Some standard content:
National Standard of the People's Republic of China
Feed grade L-lysine monohydrochlorideUDC 636.085.57
GB 82 45 -- 87
This standard applies to L-lysine hydrochloride obtained by fermentation and extraction with starch and sugar as raw materials. It is an essential amino acid for animals and is added to feed as an amino acid supplement. Molecular formula C, H, N, O, · HCI
Structural formula:
{NH,-CH,—CH,CH,—-CH,-
Molecular weight: 182.65 (according to the international atomic weight in 1983) 1 Technical requirements
1.1 Physical and chemical properties
CH--COOHI - HC1
This product is white or light brown powder. Tasteless or with a slight special smell. Soluble in water, insoluble in ethanol and ether. Optically active. The pH value of the aqueous solution (1+10) of this product is 5.0~6.0. 1.2 Feed grade L-lysine hydrochloride should meet the requirements of Table 1. Table
Indicators:
Content (based on C, N, O, · HCI dry basis)
Specific optical rotation [
Loss on drying
Ignition residue
Ammonium salt (based on NH)www.bzxz.net
Heavy metal (based on Pb)
Monument (based on As)
2Test method
+18. 0°~+21. 5°
The reagents and water used in the test, unless otherwise specified, are analytically pure reagents and distilled water, or water of corresponding purity. %
Unless other requirements are specified, the standard solution used shall be in accordance with GB601-77 "Method for Preparation of Standard Solutions"; the impurity standard solution shall be in accordance with GB602--77 "Method for Preparation of Impurity Standard Solutions"; the preparations and products shall be prepared in accordance with GB603--77 "Method for Preparation of Preparations and Products". 2.1 Identification
2.1.1 Reagents and solutions
Approved by the Ministry of Agriculture, Animal Husbandry and Fisheries of the People's Republic of China on September 14, 1987, 218
Implementation on October 1, 1988
GB 82 45-87
2.1.1.1 Benzoic acid (HG 3-984-76): 0.1% (m/V) solution; 2.1.1.2 Silver nitrate (GB670-77): 0.1mol/1 solution; 2.1.1.3 Nitric acid (GB 626-:78): 1+9 solution; 2.1.1.4 Ammonium hydroxide (GB631-77): 1+2 solution. 2.1.2 Identification method
2.1.2.1 Identification of amino acids
Weigh 0.1g of the sample and dissolve it in 100ml of water. Take 5ml of this solution and add 1ml of triketone solution (2.1.1.1). After heating for 3min, add 20ml of water and keep it in a jar for 15min. The solution will turn reddish purple. 2.1.2.2 Identification of chlorides
Weigh 1g of the sample and dissolve it in 10ml of water. Add silver nitrate solution (2.1.1.2) to produce a white precipitate. Take this precipitate and add dilute nitric acid (2.1.1.3). The precipitate does not dissolve. Take another precipitate and add excess ammonium hydroxide solution (2.1.1.4) to dissolve it. 2.2 Determination of lysine hydrochloride content
2.2.1 Reagents and solutions
2.2.1. 1 Formic acid (HG 3-1296 80); 2. 2. 1. 2 Glacial acetic acid (GB 676-78); 2.2.1.3 Mercuric acetate (HG 3-1096-77): 6% (m/V) glacial acetic acid solution; 2.2.1.4 α-phenolphenylmethanol indicator: 0.2% (m/V) glacial acetic acid indicator solution; 2.2.1,5 Perfluoric acid (GB 623-77): glacial acetic acid standard solution with a concentration (HC1O.) of approximately 0.1 mol/1. 2.2.2 Determination method
The sample is dried at 105℃ to constant weight in advance. Weigh 0.2g of the dried sample to 0.0002g, add 3ml of formic acid (2.2.1.1) and 50ml of glacial acetic acid (2.2.1.2), and then add 5ml of glacial acetic acid solution of mercuric acetate (2.2.1.3). Add 10 drops of α-naphthol phenyl methanol indicator solution (2.2.1.4), and titrate with 0.1mol/1 perchloric acid glacial acetic acid standard solution (2.2.1.5). The titration end point is when the sample solution changes from orange-yellow to yellow-green. Perform another blank test in the same way for correction. 2.2.3 Calculation of results
The percentage of L-lysine hydrochloride (CH, N, O, · HCl) is calculated according to formula (1): 0. 09132 XC. (V-Vo) × 100 Where: °C-
-Concentration of perfluoric acid standard solution, mol/l; V-Volume of perfluoric acid standard solution consumed by the sample, ml;. -Volume of perchloric acid standard solution consumed by the blank test, ml; Mass of the sample, denominator:
0.09132-Number of grams of lysine hydrochloride per millimole. The difference between the results of two parallel samples shall not exceed 0.2%, and the results shall be reported as their arithmetic mean. 2.3 Determination of specific rotation
2.3.1 Instruments and equipment
Polarimeter: Use a sodium lamp (sodium spectrum D line 589.3nm) as the light source. 2.3.2 Reagents and solutions
Hydrochloric acid (GB622-77): 1+1 solution.
2.3.3 Determination method
Dry the sample at 105°C to constant weight, weigh about 4g of the dry sample, and weigh to 0.0002g. Dissolve it with hydrochloric acid solution (2.3.2) [If the sample solution is dark, add a small amount of water after weighing the sample, add 0.5g of activated carbon after dissolution, boil, cool and filter, and wash with hydrochloric acid solution (2.3.2) several times], and transfer all into a 50ml volumetric flask. Adjust the solution temperature to 20°C and dilute to the scale with hydrochloric acid solution (2.3.2). Determine the optical rotation with a polarimeter (2.3.1).
2.3.4 Calculation of specific rotation
GB 8245-87
The specific rotation aJ of L-lysine hydrochloride to the sodium spectrum D line at 20°C is calculated according to formula (2): 100m
wherein the measured rotation;
-length of the polarimetric tube, dm;
mass of sample contained in each 100ml hydrochloric acid solution, g. 2.4 Determination of loss on drying
2.4.1 Instruments and equipment
2.4.1.1 Electric drying oven: the temperature can be controlled at 105±2°C; 2.4.1.2 Sample weighing III: Φ45mm, aluminum or glass can be used; 2.4.1.3 Dryer: calcium fluoride or silica gel is used as desiccant. 2.4.2 Determination method
-(2)
Use a dried weighing dish to weigh 1g of the sample, accurate to 0.00028, and place it in an electric drying oven at 105±2℃, open the lid of the weighing dish, and dry it for 3h. Take it out and cover it, put it in a desiccator, cool it to room temperature, and weigh it. Repeat the drying for 1h and weigh it to constant weight. 2.4.3 Calculation of results
The percentage of the drying loss of L-lysine hydrochloride is calculated according to formula (3): m = m × 100
Where:
The mass of the sample before drying, g;
The mass of the sample after drying, g.
2.5 Determination of ignition residue
2.5.1 Instruments and equipment
2.5.1.1 High temperature furnace: controllable temperature is 550±20℃; 2.5.1.2 Porcelain crucible: 30ml;
2.5.1.3 Desiccator: use calcium fluoride or silica gel as desiccant. (3)
2.5.2 Determination method
In the porcelain crucible that has been ignited to a certain weight, weigh 1g of the sample to the nearest 0.0002g. Carefully carbonize it on an electric furnace until there is no black smoke, then transfer it to a high temperature furnace and ignite it at 550℃ for 3-4h. Take it out and let it cool slightly before putting it in a desiccator. Cool it to room temperature and weigh it. Repeat the ignition for 1h and weigh it until it is heavy.
2.5.3 Calculation of results
The percentage of the residue after ignition of L-lysine hydrochloride is calculated according to formula (4): m=m×100
Wherein: m —
mass of a sample, 8;
mass of an empty crucible at constant weight, 8;
-ash content and crucible mass, 8.
2.6 Determination of ammonium salts
2.6.1 Reagents and solutions
2.6.1.1 Magnesium oxide (HG 3—1294—80); 2.6.1.2 Hydrochloric acid (CB622-77): 1+3 solution; 2201
GB 8245-87
2.6.1.3 Sodium hydroxide (GB629~-81): 10% (m/V) solution; 2.6.1.4 Potassium iodide (GB 1272-~77);
2.6.1.5 Mercuric chloride (HG3--1068-77): saturated aqueous solution; 2.6.1.6 Potassium hydroxide (HGB3006-—59); 2.6.1.7 Nessler's reagent: Dissolve 10g potassium iodide in 10ml water, slowly add saturated aqueous solution of mercuric chloride while stirring until the red precipitate is no longer soluble. Add 30g potassium hydroxide and dissolve it, then add 1ml saturated solution of mercuric chloride, and add water to 200ml. Let it stand, take the upper clear liquid and store it in a brown bottle. 2.6.1.8 Ammonium standard solution: 1ml contains 0.01mgNH+. Prepare according to the provisions of GB602-77, and accurately dilute 10 times when used.
2.6.2 Determination method
Weigh 2.5g of the sample, weigh to 0.01g, place in a distillation flask, add 70ml of water, add 1g of magnesium oxide (2.6.1.1), and distill. Use 5ml of hydrochloric acid (2.6.1.2) as the absorption liquid, the lower end of the condenser should be immersed in this liquid, collect the distillate to about 40ml, and stop distillation. Dilute the distillate accurately with water to 50ml. Transfer 2ml of the distillate, place in a Nessler colorimetric tube, add 2ml of sodium hydroxide (2.6.1.3), 20ml of water, and then add 1ml of Nessler's reagent (2.6.1.7), dilute with water to 50ml, and shake. Transfer 4ml of ammonium standard solution (2.6.1.8) to another Nessler colorimetric tube, and color it at the same time as the sample. The color of the sample solution must not be darker than this standard solution.
2.7 Determination of heavy metals
2.7.1 Reagents and solutions
2.7.1.1 Hydrochloric acid (GB622-77): 1+3 solution; 2.7.1.2 Glacial acetic acid (GB 676-78): 6% (V/V) solution; 2.7.1.3 Sodium sulfide (HG3-90576): 1g sodium sulfide is dissolved in 10ml water, freshly prepared before use. 2.7.1.4 Lead standard solution: 1ml contains 0.01mgPb. Prepare according to the provisions of GB602-77, and then accurately dilute 10 times. 2.7.2 Determination method
Weigh 1g of sample, accurate to 0.01g, place in porcelain, carefully carbonize on an electric furnace, and then burn at 550℃ for 3h (or use the residual ash after the burning residue is determined in 2.5), add 4ml of hydrochloric acid (2.7.1.1) to the residue, heat on a water bath and evaporate to dryness. Add 10ml of hot water and soak for 2min, transfer all into a Nessler colorimetric tube, add 2ml of acetic acid solution (2.7.1.2), dilute with water to 50ml, add 2 drops of sodium sulfide solution (2.7.1.3), and let stand for 5min.
Pipette 3ml of lead standard solution (2.7.1.4) and the sample at the same time to develop the same color as the standard. The color of the sample solution shall not be darker than this standard solution. 2.8 Determination of arsenic
2.8.1 Reagents and solutions
2.8.1.1 Hydrochloric acid (GB622--77): 1+1 solution; 2.8.1.2 Potassium iodide (GB1272--77): 16.5% (m/V) solution; 2.8.1.3 Stannous chloride (GB638-78): 40% (m/V) hydrochloric acid solution, valid for one month; 2.8.1.4 Arsenic-free metallic zinc (GB2304-80); 2.8.1.5 Lead acetate absorbent cotton;
2.8.1.6 Mercuric bromide test paper;
2.8.1.7 Arsenic standard solution: 1 ml contains 0.001 mg As. Prepare according to the provisions of GB602-77, and dilute accurately 100 times before use. 2.8.2 Determination method
Weigh 1g of the sample, weigh to 0.018, place it in a wide-mouth bottle, and determine it according to the provisions of "1 Arsenic Spot Method" in GB610-77 "Arsenic Determination Method". Its color shall not be darker than the standard.
Pipette 2ml of arsenic standard solution (2.8.1.7) and treat it in the same way as the sample at the same time as the standard. 221
3 Acceptance rules
GB 8245-87
3.1 This product shall be inspected by the technical inspection department of the manufacturer, and the manufacturer shall ensure that all products leaving the factory meet the requirements of this standard. Each batch of products leaving the factory shall be accompanied by a quality certificate and instructions for use. 3.2 The user unit may conduct acceptance in accordance with the provisions of this standard. If the supply and demand parties have objections to the product quality, the national authorized product quality inspection agency may conduct arbitration inspection.
3.3 The weight of each batch of this product shall not exceed 20t. 3.4 Sampling method:
3.4.1 Select the number of sample bags from each batch of products as specified in Table 2. Table 2
Total number of bags per batch
Number of sampled bags
Total number of bags
√Total number of bags
3.4.2 Use a sampler to vertically insert 3/4 of the material layer from the center of the bag mouth to take samples. Each bag should be sampled no less than 100g. 3.4.3 Mix the sample quickly, reduce it to 500g by quartering method, and pack it into two clean, dry bottles with ground stoppers. Label the bottles with: manufacturer name, product name, batch number and sampling date. One bottle is used for inspection, and the other bottle is kept for 6 months for arbitration inspection.
3.5 If one of the indicators does not meet the standard during the inspection, a sample should be selected from the twice-sized packaging for re-verification. In this verification result, even if only one indicator does not meet the standard, the entire batch cannot be accepted. 4 Packaging, marking, storage and transportation
4.1 The inner packaging of feed-grade L-lysine hydrochloride should meet the food hygiene requirements, and the outer packaging should be moisture-proof and not easy to break. The net weight of each bag should not exceed 25kg.
4.2 The packaging should be firmly marked with the product name, manufacturer name, factory address, batch number, approval number, storage conditions, usage, net weight, factory date, and the words "feed grade". 4.3 The ex-factory products should be accompanied by a quality certificate, which includes the product name, manufacturer name, factory address, batch number, approval number, product quality, this standard number and the laboratory technician code.
4.4 This product should be stored in a cool, dry and ventilated place. 4.5 During transportation, it should be strictly protected from rain and sunlight, and should not be stored or transported together with toxic and hazardous substances. Additional remarks:
This standard was proposed by the Ministry of Agriculture, Animal Husbandry and Fisheries of the People's Republic of China. This standard was drafted by the China Veterinary Drug Supervision Institute and Guangxi Lysine Factory. The main drafters of this standard are Zhong Feng, Huang Huiqiang and Li Meitong. This standard is equivalent to the Japanese Feed Safety Law. 2223) Leave it for 5 minutes.
Take 3 ml of lead standard solution (2.7.1.4) and use it as the standard solution to develop the same color as the sample solution. The color of the sample solution should not be darker than that of the standard solution. 2.8 Determination of arsenic
2.8.1 Reagents and solutions
2.8.1.1 Hydrochloric acid (GB622--77): 1+1 solution; 2.8.1.2 Potassium iodide (GB1272--77): 16.5% (m/V) solution; 2.8.1.3 Stannous chloride (GB638-78): 40% (m/V) hydrochloric acid solution, valid for one month; 2.8.1.4 Arsenic-free metallic zinc (GB2304-80); 2.8.1.5 Lead acetate absorbent cotton;
2.8.1.6 Mercuric bromide test paper;
2.8.1.7 Arsenic standard solution: 1 ml contains 0.001 mg As. Prepare according to the provisions of GB602-77, and dilute accurately 100 times before use. 2.8.2 Determination method
Weigh 1g of the sample, weigh to 0.018, place it in a wide-mouth bottle, and determine it according to the provisions of "1 Arsenic Spot Method" in GB610-77 "Arsenic Determination Method". Its color shall not be darker than the standard.
Pipette 2ml of arsenic standard solution (2.8.1.7) and treat it in the same way as the sample at the same time as the standard. 221
3 Acceptance rules
GB 8245-87
3.1 This product shall be inspected by the technical inspection department of the manufacturer, and the manufacturer shall ensure that all products leaving the factory meet the requirements of this standard. Each batch of products leaving the factory shall be accompanied by a quality certificate and instructions for use. 3.2 The user unit may conduct acceptance in accordance with the provisions of this standard. If the supply and demand parties have objections to the product quality, the national authorized product quality inspection agency may conduct arbitration inspection.
3.3 The weight of each batch of this product shall not exceed 20t. 3.4 Sampling method:
3.4.1 Select the number of sample bags from each batch of products as specified in Table 2. Table 2
Total number of bags per batch
Number of sampled bags
Total number of bags
√Total number of bags
3.4.2 Use a sampler to vertically insert 3/4 of the material layer from the center of the bag mouth to take samples. Each bag should be sampled no less than 100g. 3.4.3 Mix the sample quickly, reduce it to 500g by quartering method, and pack it into two clean, dry bottles with ground stoppers. Label the bottles with: manufacturer name, product name, batch number and sampling date. One bottle is used for inspection, and the other bottle is kept for 6 months for arbitration inspection.
3.5 If one of the indicators does not meet the standard during the inspection, a sample should be selected from the twice-sized packaging for re-verification. In this verification result, even if only one indicator does not meet the standard, the entire batch cannot be accepted. 4 Packaging, marking, storage and transportation
4.1 The inner packaging of feed-grade L-lysine hydrochloride should meet the food hygiene requirements, and the outer packaging should be moisture-proof and not easy to break. The net weight of each bag should not exceed 25kg.
4.2 The packaging should be firmly marked with the product name, manufacturer name, factory address, batch number, approval number, storage conditions, usage, net weight, factory date, and the words "feed grade". 4.3 The ex-factory products should be accompanied by a quality certificate, which includes the product name, manufacturer name, factory address, batch number, approval number, product quality, this standard number and the laboratory technician code.
4.4 This product should be stored in a cool, dry and ventilated place. 4.5 During transportation, it should be strictly protected from rain and sunlight, and should not be stored or transported together with toxic and hazardous substances. Additional remarks:
This standard was proposed by the Ministry of Agriculture, Animal Husbandry and Fisheries of the People's Republic of China. This standard was drafted by the China Veterinary Drug Supervision Institute and Guangxi Lysine Factory. The main drafters of this standard are Zhong Feng, Huang Huiqiang and Li Meitong. This standard is equivalent to the Japanese Feed Safety Law. 2223) Leave it for 5 minutes.
Take 3 ml of lead standard solution (2.7.1.4) and use it as the standard solution to develop the same color as the sample solution. The color of the sample solution should not be darker than that of the standard solution. 2.8 Determination of arsenic
2.8.1 Reagents and solutions
2.8.1.1 Hydrochloric acid (GB622--77): 1+1 solution; 2.8.1.2 Potassium iodide (GB1272--77): 16.5% (m/V) solution; 2.8.1.3 Stannous chloride (GB638-78): 40% (m/V) hydrochloric acid solution, valid for one month; 2.8.1.4 Arsenic-free metallic zinc (GB2304-80); 2.8.1.5 Lead acetate absorbent cotton;
2.8.1.6 Mercuric bromide test paper;
2.8.1.7 Arsenic standard solution: 1 ml contains 0.001 mg As. Prepare according to the provisions of GB602-77, and dilute accurately 100 times before use. 2.8.2 Determination method
Weigh 1g of the sample, weigh to 0.018, place it in a wide-mouth bottle, and determine it according to the provisions of "1 Arsenic Spot Method" in GB610-77 "Arsenic Determination Method". Its color shall not be darker than the standard.
Pipette 2ml of arsenic standard solution (2.8.1.7) and treat it in the same way as the sample at the same time as the standard. 221
3 Acceptance rules
GB 8245-87
3.1 This product shall be inspected by the technical inspection department of the manufacturer, and the manufacturer shall ensure that all products leaving the factory meet the requirements of this standard. Each batch of products leaving the factory shall be accompanied by a quality certificate and instructions for use. 3.2 The user unit may conduct acceptance in accordance with the provisions of this standard. If the supply and demand parties have objections to the product quality, the national authorized product quality inspection agency may conduct arbitration inspection.
3.3 The weight of each batch of this product shall not exceed 20t. 3.4 Sampling method:
3.4.1 Select the number of sample bags from each batch of products as specified in Table 2. Table 2
Total number of bags per batch
Number of sampled bags
Total number of bags
√Total number of bags
3.4.2 Use a sampler to vertically insert 3/4 of the material layer from the center of the bag mouth to take samples. Each bag should be sampled no less than 100g. 3.4.3 Mix the sample quickly, reduce it to 500g by quartering method, and pack it into two clean, dry bottles with ground stoppers. Label the bottles with: manufacturer name, product name, batch number and sampling date. One bottle is used for inspection, and the other bottle is kept for 6 months for arbitration inspection.
3.5 If one of the indicators does not meet the standard during the inspection, a sample should be selected from the twice-sized packaging for re-verification. In this verification result, even if only one indicator does not meet the standard, the entire batch cannot be accepted. 4 Packaging, marking, storage and transportation
4.1 The inner packaging of feed-grade L-lysine hydrochloride should meet the food hygiene requirements, and the outer packaging should be moisture-proof and not easy to break. The net weight of each bag should not exceed 25kg.
4.2 The packaging should be firmly marked with the product name, manufacturer name, factory address, batch number, approval number, storage conditions, usage, net weight, factory date, and the words "feed grade". 4.3 The ex-factory products should be accompanied by a quality certificate, which includes the product name, manufacturer name, factory address, batch number, approval number, product quality, this standard number and the laboratory technician code.
4.4 This product should be stored in a cool, dry and ventilated place. 4.5 During transportation, it should be strictly protected from rain and sunlight, and should not be stored or transported together with toxic and hazardous substances. Additional remarks:
This standard was proposed by the Ministry of Agriculture, Animal Husbandry and Fisheries of the People's Republic of China. This standard was drafted by the China Veterinary Drug Supervision Institute and Guangxi Lysine Factory. The main drafters of this standard are Zhong Feng, Huang Huiqiang and Li Meitong. This standard is equivalent to the Japanese Feed Safety Law. 222
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