Some standard content:
HG29321999
This standard is a revision of the chemical industry standard HG2932--1987 "Feed Grade Sulfuric Acid" based on the product specifications of the Japanese Feed Additive Safety Law (1995 Edition) "Copper Sulfate" (hereinafter referred to as the "Compendium") The main differences between this standard and the "Compendium" are: - The arsenic index of this standard is not more than 0.0004%, while that of the "Compendium" is not more than 0.0005%. ·According to user requirements, water content and fineness indicators have been added. - The determination of copper sulfate pentahydrate content in the test method is equivalent to the method specified in the "Compendium"; the determination of lead content adopts dithiol-chloromethane extraction colorimetry and atomic absorption spectrophotometry in parallel. The difference between the colorimetry method and the Japanese method is that chloramine is used instead of benzene in the organic phase, and hydroxylamine hydrochloride is used instead of sodium sulfite as the reducing agent; the determination methods of other items all adopt relevant standards of my country. The main technical differences between this standard and HG2932-1987 are: the content of stele is reduced from 0.0005% to 0.0004%, which improves the standard level. - The heavy metal index is cancelled and replaced by the lead content index, which is consistent with the Japanese standard, and the corresponding test methods are added. - The determination method of stele and lead content has been greatly improved. Appendix A of this standard is the appendix of the standard.
This standard will replace HG2932-1987 from the date of implementation. This standard was proposed by the former Technical Supervision Department of the Ministry of Chemical Industry. This standard is under the jurisdiction of the inorganic salt product standardization technical unit of the Ministry of Chemical Industry. The drafting units of this standard are: Tianjin Chemical Research Institute of the Ministry of Chemical Industry, Tianjin Veterinary Drug Factory No. 2, and Chengdu Shuxing Mineral Element Pretreatment Plant. The main drafters of this standard are: Liu Shuying, Gao Zhanyou, Ma Ling, Wu Chunqing, and Zhang Zhiping. This standard was first issued as a national standard in 1987, and was adjusted to a mandatory chemical industry standard in 1997, and was renumbered. This standard is entrusted to the inorganic salt product standardization technical unit of the Ministry of Chemical Industry for interpretation. 1 Scope
Chemical Industry Standard of the People's Republic of China
Feed grade
Copper sulfate
Feed grade---Cupric sulphate1999
HG 2932
Replaces HG29321987
This standard specifies the requirements, test methods, inspection rules, and marking, packaging, transportation, and storage of feed grade copper sulfate. This standard applies to feed grade copper sulfate, which is used as a copper supplement in feed after pretreatment. Molecular formula: CuSO, ·5H,O
Relative molecular mass: 249.68 (according to the 1995 international relative atomic mass) 2
Cited 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, and parties using this standard should explore the possibility of using the latest versions of the following standards. GB/T601--1988 Chemical reagents - Preparation of standard solutions for titration analysis (volumetric analysis) GB/T 602--1988
GB/T 603--1988
Chemical reagents
Chemical reagents
GB/T 6003—1985
Test sieves
GB/T 6678--1986
GB/T 6682—1992
GB 10648--1993
3 Requirements
Preparation of standard solutions for determination of impurities
Preparation of preparations and products used in test methods General rules for sampling of chemical products
Specifications and test methods for water for analytical laboratories (negISO3696:1987) Feed label
3.1 Appearance: light blue crystalline granules.
3.2Feed grade copper sulfate shall meet the requirements of Table 1. Table 1 Requirements
Content of copper sulfate (CuSO,·5H,O)
Content of copper sulfate (measured in Cu)
Content of water insoluble matter
Content of As
Content of lead (Pb)
Fineness (passing 800μm test sieve)
Note: The fineness of the product without pretreatment is not required. Approved by the State Administration of Petroleum and Chemical Industry on June 16, 1999
Implementation on June 1, 2000
4Test methods
HG2932--1999
The reagents and water used in this standard, unless otherwise specified, refer to analytical reagents and secondary water specified in GB/T6682. The standard titration solution, impurity standard solution, preparation and product used in the test, unless otherwise specified, shall be prepared in accordance with the provisions of (GB/T\601, GB/T602, GB/T603).
4.1 Identification test
4.1.1 Identification of copper ions
Weigh 0.5g of the sample and dissolve it in 20ml of water. Take 10ml of this solution, add 0.5ml of the newly prepared 100g/l potassium ferrocyanide solution, shake, and a reddish-brown precipitate will be generated. This precipitate is insoluble in dilute acid. 4.1.2 Identification of sulfate ions
Take 5mL of the above test solution, place it on a white porcelain plate, add 50g/l fluoride solution, and a white precipitate will be generated. It is not soluble in hydrochloric acid and nitric acid. Dissolve.
4.2 Determination of copper sulfate content
4.2.1 Summary of the method
The sample is dissolved in water. Under slightly acidic conditions, an appropriate amount of potassium iodide is added to react with divalent copper to precipitate an equivalent amount of iodine. Starch is used as an indicator. The precipitated iodine is titrated with a standard sodium thiosulfate solution. The copper sulfate content in the sample is calculated from the volume of the consumed standard sodium thiosulfate solution:
4.2.2 Reagents and materials
4.2.2.1 Potassium iodide.
4.2.2.2 Glacial acetic acid.
4.2.2.3 Starch indicator solution: 5g/L.
4.2.2.4 Standard sodium thiosulfate solution: c(NazS2O.) is approximately 0.1 mol/l. 4.2.3 Analysis steps
Weigh about 1g of sample (accurate to 0.0002g), place it in a 250mL iodine volumetric flask, add 100mL of water to dissolve, add 4ml of glacial acetic acid, add 2 potassium iodide, shake it, and place it in a dark place for 10min. Titrate with sodium thiosulfate standard titration solution until the solution turns light yellow, add 3ml of starch indicator solution, and continue titrating until the blue color disappears, which is the end point. 4.2.4 Expression of analysis results
The copper sulfate (CuS()4·5H,O) content (XI) expressed in mass percentage is calculated according to formula (1): X(%)=sVx0. 249 7 ×100-24. 97Vcm
The copper sulfate (Cu) content (X) expressed in mass percentage is calculated according to formula (2): X(%)-sV×0. 063 55 ×100=6. 355Vcm
Where: ---actual concentration of sodium thiosulfate standard titration solution, mol/L; V is the volume of sodium thiosulfate standard titration solution consumed during titration.mI.m---mass of sample, g;
(2)
0.2497.-mass of copper sulfate pentahydrate equivalent to 1.00mL sodium thiosulfate standard titration solution c(Na2S.O)=1.000mol/L] in grams;
0.06355--mass of copper equivalent to 1.00mL sodium thiosulfate standard titration solution Lc(Na2S0,)1.000mol/L7 in grams.
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 determination results shall not exceed 0.2%. 4.3 Determination of water-insoluble matter content
4.3.1 Method summary
HG 2932- 1999
Dissolve the sample in water, filter, wash, dry and weigh. 4.3.2 Reagents and materials
Ammonia solution: 1+1.
4.3.3 Instruments and equipment
4.3.3.1 Glass crucible: pore size 5~15μm. 4.3.3.2 Electric oven: temperature can be controlled at 105~~110℃. 4.3.4 Analysis steps
Weigh about 10g of sample (accurate to 0.0002g), place it in a 400mL beaker, add 200ml of water until the sample is dissolved, and filter it with a glass crucible that has been dried to a constant mass at 105-110℃ in advance. Wash the filter residue with hot water until the washing liquid is colorless, and check with ammonia water until there is no copper ion reaction. Place the glass crucible in an oven and dry it at 105-110℃ until the mass is constant. Take it out and place it in a desiccator to cool and then weigh it.
4.3.5 Expression of analysis results
The water-insoluble content (X3) expressed as a mass percentage is calculated according to formula (3): m×100
X,(%) =
wherein m..mass of the residue after drying, g;
mass of a sample, g.
4.3.6 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 0.05%. 4.4 Determination of arsenic content
4.4.1 Summary of the method
In an acidic solution, potassium iodide and stannous chloride are used to reduce high-valent arsenic to trivalent arsenic. Trivalent arsenic reacts with new ecological hydrogen to generate arsenic hydrogen gas, forming a brown-yellow arsenic spot on the mercuric bromide test paper, which is compared with the standard arsenic spot. 4.4.2 Reagents and materials
4.4.2.1 Hydrochloric acid.
Acetic acid.
I.-Ascorbic acid.
Arsenic-free metallic zinc.
Potassium iodide.
Stannofluoride solution: 400g/L.
Arsenic standard solution: 1ml solution contains 0.001mg arsenic, prepared before use. 4.4.2.7
Preparation: Use a pipette to transfer 10mL of arsenic standard solution prepared according to GB/T602, place it in a 1000mL volumetric flask, dilute to the mark with water, and shake it.
4.4.2.8 Lead acetate cotton.
4.4.2.9 Mercuric bromide test paper.
4.4.3 Instruments and equipment
Arsenic determination device.
4.4.4 Analysis steps
Weigh (0.25±0.01)g of sample, place it in a 100mL beaker, add 5mL of water to dissolve, add 2mL of acetic acid and 1.5g of potassium iodide, cover the surface III, and leave it for 5min. Add 0.2g L-ascorbic acid to dissolve it as the detection solution. Place the detection solution in the wide-mouth bottle of the arsenic analyzer, dilute it to 40ml with water, add 6mL hydrochloric acid, and shake well. Add 1g potassium iodide, add stannous nitride solution dropwise until the solution is colorless, shake well, and let it stand for 10)min. Add 2.5g arsenic-free zinc, and immediately put it on the arsenic test tube pre-installed with lead acetate cotton and mercuric bromide test paper. Place it in a dark place at: 25~～30（137bzxz.net
HG 2932 -- 1999
for 1～1.5h, and the mercuric bromide test paper will be a brown-yellow standard colorimetric solution that is not darker. The standard colorimetric solution is to take 1. 0 mL of arsenic standard solution with a pipette and dilute it to 40 with water ml., add 6 ml of hydrochloric acid and treat it in the same way as the test solution.
4.5 Determination of lead content
4.5.1 Atomic absorption spectrophotometry (arbitration method) 4.5.1.1 Method summary
In dilute nitric acid medium, use an air-acetylene flame at a wavelength of 283.3 nm on an atomic absorption spectrophotometer and use the standard addition method.
4.5.1.2 Reagents and materials
4.5.1.2.1 Nitric acid solution: 1+1.
4.5. 1.2.2 Lead standard solution: 1 ml. Contains 0.01 mg lead, prepared just before use. Preparation: Use a pipette to transfer 10 ml of the lead standard solution prepared according to GB/T602, place it in a 100 ml volumetric flask, dilute to the mark with water, and shake to adjust.
4.5.1.3 Instruments and equipment
4.5.1.3.1 Atomic absorption spectrophotometer. 4.5.1.3.2 Lead hollow cathode lamp.
4.5.1.4 Instrument working conditions
4.5.1.4.1 Wavelength: 2 83.3nm.
4.5.1.4.2 Flame: Air-B.
4.5.1.5 Analysis steps
Weigh about 10g of sample (accurate to 0.01g), add 50ml of water and 5ml of nitric acid solution to dissolve the sample. Transfer to a 250ml volumetric flask, dilute to the mark with water, and shake to hang. Use a pipette to transfer 25ml of the test solution to 4 100ml volumetric flasks, and then use a pipette to add 0, 1, 2, and 3ml of lead standard solution, dilute to the mark with water, and shake to hang. Hook. Adjust the instrument to the optimal condition, adjust it to zero with water, and measure the absorbance. Use the mass of lead as the horizontal axis and the corresponding absorbance as the vertical axis to draw a working curve, and extend the curve in the opposite direction to the intersection with the horizontal axis. This is the lead content in the test solution.
4.5.1.6 Expression of analysis results
The lead (Pb) content (X.) expressed as mass percentage is calculated according to formula (4): m
m×1000×100=
Where m is the mass of lead in the test solution found from the working curve, mgm - Mass of the sample, g.
4.5.1.7 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 0.0003%. (4)
4.5.2 Dithiol colorimetric method
Safety tips: The sodium cyanide (or potassium cyanide) used in this test is a highly toxic drug. Be careful when operating it, prepare safety equipment, and avoid contact or inhalation. For the treatment of cyanide-containing waste liquid, see Appendix A. 4.5.2.1 Method summary
After the sample is dissolved in water, ammonium citrate, potassium cyanide and hydroxylamine hydrochloride are added to eliminate the interference of iron, copper, zinc and other ions. At pH=10, lead ions and dithiol form a red complex. Use chloroform to extract metallic lead from the sample solution and compare the color with the standard colorimetric solution.
4.5.2.2 Reagents and materials
4.5.2.2.1 Hydroxylamine hydrochloride.
4.5.2.2.2 Ammonium citrate solution: 400g/1. HG 2932--1999
4.5.2.2.3 Ammonia-ammonium chloride buffer solution A (pH=10). 4.5.2.2.4 Sodium cyanide (or potassium cyanide) solution: 200g/L. 4.5.2.2.5 Dithiol-chloroform solution: 0.02g/1 (stored in refrigerator) 4.5.2.2.6 Lead standard solution: 1ml contains 0.01mg lead, prepared before use. Preparation: Use a pipette to take 10ml of the lead standard solution prepared according to GB/T602, place it in a 100ml volumetric flask, dilute to the mark with water, and shake to check.
4.5.2.3 Analysis steps
Weigh (0.5±0.01)g of sample, place in a 50ml colorimetric tube, add about 10ml of water to dissolve, add 5ml of ammonium citrate, 5ml of ammonia-ammonium nitride buffer solution A (pH=10), add sodium cyanide (or potassium cyanide) solution until the solution is colorless, then add 5 drops of excess, add 0.5g of hydroxylamine hydrochloride, shake the spoon, add 5ml of disulfide-trichloromethane, shake for 1min, and compare the color of the extraction layer with the standard colorimetric solution according to the red color. The darker the red, the higher the lead content.
The standard filling colorimetric solution is to pipette 0.5mL of standard solution, and write the sample at the same time. 4.6 Determination of fineness
4.6.1 Summary of methods
The content of the sieve is determined by sieving method.
4.6.2 Instruments and equipment
Test sieve: meet the requirements of GB/T6003R40/3 series, $200mm×500mm/800μm. 4.6.3 Analysis steps
Weigh 50g of sample (accurate to 0.1g). Place it in the test sieve for sieving, and weigh the sieve underweight (accurate to 0.1g). 4.6.4 Expression of analysis results
The fineness (X) expressed as mass percentage is calculated according to formula (5): X, (%)-m×100
Where: n\mass of sieve underweight;
mass of sample, g.
4.6.5 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 0.1%. 5 Inspection rules
5.1 All items specified in this standard are factory inspection items. (5)
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. When sampling, insert the sampler obliquely from the top of the packaging bag to three-quarters of the depth of the material layer to take samples. After the sample is fully mixed, it is divided into about 500g according to the quartering method and immediately divided into two clean and dry wide-mouth bottles with stoppers and sealed. Labels are attached to 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 The quality supervision and inspection department of the manufacturer shall inspect the feed-grade copper sulfate in accordance with the provisions of this standard. The manufacturer shall ensure that all feed-grade copper sulfate shipped out of the factory meets the requirements of this standard. Each batch of feed-grade copper sulfate shipped out of the factory should be accompanied by a quality certificate, the content of which is the same as that of GB10648.
5.5 If any index in 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 index in the re-test results does not meet the requirements of this standard, the entire batch of products will be unqualified. 13
6 Marking, packaging, transportation, storage
HG2932
6.1. The packaging bag of feed-grade copper sulfate should have a firm and clear mark, and the content is the same as that of GB10648. 6.2 Feed-grade copper sulfate is double-packed. The inner packaging is a two-layer food-grade polyethylene plastic film bag with a thickness of not less than 0.06mm, and the outer packaging is a polypropylene plastic woven bag. The net content of each bag of this product is 25kg, or it can be packaged according to user requirements. 6.3 For the packaging of feed-grade copper sulfate, the inner bag is tied with vinyl rope or 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 edge of the bag, and sewn with vinyl thread or other thread of equivalent quality at a distance of not less than 15mm from the edge of the bag. The stitches are neat, the stitches are uniform, and there is no leakage or skipping. 6.4 Feed-grade copper sulfate should be covered during transportation to prevent rain and moisture, and it must not be mixed with toxic and harmful substances. 6.5 Feed-grade copper sulfate should be stored in a cool and dry place to prevent rain and moisture. It must not be mixed with toxic and harmful substances. 140
HG2932--1999
Appendix A
(Standard Appendix)
Treatment of cyanide waste liquid
In order to prevent the pollution of cyanide waste liquid, the cyanide waste liquid should be post-treated before discharge after each analysis. Method Summary
Under alkaline conditions, divalent iron and cyanide ions form stable complex ions. Analysis steps
Collect the waste liquid in a 500mL beaker, add 50ml of 200g/L ferrous sulfate solution, stir, and discharge after sufficient reaction. The above-mentioned reagents are all industrial grade.
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