatory funnel). Collect 70mL of distillate, neutralize with 10% sodium hydroxide until the phenol turns light pink, then neutralize with acetic acid (0.2mol/L) until colorless, dilute to 80mL, take 8mL, put it in a 25ml volumetric flask, add 5mL of compound reagent and 6mL of acetone, dilute with water to the scale, and shake well. After 25min, transfer to a dry colorimetric tube, and the blue-purple color should not be large. The standard is to take 2.5mL of fluoride impurity standard solution, add 10% sodium hydroxide, that is, one-tenth of the amount of 10% sodium hydroxide used when neutralizing the sample, and 8mL of water, add 1 drop of phenolic acid and treat it in the same way as the sample solution. 283
6 Inspection rules
GB 15572-1995
6.1 The finished product with uniformity after the final mixing is a batch. 6.2 This product shall be inspected by the quality inspection department of the manufacturer. 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. 6.3 The user unit may conduct quality inspection on the received products in accordance with the inspection rules and test methods specified in this standard. Check whether its indicators meet the requirements of this standard.
6.4 Sampling method and sampling quantity
The number of pieces per package, when the total number of pieces n<3, the sampling number is each piece; when the total number of pieces n≤300, the sampling number is√n+1; when the total number of pieces n>300, the sampling number is one+1. Take an equal amount of sample from each piece, use the quartering method to reduce the sample to 10 times the amount of the test, put it into a clean and dry glass bottle, and label it. One copy should be sent to the laboratory for inspection, and the other copy should be sealed and stored for arbitration analysis. 6.5 If one indicator does not meet the standard during the inspection, a new sample should be taken from twice the number of pieces for verification. If the product re-inspection result still fails to meet one indicator, the product will be judged as unqualified. 6.6 If the supply and demand parties have objections to the product quality, the two parties can negotiate to select an arbitration unit and conduct arbitration in accordance with the relevant provisions of this standard. 7 Marking, packaging, transportation and storage
7.1 The packaging should have a firm mark, which should at least include the words "food additives" and the product name, batch number, factory name, net weight, standard number, production license number, registered trademark, shelf life, etc. 7.2 This product is packed in double-layer plastic bags for food and packaged in plastic or cardboard drums. Each drum is 5kg, 25kg or packaged according to customer requirements. The packaging should meet the requirements of transportation and storage. 7.3 It must not be mixed with harmful substances during transportation, and prevent heavy pressure, collision, exposure to the sun and rain. 7.4 This product should be stored in a cool, dark and dry place and must not be mixed with toxic and harmful substances. 7.5 The shelf life of this product is two years under the original packaging conditions. Additional remarks:
This standard is proposed by the State Drug Administration
This standard is under the technical jurisdiction of the State Drug Administration China Pharmaceutical Industry Corporation and Tianjin Pharmaceutical Research Institute. This standard was drafted by Guangdong Jiulianshan Pharmaceutical Factory and Guangdong Gaishibao Co., Ltd. The main drafters of this standard are Liao Yuexing, Li Jiucheng, Xie Huiming and Xiong Qinghua. This standard is not equivalent to the US Food Chemical Codex FCC 1983 (General) standard. 2842 This product is packed in double-layer plastic bags for food and packaged in plastic or cardboard drums. Each drum is 5kg, 25kg or packaged according to customer requirements. The packaging should meet the requirements of transportation and storage. 7.3 It must not be mixed with harmful substances during transportation, and prevent heavy pressure, collision, exposure to the sun and rain. 7.4 This product should be stored in a cool, dark and dry place and must not be mixed with toxic and harmful substances. 7.5 The shelf life of this product is two years under the original packaging conditions. Additional notes:
This standard is proposed by the State Drug Administration
This standard is under the technical jurisdiction of the State Drug Administration China Pharmaceutical Industry Corporation and Tianjin Pharmaceutical Research Institute. This standard was drafted by Guangdong Jiulianshan Pharmaceutical Factory and Guangdong Gaishibao Co., Ltd. The main drafters of this standard are Liao Yuexing, Li Jiucheng, Xie Huiming and Xiong Qinghua. This standard is not equivalent to the US Food Chemical Codex FCC 1983 (General) standard. 2842 This product is packed in double-layer plastic bags for food and packaged in plastic or cardboard drums. Each drum is 5kg, 25kg or packaged according to customer requirements. The packaging should meet the requirements of transportation and storage. 7.3 It must not be mixed with harmful substances during transportation, and prevent heavy pressure, collision, exposure to the sun and rain. 7.4 This product should be stored in a cool, dark and dry place and must not be mixed with toxic and harmful substances. 7.5 The shelf life of this product is two years under the original packaging conditions. Additional notes:
This standard is proposed by the State Drug Administration
This standard is under the technical jurisdiction of the State Drug Administration China Pharmaceutical Industry Corporation and Tianjin Pharmaceutical Research Institute. This standard was drafted by Guangdong Jiulianshan Pharmaceutical Factory and Guangdong Gaishibao Co., Ltd. The main drafters of this standard are Liao Yuexing, Li Jiucheng, Xie Huiming and Xiong Qinghua. This standard is not equivalent to the US Food Chemical Codex FCC 1983 (General) standard. 284
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