Some standard content:
Record number: 7472-2000
HG2636-2000
This standard is a revision of the chemical industry standard HG2636-1994 "Feed Grade Calcium Hydrogen Phosphate" by using the calcium hydrogen phosphate in the "German Feed Regulations" in a non-equivalent manner.
The main differences between this standard and the calcium hydrogen phosphate in the "German Feed Regulations" are: the addition of arsenic, fluoride, lead content and fineness index items. The main differences between this standard and HG2636-1994 are: - The heavy metal index item is changed to the lead content index, and the index parameters remain unchanged; - The determination of calcium content adopts the determination method of calcium in the national standard feed; - The determination of fluoride content adopts the determination method of fluoride in the national standard feed; the determination of lead content adopts the determination method of lead in the national standard feed, and the dithiol spectrophotometry is added. This standard will replace HG2636-1994 from the date of implementation. Appendix A of this standard is the appendix of the standard.
This standard is proposed by the Policy and Regulations Department of the State Administration of Petroleum and Chemical Industry. This standard is under the jurisdiction of the Inorganic Chemical Subcommittee of the National Technical Committee for Chemical Standardization. The drafting units of this standard are: Tianjin Chemical Research and Design Institute, Sichuan Mianzhu Long Mineral Feed Group Co., Ltd., Guangdong Zhanhua Enterprise Group Co., Ltd., Zigong Honghe Chemical Co., Ltd., Chaobei Xiangfan Chemical Plant, Zibo Beiwei Phosphorus Chemical Co., Ltd., Sichuan Jinhui Modern Agricultural Chemical Co., Ltd.
The main drafters of this standard are: Li Guangming, Zhou Xiaokui, Chen Youjun, Lai Ximin, Ge Bin, Zhang Aiguo, Li Xiuhui. This standard was first issued in 1987 and revised for the first time in 1994. This standard is entrusted to the Inorganic Chemical Subcommittee of the National Technical Committee for Chemical Standardization for interpretation. 101
1 Scope
Chemical Industry Standard of the People's Republic of China
Feed grade dicalcium phosphate
Feed grade
Calcium hydrogen pyrophosphateHG 2636—2000
Replaces HG2636--1994
This standard specifies the requirements, test methods, inspection rules, and marking, labeling, packaging, transportation, and storage of feed grade dicalcium phosphate. This standard applies to feed grade dicalcium phosphate produced by neutralizing industrial phosphoric acid with lime milk or calcium carbonate. It does not apply to dicalcium phosphate produced from toxic and harmful phosphoric acid. This product is used as a calcium and phosphorus supplement in feed processing. Molecular formula: CaHPO4·2H,O
Relative molecular mass: 172.10 (according to the 1995 international relative atomic mass) 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. GB/T 601-1988
GB/T 602--1988
GB/T 603-1988
Chemical reagents-Preparation of standard solutions for titration analysis (volume analysis) Chemical reagents
Preparation of standard solutions for impurity determination
Preparation of preparations and products used in test methods Chemical reagents
GB/T 610. 1--1988
GB/T 6436--1992
GB/T 6678-1986
GB/T 6682--1992
GB 10648--1999
Chemical reagentsGeneral method for determination of arsenic (monolithic plaque method)Determination of calcium in feed
General rules for sampling of chemical products
Specifications and test methods for water used in analytical laboratories (negISO3696:1987)Feed labeling
GB/T 13079--1991
GB/T 13080-1991
GB/T 13083—1991
Method for determination of total arsenic in feed
Method for determination of lead in feed
Method for determination of fluoride in feed
GB/T 14539.4—1993
3 Requirements
Method for determination of lead in compound fertilizers
3.1 Appearance: This product is white, slightly yellowish, slightly grey powder or granules. 3.2 Feed grade calcium hydrogen phosphate shall meet the requirements of Table 1. Table 1 Requirements
Phosphorus (P) content
Calcium (Ca) content
Approved by the State Administration of Petroleum and Chemical Industry on June 5, 2000 102
Implemented on March 1, 2001
Chlorine (F) content
As content
Lead (Pb) content
Fineness (powdered through 500μm test sieve) 4
Test method
HG 2636 --- 2000
Table 1 (end)
The reagents and water used in this standard, unless otherwise specified, refer to analytical reagents and grade 3 water specified in GB/T6682. The standard titration solutions, impurity standard solutions, preparations and products used in the test, unless otherwise specified, are prepared in accordance with the provisions of GB/T601, GB/T602 and GB/T603.
Safety Tips: The hydrochloric acid used in the test is a corrosive reagent and should be handled with caution. If it splashes on the skin, rinse immediately with water. 4.1 Identification
4.1.1 Reagents and Materials
4.1.1.1 Glacial acetic acid.
4.1.1.2 Ammonium oxalate solution: 30g/L.
4.1.1.3 Silver nitrate solution: 17g/L.
4.1.2 Identification method
4.1.2.1 Identification of phosphate
Weigh 0.1g sample, dissolve in 10mL water, add 1mL silver nitrate solution, generate yellow precipitate, this precipitate is soluble in ammonia water, insoluble in glacial acetic acid.
4.1.2.2 Identification of calcium ion
Weigh 0.1g sample, dissolve in 5mL glacial acetic acid. Boil and cool, filter, add 5mL ammonium oxalate solution to the filtrate, generate white precipitate. This solution dissolves in hydrochloric acid solution.
4.1.2.3 Distinguishing between tricalcium phosphate and dicalcium phosphate According to the test method in Appendix A, the phosphate soluble content is greater than or equal to 13%, which is dicalcium phosphate. 4.2 Determination of phosphorus content
4.2.1 Summary of method
In acidic medium, all phosphates in the test solution react with the added quinoline molybdate to form quinoline phosphomolybdate precipitate, which is filtered, dried, weighed, and the phosphorus content is calculated.
4.2.2 Reagents and materials
4.2.2.1 Hydrochloric acid solution: 1+1.
4.2.2.2 Nitric acid solution: 1+1.
4.2.2.3 Preparation of quinomolybdic acid solution:
a) Weigh 70g sodium molybdate and dissolve it in 150mL water; b) Weigh 60g citric acid and dissolve it in 150mL water and 85mL nitric acid; c) Pour solution a) into solution b) under stirring; d) Add 35mL nitric acid and 5mL quinoline to 100mL water; e) Pour solution d) into solution c), let stand for 24h, filter with a crucible filter, add 280mL acetone, dilute with water to 1000ml, mix well. And store in a polyethylene bottle. 4.2.3 Instruments and equipment
4.2.3.1 Glass sand: pore size is 5~15μm. 103
HG 2636-2000
4.2.3.2 Electric oven: temperature can be controlled at (180±5)C. 4.2.4 Analysis steps
4.2.4.1 Preparation of test solution A
Weigh about 1g of sample (accurate to 0.0002g), place it in a 250ml volumetric flask, add 10mL of hydrochloric acid solution, dilute to the mark with water, and shake the spoon. This solution is test solution A, which is used to determine the phosphorus and calcium contents. 4.2.4.2 Preparation of blank solution
Except for not adding the sample, the amount of other added reagents is exactly the same as that of the test solution, and the same treatment is performed at the same time as the sample. 4.2.4.3 Determination
Use a pipette to transfer 20mL of test solution A and blank solution to 250ml.In a beaker, add 10mL nitric acid solution, add water to a total volume of about 100mL, heat and boil for 5min, add 50mL molybdenum citric acid solution, cover the surface, keep warm for 30s (do not use open flames or stir during the addition of reagents and heating to avoid condensation) and cool. Stir 3 to 4 times during the cooling process, and filter with a glass sand filter that has been dried to constant weight at (180±5)°C. First filter the upper clear liquid, wash the precipitate 6 times by pouring, using about 30ml of water each time, and finally transfer the precipitate to a glass sand crucible for filtration, then wash the precipitate 3 times with water, place the glass sand crucible and the precipitate in an electric oven and start timing from the time the temperature stabilizes, dry at (180±5)°C for 45min, take it out and cool it slightly, place it in a desiccator to cool to room temperature, and weigh it. 4.2.5 Expression of analysis results
Phosphorus (P) content (X,) expressed as mass fraction is calculated according to formula (1): (m/mz) X 0. 014 00
X 100 =
m×250bZxz.net
Wherein: m,-mass of quinoline phosphoaluminate precipitate generated by test solution, g; m-mass of quinoline phosphomolybdate precipitate generated by blank solution, g; m -mass of sample, g;
0.01400-coefficient for converting quinoline phosphoaluminate into phosphorus. 4.2.6 Allowable difference
17. 5 (ml - mz)
The arithmetic mean of the parallel determination results is taken as the determination result. The absolute difference of the parallel determination results shall not exceed 0.1%. 4.3 Determination of calcium content
4.3.1 Principle of the method
Same as B2 of Appendix B in GB/T 6436-~1992. 4.3.2 Reagents and materials
Same as B3 of Appendix B in GB/T 6436-~1992. 4.3.2.1 Sucrose solution: 25g/1.
4.3.2.2 Standard titration solution of disodium ethylenediaminetetraacetic acid: c(EDTA) 0.02mol/L. (1)
4.3.3 Analysis steps
Use a pipette to transfer 25mL of test solution A into a 250mL chain bottle. Add 50mL of water, 5mL of sucrose solution, 2mL of triethanolamine, 1mL of ethylenediamine, 1 drop of malachite green indicator solution, add potassium hydroxide solution until colorless, then add 10mL in excess, add 0.1g of hydroxylamine hydrochloride (shake well each time adding a reagent), add a little calcein, and titrate with EDTA standard titration solution against a black background until the green charcoal light disappears and turns purple-red, which is the titration endpoint. 4.3.4 Expression of analysis results
Calcium (Ca) content (X) expressed as mass fraction is calculated according to formula (2): Xz = × 0. 040 08 × 100 =
40. 08 Vc
Wherein: c--actual concentration of disodium ethylenediaminetetraacetic acid standard titration solution, mol/1; m
V--volume of disodium ethylenediaminetetraacetic acid standard titration solution consumed during titration, ml.104
m:-mass of sample g;
HG 2636-2000
mass of calcium expressed in grams equivalent to 1.00ml disodium ethylenediaminetetraacetic acid standard titration solution Lc (EDTA) = 1.000mol/L.].
4.3.5 Allowable difference
Take the arithmetic mean of the parallel determination results as the determination result. The absolute difference of the parallel determination results shall not exceed 0.2%. 4.4 Determination of fluorine content
4.4.1 Principle of the method
Same as Chapter 2 of GB/T13083-1991.
4.4.2 Reagents and materials
Same as Chapter 3 of GB/T13083--1991 and
Hydrochloric acid solution: 1+4.
4.4.3 Apparatus and equipment
Same as Chapter 4 of GB/T13083--1991.
4.4.4 Analysis steps
4.4.4.1 Drawing of working curve
Use a pipette to transfer 1.00mL, 2.00mL, 3.00ml, 4.00ml, and 5.00mL of fluorine standard solution (1mL100 gF) to a 50ml volumetric flask, add 4ml hydrochloric acid solution (1+4), add 25ml total ionic strength buffer, dilute to scale with water, and shake well. 4.4.4.2 Preparation of test solution
Weigh 0.5~1.0g of sample (to ensure that the fluorine content is between 1000~~1600ug) (accurate to 0.01g), place in a 100ml volumetric flask, add 16mL hydrochloric acid solution (1+4), dilute to scale with water, and shake well. Transfer 25mL of test solution to a 50mL volumetric flask, add 25mL total ionic strength buffer, and shake well. 4.4.4.3 Determination
Operate according to 6.3 of GB/T130831991.
4.4.5 Expression of analysis results
The fluorine (F) content (X) expressed as mass fraction is calculated according to formula (3): X m × 10-3
X 100 =
m×100
Wherein: m is the fluorine content obtained from the standard curve, mg; m is the mass of the sample, g.
4.4.6 Allowable difference
Take the arithmetic mean of the parallel determination results as the determination result. The absolute difference of the parallel determination results shall not exceed 0.02%. 4.5 Determination of arsenic content
4.5.1 Spectrophotometry (arbitration method)
4.5.1.1 Summary of method
Same as Chapter 2 of GB/T13079--1991.
4.5.1.2 Reagents and materials
Same as Chapter 3 of GB3/T13079---1991.
4.5.1.3 Apparatus and equipment
Same as Chapter 4 of GB/T13079-1991.
4.5.1.4 Analysis steps
(3)
a) Preparation of test solution B
Accurately weigh (1.0±0.01)g of sample and place it in a 100ml volumetric flask. Add 20ml of (1+4) hydrochloric acid solution and dilute with water to 105
HG 2636
scale and shake well. This solution is test solution B. It is used for the determination of arsenic and lead content. b) Determination
Use a pipette to transfer 10ml of test solution and perform determination and calculation according to 6.3 of GB/T13079-1991. 4.5.2 Arsenic spot method
Use a pipette to transfer 10ml of test solution B and perform determination according to Chapter 6 of GB/T610.1-1988. The standard colorimetric solution is 3 ml of arsenic standard solution containing 1 ug arsenic in 1 mL of solution, which is pipetted with a pipette and treated in the same way as the sample. 4.6 Determination of lead content
4.6.1 Atomic absorption spectrophotometry (arbitration method) Use a pipette to transfer 20 ml of test solution B, and perform the determination according to 6.3 of GB/T13080-1991 (without extraction) and calculate 4.6.2 Dithiol spectrophotometry
Weigh 2 g of sample (accurate to 0.01 g) and place it in a 250 ml volumetric flask, add 50 ml of (1+4) hydrochloric acid solution, dilute to the mark with water, and shake well.
Use a pipette to transfer 25 ml of test solution, and perform the determination and calculation according to 14.2 of GB/T14539.4-1993. 4.7 Determination of fineness
4.7.1 Instruments and equipment
Test sieve (GB/T6003.1): R40/3 series*200mmX50mm/0.500mm. 4.7.2 Analysis steps
Weigh 20g sample (accurate to 0.01g) and place it in the test sieve for sieving. Weigh the material under the sieve (accurate to 0.01g). 4.7.3 Expression of analysis results
The fineness expressed as mass fraction (X,) is calculated according to formula (4): X.-
Where: m. Mass of the material under the sieve, g;
Mass of the sample, g.
4.7.4 Allowable difference
Take the arithmetic mean of the parallel determination results as the determination result. The absolute difference of the parallel determination results shall not exceed 0.2%. 4.8 Determination of free moisture
When the user has requirements for free moisture, it shall be determined according to this standard method, and the indicators shall be negotiated between the supply and demand parties. 4.8.1 Instruments and equipment
4.8.1.1 Glass crucible: pore size is 5~15μm. 4.8.1.2 Electric oven: temperature can be controlled at (50±2)℃. (4)
4.8.2 Analysis steps
Weigh 2g of sample (accurate to 0.0002g), place it in a glass crucible that has been dried to constant weight at 50℃, add 5mL of acetone, stir with a thin glass rod, filter, and then wash twice with acetone, using 5mL each time.Acetone. Place the glass crucible containing the sample in a ventilated place for 10 minutes, then place it in an electric oven at (50 ± 2) °C and dry it for 2 hours, cool it in a dryer for 20 minutes, and weigh it. 4.8.3 Expression of analysis results
The free moisture content (X.) expressed as mass fraction is calculated according to formula (5): m2×100
The mass of the sample and the glass sand plug, g;
Formula A m,-
m2--The mass of the sample and the glass sand after drying, g---The mass of the sample, g.
4.8.4 Allowable difference
(5)
HG 2636-2000
The arithmetic mean of the test results is taken as the test result. The absolute difference of the test results is not greater than 0.2%. 5 Inspection rules
5.1 All items specified in this standard are inspection items. 5.2 Each batch of products shall not exceed 60t.
5.3 Determine the number of sampling units in accordance with the provisions of GB/T6678. Each plastic woven bag is a packaging unit. When sampling, insert the sample obliquely from the top of each selected packaging bag to three-quarters of the depth of the material layer, and use a sampler to take out no less than 500g of sample. 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. Paste labels on the bottles, indicating: 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. 5.4 Feed-grade calcium hydrogen 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 all feed-grade calcium hydrogen phosphate shipped from the factory meets the requirements of this standard. 5.5 The user has the right to inspect and accept the received feed-grade calcium hydrogen phosphate products in accordance with the provisions of this standard, and the inspection time shall be within 1 month from the date of arrival of the goods.
5.6 If one of the test results does not meet the requirements of this standard, samples should be taken from twice the amount of packaging for re-testing. If even one of the re-test results does not meet the requirements of this standard, the entire batch of products will be unqualified. 6 Marks and labels
6.1 The packaging bags of feed-grade calcium hydrogen phosphate should have firm and clear marks, including the manufacturer's name, address, product name, trademark, the word "feed grade", net content, batch number or production date, production license number and this standard number. 6.2 Each batch of products leaving the factory should be accompanied by a label, and the content of the label should comply with the provisions of GB10648. 7 Packaging, transportation and storage
7.1 The inner packaging of feed-grade calcium hydrogen phosphate adopts food-grade polyethylene film bags, and the outer packaging adopts plastic woven bags. The net content of each bag is 50kg. If the user has special requirements for packaging, the supply and demand parties can negotiate. 7.2 For the packaging of feed-grade calcium ammonium phosphate, the film bag should be tied twice with vinyl rope or rope of equivalent quality, or sealed with other equivalent methods; the outer bag should be folded at a distance of not less than 30mm from the bag edge, and the opening should be sewed with vinyl thread or other thread of equivalent quality at a distance of not less than 15mm from the bag edge. The stitches should be neat and the stitches should be evenly spaced. There should be no leaking seams or skipped stitches. 7.3 During transportation, feed-grade calcium hydrogen phosphate should be covered to prevent sun exposure, rain, and moisture. It should not be transported together with toxic and hazardous substances. 7.4 Feed-grade calcium hydrogen phosphate should be stored in a dry warehouse to prevent rain, moisture, and sun exposure. It should not be mixed with toxic and hazardous substances. 107
A1 Method Summary
—2000
HG2636-
Appendix A
(Standard Appendix)
Determination of Soluble Phosphorus Content
Use neutral ammonium citrate solution to dissolve and extract the phosphate in the sample, and determine the phosphorus according to the method for determining phosphorus content in 4.2. When the phosphorus content is greater than 13%, the sample is considered to be calcium ammonium phosphate. A2 Reagents and Materials
A2.1 Citric acid.
A2.2 Anhydrous ethanol.
A2.3 Ammonia water.
A2.4 Neutral ammonium citrate solution. Dissolve 74g citric acid in 300mL water, add 69mL ammonia water, adjust the pH value to 7.0 with ammonia water on the acidometer, and measure its relative density with a hydrometer to 1.09 (20℃C). Store the solution in a sealed bottle for later use (if used for a long time, calibrate its acidity before use).
A3 Instruments and equipment
A3.1 Acidometer: graduation value is 0.2pH, equipped with glass electrode and saturated calomel electrode A3.2 Hydrometer.
A4 Analysis steps
Weigh 1g sample (accurate to 0.0002g), place it in a 250mL volumetric flask, add 100mL neutral ammonium citrate solution, place the volumetric flask in a (65±1)℃ water bath and keep warm for 1h, open the bottle stopper frequently, shake it every 15min, shake it for about 30s each time, take out the volumetric flask, cool it to room temperature, add water to the scale, and shake it. Dry filter and discard the initial 30 mL of filtrate. Follow the steps in 4.2.4.3, starting from “take 20 mL of test solution A with a pipette” and calculate according to 4.2.5 of this standard. The measured phosphorus content should be greater than 13%.0, and its relative density is 1.09 (20℃C) measured by hydrometer. Store the solution in a sealed bottle for later use (if used for a long time, calibrate its acidity before use).
A3 Instruments and equipment
A3.1 Acidometer: the graduation value is 0.2pH, equipped with glass electrode and saturated calomel electrode A3.2 Hydrometer.
A4 Analysis steps
Weigh 1g sample (accurate to 0.0002g), place it in a 250mL volumetric flask, add 100mL neutral ammonium citrate solution, place the volumetric flask in a (65±1)℃ water bath and keep warm for 1h, open the bottle stopper frequently, shake it every 15min, and shake it for about 30s each time, take out the volumetric flask, cool it to room temperature, add water to the scale, and shake it. Dry filter and discard the initial 30 mL of filtrate. Follow the steps in 4.2.4.3, starting from “take 20 mL of test solution A with a pipette” and calculate according to 4.2.5 of this standard. The measured phosphorus content should be greater than 13%.0, and its relative density is 1.09 (20℃C) measured by hydrometer. Store the solution in a sealed bottle for later use (if used for a long time, calibrate its acidity before use).
A3 Instruments and equipment
A3.1 Acidometer: the graduation value is 0.2pH, equipped with glass electrode and saturated calomel electrode A3.2 Hydrometer.
A4 Analysis steps
Weigh 1g sample (accurate to 0.0002g), place it in a 250mL volumetric flask, add 100mL neutral ammonium citrate solution, place the volumetric flask in a (65±1)℃ water bath and keep warm for 1h, open the bottle stopper frequently, shake it every 15min, and shake it for about 30s each time, take out the volumetric flask, cool it to room temperature, add water to the scale, and shake it. Dry filter and discard the initial 30 mL of filtrate. Follow the steps in 4.2.4.3, starting from “take 20 mL of test solution A with a pipette” and calculate according to 4.2.5 of this standard. The measured phosphorus content should be greater than 13%.
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