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GB 21034-2017: Feed additive -- Calcium salt of hydroxyl analogue of methionine
Status: Valid GB 21034: Evolution and historical versions
| Standard ID | Contents [version] | USD | STEP2 | [PDF] delivered in | Standard Title (Description) | Status | PDF |
| GB 21034-2017 | English | 199 |
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Feed additive -- Calcium salt of hydroxyl analogue of methionine
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GB 21034-2017
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| GB/T 21034-2007 | English | 239 |
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Feed additive -- Methionine hydroxy calcium
| Obsolete |
GB/T 21034-2007
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PDF similar to GB 21034-2017
Basic data | Standard ID | GB 21034-2017 (GB21034-2017) | | Description (Translated English) | Feed additive -- Calcium salt of hydroxyl analogue of methionine | | Sector / Industry | National Standard | | Classification of Chinese Standard | B46 | | Classification of International Standard | 65.120 | | Word Count Estimation | 10,135 | | Date of Issue | 2017-10-14 | | Date of Implementation | 2018-05-01 | | Issuing agency(ies) | General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China, Standardization Administration of the People's Republic of China | GB 21034-2017: Feed additive -- Calcium salt of hydroxyl analogue of methionine---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
Feed additive - Calcium salt of hydroxyl analogue of methionine
ICS 65.120
B46
National Standards of People's Republic of China
Replacing GB/T 21034-2007
Feed additive methionine hydroxy analog calcium salt
2017-10-14 Published
2018-05-01 implementation
General Administration of Quality Supervision, Inspection and Quarantine of People's Republic of China
China National Standardization Administration released
Foreword
The first chapter of this standard, Chapter 3 and Chapter 5 is mandatory, the rest are recommended.
This standard was drafted in accordance with the rules given in GB/T 1.1-2009.
This standard replaces GB/T 21034-2007 "feed additive hydroxy methionine calcium."
This standard compared with GB/T 21034-2007, the main technical differences are as follows.
--- The standard name changed to "feed additive methionine hydroxy analog calcium salt";
--- The appearance and traits changed to "This product is white, light gray or taupe powder or granules, a unique stench";
--- Increased product methionine hydroxy analog identification method (high performance liquid chromatography);
--- Remove the technical indicators in the requirements of granularity;
--- Test rules to add a "type test."
This standard is proposed and managed by the National Feed Industry Standardization Technical Committee (SAC/TC76).
This standard drafting unit. China Agricultural University, China Feed Industry Association, Novartis (China) Investment Co., Ltd..
The main drafters of this standard. Shi Shi Yan, Sun Xiangli, had Xiangfang, Xie Chunyuan, Hou Chengli, Wu Yubo.
This standard replaces the standards previously issued as.
--- GB/T 21034-2007.
Feed additive methionine hydroxy analog calcium salt
1 Scope
This standard specifies the feed additive methionine hydroxy analog calcium salt requirements, test methods, inspection rules and labeling, packaging, transportation
Lose, storage and shelf life.
This standard applies to methionine hydroxy analogues and calcium hydroxide as the main raw material feed additive methionine hydroxy analogues
Calcium salt.
Chemical name .2-hydroxy-4-methylthiobutyric acid calcium salt; 2-hydroxy-4-methylthiobutyric acid calcium; hydroxy methionine calcium.
Molecular formula (CH3SCH2CH2CHOHCOO) 2Ca.
Relative molecular mass .338.44 (By International Relative Atomic Weight in.2007).
2 Normative references
The following documents for the application of this document is essential. For dated references, only the dated version applies to this article
Pieces. For undated references, the latest edition (including all amendments) applies to this document.
GB/T 601 chemical reagent standard titration solution preparation
GB/T 603 chemical reagent test methods used in the preparation of preparations and products
GB/T 6435 Determination of moisture in feed
GB/T 6436 Determination of calcium in feed
GB/T 6682 analytical laboratory water specifications and test methods
GB/T 9725 chemical reagent potentiometric titration General
GB 10648 feed label
GB/T 13079 Determination of total arsenic in feed
GB/T 14699.1 feed sampling
GB/T 19371.2 feed methionine hydroxy analogues Determination of high performance liquid chromatography
3 requirements
3.1 Appearance and traits
This product is white, light gray or taupe powder or granules, a unique stench.
3.2 Specifications
Technical indicators should be consistent with the provisions of Table 1.
Table 1 technical indicators
Project Indicators
Methionine hydroxy analog calcium salt content (dry basis) /% ≥ 95.0
Methionine hydroxy analog content (dry basis) /% ≥84.0
Table 1 (continued)
Project Indicators
Calcium /% 11.0 ~ 15.0
Loss on drying /% ≤1.0
Heavy metals (Pb)/(mg/kg) ≤ 20
Total arsenic (As)/(mg/kg) ≤2
4 test methods
Unless otherwise specified, the reagents used are of analytical grade; the water used in chromatographic analysis shall comply with the requirements of Class I water in GB/T 6682, other
Test water in line with the provisions of three water GB/T 6682 provisions; reagents and solution preparation should be consistent with the provisions of GB/T 601 and GB/T 603.
4.1 Sensory test
Under natural light conditions, the product is placed on a white porcelain plate and visually identified as light gray or beige particles. Open the package, product
Odor in the unique stench.
4.2 Identification test
4.2.1 Reagents and solutions
Anhydrous copper sulfate saturated sulfuric acid solution. Take anhydrous copper sulfate by adding concentrated sulfuric acid until precipitation appears.
4.2.2 Amino acid identification method
Weigh the sample 25mg in a dry test tube, add anhydrous copper sulfate saturated sulfuric acid solution (4.2.1) 1mL, the solution was immediately yellow, and then turn
Into yellow-green.
4.2.3 methionine hydroxy analog qualitative identification
4.2.3.1 Reagents and solutions
4.2.3.1.1 Standard. Methionine hydroxy analog calcium salt standard (purity 99%).
4.2.3.1.2 methionine hydroxy analog calcium salt standard solution (100mg/L). Weigh methionine hydroxy analog calcium salt standard (4.2.3.1.1)
0.1g (accurate to 0.0001g), add water after ultrasonic solubilization volume to 100mL, take the solution 10mL, water volume to 100mL.
4.2.3.2 Identification method
Weigh the sample 0.1g (accurate to 0.0001g), add water ultrasonic assisted solution volume to 100mL, take the solution 10mL, water to volume
100mL.
According to GB/T 19371.2 determination, the sample solution of methionine hydroxy analog calcium salt solution peak retention time and methionine hydroxyl
Analogues calcium salt standard solution (4.2.3.1.2) the same, and the hydroxy analog content ≥ 80%.
4.3 methionine hydroxy analog calcium salt and methionine hydroxy analog content determination
4.3.1 Reagents and materials
4.3.1.1 Acid solution. Glacial acetic acid. water. concentrated hydrochloric acid = 50 10 3.
4.3.1.2 potassium bromate - potassium bromide standard titration solution, c (
6KBrO3
) Is about 0.6 mol/L.
Weigh 17.5g potassium bromate (accurate to 0.0001g) and 112.5g potassium bromide (accurate to 0.0001g), dissolved in water after the volume to
1L. According to GB/T 601 provisions of the method of calibration, this solution stored in a brown bottle, valid for one month.
4.3.2 equipment
4.3.2.1 automatic potentiometer or pH meter.
4.3.2.2 platinum saturated calomel electrode composite electrode.
4.3.3 Analysis method
4.3.3.1 Principle
In acidic media, methionine hydroxy analogues undergo the following redox reactions.
3RSR 'BrO-3 → 3RSOR' Br-
In the test solution into a platinum saturated calomel electrode composed of composite electrode (or Pt saturated calomel composite electrode), with the titration
The addition of liquid, the concentration of ions to be tested constantly changing, the electrode potential also occurred in the corresponding changes occur at the equivalence point potential over, in order to determine the titration
end.
4.3.3.2 Procedure
Weigh 0.5g (accurate to 0.0001g) crushed, dried (105 ℃ ± 2 ℃) to a constant weight of the sample in a 150mL beaker, add
50mL acid solution (4.3.1.1), ultrasonic dissolved beaker set magnetic stirrer, the electrode into the solution, adjust the stirring speed to the solution
Fully vortex, potassium bromate - potassium bromide standard titration solution (4.3.1.2) titration, according to GB/T 9725, confirm the titration volume.
4.3.4 Calculation Results
Methionine hydroxy analog calcium salt [(CH3SCH2CH2CHOHCOO) 2Ca] content X1 mass fraction, the value is expressed in%
According to equation (1) calculation.
X1 =
c1 × V1 × 0.0846
m1 ×
100 (1)
In the formula.
c1 --- potassium bromate - potassium bromide standard titration solution concentration in units of moles per liter (mol/L);
V1 --- titration sample consumed potassium bromate - potassium bromide standard titration solution volume, in milliliters (mL);
0.0846 --- and 1.0mL potassium bromate - potassium bromide standard titration solution [c (
6KBrO3
) = 1.0mol/L] equivalent, in grams
The methionine hydroxy analog calcium salt mass;
m1 --- sample quality, in grams (g).
Methionine hydroxy analog [CH3SCH2CH2CHOHCOOH] Content X2 in terms of mass fraction, the value is expressed in%, according to equation (2)
Calculate.
X2 =
c1 × V1 × 0.0751
m1 ×
100 (2)
In the formula.
c1 --- potassium bromate - potassium bromide standard titration solution concentration in units of moles per liter (mol/L);
V1 --- titration sample consumed potassium bromate - potassium bromide standard titration solution volume, in milliliters (mL);
0.0751 --- and 1.0mL potassium bromate - potassium bromide standard titration solution [c (
6KBrO3
) = 1.0mol/L] equivalent, in grams
Of methionine hydroxy analogues;
m1 --- sample quality, in grams (g).
Take two parallel determination of the arithmetic mean measurement results. The result is one decimal place.
4.3.5 Repeatability
The absolute difference between two parallel determination results is not more than 0.2%.
4.4 Determination of loss on drying
According to GB/T 6435 determination.
4.5 Determination of calcium
According to GB/T 6436 determination.
4.6 heavy metals determination
4.6.1 Reagents and solutions
4.6.1.1 Sulfuric acid.
Note that sulfuric acid is a strong corrosive liquid, the operator should wear safety goggles and gloves to prevent burns.
4.6.1.2 Nitric acid.
4.6.1.3 Hydrochloric acid.
4.6.1.4 Lead standard solution .1000μg/mL.
4.6.1.5 Sodium hydroxide solution .40g/L.
4.6.1.6 Ammonia solution (10%) Prepared according to GB/T 603
4.6.1.7 hydrochloric acid solution Ⅰ Take hydrochloric acid 63mL, add water to make 100mL, shake.
4.6.1.8 hydrochloric acid solution II. Take hydrochloric acid 18mL, add water to make 100mL, shake.
4.6.1.9 thioacetamide solution Take thioacetamide 4g, add water to dissolve into 100mL, set the refrigerator for storage. Pro use before
1.0 mL and a mixed solution [consisting of 15 mL of sodium hydroxide solution (4.6.1.5), 5.0 mL of water and 20 mL of glycerol] were placed in a water bath
Heat 20s, mix well, cool and use immediately.
4.6.1.10 Acetate buffer (pH 3.5) Take 25g of ammonium acetate and add 25mL of water to dissolve. Add 38mL of hydrochloric acid solution I (4.6.1.7)
Acid solution Ⅱ (4.6.1.8) or ammonia solution (4.6.1.6) accurately adjust the pH to 3.5 (potentiometer instructions), diluted with water to 100mL,
Shake well.
4.6.1.11 phenolphthalein indicator solution. Prepared according to GB/T 603.
4.6.1.12 Preparation of lead standard working solution Amount of lead standard solution (4.6.1.4) 2.00mL, set.200mL flask, diluted with water to the mark,
Shake well (equivalent to 10 μg of Pb per ml).
4.6.2 Analysis steps
4.6.2.1 Preparation of sample solution
Weigh the sample 1g (accurate to 0.01g), home porcelain crucible, slowly burning to fully carbonized, let cool. Add sulfuric acid (4.6.1.1) 0.5mL ~
1mL humid, low temperature heating to sulfuric acid vapor removed, the ignition at 550 ℃ completely ashed, let cool. Add nitric acid (4.6.1.2) 0.5mL,
Steam dry until the nitrogen oxide vapor removed, let it cool. Add hydrochloric acid (4.6.1.3) 2.0mL, water bath and add water 15mL, ammonia solution was added dropwise
(4.6.1.6) to phenolphthalein indicator solution (4.6.1.11) was reddish, coupled with acetate buffer (4.6.1.10) 2.0mL, after the solution was slightly dissolved, the displacement
Nessler colorimetric tube, diluted with water into 25mL, as B tube.
4.6.2.2 Preparation of standard colorimetric solution
Another preparation of sample solution reagents, home-made porcelain crucible evaporated, add acetate buffer (4.6.1.10) 2.0mL and water 15mL, micro
After thermal dissolution, remove the Nessler colorimetric tube, add 2.0mL of standard working solution (4.6.1.12) of lead and dilute it with water to 25mL as a tube.
4.6.3 determine the result
In A, B two were added thioacetamide solution (4.6.1.9) each 2.0mL, shake, place 2min, with the same white paper, from the top to
Under the perspective of observation and comparison of the color of the tube A and B, such as the color of the tube was not deeper than the A tube, then judged to comply with the provisions.
4.7 Determination of total arsenic
According to GB/T 13079 determination.
5 inspection rules
5.1 group approved
With the same raw materials, the same production process, continuous production or the same batch of products produced for a group.
5.2 Sampling methods
According to GB/T 14699.1.
5.3 factory inspection
Appearance and traits, methionine hydroxy analog content, loss on drying, total arsenic, heavy metals for the factory inspection items.
5.4 type test
Type test items for the provisions of Chapter 3 of all projects. Product normal production, at least once every six months type test, but there
When one of the cases is listed, type tests are also conducted.
a) When the production process and equipment have major changes;
b) when there is a significant change in the raw materials used;
c) stop production for more than three months to resume production;
d) the factory test results and the last type test results are quite different.
5.5 determine the method
Inspection results have an indicator does not meet the requirements of this standard, should be re-sampled twice from the amount of packaging reinspection, retest results even
There is an indicator does not meet the requirements of this standard, the entire batch of products is unqualified.
6 labels, packaging, transportation, storage
6.1 Label
According to the provisions of GB 10648 implementation.
6.2 Packaging
Using paper-plastic composite bags or according to customer requirements packaging, packaging should ensure that the dark.
6.3 Transportation
In the transport process should be dark, moisture-proof, anti-high temperature, to prevent damage to the packaging, non-toxic and hazardous materials mixed operation.
6.4 Storage
Should be stored in a dry, dark place, to prevent rain, toxic substances are prohibited mixed storage.
7 shelf life
Under the stipulated transportation and storage conditions, the shelf life of 24 months from the date of production.
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