Some standard content:
HG2940---2000
This standard is a revision of the chemical industry standard HG2940-1987 (1997) "Feed Grade Light Calcium Carbonate". This standard was revised with reference to the "Japanese Food Additives Code".
Compared with HG2940-1987 (1997), the content index of calcium carbonate has been adjusted. This standard will replace HG2940-1987 (1997) from the date of implementation. 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 Branch of the National Chemical Standardization Technical Committee. The drafting units of this standard are: Tianjin Chemical Research and Design Institute, Zhejiang Linghua Group Co., Ltd., and Sichuan Dujiangyan Calcium Products Co., Ltd. The main drafters of this standard are: Yao Jinjuan, Shi Jie, Sun Xiaodong, and Wang Liangjin. This standard was first issued in 1987 as the national standard GB8257-1987. In 1997, it was adjusted to the chemical industry standard and numbered HG 2940-1987 (1997).
This standard is entrusted to the Inorganic Chemical Branch of the National Technical Committee for Chemical Standardization for interpretation. 178
1 Scope
Chemical Industry Standard of the People's Republic of China
Feed grade
Light calcium carbonate
Feed grade--Light calcium carbonateHG 2940 ---2000
Replaces HG 2940 1987 (1997)
This standard specifies the requirements, test methods, inspection rules, marking, labeling, packaging, transportation and storage of feed grade light calcium carbonate. This standard is applicable to light calcium carbonate obtained by carbonization method and used as a calcium supplement in feed processing. Molecule: CaC03
Molecular mass: 100.09 (according to the 1997 international relative atomic mass) 2 Reference 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 will be revised, and the parties using this standard should explore the possibility of using the latest versions of the following standards. GB 191--1990
Picture mark for packaging, storage and transportation
GB/T 601--1988
GB/T 602—1988
GB/T 603—1988
GB/T 6678—--1986
Chemical reagents
Chemical reagents
Chemical reagents
Preparation of standard solutions for titration analysis (volumetric analysis)Preparation of standard solutions for determination of impurities
Preparation of preparations and products used in test methodsGeneral rules for sampling of chemical products
GB/T6682--1992
GR 10648 --1999
3 Requirements
Appearance: white powder.
Specifications and test methods for water used in analytical laboratories (neqISO3696:1987) Feed label
3.2 Feed-grade light calcium carbonate should comply with the requirements of Table 1. Requirements
Calcium carbonate (CaCO) content (dry basis)Calcium (Ca) content (dry basis)
Moisture content
HCl insoluble matter content
Heavy metal sulfide (Pb) content
As content
Barium salt (B3a) content
Approved by the State Administration of Petroleum and Chemical Industry on June 5, 2000
Implementation on March 1, 2001
4 Test method
HG 29402000
The reagents and water used in this standard refer to analytical pure reagents and grade water specified in GB/T6682 unless otherwise specified. The standard titration solution, impurity standard solution, preparation and product used in the test shall be prepared in accordance with the provisions of GB/T601, GB/T602 and GB/T603 unless otherwise specified.
Safety Tips: The strong acid and alkali used in this standard are corrosive and users should be careful when handling them. If they splash on the skin, rinse immediately with plenty of water and treat immediately if they are seriously fumigated.
4.1 Identification Test
4.1.1 Identification of Carbonate Ions
Take a small amount of the sample and add (1+2) hydrochloric acid solution to generate carbon dioxide gas. The generated carbon dioxide gas is passed into 3g/L calcium hydroxide solution to generate a white precipitate.
4.1.2 Identification of Calcium Ions
Take the above test solution, add phenol anhydride indicator solution, adjust to neutral with (1+3) ammonia water, add 35g/L ammonium oxalate solution, and generate a white precipitate. This precipitate can be dissolved in hydrochloric acid solution, but not in glacial acetic acid. Take a platinum wire, moisten it with hydrochloric acid, and burn it in a colorless flame until it becomes colorless. Dip the sample and burn it again, and the flame will be brick red. 4.2 Determination of calcium carbonate and calcium content
4.2.1 Method summary
In a medium with a pH value greater than 12, use triethanolamine to mask a small amount of Fe3+, A13+, Mn2+ ions, and use the calcium reagent carboxylate sodium salt indicator to indicate the end point. Use the disodium ethylenediaminetetraacetic acid standard titration solution to titrate Ca2+. Excess disodium ethylenediaminetetraacetic acid captures the Ca2+ complexed with the indicator and releases the indicator. The end point of the reaction is determined by the color change. 4.2.2 Reagents and materials
4.2.2.1 Hydrochloric acid solution: 1+1.
4.2.2.2 Sodium hydroxide solution: 100g/L. 4.2.2.3 Triethanolamine solution: 1+3.
4.2.2.4 Ethylenediaminetetraacetic acid disodium standard titration solution: c(EDTA) is about 0.02mol/L. 4.2.2.5 Calcium reagent carboxylate sodium salt indicator. Weigh 10g of sodium chloride dried at 105~110℃ for 2h, grind it in a mortar, add 0.1g of calcium reagent carboxylate sodium salt, grind it, and mix it. Put it in a weighing bottle and store it in a desiccator. 4.2.3 Analysis steps
Weigh 0.6g of the sample that has been dried to constant weight at 105~110℃ in advance (accurate to 0.0002g), put it in a 250mL beaker, add a little water to moisten it, cover it with surface III, add hydrochloric acid solution until the sample is completely dissolved, transfer it all to a 250ml volumetric flask, dilute it to the scale with water, and shake the spoon. Use a pipette to transfer 25 mL of the test solution into a can-shaped bottle, add 5 mL of triethanolamine solution, 25 mL of water and a small amount of calcium reagent sodium carboxylate indicator, adjust to wine red with sodium hydroxide solution, and titrate with disodium ethylenediaminetetraacetic acid standard titration solution until pure blue is the end point. 4.2.4 Expression of analysis results
Calcium carbonate (CaCO3) content (X,) expressed as mass percentage is calculated according to formula (1): X: (%) - V × 0. 100 1 × 100X100 125
m × 250
Calcium (Ca) content (X2) expressed as mass percentage is calculated according to formula (2): cV × 0. 040 08 × 100 = bZxz.net
X2 (%) =
cVX40. 08
Where: ---actual concentration of disodium ethylenediaminetetraacetic acid standard titration solution, mol /I.;V---Volume of disodium ethylenediaminetetraacetic acid standard titration solution consumed during titration, ml.;180
（1）
·（2）
mMass of sample, g.;
HG 2940--- 2000
0.1001----Mass of calcium carbonate equivalent in grams to 1.00mL disodium ethylenediaminetetraacetic acid standard titration solution (EDTA) 1.000mol/1.］;
0.04008--Mass of calcium equivalent in grams to 1.00mL disodium ethylenediaminetetraacetic acid standard titration solution Lc (EDTA) = 1.000mol/1.
4.2.5 Allowable difference
Take the arithmetic mean of the parallel determination results as the determination result. The absolute difference of parallel determination results: calcium carbonate content is not more than 0.2%; calcium content is not more than 0.1%.
4.3 Determination of moisture
4.3.1 Summary of method
Bake the sample at 105~~110℃ to constant weight, and determine the moisture content based on the weight loss before and after heating. 4.3.2 Instruments and equipment
Weighing bottle: 60mm×30mms
4.3.3 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, and dry it at 105~110℃ to constant weight.
4.3.4 Expression of analysis results
The moisture content (X:) expressed as mass percentage is calculated according to formula (3): X(%)
Where.m-
--the mass of the weighing bottle and the sample before drying, g, m2---the mass of the weighing bottle and the sample after drying, g; m---the mass of the sample, g.
m=m2×100
4.3.5 Allowable difference
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 0.02%. 4.4 Determination of hydrochloric acid insoluble matter
4.4.1 Method summary
Dissolve the sample with hydrochloric acid, filter and wash. Burn the insoluble matter at (875±25)°C to constant weight. 4.4.2 Reagents and materials
4.4.2.1 Hydrochloric acid solution: 1+1.
4.4.2.2 Silver nitrate solution: 10g/L.
4.4.2.3 Methyl orange indicator solution: 1g/L.
4.4.3 Instruments and equipment
High temperature furnace: capable of controlling the temperature at (875±25)°C. (3)
4.4.4 Analysis steps
Weigh 1g of sample (accurate to 0.01g), place in a tall beaker, moisten with a small amount of water, add 2 drops of methyl orange indicator solution, cover with surface III, slowly add hydrochloric acid solution until the solution changes from yellow to red, then add 5ml in excess, heat to boiling, filter with medium-speed quantitative filter paper while hot, wash the precipitate with hot water until the filtrate is free of chloride ions (check with silver nitrate solution), transfer the filter paper and insoluble matter into a porcelain snail with constant weight, ashed, and burn at (875±25)°C to constant weight.
4.4.5 Expression of analysis results
The content of hydrochloric acid insoluble matter (X,) expressed as a mass percentage is calculated according to formula (4): m
X, (%) =
HG 2940.- 2000
·Mass of the crucible and insoluble matter after calcination,; Wu: m-
Mass of the crucible·g:
:Mass of the sample,.
4.4.6 Allowable difference
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 0.02%. 4.5 Determination of heavy metal content
4.5.1 Summary of the method
In a slightly acidic medium, heavy metal ions react with S" to produce a stable brown suspension, which is compared with the standard comparison solution. 4.5.2 Reagents and materials
4. 5. 2. 1
Ascorbic acid.
Hydrochloric acid solution: 1+1.
Glacial acetic acid solution: 1+16.
Ammonia solution: 1+1.
Saturated hydrogen sulfide water: Prepare immediately before use.
Lead standard solution: 1mL solution contains 0.01mg lead, accurately diluted 10 times after preparation according to GB/T602. 4.5.2.7
Phenol indicator solution: 10g/1.Ethanol solution.
|4.5.3 Instruments and equipment
Colorimetric tube: 50ml.
4.5.4 Analysis steps
Weigh (1±0.01)g of sample, place in a beaker, moisten with a small amount of water, cover with a watch glass, slowly add hydrochloric acid solution to completely dissolve the sample, heat to boiling, and cool. Transfer all to a colorimetric tube, add 20mL of water and 1 drop of phenolic acid indicator solution, neutralize with ammonia solution until slightly red, add 0.5ml of glacial acetic acid solution and 0.5g Ascorbic acid, add 10mL saturated hydrogen sulfide water, shake and hang. Place in the dark for 10 minutes, the color should not be darker than the standard colorimetric solution.
The standard colorimetric solution is a 3mL lead standard solution taken with a pipette as a standard, except that no sample is added, and the sample is processed at the same time. 4.6 Determination of content
4.6.1 Summary of method
After the sample is treated, potassium iodide and stannous chloride are used to reduce the high valence to trivalent arsenic, and then the sample is treated with zinc metal. The new ecological hydrogen generated by the reaction with the acid will react to form arsenic hydrogen, which will form an arsenic spot on the mercuric bromide test paper. The arsenic content in the sample can be determined by comparing it with the standard arsenic spot. 4.6.2 Reagents and materials
4.6.2.1 Arsenic-free zinc particles.
4.6.2.2 Hydrochloric acid solution: 1+1.
4.6.2.3 Potassium iodide solution: 150g/L.
Stannic chloride solution: 400g/L.
4. 6.2. 4
Lead acetate cotton.
4.6.2.6 Mercuric bromide test paper.
4.6.2.7 Arsenic standard solution: 1mL solution contains 0.001mg of arsenic. Preparation: Use a pipette to take 10mL of arsenic standard solution prepared according to GB/T602, place it in a 1000mL volumetric flask, dilute with water to the scale, and shake it.
4.6.3 Instruments and equipment
Arsenic determination device. ||tt| |4.6.4 Analysis steps
Weigh about (1±0.01)g of sample, place in an arsenic test bottle, add 30mL of water to dissolve. Add 10mL of hydrochloric acid solution and shake. Add 2ml of potassium iodide solution and 1ml of stannous chloride solution, shake well, and leave for 15min. Add 3g of zinc granules, immediately assemble the device, and place at 251°C (in the dark) for 1S2
HG2940--2000
1～1.5h. The brown-yellow color of mercuric bromide test paper shall not be darker than the standard. The standard is to take 2ml of arsenic standard solution with a pipette, and treat it in the same way as the sample except that no sample is added. 4.7 Determination of barium content
4.7.1 Summary of the method
Add potassium chromate to the test solution with a pH value of 5 to 6 to generate barium chromate precipitation. Compare it with the standard turbidity solution. 4.7.2 Reagents and materials
4.7.2.1 Anhydrous sodium acetate.
4.7.2.2 Hydrochloric acid solution: 1+4,
4.7.2.3 Glacial acetic acid solution: 1+5.
4.7.2.4 Potassium chromate solution: 100g/1.
4.7.2.5 Nitrogen aqueous solution: 1+1.
4.7.2.6 Barium standard solution: 1ml. The solution contains 0.1mg of barium. 4.7.3 Instruments and equipment
Colorimetric tube: 50ml.
4.7.4 Analysis steps
Weigh (1 ± 0.01) g of the sample, place it in a beaker, add 10 ml of water, cover the surface blood, slowly add 8 ml of hydrochloric acid solution to dissolve it completely, heat and boil for 1 min, add ammonia solution until the pH value is about 8 (test with pH test paper), heat to boil, cool, filter with slow filter paper into a colorimetric tube, wash with a small amount of water, add 2 g of anhydrous sodium acetate, 1 mL of glacial acetic acid solution, 1 mL of potassium chromate solution, add water to the scale, and place it for 15 minutes for turbidity comparison. The turbidity of the sample should not be deeper than that of the standard turbidity solution. The standard turbidity solution is to take 3 mL of barium standard solution and add 3 mL of hydrochloric acid solution. The following operations are handled in the same way as the sample. 5 Inspection rules
5.1 All items in this standard are factory inspection items. 5.2 Each batch of feed-grade light calcium carbonate products shall not exceed 5 tons. 5.3 Determine the number of sampling units according to 6.6 of GB/T6678-1986. When sampling, insert the sampler vertically from the center of the package to three-quarters of the depth of the material layer. Mix the collected samples, reduce them to no less than 500g by the quartering method, and pack them in two clean and dry wide-mouth bottles with wall, and seal them. Paste labels on the bottles, indicating: manufacturer name, product name, batch number, sampling date and name of the sampler. · Bottle as laboratory sample. The other bottle is kept for three months for future reference. 5.4 Feed-grade light calcium carbonate 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 light calcium carbonate shipped from the factory meets the requirements of this standard. 5.5 The user has the right to accept the received feed-grade light calcium carbonate in accordance with the provisions of this standard, and the acceptance time shall be within one month after the arrival of the goods.
5.6 If one of the indicators in the inspection results does not meet the requirements of this standard, re-sampling shall be carried out from twice the amount of packaging for re-inspection. If even one of the indicators in the retest results does not meet the requirements of this standard, the entire batch of products shall be unqualified. 6 Marks and labels
6.1 The packaging container of feed-grade light calcium carbonate shall be firmly and clearly marked, including: manufacturer name, factory address, product name, trademark, "feed grade", net content batch number or production date, this standard number and the "wet-afraid" mark specified in GB191. 6.2 Each batch of feed-grade light calcium carbonate shipped out of the factory shall be accompanied by a firm and clear label printed in accordance with the requirements of GB10648. 7 Packaging, transportation and storage
7.1 Feed-grade light calcium carbonate is packaged in a plastic woven bag lined with a food-grade polyethylene film bag and an outer coat. The net content of each bag is 50kg. If the user has other requirements for packaging, they shall be resolved through negotiation.
HG29402000
7.2 When packaging feed grade light calcium carbonate, the inner packaging plastic bag should be tied twice with nylon rope, or sealed with other equivalent means. 11: The outer bag should be sewn with nylon 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 stitch lengths should be even. There should be no leaking seams or skipping.
7.3 During transportation, feed grade light calcium carbonate should be covered to prevent sun exposure, rain, and moisture. It is strictly forbidden to mix it with toxic and harmful substances. 7.4 Feed grade light calcium carbonate should be stored in a cool and dry place to prevent rain and moisture. It is strictly forbidden to coexist with toxic and harmful substances.
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