Some standard content:
HG2936
This standard is a non-equivalent revision of the chemical industry standard HG2936-1987 "Feed Grade Manganese Sulfate" based on the Japanese Feed Additive Safety Law Compendium (1995 Edition) "Manganese Sulfate" (hereinafter referred to as the "Compendium"). The technical indicators have reached the level of the Japanese Feed Additive Safety Law Compendium. The test method has made necessary modifications and supplements based on the actual verification of the current domestic production products. The main technical differences between this standard and the "Compendium" are:--The main content test method adopts the ammonium nitrate method, which is the same as the industrial manganese sulfate standard. It is safer, has a clear endpoint, and is easier to master than the method specified in the "Compendium".
The determination of lead content adopts the dithiol colorimetric method and atomic absorption spectrometry in parallel. The difference between the colorimetric method and the "Compendium" method is that chloroform is used instead of benzene in the organic phase, and hydroxylamine hydrochloride is used instead of sodium sulfite as the reducing agent. The test shows that the effect is better. According to the requirements of the feed industry, the fineness control is increased. The main technical differences between this standard and HG2936--1987 are as follows: the main content test method adopts the ammonium nitrate method, which is the same as the industrial manganese sulfate standard, which is more accurate, has a clear endpoint and is easier to master than the original method. … The heavy metal index is replaced by the lead content index, which is consistent with the "Essentials", and the corresponding test methods are added. … The provisions on fineness are corrected.
Appendix A of this standard is the appendix of the standard.
This standard will replace HG2936--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 Processing Plant. The main drafters of this standard are: Fan Guoqiang, Gao Zhanyou, Ma Ling, and Wu Chunqing. This standard was first issued as a national standard in 1987, and was adjusted to a mandatory chemical industry standard in 1997 and renumbered. This standard is entrusted to the technical unit responsible for standardization of inorganic salt products of the Ministry of Chemical Industry for interpretation. 165
Chemical Industry Standard of the People's Republic of China
Feed grade
Manganous sulfate
Feed grade-- Manganous sulphateHG2936-1999
Replaces HG29361987
This standard specifies the requirements, test methods, inspection rules, marking, packaging, transportation and storage of feed grade manganous sulfate. This standard applies to feed grade manganese sulfate. This product is used as a manganese supplement in feed after pretreatment. Molecular formula: MnSO4·H2O.
Relative molecular mass: 169.01 (according to the international 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 was published, the versions shown were all valid. All standards are subject to revision. Parties using this standard should explore the possibility of using the latest version of the following standards. GB/T 601--19881
Preparation of standard solutions for titration analysis (volume analysis) of chemical reagents GB/T 602--1988
Preparation of standard solutions for determination of impurities in chemical reagents (GB/T603--1988 Preparation of preparations and products used in test methods for chemical reagents GB/T 6003.1--1997
Wire mesh test sieves
GB/T6678-1986 General principles for sampling of chemical products GB/T 6682-1992
Specifications and test methods for water for analytical laboratories (negISO) 3696:1987) GB10648-1993 Feed labeling
3 Requirements
3.1 Appearance: White, slightly pink crystalline powder. 3.2
Feed grade manganese sulfate shall meet the requirements of Table 1.
Requirements of Table 1
Content of manganese sulfate (MnSO,·H,O)
Content of manganese sulfate (calculated as Mn)
Content of arsenic (As)
Content of lead (Pb)
Content of water-insoluble matter
Fineness (through 250um sieve)
Test methodWww.bzxZ.net
The reagents and water used in this standard, unless otherwise specified, refer to analytically pure reagents and grade 3 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 GB/T601, GB/T602 and GB/T603 as approved by the State Administration of Petroleum and Chemical Industry on 1999-06-16 and implemented on 2000-06-01.
4.1 Identification test
4.1.1 Identification of manganese ion
HG 2936--- 1999
Take 0.2g of sample and dissolve it in 50mL of water. Take 3 drops on the drip plate, add 2 drops of nitric acid, and add a little sodium bismuthate powder. No purple-red color is produced. 4.1.2 Identification of sulfate ions
Take the test solution, place it on a white porcelain plate, add 50g/L barium chloride solution, and a white precipitate will be produced, which is insoluble in hydrochloric acid and nitric acid. 4.2 Determination of manganese sulfate content
4.2.1 Summary of method
In phosphoric acid medium, use ammonium nitrate to quantitatively oxidize the divalent manganese in the sample to trivalent manganese at 220-240°C, use N-phenylanthranilic acid as an indicator, and titrate with standard ammonium ferrous sulfate titration solution. 4.2.2 Reagents and materials
4.2.2.1 Phosphoric acid.
4.2.2.2 Ammonium nitrate.
4.2.2.3 Anhydrous sodium carbonate.
4.2.2.4 N-phenylanthranilic acid indicator solution: 2g/L Weigh 0.2g N-phenylanthranilic acid, dissolve in a small amount of water, add 0.2g anhydrous sodium carbonate, heat at low temperature to dissolve, add water to 100mL, shake well:
4.2.2.5 Sulfur-phosphorus mixed acid.
Slowly add 150ml sulfuric acid and 150ml phosphoric acid to 700ml water, shake well, and cool. 4.2.2.6 Potassium dichromate standard solution: c (1/6K, Crz0,) is about 0.1mol/l. Accurately weigh about 4.9g (accurate to 0.0002g) of the standard potassium dichromate that has been baked at 120C to a constant mass, place it in a 1000ml volumetric flask, add appropriate amount of water to dissolve, dilute to the scale, and shake well. 4.2.2.7 Standard ammonium ferrous sulfate titration solution: c[Fe(NH4),(SO4), is about 0.1mol/L. The calibration of the standard ammonium ferrous sulfate titration solution should be carried out simultaneously with the sample determination. Preparation: Weigh 40g of ammonium ferrous sulfate, add 300mL of (1+4) sulfuric acid solution, add 700mL of water after dissolution, and shake. Calibration: Weigh 25mL of potassium dichromate standard solution, add 10mL of sulfuric acid and phosphorus mixed acid, and add water to 100mL. Titrate with the standard ammonium ferrous sulfate titration solution until the orange-yellow color disappears. Add 2 drops of N-phenylated anthranilic acid indicator solution and continue titrating until the solution turns bright green, which is the end point. The concentration (c) of the standard titration solution of ammonium ferrous sulfate is calculated according to formula (1): Vim
wherein. m-actual mass of potassium dichromate weighed, g; 49.03m molar mass of potassium dichromate (1/6KzCrz0,) g/mol; V.--volume of the standard potassium dichromate solution transferred, mL; V-----volume of the standard titration solution of ammonium ferrous sulfate consumed in the titration, mL. (1)
4.2.3 Analysis steps
Weigh about 0.5g of the sample (accurate to 0.0002g), place it in a 500mL conical flask, and moisten it with a small amount of water. Add 20ml of phosphoric acid, shake well, and heat to boil until the liquid surface is calm and white smoke is emitted slightly (the temperature is 220-240C at this time), remove from the heat source, immediately add 2g of ammonium nitrate and shake thoroughly to let the yellow smoke escape. After cooling to about 70°C, add 100 mL of water, shake thoroughly to dissolve the salts, and cool to room temperature. Titrate with standard ammonium ferrous sulfate solution until it turns light red, add 2 drops of N-phenylanthranilic acid indicator solution, and continue titrating until the solution changes from red to bright yellow, which is the end point.
4.2.4 Expression of analysis results
The content of manganese sulfate (MnS)·H) expressed as mass fraction (X,) is calculated according to formula (2): X(%)=
HG2936—1999
cV×0.169 0
The content of manganese sulfate (in terms of Mn) expressed as mass percentage (X,) is calculated according to formula (3): X(%)×0. 054 94×100V×5. 494. m
Wherein: c----actual concentration of ammonium ferrous sulfate standard titration solution, mol/LV---volume of ammonium ferrous sulfate standard titration solution consumed in titration, mL; mass of sample, g;
(2)
(3)
and 1.0.1690--
The mass of manganese sulfate expressed in grams equivalent to 1.00mL of standard ammonium ferrous sulfate titration solution (c[Fe(NH4+)(SO4+)]-1.000mol/L);
0.05494---The mass of manganese expressed in grams equivalent to 1.00mL of standard ammonium ferrous sulfate titration solution c[Fe(NH4+)z(SO4+)]-1.000mol/L).
4.2.5 Allowable difference
The arithmetic mean of the parallel determination results is taken as the determination result. The absolute difference between the two parallel determination results shall not exceed 0.5% in terms of MuSO4·H4+; and not exceed 0.2% in terms of manganese.
4.3 Determination of content
4.3.1 Summary of 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 hydrogen hydride gas, forming a brown-yellow arsenic spot on the mercuric bromide test paper, which is compared with the standard arsenic spot. 4.3.2 Reagents and materials
4.3.2.1 Hydrochloric acid.
4.3.2.2 Arsenic-free metallic zinc.
4.3.2.3 Potassium iodide.
4.3.2.4 Stannous chloride solution: 400g/1. 4.3.2.5 Standard solution: 1mL of solution contains 0.001mg of arsenic. Use a pipette to transfer 10mL of the arsenic standard solution prepared according to GB/T602, place it in a 1000mL volumetric flask, dilute it to the mark with water, and shake it well. This solution is for use only on the same day.
4.3.2.6 Lead acetate cotton.
4.3.2.7 Mercuric bromide test paper.
4.3.3 Instruments and equipment
Arsenic analyzer.
4.3.4 Analysis steps
Weigh (1.00±0.01)g of sample, place in a test bottle, dissolve with water and dilute to about 70mL. Add 6mL of hydrochloric acid, shake well, add 1g of potassium iodide and 5 drops of stannous chloride solution, shake well, and leave for 10min. Add 3g of arsenic-free metal zinc to the arsenic test bottle, immediately plug the arsenic test tube pre-filled with lead acetate cotton and mercuric bromide test paper and place in the dark for 1h. Take out the mercuric bromide test paper and observe. The color of the sample spot should not be darker than the standard. The standard is to use a pipette to transfer 5.00mL of arsenic standard solution and treat it in the same way as the sample. 4.4 Determination of lead content
4.4.1 Atomic absorption spectrometry (arbitration method) 4.4.1.1 Summary of the method
Dissolve the sample with acid and determine with air-acetylene flame at 283.3nm. 4.4.1.2 Reagents and materials
4.4.1.2.1 Nitric acid solution: 2+3.
4.4.1.2.2 Hydrochloric acid solution: 1+1
HG 2936---1999
4.4.1.2.3 Lead standard stock solution: 1ml solution contains 0.1mg lead. Accurately weigh 0.1598g lead nitrate [Pb(NO:)], add 8mL of 1+1 nitric acid, and after all are dissolved, transfer to a 1000ml volumetric flask and add water to the mark.
4.4.1.2.4 Lead standard working solution: 1 ml of solution contains 0.01 mg of lead. Accurately transfer 10 ml of lead standard stock solution into a 100 ml volumetric flask, add water to the mark, and shake to check. 4.4.1.3 Instruments and equipment
Atomic absorption spectrophotometer: equipped with a lead hollow cathode lamp. 4.4.1.4 Analysis steps
4.4.1.4.1 Drawing of working curve
Take 5 100 ml volumetric flasks, transfer 0.00, 1.00, 1.50, 2.00, and 3.00 ml of lead standard working solution, dilute with water to the mark, and shake well.
On the atomic absorption spectrophotometer, use an air-acetylene flame, adjust to zero with distilled water at a wavelength of 283.3 nm, and measure the absorbance of the above solution.
Use the mass of lead added to the standard solution as the horizontal axis and the corresponding absorbance as the vertical axis to draw a working curve. 4.4.1.4.2 Determination
Weigh about 2.5g of the sample (accurate to 0.01g), place it in a 100mL beaker, moisten it with a small amount of water, add 10ml. nitric acid solution and 10mL hydrochloric acid solution, place it on an electric heating plate, steam it until it is almost dry, add appropriate amount of water to dissolve it, and then transfer it to a 100mL volumetric flask to make up the volume (if there is a precipitate, it should be dry filtered before being introduced into the atomic absorption spectrophotometer). At the same time, perform a blank test. Measure the absorbance on the atomic absorption spectrophotometer under the same conditions as the working curve, and find the corresponding mass of lead on the working curve. 4.4.1.5 Expression of analysis results
The lead (Pb) content (X:) expressed as a mass percentage is calculated according to formula (4): X3(%) =
(mlmo)X10-3
Wherein: ml---the mass of lead in the sample found on the working curve, mg; mo---the mass of lead in the blank test found on the working curve, mg; m---the mass of the sample, g.
4.4.1.6 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 0.0004%. 4.4.2 Extraction colorimetry
Safety tips: This method uses highly toxic potassium cyanide during operation, so be careful to avoid contact or inhalation by the human body. 4.4.2.1 Method Summary
(4)
Under normal conditions, use potassium fluoride to mask interfering metal ions other than lead, use disulfide-chloroform solution to extract lead in the sample and develop color with it, compare with the standard, and judge whether the lead content is within the limit. 4.4.2.2 Reagents and Solutions
4.4.2.2.1 Hydroxylamine hydrochloride.
4.4.2.2.2 Ammonium citrate solution: 400g/L. 4.4.2.2.3 Ammonia-ammonium chloride buffer solution: pH=10. 4.4.2.2.4 Potassium cyanide solution: 150g/L. 4.4.2.2.5 Disulfide-chloroform solution. Dissolve 0.02g disulfide in 1L chloroform and store at 10℃ away from light. 4.4.2.2.6 Lead standard solution: 1mL solution contains 0.010mg lead. Prepare according to GB/T602 and dilute accurately 10 times. 4.4.2.3 Analysis steps
HG 2936--1999
Weigh (0.500.01)g sample, add 20mL water to dissolve the sample, add 5ml ammonium citrate, shake to hook; add 0.5g hydroxylamine hydrochloride, shake with a spoon. Add 5ml ammonia-ammonium chloride buffer solution and 2ml potassium chloride solution, shake well. Add 5ml dithiol-chloroform solution and shake for 1min. The color of the solution shall not turn red.
The standard is to use a pipette to transfer 0.5ml lead standard solution and treat it in the same way as the sample. 4.5 Determination of water-insoluble matter content
4.5.1 Reagents and materials
Barium chloride solution: 100g/l.
4.5.2 Instruments and equipment
Glass sand: The pore size of the filter plate is 5~15μm.
4.5.3 Analysis steps
Weigh about 10g of sample (accurate to 0.01g), place it in a 250mL beaker, and add 100mL of water to remove carbon oxides to dissolve it. Filter it with a glass sand crucible that has been dried to a constant mass at 105~110℃, wash it with hot water until there is no sulfate (check with barium chloride solution), and dry it at 105~~110℃ to a constant mass.
4.5.4 Expression of analysis results
The water-insoluble content (X,) expressed as a mass percentage is calculated according to formula (5): X(%)=ml=\2 ×100 **
Where: m\-the mass of the glass sand crucible and water-insoluble matter, g, m…-·the mass of the glass sand crucible, g;
m.-- The mass of the sample, g.
4.5.5 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 0.01%. 4.6 Determination of fineness
4.6.1 Instruments and equipment
Test sieve: in accordance with the requirements of GB/T6003R40/3 series, Φ200mm×50mm/250μm, equipped with sieve cover and sieve bottom. 4.6.2 Analysis steps
Weigh (50±0.1)g of sample, put it into the test sieve, install the sieve cover and sieve bottom The sieve bottom is screened. Collect the sieve underflow that falls to the sieve bottom and weigh the mass of the sieve underflow (accurate to 0.1g).
4.6.3 Expression of analysis results
The mass percentage (Xs) passing through the test sieve is calculated according to formula (6): m×100
X;(%)=
Where.㎡.Mass of the sieve underflow, g;
Mass of the sample, g.
4.6.4 Filling the 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 0.5%. 5 Inspection rules
5.1 All items specified in this standard are used as factory inspection items. 5.2 The batch of products shall not exceed 50.
(6)
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 reduced to about 500g by the quartering method and immediately packaged into two smooth and clean bottles and sealed. Labels are attached to the bottles, indicating: manufacturer name, product name, batch number, sampling date and sampler name. 170
bottles are used for inspection, and the other bottle is kept for three months for reference. HG2936--1999
5.4 Feed-grade manganese sulfate shall be inspected by the quality supervision and inspection department of the manufacturer in accordance with this standard. The manufacturer shall ensure that all the feed-grade manganese sulfate shipped out of the factory meets the requirements of this standard. Each batch of feed-grade manganese sulfate shipped out of the factory shall be accompanied by a quality certificate, the content of which is the same as that of GB10648.
5.5 If one of the indicators does not meet the requirements of this standard, samples shall be taken from twice the amount of packaging for re-inspection. If only one indicator does not meet the requirements of this standard as a result of the re-inspection, the entire batch of products shall be unqualified. 6 Marking, packaging, transportation, storage
6.1 The packaging of feed-grade manganese sulfate shall have a quality certificate in accordance with GB1 0648 requires a firm and clear printed mark. 6.2 Each batch of products leaving the factory should have a quality certificate. The content includes: manufacturer name, factory address, product name, trademark, net content, batch number or production date, proof that the product quality complies with this standard and the number of this standard. 6.3 Feed grade manganese sulfate is packaged in plastic woven bags. The inner lining is a layer of polyethylene film bag with a thickness of not less than 0.07mm, and the outer cover is a polypropylene woven bag. The net content of each bag is 25kg or 50kg, and it can also be packaged according to user requirements. 6.4 The inner bag is tied with nylon rope or other equivalent quality The outer bag should be folded at a distance of not less than 30mm from the bag edge, and the edge should be sewn 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, the stitches should be evenly spaced, and there should be no leakage or skipping.
6.5 During storage, feed grade manganese sulfate products should be protected from sunlight and rain, and it is forbidden to store them together with toxic and hazardous substances. 6.6 During transportation, feed grade manganese sulfate products should be protected from packaging damage, sunlight and rain, and it is forbidden to transport them together with toxic and hazardous substances. The shelf life is 24 months
HG 2936--1999
(Appendix to the standard)
Treatment of cyanide waste liquid
In order to prevent the pollution of cyanide waste liquid, the fluoride waste liquid should be post-treated after daily analysis before it can be discharged. A1 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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