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Record number: 3720-1999
HG 2927-1999
This standard is equivalent to the sixth edition of the Japanese Food Additives Code (1992) [JSFA-V (1992) "Calcium Dihydrogen Phosphate" revised from the chemical industry standard HG2927--1989 "Food Additive Calcium Dihydrogen Phosphate". The main technical differences between this standard and JSFA-V "Calcium Dihydrogen Phosphate" are: the content of calcium dihydrogen phosphate in JSFA-V is calculated as Ca(H,PO)2, and the content of calcium dihydrogen phosphate in this standard is calculated as Ca. 1. According to my country's requirement that toxic and harmful impurities in food additives must be monitored, the fluoride content index is added, and the determination method adopts the lanthanum nitrate-distillation colorimetric method.
——The determination of arsenic and heavy metal content adopts the general test method of food additives in my country. The main technical differences between this standard and HG 2927-1989 are: - Equivalently adopt JSFA- "Calcium dihydrogen phosphate", and add clarity, carbonate, free acid and its secondary salt. - Moisture determination is changed to heating reduction method, and the determination condition is stipulated as drying at 180℃ for 3h, and the index parameters are adjusted accordingly. This standard will replace HG2927-1989 from the date of implementation. This standard is proposed by the Technical Supervision Department of the former Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the inorganic salt product standardization technical unit of the Ministry of Chemical Industry and the Food Hygiene Supervision and Inspection Institute of the Ministry of Health. The drafting units of this standard are Tianjin Chemical Research Institute of the Ministry of Chemical Industry and Lianyungang Hongqi Chemical Plant. The main drafters of this standard are Lu Siwei and Pan Hangjun. This standard was first issued as a national standard in March 1989, adjusted to a mandatory chemical industry standard in 1997, and renumbered.
This standard is entrusted to the inorganic salt product standardization technical unit of the Ministry of Chemical Industry for interpretation. 803
Chemical Industry Standard of the People's Republic of China
Food additive
Calcium phosphate monobasic
Food additive-
Calcium phosphate monobasic
HG 2927--1999
Replaces HG 2927-1989
This standard specifies the requirements, test methods, inspection rules, marking, packaging, transportation and storage of calcium phosphate monobasic, a food additive. This standard applies to calcium phosphate monobasic, a food additive made from calcium salt and thermal phosphoric acid as raw materials. This product is used as a calcium supplement and bulking agent in food processing.
Molecular formula: Ca(H2PO)2·H20
Relative molecular mass: 252.07 (according to the relative atomic mass in 1995) 2 Referenced standards
The provisions contained in the following standards constitute the provisions of this standard through reference in this standard. When this standard is published, the versions shown are valid. All standards are subject to revision. Parties using this standard should explore the possibility of using the latest versions of the following standards. GB191—1990 Pictorial markings for packaging, storage and transportation
GB/T 601—1988
GB/T 602-—1988
GB/T 603---1988
GB/T 6678—1986
—1992
GB/T 6682-
GB/T 8450-
—1987
GB/T 8451—1987
3 Requirements
Chemical reagents Preparation of standard solutions for titration analysis (volume analysis) Preparation of standard solutions for impurity determination (negISO6353-1:1982) Chemical reagents
Preparation of preparations and products used in chemical reagent test methods (neqISO6353-1:1982) General rules for sampling of chemical products
Specifications and test methods for water used in analytical laboratories (eqvISO3696:1987) Determination of arsenic in food additives
Test methods for heavy metal limits in food additives 3.1 Appearance: This product is colorless triclinic crystals or white powder. 3.2 Food additives Calcium dihydrogen phosphate should meet the requirements of Table 1. Table 1
Content of monocalcium phosphate (calculated as Ca)/%
Content of arsenic (As)/%
Content of heavy metal (calculated as Ph)/%
Content of fluoride (calculated as F)\/%
Note:
1This item is not set in JJSFA-V1992).
Approved by the State Administration of Petroleum and Chemical Industry on June 16, 1999804
15. 2 ~ 17. 0
Implementation on June 1, 2000
Heating loss/%
Clarity
Carbonate
Free acid and its secondary salts
Test method
HG 2927—1999
Table 1 (end)
Pass the test
Pass the test
Pass the test
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 products 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 Reagents and materials
4.1.1.1 Silver nitrate solution: 20g/L.
4.1.1.2 Ammonium oxalate solution: 33g/L
4.1.2 Identification method
4.1.2.1 Take a small amount of sample on the surface blood, and when moistened with silver nitrate solution, it will turn yellow. 4.1.2.2 Weigh about 0.1g of sample, add 20mL of water, shake well and filter, add 5mL of ammonium oxalate solution to the filtrate, and a white precipitate will be produced. 4.2 Determination of monocalcium phosphate content
4.2.1 Method summary
Add an excess of disodium ethylenediaminetetraacetic acid standard solution to the test solution to complex with Ca ions, and use chrome black T-sodium chloride as an indicator to titrate the excess disodium ethylenediaminetetraacetic acid standard solution with zinc standard titration solution. 4.2.2 Reagents and materials
4.2.2.1 Hydrochloric acid solution: 1+1.
4.2.2.2 Ammonia-ammonium chloride buffer solution: pH~10. 4.2.2.3 Disodium ethylenediaminetetraacetic acid (EDTA) standard titration solution: c(EDTA) is about 0.02 mol/L. 4.2.2.4 Zinc acetate standard titration solution: c[Zn(CH.COO)2·H2O] is about 0.02 mol/L. Preparation: Weigh 4.43g zinc acetate, add 20ml water and 2ml (1+19) acetic acid solution, dissolve and add water to 1000ml, shake. Calibration: Use a pipette to transfer 25ml of the prepared zinc acetate standard titration solution, place it in a 250ml volumetric flask, add 2ml ammonia-ammonium chloride buffer solution and 75ml water, add 0.025g chrome black T-sodium chloride indicator, and titrate with 0.02mol/L EDTA standard titration solution until the solution turns blue and remains blue for 30s without fading, which is the end point. 4.2.2.5 Chrome black T-sodium chloride indicator.
Weigh 0.5g chrome black T, add 10g sodium chloride, grind and mix well. 4.2.3 Analysis steps
4.2.3.1 Preparation of test solution
Weigh about 0.8g of sample (accurate to 0.0002g), place in a 100mL beaker, moisten with a small amount of water, add 8mL of hydrochloric acid solution to dissolve the sample completely, and dry filter if necessary. Transfer to a 250mL volumetric flask, dilute to scale with water, and shake well. 4.2.3.2 Determination
Use a pipette to transfer 25ml of test solution. Place in a 500mL conical flask, and use another pipette to transfer 30mL of LEDTA standard titration solution, add 50ml of water and 10mL of ammonia-ammonium chloride buffer solution, shake well, and let stand for 5min. Add 0.025g of chrome black T-sodium nitride indicator, and titrate with zinc acetate standard titration solution until the solution changes from blue to blue-purple. The end point is that the purple does not fade within 30s. 4.2.4 Expression of analysis results
HG 2927--1999
The content of calcium dihydrogen phosphate (calculated as Ca) expressed as mass percentage (X,) is calculated according to formula (1): Xi = (Vicl -Vec)X0. 040 08 × 100 = 40. 08(Vicl-Vac2)m×250
Wherein: ci—actual concentration of EDTA standard titration solution, mol/L; C2—actual concentration of zinc acetate standard titration solution, mol/L; V, the volume of EDTA standard titration solution added, mL; V—the volume of zinc acetate standard titration solution consumed in titration, mL; m—the mass of the sample, g;
.(1)
0.04008—The mass of calcium dihydrogen phosphate (calculated as Ca) in grams equivalent to 1.00 mL of zinc acetate standard titration solution (cLZn(CH.COO)2·H,O]=1.000 mol/L). 4.2.5 Allowable difference
The arithmetic mean of the parallel determination results is taken as the determination result. The absolute difference of the parallel determinations shall not exceed 0.2%. 4.3 Determination of arsenic content
Weigh about 0.5 g of the sample (accurate to 0.01 g), place it in the arsenic test bottle specified in 2.4 of GB/T8450-1987, add a small amount of water to moisten it, add 6 mL of hydrochloric acid, wait for the sample to dissolve, add water to a total volume of about 40 mL, and shake well. The following operations shall be carried out in accordance with 2.4 of GB/T8450-1987.
The standard is to use a pipette to transfer 1.5mL (1mL solution contains 1μgAs) of arsenic standard solution, and treat it in the same way as the sample. 4.4 Determination of heavy metal content
Weigh about 1g of sample (accurate to 0.01g), place it in a 50mL beaker, add 5mL of water and 5mL of (1+4) hydrochloric acid solution, heat to dissolve, cool and adjust with (1+2.5) ammonia solution until the solution precipitates, then adjust with hydrochloric acid solution until the precipitate just dissolves, dry filter if necessary. Transfer all to a 50mlL colorimetric tube. The following operations are in accordance with Chapter 6 of GB/T8451-1987. The standard colorimetric solution is to use a pipette to transfer 2mL (1mL solution contains 10μgPb) of lead standard solution, and treat it in the same way as the sample. 4.5 Determination of fluoride content
4.5.1 Summary of the method
In a perfluoric acid medium, fluorine is separated from the sample by steam distillation. Fluorine forms a blue complex with a mixture of alizarin aminocarboxylic acid complexing agent and lanthanum nitrate. The color of the test solution is compared with that of the standard. 4.5.2 Reagents and materials
4.5.2.1 Perchloric acid.
4.5.2.2 Acetone.
4.5.2.3 Silver nitrate solution: 17 g/L.
4.5.2.4 Phenolic acid indicator solution: 10 g/L.
Sodium hydroxide solution: 40 g/L.
Sodium hydroxide solution: 4 g/L.
4. 5. 2. 7
Hydrochloric acid solution: 1+10.
Alizarin aminocarboxylic acid complexing agent.
4. 5. 2. 8
Weigh 0.193g of alizarin aminocarboxylic acid complexing agent, dissolve it with a small amount of water and sodium hydroxide solution (4.5.2.5), add 0.13g of sodium acetate, adjust the solution pH to 5.0 with (1+16) acetic acid solution (check with precision pH test paper, the solution is red at this time), transfer to a 500mL volumetric flask, dilute to the mark with water, shake well, and store in a refrigerator. When precipitation occurs, it should be prepared again. 4.5.2.9 Lanthanum nitrate solution.
Weigh 0.217g of lanthanum nitrate, dissolve it with a small amount of (1+16) acetic acid solution, add water to 450mL, adjust the pH to 5.0 with 25g/L sodium acetate solution (check with precision pH test paper), transfer to a 500mL volumetric flask, dilute to the mark with water, and store in a refrigerator. Prepare again after mold growth.
4.5.2.10 Buffer solution.
HG 2927-1999
Weigh 44g of sodium acetate and dissolve it in 400mL of water, add 22ml of glacial acetic acid, and then add glacial acetic acid dropwise to adjust the solution pH to 4.7 (check with precision pH test paper), transfer to a 500mL volumetric flask, and then dilute to scale with water. 4.5.2.11 Fluoride standard solution: 1mL of solution contains 0.010mgF. Preparation: Use a pipette to transfer 10ml of fluoride standard solution prepared according to GB/T602, place it in a 100mL volumetric flask, dilute to scale with water, and shake well.
4.5.3 Instruments and equipment
Fluoride measurement distillation device: See Figure 1.
1--Steam generator (1000ml. flask); 2.-Safety tube (d5mm); 3--Glass tube (5mm); 4, 13.14-Rubber stopper; 5-Tee pipe and screw clamp: 6--Thermometer (200℃); 7-Three-necked flask (250ml.); 8-Glass elbow; 9-Straight condenser (500 mm); 10-Glass elbow; 11-Volume flask (250 mL); 12-Heating jacket or electric furnace Figure 1 Schematic diagram of fluorine distillation device
4.5.4 Analysis steps
Weigh 2.00g sample (accurate to 0.01g), place it in a 250ml three-necked flask (see Figure 1), add a few glass beads, slowly add 10mL perchloric acid, rinse the flask wall with about 8mL water, add 4 to 6 drops of silver nitrate solution, the thermometer on the bottle stopper should be tightly plugged, and the mercury ball of the thermometer is inserted into the test solution, connect the water vapor generator and the straight condenser, connect the end of the condenser to the glass elbow, and insert the elbow into a 250mL volumetric flask containing 10mlL sodium hydroxide solution (4.5.2.6) and 2 drops of phenol indicator solution. Add 500ml water to the water vapor generator, and add sodium hydroxide solution (4.5.2.5) to make the solution alkaline. Open the screw clamp and heat to near boiling. Close the screw clamp, pass water vapor into the three-necked flask, heat the three-necked flask at the same time, and adjust the amount of water vapor entering so that the temperature rises and remains between 135℃ and 140℃. If the solution in the volumetric flask fades, add an appropriate amount of sodium hydroxide solution (4.5.2.6) until the distillate is about 200mL, stop distillation, and shake well. Use sodium hydroxide solution (4.5.2.6) or hydrochloric acid solution to adjust the pH value to 7.0 (check with precision pH test paper), add 2 drops of hydrochloric acid solution, dilute with water to the scale, and shake well. Use a pipette to transfer 25mL of the test solution, place it in a 50mL colorimetric tube, add 5mL of alizarin aminocarboxylic acid complexing agent and 3mL of buffer solution, and mix well. Slowly add 5ml of lanthanum nitrate solution and shake. Add 10mL of acetone, add water to 50ml, and leave at room temperature for 20min. Compared with the standard colorimetric solution, its color should not be darker than the standard colorimetric solution. The standard colorimetric solution is 0.5 mL of fluoride standard solution transferred by pipette into a three-necked flask and treated in the same way as the test solution.
4.6 Determination of heating loss
4.6.1 Summary of the method
After the sample is heated, dried, cooled and weighed, its content is determined. 807
4.6.2 Analysis steps
HG 2927--1999
Weigh 1g to 2g of the sample (accurate to 0.0002g), place it in a weighing bottle that has been dried at 180℃ to a constant mass, and heat it in a drying oven at 180℃ for 31. Cool it to room temperature in a desiccator and weigh it. 4.6.3 Expression of analysis results
The heating loss (X) expressed as a mass percentage is calculated according to formula (2): Xz=m=m×100
Wherein: m——-mass of the sample before heating, g; m1——-mass of the sample after heating, g.
4.6.4 Allowable difference
The arithmetic mean of the parallel determination results is taken as the determination result. The absolute difference of the parallel determinations shall not exceed 0.1%. 4.7 Clarity test
4.7.1 Method summary
After dissolving the sample in hydrochloric acid, observe the clarity of the solution. 4.7.2 Reagents and materials
4.7.2.1 Hydrochloric acid.
4.7.2.2 Nitric acid solution: 1+2.
4.7.2.3 Silver nitrate solution: 20g/L.
4.7.2.4 Chloride standard solution: 1 mL of solution contains 0.01 mgCl. (2)
Use a pipette to transfer 10 mL of the chloride standard solution prepared according to GB/T602 into a 100 mL volumetric flask, dilute to the mark with water, and shake well.
4.7.3 Analysis steps
Weigh 2.0 g of the sample, place it in a 50 mL beaker, add 18 mL of water and 2 mL of hydrochloric acid, and heat in a boiling water bath for 5 min to dissolve. The turbidity of the solution shall not be greater than that of the standard turbidity solution. The standard turbidity solution is to transfer 1.2 mL of the nitride standard solution into a colorimetric tube, add water to 20 mL, add 1 mL of nitric acid solution, add 1 mL of silver nitrate solution, and shake well. Place in a dark place for 15 min. 4.8 Test of carbonate
4.8.1 Summary of method
After boiling the sample with water, add hydrochloric acid dropwise and observe whether bubbles are generated. 4.8.2 Reagents and materials
Hydrochloric acid.
4.8.3 Analysis steps
Weigh 2.0g of sample, place it in a 50mL conical flask, add 6mL of water and boil it, and after cooling, add 2mL of hydrochloric acid dropwise. No bubbles should be generated in the test solution.
4.9 Test of free acid and its secondary salt
4.9.1 Method Summary
Mix the sample with water, use methyl orange as the indicator solution, add sodium hydroxide solution dropwise, and observe the color change of the solution. 4.9.2 Reagents and Materialswww.bzxz.net
4.9.2.1 Standard sodium hydroxide solution: c(NaOH) about 1 mol/L. 4.9.2.2 Methyl orange indicator solution: 1 g/1.
4.9.3 Analysis Steps
Weigh 1.0 g of the sample, put it in a mortar, add 3 mL of water to mix, transfer it to a 250 mL beaker, add 100 mL of water to shake, add 1 drop of methyl orange indicator solution, add 1.0 ml of sodium hydroxide solution dropwise, and the test solution should be yellow. 808
5 Inspection rules
HG 2927-1999
5.1 All eight indicators specified in this standard are type inspection items, among which calcium dihydrogen phosphate, arsenic, heavy metals, fluoride, and dryness loss are factory inspection items and should be inspected batch by batch. Under normal production conditions, type inspection shall be carried out at least once every three months. 5.2 Each batch of products shall not exceed 5t.
5.3 Determine the number of sampling units in accordance with the provisions of 6.6 of GB/T6678-1986. Each plastic woven bag is a packaging unit. When sampling, insert obliquely from the top of each selected packaging bag to 3/4 of the depth of the material layer, and use a sampler to take out a sample of not less than 50g. After mixing the sample, reduce it to about 200g by quartering method, and immediately put it into two clean and dry wide-mouth bottles with ground stoppers and seal them. A label is attached to the bottle, indicating: manufacturer name, product name, batch number, sampling date and name of the sampler. One bottle is used for inspection and the other is kept for three months for future reference. 5.4 The food additive monocalcium phosphate 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 each batch of products shipped out of the factory meets the requirements of this standard. If one of the indicators in the inspection results does not meet the requirements of this standard, samples should be taken from twice the amount of packaging for re-inspection. Even if only one indicator in the inspection results does not meet the requirements of this standard, the entire batch of products shall be unqualified. 6 Marking, packaging, transportation and storage
6.1 The packaging bag of the food additive monocalcium phosphate shall have firm and clear markings, including: manufacturer name, address, product name, trademark, "food additive", net content, batch number or production date, shelf life, production license number, this standard number and the "wet-afraid" mark in GB190.
6.2 Each batch of products leaving the factory should be accompanied by a quality certificate, which includes: the name of the manufacturer, address, product name, trademark, the word "food additive", batch, batch number or production date, shelf life, production license number, proof that the product quality meets this standard and the number of this standard. 6.3 The food additive monocalcium phosphate is double-packed. The inner packaging is a polyethylene film bag for food, with a thickness of not less than 0.06mm; the outer packaging is a plastic woven bag. The net content of each bag is 25kg, or it can be packaged according to user requirements. 6.4 For the packaging of the food additive monocalcium phosphate, the inner bag is tied twice with vinyl rope or a rope of equivalent quality, or sealed with other equivalent methods; the outer bag is folded at a distance of not less than 30mm from the bag edge, and the opening is sewn with vinyl thread or other thread of equivalent quality at a distance of not less than 15mm from the bag edge. The stitches are neat and the stitch length is uniform. There is no leakage or skipping. 6.5 Food additive monocalcium phosphate should be covered during transportation to prevent sun exposure, rain and moisture. It should not be transported together with toxic and hazardous substances. Prevent contamination.
6.6 Food additive monocalcium phosphate should be stored in a cool, dry place to prevent rain, moisture and sun exposure. It should not be stored together with toxic and hazardous substances. Prevent contamination.
6.7 Under the conditions of packaging, transportation and storage in accordance with this standard, the shelf life of the product is two years from the date of production. If it is overdue, it should be re-inspected to see if it meets the requirements of this standard. Those that meet the requirements can continue to be used. 809
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