Some standard content:
HG2935--2000
This standard is a non-equivalent adoption of the "Ferrous Sulfate" in the "Japanese Feed Safety Law Summary" (1995 edition), and is revised from the chemical industry standard HG2935---1987 "Feed Grade Ferrous Sulfate". The main differences between this standard and the "Ferrous Sulfate" in the "Japanese Feed Safety Law Summary" (1995 edition) are as follows: In addition to ferrous sulfate monohydrate, this standard also stipulates the technical requirements for ferrous sulfate heptahydrate. The drying loss is cancelled, and the fineness requirements are stipulated for monohydrate products. The determination of ferrous sulfate content is changed to potassium dichromate method. The technical differences between this standard and HG2935-1987 are as follows: ... The original standard only stipulates the indicators of ferrous sulfate heptahydrate. At present, most of the ferrous sulfate used in feed in China is ferrous sulfate water. Therefore, based on the actual use of the product, this standard adds the requirements for ferrous sulfate monohydrate on the basis of the original standard--·Cancel the fineness of ferrous sulfate heptahydrate. The potassium dichromate method was used to determine the content of ferrous sulfate, and the dissolution of the sample was improved. …---The silver diethyldithiocarbamate spectrophotometry method was used to determine the content of arsenic. \--The method for determining the content of lead (Pb) was the method specified in the "Japanese Feed Safety Law Summary", and the atomic absorption method was added. This standard will replace HG2935-1987 from the date of implementation. This standard was 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 Technical Committee for Chemical Standardization. The drafting units of this standard are: Tianjin Chemical Research and Design Institute, Hunan Wangcheng Feed Additive Factory, and Shandong Anqiu Chemical Agent Factory. The main drafters of this standard are: Lu Siwei, Dai Deheng, Huang Nini, Wang Heping, and Meng Fanyu. This standard was first issued as the national standard GB8252-1987 in 1987. It was adjusted to the chemical industry standard in 1997 and the number was changed to HG 2935-1987.
This standard is entrusted to the Inorganic Chemical Branch of the National Technical Committee for Chemical Standardization for interpretation. 1
1 Scope
Chemical Industry Standard of the People's Republic of China
Feed grade
Ferrous sulfate
Feed grade--Ferrous sulfate
HG2935—2000
Replaces HG2935---1987
This standard specifies the requirements, test methods, inspection rules, signs, labels, packaging, transportation and storage of feed grade ferrous sulfate. This standard applies to feed grade ferrous sulfate in monohydrate or heptahydrate. This product is used as an iron supplement in feed processing. Molecular formula: FeSO4nH2O, n=1 or 7
Relative molecular mass: 169.93 (n=1) 278.01 (n-7) (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. Parties using this standard should explore the possibility of using the latest versions of the following standards: GB/T601--1988 Preparation of standard solutions for titration analysis (volumetric analysis) of chemical reagents GB/T602—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 6678--1986 General rules for sampling of chemical products GB/T6682-1992 Specifications and test methods for water for analytical laboratories (neqISO3696:1987) GB 10648—1999 3 Classification Feed labeling Feed-grade ferrous sulfate is divided into two categories: ferrous sulfate monohydrate and ferrous sulfate heptahydrate. 4 Requirements
4.1 Appearance: Ferrous sulfate heptahydrate is grayish white powder; ferrous sulfate heptahydrate is blue-green crystals. 4.2 Feed grade ferrous sulfate shall meet the requirements of Table 1. Table 1 Requirements
Ferrous sulfate content
Iron (Fc) content
Lead (Pb) content
Arsenic (As) content
Fineness (passing 180μm test sieve)
Approved by the State Administration of Petroleum and Chemical Industry on June 5, 2000158
Ferrous sulfate heptahydrate
(FeSO, : H2O)
Ferrous sulfate heptahydrate
(FeSO4 : 7H,0)
Implementation on March 1, 2001
5 Test method
HG 2935-2000
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 product used in the test, unless otherwise specified, shall be prepared in accordance with the provisions of (13/T601, GB/T602. GB/T603.
Safety Tips: The strong acid and alkali used in this standard are corrosive, and users should be careful when handling; if splashed on the skin, rinse immediately with plenty of water, and seek medical treatment immediately in severe cases.
5.1 Identification Test
5.1.1 Reagents and Materials
5.1.1.1 Potassium ferrocyanide solution: 100g/l. 5.1.1.2 Barium chloride solution: 50g/l. 5.1.2 Identification Method
5.1.2.1 Identification of Sulfate Ions
Take a small amount of sample, dissolve it in water, and add barium chloride solution dropwise to generate a white precipitate. This precipitate is insoluble in hydrochloric acid and nitric acid. 5.1.2.2 Ferrous Ions Identification
Take a small amount of sample, add water to dissolve, add potassium ferrofluoride solution, and generate a dark blue precipitate. 5.2 Determination of ferrous sulfate content and iron content 5.2.1 Method summary
After the sample is dissolved, add sulfuric acid and phosphoric acid, use sodium diphenylamine sulfonate as an indicator, and titrate with potassium dichromate standard titration solution to determine the ferrous sulfate content and iron content.
5.2.2 Reagents and materials
5.2.2. 1 sodium bicarbonate.
Hydrochloric acid solution: 1 + 1.
Sulfur-phosphorus mixed acid: add 150mL sulfuric acid (p = 1.84g/ml) and 150mL phosphoric acid (p - 1.70g/ml) to 700mL water, and mix 5.2.2.4
Saturated sodium bicarbonate solution.
Potassium dichromate standard titration solution: c (1/6K, Cr20,) is about 0.1mol/1.5. 2.2. 5
Sodium diphenylamine sulfonate indicator solution: 5g/L.
5.2.3 Analysis steps
Weigh about 0.15g of sample (accurate to 0.0002g), place in a 250ml iodine volumetric flask, add 10mL hydrochloric acid solution, add 5g sodium bicarbonate, quickly cover the bottle mouth with a rubber stopper with a catheter, slowly heat on an electric stove until the sample is completely dissolved, remove it, and quickly insert the other end of the catheter into a saturated sodium bicarbonate solution. After cooling to room temperature, remove the rubber stopper, add 10ml sulfuric acid and phosphorus mixed acid, 2 drops of sodium diphenylamine sulfonate indicator solution, and titrate with potassium dichromate standard titration solution until the solution turns purple as the end point. Perform a blank test at the same time.
5.2.4 Expression of analysis results
The content of ferrous sulfate (FeSO4·H2O) (X) expressed as mass percentage is calculated according to formula (1): (Vi-Vo)c×0. 169 9 × 100 16. 99 (V-Vo) cX, (%) =
The content of ferrous sulfate heptahydrate (FeSO,·7HzO) expressed as mass percentage (X,) is calculated according to formula (2): (V-Vo) c × 0. 278 0 × 10 = 27. 80 (V.-Vo) cX2 (%) =
The content of iron (Fe) expressed as mass percentage (X:) is calculated according to formula (3): Xx (%) = V-Vo) c × 0. 55 85 × 100 = 5. 585 (V = Va) cm
(3)
HG 2935-2000
Wherein: .--Actual concentration of potassium dichromate standard titration solution, mol/.V,--Volume of potassium dichromate standard titration solution consumed by titrating blank solution, mL; V,--Volume of potassium dichromate standard titration solution consumed by titrating test solution, ml.; m:
Mass of sample,
0.1699---Mass of ferrous sulfate in water equivalent to 1.00mL potassium dichromate standard titration solution [c(1/6K.Cr0,)=1.000mol/L.1 in grams;
0.2780---Mass of ferrous sulfate heptahydrate equivalent to 1.00mL potassium dichromate standard titration solution [c(1/6K,Cr2,)=1.000mol/L] in grams;
0.05585--.Equivalent to 1.00ml potassium dichromate standard titration solution Lc (1/6K.Cr20) 1.000mol/1] is equivalent to the mass of iron in grams.
5.2.5 Allowable difference
The arithmetic mean of the parallel determination results is taken as the determination result. The absolute difference of the parallel determination results: ferrous sulfate is not more than 0.3%, and the iron content is not more than 0.1%.
5. 3 Determination of arsenic content
5.3.1 Method summary
After the sample is treated, potassium iodide and stannous chloride are used to reduce the high-valent arsenic to trivalent arsenic, and then the new ecological hydrogen generated by the reaction with metallic zinc and acid reacts to generate arsenic hydrogen. After being absorbed by the silver salt solution, a red complex is formed, and its absorbance is measured at a wavelength of 522nm using a spectrophotometer.
5.3.2 Reagents and materials
5.3.2.1 Arsenic-free zinc particles.
5.3.2.2 Sulfuric acid solution: 1+1.
5. 3.2. 5
Tartaric acid solution: 500g/L.
Potassium iodide solution: 150g/L.
Stannoic chloride solution: 400g/L.
Lead acetate cotton.
Silver ethyl dithiocarbamate-blue ethylamine-trifluoromethane absorption solution. 5.3.2.7
Arsenic standard solution: 1ml. The solution contains 0.001mg of stelae. 5.3.2.8
Preparation: Use a pipette to transfer 10mL of the arsenic standard solution prepared according to GB/T602, place it in a 1000mL volumetric flask, dilute to the mark with water, and shake well (this solution is prepared when used). 5.3.3 Instruments and equipment
5.3.3.1 Arsenic generator (see Figure 1). 160
HG2935
1--Monument generator bottle; 2-Connecting tube; 3-15-ball absorption tube Figure 1 Arsenic generator
5.3.3.2 Spectrophotometer: with 1cm cuvette. 5.3.4 Drawing of working curve
Use a pipette to transfer 0.00, 2.00mL, 5.00mL, 6.00mL, 8.00mL, and 10.0mL of arsenic standard solution, respectively, into the conical flask in the arsenic generator, add 10mL of sulfuric acid solution, and add water to about 40mL. Add 2mL of potassium iodide solution and 1mL of stannous chloride solution, shake well, and let stand for 15min. After installing all parts of the device, take 5mL of silver diethyldithiocarbamate-triethylamine-trifluoromethane absorption liquid and add it to the absorption tube, add 3g of arsenic-free zinc particles to the conical flask, and quickly install the absorption tube. React at room temperature for 45min, remove the absorption tube, add the absorption liquid to 5ml., and mix. Use 1cm colorimetric blood and reagent blank as reference to measure the absorbance at a wavelength of 522nm. Draw a working curve with arsenic content as the horizontal axis and absorbance as the vertical axis.
5.3.5 Determination
Weigh about 2g of sample (accurate to 0.01g), place it in a 100mL beaker, add 10mL of sulfuric acid solution, and heat to completely dissolve the sample. After cooling, transfer to the conical flask in the asphaltene generator. For example, add 5 mL of tartaric acid solution to about 40 mL of water. Then follow the steps of drawing the working curve, starting from "… Add 2 mL of potassium iodide solution, add 1 mL of stannous nitride solution, shake well…" to "… Measure the absorbance". Find the corresponding asphaltene content from the asphaltene curve. 5.3.6 Expression of analysis results
The asphaltene (As) content (X.) expressed as mass percentage is calculated according to formula (4): mX10-
In the formula: ml—-the asphaltene content found from the working curve, mg; m…the mass of the sample. g.
5.3.7 Tolerance
HG 2935-2000
Take the arithmetic mean of the parallel determination results as the determination result. The absolute difference between the results of parallel determinations shall not exceed 0.00005%. 5.4 Determination of lead content
5.4.1 Atomic absorption spectrometry (arbitration method) 5.4.1.1 Summary of the method
Dissolve the sample with acid and determine with air-acetylene flame at 283.3nm. 5.4.1.2 Reagents and materials
a) Hydrochloric acid solution: 1+1.
b) Lead standard solution: 1ml solution contains 0.01mg lead. Preparation: Use a pipette to transfer 10ml of the lead standard solution prepared according to GB/T602, place it in a 100ml volumetric flask, dilute with water to the scale, and shake it. wwW.bzxz.Net
5.4.1.3 Instruments and equipment
Atomic absorption spectrophotometer: equipped with a lead hollow cathode lamp. 5.4.1.4 Analysis steps
5.4.1.4.1 Drawing of working curve
Take 5 100ml volumetric flasks, take 0.00, 1.00ml, 2.00ml, 3.00ml, 5.00ml of lead standard working solution respectively, dilute to scale with water, and shake well.
On an atomic absorption spectrophotometer, use air-acetylene flame, adjust to zero with distilled water at a wavelength of 283.3nm, and measure the absorbance of the above solution.
Draw the working curve with the mass of lead added to the standard solution as the horizontal axis and the corresponding absorbance as the vertical axis. 5.4.1.4.2 Determination
Weigh about 0.3g of sample (accurate to 0.01g), place in a 100mL beaker, moisten with a small amount of water, add 5mL of hydrochloric acid solution, place on an electric stove to heat until the sample is completely dissolved, transfer to a 50mL volumetric flask after cooling, dilute with water to the scale, shake well (if there is sediment, dry filter before introducing into the atomic absorption spectrophotometer). Perform a blank test at the same time.
Measure the absorbance on the atomic absorption spectrophotometer under the same conditions as the working curve, and find the corresponding lead mass on the working curve. 5.4.1.5 Expression of analysis results
The lead (Pb) content (Xs) expressed as mass percentage is calculated according to formula (5): Xs (%) =
Wherein: m,--
(mlmo)X10-
The mass of lead in the sample found on the working curve, mg; m.--——The mass of lead in the blank test found on the working curve, mg; m—.-The mass of the sample, g.
5.4.1.6 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%. 5.4.2 Extraction colorimetric method
(5)
5.4.2.1 Summary of the method
After the sample is treated, the interfering substances in the sample are extracted with ether. Sulfide is added to the aqueous phase to form a brown precipitate with the lead in the sample. Compare it with the standard reference solution to determine whether the lead content is within the limit. 5.4.2.2 Reagents and solutions
a) Ether.
b) Hydroxylamine hydrochloride.
c) Ammonia water.
d) Aqua regia: 70mL hydrochloric acid + 30ml nitric acid. e) Hydrochloric acid solution: 1+1.
f) Acetic acid solution: 1+19.
HG 2935 --- 2000
g) Sodium sulfate-glycerol solution.
Preparation: Weigh 5g sodium sulfide, place in a 100ml beaker, add 30ml of endotriol and 10ml of water, dissolve and transfer to a brown bottle, keep in a sealed container away from light, valid for three months. h) Lead standard solution: 1ml of solution contains 0.010mg of lead Preparation: Use a pipette to transfer 10mL of the lead standard solution prepared according to GB/T602, place in a 100ml volumetric flask, dilute with water to the mark, and shake well.
i) Phenolphthalein indicator solution: 10g/L
5.4.2.3 Analysis steps
Weigh (0.50±0.01)g of sample, place in a porcelain evaporating dish, add 3ml of aqua regia, and evaporate to dryness on a water bath. Dissolve the residue with 5ml hydrochloric acid solution and transfer to a 150ml separatory funnel. Wash the porcelain evaporator III twice with 5ml hydrochloric acid solution each time, and combine the washings into the separatory funnel; extract twice with 40ml ether each time, then add 20ml. ether and shake for 1min. After standing and stratifying, transfer the water layer to a 50ml colorimetric tube, add 0.05g hydroxylamine hydrochloride and dissolve. After heating on a water bath for 10min, add 1 drop of phenolic acid indicator solution and drip with ammonia water until the solution turns red. After cooling, drip hydrochloric acid solution until the solution is almost colorless, add 2ml acetic acid solution, dilute with water to about 50ml, add 2 drops of sodium sulfide-glycerol solution, dilute with water to the scale, and shake. Let stand for 5min and compare with the standard colorimetric solution. The color should not be darker than the standard comparison solution.
The standard colorimetric solution is 1.0mL (ferrous sulfate monohydrate) and 2.0mL (ferrous sulfate heptahydrate) of lead standard solution are pipetted and treated in the same way as the sample.
5.5 Determination of particle size
5.5.1 Method summary
The sample is sieved through the test sieve, and the product particle size is determined based on the mass of the sample passing through the test sieve. 5.5.2 Instruments and equipment
Test sieve: R40/3 series. $200mmX50mm/180μm or 200mmX50mm/800μm. 5.5.3 Analysis steps
Weigh about 100g of sample (accurate to 0.01g), place it on the test sieve (ferrous sulfate monohydrate uses a 180μm test sieve, ferrous sulfate heptahydrate uses an 800μm test sieve), and install the test sieve chassis. Shake horizontally at a speed of 2 times/s until no sample passes through the test sieve, move the sample that passes through the test sieve to a dry surface blood of known mass, and weigh it. 5.5.4 Expression of analysis results
Fineness expressed as mass percentage (X.) is calculated according to formula (6): X(%) = mi-mo
Wherein: m1--——-mass of the sample and surface blood passing through the test sieve, g; ma\--mass of surface III.g;
m--—·mass of the sample, g.
5.5.5 Allowable difference
The arithmetic mean of the results of two parallel determinations is taken as the determination result. The absolute difference of the parallel determination results shall not exceed 0.5%. 6 Inspection rules
6.1 All items specified in this standard are factory inspection items. (6)
6.2 Each batch of products shall not exceed 20t.
6.3 Determine the number of sampling units according to the provisions of 6.6 in GB/T6678.--1986. When sampling, insert the sampler obliquely from the mouth of the packaging container to three-quarters of the depth of the material layer 163
HG 2935 -2000
to collect samples. Mix the collected samples, reduce them to no less than 500g according to the quartering method, and pack them into two clean and dry bottles and seal them. Stick labels on the bottles and indicate: manufacturer name, product name, batch number, sampling date and name of the sampler. "One bottle shall be used for inspection, and the other bottle shall be kept for three months for future reference. 6.4 Feed grade ferrous sulfate shall be inspected by the quality inspection department of the manufacturer in accordance with the provisions of this standard. The manufacturer shall ensure that all feed grade ferrous sulfate shipped from the factory meets the requirements of this standard. 6.5 The user has the right to inspect and accept the received feed grade ferrous sulfate products in accordance with the provisions of this standard. The inspection time shall be within one month after the arrival of the goods.
6.6 If one of the indicators in the inspection results does not meet the requirements of this standard, re-samples shall be taken from the packaging of twice the amount for re-inspection. If even one of the indicators in the re-inspection results does not meet the requirements of this standard, the entire batch of products shall be unqualified. 7 Marks and labels
7.1 The packaging of feed grade ferrous sulfate shall be firmly and clearly marked, including: manufacturer name, address, product name, trademark, net content, "feed grade", batch number or production date, product quality certification that meets this standard and this standard number. 7.2 Each batch of feed grade ferrous sulfate shipped from the factory shall be accompanied by a printed firm and clear label, and the label content shall comply with GB 10648 Requirements 8 Packaging, transportation, storage
8.1 Feed grade ferrous sulfate is double packed. The inner packing is a polyethylene film bag; the outer packing is a polypropylene plastic woven bag. The net content of each bag is 25kg or 50kg. If the user has special requirements for packaging, it can be negotiated by the supply and demand parties. 8.2 For the packaging of feed grade ferrous sulfate, the film bag is tied with vinyl rope or rope of equivalent quality, or sealed with other equivalent methods; the outer bag is not less than 100 kg from the edge of the bag. Fold the edge at 30mm, and sew the bag 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 stitch length should be uniform. No leaking or skipping. 8.3 During transportation, feed grade ferrous sulfate should be covered to prevent sun exposure, rain, and moisture. It should not be mixed with toxic and hazardous substances. Prevent pollution
8.4 Feed grade ferrous sulfate should be stored in a cool, dry place to prevent rain, moisture, and sun exposure. It should not be mixed with toxic and hazardous substances. Prevent pollution.
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