GB 7300.103-2020 PDF in English
GB 7300.103-2020 (GB7300.103-2020) PDF English
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Feed additives -- Part 1: Amino acids, their salts and analogues--Methionine hydroxy analogue
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Standards related to (historical): GB 7300.103-2020
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GB 7300.103-2020: PDF in English GB 7300.103-2020
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 65.120
B 46
Replacing GB/T 19371.1-2003
Feed additives - Part 1: Amino acids, their salts and
analogues - Methionine hydroxy analogue
ISSUED ON: MAY 29, 2020
IMPLEMENTED ON: DECEMBER 1, 2020
Issued by: State Administration for Market Regulation;
Standardization Administration of PRC.
Table of Contents
Foreword ... 3
1 Scope ... 5
2 Normative references ... 5
3 Requirements ... 6
4 Test method ... 6
5 Inspection rules ... 13
6 Labeling, packaging, transportation, and storage ... 14
7 Shelf life ... 15
Feed additives - Part 1: Amino acids, their salts and
analogues - Methionine hydroxy analogue
1 Scope
This part of GB 7300 specifies the requirements, test methods, inspection rules and
labeling, packaging, transportation, storage, and shelf life requirements for feed
additives methionine hydroxy analogues.
This part applies to feed additives methionine hydroxy analogues produced by chemical
synthesis with acrolein, methyl mercaptan, and hydrogen cyanide used as the main raw
materials.
Chemical name: 2-Hydroxy-4-(methylthio)butyric acid
Molecular formula: C5H10O3S
Relative molecular mass: 150.2 (in C5H10O3S, calculated according to the 2016
International Standard Relative Atomic Mass)
2 Normative references
The following documents are essential to the application of this document. For the dated
referenced documents, only the versions with the indicated dates are applicable to this
document; for the undated referenced documents, only the latest version (including all
the amendments) is applicable to this document.
GB/T 601 Chemical reagent - Preparations of reference titration solutions
GB/T 602 Chemical reagent - Preparations of standard solutions for impurity
GB/T 603 Chemical reagent - Preparations of reagent solutions for use in test
methods
GB/T 6680 General rules for sampling liquid chemical products
GB/T 6682 Water for analytical laboratory use - Specification and test methods
GB 10648 Feed label
GB/T 13079-2006 Determination of total arsenic in feeds
4.2.1.3 2,7-Dihydroxynaphthalene.
4.2.1.4 Anhydrous copper sulfate saturated sulfuric acid solution: Take anhydrous
copper sulfate (4.2.1.1), add sulfuric acid (4.2.1.2) and stir until it is insoluble.
4.2.1.5 2,7-dihydroxynaphthalene sulfuric acid solution: 0.01%; weigh 0.01 g of 2,7-
dihydroxynaphthalene (4.2.1.3), dissolve it with sulfuric acid (4.2.1.2) and make up the
volume to 100 mL, and newly prepare it when it will be used.
4.2.2 Identification test
4.2.2.1 Take 25 mg of this product and put it into a dry test tube, add 1 mL of anhydrous
copper sulfate saturated sulfuric acid solution (4.2.1.4), the solution immediately turns
yellow, and then turns yellow-green.
4.2.2.2 Take 1 drop of this product and put it into a dry test tube, add the newly prepared
2,7-dihydroxynaphthalene sulfuric acid solution (4.2.1.5), put the tube in a boiling
water bath and boil for 10 min~15 min, and then the color turns from yellow to reddish
brown.
4.3 Determination of content of methionine hydroxy analogues
4.3.1 Principle
In an acidic medium, methionine hydroxy analogues undergo the following redox
reactions:
3C4H6O3SCH3+BrOଷି→ 3C4H6O3SOCH3+Brି
The color change of bromine can be used to judge the end point of the reaction.
4.3.2 Reagents
4.3.2.1 Potassium bromate.
4.3.2.2 Potassium bromide.
4.3.2.3 Potassium iodide.
4.3.2.4 Hydrochloric acid.
4.3.2.5 Hydrochloric acid solution: hydrochloric acid + water = 1 + 1.
4.3.2.6 Acid solution: glacial acetic acid + water + concentrated hydrochloric acid = 50
+ 10 + 3.
4.3.2.7 Sodium thiosulfate standard titration solution: c(Na2S2O3) = 0.1 mol/L
(according to the provision of GB/T 601).
4.5.1.2 Nitric acid.
4.5.1.3 Hydrochloric acid.
4.5.1.4 Lead standard solution: 1000 μg/mL; weigh 0.1599 g of lead nitrate, put it in a
1000 mL measuring bottle, add 5 mL of nitric acid and 50 mL of water to dissolve;
dilute with water to the mark, shake well, and use it as a stock solution (according to
the provisions of GB/T 602); or use a commercially available lead single-element
standard solution of 1000 μg/mL.
4.5.1.5 Ammonia solution (10%): Take 40 mL of ammonia water, add an appropriate
amount of water to make up to 100 mL, and shake well (prepared according to GB/T
603).
4.5.1.6 Hydrochloric acid solution Ⅰ: Take 63 mL of hydrochloric acid, add an
appropriate amount of water to make up to 100 mL, and shake well.
4.5.1.7 Hydrochloric acid solution II: Take 18 mL of hydrochloric acid, add water to
make up to 100 mL, and shake well.
4.5.1.8 Sodium sulfide solution: Take 100 g of sodium sulfide and add water to dissolve
it into 1000 mL.
4.5.1.9 Acetate buffer solution (pH 3.5): Take 25 g of ammonium acetate, add 25 mL
of water to dissolve, add 38 mL of hydrochloric acid solution Ⅰ (4.5.1.6), and use
hydrochloric acid solution Ⅱ (4.5.1.7) or ammonia solution (4.5.1.5 ) to accurately
adjust the pH value to 3.5 (indicated by the potentiometer); dilute to 100 mL with water,
and shake well.
4.5.1.10 Phenolphthalein indicator solution: Take 1 g of phenolphthalein, add 100 mL
of ethanol to dissolve it, and then the solution is obtained (prepared according to GB/T
603). The range of discoloration is pH 8.3~10.0 (colorless→red).
4.5.1.11 Preparation of lead standard working solution: Accurately measure 2 mL of
lead standard solution (4.5.1.4), put it in a 200 mL measuring bottle, dilute with water
to the mark, and shake well (each mL solution is equivalent to 10 μg of Pb).
4.5.2 Analysis steps
4.5.2.1 Sample solution preparation
Weigh 1 g of the sample (accurate to 10 mg), place it in a porcelain crucible, blaze
slowly until it is completely carbonized, and let it cool. Add 0.5 mL~1 mL of sulfuric
acid (4.5.1.1) to make it moist, heat at low temperature until the sulfuric acid vapor is
completely removed, burn it at 550 ℃ to make it completely ash, and let it cool. Add
0.5 mL of nitric acid (4.5.1.2), evaporate to dryness until the nitrogen oxide vapor is
completely removed, and let it cool. Add 2.0 mL of hydrochloric acid (4.5.1.3),
evaporate to dryness on a water bath, and add 15 mL of water; add dropwise ammonia
solution (4.5.1.5) until it reacts to phenolphthalein indicator solution (4.5.1.10) and the
solution turns slightly red, and then add 2.0 mL of acetate buffer (4.5.1.9); after slightly
heating to dissolve, transfer the solution to a Nessler colorimetric tube, add water to
dilute it to 25 mL, which is used as tube B.
4.5.2.2 Preparation of standard colorimetric solution
Take another reagent for preparing the sample solution, evaporate it to dryness in a
porcelain crucible, add 2.0 mL of acetate buffer solution (4.5.1.9) and 15 mL of water;
after slightly heating to dissolve, transfer the solution to a Nessler colorimetric tube,
add 1.00 mL of lead standard working solution (4.5.1.11), and then dilute it with water
to 25 mL, which is used as tube A.
4.5.3 Measurement and result judgment
Add 5 drops of sodium sulfide solution (4.5.1.8) to tubes A and B respectively, shake
well, and let them stand for 2 minutes; place them on white paper, see through from top
to bottom, and compare the colors of tubes A and B with naked eyes. If the color in tube
B is not darker than that in tube A, it is judged that the requirements are met.
4.6 Determination of ammonium salt
4.6.1 Reagents
4.6.1.1 Magnesium oxide.
4.6.1.2 Hydrochloric acid solution: hydrochloric acid + water = 1 + 3 (volume ratio).
4.6.1.3 Sodium hydroxide solution: 10%.
4.6.1.4 Saturated aqueous solution of mercuric chloride: Add mercuric chloride into
water and stir until it is insoluble.
4.6.1.5 Nessler reagent: Dissolve 10 g of potassium iodide in 10 mL of water, and add
mercuric chloride saturated aqueous solution (4.6.1.4) while stirring, until the formed
red precipitate is no longer dissolved; add potassium hydroxide and dissolve it, then
add 1 mL of mercuric chloride saturated aqueous solution, and add water to 200 mL;
let it stand, and then take the supernatant out and store it in a brown bottle.
4.6.1.6 Ammonium standard solution: 0.01 mg/mL (according to the provisions of
GB/T 602).
4.6.2 Analysis steps
Accurately weigh 0.20 g of the sample, put it in a distillation bottle, add 70 mL of water,
then add 1 g of magnesium oxide (4.6.1.1), and carry out distillation; use 5 mL of
hydrochloric acid solution (4.6.1.2) as the absorption liquid, put the lower end of the
condenser tube to be immersed in the absorption liquid, collect about 70 mL of the
distillate, and stop the distillation; dilute the distillate to 100 mL with water, and
accurately measure 1 mL of the distillate into a Nessler colorimetric tube; add 2 mL of
sodium hydroxide solution (4.6.1.3), 20 mL of water, 1 mL of Nessler reagent (4.6.1.5),
diluted with water to 50 mL, and shake well.
Accurately pipette 3 mL of ammonium standard solution (4.6.1.6) into another Nessler
colorimetric tube, and at the same time, carry out the colour reaction with the same
steps as the sample test; the color of the sample solution shall not be darker than the
standard solution.
4.7 Determination of cyanide
4.7.1 Reagents or materials
4.7.1.1 Tartaric acid solution: Dissolve 10 g of tartaric acid in water, and dilute to 100
mL.
4.7.1.2 Ferrous sulfate solution: Take 8 g of ferrous sulfate (FeSO4 • 7H2O), and add
100 mL of freshly boiled cold water.
4.7.1.3 Sodium hydroxide solution: Take 4.3 g of sodium hydroxide, dissolve it in water,
and dilute the solution to 100 mL.
4.7.1.4 Ferric chloride solution: Take 9 g of ferric chloride, dissolve it in water, and
dilute the solution to 100 mL.
4.7.1.5 Alkaline ferrous sulfate test paper: Before use, take a piece of filter paper and
add 1 drop of ferrous sulfate test solution (4.7.1.2) and 1 drop of sodium hydroxide test
solution (4.7.1.3).
4.7.1.6 Hydrochloric acid.
4.7.2 Instruments and apparatus
The instruments and apparatus are shown in Figure 1.
4.7.3 Analysis steps
Weigh 1 g of the sample (accurate to 0.0001 g), add 10 mL of water and 3 mL of tartaric
acid solution (4.7.1.1), quickly and closely plug a gas-guide tube containing alkaline
ferrous sulfate test paper (4.7.1.5) into the conical flask; shake well, heat on a low heat,
and boil slightly for 1 min. Take off the alkaline ferrous sulfate test paper, and add 1
drop of ferric chloride solution (4.7.1.4) and 1 drop of hydrochloric acid (4.7.1.6); the
When one of the following situations occurs, type inspection shall be carried out, and
the inspection items include all technical indexes specified in Chapter 3:
a) When the product is finalized, and when there are major changes in raw
materials, production processes, and equipment;
b) During normal production, once every six months;
c) When the production is resumed after the suspension of production for more
than 3 months;
d) When the industry administrative department requests a type inspection;
e) When the factory inspection results are significantly different from the last type
inspection results.
5.5 Judgment rules
If one of the indexes of the inspection results does not meet the requirements of this
part, samples shall be taken from a doubled number of packaging units for re-inspection.
If one of the indexes of the re-inspection results still does not meet the requirements of
this part, the batch of products is judged as unqualified.
6 Labeling, packaging, transportation, and storage
6.1 Labeling
Labeling shall be implemented according to GB 10648. The corrosion warning labels
shall be indicated in a prominent position.
6.2 Packaging
This product shall be packaged in acid-resistant plastic barrels or other acid-resistant
containers and sealed.
6.3 Transportation
Collision shall be strictly prohibited during the transportation of this product to prevent
damage to the packaging, and transportation mixed with toxic and harmful substances
is strictly prohibited.
6.4 Storage
This product shall be stored in a clean place, protected from sunlight, rain, and moisture,
and it is strictly forbidden to store it with toxic and harmful items.
......
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
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